Polymer-aerogel / fiber composites and polymer-aerogel / fabric composites and related systems and methods

Abstract

The present disclosure generally relates to polymer-aerogel / fiber composites, polymer-aerogel / fabric composites, and systems and methods for producing the same. In some embodiments, the gel material may comprise a polymer network. The fiber and / or fabric material may comprise at least one of any natural fiber, synthetic fiber, and / or mineral fiber. In some cases, certain combinations of materials, solvents, and / or processing steps may be employed synergistically to enable the manufacture of materials suitable for use in clothing, textiles, and other consumer applications that may benefit from the properties of polymer-aerogel / fiber composites and / or polymer-aerogel / fabric composites.

Description

[0001] Related Applications

[0002] This application claims priority under 35 U.S.C. §119(e) to U.S. Provisional Patent Application No. 62 / 914,298, filed on October 11, 2019, entitled “Polymer-Aerogel / Fiber and Polymer-Aerogel / Textile Composites, and Related Systems and Methods,” and U.S. Provisional Patent Application No. 62 / 914,354, filed on October 11, 2019, entitled “Insitive Polyimide-Aerogel / Fiber Composites for Apparel and Methods of Production,” each of which is incorporated herein by reference in its entirety for all purposes. Technical Field

[0003] Various aspects described herein relate to polymer-aerogel / fiber composites and polymer-aerogel / fabric composites and methods of producing the same. Summary of the invention

[0004] The present disclosure relates to composite materials of polymer aerogels and fibers, and composite materials of polymer aerogels and fabrics, and methods for producing such composite materials. According to certain embodiments, the aerogel material can provide insulating properties. In some cases, the subject matter of the present invention relates to related products, alternative solutions to specific problems, and / or multiple different uses of one or more systems and / or articles.

[0005] It is recognized that combining polymer aerogel materials with fibers or fabrics (such as those used in clothing articles) can produce composite fibers or composite fabrics with improved properties that cannot be achieved with polymer aerogels, fibers or fabrics alone. In some cases, the resulting composites exhibit desirable material properties for use in applications including, but not limited to, clothing, footwear, textiles, aviation interiors, automotive, aerospace, construction, and architecture.

[0006] In some embodiments, a polymer-aerogel / fiber composite can be prepared in which the fiber is a single strand. In certain embodiments, the polymer-aerogel / fiber composite can include a single strand of fiber, and the circumferential volume surrounding the outer surface of the single strand of fiber can include polymer aerogel.

[0007] In some embodiments, a polymer-aerogel / fiber composite material can be prepared in which the fibers are multiple strands. In certain embodiments, in the composite material, some or all of the interstitial spaces between the strands that make up the fibers and / or some or all of the circumferential volume of the outer cross-sectional envelope surrounding the fibers can contain polymer aerogel.

[0008] In some embodiments, a polymer-aerogel / fabric composite material is prepared in which the fabric is a knitted fabric. In other embodiments, a polymer-aerogel / fabric composite material is prepared in which the fabric is a woven fabric. In yet other embodiments, a polymer-aerogel / fabric composite material is prepared in which the fabric is a nonwoven fabric. In certain embodiments, in the composite material, some or all of the interstitial spaces within the fibers constituting the fabric and / or some or all of the spaces between the fibers constituting the fabric may contain polymer aerogel.

[0009] In an illustrative embodiment, a composition is provided. The composition comprises a polymer-aerogel / fiber composite or a polymer-aerogel / fabric composite, wherein the polymer aerogel comprises a polyimide. In certain preferred embodiments, the polyimide is derived from oxydiphenylamine, dimethylbenzidine, dianiline-m and biphenyl dianhydride. In certain preferred embodiments, the fiber comprises polyester, polyamide and / or cotton.

[0010] In some embodiments, polymer-aerogel / fiber composites or polymer-aerogel / fabric composites exhibit lower thermal conductivity than individual bulk fibers or fabrics, respectively. In some embodiments, polymer-aerogel / fiber composites, fabrics comprising polymer-aerogel / fiber composites, or fabrics comprising polymer-aerogel / fabric composites maintain low thermal conductivity when subjected to compressive loads, and correspondingly, when subjected to the same compressive load, the bulk fibers, fabrics comprising individual bulk fibers, or fabrics comprising individual bulk fabrics increase in thermal conductivity. In some embodiments, in the presence of moisture or when wetted by liquid water, the thermal conductivity of polymer-aerogel / fiber composites, fabrics comprising polymer-aerogel / fiber composites, or fabrics comprising polymer-aerogel / fabric composites is correspondingly lower than the thermal conductivity of bulk fibers or fabrics comprising individual bulk fibers under the same conditions.

[0011] In certain embodiments, compositions are provided. In certain embodiments, compositions include polymer-aerogel / fiber composites or polymer-aerogel / fabric composites having mechanical strength and flexibility suitable for incorporation and use in applications including but not limited to clothing, footwear, textiles, aviation interiors, automobiles, aerospace, construction and architecture. In certain embodiments, polymer-aerogel / fiber composites or polymer-aerogel / fabric composites are highly hydrophobic and can withstand normal consumer care washing. In certain embodiments, polymer-aerogel / fiber composites or polymer-aerogel / fabric composites can be integrated into fabrics using industrial standard manufacturing equipment. In an illustrative embodiment, accordingly, relative to a fabric made of a separate bulk fiber or a separate bulk fabric, a fabric incorporated with polymer-aerogel / fiber composites or polymer-aerogel / fabric composites allows water vapor and other gases to pass through the fabric, and liquid water transmission is suppressed through the fabric. In another embodiment, accordingly, relative to a fabric made of a separate bulk fiber or a separate bulk fabric, a fabric incorporated with polymer-aerogel / fiber composites or polymer-aerogel / fabric composites can suppress the flow of air through the fabric. In some embodiments, accordingly, a fabric comprising a polymer-aerogel / fiber composite or a polymer-aerogel / fabric composite can exhibit lower thermal conductivity than a comparable fabric made from a single bulk fiber or a single bulk fabric. In some embodiments, a fabric comprising a polymer-aerogel / fiber composite or a polymer-aerogel / fabric composite can be suitable for use in applications requiring thermal insulation, windproof, waterproof, and breathable functions, such as clothing, footwear, textiles, aviation interiors, automotive, aerospace, construction, and architecture.

[0012] In some embodiments, methods for making polymer-aerogel / fiber composites or polymer-aerogel / fabric composites are provided. In some embodiments, fibers or fabrics are prepared to facilitate incorporation of polymer aerogels onto and / or into fibers or fabrics to produce polymer-aerogel / fiber composites or polymer-aerogel / fabric composites.

[0013] In some embodiments, methods for incorporating a polymer aerogel precursor sol onto and / or into a fiber or fabric are provided.

[0014] According to certain embodiments, methods are provided for incorporating a polymer-aerogel-precursor sol onto and / or into a fiber or fabric and gelling the sol onto and / or into the fiber or fabric.

[0015] In another embodiment, a method for forming a polymer gel on and / or in a fiber or fabric is provided, wherein two components that do not form a gel individually are combined to produce a polymer gel on and / or in a fiber or fabric. In some embodiments, the amount of polymer-aerogel / fiber composite or polymer-aerogel / fabric composite that can be produced in a single batch may be limited by the gel time of the polymer aerogel precursor. In some embodiments, a method for forming a polymer gel is provided, the method employing mixing two separate components that form a polymer gel within a specific amount of time, the method can be suitable for producing large quantities of polymer-aerogel / fiber composites or polymer-aerogel / fabric composites, for example, by achieving production of polymer-aerogel / fiber composites or polymer-aerogel / fabric composites in a continuous process, such as in a roll-to-roll manner.

[0016] In certain embodiments, the polymer-gel / fiber composite or polymer-gel / fabric composite may be immersed in a solvent bath to replace the pore fluid composition within the polymer-gel with additional pore fluid.

[0017] In some embodiments, the polymer-gel / fiber composite or polymer-gel / fabric composite can be further processed to produce a polymer-aerogel / fiber composite or a polymer-aerogel / fabric composite. In some embodiments, a method for producing a polymer-aerogel / fiber composite or a polymer-aerogel / fabric composite by a supercritical extraction method is provided. In other embodiments, a method for producing a polymer-aerogel / fiber composite or a polymer-aerogel / fabric composite at atmospheric pressure is provided. In certain embodiments, the method can be performed in a continuous process, for example, in a roll-to-roll manner.

[0018] Other advantages and novel features of the present invention will become apparent from the following detailed description of multiple non-limiting embodiments of the present invention when considered in conjunction with the accompanying drawings. In the event that this specification and the documents incorporated by reference contain conflicting and / or inconsistent disclosures, this specification shall prevail. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Non-limiting embodiments of the present invention will be described by way of example with reference to the accompanying drawings, which are schematic and are not intended to be drawn to scale. In the drawings, each identical or nearly identical component shown is typically represented by the same reference numeral. For clarity, not every component is labeled in every drawing, nor is every component of every embodiment of the present invention shown, where illustration is not required for one of ordinary skill in the art to understand the present invention. In the drawings:

[0020] Figure 1 Depicted is a cross-sectional area of ​​a single-strand fiber having a conformal coating comprising a polymer aerogel, according to some embodiments.

[0021] Figure 2A Depicted is a cross-sectional area of ​​a multi-strand fiber in which a polymer aerogel material infiltrates the spaces between strands of the fiber, according to some embodiments.

[0022] Figure 2B Depicted is a cross-sectional area of ​​a multi-strand fiber in which a conformal coating of polymer aerogel material surrounds individual strands of the fiber, according to some embodiments.

[0023] Figure 3 Depicted are materials in which a polymer-aerogel / fiber composite has been incorporated into a fabric, according to some embodiments.

[0024] Figure 4 Depicted is a standard industrial manufacturing process in which a polymer-aerogel / fiber composite can be incorporated into a fabric according to some embodiments.

[0025] Figure 5 Depicted are polymer-aerogel / fiber composites in which the polymer aerogel material is substantially continuous along the length of the fiber, according to some embodiments.

[0026] Fig. 6A Depicted are examples of polymer-aerogel / fiber composites in which the polymer aerogel material is discontinuous along the length of the fiber, according to some embodiments.

[0027] Figure 6B Depicted are examples of polymer-aerogel / fiber composites in which the polymer aerogel material is discontinuous around a single-strand fiber or around any given strand in a multi-strand fiber in any given cross-section of the composite, according to some embodiments.

[0028] Fig. 7A Depicted is a portion of a construction of a dual-layer mat comprising a polymer-aerogel / fiber composite material, according to some embodiments.

[0029] Figure 7B Depicted are methods for measuring thermal conductivity according to the Calibrated Hot Plate (CHP) method described herein, according to some embodiments.

[0030] Figure 7C Depicted Figure 7B 3-dimensional view of the method depicted in .

[0031] Figure 8Depicted is a method for immersing a composite material sample in water at 25° C. to measure liquid water absorption, according to some embodiments.

[0032] Fig. 9 Depicted are methods of forming a spool of fiber using a tension controller to control the tension of the fiber from a larger volume spool, according to some embodiments.

[0033] Fig.10 Depicted is a method of infiltrating a fiber spool by immersing or partially immersing the spool in a liquid solution comprising a polymer-aerogel-precursor according to some embodiments.

[0034] Fig.11 Depicted are methods of infiltrating fibers with a liquid solution comprising a polymer-aerogel-precursor in a continuous or semi-continuous manner according to some embodiments.

[0035] Fig.12 Depicted is a method of infiltrating fibers with a liquid solution comprising a polymer-aerogel-precursor in a roll-to-roll manner according to some embodiments.

[0036] Fig.13 Depicted are methods of infiltrating fibers with a liquid solution comprising a polymer-aerogel-precursor, wherein the liquid solution is prepared in a continuous or semi-continuous manner, according to some embodiments.

[0037] Fig.14 Depicted is a method of infiltrating a fiber with a liquid solution comprising a polymer-aerogel-precursor in a continuous or semi-continuous manner in two sequential steps according to some embodiments.

[0038] Fig.15A Depicted is a cross-sectional area of ​​a single strand fiber according to some embodiments, wherein a liquid solution containing a polymer-aerogel-precursor forms a continuous polymer gel on and / or within the fiber after a period of time, thereby forming a polymer-gel / fiber composite.

[0039] Fig. 15B Depicted is a cross-sectional area of ​​a multi-strand fiber according to some embodiments, wherein a liquid solution containing a polymer-aerogel-precursor forms a polymer gel on the fiber and / or in the spaces between the strands of the fiber after a period of time, thereby forming a polymer-gel / fiber composite.

[0040] Fig. 15C Depicted is a cross-sectional area of ​​a multi-strand fiber, according to some embodiments, wherein a liquid solution containing a polymer-aerogel-precursor forms a conformal coating of polymer gel around individual strands of the fiber, thereby forming a polymer-gel / fiber composite.

[0041] Fig.15DDepicted is a cross-sectional area of ​​a single strand fiber according to some embodiments, wherein a liquid solution containing a polymer-aerogel-precursor forms a discontinuous polymer gel on and / or within the fiber after a period of time, thereby forming a polymer-gel / fiber composite.

[0042] Fig.16 Depicted is a method of infiltrating a fiber with a liquid solution comprising a polymer-aerogel-precursor in a continuous or semi-continuous process by passing the fiber through a bath of a Part A liquid solution and then through a vapor environment, according to some embodiments.

[0043] Fig.17 Depicted are methods in which a pore fluid of a polymer-gel / fiber composite is replaced with a different pore fluid, according to some embodiments.

[0044] Fig.18 Depicted are methods in which the pore fluid of a polymer-gel / fiber composite is replaced with an additional solvent in a continuous or semi-continuous process, according to some embodiments.

[0045] Fig.19 Depicted are methods in which the pore fluid of a polymer-gel / fiber composite is replaced with additional solvent in a roll-to-roll manner, according to some embodiments.

[0046] Fig. 20 Depicted are methods according to some embodiments in which a polymer-gel / fiber composite is placed in a drying chamber to remove pore fluid in the polymer-gel material to produce a polymer-aerogel / fiber composite.

[0047] Fig.21 Depicted are methods in which a polymer-aerogel / fiber composite is subjected to a continuous or semi-continuous process of moving the polymer-gel / fiber composite through a drying chamber to produce a polymer-aerogel / fiber composite, according to some embodiments.

[0048] Fig. 22 Depicted are methods in which a polymer-gel / fiber composite is processed in a roll-to-roll manner through a drying chamber to produce a polymer-aerogel / fiber composite according to some embodiments.

[0049] Fig.23 Depicted are methods of mechanically treating a polymer-aerogel / fiber composite on a sharp edge, according to some embodiments.

[0050] Fig.24 Depicted are methods of mechanically treating polymer-aerogels / fibers by an industrial texturing machine according to some embodiments.

[0051] Fig.25A An example of a polymer-aerogel / fabric composite material according to some embodiments is depicted, comprising: a fabric; and a polymer aerogel material that may be found infiltrated into spaces between fibers of the fabric and / or into pores within the fibers comprising the fabric.

[0052] Fig.25B An example of a polymer-aerogel / fabric composite material is depicted, according to some embodiments, comprising: a fabric; and a conformal coating of a polymer aerogel material that may be found on an outer surface of the fabric.

[0053] Fig.25C An example of a woven polymer-aerogel / fabric composite is depicted, comprising: a fabric; and a polymer aerogel material.

[0054] Fig.25D An example of a knitted polymer-aerogel / fabric composite is depicted, comprising: a fabric; and a polymer aerogel material.

[0055] Fig.25E An example of a nonwoven polymer-aerogel / fabric composite is depicted, comprising: a fabric; and a polymer aerogel material.

[0056] Fig.26 An example of a cross-sectional area of ​​a polymer-aerogel / fabric composite material is depicted, according to some embodiments, wherein the polymer aerogel material is substantially continuous over the surface of any given cross-section of the fabric.

[0057] Fig.27A An example of a polymer-aerogel / fabric composite material is depicted in accordance with some embodiments, wherein the polymer aerogel material is substantially discontinuous along the length of the fabric.

[0058] Fig.27B Depicted are cross-sectional regions of polymer-aerogel / fabric composites according to some embodiments, wherein the polymer aerogel material is substantially discontinuous across the surface of any given cross-section of the fabric.

[0059] Fig.28 Depicted are methods that may be used according to some embodiments in which a polymer-aerogel / fabric composite is deknitted into a polymer-aerogel / fiber composite using standard industrial deknitting equipment.

[0060] Fig.29 Depicted is a method of infiltrating a spool of fabric by immersing or partially immersing the spool in a liquid solution comprising a polymer-aerogel-precursor, according to some embodiments.

[0061] Fig.30 Depicted is a method of infiltrating a prefabricated garment by immersing or partially immersing the garment in a liquid solution comprising a polymer-aerogel-precursor according to some embodiments.

[0062] Fig.31 Depicted are methods of infiltrating a fabric with a liquid solution comprising a polymer-aerogel-precursor in a continuous or semi-continuous process according to some embodiments.

[0063] Fig.32 Depicted is a method of impregnating a fabric with a liquid solution comprising a polymer-aerogel-precursor in a roll-to-roll manner according to some embodiments.

[0064] Fig.33 Depicted are methods of infiltrating a fabric with a liquid solution comprising a polymer-aerogel-precursor, wherein the liquid solution is prepared in a continuous or semi-continuous manner, according to some embodiments.

[0065] Fig.34 Depicted is a method of infiltrating a fabric with a liquid solution comprising a polymer-aerogel-precursor in a continuous or semi-continuous manner in two sequential steps according to some embodiments.

[0066] Fig.35A Depicted is a cross-sectional area of ​​a polymer-gel / fabric composite material in which a liquid solution comprising a polymer-aerogel-precursor forms a discontinuous polymer gel on and / or within a fabric, according to some embodiments.

[0067] Fig.35B Depicted is a cross-sectional area of ​​a polymer-gel / fabric composite material in which a liquid solution comprising a polymer-aerogel-precursor forms a continuous polymer gel on and / or within a fabric, according to some embodiments.

[0068] Fig.36 Depicted is a method of infiltrating a fabric with a liquid solution comprising a polymer-aerogel-precursor in a continuous or semi-continuous process by passing the fabric through a bath of a Part A liquid solution and then through a vapor environment, according to some embodiments.

[0069] Fig.37 Depicted are methods according to some embodiments in which the pore fluid of a polymer-gel / fabric composite is replaced with a different solvent by placing a roll of fabric into a bath or series of baths.

[0070] Fig.38 Depicted are methods according to some embodiments in which the pore fluid of a polymer-gel / fabric composite is replaced with additional solvent in a continuous or semi-continuous process by passing the fabric through a solvent bath.

[0071] Fig.39 Depicted are methods in which the pore fluid of a polymer-gel / fabric composite is replaced with additional solvent on a roll-to-roll basis, according to some embodiments.

[0072] Fig.40 Depicted are methods in which a polymer-gel / fabric composite is dried to produce a polymer-aerogel / fabric composite according to some embodiments.

[0073] Fig.41 Depicted are methods according to some embodiments in which a polymer-gel / fabric composite is subjected to a continuous or semi-continuous drying process to produce a polymer-aerogel / fabric composite.

[0074] Fig.42 Depicted are methods in which a polymer-gel / fabric composite is processed in a roll-to-roll drying process to produce a polymer-aerogel / fabric composite according to some embodiments.

[0075] Fig.43 Depicted are methods of mechanically treating or finishing a polymer-aerogel / fabric composite to mechanically separate fibers of the fabric composite from one another and remove excess polymer aerogel material, according to some embodiments. DETAILED DESCRIPTION

[0076] The present disclosure generally relates to composite materials of polymer aerogels and fibers and composite materials of polymer aerogels and fabrics and methods for producing such composite materials. Certain embodiments of the present invention relate to a group of material compositions comprising polymer-based aerogel materials composited with traditional textile fibers or fabrics, and methods for making the composite materials. As provided herein, such composite materials are generally referred to as polymer-aerogel / fiber composite materials or polymer-aerogel / fabric composite materials, respectively. For the purposes of the present disclosure, the terms "polymer-aerogel / fiber composite materials", "composite fibers" and "fiber composite materials" are used interchangeably throughout the specification and claims. For the purposes of the present disclosure, the terms "polymer-aerogel / fabric composite materials", "composite fabrics" and "fabric composite materials" are used interchangeably throughout the specification and claims. In some embodiments, the polymer-aerogel / fiber composite material comprises fibers and polymer aerogel materials on the outer surface of the fibers. In certain embodiments, the polymer-aerogel / fiber composite material comprises fibers and polymer aerogel materials infiltrated into the pores within the fibers. In some embodiments, the polymer-aerogel / fiber composite material comprises fibers and polymer aerogel materials both on the outer surface of the fibers and infiltrated into the pores within the fibers. Those of ordinary skill in the art are familiar with fibers, which are elongated strands of material that can be arranged (e.g., knitted, woven, etc.) into fabrics and other textiles. In some embodiments, the fibers are or include single-strand fibers (e.g., monofilament fibers). For example, in Figure 1 In the embodiment, the polymer-aerogel / fiber composite material comprises a polymer aerogel (2) on the outer surface of a single-strand fiber (1), as shown in the cross-sectional view. In some embodiments, the fiber is a multi-strand fiber (e.g., yarn, thread, spun fiber, etc.) or comprises a multi-strand fiber (e.g., yarn, thread, spun fiber, etc.). For example, in Figure 2A In one embodiment, the polymer-aerogel / fiber composite material comprises a polymer aerogel (2) on the outer surface of a fiber (1) and infiltrated into the pores of the fiber (1), wherein the fiber (1) comprises a plurality of strands, as shown in a cross-sectional view. In another embodiment, Figure 2B In the embodiment, the polymer-aerogel / fiber composite material comprises a polymer aerogel (2) conformally coating the strands of a multi-strand fiber (1), as shown in the cross-sectional view. In some embodiments, the polymer-aerogel / fabric composite material comprises a fabric and a polymer aerogel material on the outer surface of the fabric. In certain embodiments, the polymer-aerogel / fabric composite material comprises a fabric and a polymer aerogel material infiltrated into pores within the fabric. In some embodiments, the polymer-aerogel / fabric composite material comprises a fabric and a polymer aerogel material both on the outer surface of the fabric and infiltrated into pores within the fabric. For example, in Fig.25AIn one embodiment, the polymer-aerogel / fabric composite material comprises a polymer aerogel (2) infiltrated into the pores of a fabric (24). In another embodiment, Fig.25B In the embodiment of the present invention, the polymer-aerogel / fabric composite material comprises a polymer aerogel (2) on the outer surface of a fabric (24). One of ordinary skill in the art is familiar with fabrics, which are made from fibers into structures such as woven fabrics, knitted fabrics, or nonwoven fabrics. In some embodiments, the fabric comprises a woven fabric. In other embodiments, the fabric comprises a knitted fabric. In yet other embodiments, the fabric comprises a nonwoven fabric. For example, in Fig.25C In another example, the fabric composite material (25) comprises a knitted fabric. Fig.25D In another example, the fabric composite material (25) comprises a woven fabric. Fig.25E In the invention, the fabric composite material (25) comprises a nonwoven fabric.

[0077] Those of ordinary skill in the art are familiar with woven fabrics, knitted fabrics, and nonwoven fabrics. The term knitted refers to a non-random structure mechanically held together by yarns by interlocking a series of loops from one or more yarns or from a group of yarns. Types of knitted fabrics may include, but are not limited to, flat knits, circular knits, warp knits, or engineered knits. Types of warp knits may include, but are not limited to, tricot, raschel, or lace. Types of circular single-sided knits may include, but are not limited to, plain knits, jacquards, terry fabrics, napped fabrics, fleece fabrics, French terry, or leno fabrics. Types of circular double-sided knits may include, but are not limited to, interlocked knits, ribs, or jacquards. The term woven fabric refers to a non-random structure mechanically held together by interlacing two yarns so that they cross each other at right angles to produce a fabric in which the warp yarns extend longitudinally and the weft yarns extend from one side to the other. Types of woven fabrics may include, but are not limited to, plain, basket, twill, satin, dobby, jacquard, crepe, double-layer, fleece, or combinations thereof. The term nonwoven refers to a structure composed of fibers that do not have a woven or interwoven structure. Types of nonwovens may include, but are not limited to, carded webs, spunlace, spunbond, meltblown, needlepunched, fusible, and felt.

[0078] As used herein, the term "fabric" includes fabrics that have not yet been made into garments or otherwise incorporated into garments, as well as fabrics that have been made into garments or otherwise incorporated into garments. In some embodiments, the fabric may be treated to produce a polymer-aerogel / fabric composite before it is made into garments. In some embodiments, the fabric may already comprise a garment when it is treated to produce a polymer-aerogel / fabric.

[0079] As provided herein, polymer-aerogel / fiber composites and polymer-aerogel / fabric composites are distinguished from fiber-reinforced aerogel composites, such as blankets and boards found in industry, where, for example, the fluff is infiltrated with aerogel.

[0080] In some embodiments, the fiber includes a multi-strand fiber, and the multi-strand fiber includes a pore between its constituent strands, that is, a porous multi-strand fiber. The pore of a multi-strand fiber refers to the space between the constituent strands of the fiber. In some embodiments, when used in a polymer-aerogel / fiber composite material, some or all of the pores of the multi-strand fiber can be occupied by aerogel. In some embodiments, the pore of the fiber affects the amount of polymer aerogel that can be incorporated into the fiber and / or in the fiber. In certain embodiments, the pore of the fiber serves as the volume of the absorbed polymer-aerogel precursor solution.

[0081] In certain embodiments, when the fiber is wound onto the bobbin, the fiber bobbin contains its own porosity due to the inter-fiber porosity. The porosity of the fiber bobbin refers to the space between the fibers wound onto the bobbin and the porosity of the fibers. In some embodiments, when the fiber bobbin is made into a polymer-aerogel / fiber composite material, some or all of the porosity of the fiber bobbin may be occupied by aerogel. In an illustrative embodiment, a porous fiber bobbin comprising porous multi-strand fibers is prepared, and the porosity of the fiber bobbin serves as the volume of the absorbed polymer-aerogel-precursor solution.

[0082] For the purpose of the present disclosure, the terms "polymer-aerogel precursor solution" and "liquid solution comprising a polymer-aerogel-precursor" are used interchangeably throughout the specification and claims.

[0083] In some embodiments, the fabric includes a knitted fabric, a woven fabric or a nonwoven fabric containing its own pores. The pores of the fabric refer to the spaces between the fibers constituting the fabric and the pores of the fibers constituting the fabric. In certain embodiments, the pores of the fabric serve as the volume of the absorbed polymer-aerogel precursor solution. In some embodiments, the fiber is selected as the base substrate of the polymer-aerogel / fiber composite material. In some embodiments, the fiber includes manufactured fibers, such as but not limited to synthetic fibers and / or cellulose fibers. In certain embodiments, the fiber includes synthetic fibers, such as but not limited to polyester, polyamide, polyimide, acrylic, spandex and / or other commonly used fibers. In certain embodiments, the fiber includes cellulose fibers, such as but not limited to bamboo, acetate and / or rayon. In certain embodiments, the fiber includes natural fibers, such as but not limited to cotton, wool and / or silk. In some preferred embodiments, the fiber includes polyester, polyamide or cotton. In certain embodiments, the fiber includes industrial fibers, such as but not limited to glass, carbon, para-aramid or meta-aramid. In some embodiments, the fiber includes fire-resistant fibers, such as but not limited to fire-resistant polyester. In some embodiments, the fibers include self-extinguishing fibers such as, but not limited to, cotton. Figure 1 In the composite fiber, the fiber (1) may include polyester, polyamide, cotton and / or other types of fibers. In some embodiments, the fiber includes a blend of one or more fiber types. For example, in Figure 2A In the composite fiber, the multi-stranded fibers (1) may include a blend of polyester, polyamide, cotton and / or other types of fibers. In some embodiments, the fibers include bicomponent or multicomponent fibers in which two or more synthetic fiber types are coextruded into a single fiber.

[0084] According to certain embodiments, a number of mechanical properties of the polymer aerogel, such as strength, modulus, elasticity, and radius of curvature, may be important for determining a suitable polymer aerogel for incorporation into a polymer-aerogel / fiber composite or a polymer-aerogel / fabric composite. In some embodiments, the aerogel has suitable mechanical properties that allow the polymer-aerogel / fiber composite to be incorporated into, for example, a fabric and / or allow the polymer-aerogel / fiber composite to be used in a target application (e.g., clothing and textiles). As a non-limiting example, if the aerogel is too weak and / or too brittle relative to the polymer aerogel, such as may be the case with silica aerogels, most of the aerogel may be easily worn off the fiber or fabric.

[0085] In an illustrative embodiment, a composition is provided. In some embodiments, the composition comprises a polymer-aerogel / fiber composite material, wherein the polymer aerogel comprises a polyimide. In certain embodiments, the polyimide comprises a polyimide backbone derived from oxydiphenylamine, dimethylbenzidine, dianiline-m and biphenyl dianhydride. In some embodiments, the polymer-aerogel / fiber composite material wherein the polymer aerogel comprises a polyimide has specific advantages over other compositions, such as, but not limited to, suitable mechanical properties, non-flammability, high temperature resistance, low thermal conductivity and hydrophobicity as described above.

[0086] In an illustrative embodiment, a composition is provided. The composition comprises a polymer-aerogel / fiber composite material, wherein the polymer aerogel comprises a polyurea. In certain embodiments, the polyurea comprises a polyurea backbone derived from the reaction of an isocyanate with an amine formed in situ. In some embodiments, the polymer-aerogel / fiber composite material wherein the polymer aerogel comprises a polyurea has specific advantages over other compositions, such as, but not limited to, suitable mechanical properties, simplified chemical properties, low cost, low thermal conductivity, and hydrophobicity as described above.

[0087] In some embodiments, a fabric is selected as the base substrate for the polymer-aerogel / fabric composite. In some embodiments, the fabric comprises manufactured fibers, such as, but not limited to, synthetic fibers and / or cellulose fibers. In certain embodiments, the fabric comprises synthetic fibers, such as, but not limited to, polyester, polyamide, polyimide, acrylic, spandex, and / or other commonly used fibers. In certain embodiments, the fabric comprises cellulose fibers, such as, but not limited to, bamboo, acetate, and / or rayon. In certain embodiments, the fabric comprises natural fibers, such as, but not limited to, cotton, wool, and / or silk. In some preferred embodiments, the fabric comprises polyester, polyamide, and / or cotton. For example, in Fig.25B In the fabric composite material, the fabric (24) may include polyester, polyamide, cotton, and / or other types of fibers. In some embodiments, the fabric may include a blend of two or more fiber types. For example, in Fig.25B In the fabric composite material, the fabric (24) can include a blend of polyester, polyamide, cotton and / or other types of fibers. In certain embodiments, the fabric includes industrial fibers, such as but not limited to glass, carbon, para-aramid or meta-aramid. In some embodiments, the fabric includes fire-resistant fibers, such as but not limited to fire-resistant polyester. In some embodiments, the fabric includes self-extinguishing fibers, such as but not limited to cotton. In some embodiments, the fabric includes bicomponent or multicomponent fibers. In some embodiments, the fabric includes a blend of two or more of the aforementioned fiber compositions.

[0088] In one illustrative embodiment, a composition is provided. According to certain embodiments, the composition comprises a polymer-aerogel / fabric composite material, wherein the polymer aerogel comprises a polyimide. In certain embodiments, the polyimide comprises a polyimide backbone derived from oxydiphenylamine, dimethylbenzidine, dianiline-m, and biphenyl dianhydride.

[0089] In one illustrative embodiment, a composition is provided. According to certain embodiments, the composition comprises a polymer-aerogel fabric composite, wherein the polymer aerogel comprises a polyurea. In certain embodiments, the polyurea comprises a polyurea backbone derived from the reaction of an isocyanate with an amine formed in situ.

[0090] In some embodiments, the aerogel in a polymer-aerogel / fiber composite or polymer-aerogel / fabric composite is mechanically bonded to the fiber or fabric, such as an aerogel geometrically interwoven with the fiber or fabric. In certain embodiments, the aerogel in a polymer-aerogel / fiber composite or polymer-aerogel / fabric composite is chemically bonded to the fiber or fabric, such as an aerogel covalently bonded to the fiber or fabric. In some embodiments, the aerogel in a polymer-aerogel / fiber composite or polymer-aerogel / fabric composite can be bonded to the fiber or fabric by a combination of chemical and mechanical attachment.

[0091] In some embodiments, the mass fraction of polymer-aerogel in the polymer-aerogel / fiber composite is greater than 1%, greater than 5%, greater than 10%, greater than 15%, greater than 20%, greater than 25%, greater than 30%, greater than 35%, or greater than 50%. For example, Figure 1 In the embodiment of the present invention, the polymer aerogel (2) can account for a certain percentage of the total mass of the fiber composite material. In some embodiments, the polymer aerogel in the polymer-aerogel / fiber composite material comprises polyimide. In some embodiments, the mass fraction of the polyimide-aerogel in the polymer-aerogel / fiber composite material is greater than 1%, greater than 5%, greater than 10%, greater than 15%, greater than 20%, greater than 25%, greater than 30%, greater than 35%, or greater than 50%. For example, in Figure 1 In the embodiment, the polymer aerogel (2) may include polyimide, and the polyimide may account for a certain percentage of the total mass of the fiber composite material. In some embodiments, the mass fraction of the polymer-aerogel in the polymer-aerogel / fabric composite material is greater than 1%, greater than 5%, greater than 10%, greater than 15%, greater than 20%, greater than 25%, greater than 30%, greater than 35%, or greater than 50%. For example, in Fig.25BIn the embodiment of the present invention, the polymer aerogel (2) may account for a certain percentage of the total mass of the fabric composite material shown. The mass fraction of aerogel loaded onto the fiber or fabric can be measured by comparing the mass of the bulk fiber or fabric with the mass of the polymer-aerogel / fiber composite or the polymer-aerogel / fabric composite. In some embodiments, when the polymer-aerogel / fiber composite is formed into a mat as defined herein, the volume fraction of aerogel is less than 1%, less than 5%, less than 10%, less than 15%, or between 15% and 100%. The volume fraction of aerogel in the mat is calculated by multiplying the known mass fraction of aerogel in the composite material by the density of the composite mat measured at 0.31 psi (to obtain the effective aerogel density in the mat), and then dividing this amount by the known bulk density of the aerogel material.

[0092] In some embodiments, polymer-aerogel / fiber composites are incorporated into fabrics. In some embodiments, polymer-aerogel / fiber composites can be woven, knitted, or otherwise incorporated into fabrics. The fabric can comprise a woven structure, a knitted structure, a nonwoven structure, or a combination thereof. In some embodiments, the composite fibers described herein account for at least 1% by weight, at least 5% by weight, at least 10% by weight, at least 25% by weight, at least 50% by weight, or at least 99% of the fabric comprising the composite fibers. In some embodiments, the composite fibers described herein account for 100% of the fabric comprising the composite fibers. In some embodiments, the composite fibers can be knitted into fabrics using standard commercial knitting equipment. For example, in Figure 3 In another example, the polymer-aerogel / fiber composite material (3) is incorporated into the fabric. Figure 4 As shown, the fiber composite material (3) is knitted into a fabric (31) comprising the fiber composite material using commercial knitting equipment (32). In some embodiments, the composite fibers may be knitted using equipment such as, but not limited to, a single cylinder circular knitting machine.

[0093] In some embodiments, the polymer-aerogel / fiber composite material can exhibit any minimum radius of curvature suitable for knitting, weaving, or otherwise incorporating into a fabric. In some embodiments, the polymer-aerogel / fiber composite material can exhibit a minimum radius of curvature of less than 0.1 mm, less than 0.25 mm, less than 0.5 mm, less than 1 mm, less than 5 mm, or less than 1 cm.

[0094] In some embodiments, the polymer-aerogel / fabric composite material can exhibit any suitable minimum radius of curvature. In some embodiments, the radius of curvature can be suitable for incorporating the fabric composite material into clothing. In some preferred embodiments, the polymer-aerogel / fiber composite material can exhibit a minimum radius of curvature of less than 0.1 mm, less than 0.25 mm, less than 0.5 mm, less than 1 mm, less than 5 mm, or less than 1 cm.

[0095] In certain embodiments, the polymer-aerogel / fiber composite or polymer-aerogel / fabric composite can exhibit mechanical strength and flexibility suitable for incorporation into, for example, clothing applications and for use in, for example, apparel applications. In some preferred embodiments, the polymer-aerogel / fiber composite or polymer-aerogel / fabric composite is highly hydrophobic and can withstand normal consumer care laundering according to the procedures outlined in the AATCC LP1 standard for home landering.

[0096] In certain embodiments, polymer-aerogel / fiber composites can show suitable breaking force. Breaking force can be determined according to the process outlined in ASTM D2256 by the standard test method for tensile properties of yarns measured by the single-strand method or any other suitable standard. In some embodiments, polymer-aerogel / fiber composites can show a breaking force within 10%, 15%, 20%, 25%, 30%, 40%, 50%, 60%, 70%, 75%, 80%, 85%, 90%, 95%, 100%, 110%, 120%, 130%, 140%, or 150% of the breaking force of the bulk fiber.

[0097] In some embodiments, the distribution of the polymer aerogel material on the fiber is substantially continuous along the length of the composite fiber. Figure 5 In some embodiments, the polymer aerogel (2) in the fiber composite is substantially continuous along the length of the fiber (1). In some embodiments, the aerogel may conformally coat some or all of the fibers and / or some or all of the strands of a multi-stranded fiber. In some embodiments, the polymer aerogel material is discontinuous along the length of the composite fiber. For example, in Fig. 6A and 6BIn the fiber composite, the polymer aerogel (2) is substantially discontinuous along the length of the fiber (1), as shown in the 3D and cross-sectional views, respectively. That is, along the length of the polymer-aerogel / fiber composite, the amount of aerogel in any given cross-sectional area of ​​the composite varies. In one example, the aerogel is nearly uniformly distributed along the length of the fiber.

[0098] In some embodiments, the polymer aerogel in the polymer-aerogel / fiber composite comprises polyimide. In some embodiments, the distribution of the polyimide aerogel material on the fiber is substantially continuous along the length of the composite fiber. In some embodiments, the polyimide aerogel material is discontinuous along the length of the composite fiber.

[0099] In some embodiments, the distribution of the polymer aerogel material on the fabric is substantially continuous across the surface of any given cross-section of the composite fabric. Fig.26 In some embodiments, the polymer aerogel (2) in the fabric composite material is substantially continuous on the surface of the fabric (25). In some embodiments, the aerogel may conformally coat some or all of the fibers that make up the fabric and / or some or all of the strands of the multi-stranded fibers that make up the fabric. In some embodiments, the polymer aerogel material is substantially discontinuous on the surface of any given cross-section of the composite fabric. For example, in Fig.27A and Fig.27B In the fabric composite material, the polymer aerogel (2) is substantially discontinuous on the surface of the fabric (25), as shown in the cross-sectional view. That is, the amount of aerogel on the surface of any given cross-section of the composite fabric varies.

[0100] In some embodiments, the polymer aerogel in the polymer-aerogel / fabric composite comprises polyimide. In some embodiments, the distribution of the polyimide aerogel material on the fabric is substantially continuous on the surface of any given cross-section of the composite fabric. In some embodiments, the polyimide aerogel material is discontinuous on the surface of any given cross-section of the composite fabric.

[0101] In some embodiments, the thermal conductivity of a polymer-aerogel / fiber composite or bulk fiber is measured. In some embodiments, a polymer-aerogel / fiber composite or bulk fiber is prepared by forming a mat for this measurement. A mat is defined herein as one or more sheets or one or more layers of oriented bulk fibers or polymer-aerogel / fiber composites. A mat may include a single layer mat or a multilayer mat. A single layer mat contains fibers that are oriented parallel to each other on a flat horizontal surface and are evenly distributed on a surface orthogonal to the fiber orientation, so that there is contact between adjacent fibers and a single layer mat of uniform thickness is achieved. A multilayer mat includes two or more such single layers arranged on top of each other, with the fibers in each layer oriented orthogonally to the adjacent layers, thereby achieving a multilayer fiber mat. For example, as Fig. 7A As shown, the sample portion of the pad is shown to include two layers of polymer-aerogel / fiber composite material (3). In some embodiments, a fabric comprising a polymer-aerogel / fiber composite material or bulk fibers can be prepared, and the thermal conductivity of a single layer or multiple layers of the fabric can be measured. In some embodiments, the thermal conductivity of the polymer-aerogel / fabric composite material or bulk fabric can be measured as a single layer or multiple layers. The thermal conductivity of the pad or fabric can be measured by the method described herein. The thermal conductivity of the pad or fabric comprising the polymer-aerogel / fiber composite material can be compared with a pad or fabric of a comparably constructed material comprising separate bulk fibers. The thermal conductivity of the fabric comprising the polymer-aerogel / fabric composite material can be compared with a comparably constructed material comprising separate bulk fibers.

[0102] In some embodiments, when the polymer-aerogel / fiber composite is formed into a mat as defined herein and the thermal conductivity is measured by the calibrated hot plate (CHP) method described herein at an average sample temperature of 25° C. and an applied pressure of 0.31 psi, the composite exhibits a thermal conductivity of less than 80 mW / mK or less than 40 mW / mK. For example, Fig. 7A As shown, the fiber composite material can be made into a mat. Figure 7B and Figure 7C As shown, the thermal conductivity of sample (6) (including the mat in this case) can be measured using the CHP method to be less than 80 mW / mK or less than 40 mW / mK. In some embodiments, the thermal conductivity of the mat can be measured using the ASTM C518 method to be less than 80 mW / mK or less than 40 mW / mK.

[0103] In some embodiments, the fabric comprising the polymer-aerogel / fiber composite exhibits a thermal conductivity of less than 80 mW / mK or less than 40 mW / mK when measured by the calibrated hot plate (CHP) method described herein at an average sample temperature of 25° C. and an applied pressure of 0.31 psi. In some embodiments, the thermal conductivity of the fabric comprising the polymer-aerogel / fiber composite can be measured using the ASTM C518 method to be less than 80 mW / mK or less than 40 mW / mK.

[0104] In some embodiments, the polymer-aerogel / fabric composite exhibits a thermal conductivity of less than 80 mW / mK or less than 40 mW / mK when the thermal conductivity is measured by the calibrated hot plate (CHP) method described herein at an average sample temperature of 25°C and an applied pressure of 0.31 psi. Figure 7B and Figure 7C As shown, the thermal conductivity of sample (6) (in this case, the fabric composite material) can be measured using the CHP method to be less than 80 mW / mK or less than 40 mW / mK. In some embodiments, the thermal conductivity of the fabric composite material can be measured using the ASTM C518 method to be less than 80 mW / mK or less than 40 mW / mK.

[0105] An exemplary method for measuring thermal conductivity is the calibrated hot plate method as follows. Thermal conductivity can be measured using a calibrated hot plate (CHP) apparatus. The CHP method is based on the basic principles of ASTM E1225 "Standard Test Method for Thermal Conductivity of Solids by Means of the Guarded-Comparative-Longitudinal HeatFlow Technique". An apparatus in which aerogels and other sample materials (whose mass, thickness, length, and width have been measured as described in the process for measuring bulk density described herein) are placed continuously between a hot surface and a cold surface along with a standard reference material (e.g., NIST SRM 1453 EPS plate) of precisely known thermal conductivity, density, and thickness. The hot side of the system consisted of an aluminum block (4" x 4" x 1") in which three cartridge heaters were embedded. The cartridge heaters were controlled by a temperature controller operating in an on / off mode. The set point feedback temperature of the controller was measured by a K-type thermocouple (referred to as TC_H) at the center of the top surface of the aluminum block (at the interface between the block and the sample material). A second identical thermocouple was placed directly next to this thermocouple (referred to as TC_1). The sample material was placed on top of the aluminum block so that the thermocouple was close to its center. A third identical thermocouple (TC_2) was placed directly on the other thermocouples at the interface between the sample material and the reference material. The reference material was then placed on top of the sample material covering the thermocouples. A fourth identical thermocouple (TC_3) was placed on top of the reference material, in line with the other three thermocouples. On top of the stack of materials was placed a 6" diameter flat-bottomed stainless steel cup filled with ice water so that the total weight of the cup (including ice and water) was 5 pounds. The cup was used to provide an isothermal cold surface at its bottom. The heater is powered and regulated by the temperature controller so that the hot side of the system is maintained at a constant temperature of about 37.5°C. After ensuring that all components are correctly in place, the system is turned on and allowed to reach equilibrium. At this point, the temperatures at TC_1, TC_2, and TC_3 are recorded. The recording is repeated every 15 minutes for at least one hour. From each set of temperature measurements (a set is three temperatures measured simultaneously), the unknown thermal conductivity can be calculated as follows. By assuming one-dimensional conduction (i.e., ignoring edge losses and conduction perpendicular to the lines where TC_1, TC_2, and TC_3 are located), it can be concluded that the heat flux through each material is defined by the temperature difference on the material divided by the thermal resistance per unit area of ​​the material (where the thermal resistance per unit area is defined by R "=t / k, where t is the thickness in meters, and k is the thermal conductivity in W / mK). The thickness t is measured when the sample material is subjected to a pressure equal to that experienced by the sample material during the CHP thermal conductivity test.For example, the thickness of the sample material can be measured by clamping the sample material between a fixed rigid surface and a movable rigid plate parallel to the rigid surface, and applying a known pressure to the material sample by applying a known force to the rigid plate. Using any suitable device, such as a dial indicator or a depth gauge, the thickness t_1 of this material stack can be measured. The material sample is then removed from this material stack and the thickness t_2 of the rigid plate is measured under the same force as previously specified. Therefore, the thickness of the material sample under a specified pressure can be calculated by subtracting t_2 from t_1. The preferred range of the material sample thickness used in the thermal conductivity measurement is 2mm to 10mm. Using the material sample thickness outside this range may introduce a certain degree of uncertainty and / or error in the thermal conductivity calculation, so that the measured value is no longer accurate and / or reliable. By setting the heat flux through the sample material to be equal to the heat flux through the reference material, the thermal conductivity (unique unknown in the equation) of the sample material can be solved. This calculation is performed for each temperature group, and the average value is reported as the sample thermal conductivity. The thermocouples used can be individually calibrated against a platinum RTD and assigned unique corrections for zero offset and slope, resulting in a measurement uncertainty of ±0.25°C instead of ±2.2°C.

[0106] For example, Figure 7B and Figure 7C A method for measuring thermal conductivity according to the calibrated hot plate (CHP) method described herein is depicted, wherein a hot plate (7) is placed on top of an insulating material (8), and a sample to be tested (6) is placed on top of the hot plate. According to some embodiments, a NIST standard foam (5) is placed on top of the sample, an ice bucket (4) of known weight is placed on top of the stack, and a thermometer (9) is used to measure the interface temperature. Figure 7B and Figure 7C As shown, the CHP method is shown in a front view and a 3D view, respectively.

[0107] In some embodiments, the thermal conductivity of the polymer-aerogel / fiber composite or polymer-aerogel / fabric composite is lower than that of the bulk fiber or bulk fabric, respectively, when measured according to any suitable method described herein.

[0108] Without wishing to be bound by any particular theory, it is believed that the aerogel that coats the outer surface of the fibers in the polymer-aerogel / fiber composite material and / or occupies the space between the strands of the fibers when being stacked into a mat or incorporated into a fabric hinders heat transfer between adjacent fibers and / or adjacent strands of fibers by preventing direct contact between the fibers and / or between the strands of the fibers, and provides thermal insulation due to the low thermal conductivity of the aerogel. For example, in some embodiments, a mat or fabric comprising a polymer-aerogel / fiber composite material exhibits a reduction in thermal conductivity relative to a comparable mat or fabric comprising separate bulk fibers. In some embodiments, this reduction in thermal conductivity can be greater than 10%, greater than 20%, greater than 30%, greater than 40%, greater than 50%, or greater. In certain embodiments, relative to a comparable mat or fabric comprising separate bulk fibers, this reduction in thermal conductivity can be achieved without significantly increasing the weight or volume of the mat or fabric comprising the polymer-aerogel / fiber composite material. In some such embodiments, a 30% reduction in thermal conductivity may be achieved by adding less than 1%, 2%, 3%, 5%, 10%, 20%, or 40% by mass of polymer aerogel to the polymer-aerogel / fiber composite.

[0109] Without wishing to be bound by any particular theory, it is believed that the aerogel coating the outer surface of the fibers in the polymer-aerogel / fabric composite material and / or occupying the space between the fibers constituting the fabric and / or occupying the space between the strands of the fibers constituting the fabric hinders the heat transfer between adjacent fibers of the fabric and / or adjacent strands of fibers by preventing direct contact between the fibers and / or between the strands of fibers, and provides thermal insulation due to the low thermal conductivity of the aerogel. For example, in some embodiments, the polymer-aerogel / fabric composite material exhibits a reduction in thermal conductivity relative to a comparable bulk fabric. In some embodiments, this reduction in thermal conductivity can be greater than 10%, greater than 20%, greater than 30%, greater than 40%, greater than 50%, or greater. In certain embodiments, relative to a comparable fabric comprising a separate bulk fabric, this reduction in thermal conductivity can be achieved without significantly increasing the weight or volume of the fabric comprising the polymer-aerogel / fabric composite material. In some such embodiments, a 30% reduction in thermal conductivity may be achieved by adding less than 1%, 2%, 3%, 5%, 10%, 20%, or 40% by mass of polymer aerogel to the polymer-aerogel / fabric composite.

[0110] Without wishing to be bound by any particular theory, it is believed that a higher mass percentage of polymer aerogel relative to fiber or fabric in a polymer-aerogel / fiber composite or polymer-aerogel / fabric composite is directly related to lower thermal conductivity, respectively.

[0111] In some embodiments, when the polymer-aerogel / fiber composite is stacked into a pad comprising a polymer-aerogel / fiber composite, a fabric comprising a polymer-aerogel / fiber composite, or a polymer-aerogel / fabric composite, the thermal conductivity of the polymer-aerogel / fiber composite can be measured under compression. The thermal conductivity of a fluffy material (e.g., wadding, down, or fluffy knitted fabric) typically increases as the material is compressed and the volume fraction of air in the insulating layer decreases. In certain embodiments, when subjected to a compressive load, the thermal conductivity of the pad comprising a polymer-aerogel / fiber composite, the fabric comprising a polymer-aerogel / fiber composite, or the polymer-aerogel / fabric composite is maintained within 1%, within 5%, within 10%, within 30%, or within 100% of the thermal conductivity of the same pad comprising a polymer-aerogel / fiber composite, the fabric comprising a polymer-aerogel / fiber composite, or the polymer-aerogel / fabric composite. In certain embodiments, when subjected to an increased compressive load, the thermal conductivity of the pad comprising a polymer-aerogel / fiber composite, the fabric comprising a polymer-aerogel / fiber composite, or the polymer-aerogel / fabric composite is correspondingly lower than that of a comparable pad comprising bulk fibers, the fabric comprising bulk fibers, or the bulk fabric. In certain embodiments, when placed under compression, the thermal conductivity of the pad comprising a polymer-aerogel / fiber composite, the fabric comprising a polymer-aerogel / fiber composite, or the polymer-aerogel / fabric composite is correspondingly 1%, 5%, 10%, 20%, 30%, 40%, 50%, 60%, 75%, 90%, or 100% lower than that of a comparable pad comprising bulk fibers, the fabric comprising bulk fibers, or the bulk fabric under the same amount of compression. In some embodiments, when exposed to liquid water and / or moisture, the thermal conductivity of the pad comprising a polymer-aerogel / fiber composite, the fabric comprising a polymer-aerogel / fiber composite, or the polymer-aerogel / fabric is lower than that of a comparable pad comprising bulk fibers, the fabric comprising bulk fibers, or the bulk fabric. In certain embodiments, when exposed to liquid water and / or moisture, the thermal conductivity of the pad comprising a polymer-aerogel / fiber composite, the fabric comprising a polymer-aerogel / fiber composite, or the polymer-aerogel / fabric composite is maintained within 1%, within 5%, within 10%, within 30%, or within 100% of the thermal conductivity of the dry pad comprising a polymer-aerogel / fiber composite, the dry fabric comprising a polymer-aerogel / fiber composite, or the dry polymer-aerogel / fabric composite.In certain embodiments, when exposed to liquid water and / or moisture, the thermal conductivity of the pad comprising a polymer-aerogel / fiber composite, the fabric comprising a polymer-aerogel / fiber composite, or the polymer-aerogel / fabric composite is correspondingly lower than that of a comparable pad comprising bulk fibers, the fabric comprising bulk fibers, or the bulk fabric. In certain embodiments, when exposed to liquid water and / or moisture, the thermal conductivity of the pad comprising a polymer-aerogel / fiber composite, the fabric comprising a polymer-aerogel / fiber composite, or the polymer-aerogel / fabric composite is correspondingly lower than that of a comparable pad comprising bulk fibers, the fabric comprising bulk fibers, or the bulk fabric when exposed to liquid water and / or moisture by 1%, 5%, 10%, 20%, 30%, 40%, 50%, 60%, 75%, 90%, or 100%.

[0112] In some embodiments, when placed under compression and exposed to liquid water and / or moisture, the thermal conductivity of the pad comprising a polymer-aerogel / fiber composite, the fabric comprising a polymer-aerogel / fiber composite, or the polymer-aerogel / fabric composite is respectively maintained within 1%, within 5%, within 10%, within 30%, or within 100% of the thermal conductivity of the same dry, uncompressed material. In certain embodiments, when under compression and exposed to liquid water and / or moisture, the thermal conductivity of the pad comprising a polymer-aerogel / fiber composite, the fabric comprising a polymer-aerogel / fiber composite, or the polymer-aerogel / fabric composite is respectively lower than that of a comparable pad comprising bulk fibers, the fabric comprising bulk fibers, or the bulk fabric. In certain embodiments, the thermal conductivity of a pad comprising a polymer-aerogel / fiber composite, a fabric comprising a polymer-aerogel / fiber composite, or a polymer-aerogel / fabric composite, when under compression and exposed to liquid water and / or moisture, is 1%, 5%, 10%, 20%, 30%, 40%, 50%, 60%, 75%, 90%, or 100% lower than a comparable pad comprising bulk fibers, a fabric comprising bulk fibers, or a bulk fabric, respectively, when under compression and exposed to liquid water and / or moisture.

[0113] In some embodiments, the specific surface area of ​​the polymer-aerogel / fiber composite and / or polymer-aerogel / fabric composite is correspondingly greater than the specific surface area of ​​the bulk fiber or bulk fabric. In some embodiments, the polymer-aerogel / fiber composite exhibits a surface area greater than 2 m / s as measured using nitrogen adsorption porosimetry and derived from the Brunauer-Emmett-Teller (BET) model. 2 / g, greater than 5m 2 / g, or greater than 10m 2In some embodiments, the polymer-aerogel / fabric composite exhibits an internal surface area greater than 2 m / g as measured using nitrogen adsorption porosimetry and derived from the Brunauer-Emmett-Teller (BET) model. 2 / g, greater than 5m 2 / g, or greater than 10m 2 / g of internal surface area. The internal surface area of ​​the material measured by this method is referred to as the BET surface area of ​​the material in this article. For example, nitrogen adsorption porosimetry can be performed using a Micromeritics Tristar II 3020 surface area and porosity analyzer. Prior to porosimetry analysis, the sample can be subjected to a vacuum of about 100 torr for 24 hours to remove adsorbed water or other solvents from the pores of the sample. The porosimeter can provide an adsorption isotherm and a desorption isotherm, which include the amount of analyte gas adsorbed or desorbed as a function of partial pressure. The specific surface area can be calculated from the adsorption isotherm using the Brunauer-Emmett-Teller (BET) method within the range commonly used to measure surface area. In certain embodiments, the specific surface area of ​​the polymer-aerogel / fiber composite or polymer-aerogel / fabric composite is greater than 2 m 2 / g, greater than 5m 2 / g, greater than 10m 2 / g, greater than 20m 2 / g, greater than 30m 2 / g, greater than 40m 2 / g, greater than 50m 2 / g, greater than 100m 2 / g, greater than 200m 2 / g, or 500m 2 / g to 1000m 2 In certain preferred embodiments, the specific surface area of ​​the polymer-aerogel / fiber composite material or polymer-aerogel / fabric composite material is greater than 50 m 2 / g. Standard fabrics or fabric fibers usually exhibit much lower specific surface area values ​​than the ranges listed here, less than 10m 2 / g and are generally too low to be measured using nitrogen adsorption porosimetry.

[0114] It will be understood by those skilled in the art that internal surface area and specific surface area have the same meaning and describe the same phenomenon. As described herein, these values ​​may also be referred to as BET surface area.

[0115] Without wishing to be bound by any particular theory, it is believed that higher BET surface area is directly correlated to higher aerogel mass loading percentage within polymer-aerogel / fiber composites or polymer-aerogel / fabric composites and also to lower thermal conductivity of the composites.

[0116] In some embodiments, a polymer-aerogel / aerogel-composite-precursor solution can be prepared, wherein particles of an aerogel material are dispersed throughout the polymer-aerogel-precursor-solution. The aerogel particles can be hydrophobic or hydrophilic, for example, a composite material in which hydrophobic silica aerogel particles having a diameter of 1 micron to 5 microns, 1 micron to 10 microns, 1 micron to 20 microns, 1 micron to 40 microns, 1 micron to 100 microns, or 1 micron to 1000 microns are dispersed throughout the polymer aerogel. In certain embodiments, the aerogel particles may include trimethylsilyl functionalized silica aerogel, wherein the silica aerogel may contain sodium ions. In certain embodiments, the mass percentage of the dispersant aerogel material (e.g., silica aerogel particles) relative to the mass of the host aerogel (e.g., polymer aerogel) is less than 55%, less than 50%, less than 40%, less than 30%, less than 20%, less than 10%, less than 5%, less than 2%, or less than 1%. In some embodiments, a polymer-aerogel / aerogel-composite precursor solution is applied to a fiber and treated to form a polymer-aerogel / aerogel / fiber composite. In some embodiments, a polymer-aerogel / aerogel-composite precursor solution is applied to a fabric and treated to form a polymer-aerogel / aerogel / fabric composite. In some embodiments, the polymer-aerogel / fiber composite comprises a polymer aerogel, wherein the polymer aerogel material comprises a silica aerogel. In some embodiments, the silica aerogel comprises a trimethylsilyl functionalized silica aerogel. In some embodiments, the silica aerogel comprises sodium ions. For example, Figure 1 As shown, the aerogel (2) in the polymer-aerogel / fiber composite material can include polymer aerogel and silica material particles containing sodium ions. In some embodiments, the polymer-aerogel / fabric composite material includes a polymer aerogel, wherein the polymer aerogel material includes silica aerogel. In some embodiments, the silica aerogel includes trimethylsilyl functionalized silica aerogel. In some embodiments, the silica aerogel includes sodium ions. For example, in Fig.25BIn the polymer-aerogel / fabric composite material, the aerogel (2) may comprise a polymer aerogel and silica material particles containing sodium ions. As described herein, in some embodiments, a polymer-aerogel / fiber composite material or a polymer-aerogel / fabric composite material may also refer to a composition comprising a polymer-aerogel / aerogel / fiber composite material or a polymer-aerogel / aerogel / fabric composite material, respectively. In some embodiments, the polymer aerogel in the polymer-aerogel / aerogel / fiber composite material comprises a polyimide aerogel. In some embodiments, the polyimide aerogel material comprises a trimethylsilyl-functionalized silica aerogel, wherein the silica aerogel comprises sodium ions.

[0117] Without wishing to be bound by theory, it is believed that the presence of the silica aerogel particles in the polymer-aerogel / fiber composite or polymer-aerogel / fabric composite helps prevent adsorption of some water and detergent mixtures during washing due to the presence of sodium ions within the silica aerogel particles and the hydrophobic surface chemistry of these particles.

[0118] Consumer care washing can be performed to polymer-aerogel / fiber composites, fabrics comprising polymer-aerogel / fiber composites, or polymer-aerogel / fabric composites. In some embodiments, composite materials can be washed according to the process outlined in the AATCC LP1 household washing standard. The process may need to be washed, for example, using a standard electric washing machine, and then dried in a standard drum dryer. In some embodiments, after washing according to the process outlined in the AATCC LP1 standard, polymer-aerogel / fiber composites, fabrics comprising polymer-aerogel / fiber composites, or polymer-aerogel / fabric composites maintain a measurable BET surface area. It is not desirable to be bound by any particular theory, and it is believed that measurable BET surface area indicates that aerogels continue to exist in composite materials. In certain embodiments, after being subjected to consumer care washing, pads comprising polymer-aerogel / fiber composites, fabrics comprising polymer-aerogel / fiber composites, or polymer-aerogel / fabric composites correspondingly maintain a thermal conductivity lower than comparable pads comprising bulk fibers, fabrics comprising bulk fibers, or bulk fabrics. In some embodiments, after being subjected to consumer care washes, the polymer-aerogel / fiber composite or polymer-aerogel / fabric composite may exhibit a relative humidity of greater than 2 m / s. 2 / g, greater than 5m 2 / g, greater than 10m 2 / g, greater than 20m 2 / g, greater than 30m 2 / g, greater than 40m 2 / g, greater than 50m2 / g, greater than 100m 2 / g, greater than 200m 2 / g, or 500m 2 / g to 1000m 2 In certain preferred embodiments, the polymer-aerogel / fiber composite can be washed according to the AATCC LP1 home wash standard, and the washed material exhibits a BET surface area of ​​at least 10 m / g. 2 In certain preferred embodiments, the polymer-aerogel / fabric composite can be washed according to the AATCC LPl home washing standard, and the washed material exhibits a BET surface area of ​​at least 10 m 2 As will be appreciated by one of ordinary skill in the art, the BET surface area of ​​the composite materials described herein will be measured using nitrogen adsorption porosimetry and derived from the Braunauer-Emmett-Teller (BET) model.

[0119] In some embodiments, the polymer-aerogel / fiber composite or polymer-aerogel / fabric composite can exhibit hydrophobicity. The term hydrophobic refers to the absence of an attractive force between the material and a large amount of water. In certain embodiments, the apparent hydrophobicity of the textured surface can be higher than the chemical hydrophobicity of the bulk material.

[0120] The hydrophobicity of polymer-aerogel / fiber composites, fabrics comprising polymer-aerogel / fiber composites, or polymer-aerogel / fabric composites can be expressed as liquid water absorption. The term liquid water absorption refers to the ability of a material or composition to absorb, adsorb, or otherwise retain water due to contact with liquid water. In some embodiments, the liquid water absorption of polymer-aerogel / fiber composites, fabrics comprising polymer-aerogel / fiber composites, or polymer-aerogel / fabric composites can be correspondingly higher than comparable bulk fibers, fabrics comprising bulk fibers, or bulk fabrics. Liquid water absorption can be expressed in one of several ways, for example, expressed as a fraction or percentage of the open pore volume or the volume of the encapsulate of the material, or expressed as a fraction or percentage relative to the mass of the unwetted material. The reported liquid water absorption is understood to be a measurement performed under specific conditions. Liquid water absorption can be determined by methods including but not limited to ASTM C1511, ASTM C1763, EN 1609, or any suitable standard for measuring liquid water absorption. In some embodiments, the liquid water absorption of a polymer-aerogel / fiber composite, a fabric comprising a polymer-aerogel / fiber composite, or a polymer-aerogel / fabric composite can be less than 100 wt%, less than 80 wt%, less than 70 wt%, less than 60 wt%, less than 50 wt%, less than 40 wt%, less than 30 wt%, less than 20 wt%, less than 10 wt%, less than 5 wt%, less than 4 wt%, less than 3 wt%, less than 2 wt%, less than 1 wt%, or less than 0.1 wt%, relative to the weight of the composite before contact with liquid water.

[0121] In some embodiments, when the polymer-aerogel / fiber composite is immersed in water at 25° C. for 24 hours, the mass of water absorbed by the composite within its outer boundaries is less than 20% of the dry mass of the corresponding aerogel prior to immersion in water.

[0122] In some preferred embodiments, when the polymer-aerogel / fiber composite is immersed in water at 25°C for 24 hours, the mass of water absorbed by the composite within its outer boundary is less than 20% of the dry mass of the corresponding composite before immersion in water. Figure 8 As shown, when the composite fiber (3) is immersed in water (33) at 25°C for 24 hours, the mass of water absorbed by the composite within its outer boundary is less than 20% of the dry mass of the corresponding composite before immersion in water.

[0123] In some embodiments, when the polymer-aerogel / fabric composite is immersed in water at 25° C. for 24 hours, the mass of water absorbed by the composite within its outer boundaries is less than 20% of the dry mass of the corresponding aerogel before immersion in water.

[0124] In some preferred embodiments, when the polymer-aerogel / fabric composite is immersed in water at 25°C for 24 hours, the mass of water absorbed by the composite within its outer boundary is less than 20% of the dry mass of the corresponding composite before immersion in water. Figure 8 As shown, when the composite fabric (25) is immersed in water (33) at 25°C for 24 hours, the mass of water absorbed by the composite within its outer boundary is less than 20% of the dry mass of the corresponding composite before immersion in water.

[0125] The hydrophobicity of polymer-aerogel / fiber composites, fabrics comprising polymer-aerogel / fiber composites, or polymer-aerogel / fabric composites can be expressed as water vapor absorption. The term water vapor absorption refers to the ability of a material or composition to absorb, adsorb, or otherwise retain water due to contact with water in a vapor state. In some embodiments, the water vapor absorption of a fabric comprising a polymer-aerogel / fiber composite or a polymer-aerogel / fabric composite can be lower than a comparable fabric comprising a separate bulk fiber. In some embodiments, the water vapor absorption of a fabric comprising a polymer-aerogel / fiber composite or a polymer-aerogel / fabric composite can be higher than a comparable fabric comprising a separate bulk fiber. Water vapor absorption can be expressed as a fraction or percentage of the mass of the aerogel relative to the water retained before exposure to water vapor. The reported water vapor absorption is understood to be a measurement performed under specific conditions. Water vapor absorption can be determined by methods including but not limited to ASTM C1104 or any suitable standard for measuring water vapor absorption or retention. In some embodiments, the water vapor absorption of the polymer-aerogel / fiber composite or polymer-aerogel / fabric composite can be less than 100 wt%, less than 80 wt%, less than 70 wt%, less than 60 wt%, less than 50 wt%, less than 40 wt%, less than 30 wt%, less than 20 wt%, less than 10 wt%, less than 5 wt%, less than 4 wt%, less than 3 wt%, less than 2 wt%, less than 1 wt%, or less than 0.1 wt%, relative to the weight of the composite before exposure to water vapor.

[0126] In some embodiments, the polymer-aerogel / fiber composite can be washed according to the AATCC LP1 standard for home washing, and the washed material exhibits a thermal conductivity of less than 80 mW / mK or less than 40 mW / mK when the composite is laid into a mat and measured according to the Calibrated Hot Plate (CHP) method described herein at an average sample temperature of 25°C and an applied pressure of 0.31 psi.

[0127] In some embodiments, the polymer-aerogel / fiber composite can be incorporated into a fabric and laundered according to the AATCC LP1 standard for home laundering, and the laundered material exhibits a thermal conductivity of less than 80 mW / mK or less than 40 mW / mK when measured according to the Calibrated Hot Plate (CHP) method described herein at an average sample temperature of 25°C and an applied pressure of 0.31 psi.

[0128] In some embodiments, the polymer-aerogel / fabric composite can be washed according to the AATCC LP1 standard for home laundering, and the washed material exhibits a thermal conductivity of less than 80 mW / mK or less than 40 mW / mK when measured according to the Calibrated Hot Plate (CHP) method described herein at an average sample temperature of 25°C and an applied pressure of 0.31 psi.

[0129] In some embodiments, the fabric comprising polymer-aerogel / fiber composites passes the flammability test described herein. In some embodiments, the polymer-aerogel / fabric composite passes the flammability test described herein. In some embodiments, the polymer-aerogel / fiber composite or polymer-aerogel / fabric composite is non-flammable. In some embodiments, relative to a comparable fabric comprising a separate bulk fiber, a fabric comprising a polymer-aerogel / fiber composite or a polymer-aerogel / fabric composite can show improved non-flammability. Non-flammability can be characterized as no melting, dripping, and burning through when exposed to a vertical flame for 3 seconds under specific conditions. The vertical flame test is performed using a fabric comprising a polymer-aerogel / fiber composite in a laboratory fume hood and a flame hood as described in Federal Standard 191A Method 5903. All samples are pre-treated for 2 hours at 21°C and 50%+ / -2% relative humidity. A movable Fisher burner supplying butane was used as a flame source by a supply valve, regulator, needle valve and flexible hose arrangement capable of supplying a steady flow of 17.3 kPa + / - 1.7 kPa as specified in NFPA1971-34. A steel sample holder was used to center the bottom of the sample about 38 mm above the top of the Fisher burner in the flame cabinet. The sample was placed horizontally on the sample holder and fixed in place using a medium-sized binder clip. The laboratory fume hood airflow was set to low and the burner was ignited with its back to the sample. The flame height was adjusted to about 75 mm and allowed to burn for 1 minute, adjusting the height as needed. The burner was then moved under the sample so that the flame was as close to the center of the sample as possible, and a timer was started for 3 seconds. At the end of 3 seconds, the burner was removed from under the sample. If the sample burns, the timer is allowed to continue timing until the flame goes out. Any time that the sample is exposed to the flame for more than 3 seconds is called the afterflame time. The formation of holes by ablation or burning is called burn-through. Any melting, dripping, burn-through or afterflame time is recorded. Any melting, dripping or burning through shall constitute failure of the sample to pass the test.

[0130] As it applies to different applications, non-flammability can also be characterized as passing certain standards. In certain embodiments, a fabric comprising a polymer-aerogel / fiber composite, or a polymer-aerogel / fabric composite passes the FAR 25.853 flammability requirements for use in aviation interiors.

[0131] In certain embodiments, a fabric comprising a polymer-aerogel / fiber composite, or a polymer-aerogel / fabric composite passes the ASTM D6413 Standard Test Method for Flame Retardancy of Fabrics.

[0132] In certain embodiments, a fabric comprising a polymer-aerogel / fiber composite, or a polymer-aerogel / fabric composite, passes the 16 CFR 1615 standard for flammability of children's sleepwear.

[0133] In certain embodiments, a fabric comprising a polymer-aerogel / fiber composite, or a polymer-aerogel / fabric composite passes the CPAI-84 specification for flame retardant materials used in camping tents.

[0134] In certain embodiments, a fabric comprising a polymer-aerogel / fiber composite, or a polymer-aerogel / fabric composite passes the ASTM D1230 specification for flame retardant materials used in clothing fabrics.

[0135] In some embodiments, the fabric comprising polymer-aerogel / fiber composite material or polymer-aerogel / fabric composite material can show oleophobicity.The term oleophobicity refers to the absence of attraction between material and a large amount of organic liquids.In some embodiments, the oleophobicity of bulk material refers to this behavior when it is applied to a surface.In certain embodiments, the apparent oleophobicity of textured surface can be higher than the chemical oleophobicity of bulk material.The oleophobicity of the fabric comprising polymer-aerogel / fiber composite material or polymer-aerogel / fabric composite material can be characterized by the method described in AATCC test method 118-2013 or any other suitable standard.In certain embodiments, the fabric comprising polymer-aerogel / fiber composite material or polymer-aerogel / fabric composite material can have 0,1,2,3,4,5,6,7,8 or the AATCC oil repellency grade of any other appropriate grade.In some embodiments, relative to the fabric comprising a single bulk fiber comparable, the fabric comprising polymer-aerogel / fiber composite material or polymer-aerogel / fabric composite material can show improved oleophobicity.

[0136] In certain embodiments, fabrics comprising polymer-aerogel / fiber composites, or polymer-aerogel / fabric composites exhibit air permeability. In certain embodiments, fabrics comprising polymer-aerogel / fiber composites, or polymer-aerogel / fabric composites may exhibit reduced air permeability through fabrics relative to comparable fabrics comprising separate bulk fibers. In certain embodiments, fabrics comprising polymer-aerogel / fiber composites, or polymer-aerogel / fabric composites may exhibit improved air permeability through fabrics relative to similar fabrics comprising bulk fibers and standard fabric coatings. The air permeability of a sample may be determined using the method outlined in ASTM D737 or any other standard applicable to determining the air permeability of a fabric. In certain embodiments, the average air permeability is 0 cm 3 / sec / cm 2 Up to 30cm 3 / sec / cm 2 、30cm 3 / sec / cm 2 Up to 150cm 3 / sec / cm 2 , or higher than 150cm 3 / sec / cm 2 Combinations of the above ranges or values ​​outside these ranges are possible for the air permeability of a fabric comprising a polymer-aerogel / fiber composite, or a polymer-aerogel / fabric composite.

[0137] In certain embodiments, the fabric comprising polymer-aerogel / fiber composite material or polymer-aerogel / fabric composite material can show water repellency. In certain embodiments, relative to the fabric comprising a single bulk fiber, the fabric comprising polymer-aerogel / fiber composite material or polymer-aerogel / fabric composite material can show improved water repellency. In an example, the fabric comprising polymer-aerogel / fiber composite material shows both water repellency and air permeability. In an example, polymer-aerogel / fabric composite material shows both water repellency and air permeability. The phrase water repellency refers to the characteristic that the fiber resists wetting. Water repellency can be determined by including but not limited to the method outlined in the spray test outlined in AATCCTM22 or any suitable standard for measuring water repellency. In some embodiments, the spray test grade can be 100, 90, 80, 70, 50, or 0. For the water repellency spray test grade of polymer-aerogel / fiber composite material or polymer-aerogel / fabric composite material, the combination of the above ranges or the value outside these ranges is possible.

[0138] In some embodiments, a fabric comprising a polymer-aerogel / fiber composite, or a polymer-aerogel / fabric composite, can exhibit an overall [liquid] moisture management capability (OMMC). In certain embodiments, a fabric comprising a polymer-aerogel / fiber composite, or a polymer-aerogel / fabric composite, can exhibit a higher OMMC rating relative to a comparable fabric comprising a single bulk fiber. In certain embodiments, a fabric comprising a polymer-aerogel / fiber composite, or a polymer-aerogel / fabric composite, can exhibit a lower OMMC rating relative to a comparable fabric comprising a single bulk fiber. OMMC is defined herein as an indicator of the overall ability of a fabric to transport liquid moisture as calculated by combining the liquid absorption rate on the bottom surface of the sample, the unidirectional liquid transmission capacity, and the maximum liquid moisture diffusion rate on the bottom surface of the sample as described in AATCC Test Method 195. In some embodiments, the OMMC rating can be 1, 2, 3, 4, or 5. Combinations of the above-recited ranges or values ​​outside these ranges are possible for fabrics comprising polymer-aerogel / fiber composites, or OMMC grades of polymer-aerogel / fabric composites.

[0139] In certain embodiments, the fabric comprising the polymer-aerogel / fiber composite, or the polymer-aerogel / fabric composite exhibits a weight per unit area. As described herein, weight per unit area refers to the mass per unit area of ​​the fabric. In certain embodiments, the weight per unit area of ​​the fabric can be calculated according to ASTM D3776. In certain embodiments, the weight per unit area of ​​the fabric is 0 g / m 2 Up to 100g / m 2 , 100g / m 2 Up to 200g / m 2 , 200g / m 2 Up to 300g / m 2 , or greater than 300g / m 2 Combinations of the above ranges or values ​​outside of these ranges are possible for the weight per unit area of ​​a fabric comprising a polymer-aerogel / fiber composite, or a polymer-aerogel / fabric composite. In some embodiments, the weight per unit area of ​​a fabric comprising a polymer-aerogel / fiber composite, or a polymer-aerogel / fabric composite is less than 1%, less than 5%, less than 10%, less than 20%, less than 30%, less than 40%, less than 50%, less than 60%, less than 75%, or less than 100% greater than the weight per unit area of ​​a comparable fabric comprising individual bulk fibers.

[0140] In some embodiments, the fabric comprising polymer-aerogel / fiber composite material, or polymer-aerogel / fabric composite material can show ultraviolet (UV) radiation blocking. In some embodiments, when compared with the fabric comprising a single bulk fiber comparable, the fabric comprising polymer-aerogel / fiber composite material, or polymer-aerogel / fabric composite material can show improved UV radiation blocking. The degree of UV radiation blocking is reported as ultraviolet protection factor (ultraviolet protection factor, UPF) grade. The UPF grade can be measured according to the method described in AATCC test method 183 or any other standard applicable to measuring fabric UPF grade. In some embodiments, the fabric comprising polymer-aerogel / fiber composite material, or polymer-aerogel / fabric composite material can show a UPF grade of 15 to 24, and therefore meet the requirements of "good" UV protection category. In some embodiments, the fabric comprising polymer-aerogel / fiber composite material, or polymer-aerogel / fabric composite material can show a UPF grade of 25 to 39, and therefore meet the requirements of "very good" UV protection category. In some embodiments, a fabric comprising a polymer-aerogel / fiber composite, or a polymer-aerogel / fabric composite, can exhibit a UPF rating greater than 40 and thus meet the requirements of an "excellent" UV protection category. Combinations of the above ranges or values ​​outside these ranges are possible for the UPF rating of the fabric.

[0141] In some embodiments, a fabric comprising a polymer-aerogel / fiber composite, or a polymer-aerogel / fabric composite, can exhibit improved abrasion resistance compared to a comparable fabric comprising bulk fibers alone. In some embodiments, abrasion resistance can be measured by the method described in ASTM D4966 or any suitable standard for measuring abrasion resistance.

[0142] In some embodiments, when under the tension force such as seen in a normal fiber cone, the amount of aerogel applied to the fiber makes the thickness of the polymer-aerogel / fiber composite or polymer-aerogel / fabric composite comparable to the thickness of the bulk fiber alone. In other embodiments, the amount of aerogel applied to the fiber increases the thickness of the polymer-aerogel / fiber composite relative to the thickness of the bulk fiber alone. For example, relative to the bulk fiber under the same conditions, the polymer-aerogel / fiber composite can have a greater thickness when subjected to a 10g tension. In some embodiments, the thickness of the composite fiber can be several times the diameter of the bulk fiber alone.

[0143] In some embodiments, when tension is removed, compared with a single bulk fiber, the polymer-aerogel / fiber composite material exhibits a lower thickness. In an illustrative example, the multi-strand fiber is removed from the tension, and the spacing between the strands of the fiber increases, producing thicker fibers. In a polymer-aerogel / fiber composite material comprising the same multi-strand fiber, the strands of the fiber can be mechanically bonded to each other, so when tension is reduced, the thickness of the composite fiber will not increase as much as the bulk multi-strand fiber. In some embodiments, when tension is removed, compared with a single bulk fiber, the composite fiber exhibits the same or greater thickness. In an illustrative example, the multi-strand fiber is removed from the tension, and the spacing between the strands of the fiber increases, producing thicker fibers. In a polymer-aerogel / fiber composite material comprising the same multi-strand fiber, the strands of the fiber are not completely mechanically bonded to each other, so when tension is reduced, relative to a single bulk multi-strand fiber, the thickness of the composite fiber increases by the same amount or more.

[0144] In some embodiments, the fibers have at least one cross-sectional dimension less than or equal to 10 microns, less than or equal to 20 microns, less than or equal to 50 microns, less than or equal to 100 microns, less than or equal to 200 microns, less than or equal to 500 microns, less than or equal to 1 millimeter, or less than or equal to 3 millimeters.

[0145] In certain embodiments, the fibers have an average cross-sectional dimension of less than or equal to 10 microns, less than or equal to 20 microns, less than or equal to 50 microns, less than or equal to 100 microns, less than or equal to 200 microns, less than or equal to 500 microns, less than or equal to 1 millimeter, or less than or equal to 3 millimeters.

[0146] In certain embodiments, the fibers have an average cross-sectional dimension of at least 5 microns, at least 10 microns, at least 20 microns, at least 50 microns, at least 100 microns, at least 500 microns, at least 1 mm, or at least 3 mm.

[0147] In some embodiments, the composite fibers have at least one cross-sectional dimension of less than or equal to 10 microns, less than or equal to 20 microns, less than or equal to 50 microns, less than or equal to 100 microns, less than or equal to 200 microns, less than or equal to 500 microns, less than or equal to 1 millimeter, or less than or equal to 3 millimeters.

[0148] In certain embodiments, the composite fibers have an average cross-sectional dimension of less than or equal to 10 microns, less than or equal to 20 microns, less than or equal to 50 microns, less than or equal to 100 microns, less than or equal to 200 microns, less than or equal to 500 microns, less than or equal to 1 millimeter, or less than or equal to 3 millimeters.

[0149] In certain embodiments, the composite fibers have an average cross-sectional dimension of at least 5 microns, at least 10 microns, at least 20 microns, at least 50 microns, at least 100 microns, at least 500 microns, at least 1 mm, or at least 3 mm.

[0150] The cross-sectional dimension of a fiber or composite fiber is measured in a direction perpendicular to its length. The average cross-sectional dimension of a fiber or composite fiber is taken as the number average of the cross-sectional dimensions along its length.

[0151] In some embodiments, the fiber has an aspect ratio of at least 100:1, at least 1000:1, at least 100,000:1, at least 10 7 :1. At least 10 9 :1, or larger.

[0152] In certain embodiments, the aspect ratio of the composite fiber is at least 100:1, at least 1000:1, at least 100,000:1, at least 10 7 :1. At least 10 9 :1, or larger.

[0153] The aspect ratio of a fiber or composite fiber is expressed as the ratio of its length to its average cross-sectional diameter.

[0154] In an illustrative embodiment, the multi-strand fiber or fiber composite may have an average cross-sectional diameter of 100 microns and a length of 100,000 meters, and a length of about 10 9 In another embodiment, the fiber or fiber composite may have an average cross-sectional diameter of 100 microns and a length of 1 meter, and a length: diameter aspect ratio of 10,000:1.

[0155] Those skilled in the art will appreciate that fabrics and composite fabrics exist in three-dimensional space and have three dimensions: width, length and thickness. Each of these three dimensions is orthogonal to the other two. The thickness of a fabric or composite fabric corresponds to the smallest of these three dimensions, with the other two dimensions (width and length) defining the face of the fabric. The thickness of a fabric or composite fabric generally refers to its average thickness, which is considered to be the number average of its thickness over its entire face.

[0156] In certain embodiments, the fabric has a thickness of less than or equal to 10 microns, less than or equal to 20 microns, less than or equal to 50 microns, less than or equal to 100 microns, less than or equal to 200 microns, less than or equal to 500 microns, less than or equal to 1 mm, or less than or equal to 5 mm. In certain embodiments, the fabric has a thickness of at least 5 microns, at least 10 microns, at least 20 microns, at least 50 microns, at least 100 microns, at least 500 microns, at least 1 mm, or at least 5 mm.

[0157] In some embodiments, the width of the fabric is at least 10 times, at least 50 times, at least 100 times, at least 1000 times, at least 5000 times, or at least 10,000 times the thickness of the fabric. In certain embodiments, the length of the fabric is at least 100 times, at least 1,000 times, at least 10 ... 6 times, or at least 10 7 In some embodiments, both the width and length of the fabric are at least 10 times, at least 50 times, at least 100 times, at least 1000 times, at least 5000 times, or at least 10,000 times the thickness of the fabric.

[0158] In some embodiments, the width of the composite fabric is at least 10 times, at least 50 times, at least 100 times, at least 1000 times, at least 5000 times, or at least 10,000 times the thickness of the composite fabric. In certain embodiments, the length of the composite fabric is at least 100 times, at least 1,000 times, at least 10,000 times, at least 100,000 times, at least 100,000 times, or at least 100,000 times the thickness of the composite fabric. 6 times, or at least 10 7 In some embodiments, both the width and length of the composite fabric are at least 10 times, at least 50 times, at least 100 times, at least 1000 times, at least 5000 times, or at least 10,000 times the thickness of the composite fabric.

[0159] In some embodiments, the composite fabric has at least one lateral dimension of at least 5 cm. In some embodiments, the composite fabric has at least two orthogonal dimensions of at least 5 cm. For example, Fig.25A The composite fabric shown in can have a length and width that are both at least 5 cm. In some embodiments, the composite fabric has a thickness of less than 0.1 inches. For example, Fig.25A The composite fabric shown in can have a thickness of less than 0.1 inches.

[0160] In some embodiments, the fiber is exposed to a liquid solution containing a polymer-aerogel-precursor and a polymer aerogel is formed from the polymer-aerogel-precursor such that the polymer aerogel is on the outer surface of the fiber and / or penetrates into the pores of the fiber. Fig.10 As shown, the fiber bobbin (10) is exposed to a liquid solution (12) containing a polymer-aerogel-precursor. The fiber exposed to the polymer-aerogel-precursor solution can be processed to produce a polymer-aerogel / fiber composite material such that Figure 1As shown, the polymer aerogel (2) is on the outer surface of the fiber (1) and / or penetrates into the pores of the fiber. In some embodiments, the fabric is exposed to a liquid solution containing a polymer-aerogel-precursor and a polymer aerogel is formed from the polymer-aerogel-precursor, so that the polymer aerogel is on the outer surface of the fabric and / or penetrates into the pores of the fabric. For example, Fig.29 As shown, the fabric spool (26) is exposed to a liquid solution (12) containing a polymer-aerogel-precursor. The fabric exposed to the polymer-aerogel-precursor solution can be treated to produce a polymer-aerogel / fabric composite material such that Fig.25B As shown, the polymer aerogel (2) is on the outer surface of the fabric (24) and / or penetrates into the pores of the fabric. In some embodiments, the polymer aerogel substantially conformally coats the fabric. For example, Fig.26 As shown, the polymer aerogel (2) substantially conformally coats the fabric (24).

[0161] The polymer-aerogel / fiber composite or polymer-aerogel / textile composite can be produced by any suitable method.

[0162] In some embodiments, a fiber or fabric having a chemical composition suitable for mechanically and / or chemically bonding the polymer aerogel to the fiber or fabric is selected. For example, in certain preferred embodiments, the fiber or fabric may include polyester, polyamide, cotton, or any suitable fiber.

[0163] In some embodiments, before the fiber is exposed to the liquid solution containing polymer-aerogel-precursor, the fiber is pretreated. In some embodiments, before the fabric is exposed to the liquid solution containing polymer-aerogel-precursor, the fabric is pretreated. Pretreatment of fiber or fabric can involve preparation of fiber or fabric to be combined with polymer-aerogel-precursor solution. In some embodiments, the pretreatment of fiber or fabric can change one or more surfaces of fiber or fabric. In certain embodiments, the surface of this change can be used as the interface of polymer aerogel and the fiber or fabric adhesion and / or maintenance in the resulting polymer-aerogel / fiber composite material or polymer-aerogel / fabric composite material. In some embodiments, the surface of fiber or fabric is etched by etching process. In certain embodiments, etching process includes chemical etching, electrochemical etching, acid etching, alkali etching, plasma etching or any other suitable etching process. In some embodiments, fiber or fabric is pretreated by exposing fiber to liquid phase or vapor phase environment under specific temperature or temperature range. In certain embodiments, fiber or fabric is exposed to liquid phase or vapor phase environment so that fiber or fabric swells. In certain embodiments, the fibers or fabrics are exposed to liquid N-methyl-2-pyrrolidone at a temperature of 70° C., 80° C., 90° C., 100° C., or any other suitable temperature. In some embodiments, the swollen fibers or fabrics are infiltrated with a solvent, a catalyst, and / or a liquid aerogel precursor.

[0164] In some embodiments, the fibers or fabrics are pretreated by exposing them to ultraviolet radiation, infrared radiation, and / or treating with plasma to increase the surface reactivity of the bulk material.

[0165] In some embodiments, the fiber or fabric is pretreated to better allow aerogel precursors to penetrate and / or adhere to the fiber or fabric and / or the fiber or fabric by exposing it to reactive liquids, vapors and / or solids that chemically functionalize the surface of the fiber or fabric and / or the surface of the fiber strands or fabric. In certain embodiments, the fiber or fabric is chemically functionalized to introduce reactive functional groups on its surface. In some embodiments, these functional groups can react with polymer-aerogel-precursor solution to produce the resulting polymer-aerogel / fiber composite or polymer-aerogel / fabric composite when dry. For example, the fiber or fabric can be chemically functionalized to introduce reactive nucleophilic amines and / or anhydrides on its surface, which can react with polyimide-aerogel-precursor solution to produce the resulting polyimide-aerogel / fiber composite or polyimide-aerogel / fabric composite when dry.

[0166] In some embodiments, the fiber or fabric is pretreated by exposing it to a liquid, vapor or solid containing reactive monomers. In some embodiments, these monomers chemically react with the fiber or fabric to form reactive sites on the fiber or fabric. In some embodiments, these monomers are physically adsorbed to the fiber or fabric to provide reactive sites on the fiber or fabric. In certain embodiments, these reactive sites can react with complementary reactive sites on components of the polymer-aerogel-precursor solution and / or the polymer aerogel.

[0167] In some embodiments, the fiber or fabric is coated or sized before the polymer-aerogel-precursor is introduced. An example of a slurry is a polymer coating on the fiber or fabric. The slurry can serve as an interface layer between the fiber or fabric and the aerogel and can affect the adhesion of the aerogel to the fiber or fabric.

[0168] In some embodiments, a multi-strand fiber of mechanical texture or a fabric comprising a multi-strand fiber of mechanical texture is selected. In some embodiments, the mechanical texture of the fiber may include a corrugation, curl or coil in a single strand of a multi-strand fiber or a multi-strand fiber constituting a fabric. In some embodiments, the mechanical texture of the fiber has an increased exposed surface area relative to non-textured fibers, which can increase the potential interface area between the polymer aerogel and the fiber or fabric in the polymer-aerogel / fiber composite or polymer-aerogel / fabric composite, respectively. In certain embodiments, the polymer-aerogel / fiber composite or polymer-aerogel / fabric composite comprises a mechanically textured fiber. In certain embodiments, the polymer-aerogel / fiber composite or polymer-aerogel / fabric composite comprising one or more mechanically textured fibers loses less aerogel mass when subjected to wear, bending or processing, respectively, relative to a polymer-aerogel / fiber composite or polymer-aerogel / fabric composite that does not comprise one or more mechanically textured fibers. In certain embodiments, the mechanical texture of the multi-strand fiber includes a certain amount of space between the fiber strands, so that pores or bulkiness are generated in the fiber or a fabric made of the fiber. In some embodiments, the porosity can affect the amount of polymer aerogel that can be loaded into / on the fiber or fabric comprising the fiber. In certain embodiments, a mechanically textured fiber or fabric comprising the mechanically textured fiber is selected that comprises intra-fiber porosity, wherein the porosity provides volume for absorbing the polymer-aerogel precursor.

[0169] In certain embodiments, the fiber is pre-treated by controlling the tension of the fiber. The tension of the fiber can be controlled to be 0 gram (g) to 1 gram (g), 1g to 10g, 10g to 100g, greater than the tension of 100g or any suitable tension. In some embodiments, the tension of the fiber is controlled by winding the fiber from one spool to another spool. In certain embodiments, the sending spool and the receiving spool are rotated at different speeds relative to each other, which then increases or reduces the tension in the fiber when the fiber moves from one spool to another spool. In some embodiments, the tension in the fiber is controlled when the fiber is wound on a spool, a cone, a mandrel and / or other suitable roller forms. In certain embodiments, the tension of the fiber is controlled to allow the amount of the pore in the spool of the fiber and / or the fiber to be controlled. In some embodiments, the pore can affect the amount of the polymer aerogel that can be loaded into the fiber / on the fiber. In certain embodiments, the fiber is wound on a standard carrier, such as a cone, a cylinder, a flanged bobbin, a bale or a loom, and shows tension after winding. In some embodiments, the fiber on the carrier is wound onto a second carrier to reduce its post-winding tension. In some embodiments, by reducing its tension relative to the post-winding tension on the initially provided carrier spool of the fiber, the porosity of the spool of the tension-reduced fiber is increased relative to a higher tension post-winding spool of the same fiber. In certain embodiments, a commercially available tension control device is used to precisely tension the spool or cone of the fiber. In certain embodiments, a highly textured fiber is wound onto a spool at a tension of 0.5 g to 10 g, producing a porous spool of fiber. In some embodiments, a polymer-aerogel-precursor solution may be introduced into the porous spool of fiber. In certain preferred embodiments, the tension of the fiber is controlled to a tension of 1 g to 20 g during the time the fiber is exposed to a liquid solution comprising a polymer-aerogel-precursor and / or before the time the fiber is exposed to a liquid solution comprising a polymer-aerogel-precursor. For example, as Fig. 9 As shown, the fiber (3) is taken from a commercial fiber bundle (34), passed through a tension control device (11), and rewound at a controlled tension to form a second bobbin (10) of fiber before exposing the fiber to the polymer-aerogel / precursor solution. In another example, Fig.11 In the process, the fiber (1) is passed under a roller (13) through a bath (12) of a polymer-aerogel / precursor solution, and the tension of the fiber can be controlled during the time the fiber is exposed to the polymer-aerogel / precursor solution.

[0170] In some embodiments, when the fiber is not on a bobbin, the tension in the fiber is controlled. In certain embodiments, a polymer-aerogel-precursor solution can be applied to the fiber when the fiber is not on a bobbin or a carrier. In certain embodiments, the tension of the fiber is controlled. In certain embodiments, relative to the same fiber under a larger tension, the fiber having a tension lower than the tension after winding on a standard carrier bobbin without fiber winding can show increased pores between its strands. In certain embodiments, the fiber under a tension of 1g to 20g can be contacted with a polymer-aerogel-precursor solution to produce a polymer-gel / fiber composite. In certain embodiments, relative to a composite made of the same fiber, when the fiber is under a higher degree of tension, when in contact with a polymer-aerogel-precursor solution, the resulting polymer-aerogel / fiber composite shows an increased aerogel mass load.

[0171] In an illustrative embodiment, the tension of the multi-stranded fibers is controlled to be 10 g as the multi-stranded fibers are moved through the polymer-aerogel-precursor solution in a roll-to-roll process.

[0172] As will be understood by those of ordinary skill in the art, when applied to the processing of fibers or fabrics, the term roll-to-roll means a process performed when the fibers or fabrics are in an unwound form while moving from a distribution spool or roller to a collection spool or roller. In some embodiments, several continuous processing steps may be sequentially performed in the production of a fiber composite material or a fabric composite material, forming a single roll-to-roll process. In some embodiments, several continuous processing steps may be sequentially performed in the production of a fiber composite material or a fabric composite material, forming a single continuous process, wherein the feeding of fibers or fabrics to the process is continuous. Without wishing to be bound by any particular theory, it is believed that lower tension increases the space between the strands of a multi-strand fiber or a fabric comprising multi-strand fibers, and therefore increases the amount of polymer-aerogel-precursor solution that can be applied to the fiber or fabric.

[0173] In certain embodiments, the fiber or fabric is pretreated by any of the various combinations of pretreatment processes described herein. In a non-limiting illustrative embodiment, a multi-stranded mechanically textured polyamide fiber is selected and treated with a chemical etching process. The fiber is then exposed to an N-methyl-2-pyrrolidone vapor atmosphere that swells the fiber. The fiber is then wound onto a bobbin with a controlled tension. The bobbin of the fiber is then contacted with a polymer-aerogel-precursor solution.

[0174] In certain embodiments, the fibers or fabric are not pretreated prior to exposing them to the liquid solution comprising the polymer-aerogel-precursor.

[0175] In some embodiments, the fiber or fabric is wound on a bobbin and covered with a layer of covering fiber, fabric, sheet or other suitable covering material. The covering material is applied to the fiber-wound or fabric-wound bobbin before gelling the polymer-aerogel-precursor solution, or before or after the fiber or fabric bobbin is introduced into the polymer-aerogel-precursor solution. In certain embodiments, the covering prevents uneven and / or excessive loading of the polymer gel precursor on the entire exterior of the fiber or fabric bobbin, for example, reducing the accumulation of gel adhesion and / or excessive loading to the outer layer of the fiber or fabric bobbin.

[0176] In some embodiments, the fibers are exposed to a liquid solution comprising a polymer-aerogel-precursor. Fig.11 As shown, the fiber (1) is exposed to a polymer-aerogel-precursor solution (12). In some embodiments, the fabric is exposed to a liquid solution containing a polymer-aerogel-precursor. For example, Fig.31 As shown, the fabric (24) is exposed to the polymer-aerogel-precursor solution (12). In some embodiments, the fabric including the prefabricated garment is exposed to the polymer-aerogel-precursor solution. For example, Fig.30 As shown, a fabric (27) including a prefabricated garment is exposed to a liquid solution (12) comprising a polymer-aerogel-precursor. In certain embodiments, the polymer-aerogel-precursor solution wets the fiber or fabric to a certain extent. In some embodiments, the solution wets the fiber or fabric by capillary action driven wetting. In some embodiments, a driving force is applied to increase the wetting of the fiber by the solution. In certain embodiments, the driving force comprises an increased or decreased gas pressure. The pressure can vary throughout the process and can involve a pressure less than or equal to 760 Torr, greater than 760 Torr, 700 Torr to 760 Torr, 760 Torr to 1000 Torr, 1 Torr to 760 Torr, 760 Torr to 2000 Torr, or any suitable pressure. In certain embodiments, the wetting of the fiber or fabric can be driven by pumping the polymer-aerogel-precursor solution onto the fiber or fabric and / or pumping through the fiber or fabric.

[0177] Typically, polymer aerogel materials can be made from precursors such as gels. As provided herein, gels can be colloidal systems in which nanoporous, nanostructured solid networks span the volume occupied by a liquid medium. Therefore, gels can have two components: a spongy solid skeleton that imparts gel solid-like cohesiveness and a liquid that infiltrates the holes of the skeleton. In some embodiments, polymer aerogels are derived from polymer gels.

[0178] Gels of different compositions can be synthesized by a variety of methods that can include sol-gel methods. The sol-gel method involves producing a sol or colloidal suspension of very small solid particles in a continuous liquid medium, wherein nanostructures (e.g., nanoparticles, nanotubes, nanosheets, graphene, nanophase oligomers or polymer aggregates) form solid particles dispersed in the liquid medium. Very small solid particles can be formed in situ or non-in situ and dispersed in a liquid. The sol-gel method also involves interconnecting the nanostructures in the sol (e.g., by covalent bonding or ionic bonding, polymerization, physical adsorption or other mechanisms) to form a 3D network, thereby forming a gel.

[0179] In some embodiments, fiber or fabric is provided. In certain embodiments, fiber or fabric is contacted with polymer-aerogel-precursor solution. In certain embodiments, liquid phase polymer-aerogel-precursor solution forms gel material on fiber or fabric, around fiber or fabric and / or in fiber or fabric to form polymer-gel / fiber composite material or polymer-gel / fabric composite material respectively. In some embodiments, polymer-aerogel composite material is derived from polymer-gel composite material. In certain embodiments, polymer-gel / fiber composite material or polymer-gel / fabric composite material is subjected to drying step to form polymer-aerogel / fiber composite material or polymer-aerogel / fabric composite material respectively using any suitable drying method.

[0180] In some embodiments, the polymer aerogel material in the fiber composite material comprises a polyimide. Figure 1 As shown, the aerogel (2) in the fiber composite material can include polyimide. In some embodiments, the polymer aerogel material in the fabric composite material includes polyimide. For example, Fig.25BAs shown, the aerogel (2) in the fabric composite material can contain polyimide. In some embodiments, a fiber or fabric is provided. In some embodiments, the fiber or fabric is contacted with a polyimide-aerogel-precursor solution. In some embodiments, the liquid phase polyimide-aerogel-precursor solution forms a gel material on the fiber or fabric, around the fiber or fabric, and / or within the fiber or fabric to form a polymer-gel / fiber composite or a polymer-gel / fabric composite, respectively. In some embodiments, the polymer-gel / fiber composite or the polymer-gel / fabric composite can be imidized to form a polyimide-gel / fiber composite or a polyimide-gel / fabric composite. In some embodiments, the polyimide-aerogel composite is derived from a polyimide-gel composite. In some embodiments, the polyimide-gel / fiber composite or the polyimide-gel / fabric composite is subjected to a drying step using any suitable drying method to form a polyimide-aerogel / fiber composite or a polyimide-aerogel / fabric composite, respectively. In some embodiments, the polymer-gel / fiber composite comprises a polyimide gel. For example, in Fig.15A , Fig. 15B , Fig. 15C and Fig.15D In some embodiments, the polymer-gel (28) in the polymer-gel / fiber composite material may include a polyimide gel. In some embodiments, the polymer-aerogel / fiber composite material includes a polyimide aerogel.

[0181] In some embodiments, the polyimide gel is derived from the reaction of one or more amines with one or more anhydrides. Suitable amines may include those listed below and elsewhere herein. Suitable anhydrides may include those listed below and elsewhere herein. In some embodiments, the anhydrides and amines are contacted in a suitable solvent. Suitable solvents may include those listed below and elsewhere herein. In some embodiments, the amine reacts with the anhydride to form a polyamic acid, which is then imidized to form a polyimide. In certain embodiments, the polyamic acid is chemically imidized. In some embodiments, the polyamic acid is thermally imidized.

[0182] In some embodiments, the polyimide gel is derived from the reaction of one or more anhydrides with one or more isocyanates. In some embodiments, the anhydrides include dianhydrides. In some embodiments, the isocyanates include diisocyanates, triisocyanates, triisocyanatophenylmethane, toluene diisocyanate trimer and / or methylene diphenyl diisocyanate trimer. In some embodiments, the anhydrides and isocyanates are contacted in a suitable solvent.

[0183] In some embodiments, the polyimide gel is derived from norbornene-terminated bisnadimide oligomers.

[0184] In some embodiments, the polyimide gel is derived from poly(amic acid) ammonium salt. The poly(amic acid) salt is produced by the following process: reacting a diamine and a dianhydride in a suitable solvent to prepare a poly(amic acid) solution; pouring the poly(amic acid) solution into deionized water; washing, drying, and crushing the resulting sediment to prepare a poly(amic acid) powder; reacting the poly(amic acid) powder with an imidization catalyst in deionized water until uniform and transparent. The resulting suspension can then be frozen and subsequently dried using a freeze dryer for 24 to 36 hours. After freeze drying, the dry gel can be heated at 100°C, 120°C, 150°C for 1 hour, at 180°C for 0.5 hours, and at 250°C or 300°C for 0.25 hours.

[0185] In some embodiments, the anhydride includes an aromatic dianhydride; an aromatic trianhydride; an aromatic tetraanhydride; an aromatic anhydride having 6 to 24 carbon atoms and 1 to 4 aromatic rings, which may be fused, coupled by a biaryl bond, or connected by one or more linking groups selected from C1 to C6 alkylene, oxygen, sulfur, ketone, sulfoxide, sulfone, etc.; biphenyl-3,3',4,4'-tetracarboxylic dianhydride (BPDA); 3,3',4,4' -biphenyltetracarboxylic dianhydride; 2,3,3',4'-biphenyltetracarboxylic dianhydride (a-BPDA); 2,2',3,3'-biphenyltetracarboxylic dianhydride; 3,3',4,4'-benzophenone-tetracarboxylic dianhydride; benzophenone-3,3',4,4'-tetracarboxylic dianhydride (BTDA); pyromellitic dianhydride; 4,4'-hexafluoroisopropylidene diphthalic dianhydride (6FDA); 4,4'-(4,4' -isopropylidene diphenoxy)-bis(phthalic anhydride); 4,4'-oxydiphthalic anhydride (ODPA); 4,4'-oxydiphthalic dianhydride; 3,3',4,4'-diphenylsulfone tetracarboxylic dianhydride (DSDA); hydroquinone dianhydride; hydroquinone diphthalic anhydride (HQDEA); 4,4'-bisphenol A dianhydride (BPADA); ethylene glycol bis(trimellitic anhydride) (TMEG); 2,2 -bis(3,4-dicarboxyphenyl)propane dianhydride; bis(3,4-dicarboxyphenyl)sulfoxide dianhydride; poly(siloxane-containing dianhydride); 2,3,2',3'-benzophenonetetracarboxylic dianhydride; 3,3',4,4'-benzophenonetetracarboxylic dianhydride; naphthalene-2,3,6,7-tetracarboxylic dianhydride; naphthalene-1,4,5,8-tetracarboxylic dianhydride; 3,3',4,4'-biphenylsulfonetetracarboxylic dianhydride; 3,4,9,10- Tetracarboxylic dianhydride; bis(3,4-dicarboxyphenyl)sulfide dianhydride; bis(3,4-dicarboxyphenyl)methane dianhydride; 2,2-bis(3,4-dicarboxyphenyl)propane dianhydride; 2,2-bis(3,4-dicarboxyphenyl)hexafluoropropylene; 2,6-dichloronaphthalene 1,4,5,8-tetracarboxylic dianhydride; 2,7-dichloronaphthalene-1,4,5,8-tetracarboxylic dianhydride; 2,3,6,7-tetrachloronaphthalene-1,4,5,8-tetracarboxylic dianhydride; phenanthrene-8,9,10-tetracarboxylic dianhydride; pyrazine-2,3,5,6-tetracarboxylic dianhydride; benzene-1,2,3,4-tetracarboxylic dianhydride; and / or thiophene-2,3,4,5-tetracarboxylic dianhydride.

[0186] In some preferred embodiments, the anhydride comprises biphenyl-3,3',4,4'-tetracarboxylic dianhydride (BPDA).

[0187] In some embodiments, the amine includes 3,4'-oxydiphenylamine (3,4-ODA); 4,4'-oxydiphenylamine (4,4-ODA or ODA); p-phenylenediamine (pPDA); m-phenylenediamine (mPDA); p-phenylenediamine (mPDA); 2,2'-dimethylbenzidine (DMBZ); 4,4'-bis(4-aminophenoxy)biphenyl; 2,2'-bis[4-(4-aminophenoxy)phenyl]propane; diphenylamine p-xylidine (BAX); 4,4'-methylenedianiline (MDA); 4,4'-[1,3-phenylenebis(1-methyl-ethylidene)]dianiline (dianiline-m); 4,4'-[1,4-phenylenebis(1-methyl-ethylidene)]dianiline (dianiline-m). p); 3,3'-dimethyl-4,4'-diaminobiphenyl (o-tolidine); 2,2-bis[4-(4-aminophenoxy)phenyl]propane (BAPP); 3,3'-dihydroxy-4,4'-diaminobiphenyl (HAB); 3,3'-diaminodiphenyl sulfone (3,3'-DDS); 4,4'-diaminodiphenyl sulfone (4,4'-DDS); 4,4'-diaminodiphenyl sulfide (ASD); 2,2-bis[4-(4-aminophenoxy)phenyl]sulfone (BAPS); 2,2-bis[4-(3-aminophenoxy)benzene] (m-BAPS); 1,4-bis(4-aminophenoxy)benzene (TPE-Q); 1,3-bis(4-aminophenoxy)benzene (TPE-R) ; 1,3'-bis(3-aminophenoxy)benzene (APB-133); 4,4'-bis(4-aminophenoxy)biphenyl (BAPB); 4,4'-diaminobenzanilide (DABA); 9,9'-bis(4-aminophenyl)fluorene (FDA); o-tolidine sulfone (TSN); methylenebis(o-aminobenzoic acid) (MBAA); 1,3'-bis(4-aminophenoxy)-2,2-dimethylpropane (DANPG); 2,3,5,6-tetramethyl-1,4-phenylenediamine (TMPD); 3,3',5,5'-tetramethylbenzidine (3355TMB); 1,5-bis(4-aminophenoxy)pentane (DA5MG); 2,5-diaminotrifluorotoluene (25DBTF ); 3,5-diaminotrifluorotoluene (35DBTF); 1,3-diamino-2,4,5,6-tetrafluorobenzene (DTFB); 2,2'-bis(trifluoromethyl)benzidine (22TFMB); 3,3'-bis(trifluoromethyl)benzidine (33TFMB); 2,2-bis[4-(4-aminophenoxyphenyl)]hexafluoropropane (HFBAPP); 2,2-bis(4-aminophenyl)hexafluoropropane (Bis-A-AF); 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane (Bis-AP-AF); 2,2-bis(3-amino-4-methylphenyl)hexafluoropropane (Bis-AT-AF); o-phenylenediamine; diaminobenzanilide; 3,5-diaminobenzoic acid;3,3'-diaminodiphenyl sulfone; 4,4'-diaminodiphenyl sulfone; 1,3-bis-(4-aminophenoxy)benzene; l,3-bis(3-aminophenoxy)benzene; 1,4-bis(4-aminophenoxy)benzene; 1,4-bis(3-aminophenoxy)benzene; 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluoropropane; 2,2-bis(3-aminophenyl)hexafluoropropane; 4,4'-isopropylidene diphenylamine; 1-(4-aminophenoxy)-3-(3-aminophenoxy)benzene; 1-(4-aminophenoxy)-4-(3-aminophenoxy)benzene; bis[4-(4-aminophenoxy)phenyl]sulfone; bis[4-(3-aminophenoxy)phenyl]sulfone; bis(4-[4-aminophenoxy)phenyl]sulfone phenyl) ether; 2,2'-bis(4-aminophenyl)hexafluoropropylene; 2,2'-bis(4-phenoxyaniline)isopropylidene; 1,2-diaminobenzene; 4,4'-diaminodiphenylmethane; 2,2-bis(4-aminophenyl)propane; 4,4'-diaminodiphenylpropane; 4,4'-diaminodiphenylsulfide; 4,4-diaminodiphenylsulfone; 3,4'-diaminodiphenyl ether; 4,4'-diaminodiphenyl ether; 2,6-diaminopyridine; bis(3-aminophenyl)diethylsilane; 4,4'-diaminodiphenyldiethylsilane; benzidine-3'-dichlorobenzidine; 3,3'-dimethoxybenzidine; 4,4'-diaminobenzophenone; N,N-bis(4-aminophenyl)propane 1,5-Diaminonaphthalene; 3,3'-dimethyl-4,4'-diaminobiphenyl; 4-aminophenyl-3-aminobenzoate; N,N-bis(4-aminophenyl)aniline; bis(p-β-aminotert-butylphenyl)ether; p-bis-2-(2-methyl-4-aminopentyl)benzene; p-bis(1,1-dimethyl-5-aminopentyl)benzene; l,3-bis(4-aminophenoxy)benzene; m-xylene diamine; p-xylene diamine; 4,4'-diaminodiphenyl ether phosphine oxide; 4,4'-diaminodiphenyl N-methylamine; 4,4'-diaminodiphenyl N-aniline; amino-terminated polydimethylsiloxane; amino-terminated polypropylene oxide; Amino-terminated polybutylene oxide; 4,4'-methylenebis(2-methylcyclohexylamine); 1,2-diaminoethane; 1,3-diaminopropane; 1,4-diaminobutane; 1,5-diaminopentane; 1,6-diaminohexane; 1,7-diaminoheptane; 1,8-diaminooctane; 1,9-diaminononane; 1,10-diaminodecane; 4,4'-methylenebis(aniline); 2,2'-dimethylbenzidine; dianiline-p-xylidine; 4,4'-bis(4-aminophenoxy)biphenyl; 3,3'-bis(4-aminophenoxy)biphenyl; 4,4'-(1,4-phenylenediisopropylidene)dianiline; and / or 4,4'-(1,3-phenylenediisopropylidene)dianiline. ;

[0188] In some preferred embodiments, the amine includes 4,4'-oxydiphenylamine (4,4-ODA or ODA), 2,2'-dimethylbenzidine (DMBZ), and / or 4,4'-[1,3-phenylenebis(1-methyl-ethylene)]dianiline (dianiline-m).

[0189] In some embodiments, the isocyanate includes a triisocyanate; an aliphatic triisocyanate; an aromatic isocyanate containing three or more isocyanate groups; an aromatic triisocyanate; a triisocyanate based on hexamethylene diisocyanate; a trimer of hexamethylene diisocyanate; hexamethylene diisocyanate; a triisocyanate containing an isocyanurate; a diisocyanate containing an isocyanurate; Desmodur N3200; Desmodur N3300; Desmodur N100; Desmodur N3400; Desmodur N3390; Desmodur N3390 BA / SN; Desmodur N3300 BA; Desmodur N3600; Desmodur N3790 BA; 2675; Desmodur blulogiq 3190; Desmodur XP 2860; Desmodur N3400; Desmodur XP 2840; Desmodur N3580 BA; MR; Mondur MRS; methylene diphenyl diisocyanate; diphenylmethane 2,2'-diisocyanate, diphenylmethane 2,4'-diisocyanate and / or diphenylmethane 4,4'-diisocyanate (MDI); naphthylene 1,5-diisocyanate (NDI); toluene diisocyanate; toluene 2,4-diisocyanate and / or toluene 2,6-diisocyanate (TDI); 3,3'-dimethylbiphenyl diisocyanate; 1,2-diphenylethane diisocyanate and / or p-phenylene diisocyanate (PPDI); trimethylene diisocyanate, tetramethylene diisocyanate, pentamethylene diisocyanate, hexamethylene diisocyanate, heptamethylene diisocyanate and / or octamethylene diisocyanate; 2-methyl Pentamethylene 1,5-diisocyanate; 2-ethylbutene 1,4-diisocyanate; pentamethylene 1,5-diisocyanate; butene 1,4-diisocyanate; 1-isocyanato-3,3,5-trimethyl-5-isocyanatomethylcyclohexane (isophorone diisocyanate, IPDI); 1,4-bis(isocyanatomethyl)cyclohexane and / or 1,3-bis(isocyanatomethyl)cyclohexane (HXDI); cyclohexane 1,4-diisocyanate; 1-methylcyclohexane 2,4-diisocyanate; 1-methylcyclohexane 2,6-diisocyanate; dicyclohexylmethane 4,4'-diisocyanate; dicyclohexylmethane 2,4'-diisocyanate; and / or dicyclohexylmethane 2,2'-diisocyanate.

[0190] In some embodiments, polyimide gel is derived from the reaction of amine and anhydride. In some embodiments, the reaction of amine and anhydride forms poly (amic acid) oligomer. In some embodiments, poly (amic acid) oligomer chemical imidization is made to produce polyimide oligomer. In some embodiments, chemical imidization is realized by contacting poly (amic acid) oligomer with a dehydrating agent. In some embodiments, the dehydrating agent includes acetic anhydride, propionic anhydride, n-butyric anhydride, benzoic anhydride, trifluoroacetic anhydride, phosphorus trichloride, and / or dicyclohexylcarbodiimide. In some embodiments, chemical imidization is catalyzed by contacting a solution comprising poly (amic acid) oligomer and a dehydrating agent with an imidization catalyst.

[0191] In some embodiments, the imidization catalyst includes pyridine; picoline; quinoline; isoquinoline; 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU); DBU phenolate; carboxylate of DBU; triethylenediamine; carboxylate of triethylenediamine; lutidine; n-methylmorpholine; triethylamine; tripropylamine; tributylamine; N,N-dimethylbenzylamine; N,N'-dimethylpiperazine; N,N-dimethylcyclohexylamine; N,N',N"-tris(dialkylaminoalkyl)-s-hexahydrotriazine, such as N,N',N"-tris(dimethylaminopropyl)-s-hexahydrotriazine; tris(dimethylaminomethyl)phenol; bis(2-dimethylaminoethyl) ether; N,N,N,N,N-pentamethyldiethylenetriamine; methylimidazole; dimethylimidazole; dimethylbenzylamine; 1,6-diazabicyclo[5.4.0]undec-7-ene (IUPAC: 1,4-diazabicyclo[2.2.2]octane); triethylenediamine; dimethylaminoethanolamine; dimethylaminopropylamine; N,N-dimethylaminoethoxyethanol; N,N,N-trimethylaminoethylethanolamine; triethanolamine; diethanolamine; triisopropanolamine; diisopropanolamine; and / or any suitable trialkylamine.

[0192] In some embodiments, the polyimide gel is derived from the reaction of an amine with an anhydride. In some embodiments, the reaction of an amine and an anhydride forms a poly(amic acid) oligomer. In some embodiments, the poly(amic acid) oligomer is thermally imidized to produce a polyimide oligomer. In some embodiments, the poly(amic acid) oligomer is heated to a temperature greater than 80°C, greater than 90°C, greater than 100°C, greater than 150°C, greater than 180°C, greater than 190°C, or any suitable temperature.

[0193] In some embodiments, diamine and / or dianhydride can be selected based on commercial availability and / or price. In some embodiments, diamine and / or dianhydride can be selected based on desired material properties. In some embodiments, specific diamine and / or dianhydride can impart specific properties to polymer. For example, in some embodiments, diamine and / or dianhydride with flexible linking group between phenyl groups can be used to prepare polyimide aerogel with increased flexibility. In some embodiments, diamine and / or dianhydride comprising side methyl groups can be used to prepare polyimide aerogel with increased hydrophobicity. In other embodiments, diamine and / or dianhydride comprising fluorinated moieties such as trifluoromethyl groups can be used to prepare polyimide aerogel with increased hydrophobicity.

[0194] In some embodiments, two or more diamines and / or two or more dianhydrides are used. In an illustrative embodiment, two diamines are used. Relative to all two diamines, the mole percentage of the first diamine can vary from 0% to 100%. In some embodiments, relative to all two diamines, the mole percentage of the first diamine includes less than 100%, less than 90%, less than 80%, less than 70%, less than 60%, less than 50%, less than 40%, less than 30%, less than 20%, less than 10%, or 0%. In other embodiments where more than two diamines are used, relative to all diamines, the mole percentage of each diamine can vary from 0% to 100%. In another illustrative example, two dianhydrides are used. Relative to all two dianhydrides, the mole percentage of the first dianhydride can vary from 0% to 100%. The mole percentage of the first dianhydride relative to all two dianhydrides includes less than 100%, less than 90%, less than 80%, less than 70%, less than 60%, less than 50%, less than 40%, less than 30%, less than 20%, less than 10%, or 0%. In other embodiments where more than two dianhydrides are used, the mole percentage of each dianhydride relative to all dianhydrides can vary from 0% to 100%.

[0195] In some embodiments, multiple diamines are used. In some embodiments, the first diamine is added to the solvent, and then the dianhydride is added. In some embodiments, each amino site on the diamine reacts with the anhydride site on the different dianhydrides to form an anhydride-terminated oligomer. In some embodiments, the second diamine is then added to the solution. These diamines react with the terminal anhydrides on the oligomers in the solution to form longer amino-terminated oligomers. Oligomers of different lengths are produced by such a process, and an alternating motif of the first diamine, then the dianhydride, and then the second diamine is produced. In some embodiments, three diamines are used. In some embodiments, the first diamine is reacted with about half of the total dianhydride. In some embodiments, the second diamine is then added to the solution, and then the remaining dianhydride is added, and finally the third diamine is added. Without wishing to be bound by any particular theory, it is believed that this method promotes spatial uniformity of properties throughout the gel network, where simply mixing all monomers together at the same time and allowing dianhydrides and diamines to react randomly with others at the same time may result in phase separation and / or spatial heterogeneity of domains rich in a specific diamine.

[0196] In some embodiments, the polymer weight percentage in the solution is controlled during the polymer gel synthesis. The term polymer weight percentage in the solution refers to the weight of the monomers in the solution minus the weight of the by-products produced by the condensation reaction between the monomers, relative to the weight of the solution. The polymer weight percentage in the solution can be less than 1%, less than 2%, less than 3%, less than 4%, less than 5%, less than 6%, less than 7%, less than 8%, less than 9%, less than 10%, less than 12%, less than 14%, less than 16%, less than 18%, less than 20%, and / or 20% to 30%. In some preferred embodiments, the polymer weight percentage is 5% to 15%.

[0197] In some embodiments, the reaction of diamine and dianhydride produces an oligomer comprising at least a repeating unit of diamine and dianhydride. In some embodiments, the oligomer comprises 1 repeating unit, is less than 2 repeating units, is less than 5 repeating units, is less than 10 repeating units, is less than 20 repeating units, is less than 30 repeating units, is less than 40 repeating units, is less than 50 repeating units, is less than 60 repeating units, is less than 80 repeating units, is less than 100 repeating units or is less than 200 repeating units. In some embodiments, the oligomer has an average degree of polymerization of less than 10, less than 20, less than 30, less than 40, less than 60, less than 80 or less than 100. In some embodiments, the oligomer comprises an end anhydride group, i.e., the two ends of the oligomer comprise an end anhydride group. In some embodiments, the oligomer comprises an end amine group, i.e., the two ends of the oligomer comprise an end amine group.

[0198] In some embodiments, the oligomers are crosslinked by a crosslinking agent. In some embodiments, the terminal groups on the oligomers are reacted with a multifunctional crosslinking agent and then reacted with the terminal groups on at least one additional oligomer. In some embodiments, the crosslinking agent includes triamines; aliphatic triamines; aromatic amines containing three or more amine groups; aromatic triamines; 1,3,5-tris(aminophenoxy)benzene (TAB); tris(4-aminophenyl)methane (TAPM); tris(4-aminophenyl)benzene (TAPB); tris(4-aminophenyl)amine (TAPA); 2,4,6-tris(4-aminophenyl)pyridine (TAPP); 4,4',4"-methanetriyltriphenylamine; N,N,N ',N'-tetrakis(4-aminophenyl)-1,4-phenylenediamine; polyoxypropylene triamine; N',N'-bis(4-aminophenyl)benzene-1,4-diamine; triisocyanates; aliphatic triisocyanates; aromatic isocyanates containing three or more isocyanate groups; aromatic triisocyanates; triisocyanates based on hexamethylene diisocyanate; trimers of hexamethylene diisocyanate; hexamethylene diisocyanate; polyisocyanates; polyisocyanates containing isocyanurates; Desmodur N3300; Desmodur N100; Desmodur N3400; Desmodur N3390; Desmodur N3390 BA / SN; Desmodur N3300 BA; Desmodur N3600; Desmodur N3790BA; Desmodur N3800; Desmodur N3900; Desmodur XP 2675; Desmodur blulogiq 3190; Desmodur XP 2860; Desmodur N3400; Desmodur XP 2840; Desmodur N3580 BA; Mondur MRS; methylene diphenyl diisocyanate; diphenylmethane 2,2'-diisocyanate, diphenylmethane 2,4'-diisocyanate and / or diphenylmethane 4,4'-diisocyanate (MDI); naphthylene 1,5-diisocyanate (NDI); toluene diisocyanate; toluene 2,4-diisocyanate and / or toluene 2,6-diisocyanate (TDI); 3,3'-dimethylbiphenyl diisocyanate; 1,2-diisocyanate Phenylethane diisocyanate and / or p-phenylene diisocyanate (PPDI); trimethylene diisocyanate, tetramethylene diisocyanate, pentamethylene diisocyanate, hexamethylene diisocyanate, heptamethylene diisocyanate, and / or octamethylene diisocyanate; 2-methylpentamethylene 1,5-diisocyanate; 2-ethylbutene 1,4-diisocyanate; pentamethylene 1,5-diisocyanate; butene 1,4-diisocyanate ; 1-isocyanato-3,3,5-trimethyl-5-isocyanatomethylcyclohexane (isophorone diisocyanate, IPDI); 1,4-bis(isocyanatomethyl)cyclohexane and / or 1,3-bis(isocyanatomethyl)cyclohexane (HXDI); cyclohexane 1,4-diisocyanate; 1-methylcyclohexane 2,4-diisocyanate and / or 1-methylcyclohexane 2,6-diisocyanate; dicyclohexylmethane 4,4'-diisocyanate cyanate, dicyclohexylmethane 2,4'-diisocyanate and / or dicyclohexylmethane 2,2'-diisocyanate; octa(aminophenoxy)silsesquioxane (OAPS); 4,4-oxydiphenylamine (ODA); (3-aminopropyl)triethoxysilane (APTES); modified graphene oxide (m-GO); 1,3,5-benzenetricarbonyltrichloride (BTC); poly(maleic anhydride) (PMA); and / or melamine.

[0199] In some embodiments, the reaction between the amine and the anhydride, and / or the chemical imidization occurs in a solvent. In some embodiments, the solvent includes dimethyl sulfoxide; diethyl sulfoxide; N,N-dimethylformamide; N,N-diethylformamide; N,N-dimethylacetamide; N,N-diethylacetamide; N-methyl-2-pyrrolidone; 1-methyl-2-pyrrolidone; N-cyclohexyl-2-imidazolidinone; diethylene glycol dimethoxy ether; o-dichlorobenzene; phenols; cresol; xylenol; catechol; butyrolactone; and / or hexamethylphosphoramide.

[0200] In some embodiments, the aerogel material in the polymer-aerogel / fiber composite material comprises polyurea aerogel. Figure 1 As shown, the aerogel (2) in the fiber composite material may include polyurea. In some embodiments, the aerogel material in the polymer-aerogel / fabric composite material includes polyurea aerogel. For example, Fig.25B As shown, the aerogel (2) in the textile composite material may include polyurea. In some embodiments, the polyurea aerogel is derived from a polyurea gel.

[0201] In some embodiments, the polyurea gel is derived from the reaction of isocyanate with water, wherein the amine is formed in situ. In some embodiments, the polyurea gel is derived from the reaction of isocyanate with amine. Suitable isocyanates may include those listed above and elsewhere herein. Suitable amines may include those listed above and elsewhere herein. In some embodiments, the polyurea gel comprises aromatic groups. In some embodiments, the polyurea gel comprises isocyanurate. In some embodiments, the polyurea gel comprises a flame retardant portion, such as bromide, bromate, phosphate.

[0202] In some embodiments, monomers polymerized by free radical mediated polymerization are used to prepare the solid phase of the gel. In some embodiments, the monomers include acrylonitrile, methyl (methacrylate), styrene, 1,3-divinylbenzene, 1,3,5-trivinylbenzene, or any suitable monomer polymerized by free radical mediated polymerization.

[0203] In some embodiments, the solid phase of the gel comprises polyisocyanates, polyureas, polyurethanes, polyisocyanurates, polyimides, polyamides, polymer cross-linked oxides, polybenzoic acid, Oxazine.

[0204] In some embodiments, the polymer aerogel in the polymer-aerogel / fiber composite comprises polyurea, polyurethane, polyimide, polyamide, polymer cross-linked oxide, or polybenzoic acid. For example, Figure 1As shown, the aerogel (2) in the fiber composite material may comprise polyurea, polyurethane, polyimide, polyamide, polymer cross-linked oxide, or polybenzoic acid. Oxazine.

[0205] In some embodiments, the polymer aerogel in the polymer-aerogel / fabric composite material comprises polyurea, polyurethane, polyimide, polyamide, polymer cross-linked oxide, or polybenzoic acid. For example, Fig.25B As shown, the aerogel (2) in the fabric composite material may comprise polyurea, polyurethane, polyimide, polyamide, polymer cross-linked oxide, or polybenzoic acid. Oxazine.

[0206] In some embodiments, polymer aerogel (for example, polymer aerogel in polymer-aerogel / fiber composite material and / or polymer-aerogel / fabric composite material) comprises biopolymer. In some embodiments, polymer aerogel comprises cellulose. In some embodiments, cellulose aerogel is synthesized via molten salt hydrate method. In some embodiments, cellulose aerogel is derived from microcrystalline cellulose and / or nanocellulose. In some embodiments, cellulose is made hydrophobic by treating with hydrophobic substance such as methyltrimethoxysilane, trimethylchlorosilane, hexamethyldisilazane, hexamethyldisiloxane or other hydrophobic substance.

[0207] In some embodiments, the polymer aerogel (e.g., a polymer aerogel in a polymer-aerogel / fiber composite and / or a polymer-aerogel / fabric composite) comprises a phenolic polymer. In some embodiments, the polymer aerogel comprises a condensation product of resorcinol, phenol, phloroglucinol, melamine, and / or cresol with formaldehyde.

[0208] In some embodiments, polyols are used to prepare the solid phase of the gel material. In some preferred embodiments, the polyols include resorcinol, phloroglucinol, bisphenol A, tris(hydroxyphenyl)ethane, sulfonyl diphenol, dihydroxybenzophenone, polyether alcohol, ethylene glycol, propylene glycol, or another suitable polyol.

[0209] In some embodiments, the gel material is prepared using a solvent for preparing a polymer aerogel material. In some embodiments, the solvent includes ketones; aldehydes; alkyl alkanoates; ethyl acetate; amides, such as formamide; N-methyl-2-pyrrolidone; sulfoxides, such as dimethyl sulfoxide; aliphatic halogenated hydrocarbons; alicyclic halogenated hydrocarbons; halogenated aromatic compounds; and / or fluorinated ethers.

[0210] In some embodiments, aldehyde and / or ketone solvents are used to prepare the gel material. In some embodiments, the solvent includes acetaldehyde; propionaldehyde; n-butyraldehyde; isobutyraldehyde; 2-ethylbutyraldehyde; valeraldehyde; isovaleraldehyde; 2-methylvaleraldehyde; 2-ethylhexanal; acrolein; methacrolein; crotonaldehyde; furfural; acrolein dimer; methacrolein dimer; 1,2,3,6-tetrahydrobenzaldehyde; 6-methyl-3-cyclohexenal; cyanoacetaldehyde; ethyl glyoxylate; benzaldehyde; acetone; diethyl ketone; methyl ethyl ketone; methyl isobutyl ketone; methyl n-butyl ketone; ethyl isopropyl ketone; 2-acetylfuran; 2-methoxy-4-methylpentan-2-one; cyclohexanone; and / or acetophenone.

[0211] In some embodiments, an alkyl alkanoate solvent is used to prepare the gel material. In some embodiments, the solvent includes methyl formate; methyl acetate; ethyl formate; butyl acetate; and / or ethyl acetate.

[0212] In some embodiments, an acetal solvent is used to prepare the gel material. In some embodiments, the solvent includes diethoxymethane; dimethoxymethane; and / or 1,3-dioxolane.

[0213] In some embodiments, dialkyl ether and / or cyclic ether solvents are used to prepare the gel material. In some embodiments, the solvent includes methyl ethyl ether; diethyl ether; methyl propyl ether; methyl isopropyl ether; propyl ethyl ether; ethyl isopropyl ether; dipropyl ether; propyl isopropyl ether; diisopropyl ether; methyl butyl ether; methyl isobutyl ether; methyl tert-butyl ether; ethyl n-butyl ether; ethyl isobutyl ether; and / or ethyl tert-butyl ether. In some but not necessarily all embodiments, cyclic ethers, especially tetrahydrofuran, di ... Alkanes and / or tetrahydropyrans may be advantageous.

[0214] In some embodiments, a hydrocarbon solvent is used to prepare the gel material. In certain embodiments, the solvent includes ethane; propane; n-butane; isobutane; n-pentane; isopentane; cyclopentane; neopentane; hexane; and / or cyclohexane.

[0215] In some embodiments, a fluorocarbon solvent is used to prepare the gel material. In certain embodiments, the solvent includes difluoromethane; 1,2-difluoroethane; 1,1,1,4,4,4-hexafluorobutane; pentafluoroethane; 1,1,1,2-tetrafluoroethane; 1,1,2,2-tetrafluoroethane; pentafluorobutane and / or its isomers; tetrafluoropropane and / or its isomers; and / or pentafluoropropane and / or its isomers. Substantially fluorinated or perfluorinated (cyclo)alkanes having 2 to 10 carbon atoms may also be used.

[0216] In some embodiments, a fluorochlorocarbon solvent is used to prepare the gel material. In certain embodiments, the solvent includes chlorodifluoromethane; 1,1-dichloro-2,2,2-trifluoroethane; 1,1-dichloro-1-fluoroethane; 1-chloro-1,1-difluoroethane; 1-chloro-2-fluoroethane; 1,1,1,2-tetrafluoro-2-chloroethane; trichlorofluoromethane; dichlorodifluoromethane; trichlorotrifluoroethane; tetrafluorodichloroethane; 1-chloropropane and / or 2-chloropropane; dichloromethane; monochlorobenzene; and / or dichlorobenzene.

[0217] In some embodiments, a fluorinated ether solvent is used to prepare the gel material. In certain embodiments, the solvent includes bis-(trifluoromethyl) ether; trifluoromethyl difluoromethyl ether; methyl fluoromethyl ether; methyl trifluoromethyl ether; bis(difluoromethyl) ether; fluoromethyl difluoromethyl ether; methyl difluoromethyl ether; bis(fluoromethyl) ether; 2,2,2-trifluoroethyl difluoromethyl ether; pentafluoroethyl trifluoromethyl ether; pentafluoroethyl difluoromethyl ether; 1,1,2,2-tetrafluoroethyl difluoromethyl ether; 1,2,2,2-tetrafluoroethyl fluoromethyl ether; 1,2,2-trifluoroethyl difluoromethyl ether; 1,1-difluoroethyl methyl ether; and / or 1,1,1,3,3,3-hexafluoropropyl-2-yl fluoromethyl ether.

[0218] In some embodiments, the fibers are exposed to a liquid solution containing a polymer-aerogel-precursor in a continuous process. Fig.11 As shown, the fiber (1) moves through a bath of polymer-aerogel-precursor solution (12) in a continuous process. In certain embodiments, the fiber is exposed to the liquid solution containing the polymer-aerogel-precursor in a roll-to-roll manner. For example, Fig.12 As shown, the fiber (1) moves from a conveyor roll or spool (14) through a bath of polymer-aerogel-precursor solution (12) to a receiving roll or spool (15) in a roll-to-roll process. In some embodiments, the fabric is exposed to the liquid solution containing the polymer-aerogel-precursor in a continuous process. For example, Fig.31 As shown, the fabric (24) moves through a bath of polymer-aerogel-precursor solution (12) in a continuous process. In certain embodiments, the fabric is exposed to the liquid solution containing the polymer-aerogel-precursor in a roll-to-roll manner. For example, Fig.32As shown, the fabric (24) moves from a conveying roller or spool (14) through a bath of a polymer-aerogel-precursor solution (12) to a receiving roller or spool (15) in a roll-to-roll process. In certain embodiments, the fiber or fabric is exposed to the polymer-aerogel-precursor solution as it moves through the bath of the polymer-aerogel-precursor solution. In some embodiments, the movement of the fiber through the bath of the polymer-aerogel-precursor solution is performed by unwinding the fiber or fabric from one roller and winding it onto another roller. In some embodiments, the fiber or fabric is exposed to the polymer-aerogel-precursor solution by pouring and / or spraying the polymer-aerogel-precursor solution onto the fiber or fabric. In some embodiments, the fiber or fabric is exposed to the polymer-aerogel-precursor solution by immersing the fiber or fabric in a bath of the polymer-aerogel-precursor solution. In certain embodiments, the polymer-aerogel-precursor solution is applied to the fiber or fabric on a moving conveyor belt. In some embodiments, any combination of the above methods may be used. In some embodiments, the fiber or fabric is exposed to the liquid solution comprising the polymer-aerogel-precursor in a continuous process for less than 0.01 seconds, less than 0.05 seconds, less than 0.1 seconds, less than 0.5 seconds, less than 1 second, less than 5 seconds, less than 10 seconds, less than 15 seconds, less than 30 seconds, less than 1 minute, less than 5 minutes, less than 10 minutes, less than 30 minutes, or less than 1 hour. In some embodiments, a spool of fiber is exposed to the liquid solution comprising the polymer-aerogel-precursor. For example, Fig.10 As shown, a spool of fiber (10) is exposed to a bath of a polymer-aerogel-precursor solution (12). In some embodiments, a spool of fabric is exposed to a liquid solution containing a polymer-aerogel-precursor. For example, Fig.30As shown, the bobbin of fabric (26) is exposed to a bath of polymer-aerogel-precursor solution (12). In some embodiments, the bobbin of fiber or fabric is immersed in a bath of polymer-aerogel-precursor solution. In certain embodiments, the polymer-aerogel-precursor solution penetrates the pores of the fiber or fabric bobbin by diffusion. In some embodiments, the bobbin rotates while being partially immersed in a bath of polymer-aerogel-precursor solution. In some embodiments, the bobbin of fiber or fabric is immersed in a bath of liquid phase polymer-aerogel-precursor solution at ambient temperature and ambient pressure for a prescribed time, then removed from the bath, after which a polymer gel is formed in and / or on the fiber or fabric. In some embodiments, before gelation, the bobbin of fiber or fabric is left in a bath of polymer-aerogel-precursor solution and is not removed. In some embodiments, the bobbin of fiber or fabric is sprayed with a polymer-aerogel-precursor solution. In some embodiments, the polymer-aerogel-precursor solution is poured onto the bobbin of fiber or fabric. In some embodiments, the polymer-aerogel-precursor solution is applied to a spool of fiber or fabric using some combination of the foregoing methods. In some embodiments, the spool of fiber or fabric is exposed to a liquid solution comprising a polymer-aerogel-precursor for less than 1 minute, less than 10 minutes, less than 15 minutes, less than 25 minutes, less than 35 minutes, less than 45 minutes, less than 1 hour, or less than 2 hours.

[0219] In certain embodiments, a single fiber is exposed to a polymer-aerogel-precursor solution. In some embodiments, a plurality of parallel fibers such as a fiber bundle is exposed to a polymer-aerogel-precursor solution. In some embodiments, a portion of a fiber or fabric that is not on a spool, roller, core, beam, or carrier is exposed to a polymer-aerogel-precursor solution when it is unfolded from a spool, roller, core, beam, or carrier and wound on a second spool, roller, core, beam, or carrier. In some embodiments, the unwound portion of a fiber or fabric moves through a bath of a polymer-aerogel-precursor solution. In some embodiments, the unwound portion of a fiber or fabric is sprayed with a polymer-aerogel-precursor solution. In some embodiments, a polymer-aerogel-precursor solution is poured on the unwound portion of a fiber or fabric. In some embodiments, a polymer-aerogel-precursor solution is applied to an unwound fiber or fabric using some combinations of the aforementioned spraying method, bath method, and pouring method.

[0220] In some embodiments, the fiber or fabric is exposed to the polymer-aerogel-precursor in a continuous process. In certain embodiments, the fiber or fabric is exposed to the polymer-aerogel-precursor solution in a roll-to-roll manner. In certain embodiments, the fiber or fabric is unfolded from a spool, a roller, a core, a beam or other carriers, exposed to the polymer-aerogel-precursor solution, and then wound on another spool, a roller, a core, a beam or a carrier. In some embodiments, when the fiber or fabric contacts the polymer-aerogel-precursor, the tension in the unwound part of the fiber or fabric is controlled to a specific value. In certain embodiments, the tension of the control fiber or fabric allows some control of the amount of the pores in the fiber or fabric. In certain embodiments, the degree of tension affects the mass load of the polymer aerogel in the resulting polymer-aerogel / fiber composite or polymer-aerogel / fabric composite. In some embodiments, the tension of the fiber or fabric is controlled. In some embodiments, the tension of the fiber or fabric is controlled after the fiber or fabric contacts the polymer-aerogel-precursor solution. In certain embodiments, the fibers or fabrics can then be wound onto a spool at a controlled tension prior to gelation of the polymer-aerogel-precursor solution.

[0221] In some embodiments, the polymer-aerogel-precursor solution is prepared in a continuous manner. In some embodiments, the solution is continuously supplied to an application device or location where the solution is applied to the fibers or fabric. For example, Fig.13 As shown, the mixing device (16) combines two or more components in a continuous manner to form a polymer-aerogel-precursor solution (12), which is applied to the fiber (1). Fig.33As shown, a mixing device (16) combines two or more components in a continuous manner to form a polymer-aerogel-precursor solution (12), which is applied to a fabric (24). In some embodiments, the solution is supplied to a bath, wherein the fiber or fabric moves through the bath in a roll-to-roll manner. In some embodiments, two or more fibers or fabrics move through the bath simultaneously in a roll-to-roll manner. In an illustrative embodiment, the rate at which the solution is prepared and supplied to the bath in a continuous manner matches the rate at which the solution is applied to the fiber or fabric when the fiber or fabric moves through the bath in a roll-to-roll manner. In this way, the volume of the solution in the bath remains constant because the solution is continuously and simultaneously supplied to the bath and removed from the bath when applied to the fiber or fabric. Without wishing to be bound by any particular theory, it is believed that by preparing the polymer-aerogel-precursor solution in a continuous or semi-continuous manner, the processing time of the polymer-aerogel-precursor solution combined with the fiber or fabric may be extended beyond the gelation time of the solution, which is equivalent to the solution prepared in a single batch in a discontinuous process. In some embodiments, when the solution is applied to the fibers or fabric in a roll-to-roll manner, this can allow the solution to be applied to a larger amount of fibers or fabric than a solution prepared using a batch process could apply to the fibers or fabric. In some embodiments, the polymer-aerogel-precursor solution is prepared over a period of greater than 1 hour, greater than 2 hours, greater than 3 hours, greater than 4 hours, greater than 5 hours, greater than 6 hours, greater than 7 hours, or greater than 8 hours.

[0222] In some embodiments, a liquid solution comprising a polymer-aerogel-precursor is applied to the fiber in two sequential steps. In some embodiments, a liquid solution comprising a polymer-aerogel-precursor is applied to the fabric in two sequential steps. In certain embodiments, the fiber or fabric is contacted with a polymer-aerogel-precursor solution that will not gel without adding other components. In some embodiments, the amount of polymer-aerogel / fiber composites or polymer-aerogel / fabric composites that can be produced in a single batch may be limited by the gelation time of the polymer-aerogel-precursor solution. In certain embodiments, the timing of the treatment can be controlled by dividing the reactive components of the polymer-aerogel-precursor solution into at least two parts. In some embodiments, the method can be used to enable the polymer-aerogel-precursor solution to be continuously applied to any amount of fiber or fabric, without being limited by the gelation time of the polymer-aerogel-precursor solution. In certain embodiments, a portion of the polymer-aerogel-precursor solution can be combined in a continuous manner or in a discrete manner. In some embodiments, two solutions, a Part A solution and a Part B solution, are prepared such that neither the Part A solution nor the Part B solution forms a gel alone, but when the Part A precursor solution and the Part B precursor solution are contacted with each other, a polymer gel is obtained. In some embodiments, the Part A solution and the Part B solution are mixed and then the combined solution is contacted with the fiber or fabric. In some embodiments, the fiber or fabric is exposed to a liquid solution comprising the Part A polymer-aerogel-precursor and then to a liquid solution comprising the Part B polymer-aerogel-precursor. For example, Fig.14 As shown, the fiber (1) moves on roller (13) through the Part A solution (17) and then through the Part B solution (18). In some embodiments, the fabric is exposed to a liquid solution containing the Part A polymer-aerogel-precursor and then to a liquid solution containing the Part B polymer-aerogel-precursor. For example, Fig.34As shown, the fabric (24) moves on the roller (13) through the A part solution (17), followed by the B part solution (18). In some embodiments, the fiber or fabric is exposed to the polymer-aerogel-precursor solution and is infiltrated by the solution. In some embodiments, the infiltrated fiber or fabric is then subjected to an elevated temperature until gelation of the polymer-aerogel-precursor solution occurs. In certain embodiments, the infiltrated fiber or fabric is exposed to an atmosphere of gas or vapor that causes and / or accelerates the gelation of the polymer-aerogel-precursor solution. In some embodiments, the fiber or fabric infiltrated by the A part precursor solution is exposed to a vapor phase catalyst that causes the A part solution to form a polymer gel. In certain embodiments, the A part precursor solution is sprayed on the bobbin of the fiber or fabric, and then the B part precursor solution is sprayed on the bobbin of the fiber or fabric. In certain embodiments, the A part precursor solution is poured on the bobbin of the fiber or fabric, and then the part B precursor solution is poured on the bobbin of the fiber or fabric. In some embodiments, any combination of the above methods can be used. In some embodiments, the fibers are exposed to a liquid solution containing a polymer-aerogel-precursor and then to a vapor environment, such that the liquid solution containing a polymer-aerogel-precursor forms a polymer gel on and / or within the fibers after a period of time, forming a polymer-gel / fiber composite. Fig.16 In the process, the fiber (1) moves on a roller (13) through a liquid solution (12) and then through a vapor environment (35).

[0223] In some embodiments, the fabric is exposed to a liquid solution containing a polymer-aerogel-precursor and then to a vapor environment, so that the liquid solution containing a polymer-aerogel-precursor forms a polymer gel on and / or in the fabric after a period of time, forming a polymer-gel / fabric composite. Fig.36 In the process, the fabric (24) moves on a roller (13) through a liquid solution (12) and then through a vapor environment (35).

[0224] In some embodiments, the liquid solution containing the polymer-aerogel-precursor on and / or in the fibers forms a polymer gel on and / or in the fibers after a period of time, forming a polymer-gel / fiber composite. Fig.15A and Fig.15D In another example, the polymer-gel / fiber composite comprises a polymer gel (28) on a fiber (1). Fig. 15B and Fig. 15CIn some embodiments, the polymer-gel / fiber composite material comprises a polymer gel (28) on and within the fibers (1). In some embodiments, the liquid solution comprising a polymer-aerogel-precursor on and / or within the fabric forms a polymer gel on and / or within the fabric after a period of time, forming a polymer-gel / fabric composite material. For example, in Fig.35A and Fig.35B In some embodiments, the polymer-gel / fabric composite material comprises a polymer gel (28) on the surface of a fabric (24). In some embodiments, once the fiber or fabric is in contact with the polymer-aerogel-precursor solution, the fiber or fabric is wound on the bobbin and gelation of the polymer-aerogel-precursor solution occurs while the fiber or fabric is on the bobbin. In some embodiments, the bobbin is not actively wound or unwound during gelation of the polymer-aerogel-precursor solution. In some embodiments, once the fiber or fabric is in contact with the polymer-aerogel-precursor solution, the fiber or fabric is not wound while gelation of the polymer-aerogel-precursor solution occurs.

[0225] After the fiber or fabric is exposed to the polymer-aerogel-precursor solution, a method for causing gelation of the polymer-aerogel-precursor solution in and / or on the fiber or fabric can be applied. In some embodiments, the fiber or fabric is contacted with the polymer-aerogel-precursor solution. The fiber or fabric is then kept at a specified temperature for a specified amount of time to allow the polymer-aerogel-precursor solution to gel. In some embodiments, gelation occurs at ambient temperature. In some embodiments, gelation occurs at temperatures above ambient temperature. In some embodiments, gelation occurs at temperatures below ambient temperature.

[0226] In some embodiments, after gelation, polymer-gel / fiber composite or polymer-gel / fabric composite is aged for a specific time period. In certain embodiments, during this aging period, the solid network of gel is enhanced. In certain embodiments, the aging process is allowed to occur at ambient temperature. In certain embodiments, the aging process is allowed to occur at temperatures below ambient temperature. In certain embodiments, the aging process is allowed to occur at temperatures above ambient temperature. In certain embodiments, polymer-gel / fiber or polymer-gel / fabric is aged on a bobbin, roller, core, beam or other carrier. In certain embodiments, polymer-gel / fiber or polymer-gel / fabric is not aged on a bobbin, roller, core, beam or other carrier.

[0227] In some embodiments, the method for producing a polymer-aerogel / fiber composite or a polymer-aerogel / fabric composite includes a batch process that can be implemented on an industrial scale. In one non-limiting illustrative example, multiple spools of fiber or fabric can be infiltrated simultaneously with a polymer-aerogel-precursor solution. In some embodiments, the polymer-aerogel / fiber or polymer-aerogel / fabric production process is designed so that industrially available roll-to-roll processing equipment, or other industrially available batch or continuous processing equipment, can be used in the process.

[0228] In some embodiments, the temperature of the fiber or fabric, polymer-aerogel-precursor solution, and the surrounding atmosphere is controlled to a specific temperature. In certain embodiments, the temperature is 10°C to 15°C, 15°C to 20°C, 20°C to 25°C, 25°C to 30°C, or any suitable temperature. In some embodiments, the fiber or fabric is contacted with the polymer-aerogel-precursor solution for a fixed amount of time. In certain embodiments, the time is 0 seconds to 30 seconds, 0 seconds to 60 seconds, 0 seconds to 120 seconds, 0 seconds to 240 seconds, greater than 240 seconds, or any suitable time.

[0229] In some embodiments, the liquid in the pores of the polymer-gel / fiber composite is replaced with another solvent. Fig.17 In some embodiments, the liquid in the pores of the polymer-gel / fiber composite (20) is replaced with another solvent (19). In some embodiments, the liquid in the pores of the polymer-gel / fabric composite is replaced with another solvent. For example, in Fig.37 In the process, the liquid in the pores of the spool of the polymer-gel / fabric composite (29) is replaced with another solvent (19). Generally, the pore fluid refers to the liquid, vapor, gas, or fluid contained in the pores of the gel, and may include a solvent. In some embodiments, when the pore fluid in the polymer-gel / fiber composite or polymer-gel / fabric composite is replaced with a solvent, the pore fluid in the polymer-gel / fiber composite or polymer-gel / fabric composite already contains a solvent. In some embodiments, the solvent that replaces the original pore fluid is selected for its miscibility or partial miscibility with liquid carbon dioxide and / or supercritical carbon dioxide, so that the subsequent drying process can be carried out using supercritical carbon dioxide. In some embodiments, multiple solvent changes can be performed in a specific order.

[0230] In some embodiments, the pore fluid in the polymer-gel / fiber composite or polymer-gel / fabric composite can be replaced with a desired solvent (e.g., tert-butyl alcohol). In some embodiments, the solvent has a desired property relative to room temperature. Room temperature refers to a temperature in the range of 18°C ​​to 27°C. In certain embodiments, the following conditions may be advantageous: the solvent includes a solvent having a triple point near room temperature (e.g., -60°C to 60°C) and having a relatively high vapor pressure (e.g., greater than 0.01 Torr, greater than 0.1 Torr, greater than 1 Torr, greater than 10 Torr, greater than 20 Torr, greater than 30 Torr, greater than 40 Torr, greater than 50 Torr, greater than 60 Torr, greater than 70 Torr, greater than 80 Torr, greater than 90 Torr, or greater than 100 Torr) under ambient conditions. Environmental conditions may include ambient pressure conditions and ambient temperature conditions, such as a temperature close to room temperature, such as 0°C to 50°C. In some embodiments, the bulk form of the solvent has a freezing point below room temperature or close to room temperature (e.g., 25°C, 10°C to 35°C, 0°C to 50°C) under ambient pressure conditions. In certain embodiments, it may be advantageous for the solvent to undergo a low density change upon solidification. In certain embodiments, the solvent undergoes a density change of less than 3×10 -4 g / cc, less than 4×10 -4 g / cc, less than 8×10 -4 g / cc, less than 1×10 -3 g / cc, or less than 2×10 -3 In some embodiments, the polymer-gel / fiber composite material or polymer-gel / fabric composite material is soaked in a part of the excess solvent volume of the expectation, the pore fluid in the polymer-gel / fiber composite material or polymer-gel / fabric composite material is mixed with the solvent, the concentration of the material in the resulting mixture reaches an approximate balance, a new excess solvent of another part is provided, and the process is repeated until the excess solvent of the desired amount has been used. In some embodiments, the pore fluid in the polymer-gel / fiber composite material or polymer-gel / fabric composite material is replaced with an excess solvent equivalent to at least about 2 times, at least about 5 times, at least about 10 times, at least about 20 times, at least about 50 times, at least about 100 times or less than about 2 times the volume of the gel. However, in certain embodiments, the volume of the excess solvent is suitable enough to replace the purity of the solvent in the pores of the polymer-gel / fiber composite material or polymer-gel / fabric composite material by diffusion replacement to reach the level of minimizing the shrinkage of the gel produced by the subsequent freeze drying process. In some of these embodiments, the volume of the excess solvent is at least about 20 times, or at least about 50 times, the volume of the polymer-gel / fiber composite or polymer-gel / fabric composite.

[0231] Any suitable solvent can be used to replace the pore fluid. In some embodiments, the pore fluid in the polymer-gel / fiber composite or polymer-gel / fabric composite is replaced with alcohol. In some embodiments, the pore fluid in the polymer-gel / fiber composite or polymer-gel / fabric composite is replaced with methanol, ethanol, isopropanol, n-propanol, n-butanol, sec-butanol, tert-butanol, amyl alcohol, 2-methoxyethanol, amyl alcohol, and / or cyclohexanol. In some embodiments, the pore fluid in the polymer-gel / fiber composite or polymer-gel / fabric composite is replaced with C1 to C6 alcohol. In some embodiments, alcohol meets the purity specification of ACS reagent grade. In some of these embodiments, only one alcohol is used. In some embodiments, the pore fluid in the polymer-gel / fiber composite or polymer-gel / fabric composite is replaced with other suitable solvents / materials, such as acetone, acetonitrile, water, cyclohexanone, dimethyl sulfoxide, N-methylpyrrolidone, N, N'-dimethylformamide, dimethylacetamide, and / or carbon dioxide, etc. In some embodiments, the solvent meets the purity specifications of the American Chemical Society reagent grade purity. In some embodiments, only one solvent is used. In some embodiments, the pore fluid in the polymer-gel / fiber composite or polymer-gel / fabric composite is replaced with water. In some embodiments, the water is deionized and / or distilled. In some embodiments, the water meets the purity specifications of analytical reagent grade. In some embodiments, the pore fluid in the polymer-gel / fiber composite or polymer-gel / fabric composite is replaced with liquid carbon dioxide. In some embodiments, the carbon dioxide is industrial grade. In some embodiments, the carbon dioxide is ultra-high purity grade.

[0232] In some embodiments, the purity of the pore fluid in the polymer-gel / fiber composite or polymer-gel / fabric composite after solvent exchange is within 2 v / v %, within 1 v / v %, within 0.1 v / v %, within 0.5 v / v %, within 0.01 v / v %, within 0.005 v / v %, within 0.001 v / v % of the purity of the solvent used for solvent exchange before contact with the gel. Purity values ​​for the pore fluid in the polymer-gel / fiber composite or polymer-gel / fabric composite after solvent exchange outside of these ranges are also possible.

[0233] In some embodiments, solvent replacement can be performed by immersing a spool of polymer-gel / fiber composite or polymer-gel / fabric composite in a solvent bath for a certain amount of time. In certain embodiments, a continuous process is used to replace the liquid in the pores of the polymer-gel / fiber composite with another solvent. For example, Fig.18As shown, the polymer-gel / fabric composite (20) moves on a roller (13) and through a solvent bath (19) in a continuous process. In certain embodiments, the liquid in the pores of the polymer-gel / fiber composite is replaced with another solvent in a roll-to-roll manner. For example, Fig.19 As shown, the polymer-gel / fiber composite (20) moves from a conveying roll or spool (14) through a solvent bath (19) to a receiving roll or spool (15) in a roll-to-roll process. In certain embodiments, a continuous process is used to replace the liquid in the pores of the polymer-gel / fabric composite with another solvent. For example, Fig.38 As shown, the polymer-gel / fabric composite (29) moves on rollers (13) and through a solvent bath (19) in a continuous process. In certain embodiments, the liquid in the pores of the polymer-gel / fabric composite is replaced with another solvent in a roll-to-roll manner. For example, Fig.39 As shown, the polymer-gel / fabric composite (29) moves from a conveying roller or spool (14) through a solvent bath (19) to a receiving roller or spool (15) in a roll-to-roll process. Without wishing to be bound by any particular theory, it is believed that by replacing the liquid in the pores of the polymer-gel / fiber composite or polymer-gel / fabric composite with another target solvent in a continuous manner, so that the polymer-gel / fiber composite or polymer-gel / fabric composite is exposed to the target solvent in a non-wound manner rather than on a spool, the amount of time required to complete the replacement can be reduced. In some embodiments, the time required for the solvent replacement is limited by the diffusion transmission of the target solvent into the polymer-gel / fiber composite or polymer-gel / fabric composite. It is believed that by completing the replacement step in a continuous manner, the characteristic diffusion length of the solvent through the unwound composite is reduced relative to the wound polymer-gel / fiber composite or polymer-gel / fabric composite, respectively, and thus the time required for the solvent replacement process can be reduced.

[0234] In some embodiments, the polymer-gel / fiber composite or polymer-gel / fabric composite is colored, dyed, and / or treated by chemical agents.

[0235] In certain embodiments, the polymer-aerogel / fiber composite or polymer-gel / fabric composite comprises fibers or fabrics, respectively, that are colored, dyed and / or treated with a chemical agent prior to infiltration with the polymer-aerogel-precursor solution.

[0236] In some embodiments, the polymer-gel / fiber composite is treated so that the liquid in the pores of the gel is removed, so that the structure of the solid phase of the gel remains substantially intact to produce a polymer-aerogel / fiber composite. Fig. 20As shown, the polymer-gel / fiber composite material (20) is treated by a drying chamber (21) for removing liquid from the pores of the composite material so that the structure of the solid phase of the gel is substantially intact to produce a polymer-aerogel / fiber composite material (3). In some embodiments, the polymer-gel / fabric composite material is treated so that the liquid in the pores of the gel is removed so that the structure of the solid phase of the gel is substantially intact to produce a polymer-aerogel / fabric composite material. For example, Fig.40 As shown, the polymer-gel / fabric composite (29) is processed through a drying chamber (21) for removing liquid from the pores of the composite so that the structure of the solid phase of the gel remains substantially intact to produce a polymer-aerogel / fabric composite (25). In some embodiments, the polymer-gel / fiber composite or polymer-gel / fabric composite is converted to a polymer-aerogel / fiber composite or polymer-aerogel / fabric composite, respectively, by heating the composite under pressure until the conditions exceed the critical point of the pore fluid so that the fluid in the pore is in a supercritical state. Once the pore fluid is in a supercritical state, it can be isothermally depressurized and removed from the composite as a gas, thereby avoiding the presence of a liquid-vapor interface within the composite and the destructive capillary stresses that come with it, and keeping the solid phase of the composite intact.

[0237] In some embodiments, evaporative drying can be used to dry the wet polymer-gel / fiber composite or polymer-gel / fabric composite. In some embodiments, the pore fluid exhibits a sufficiently low surface tension to prevent damage to the polymer-gel / fiber composite or polymer-gel / fabric composite, respectively, for example, less than 20 dynes / cm, less than 15 dynes / cm, less than 12 dynes / cm, less than 10 dynes / cm. In certain embodiments, the surface tension of the solvent is equal to or less than 20 dynes / cm, equal to or less than 15 dynes / cm, equal to or less than 12 dynes / cm, equal to or less than 10 dynes / cm. Combinations of these ranges are also possible (e.g., at least 5 and less than or equal to 25). Other ranges are also possible.

[0238] In some embodiments, the wet polymer-gel / fiber composite or polymer-gel / fabric composite can be dried by sublimation of the pore fluid rather than evaporation. The pore fluid can solidify and sublimate appropriately in the absence of capillary forces to produce a polymer-aerogel / fiber composite or a polymer-aerogel / fabric composite, respectively. That is, rather than removing the solvent by evaporation from the liquid state, the solvent is sublimated from the solid state (already solidified), thereby minimizing the capillary forces that might otherwise be caused by evaporation.

[0239] In some embodiments, the polymer-gel / fiber composite or polymer-gel / fabric composite is processed to produce a polymer-aerogel / fiber composite or a polymer-aerogel / fabric composite, respectively, while the composite is being wound on a spool, roller, or other carrier. In some embodiments, a polymer-gel / fiber composite is processed to produce a polymer-aerogel / fiber composite using a continuous process. For example, Fig.21 As shown, the polymer-gel / fiber composite (20) moves through a drying chamber (21) in a continuous process to produce a polymer-aerogel / fiber composite. In certain embodiments, the polymer-gel / fiber composite is processed in a roll-to-roll manner to produce a polymer-aerogel / fiber composite. For example, Fig. 22 As shown, the polymer-gel / fiber composite (20) moves from a conveying roll or spool (14) through a drying chamber (21) to a receiving roll or spool (15) in a roll-to-roll process to produce a polymer-aerogel / fiber composite (3). In some embodiments, the polymer-gel / fabric composite is processed using a continuous process to produce a polymer-aerogel / fabric composite. For example, Fig.41 As shown, the polymer-gel / fabric composite (29) moves through the drying chamber (21) in a continuous process to produce the polymer-aerogel / fabric composite (25). In certain embodiments, the polymer-gel / fabric composite is processed in a roll-to-roll manner to produce the polymer-aerogel / fabric composite. For example, Fig.42 As shown, the polymer-gel / fabric composite (29) moves from a conveying roller or spool (14) through a drying chamber (21) to a receiving roller or spool (15) in a roll-to-roll process to produce a polymer-aerogel / fabric composite (25). Without wishing to be bound by any particular theory, it is believed that by processing the polymer-gel / fiber composite or polymer-gel / fabric composite into a polymer-aerogel / fiber composite or polymer-aerogel / fabric composite, respectively, in a continuous manner, such that the composite is processed in a non-wound manner rather than on a spool, the amount of time required to complete the process can be reduced. In some embodiments, the time required to process the polymer-gel / fiber composite or polymer-gel / fabric composite into a polymer-aerogel / fiber composite or polymer-aerogel / fabric composite, respectively, is limited by the diffusion of solvent out of the polymer-gel / fiber composite or polymer-gel / fabric composite. It is believed that by completing this step in a continuous manner, the characteristic diffusion length of the solvent through the unwound composite is reduced relative to the wound polymer-gel / fiber composite or polymer-gel / fabric composite, respectively, and therefore the time required for the process can be reduced.

[0240] In some embodiments, the polymer-aerogel / fiber composite comprises multiple strands of fibers and is mechanically treated to separate the strands of the fiber composite from each other. Fig.23 As shown, a polymer-aerogel / fiber composite (3) comprising multiple strands of fibers is run under a sharp edge (22) to separate the strands of the fiber composite from each other. Fig.24 As shown, a polymer-aerogel / fiber composite (3) comprising multiple strands of fibers is run through a deformation device (23) to separate the strands of the fiber composite from each other. In some embodiments, prior to this deformation, the composite fibers may be Figure 2A After deformation, the composite fiber may be more similar to Figure 2B In some embodiments, the polymer-aerogel / fabric composite is mechanically treated or finished to separate the fibers in the fabric composite from each other. For example, Fig.43As shown, the polymer-aerogel / fabric composite (25) is run through a finishing device (30) to mechanically separate the fibers of the fabric composite from each other and remove excess aerogel from the composite. In some embodiments, the mechanical treatment can be performed by blowing air at a specific speed through the polymer-aerogel / fiber composite or polymer-aerogel / fabric composite as the polymer-aerogel / fiber composite or polymer-aerogel / fabric composite runs from one roller to another. In some embodiments, the mechanical treatment is performed by running the polymer-aerogel / fiber composite or polymer-aerogel / fabric composite over a series of rollers, between a series of rollers, and / or around a series of rollers to apply an appropriate amount of friction and agitation. In some embodiments, the polymer-aerogel / fiber composite is mechanically treated using a false twisting device including, for example, a series of disks or belts that impart twisting friction on the fibers as the fibers run through the device. In some embodiments, the mechanical treatment is performed by running the polymer-aerogel / fiber composite or polymer-aerogel / fabric composite on a blade or a series of blades having an edge radius of less than about 0.5 mm. In some embodiments, any combination of these mechanical treatment methods can be used. Without wishing to be bound by any particular theory, it is believed that the mechanical treatment of polymer-aerogel / fiber composites makes it easier to introduce composites into fabrics using standard industrial manufacturing equipment. In an illustrative embodiment, a polymer-aerogel / fiber composite comprising multiple strands of fibers is selected for mechanical treatment, wherein the constituent fiber strands are substantially combined with other strands in the fiber composite by the aerogel present in the interstitial space within the fiber. After the fiber composite is mechanically treated, the individual strands in the composite are no longer combined together by the aerogel. In an illustrative embodiment, a polymer-aerogel / fiber composite comprising multiple strands of fibers is selected for knitting on a commercial circular knitting machine. Prior to mechanical treatment, when the fiber composite is knitted with the machine, the fiber composite is prone to frequent breaks. Relative to the same fiber composite that has not been mechanically treated, after mechanical treatment, when on the same circular knitting machine, the fiber composite has a lower frequency of breakage.

[0241] The preparation of polymer-aerogel / fiber or polymer-aerogel / fabric composites can involve processes that affect the interfacial strength of the bond between the polymer gel and the fiber. In some embodiments, such a process can be performed before, during and / or after the gelation of the polymer-aerogel-precursor solution occurs. In certain embodiments, the resulting produced polymer-aerogel / fiber or polymer-aerogel / fabric composite can exhibit a stronger bond between the polymer aerogel and the fiber relative to a similar polymer-aerogel / fiber or polymer-aerogel / fabric composite that does not incorporate such a processing step. In some embodiments, the fiber or fabric is contacted with a polymer-aerogel-precursor solution, an interfacial bond is formed between the components of the polymer-aerogel-precursor solution and the fiber or fabric, and then the polymer-aerogel-precursor solution is gelled to form a polymer-gel / fiber or polymer-gel / fabric composite in which the polymer gel is mechanically bonded to the fiber or fabric, respectively. In some embodiments, the fiber or fabric is contacted with a polymer-aerogel-precursor solution, a chemical reaction occurs between the components of the polymer-aerogel-precursor solution and the fiber or fabric, and then the polymer-aerogel-precursor solution is gelled to form a polymer-gel / fiber or polymer-gel / fabric composite material in which the polymer-gel is chemically bonded to the fiber or fabric. In some embodiments, this chemical reaction is spontaneous. In some embodiments, this chemical reaction is initiated by exposure to one or more of heat, light, ultraviolet radiation, infrared radiation, microwave radiation, other electromagnetic radiation, chemical catalysts, and / or free radical polymerization. In certain embodiments, the chemical reaction that causes the polymer gel to be bonded to the fiber or fabric can be performed after the gelation of the polymer-aerogel-precursor solution. In certain embodiments, this chemical bonding between the polymer gel and the fiber or fabric after gelation can be spontaneous or initiated, and can occur during the gel aging step and / or during the solvent replacement step after the gel has been formed. In some embodiments, the chemical bond between the polymer aerogel and the fiber or fabric in the polymer-aerogel / fiber or polymer-aerogel / fabric composite is formed after the composite is dried to form the polymer aerogel. In certain embodiments, the bonding process described herein can be performed on a spool of fiber or fabric. In some embodiments, the bonding process described herein can be performed on an unwound fiber or fabric.

[0242] In certain embodiments, the polymer-aerogel / fiber or polymer-aerogel / fabric composite can be coated with any common water repellent finish. In some embodiments, the finish comprises a fluoroalkyl acrylate copolymer. In some embodiments, the finish comprises a commercially available finish such as, but not limited to, DAN New liquid, N92111 liquid, N1811 liquid, Hydro AM Liquid, N2114 liquid, N9334 liquid, UD liquid, or any combination thereof. In some embodiments, the finishing agent is diluted with water or another acceptable solvent or dispersant to be applied to polymer-aerogel / fiber or polymer-aerogel / fabric composite material. In some embodiments, the finishing agent can be applied by typical fiber or fabric finishing methods such as but not limited to spraying, foaming, bathing, padding, and / or direct roller coating. Those of ordinary skill in the art are familiar with these methods for applying finishing agents to fibers or fabrics. In some embodiments, the water-repellent finishing agent can be applied by running the polymer-aerogel / fiber or polymer-aerogel / fabric composite material through a dilute solution of the finishing agent. In some embodiments, the water-repellent finishing agent can be applied by immersing the bobbin of the polymer-aerogel / fiber or polymer-aerogel / fabric composite material or any other carrier in a dilute solution of the finishing agent for a specified amount of time. In some embodiments, the water-repellent finishing agent can be dried and cured on the polymer-aerogel / fiber or polymer-aerogel / fabric composite material at ambient temperature and pressure. In some embodiments, the water repellent finish may be dried and cured on the polymer-aerogel / fiber or polymer-aerogel / fabric composite by baking the spool or other carrier in an oven at a specific temperature for a specific amount of time.

[0243] In certain embodiments, certain processing steps are selected to be compatible with implementation on an industrial production scale. That is, the processes are compatible with equipment and processing methods currently used in the fiber processing and fabric manufacturing fields.

[0244] In some embodiments, polymer-aerogel / fiber composites are woven or knitted into fabrics. In certain embodiments, polymer-aerogel / fiber composites are chopped and integrated into nonwoven fabrics. In some embodiments, polymer-aerogel / fiber composites are chopped to form staple fibers. In some embodiments, polymer-aerogel / fiber composite staple fibers can be woven to produce knittable fibers. In some embodiments, polymer-aerogel / fiber staple fibers can be woven together with other staple fiber types (including but not limited to cotton or polyester) to produce knittable fibers.

[0245] In some embodiments, the polymer-aerogel / fiber composite is mechanically bonded to another fiber or fibers using methods that may include, but are not limited to, twisting, wrapping, core spinning, or blending in any other manner. In some embodiments, the mechanically bonded polymer-aerogel / fiber / fiber composite can be woven or knitted into a fabric.

[0246] In some embodiments, the polymer-aerogel / fabric composite material can be dewoven to form a false knit. Fig.28 In the embodiment of the present invention, the polymer-aerogel / fabric composite material (25) is dewoven and dewoven into its constituent fibers or fibers using a commercial dewoven texturing machine (36) to form a polymer-aerogel / fiber composite material (3). One of ordinary skill in the art is familiar with dewoven to dewoven texturing, which includes reducing a knitted fabric to its fiber form. In some embodiments, the polymer-aerogel / fabric composite material can be prepared by the method described herein and then dewoven and dewoven to form a polymer-aerogel / fiber composite material.

[0247] In some embodiments, polymer-aerogel / fiber composites can be woven, knitted or otherwise incorporated into fabrics. In some embodiments, fabrics comprising polymer-aerogel / fiber composites can also include another fiber or multiple fibers. In some embodiments, composite fibers as described herein account for at least 1 wt %, at least 5 wt %, at least 10 wt %, at least 15 wt %, at least 20 wt %, at least 25 wt %, at least 35 wt %, at least 50 wt %, at least 75 wt %, at least 90 wt % or more, or 100% of the fabric.

[0248] In some embodiments, polymer-aerogel / fiber or polymer-aerogel / fabric composites can be used for fabric materials (including woven, knitted and nonwoven fabric materials). In some embodiments, these fabrics can be integrated into clothing and apparel (including but not limited to shirts, pants, shorts, tights, hats and socks), outerwear (including but not limited to coats, pants, wetsuits and gloves), blankets, footwear, outdoor protective textiles (including but not limited to modular sleeping systems, tents, backpacks, and sleeping bags) and temporary modular rigid wall structures.

[0249] In certain embodiments, polymer-aerogel / fiber or polymer-aerogel / fabric composites can be used in fabric materials (including woven, knitted and nonwoven fabric materials) that are integrated into: aviation interiors (including but not limited to seats, seat coverings, pads, cables, wall panels, floors, and kitchen appliances); aerospace applications (including but not limited to space suits, satellites, antennas, radar stealth, heat shielding, stealth shielding, temporary or permanent shelter structures and thermal protection systems); automotive applications (including but not limited to seats, seat coverings, seat cushions, engine compartments, refrigeration, exhaust system insulation, heat shields, sound insulation, thermal insulation, and interior decoration); exterior and interior of construction, architecture, and non-temporary buildings (including but not limited to wall systems, carpets, interior decoration, furniture); thermal protection systems for commercial refrigerated truck shipping packaging for perishable goods and pharmaceuticals; and thermal management packaging for express delivery services.

[0250] Clothing and similar textiles are one application where the unique combination and extreme values ​​of material properties provided by aerogels may be particularly advantageous. For example, outdoor clothing generally requires multiple layers of specific functions (e.g., outer layers for water repellency) to achieve the desired performance characteristics. Outdoor clothing products generally include fabric layers or fluffy wadding specifically designed to provide protection to the wearer from external cold or heat. For example, in a winter jacket, an insulating layer can be layered between other specific functional layers to provide warmth retention, but such an insulating layer generally increases volume, weight, design complexity, and production costs. In some applications, the increased volume and weight due to the increased insulating layer hinder the use of the product in many environments and for many people. However, aerogels can be used to manufacture such fabric materials, which can be simultaneously and inherently lightweight, flexible, waterproof, and most importantly highly insulating at low thickness, which can be used to provide protection to the wearer from cold, rain, and wind without restricting movement or adding significant weight. Therefore, it is necessary to develop inherently insulating fabric materials containing aerogels.

[0251] Historically, aerogel materials have exhibited several disadvantages that have hindered or complicated their integration into fabric-based applications such as clothing and textiles. These disadvantages are poor mechanical properties, such as low compressive strength, low compressive stiffness, and poor fracture toughness; easy damage during washing and thus loss of thermal insulation properties; and difficulty in integration into fiber-based substrates. For example, fiber-reinforced silica aerogel composite blankets in which fluffy fiber batts (such as glass fiber mats) are infiltrated with aerogels, or in which discrete aerogel particles are glued together with bicomponent polymer fibers to form a bonded flexible substrate, have been commercially available for several years and provide the thermal insulation benefits of aerogels in a flexible and rollable form factor suitable for industrial and building insulation applications. However, such blankets are prone to shedding aerogel dust particles, losing aerogels when handled or bent, and / or being damaged during washing and thus losing insulation capabilities, and need to be integrated with additional fabrics and packaging materials to be made suitable for clothing and related textiles.

[0252] In addition, conventional fabrics cannot match the insulating capabilities of aerogels. Today's insulating clothing relies on including a dedicated fluffy insulating layer, which is usually constructed in the clothing or combined with other functional layers required for clothing durability and stability, environmental contact (e.g., moisture resistance), and wearer comfort. The need for multiple special-function materials to achieve the functionality required for insulating clothing increases the volume and weight of the clothing. In addition, many traditional insulating materials (e.g., natural or synthetic down) rely on their fluffiness to provide insulating benefits. The insulating capabilities of these materials are significantly reduced when compressed or wetted, destroying the intended function of the clothing in many situations where clothing will be relied upon (e.g., in snow or rain and during outdoor sports activities). In addition, for certain clothing articles, such as socks or gloves, where the space for incorporating a fluffy insulating layer is limited or a high degree of flexibility is required, current insulation technology does not reach the functionality required by the wearer.

[0253] Aerogels are various types of low-density solid materials that contain porous three-dimensional nanostructured networks. Many aerogels exhibit a variety of desirable and extreme material properties, such as high specific surface area, low bulk density, high specific strength and stiffness, low thermal conductivity, and low dielectric constant.

[0254] Aerogels can be made from a variety of materials such as inorganic oxides, organic polymers, carbon, and many other materials, and can accordingly have the properties of specific materials, such as high temperature stability, hydrophobicity, chemical resistance, and flexibility. Certain aerogel compositions combine multiple desired material properties into a single material encapsulation, and can therefore be beneficial for technical applications such as thermal insulation, sound insulation, lightweight structures, impact damping, electrodes, catalysts and catalyst supports, and sensors. Aerogel materials can also be produced in a variety of form factors to facilitate incorporation into different applications, such as integrally formed parts, fine particles, fiber-reinforced composite blankets, films, and coatings.

[0255] Aerogels include a solid component and a tortuous network of open pores, although in some cases may include pores as large as several microns and / or less than 2nm, but the average pore size is generally on the order of 2nm to 50nm. The pores of aerogels that may be smaller than the mean free path of air molecules at standard temperature and pressure can produce a phenomenon known as the Knudsen effect, in which convective heat transfer through the material is significantly suppressed. The solid component of the corresponding aerogel includes a highly disordered, sparsely connected, usually nanostructured, fractal-shaped continuous solid phase network. Therefore, aerogels exhibit low bulk density, ranging from <1mg / cc to 0.9g / cc, with typical values ​​of 0.05g / cc to 0.3g / cc for most materials. Low bulk density and sparsely connected solid phase networks in turn lead to inefficient conduction transmission of heat through the material. The combination of inefficient convection and conduction transmission of heat through the material makes aerogels an excellent thermal insulator, in some cases, as low as 10mW / mK at temperatures and pressures close to standard temperature and pressure (STP). STP is defined and understood as a temperature of 273.15 K and an absolute pressure of 100 kPa. For example, a silica aerogel with a bulk density of about 0.11 g / cc routinely exhibits a thermal conductivity of 14 mW / mK. Polymer aerogels can similarly exhibit low thermal conductivity, but in some cases, such as polymer aerogels that exhibit a high compression modulus, the thermal conductivity can be as high as 80 mW / mK because of increased conductive transport of heat due to increased phonon transport in the aerogel solid phase skeleton.

[0256] In certain embodiments, aerogels can be dry, nanoporous, nanostructured materials that exhibit a variety of extreme and valuable material properties, such as low density, ultra-low thermal conductivity, high density normalized strength and stiffness, and high specific internal surface area, etc. Nanoporous refers to porous materials in which the pores are predominantly nanoporous, i.e., porous materials in which at least 50% of the pores comprise an average pore size exhibiting less than 1 micrometer as determined by the Barrett-Joyner-Halena model of the nitrogen adsorption isotherm of the material.

[0257] In some embodiments, the aerogel is a polymer aerogel. In certain embodiments, the solid skeleton of the aerogel comprises greater than 10%, greater than 20%, greater than 30%, greater than 50%, greater than 80%, greater than 90%, greater than 95%, or greater than 98% polymer by mass.

[0258] Polymer-aerogel / aerogel composites can also be prepared in which particles of one aerogel material are dispersed throughout the polymer aerogel. The aerogel particles can include hydrophobic and / or hydrophilic particles. For example, a composite material in which hydrophobic silica aerogel particles having a diameter ranging from 1 μm to 1000 μm are dispersed throughout the polymer aerogel. In certain embodiments, the aerogel particles can include trimethylsilyl-functionalized silica aerogels, wherein the silica aerogel can contain sodium ions. In certain embodiments, the mass percentage of the dispersant aerogel material, such as silica aerogel particles, relative to the mass of the host aerogel, such as a polymer aerogel, is less than 55%, less than 50%, less than 40%, less than 30%, less than 20%, less than 10%, less than 5%, less than 2%, or less than 1%.

[0259] As provided herein, in some embodiments, polymer aerogel materials can include solid phase polymer-containing materials that are primarily mesoporous (i.e., comprising pores with diameters between 2 nm and 50 nm), the solid phase polymer-containing materials comprising at least 50% by volume pores, wherein the solid phase component comprises a solid network of 3D nanostructures. In some embodiments, the aerogel can include pores with diameters as large as several microns, and / or pores with diameters less than 2 nm.

[0260] Polymer aerogels can be prepared in a variety of form factors. Form factor refers to the general shape and form that the aerogel exhibits. Examples of common form factors for aerogels include monoliths, particles, films, and composite blankets. Monoliths refer to shaped continuous macroscopic components that exhibit a minimum dimension of at least 1 mm. For example, the term monolith does not refer to microscopic domains within an aerogel material or a single network within an interpenetrating network aerogel. Particles refer to small discrete pieces of aerogel materials of irregular or regular shape, with typical sizes ranging from 1 μm to 1 mm. For example, when used to refer to a form factor, the term particle does not refer to the component particles that make up the solid skeleton of the aerogel, such as nanoparticles or microparticles that are connected together to form the aerogel material.

[0261] In some embodiments, polymer aerogel can show one or more morphologies. As presented herein, morphology refers to the geometric arrangement of the solid and pores (i.e., holes) constituting aerogel materials. In some embodiments, polymer aerogel materials can show pearl string morphology, wherein the solid skeleton of aerogel comprises interconnected spherical substructures such as nanoparticles. In some embodiments, such nanoparticles are porous themselves, showing holes with a diameter of <2nm, referred to as secondary particles, which in turn comprise smaller primary particles. In some embodiments, polymer aerogel materials can show fibrous or fibrous morphology, wherein the solid skeleton of aerogel comprises high aspect ratio substructures and / or presents a reticular appearance. These fibrous substructures are essentially different from those used in long fibers and microfibers, such as for clothing or fluffy wadding. Therefore, polymer-aerogel / fiber composites provided herein can include polymer aerogel materials with fibrous substructures, and non-aerogel fiber materials compounded with aerogel materials on microscopic and / or macroscopic length scales. The fibrous substructures or fibrous particles constituting the polymer aerogel material of the described morphology are distinct from foreign microfibers or long fibers which are used, for example, to provide mechanical reinforcement of the aerogel material or as a substrate for making textiles but which are impregnated with the aerogel material.

[0262] The polymer aerogel may exhibit any suitable morphology. In some embodiments, the morphology of the polymer aerogel may be fibrous, meaning that the solid skeleton of the polymer aerogel comprises a substructure that is linear in nature and has an aspect ratio greater than or equal to 10:1, i.e., a substructure that visually resembles a fiber when viewed using a scanning electron microscope (SEM). In some embodiments, the solid skeleton of the polymer aerogel comprises secondary particles that are composed of smaller primary particles.

[0263] The polymer aerogel (e.g., in a composite fiber and / or a composite fabric) can exhibit any suitable pore structure. The pore width distribution, pore area distribution, and average pore size can be calculated from a nitrogen desorption isotherm using the Barrett-Joyner-Halenda (BJH) method within the range typically used to measure pore width and pore area distribution. The average pore width, such as the average pore size (assuming cylindrical pores), can be calculated using pore width = 4*(total specific volume) / (specific surface area), where the total specific volume and specific surface area can also be calculated using the BJH analysis of the desorption isotherm. In some embodiments, the average pore width is less than 10 nm, less than 20 nm, less than 30 nm, less than 40 nm, less than 50 nm, less than 60 nm, less than 70 nm, less than 80 nm, less than 90 nm, less than 100 nm, less than 500 nm, less than 1 μm, less than 10 μm, less than 100 μm, or less than 1 mm. In certain preferred embodiments, the average pore width is less than 50 nm. In some embodiments, the pore width distribution of the aerogel can be unimodal (i.e., exhibiting a single maximum). In some embodiments, the pore width distribution maximum occurs at less than 10 nm, less than 20 nm, less than 30 nm, less than 40 nm, less than 50 nm, less than 60 nm, less than 70 nm, less than 80 nm, less than 90 nm, less than 100 nm, less than 500 nm, less than 1 μm, less than 10 μm, less than 100 μm, or less than 1 mm.

[0264] In some embodiments, the pore width distribution of the aerogel can be bimodal, or at least bimodal. In some embodiments, the aerogel material can have two different pore populations, one having an average pore size less than a certain critical pore width, and one having an average pore size greater than a certain critical pore width. In some embodiments, the critical pore width is less than 10nm, less than 20nm, less than 30nm, less than 40nm, less than 50nm, less than 60nm, less than 70nm, less than 80nm, less than 90nm, less than 100nm, less than 500nm, less than 1μm, less than 10μm, less than 100μm, or less than 1mm. In some embodiments, the aerogel can exhibit any suitable internal surface area. In some embodiments, the internal surface area of ​​the aerogel is greater than 50m 2 / g, greater than 100m 2 / g, greater than 200m 2 / g, more than 300m 2 / g, more than 400m 2 / g, more than 500m 2 / g, more than 600m 2 / g, more than 700m 2 / g, more than 800m 2 / g, greater than 1000m 2 / g, greater than 2000m 2 / g, more than 3000m 2 / g, less than 4000m 2 / g. In certain preferred embodiments, the internal surface area of ​​the aerogel is 50m 2 / g to 800m 2 / g. Aerogel internal surface area values ​​outside these ranges may be possible.

[0265] In some embodiments, aerogels have a bulk density proportional to the bulk density of their gel precursors. For example, a gel whose aerogel has 95% porosity will have a density equal to the sum of 95% of the solvent density and 5% of the skeleton density, while a gel whose aerogel has 99% porosity will have a density equal to the sum of 99% of the solvent density and 1% of the skeleton density. In some embodiments, if the gel precursor of the aerogel material has a suitable bulk density so that evaporation and drying of the gel precursor can produce a single aerogel, the bulk density of the aerogel material can be used as a meaningful indicator. In some embodiments, the bulk density of the material can be determined by dimensional analysis. For example, the bulk density can be measured by first carefully processing the sample into a regular shape such as a block or a rod. Length, width and thickness (or length and diameter) can be measured using digital calipers (accuracy ±0.001"). These measurements can then be used to calculate the sample volume by multiplying length*width*height (in the case of a block) or length*radius squared*π (in the case of a disk). Mass can be measured using a digital analytical balance with an accuracy of 0.001g. Bulk density can then be calculated as density = mass / volume.

[0266] In some embodiments, the bulk density of the aerogel can be 0.05 g / cc to 0.1 g / cc, 0.05 g / cc to 0.2 g / cc, 0.05 g / cc to 0.3 g / cc, 0.05 g / cc to 0.4 g / cc, 0.05 g / cc to 0.5 g / cc, 0.05 g / cc to 0.6 g / cc, 0.05 g / cc to 0.7 g / cc, or greater than 0.7 g / cc. In certain embodiments, the density can be 0.15 g / cc to 0.7 g / cc.

[0267] In some embodiments, aerogels can exhibit any suitable skeletal density. Skeletal density refers to the density of the solid components of the aerogel (which does not include the volume of the pores), rather than the bulk density of the aerogel (which includes the volume of its pores). Skeletal density can be measured by measuring the skeletal volume of a sample using a pycnometer (e.g., Micromeritics AccuPyc II 1340 gas pycnometer) using helium as the working gas. Prior to measurement, the sample can be dried under a nitrogen or helium flow to remove moisture or other solvents from the pores of the aerogel. Skeletal volume measurements can be performed by averaging 100 measurements. Mass can be measured using a digital analytical balance with an accuracy of 0.001g. Skeletal density can be calculated as skeletal density=mass / skeletal volume. In some embodiments, the aerogel has a skeletal density of 1 g / cc to 1.1 g / cc, 1 g / cc to 1.2 g / cc, 1 g / cc to 1.3 g / cc, 1 g / cc to 1.4 g / cc, 1 g / cc to 1.5 g / cc, 1 g / cc to 1.6 g / cc, 1 g / cc to 1.7 g / cc, 1 g / cc to 1.8 g / cc, 1 g / cc to 1.9 g / cc, 1.1 g / cc to 1.3 g / cc, 1.1 g / cc to 1.4 g / cc, 1.8 g / cc to 2.1 g / cc, 1.8 g / cc to 2.2 g / cc, 3 g / cc to 4 g / cc, or 4 g / cc to 5 g / cc.

[0268] In some embodiments, the aerogel can exhibit any suitable thermal conductivity. In certain embodiments, the thermal conductivity of the resulting aerogel is less than 60 mW / mK, less than 50 mW / mK, less than 40 mW / mK, less than 30 mW / mK, less than 20 mW / mK, 15 mW / mK to 20 mW / mK, 15 mW / mK to 30 mW / mK, or 15 mW / mK to 40 mW / mK.

[0269] Thermal conductivity can also be measured as described using the method outlined in ASTM C518-17 "Standard Test Method for Steady-State Thermal Transmission Properties by Means of the Heat Flow Meter Apparatus".

[0270] In some embodiments, the aerogel can be subjected to a uniaxial load while measuring thermal conductivity. In some embodiments, a load can be applied to the cold side of the thermal conductivity measurement device in the direction of the hot side of the device. In some embodiments, the load applied to the aerogel is less than 0.5 kPa, less than 1 kPa, less than 2 kPa, less than 5 kPa, less than 10 kPa, less than 20 kPa, less than 40 kPa, less than 60 kPa, less than 80 kPa, or less than 100 kPa. In some embodiments, the thermal conductivity measured under load increases by less than 50%, less than 40%, less than 30%, less than 20%, less than 10%, less than 5%, or less than 1% relative to the thermal conductivity measured without the application of the load.

[0271] In some embodiments, the aerogel material has a compression modulus (also known as Young's modulus, which in some embodiments is approximately equal to the bulk modulus) and a yield strength, which can be determined using a standard uniaxial compression test. The compression modulus and yield strength can be measured as written using the method outlined in ASTM D1621-10 "Standard Test Method for Compressive Properties of Rigid Cellular Plastics", except that the specimen is compressed at a crosshead displacement rate of 1.3 mm / second (as specified in ASTM D695) instead of 2.5 mm / second.

[0272] In some embodiments, the aerogel can exhibit any suitable compression modulus. In certain embodiments, the compression modulus of the aerogel is greater than 100 kPa, greater than 500 kPa, greater than 1 MPa, greater than 10 MPa, greater than 50 MPa, greater than 100 MPa; or less than 100 MPa, less than 50 MPa, less than 10 MPa, less than 1 MPa, less than 500 kPa, less than 100 kPa, or less than 50 kPa. Combinations of the above ranges or values ​​outside of these ranges are possible for the compression modulus of the aerogel.

[0273] In some embodiments, the aerogel can exhibit any suitable compressive yield strength. In certain embodiments, the compressive yield strength of the aerogel is greater than 40 kPa, greater than 100 kPa, greater than 500 kPa, greater than 1 MPa, greater than 5 MPa, greater than 10 MPa, greater than 50 MPa, greater than 100 MPa, greater than 500 MPa; or less than 500 MPa, less than 100 MPa, less than 50 MPa, less than 10 MPa, less than 5 MPa, less than 1 MPa, less than 500 kPa, less than 100 kPa, or less than 50 kPa. Combinations of the above ranges or values ​​outside of these ranges are possible for the compressive yield strength of the aerogel.

[0274] In some embodiments, the aerogel can exhibit any suitable compressive ultimate strength. In certain embodiments, the compressive ultimate strength of the aerogel is greater than 1 MPa, greater than 10 MPa, greater than 50 MPa, greater than 100 MPa, greater than 500 MPa, greater than 1000 MPa; or less than 1000 MPa, less than 500 MPa, less than 100 MPa, less than 50 MPa, less than 10 MPa, less than 50 MPa, less than 10 MPa, less than 5 MPa, or less than 1 MPa. Combinations of the above ranges or values ​​outside these ranges are possible for the compressive ultimate strength of the aerogel.

[0275] In some embodiments, aerogels can exhibit any suitable elasticity. In some embodiments, aerogel materials that exhibit high elasticity can be produced. Elasticity can refer to the degree of strain that a material can withstand without maintaining permanent deformation (e.g., its elastic deformation state) relative to the unstrained state of the material. In some embodiments, materials that exhibit a high degree of elasticity, such as greater than 2%, greater than 5%, greater than 10%, greater than 20%, greater than 30%, greater than 40%, greater than 50%, greater than 60%, greater than 70%, greater than 80% or greater, can be produced. In some embodiments, materials that exhibit a high degree of elasticity and exhibit a bulk density of less than 0.05 g / cc or greater than 0.3 g / cc can be produced.

[0276] In some embodiments, aerogel can be able to show any suitable minimum radius of curvature without fracture.Minimum radius of curvature refers to the radius of the minimum cylinder around which material can be bent so that material is tangent to and contacts the surface in the entire bending area.In some embodiments, the minimum radius of curvature depends on the thickness of the material.In some embodiments, the radius of curvature of the aerogel with a thickness of 1 cm is less than 100 cm, less than 50 cm, less than 25 cm, less than 10 cm, less than 5 cm, less than 4 cm, less than 3 cm, less than 2 cm, less than 1 cm, less than 0.5 cm or less than 0.1 cm.In some embodiments, the radius of curvature of the aerogel with a thickness of 0.5 cm is less than 100 cm, less than 50 cm, less than 25 cm, less than 10 cm, less than 5 cm, less than 4 cm, less than 3 cm, less than 2 cm, less than 1 cm, less than 0.5 cm or less than 0.1 cm.

[0277] In some embodiments, aerogels can exhibit hydrophobicity. The hydrophobicity of aerogels can be expressed in terms of liquid water absorption as determined by the methods described herein. Aerogel materials with excellent or improved liquid water absorption are understood to have lower liquid water absorption relative to different aerogel materials. In some embodiments, liquid water absorption can be less than 100 wt %, less than 80 wt %, less than 70 wt %, less than 60 wt %, less than 50 wt %, less than 40 wt %, less than 30 wt %, less than 20 wt %, less than 10 wt %, less than 5 wt %, less than 4 wt %, less than 3 wt %, less than 2 wt %, less than 1 wt % or less than 0.1 wt % relative to the weight of the aerogel before contact with liquid water.

[0278] The hydrophobicity of the aerogel can be expressed in terms of water vapor absorption as determined by the methods described herein. In some embodiments, the water vapor absorption can be less than 100 wt%, less than 80 wt%, less than 70 wt%, less than 60 wt%, less than 50 wt%, less than 40 wt%, less than 30 wt%, less than 20 wt%, less than 10 wt%, less than 5 wt%, less than 4 wt%, less than 3 wt%, less than 2 wt%, less than 1 wt%, or less than 0.1 wt%, relative to the weight of the aerogel before exposure to water vapor.

[0279] The hydrophobicity of aerogel materials can be expressed by water contact angle. The term water contact angle refers to the equilibrium contact angle of a water droplet in contact with the surface of an aerogel material. The water contact angle can be determined by including but not limited to ASTM D7490 or any suitable standard method for measuring the water contact angle. Relative to different aerogel materials, aerogels with excellent or improved hydrophobicity can have a higher water contact angle. In some embodiments, the water contact angle can be greater than 80 °, greater than 90 °, greater than 100 °, greater than 110 °, greater than 120 °, greater than 130 °, greater than 140 °, greater than 150 °, greater than 160 °, greater than 170 ° or 170 ° to 180 °.

[0280] In some embodiments, aerogel has a maximum operating temperature. The maximum operating temperature of aerogel is the temperature at which the material undergoes harmful chemical changes, mechanical changes, phase changes, and / or density changes that cause the aerogel to lose mechanical integrity and / or most of its pores. In some embodiments, the maximum operating temperature is determined by placing the aerogel in an oven at a certain temperature under a suitable atmosphere, balancing the aerogel to the temperature of the oven, and observing whether the aerogel is broken into multiple pieces or densified to the extent that it loses most of its pores due to heating. Suitable atmospheres for determining the maximum operating temperature include those atmospheres in which the aerogel is expected to be operated. Suitable atmospheres for determining the maximum operating temperature may include air, nitrogen, argon, vacuum, or any other suitable atmosphere. In certain embodiments, the maximum operating temperature of aerogel is 100°C, 150°C, 200°C, 250°C, 300°C, 350°C, or any suitable temperature.

[0281] In some embodiments, when the aerogel is heated, the size of the aerogel may change. The article injected with aerogel exists in three-dimensional space and has three orthogonal dimensions of length, width and height. The term thickness can also refer to one of these dimensions, such as height. In certain embodiments, the size of the aerogel after being exposed to a temperature of 200°C falls within 2%, within 5%, within 10%, within 20%, or within 30% of the size of the aerogel before being exposed to the temperature. In certain embodiments, the size of the aerogel after being exposed to a temperature of 250°C falls within 2%, within 5%, within 10%, within 20%, or within 30% of the size of the aerogel before being exposed to the temperature. In certain embodiments, the size of the aerogel after being exposed to a temperature of 300°C falls within 2%, within 5%, within 10%, within 20%, or within 30% of the size of the aerogel before being exposed to the temperature. In certain embodiments, the size of the aerogel after exposure to a temperature of 350°C is within 2%, within 5%, within 10%, within 20%, or within 30% of the size of the aerogel prior to exposure to that temperature.

[0282] U.S. Provisional Patent Application No. 62 / 914,298, filed on October 11, 2019, and entitled “Polymer-Aerogel / Fiber and Polymer-Aerogel / Textile Composites, and Related Systems and Methods,” and U.S. Provisional Patent Application No. 62 / 914,354, filed on October 11, 2019, and entitled “Insulative Polyimide-Aerogel / FiberComposites for Apparel and Methods of Production,” are each incorporated herein by reference in their entirety for all purposes.

[0283] Example

[0284] The following examples are intended to illustrate certain embodiments of the invention, but are not intended to illustrate the full scope of the invention.

[0285] Example 1: Synthesis of polyimide-aerogel / PET-fiber composites by reaction of amine and anhydride to The process is applied to the fibers in a batch process and via supercritical CO 2 Extraction and drying to produce

[0286] A 38 g spool of 150 denier multi-strand PET (i.e., polyethylene terephthalate, i.e., polyester) fiber was prepared by running the fiber through a tension controller with a 6 g tension set point while the receiving spool of fiber was rotated at a rate of 2000 RPM and traversed linearly up and down over a 3 inch range at a rate of 60 inches / minute for a total of 45 complete traverses. The spool was then wrapped in a single layer of knitted PET fabric material.

[0287] The polyimide-aerogel-precursor solution is synthesized by the reaction of amine and anhydride. 2.12g of 2,2'-dimethylbenzidine is dissolved in 266.01g of N-methyl-2-pyrrolidone. The mixture is stirred until the 2,2'-dimethylbenzidine is completely dissolved (no particles are seen). After stirring for 10 minutes, 5.87g of 3,3',4,4'-biphenyltetracarboxylic acid dianhydride is added to the mixture and stirred for 10 minutes. After stirring for 10 minutes, 6.87g of 4,4'-[1,3-phenylenebis(1-methyl-ethylene)] dianiline is added to the mixture and stirred for 10 minutes. After stirring for 10 minutes, 5.87g of 3,3',4,4'-biphenyltetracarboxylic acid dianhydride is added to the mixture and stirred for 10 minutes. After stirring for 10 minutes, 1.80g of 4,4'-oxydiphenylamine is added to the mixture and stirred for 10 minutes. After 10 minutes, add a mixture of 0.45g Desmodur N3300A and 26.60g N-methyl-2-pyrrolidone to the first mixture and stir for 10 minutes. After stirring for 10 minutes, add 32.57g acetic anhydride and 8.07g triethylamine in rapid succession. The resulting sol is stirred for 2 minutes to 5 minutes until fully mixed, then poured into a container with the bobbin of the aforementioned fiber so that the bobbin of the fiber is completely immersed. The container is then closed and left for 20 minutes. After 20 minutes, take out the bobbin of the fiber infiltrated by polyimide-aerogel-precursor from the sol, place in an airtight container, and leave at room temperature for 24 hours, during which time the gelation of the polyimide-aerogel precursor solution occurs on the bobbin of the fiber and / or in the bobbin of the fiber to form a polyimide-gel / fiber composite.

[0288] After 24 hours, the spool of polyimide-gel / fiber composite was removed from the container and rewound onto another spool without controlling the tension or speed of winding. The new spool of polyimide-gel / fiber composite was then placed in a solvent exchange bath, i.e., a sealed container partially filled with about 1500 mL of acetone. It remained immersed in the acetone in the container for a total of 72 hours, during which the acetone was poured out and replaced twice with an equal volume of new acetone.

[0289] After the solvent change is complete, the spool of fiber is transferred to a pressure vessel and submerged in excess acetone. The pressure vessel is then sealed and liquid CO is introduced into the pressure vessel. 2 . Regularly discharge CO 2 -acetone mixture, while supplying fresh liquid CO 2 Until virtually all the acetone is removed. Then, while still filled with liquid CO 2 At the same time, the pressure vessel and CO 2The supply is disconnected. The pressure vessel is heated until the internal temperature reaches 54°C, during which time the pressure increases. The pressure is regulated by actuation of the solenoid valve and is not allowed to exceed 1400 psi. At this point, the CO inside the vessel 2 The pressure vessel was then cooled to room temperature before the spool of polyimide-aerogel / fiber composite was retrieved.

[0290] The resulting polyimide-aerogel / fiber composite was a pale yellow fiber with approximately 19% aerogel mass loading, 38 mW / mK thermal conductivity (when laid into a mat and measured by the Calibrated Hot Plate (CHP) method described herein), and 80 m 2 / g of BET surface area. Optical microscopy imaging shows that the polyimide aerogel is both on the outer surface of the fiber and within the pores of the multi-stranded fiber. Optical microscopy imaging also shows that a portion of the composite fiber has a substantially continuous polyimide aerogel along the length of the composite fiber, while other portions of the composite show that the polyimide aerogel is discontinuous.

[0291] Example 2: Knitted fabric formed from a polyimide-aerogel / PET-fiber composite material, wherein the polyimide- Aerogel / PET-fiber composites are obtained by reacting amines and anhydrides, applied to the fibers in a batch process, and subjected to supercritical drying. CO 2 Extraction and drying to produce

[0292] Spools of 150 denier multi-strand PET were prepared as described in Example 1. The polyimide-aerogel precursor solution was synthesized as described in Example 1. And spools of PET fiber followed the same processing steps as the spools described in Example 1 from exposing the spools to the polyimide-aerogel-precursor solution to drying.

[0293] The resulting polyimide-aerogel / fiber composite is then mechanically deformed using an air jet texturing machine to disperse the strands of the composite fibers and remove excess aerogel material. The resulting deformed polyimide-aerogel / fiber composite is then knitted into a fabric using a circular knitting machine.

[0294] The resulting fabric containing the deformed polyimide-aerogel / fiber composite material is a light yellow knitted fabric with a thickness of 11 m 2 / g, and a thermal conductivity of 48 mW / mK when measured by the calibrated hot plate (CHP) method described herein.

[0295] The resulting fabric containing the deformed polyimide-aerogel / fiber composite material was then washed according to the AATCC LP1 standard for home washing. The washed fabric containing the deformed polyimide-aerogel / fiber composite material was a light yellow knitted fabric with 8 m 2 / g, and a thermal conductivity of 49 mW / mK when measured by the calibrated hot plate (CHP) method described herein.

[0296] Example 3: Synthesis of polyimide-aerogel / nylon-fiber composites by reaction of amine and anhydride to The process is applied to the fibers in a batch process and via supercritical CO 2 Extraction and drying to produce

[0297] A 47g spool of 270 denier multi-strand nylon fiber was prepared by running the fiber through a commercial tension controller with a 6g tension set point while the receiving spool of fiber was rotated at 2000 RPM and traversed linearly up and down over a 3 inch range at a rate of 60 inches / minute for a total of 45 complete traverses. The spool was then wrapped in a single layer of knitted PET fabric material.

[0298] The polyimide-aerogel precursor solution was synthesized as described in Example 1. The spools of nylon fibers followed the same processing steps as the spools of PET fibers described in Example 1 from exposure of the spools to the polyimide-aerogel-precursor solution to drying.

[0299] The resulting polyimide-aerogel / fiber composite was a pale yellow fiber with an aerogel mass loading of approximately 12%, and a thermal conductivity of 44 mW / mK (when laid down into a mat and measured by the calibrated hot plate (CHP) method described herein).

[0300] Example 4: Synthesis of polyimide-aerogel / PET-fiber composites, which are prepared by reacting amines and anhydrides in the presence of silica The aerogel particles are reacted in the presence of additives, applied to the fibers in a roll-to-roll process, and reacted via supercritical CO 2 Extracted Drying to produce

[0301] The polyimide-aerogel-precursor solution was synthesized by adding acetic anhydride as described in Example 1. After the addition of acetic anhydride, 5.42 g of trimethylsilyl-functionalized silica aerogel particles containing sodium ions were added to the mixture, i.e. MT1200 silica aerogel particles and stirred until the particles were evenly dispersed (no particle clumps were visible). After the silica aerogel particles were dispersed, 8.07 g of triethylamine was added to the mixture and the resulting sol was stirred for 2 to 5 minutes until well mixed. The resulting sol was then poured into a container with a roller partially immersed in the sol.

[0302] 150 denier multi-strand PET fiber was fed onto a receiving bobbin under a partially submerged roller so that the fiber was exposed to and penetrated by the sol in a roll-to-roll manner without controlling the tension of the fiber or the winding speed of the receiving bobbin. About 10 g of the PET fiber passed through the sol and reached the receiving bobbin. The receiving bobbin was then placed in an airtight container and left at room temperature for 24 hours.

[0303] After 24 hours, the spool of polyimide-gel / fiber composite was removed from the container and rewound onto another spool without controlling the winding tension or speed. This new spool of polyimide-gel / fiber composite was processed by drying according to the procedure outlined in Example 1.

[0304] The obtained polyimide-aerogel / fiber composite was a light yellow fiber with about 18% aerogel mass loading, 59m 2 / g, and a thermal conductivity of 34 mW / mK when laid out into a mat and measured by the calibrated hot plate (CHP) method described herein.

[0305] The resulting polyimide-aerogel / fiber composite was then washed according to the AATCC LP1 standard for home washing.

[0306] The washed polyimide-aerogel / fiber composite material is a light yellow fiber with a thickness of 53 m 2 / g, and a thermal conductivity of 36 mW / mK when laid out into a mat and measured by the calibrated hot plate (CHP) method described herein.

[0307] Example 5: Synthesis of polyurea-aerogel / fiber composites by reaction of isocyanate with an in situ formed amine should be applied to the fibers in a batch process and via CO 2 Produced by atmospheric sublimation drying

[0308] A 40 g spool of 150 denier single strand PET fiber was prepared by running the fiber through a tension controller with a 6 g tension set point while the receiving spool of fiber was rotated at 2000 RPM and traversed linearly up and down over a 3 inch range at a rate of 60 inches / minute for a total of 45 complete traverses. The spool was then wrapped in a single layer of knitted PET fabric material.

[0309] The polyurea aerogel precursor is synthesized from isocyanate. 158.12g Desmodur N3300 (isocyanurate trimer of hexamethylene diisocyanate) is dissolved in 592.3g acetone and stirred until uniform (about 15 minutes). 11.14g deionized water is added to the mixture and stirred for 5 minutes. Finally, 0.762g triethylamine is added to the mixture and stirred for another 5 minutes. The resulting sol is then poured into a container with a bobbin of fiber as described above so that the bobbin of fiber is completely immersed. The container is then closed and allowed to stand for 30 minutes in a temperature-controlled environment set at 15°C. After 30 minutes, the bobbin of fiber infiltrated with polyurea-aerogel-precursor is taken out from the sol, placed in an airtight container, and placed in a temperature-controlled environment set at 15°C for 24 hours, during which time the gelation of the polyurea-aerogel precursor solution occurs on the bobbin of fiber and / or in the bobbin of fiber to form a polyurea-gel / fiber composite material.

[0310] After 24 hours, the spool of polyurea-gel / fiber composite was removed from the container and rewound onto another spool without controlling the tension or speed of the winding. This new spool of polyurea-gel / fiber composite was then placed in a solvent exchange bath. The volume of the solvent exchange bath was about 5 times the volume of the gel and was ACS reagent grade acetone. The acetone was replaced twice (once every 24 hours) with clean acetone.

[0311] After the solvent exchange was completed, the spool of polyurea-gel / fiber composite was transferred to a pressure vessel and immersed in excess acetone. The pressure vessel was then sealed and liquid CO was introduced into the pressure vessel. 2 . Regularly exhaust CO from the container 2 -acetone mixture, while supplying fresh liquid CO 2 Until virtually all the acetone is removed. Then, while still filled with CO 2 At the same time, the pressure vessel and CO 2 The pressure vessel is then rapidly vented, reducing the pressure to ambient over a period of about 30 seconds. In this process, excess CO 2 The liquid CO2 in the spool of polyurea-gel / fiber composite material is quickly discharged from the container. 2 Freezing, forming solid CO within the pores of the material 2 The container is then slowly heated at ambient pressure to allow the frozen CO 2 Sublimation was carried out from the frozen polyurea-gel / fiber composite until the internal temperature of the container reached 20° C. The spool of polyurea-aerogel / fiber composite was then retrieved.

[0312] The resulting polyurea-aerogel / fiber composite was white fiber with an aerogel mass loading of about 15%, and a thermal conductivity of about 35 mW / mK when laid into a mat and measured by the calibrated hot plate (CHP) method described herein.

[0313] Example 6: Synthesis of polyurethane-aerogel / fiber composites by reaction of isocyanates with polyols, applied to the fibers in a batch process and via CO 2 Produced by atmospheric sublimation drying

[0314] Spools of 150 denier multi-strand PET were prepared as described in Example 1.

[0315] A polyurethane gel is synthesized from an isocyanate and a polyol. 43.4 g of Desmodur RE (triisocyanatoaminophenylmethane) (80.6 wt % in ethyl acetate) is mixed with 513.78 g of acetone and stirred until thoroughly mixed (approximately 5 minutes). To this mixture is added 29.88 g of 1,1,1-tris(4-hydroxyphenyl)ethane and stirred for 5 minutes. Finally, 1.03 g of dibutyltin dilaurate is added and the mixture is stirred for an additional 5 minutes. The resulting sol is then poured into a container with a bobbin of fiber as described above, so that the bobbin of fiber is completely immersed. The container is then closed and allowed to stand for 30 minutes in a temperature controlled environment set at 15°C. After 30 minutes, the spool of fiber infiltrated with the polyurethane-aerogel-precursor was removed from the sol, placed in an airtight container containing acetone vapor, and placed in a temperature-controlled environment set at 15° C. for 24 hours, during which time gelation of the polyurethane-aerogel precursor solution occurred on and / or within the spool of fiber to form a polyurethane-gel / fiber composite.

[0316] The polyurethane-gel / fiber composite was then solvent exchanged and dried as described in Example 5.

[0317] The resulting polyurethane-aerogel / fiber composite was a light pink / purple fiber with approximately 15% aerogel mass loading, and a thermal conductivity of approximately 40 mW / mK when laid down into a mat and measured by the calibrated hot plate (CHP) method described herein.

[0318] Example 7: Synthesis of polyamide-aerogel / fiber composites by reaction of isocyanates with polyols, applied to the fibers in a batch process and via CO 2 Produced by atmospheric sublimation drying

[0319] Spools of 150 denier multi-strand PET were prepared as described in Example 1.

[0320] The polyamide gel is synthesized by the reaction of amine and acyl chloride. The synthesis is carried out in an inert nitrogen atmosphere. 2.02g of anhydrous calcium chloride is dissolved in 83.05g of N-methyl-2-pyrrolidone and stirred until completely dissolved (no particles are seen). 2.35g of p-phenylenediamine is added to the mixture and stirred until completely dissolved (no particles are seen). The mixture is cooled to 5°C in an ice-water bath. After the mixture reaches the target temperature, 4.25g of terephthaloyl chloride is added. The mixture is then stirred for 2 minutes (kept in an ice bath to continue cooling). The resulting sol is then poured into a container with a bobbin of the fiber as described above so that the bobbin of the fiber is completely immersed. The container is then closed and allowed to stand for 30 minutes. After 30 minutes, the bobbin of the fiber infiltrated with the polyamide-aerogel precursor is taken out from the sol, placed in an airtight container, and placed at room temperature for 24 hours, during which time the gelation of the polyurethane-aerogel precursor solution occurs on the bobbin of the fiber and / or in the bobbin of the fiber to form a polyamide-gel / fiber composite material.

[0321] The polyamide-gel / fiber composite was then solvent exchanged and dried as described in Example 5.

[0322] The resulting polyamide-aerogel / fiber composite was a light grey fiber with an aerogel mass loading of about 15%, and a thermal conductivity of about 55 mW / mK when laid down into a mat and measured by the calibrated hot plate (CHP) method described herein.

[0323] Example 8: Synthesis of polymer cross-linked oxide-aerogel / fiber composites composed of isocyanate and polyisocyanate The reaction of the alcohols is applied to the fibers in a batch process and via CO 2 Produced by atmospheric sublimation drying

[0324] Spools of 150 denier multi-strand PET were prepared as described in Example 1.

[0325] Gel is made by strengthening the oxide skeleton of silica gel with conformal polyisocyanate network.Prepare the solution called part A by mixing 36.23g acetonitrile, 7.77g tetramethoxysilane and 2.38g (3-aminopropyl) triethoxysilane.Prepare the solution called part B by mixing 36.23g acetonitrile and 16.15g deionized water.Then by placing the mixing beaker of two solutions in acetone-dry ice bath, it is cooled until temperature equilibrium.Then part B (now muddy) is added in part A, and the combined mixture is stirred vigorously.After two parts are fully mixed (vigorous stirring of <1 minute), then sol is poured into the container with the bobbin of fiber as mentioned above, so that the bobbin of fiber is fully submerged.Then the container is closed and allowed to be placed in this environment for 2 hours.After two hours, remove excessive gel from the bobbin of fiber outside, and silica-gel / fiber composite material is transferred to acetonitrile bath (being about 10 times of gel volume). The spools were kept in acetonitrile for 72 hours, during which the acetonitrile was replaced twice (at 24 hours and 48 hours) with clean acetonitrile. After 72 hours, the spools were transferred to a second bath containing a well-mixed solution of 314.4 g acetonitrile and 80.57 g Desmodur N3200 (biuret of hexamethylene diisocyanate) in which the spools were immersed for 24 hours. The spools were then subjected to three additional solvent changes to acetonitrile, identical to the first three. The gel was dried using the same method outlined in Example 5, except that the solvent within the gel and the solvent in which the gel was initially immersed was acetonitrile, not acetone, so the mixture discharged from the pressure vessel was CO 2. 2 -Acetonitrile instead of CO 2 -acetone.

[0326] The resulting polymer-crosslinked-silica-aerogel / fiber composite was a white fiber with about 15% aerogel mass loading and a thermal conductivity of about 35 mW / mK (when laid into a mat and measured by the calibrated hot plate (CHP) method described herein).

[0327] Example 9: Synthesis of polyimide-aerogel / PET-fiber composites by reaction of amine and anhydride to The invention is produced by applying the fiber to the fiber in a batch process and drying in a batch process by atmospheric sublimation of tert-butyl alcohol.

[0328] The polyimide-gel / fiber composite was prepared as described in Example 1. The spool of polyimide-gel / fiber composite was then placed in a solvent exchange bath, i.e., a sealed container partially filled with about 1500 mL of tert-butyl alcohol. The spool remained submerged in the tert-butyl alcohol in the container for 120 hours, during which time the tert-butyl alcohol was poured out and replaced four times with an equal volume of new tert-butyl alcohol.

[0329] After the solvent exchange was completed, the fiber thread shaft was transferred to a cold room to freeze the tert-butyl alcohol in the polyimide-gel / fiber composite. After it was frozen, cold air was flowed through the composite for 14 days until the tert-butyl alcohol was completely sublimated, at which time the polyimide-aerogel / fiber composite was removed.

[0330] The resulting polyimide-aerogel / fiber composite was a light yellow fiber with an aerogel mass loading of about 19% and a thermal conductivity of about 38 mW / mK (when laid down into a mat and measured by the calibrated hot plate (CHP) method described herein).

[0331] Example 10: Synthesis of polyimide-aerogel / PET-fiber composites by reaction of amine and anhydride to The product is applied to the fiber in a batch process and dried in a roll-to-roll process via atmospheric sublimation of tert-butyl alcohol.

[0332] A polyimide-gel / fiber composite is prepared as described in Example 9, including replacing the solvent with tert-butyl alcohol. The spool of polyimide-gel / fiber composite fiber is then transferred to a cold room. Inside the cold room, the fiber is unwound from the spool onto a roller. Between the spool and the roller, a jet of cold air is impacted on the fiber to freeze the tert-butyl alcohol in the polyimide gel / fiber composite. The fiber is moved through a series of rollers in the cold room until the tert-butyl alcohol is completely sublimated from the fiber, at which point the fiber is then rewound onto another spool. The process is run continuously until the transfer spool is exhausted and the tert-butyl alcohol has sublimated from the entire length of the fiber, resulting in a dry spool of polyimide-aerogel / fiber composite. The spool of polyimide-aerogel / fiber composite is then taken out.

[0333] The resulting polyimide-aerogel / fiber composite was a light yellow fiber with an aerogel mass loading of about 19% and a thermal conductivity of about 38 mW / mK (when laid down into a mat and measured by the calibrated hot plate (CHP) method described herein).

[0334] Example 11: Synthesis of polyimide-aerogel / FRPET-fiber composites by reaction of amine and anhydride, Produced by application to the fiber in a two-step process and drying in a continuous process via atmospheric sublimation of tert-butyl alcohol

[0335] The polyimide-aerogel-precursor solution was synthesized by the reaction of amine and anhydride and applied to 300 denier multi-strand flame retardant PET (FRPET) in a two-step process. 2.12g 2,2'-dimethylbenzidine was dissolved in 266.01g N-methyl-2-pyrrolidone. The mixture was stirred until 2,2'-dimethylbenzidine was completely dissolved (no particles were seen). After stirring for 10 minutes, 5.87g 3,3',4,4'-biphenyltetracarboxylic acid dianhydride was added to the mixture and stirred for 10 minutes. After stirring for 10 minutes, 6.87g 4,4'-[1,3-phenylene bis(1-methyl-ethylene)] dianiline was added to the mixture and stirred for 10 minutes. After stirring for 10 minutes, 5.87g 3,3',4,4'-biphenyltetracarboxylic acid dianhydride was added to the mixture and stirred for 10 minutes. After stirring for 10 minutes, 1.80 g of 4,4'-oxydiphenylamine was added to the mixture and stirred for 10 minutes. After 10 minutes, a mixture of 0.45 g of Desmodur N3300A and 26.60 g of N-methyl-2-pyrrolidone was added to the first mixture and stirred for 10 minutes. After stirring for 10 minutes, 32.57 g of acetic anhydride was added to the mixture and stirred for about 1 minute. After the addition of acetic anhydride, 5.42 g of trimethylsilyl-functionalized silica aerogel particles containing sodium ions were added to the mixture, i.e. MT1200 silica aerogel particles and stirred until the particles were evenly dispersed (no clumps of particles were visible). This mixture was Part A Polyimide-Aerogel-Precursor Solution. Part B Polyimide-Precursor Solution was 8.07 g triethylamine. The Part A solution and Part B solution were then poured into separate containers with the roller partially submerged in the solution.

[0336] The single strand 300 denier fireproof PET is controlled to a tension of 6g using a tension controller, then fed to the roller partially immersed in the part A solution, above the roller not in any solution, and then to the roller partially immersed in the part B solution. After passing through two solutions, the part A solution and the part B solution in the fiber react and gel to form a polyimide-gel / fiber composite. Then the polyimide-gel / fiber composite is directly run through a 10-meter-long tert-butyl alcohol bath at a speed of 10m / minute to allow complete solvent replacement of the pore fluid. Then the polyimide-gel / fiber composite is directly run into the cold room, wherein the fiber is impacted with a jet of cold air to freeze the tert-butyl alcohol in the polyimide-gel / fiber composite. Then the fiber is passed through and moved around a series of rollers in the cold room for a total residence distance of about 90 meters. This distance is enough to completely sublimate the tert-butyl alcohol from the fiber, and now it leaves the cold room and is then rewound onto another spool. The process was run continuously until the delivery spool was exhausted and the tert-butyl alcohol had sublimated from the entire length of the fiber, resulting in a spool of dry polyimide-aerogel / fiber composite.

[0337] The resulting polyimide-aerogel / fiber composite material is a light yellow fiber with an aerogel mass loading of about 19% and a thermal conductivity of about 38 mW / mK (when laid into a mat and measured by the calibrated hot plate (CHP) method described herein). After the resulting polyimide-aerogel / fiber composite material is immersed in water at 25° C. for 24 hours, the mass of water absorbed by the composite material within its outer boundary is about 19% of the dry mass of the composite material before being immersed in water.

[0338] The resulting polyimide-aerogel / fiber composite is then mechanically deformed using an air jet texturing machine to disperse the strands of the composite fiber and remove excess aerogel material. The resulting deformed polyimide-aerogel / fiber composite is then knitted into a fabric using a circular knitting machine.

[0339] The resulting fabric including the deformed polyimide-aerogel / fiber composite material was a light yellow knitted fabric that passed the FAR 25.853 standard for flammability testing.

[0340] Example 12: Synthesis of polyimide-aerogel / PET-fabric composites by reaction of amine and anhydride to The process is applied to the fabric in a batch process and via supercritical CO 2 Extraction and drying to produce

[0341] A 4-inch wide plain knit fabric containing 150 denier multi-strand PET fibers was wrapped around a 6-inch long, 2-inch diameter bobbin so that a total of 20 g of fabric was wound on the bobbin. A polyimide-aerogel precursor solution was synthesized as described in Example 1. The polyimide-aerogel precursor solution was then poured into a container with the bobbin of the aforementioned fabric so that the bobbin of the fabric was completely immersed. The container was then closed and left for 20 minutes. After 20 minutes, the bobbin of the fabric infiltrated with polyimide-aerogel-precursor was taken out of the sol, placed in an airtight container, and left at room temperature for 24 hours, during which time gelation of the polyimide-aerogel precursor solution occurred on and / or in the bobbin of the fabric to form a polyimide-gel / fabric composite.

[0342] After 24 hours, the spool of polyimide-gel / fabric composite was removed from the container and rewound onto another spool. The spool of polyimide-gel / fabric was then processed through a solvent exchange and drying process to become a polyimide-aerogel / fabric composite in the same manner as described for the polyimide-aerogel / fiber composite in Example 1.

[0343] The obtained polyimide-aerogel / fabric composite material was a light yellow fabric with an aerogel mass loading of about 18% and a 30m 2 / g, and a thermal conductivity of about 41 mW / mK (when measured by the calibrated hot plate (CHP) method described herein). Optical microscopy imaging showed that the polyimide aerogel was both on the outer surface of the fabric and within the pores of the fabric. Optical microscopy imaging also showed that a portion of the composite fabric had a substantially continuous polyimide aerogel on the surface of a cross-section of the composite fabric, while other portions of the composite showed that the polyimide aerogel was discontinuous.

[0344] Example 13: Synthesis of polyimide-aerogel / nylon-fabric composites by reaction of amines and anhydrides, applied to the fibers in a batch process and via supercritical CO 2 Extraction and drying to produce

[0345] A 4 inch wide jersey knit fabric containing 270 denier nylon fibers was wrapped around a 6 inch long, 2 inch diameter bobbin so that a total of 20 g of fabric was wound on the bobbin. The bobbin of fabric then followed the same processing steps as the bobbin of PET fabric described in Example 12, from exposing the bobbin to the polyimide-aerogel-precursor solution to drying.

[0346] The resulting polyimide-aerogel / fabric composite was a pale yellow fabric with an aerogel mass loading of about 18% and a thermal conductivity of about 41 mW / mK (when measured by the calibrated hot plate (CHP) method described herein). Optical microscopy imaging showed that the polyimide aerogel substantially conformally coated the fabric.

[0347] Example 14: Synthesis of polyimide-aerogel / PET-fabric composites prepared by reacting amines and anhydrides in the presence of carbon dioxide Continuous preparation of polymer-aerogel precursor solution by reaction in the presence of silica aerogel particles additive in a roll-to-roll process applied to the fabric, and via supercritical CO 2 Extraction and drying to produce

[0348] Spools of PET fabric were prepared as described in Example 12. A polyimide-aerogel precursor solution containing silica aerogel particles was prepared as described in Example 4, except that trimethylamine was added. The Part A solution was then mixed with a Part B solution of 8.07 g of trimethylamine in an on-demand manner using a commercially available static mixing device to produce a polyimide-aerogel precursor solution. The solutions were combined and dispensed into a tank at a constant rate over a period of time, such that the rate of dispensing matched the rate at which the fabric removed the solution from the tank. The fabric was fed onto a receiving spool at a rate of 2 m / min under a roll partially submerged in the tank, such that the fabric was exposed to the solution in a roll-to-roll manner and penetrated by the solution. The receiving spool of fabric penetrated by the polyimide-aerogel precursor solution then followed the same processing steps as the spool of fabric described in Example 12 from gelation of the spool to drying.

[0349] The obtained polyimide-aerogel / fabric composite material was a light yellow fabric with an aerogel mass loading of about 18%, a 2 / g, a BET surface area of ​​about 400 Å / g, a thermal conductivity of about 41 mW / mK (when measured by the calibrated hot plate (CHP) method described herein), and a thickness of about 0.03 inches.

[0350] The resulting polyimide-aerogel / fabric composite was then washed according to the AATCC LP1 standard for home washing.

[0351] The washed polyimide-aerogel / fabric composite material was a light yellow fabric with a thickness of about 50 m 2 / g and a thermal conductivity of about 45 mW / mK when measured by the calibrated hot plate (CHP) method described herein.

[0352] Example 15: Synthesis of polyimide-aerogel / PET-fabric composites by reaction of amine and anhydride to The fibers are applied in a batch process and produced by atmospheric sublimation of tert-butyl alcohol in a batch process for drying.

[0353] A spool of polyimide-gel / PET-fabric composite was prepared as described in Example 12. The spool then followed the same processing steps as the spool of fiber described in Example 9 from solvent change to drying.

[0354] The resulting polyimide-aerogel / fabric composite was a light yellow fabric with an aerogel mass loading of about 18% and a thermal conductivity of about 41 mW / mK (when measured by the calibrated hot plate (CHP) method described herein).

[0355] Example 16: Synthesis of polyimide-aerogel / PET-fiber composites by reaction of amine and anhydride to The fibers are applied in a batch process and dried in a roll-to-roll process via atmospheric sublimation of tert-butyl alcohol.

[0356] Spools of polyimide-gel / PET-fabric composite were prepared and solvent exchanged as described in Example 9. The spools of fabric were then dried as described in Example 10.

[0357] The resulting polyimide-aerogel / fabric composite was a light yellow fabric with an aerogel mass loading of about 18% and a thermal conductivity of about 41 mW / mK (when measured by the calibrated hot plate (CHP) method described herein).

[0358] Example 17: Synthesis of polyimide-aerogel / FRPET-cotton-blended-fabric composites prepared from amines and acids The reaction of anhydride, application to the fiber in a two-step process, and drying in a continuous process via atmospheric sublimation of tert-butyl alcohol is produced.

[0359] The polyimide-aerogel-precursor solution is synthesized by the reaction of amine and anhydride, and applied to a blended woven fabric containing both flame retardant PET (FRPET) and cotton fiber in a two-step process. 2.12g 2,2'-dimethylbenzidine is dissolved in 266.01g N-methyl-2-pyrrolidone. The mixture is stirred until 2,2'-dimethylbenzidine is completely dissolved (no particles are seen). After stirring for 10 minutes, 5.87g 3,3',4,4'-biphenyltetracarboxylic acid dianhydride is added to the mixture and stirred for 10 minutes. After stirring for 10 minutes, 6.87g 4,4'-[1,3-phenylene bis(1-methyl-ethylene)] benzidine is added to the mixture and stirred for 10 minutes. After stirring for 10 minutes, 5.87g 3,3',4,4'-biphenyltetracarboxylic acid dianhydride is added to the mixture and stirred for 10 minutes. After stirring for 10 minutes, 1.80 g of 4,4'-oxydiphenylamine was added to the mixture and stirred for 10 minutes. After 10 minutes, a mixture of 0.45 g of Desmodur N3300A and 26.60 g of N-methyl-2-pyrrolidone was added to the first mixture and stirred for 10 minutes. After stirring for 10 minutes, 32.57 g of acetic anhydride was added to the mixture and stirred for about 1 minute. After the addition of acetic anhydride, 5.42 g of trimethylsilyl-functionalized silica aerogel particles containing sodium ions were added to the mixture, i.e. MT1200 silica aerogel particles and stirred until the particles were evenly dispersed (no clumps of particles were visible). This mixture was Part A Polyimide-Aerogel-Precursor Solution. Part B Polyimide-Precursor Solution was 8.07 g triethylamine. The Part A solution and Part B solution were then poured into separate containers with the roller partially submerged in the solution.

[0360] The FRPET-cotton blended fabric is fed to the roller below the partially immersed part in the part A solution, above the roller not in any solution, and then below the roller below the partially immersed part in the part B solution. After passing through two solutions, the part A solution and the part B solution in the fabric react and gel to form a polyimide-gel / fabric composite material. Then the polyimide-gel / fabric composite material is directly run through a 10-meter-long tert-butyl alcohol bath at a speed of 10m / minute to allow the solvent replacement of the pore fluid. Then the polyimide-gel / fabric composite material is directly run into the cold room, wherein the fabric is impacted with a jet of cold air to freeze the tert-butyl alcohol in the polyimide-gel / fabric composite material. Then, the fabric is passed through and moved around a series of rollers in the cold room for a total residence distance of about 90 meters. This distance is enough to make the tert-butyl alcohol completely sublime from the fabric, and now it leaves the cold room and is then rewound onto another carrier. The process is continuously operated until the conveying carrier is exhausted, and the tert-butyl alcohol has been sublimated from the entire length of the fabric to obtain a roll of dry polyimide-aerogel / fiber composite material.

[0361] The resulting polyimide-aerogel / fabric composite was mechanically finished by running it over and through a series of deforming rollers to remove excess polyimide aerogel material.

[0362] The resulting polyimide-aerogel / fabric composite material was a light yellow fabric with an aerogel mass loading of about 19% and a thermal conductivity of about 34 mW / mK (when measured by the calibrated hot plate (CHP) method described herein). After the resulting polyimide-aerogel / fiber composite material was immersed in water at 25° C. for 24 hours, the mass of water absorbed by the composite material within its outer boundary was about 19% of the dry mass of the composite material before being immersed in water. The resulting polyimide-aerogel / fabric composite material passed the FAR 25.853 standard for flammability testing.

[0363] Example 18: Synthesis of polyurea-aerogel / fabric composites from isocyanates and in situ formed amines reaction, applied to fabric in a batch process, and via supercritical CO 2 Extraction and drying to produce

[0364] Spools of PET fabric were prepared as described in Example 12.

[0365] A polyurea aerogel precursor solution was prepared as described in Example 5. The resulting solution was then poured into a container with a roll partially immersed in the sol. The fabric was fed onto a receiving spool under the partially immersed roll so that the fabric was exposed to and penetrated by the solution in a roll-to-roll manner. The receiving spool of fabric penetrated by the polyurea-aerogel precursor solution then followed the same processing steps as the spool of fabric described in Example 12 from gelation of the spool to drying.

[0366] The resulting polyurea-aerogel / fabric composite was a white fabric with an aerogel mass loading of about 18% and a thermal conductivity of about 30 mW / mK (when measured by the calibrated hot plate (CHP) method described herein).

[0367] The resulting polyurea-aerogel / fabric composite can be dewoven and tack-textured using commercial tack-texturizing equipment to produce a polyurea-aerogel / fiber composite.

[0368] Example 19: Synthesis of polyurethane-aerogel / fabric composites by reaction of isocyanates with polyols, applied to the fabric in a batch process and via supercritical CO 2 Extraction and drying to produce

[0369] Spools of PET fabric were prepared as described in Example 12, except that a nonwoven PET fabric was used instead of a jersey knit.

[0370] A polyurethane aerogel precursor solution was prepared as described in Example 6. The resulting solution was then poured into a container with a roll partially immersed in the sol. The fabric was fed onto a receiving spool under the partially immersed roll so that the fabric was exposed to and penetrated by the solution in a roll-to-roll manner. The receiving spool of fabric penetrated by the polyurea-aerogel precursor solution then followed the same processing steps as the spool of fabric described in Example 12 from gelation of the spool to drying.

[0371] The resulting polyurethane-aerogel / fabric composite was a light pink / purple fabric with an aerogel mass loading of about 18% and a thermal conductivity of about 38 mW / mK (when measured by the calibrated hot plate (CHP) method described herein).

[0372] Example 20: Synthesis of polyamide-aerogel / fabric composites by reaction of isocyanate with polyol, applied to the fabric in a batch process and via supercritical CO 2 Extraction and drying to produce

[0373] Spools of PET fabric were prepared as described in Example 12.

[0374] A polyamide aerogel precursor solution was prepared as described in Example 6. The resulting solution was then poured into a container with a roll partially immersed in the solution. The fabric was fed onto a receiving spool under the partially immersed roll so that the fabric was exposed to and penetrated by the solution in a roll-to-roll manner. The receiving spool of fabric penetrated by the polyurea-aerogel precursor solution then followed the same processing steps as the spool of fabric described in Example 12 from gelation of the spool to drying.

[0375] The resulting polyamide-aerogel / fabric composite was a light grey fabric with an aerogel mass loading of about 18% and a thermal conductivity of about 50 mW / mK (when measured by the calibrated hot plate (CHP) method described herein).

[0376] Example 21: Synthesis of polymer cross-linked oxide-aerogel / fabric composites made from isocyanate and The polyols are reacted and applied to the fabric in a batch process and via supercritical CO 2 Extraction and drying to produce

[0377] Spools of PET fabric were prepared as described in Example 12.

[0378] Gel is made by strengthening the oxide skeleton of silica gel with conformal polyisocyanate network. Prepare the solution called part A by mixing 36.23g acetonitrile, 7.77g tetramethoxysilane and 2.38g (3-aminopropyl) triethoxysilane. Prepare the solution called part B by mixing 36.23g acetonitrile and 16.15g deionized water. Then cool it until temperature balance by placing the mixing beaker of two solutions in acetone-dry ice bath. Then add part B (now muddy) in part A, and the combined mixture is stirred vigorously. After two parts are fully mixed (vigorous stirring of <1 minute), then pour the sol into the container with the bobbin of fabric as mentioned above, so that the bobbin of fabric is fully immersed. Then the container is closed and allowed to be placed in this environment for 2 hours. After two hours, remove excessive gel from the bobbin of fabric outside, and transfer silica-gel / fabric composite material to acetonitrile bath (about 10 times of gel volume). The spools were kept in acetonitrile for 72 hours, during which the acetonitrile was replaced twice (at 24 hours and 48 hours) with clean acetonitrile. After 72 hours, the spools were transferred to a second bath of a well-mixed solution of 314.4 g acetonitrile and 80.57 g Desmodur N3200 (biuret of hexamethylene diisocyanate) in which the spools were soaked for 24 hours. The spools were then subjected to three additional solvent changes to acetonitrile, the same as the first three. The gel was dried using the same method outlined in Example 12, except that the solvent within the gel and the solvent in which the gel was initially immersed was acetonitrile, not acetone.

[0379] The resulting polymer-cross-linked-silica-aerogel / fabric composite was a white fabric with an aerogel mass loading of about 18% and a thermal conductivity of about 30 mW / mK (when measured by the calibrated hot plate (CHP) method described herein).

[0380] Example 22: Synthesis of polyimide-aerogel / PET-fabric composites including garments prepared from amines and acids anhydride reaction, applied to fabric in a batch process, and via supercritical CO 2 Produced by drying the extract.

[0381] A polyimide-aerogel precursor solution was synthesized as described in Example 1. The solution was then poured onto a 40 g portion of fabric that formed part of a garment, in this case a PET knitted shirt sleeve. The garment, now infiltrated with the polyimide-aerogel precursor solution, then followed the same processing steps for the spools of fabric described in Example 12 from gelation to drying.

[0382] The obtained polyimide-aerogel / fabric composite material was a light yellow fabric with an aerogel mass loading of about 18%, a 2 / g, and a BET surface area of ​​approximately 41 mW / mK (when measured by the calibrated hot plate (CHP) method described herein).

[0383] Example 23: Synthesis of polyimide-aerogel / PET-fabric composites including clothing made from amines and acids The anhydride is reacted in a two-part liquid and vapor process applied to the fabric, and via supercritical CO 2 Produced by drying the extract.

[0384] Part A polyimide-aerogel precursor solution was prepared as described in Example 17. A spool of PET fiber was prepared similarly as described in Example 17. The fiber was then moved through the Part A solution as described in Example 17. Thereafter, the fiber was then moved through a chamber with a saturated vapor atmosphere of triethylamine at 50°C. Thereafter, the fiber was wound onto a receiving spool. The spool of fiber infiltrated with the polyimide-aerogel precursor solution was processed from gelation to drying to produce a polyimide-aerogel-fiber composite. The resulting polyimide-aerogel / fiber composite was a light yellow fiber with an aerogel mass loading of about 19% and a thermal conductivity of about 38 mW / mK (when poured into a mat and measured by the calibrated hot plate (CHP) method described herein)

[0385] Although several embodiments of the present invention have been described and illustrated herein, a person of ordinary skill in the art will readily envision a variety of other ways and / or structures for performing the functions described herein and / or obtaining the results and / or one or more advantages described herein, and each of such variations and / or modifications is considered to be within the scope of the present invention. More generally, it will be readily understood by those skilled in the art that all parameters, dimensions, materials, and configurations described herein are intended to be exemplary, and that actual parameters, dimensions, materials, and / or configurations will depend on the specific application or application of the teachings of the present invention. Those skilled in the art will recognize or be able to determine many equivalents of the specific embodiments of the present invention described herein using only routine experiments. Therefore, it should be understood that the aforementioned embodiments are given only by way of example, and within the scope of the appended claims and their equivalents, the present invention can be implemented in a manner other than specifically described and claimed. The present invention relates to each individual feature, system, product, material, and / or method described herein. In addition, if such features, systems, products, materials, and / or methods are not inconsistent with each other, any combination of two or more such features, systems, products, materials, and / or methods is included within the scope of the present invention.

[0386] Unless explicitly stated to the contrary, as used herein in the specification and claims, nouns without quantifiers should be understood to mean "at least one".

[0387] The phrase "and / or" as used herein in the specification and claims should be understood to mean "one or both" of the elements so connected, i.e., in some cases the elements are present together, and in other cases the elements are present separately. Unless expressly indicated to the contrary, other elements other than those expressly indicated by the "and / or" conjunction may optionally be present, whether related or unrelated to those elements expressly indicated. Thus, as a non-limiting example, when used in conjunction with an open language such as "comprising", a reference to "A and / or B" may refer to A in some embodiments without B (optionally including elements other than B); to B in some embodiments without A (optionally including elements other than A); to both A and B in some embodiments (optionally including other elements); etc.

[0388] As used herein in the specification and in the claims, "or / or" shall be understood to have the same meaning as "and / or" as defined above. For example, when separating items in a list, "or / or" or "and / or" shall be interpreted as inclusive, i.e., including at least one of a plurality of elements or a list of elements, but also including more than one, and optionally including items not otherwise listed. Only explicit indication of the opposite term, such as "only one of" or "exactly one of", or when used in a claim, "consisting of...", will refer to including exactly one element of a plurality of elements or a list of elements. In general, the term "or / or" as used herein shall only be interpreted as indicating exclusive alternatives (i.e., "one or the other but not both") when preceded by an exclusive term (e.g., "either", "one of", "only one of", or "exactly one of"). "Substantially consisting of..." when used in a claim shall have its ordinary meaning as used in the field of patent law.

[0389] As used herein in the specification and claims, when referring to a list of one or more elements, the phrase "at least one" should be understood to mean at least one element selected from any one or more elements in the list of elements, but not necessarily including at least one of each and every element specifically listed in the list of elements, and not excluding any combination of elements in the list of elements. This definition also allows that elements other than the elements specifically identified in the list of elements to which the phrase "at least one" refers may optionally be present, whether related or unrelated to those elements specifically identified. Thus, as a non-limiting example, "at least one of A and B" (or equivalently, "at least one of A or B", or equivalently, "at least one of A and / or B") may refer in some embodiments to at least one A, optionally including more than one A, but no B (and optionally including elements other than B); in certain embodiments, may refer to at least one B, optionally including more than one B, but no A (and optionally including elements other than A); in certain embodiments, may refer to at least one A, optionally including more than one A, and at least one B, optionally including more than one B (and optionally including other elements); and so on.

[0390] In the claims and in the foregoing specification, all transitional phrases such as "comprising," "including," "with," "having," "containing," "involving," "having," etc. shall be construed as open ended, i.e., understood to mean including, but not limited to. Only the transitional phrases "consisting of" and "consisting essentially of" shall be closed or semi-closed transitional phrases, respectively, as provided in Section 2111.03 of the U.S. Patent Office Manual of Patent Examining Procedures.

Claims

1. A composite fiber comprising: Fiber; and a polymer aerogel material conformally coating an outer surface of the fiber, wherein the average cross-sectional diameter of the composite fiber is at least 5 μm and less than or equal to 3 mm, wherein the aspect ratio of the composite fiber is at least 100:1, and The mass fraction of the polymer aerogel in the composite fiber is greater than 10%. The composite fiber according to claim 1 , wherein the fiber is a multi-stranded fiber. The composite fiber according to claim 1 , wherein the fiber is a single-strand fiber.

4. The composite fiber according to any one of claims 1 to 3, wherein the fiber comprises polyester, polyamide and / or cotton.

5. The composite fiber according to any one of claims 1 to 3, wherein the fiber comprises a blend of two or more fiber types. 6 . The composite fiber according to claim 1 , wherein the polymer aerogel material comprises a polyimide aerogel material.

7. The composite fiber according to any one of claims 1 to 3, wherein the polymer aerogel material comprises polyurea.

8. The composite fiber according to any one of claims 1 to 3, wherein the polymer aerogel material comprises polyamide.

9. The composite fiber according to any one of claims 1 to 3, wherein the polymer aerogel material comprises polyurethane.

10. The composite fiber according to any one of claims 1 to 3, wherein the polymer aerogel material comprises a polymer cross-linked oxide.

11. The composite fiber according to any one of claims 1 to 3, wherein the mass fraction of the polymer aerogel in the composite fiber is greater than 15%.

12. The composite fiber according to any one of claims 1 to 3, wherein the mass fraction of the polymer aerogel in the composite fiber is greater than 20%.

13. The composite fiber according to any one of claims 1 to 3, wherein the mass fraction of the polymer aerogel in the composite fiber is greater than 25%.

14. The composite fiber according to any one of claims 1 to 3, wherein the mass fraction of the polymer aerogel in the composite fiber is greater than 30%.

15. The composite fiber according to any one of claims 1 to 3, wherein the mass fraction of the polymer aerogel in the composite fiber is greater than 35%.

16. The composite fiber according to any one of claims 1 to 3, wherein the mass fraction of the polymer aerogel in the composite fiber is greater than 50%.

17. The composite fiber according to claim 6, wherein the mass fraction of the polyimide aerogel material in the composite fiber is greater than 1%.

18. The composite fiber according to claim 6, wherein the mass fraction of the polyimide aerogel material in the composite fiber is greater than 5%.

19. The composite fiber according to claim 6, wherein the mass fraction of the polyimide aerogel material in the composite fiber is greater than 10%.

20. The composite fiber according to claim 6, wherein the mass fraction of the polyimide aerogel material in the composite fiber is greater than 15%.

21. The composite fiber according to claim 6, wherein the mass fraction of the polyimide aerogel material in the composite fiber is greater than 20%.

22. The composite fiber according to claim 6, wherein the mass fraction of the polyimide aerogel material in the composite fiber is greater than 25%.

23. The composite fiber according to claim 6, wherein the mass fraction of the polyimide aerogel material in the composite fiber is greater than 30%.

24. The composite fiber according to claim 6, wherein the mass fraction of the polyimide aerogel material in the composite fiber is greater than 35%.

25. The composite fiber according to claim 6, wherein the mass fraction of the polyimide aerogel material in the composite fiber is greater than 50%.

26. The composite fiber according to any one of claims 1 to 3, wherein the composite fiber is incorporated into a fabric.

27. The composite fiber according to any one of claims 1 to 3, wherein the composite fiber can be woven and / or knitted into a fabric.

28. The composite fiber according to any one of claims 1 to 3, wherein the composite fiber is capable of being knitted into a fabric using commercial knitting equipment.

29. The composite fiber of any one of claims 1 to 3, wherein the polymer aerogel material is substantially continuous along the length of the composite fiber.

30. The composite fiber of claim 6, wherein the polyimide aerogel material is substantially continuous along the length of the composite fiber.

31. The composite fiber of any one of claims 1 to 3, wherein the polymer aerogel material is discontinuous along the length of the composite fiber.

32. The composite fiber of claim 6, wherein the polyimide aerogel material is discontinuous along the length of the composite fiber.

33. The composite fiber of any one of claims 1 to 3, wherein the composite fiber exhibits a thermal conductivity of less than 80 mW / mK when the composite fiber is laid into a mat and measured using the ASTM C518 method.

34. The composite fiber of any one of claims 1 to 3, wherein the composite fiber exhibits a thermal conductivity of less than 40 mW / mK when the composite fiber is laid into a mat and measured using the ASTM C518 method.

35. The composite fiber of any one of claims 1 to 3, wherein a fabric comprising the composite fiber exhibits a thermal conductivity of less than 80 mW / mK using the ASTM C518 method.

36. The composite fiber of any one of claims 1 to 3, wherein a fabric comprising the composite fiber exhibits a thermal conductivity of less than 40 mW / mK using the ASTM C518 method.

37. The composite fiber according to any one of claims 1 to 3, wherein the composite fiber exhibits a strength greater than 10 m 2 / g of BET surface area.

38. The composite fiber of any one of claims 1 to 3, wherein the polymer aerogel material comprises silica aerogel.

39. The composite fiber of any one of claims 1 to 3, wherein the polymer aerogel material comprises a trimethylsilyl-functionalized silica aerogel.

40. The composite fiber of claim 38, wherein the silica aerogel comprises sodium ions.

41. The composite fiber of claim 6, wherein the polyimide aerogel material comprises trimethylsilyl-functionalized silica aerogel, wherein the silica aerogel comprises sodium ions.

42. The composite fiber according to any one of claims 1 to 3, wherein the composite fiber can be washed according to the AATCC LP1 home wash standard, and the washed material exhibits a laundering resistance of at least 10 m 2 / g of BET surface area.

43. The composite fiber according to any one of claims 1 to 3, wherein when the composite fiber is immersed in water at 25°C for 24 hours, the aerogel absorbs water within its outer boundary by a mass less than 20% of the dry mass of the aerogel before immersion in the water.

44. The composite fiber according to any one of claims 1 to 3, wherein when the composite fiber is immersed in water at 25°C for 24 hours, the aerogel absorbs water within its outer boundary by a mass less than 20% of the dry mass of the composite fiber before immersion in the water.

45. A fabric comprising the composite fiber according to any one of claims 1 to 3, wherein the fabric passes a flammability test.

46. ​​A fabric comprising the composite fiber according to any one of claims 1 to 3, wherein the fabric passes the FAR 25.853 flammability test.

47. A fabric comprising the composite fiber according to any one of claims 1 to 3, wherein the fabric passes at least one of the following flammability tests: ASTM D6413, 16CFR 1615, CPAI-84, ASTM D1230.

48. A method of forming a composite fiber, include: exposing the fibers to a liquid solution comprising a polymer-aerogel-precursor; as well as forming a polymer aerogel from the polymer-aerogel-precursor so that the polymer aerogel is conformally coated on the outer surface of the fiber to form the composite fiber, wherein the average cross-sectional diameter of the composite fiber is at least 5 μm and less than or equal to 3 mm, wherein the aspect ratio of the composite fiber is at least 100:1, and The mass fraction of the polymer aerogel in the composite fiber is greater than 10%.

49. The method of claim 48, wherein the fibers are pretreated before exposing them to the liquid solution comprising a polymer-aerogel-precursor.

50. The method according to any one of claims 48 to 49, wherein the tension of the fiber is controlled to a tension of 1 g to 20 g during and / or before exposing the fiber to the liquid solution comprising a polymer-aerogel-precursor.

51. The method according to any one of claims 48 to 49, wherein the bobbin of fibers is exposed to the liquid solution comprising a polymer-aerogel-precursor.

52. The method according to any one of claims 48 to 49, wherein the fibers are exposed to the liquid solution comprising a polymer-aerogel-precursor in a continuous process.

53. The method of claim 52, wherein the fibers are exposed to the liquid solution comprising a polymer-aerogel-precursor in a roll-to-roll manner.

54. The method according to any one of claims 48 to 49, wherein the liquid solution comprising a polymer-aerogel-precursor is prepared in a continuous manner.

55. The method according to any one of claims 48 to 49, wherein the liquid solution comprising the polymer-aerogel-precursor is applied in at least two sequential steps.

56. The method according to any one of claims 48 to 49, wherein the fibers are exposed to a liquid solution comprising a part A polymer-aerogel-precursor and then to a liquid solution comprising a part B polymer-aerogel-precursor.

57. The method according to any one of claims 48 to 49, wherein the liquid solution comprising a polymer-aerogel-precursor on and / or in the fibers forms a polymer gel on and / or in the fibers after a period of time, thereby forming a polymer-gel / fiber composite material.

58. The method according to any one of claims 48 to 49, wherein the fibers are exposed to a liquid solution comprising a polymer-aerogel precursor and then to a vapor environment, so that the liquid solution comprising a polymer-aerogel precursor forms a polymer gel on and / or in the fibers after a period of time, thereby forming a polymer-gel / fiber composite material.

59. The method of claim 57, wherein the liquid in the pores of the polymer-gel / fiber composite is replaced with another solvent.

60. The method of claim 59, wherein the liquid in the pores of the polymer-gel / fiber composite is replaced with another solvent using a continuous process.

61. The method of claim 60, wherein the liquid in the pores of the polymer-gel / fiber composite is replaced with additional solvent in a roll-to-roll manner.

62. The method of claim 57, wherein the polymer-gel / fiber composite is treated such that liquid within the pores of the gel is removed while leaving the solid phase structure of the gel substantially intact to produce the composite fiber.

63. The method of claim 57, wherein the polymer-gel / fiber composite is processed using a continuous process to produce the composite fiber.

64. The method of claim 63, wherein the polymer-gel / fiber composite is processed in a roll-to-roll manner to produce the composite fibers.

65. The method of any one of claims 48 to 49, wherein the composite fiber comprises a plurality of stranded fibers and is mechanically treated to separate the strands of the composite fiber from one another.

66. The method of claim 57, wherein the polymer gel is a polyimide gel.

67. The method of any one of claims 48 to 49, wherein the composite fiber is a polyimide-aerogel / fiber composite.

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