Compressed aerogel composite material and preparation method thereof

Abstract

The present disclosure relates to a method of making an aerogel composite, the method comprising compressing an aerogel composite, the aerogel composite comprising a gel dispersed around a reinforcing component. The method further includes heating the aerogel composite material. The method also results in the production of a compressed and heated aerogel composite, the produced aerogel composite comprising a plurality of pores, the majority of which have a diameter of less than 50 nm.

Description

[0001] CROSS-REFERENCE TO RELATED APPLICATIONS

[0002] This application claims priority to U.S. Provisional Patent Application Serial No. 63 / 415,897, filed on October 13, 2022, entitled “COMPRESSED AEROGEL COMPOSITE AND METHOD OF MAKING,” the disclosure of which is incorporated herein by reference in its entirety. Background Art

[0003] Low-density materials have been developed to solve many thermal insulation problems where the insulating core material is subjected to high pressure. For example, polymer materials mixed with hollow glass microspheres can form composite foams, which are generally very hard, compression-resistant materials. Composite materials are well known as insulators for underwater oil and gas pipelines and supporting equipment. However, relative to flexible aerogel composites (aerogel matrices reinforced with fibers), composite materials are relatively inflexible and exhibit high thermal conductivity.

[0004] Aerogels are a class of materials that are based on their structure, i.e. low density, open pore structure, large surface area (typically 900m 2 / g or more) and submicron pore size. Supercritical and subcritical fluid extraction techniques are commonly used to extract solvents from fragile cells of materials. Various aerogel compositions (both organic and inorganic) are known in the art. Inorganic aerogels are typically based on metal alkoxides and include materials such as silicon dioxide, zirconium oxide, titanium dioxide, aluminum oxide, carbides, etc. Organic aerogels may include carbon aerogels and polymer aerogels, such as polyimide aerogels. Summary of the invention

[0005] The present disclosure relates to a method of preparing an aerogel composite material, the method comprising compressing an aerogel composite material, the aerogel composite material comprising a gel dispersed around a reinforcing component. The method further comprises heating the aerogel composite material. The method also results in the production of a compressed and heated aerogel composite material, the produced aerogel composite material comprising a plurality of pores, wherein a majority of the pores have a diameter of less than 50 nm.

[0006] The present disclosure also relates to a method for preparing an aerogel composite material, the method comprising compressing an aerogel composite material, the aerogel composite material comprising silica gel dispersed around a reinforcing component, the reinforcing component comprising polyethylene terephthalate fibers. The method also comprises heating the aerogel composite material to a temperature above the glass transition temperature of polyethylene, polyacrylonitrile, oxidized polyacrylonitrile, polyethylene terephthalate, or a mixture thereof. The method also results in the production of a compressed and heated aerogel composite material, the produced aerogel composite material comprising a plurality of pores, wherein a majority of the pores have a diameter of less than 50 nm.

[0007] The present disclosure also relates to a compressed aerogel composite material. The compressed aerogel composite material includes a gel comprising a metal oxide compound distributed around a reinforcing component. The aerogel composite material includes a plurality of pores, wherein a majority of the pores have a diameter less than 50 nm, and the thickness of the aerogel composite material is less than about 0.6 mm.

[0008] The present disclosure also relates to a compressed aerogel composite material. The compressed aerogel composite material includes a gel comprising silica distributed around a polyethylene terephthalate fiber reinforcement component. The aerogel composite material includes a plurality of pores, wherein a majority of the pores have a diameter of less than 50 nm. BRIEF DESCRIPTION OF THE DRAWINGS

[0009] The drawings generally illustrate various aspects of the disclosure by way of example and not limitation.

[0010] Figure 1 A compression mechanism is shown, where a hydraulic press is used to densify the aerogel composite.

[0011] Figure 2 is a continuous compression scheme for the densification of aerogel composites.

[0012] Figure 3 is a graph showing the thermal conductivity of the gel of the aerogel composite material of Example 1 at different compression levels.

[0013] Figure 4 : is a graph showing the relationship between the thermal performance and stress of the composite aerogel of Example 1.

[0014] Figure 5 This is a graph showing the thermal conductivity of the composite aerogel of Example 1 at various temperatures.

[0015] Fig. 6A is a graph showing the decrease in thermal conductivity of the composite aerogel.

[0016] Figure 6B is a graph showing the average pore size of the composite aerogel of Example 1 at different degrees of permanent strain.

[0017] Figure 7 is a graph showing the pore size distribution of the composite aerogel of Example 1 at different degrees of permanent strain.

[0018] Figure 8 is a graph showing a finite fraction of the applied strain that remains in an aerogel composite when a compressive strain is applied.

[0019] Fig.9AIt is shown that lower silica density and higher compressive strain in aerogel composites are associated with higher plastic strain in aerogel composites.

[0020] Fig. 9B It was shown that the hydrophobic content (covalently bonded to the silica aerogel in the reinforced silica aerogel composite) is another parameter that can change the amount of plastic deformation retained in the aerogel composite in response to compressive strain.

[0021] Description of Reference Numerals

[0022] none. DETAILED DESCRIPTION

[0023] Reference will now be made in detail to certain aspects of the disclosed subject matter, examples of which are partially illustrated in the accompanying drawings.While the disclosed subject matter will be described in conjunction with the enumerated claims, it will be understood that the illustrated subject matter is not intended to limit the claims to the disclosed subject matter.

[0024] definition

[0025] In this article, the values ​​expressed in range format should be interpreted in a flexible manner to include not only the values ​​explicitly listed as range limits, but also all individual values ​​or sub-ranges contained in the range, as if each value and sub-range were explicitly listed. For example, the range of "about 0.1% to about 5%" or "about 0.1% to 5%" should be interpreted as including not only about 0.1% to about 5%, but also individual values ​​(e.g., 1%, 2%, 3% and 4%) and sub-ranges (e.g., 0.1% to 0.5%, 1.1% to 2.2%, 3.3% to 4.4%) within the indicated range. Unless otherwise specified, the statement "about X to Y" has the same meaning as "about X to about Y". Similarly, unless otherwise specified, the statement "about X, Y or about Z" has the same meaning as "about X, about Y or about Z".

[0026] In this article, unless the context clearly dictates otherwise, the terms "a", "an" or "the" are used to include one or more than one. Unless otherwise specified, the term "or" is used to refer to a non-exclusive "or". The statement "at least one of A and B" or "at least one of A or B" has the same meaning as "A, B, or A and B". In addition, it should be understood that the words or terms used herein and not otherwise defined are for descriptive purposes only, not for limiting purposes. Any use of section headings is intended to assist in reading this article and should not be interpreted as limiting; information related to section headings may appear within or outside that particular section. All publications, patents, and patent documents mentioned in this article are incorporated herein by reference in their entirety, as if incorporated by reference alone. In the event of inconsistency between the usage of this article and those documents incorporated by reference, the usage in the incorporated references should be considered to supplement the usage of this article; for irreconcilable inconsistencies, the usage in this article shall prevail.

[0027] In the methods described herein, except when explicitly stating a time or sequence of operations, the actions may be performed in any order without departing from the principles of the present disclosure. In addition, specified actions may be performed simultaneously unless explicit claim language states that they are performed separately. For example, a claimed action of performing X and a claimed action of performing Y may be performed simultaneously in a single operation, and the resulting process will fall within the literal scope of the claimed process.

[0028] As used herein, the term "about" may allow a certain degree of variation in a value or range, for example, within 10%, within 5%, or within 1% of the stated value or limit of the stated range, and includes the exact stated value or range.

[0029] As used herein, the term "substantially" refers to a majority or majority, such as at least about 50%, 60%, 70%, 80%, 90%, 95%, 96%, 97%, 98%, 99%, 99.5%, 99.9%, 99.99%, or at least about 99.999% or more, or 100%.

[0030] As used herein, the term "substantially free" may refer to being free of or having trace amounts such that the amount of material present does not affect the material properties of the composition containing the material, such that about 0% to about 5% by weight of the composition is the material, or about 0% to about 1% by weight, or about 5% by weight or less. Or less than or equal to about 4.5%, 4%, 3.5%, 3%, 2.5%, 2%, 1.5%, 1%, 0.9%, 0.8%, 0.7%, 0.6%, 0.5%, 0.4%, 0.3%, 0.2%, 0.1%, 0.01%, or about 0.001% by weight or less, or about 0% by weight.

[0031] As used herein, the term "compression set" refers to the amount of permanent deformation that occurs when a material is compressed to a specified deformation at a specified temperature for a specified time.

[0032] Aerogel composite synthesis

[0033] The polymers described herein can be terminated in any suitable manner. In some aspects, the polymers can be terminated with terminal groups independently selected from suitable polymerization initiators, -H, -OH, substituted or unsubstituted (C-C) interrupted by 0, 1, 2 or 3 groups independently selected from -O-, substituted or unsubstituted -NH- and -S-. 20 ) hydrocarbon group (e.g., (C1-C 10 )alkyl or (C6-C 20 ) aryl), poly(substituted or unsubstituted (C1-C 20 ) alkyloxy) and poly (substituted or unsubstituted (C1-C 20 )alkylamino).

[0034] According to various aspects presented herein, improved aerogel composite structures with low thermal conductivity at increased density can be prepared, as well as producing optimal pore size and total thickness, and further, the thermal conductivity, maximum stress at 50% strain, and compression set of aerogels that are heated and compressed (as opposed to compressed only) can be controlled. This is primarily due to the disclosed methods including compressing the aerogel composite and heating the aerogel composite.

[0035] Densified aerogels, particularly mechanically densified aerogel composites, can be formed from flexible (non-densified) precursors. Various flexible layers (including flexible fiber-reinforced aerogels) can be easily combined and shaped to obtain preforms that, when mechanically compressed along one or more axes, can obtain a compressively strong body along any of those axes. These densified aerogel bodies exhibit much better insulation values ​​than composite foams. Other composite aerogel properties that benefit from mechanical densification include increased flexural strength and modulus.

[0036] For convenience, the alcohol gel route to form inorganic aerogels is used below to illustrate the present disclosure, but this is not intended to limit the present disclosure to any particular type of aerogel and / or preparation method. The present disclosure is also applicable to other inorganic aerogels, inorganic / organic aerogels and organic aerogels and preparation methods.

[0037] Aerogels and aerogel composites suitable for compression and heating can take a variety of forms, including particle-reinforced, fiber-reinforced, or unreinforced aerogels, any of which contain an organic, inorganic, or hybrid aerogel matrix. An exemplary form is a two-phase aerogel composite, in which the first phase contains a low-density aerogel matrix and the second phase contains a reinforcement material.

[0038] In a simple form of a fiber-reinforced aerogel composite, the fiber material is embedded in a matrix material for a variety of reasons, such as improved mechanical properties. The matrix material can be prepared by a sol-gel method to produce a polymer network (comprising inorganic, organic, or inorganic / organic mixtures). During the sol-gel method, the fiber material is combined with the sol to enhance the matrix material before the polymer gelation point. The aerogel matrix of the preferred precursor material for the present disclosure can be organic, inorganic, or a mixture thereof. The wet gel for preparing aerogels can be prepared by any gel formation technique well known to those skilled in the art: examples include adjusting the pH and / or temperature of a diluted metal oxide sol to a point where gelation occurs (RK Iler, Colloid Chemistry of Silica and Silicates, 1954, Chapter 6; RK Iler, The Chemistry of Silica, 1979, Chapter 5, CJ Brinker and GW Scherer, Sol-Gel Science, 1990, Chapters 2 and 3, which are incorporated herein by reference). Examples of materials used to form inorganic aerogels are metal oxides such as silica-alumina, titania, zirconia, hafnia, yttria, vanadia, etc. In some aspects, the gel can be formed primarily from alcohol solutions of hydrolyzed silicates because of their ready availability and low cost.

[0039] A synthetic route for forming inorganic aerogels is the hydrolysis and condensation of appropriate metal alkoxides. The most suitable metal alkoxides are those having about 1 to 6 carbon atoms, 1 to 4 carbon atoms in each alkyl group. Specific examples of such compounds include tetraethoxysilane (TEOS), tetramethoxysilane (TMOS), tetra-n-propoxysilane, aluminum isopropoxide, aluminum sec-butoxide, cerium isopropoxide, hafnium tert-butoxide, magnesium aluminum isopropoxide, yttrium isopropoxide, titanium isopropoxide, zirconium isopropoxide, etc. With regard to silica precursors, these materials can be partially hydrolyzed and stabilized as polymers of polysilicates at low pH, such as polydiethoxysiloxane. These materials can be commercially available in the form of alcohol solutions. For aerogel composites described herein, prepolymerized silica precursors are also preferred.

[0040] Some variables in the inorganic aerogel formation process include the type of alkoxide, solution pH, and alkoxide / alcohol / water ratio. Control of the variables allows control of the growth and aggregation of the matrix material throughout the transition from the "sol" state to the "gel" state. Although the properties of the resulting aerogel are strongly affected by the pH of the precursor solution and the molar ratio of the reactants, any pH and any molar ratio that allows gel formation can be used in these aspects.

[0041] Typically, the solvent used in these methods is a lower alcohol, such as an alcohol having 1 to 6 carbon atoms, preferably 2 to 4 carbon atoms, but other liquids known in the art may also be used. Examples of other useful liquids include, but are not limited to, ethyl acetate, ethyl acetoacetate, acetone, methylene chloride, and the like.

[0042] Any of the following methods can be used to prepare precursor aerogel composite products, but what is needed is a method that allows the lowest density and / or the best insulation products to be obtained. For example, in a first alternative embodiment of gel preparation, a water-soluble alkaline metal oxide precursor can be gelled by acidification in water to make a hydrogel. Sodium silicate has been widely used for this purpose. Salt byproducts can be removed from the silicic acid precursor by ion exchange and / or by washing the subsequently formed gel with water. Water in the gel pores can be removed by exchange with polar organic solvents such as ethanol, methanol or acetone. The structure of the resulting dry aerogel is similar to that directly formed by supercritical extraction of a gel prepared in the same organic solvent. The second alternative method requires chemical modification of the matrix material in the wet gel state by converting the surface hydroxyl groups into trimethylsilyl ethers, thereby reducing the destructive capillary pressure at the solvent / pore interface (see, for example, U.S. Patent No. 5,877,100) to allow the aerogel material to be dried at a temperature and pressure below the critical point of the solvent.

[0043] Methods for drying gels to produce aerogels or xerogels are well known. Kistler (J. Phys. Chem., 36, 1932, 52-64) describes a drying method in which the gel solvent is kept above its critical pressure and temperature. Since there is no capillary force, such supercritical drying maintains the structural integrity of the gel. U.S. Patent No. 4,610,863 describes a method in which the gel solvent is exchanged with liquid carbon dioxide and then dried under conditions in which the carbon dioxide is in a supercritical state. Such conditions are milder than those described by Kistler. U.S. Patent No. 6,670,402 teaches the use of supercritical CO2 for drying by rapid solvent exchange of the solvent in the wet gel, by injecting supercritical (rather than liquid) CO2 into an extractor that has been preheated and pre-pressurized to substantially supercritical conditions or higher conditions to produce aerogels. U.S. Patent No. 5,962,539 describes a method for obtaining an aerogel from a polymer material in sol-gel form in an organic solvent by exchanging the organic solvent for a fluid having a critical temperature below the decomposition temperature of the polymer and supercritically drying the fluid / sol-gel. U.S. Patent No. 6,315,971 discloses a method for preparing a gel composition, comprising: drying a wet gel comprising gel solids and a desiccant under drying conditions sufficient to minimize shrinkage of the gel during drying to remove the desiccant. In addition, U.S. Patent No. 5,420,168 describes a method in which a resorcinol / formaldehyde aerogel can be made using a simple air drying procedure. U.S. Patent No. 5,565,142 describes a method in which the surface of the gel is modified to make it more hydrophobic and stronger so that it can resist any collapse of the structure during ambient or subcritical drying. The surface-modified gel is dried at ambient pressure or a pressure below the critical point (subcritical drying). The product obtained from such ambient pressure or subcritical drying is generally referred to as a xerogel.

[0044] Organic aerogels can be made from polyacrylates, polystyrene, polyacrylonitrile oxide, polyacrylonitrile, polyurethane, polyimide, polyfurfuryl alcohol, phenol furfuryl alcohol, melamine formaldehyde, resorcinol formaldehyde, cresol formaldehyde, phenol formaldehyde, polyvinyl dialdehyde, polycyanurate, polyacrylamide, various epoxy resins, agar, agarose, etc. (see, for example, CS Ashley, CJ Brinker and DM Smith, Journal of Non-Crystalline Solids, Vol. 285, 2001).

[0045] Suitable materials for preparing aerogels for use at low temperatures include non-refractory metal alkoxides based on metals that form oxides. Examples of such metals are silicon and magnesium and mixtures thereof. For higher temperature applications, suitable alkoxides are typically refractory metal alkoxides that will form oxides, for example, such as zirconium oxide, yttrium oxide, hafnium oxide, aluminum oxide, titanium dioxide, cerium dioxide, etc., and mixtures thereof, such as zirconium oxide and yttrium oxide. Mixtures of non-refractory metals and refractory metals, such as mixtures of silicon and / or magnesium with aluminum, may also be used. The advantage of using more than one metal oxide matrix material for aerogel structures is that IR opacity is enhanced, which is achieved by providing chemical functional groups that absorb radiation over a wider wavelength range. In addition, finely dispersed dopants such as carbon black, titanium dioxide, iron oxide, silicon carbide, molybdenum silicide, manganese oxide, polydialkylsiloxanes in which the alkyl group contains 1 to 4 carbon atoms, etc., may be added to improve thermal performance at higher temperatures by increasing the opacity of the article to IR transmission. Suitable amounts of such dopants are generally in the range of about 1 wt % to 40 wt % or about 2 wt % to 10 wt % of the finished composite.

[0046] In the aforementioned fiber-reinforced aerogel composite material, the reinforcing component may be a fiber reinforcement material, which is a bulky fiber structure (flocculent or web), but may also include individual randomly oriented short microfibers, as well as woven or non-woven fibers. More specifically, suitable fiber reinforcement materials are based on organic (e.g., thermoplastic polyester, high-strength carbon, aromatic polyamide, high-strength oriented polyethylene, etc.), low-temperature inorganic (e.g., metal oxide glass, such as E-glass) or refractory (e.g., silica, alumina, aluminum phosphate, aluminosilicate, etc.) fibers. Typically, the fibers may be inorganic fibers, organic fibers, particles, metal fibers, metal meshes, or mixtures thereof.

[0047] In some specific examples, the fiber can be polyethylene terephthalate. The polyethylene terephthalate can be a bicomponent polyethylene terephthalate fiber comprising an inner core and an outer core, wherein the melting temperature of the inner core is higher than the melting temperature of the outer core.

[0048] In some aspects, inorganic (e.g., alumina, metal) foams or organic foams (e.g., melamine) can be used in any of the sol chemistries described above to produce foam-reinforced aerogel composites. The sol and reinforcing foam can be combined and synthesized into a foam-reinforced composite using any of the sol chemistries and processing techniques described above in the context of fiber-reinforced aerogel composites.

[0049] The reinforcing component may range from about 5 wt % to about 75 wt %, from about 25 wt % to about 50 wt %, or from about 30 wt % to about 40 wt % of the aerogel composite.

[0050] The mechanical loads borne by the composite aerogel can be transferred to the fasteners and into other structures through the tough fabric layer. The mechanical load can be initially borne by the fabric layer and then transferred to the aerogel composite. An example of this is to fasten the aerogel composite to the vehicle chassis or other vehicle parts that can withstand force (e.g., the interior of the body panel, firewall, engine bracket, battery / battery pack housing) to serve as a thermal barrier. The method for producing the densified nanoporous body in this aspect does not require densification before installation in the application environment. The non-mechanically densified aerogel composite can be fixed to the body by fixing means (adhesive, tape, fasteners, etc.), and then physically compressed to mold the now mechanically densified nanoporous body into the shape of the product. This is a significant advantage for manufacturing insulating or protected products with the smallest possible volume or cross-sectional area.

[0051] In the above-described aerogel composites, an increase in density can be broadly defined as a measurable increase in density, such as an increase in the density of the aerogel composite by a factor of 2 to 20 or a factor of 3 to 10 relative to an aerogel composite that is neither compressed nor heated. In these aspects, the density referred to is the "encapsulated" density of the reinforced aerogel composite. Other types of density measurements, such as the "skeleton" density of an unreinforced aerogel material, may be described in other contexts.

[0052] The composite material produced can be flexible, durable, and have low thermal conductivity and good resistance to sintering. The performance of aerogel composites can be significantly enhanced by incorporating randomly distributed microfibers into the composite material, especially microfibers that help resist sintering while increasing durability and reducing dust. The effect of short fiber reinforcement (microfiber) on the performance of the composite material will depend on many variables, such as fiber arrangement, diameter, length, aspect ratio (fiber length / fiber diameter), strength, modulus, failure strain, thermal expansion coefficient, and interfacial strength between fiber and matrix. The microfibers are incorporated into the composite material by dispersing the microfibers in a gel precursor liquid and then using the liquid to infiltrate bulking flocs.

[0053] Suitable microfibers that can be used in the present invention typically have diameters in the range of 0.1 μm to 100 μm, have high aspect ratios (L / d>5 or L / d>100), and are relatively evenly distributed throughout the composite material. Since a higher aspect ratio can improve the performance of the composite material, the longest microfibers may be required. However, the length of the fibers used herein is limited to avoid (or at least minimize) being filtered by the selected bulky flocs when the gel precursor containing the microfibers is injected into the flocs. The microfibers should be short enough to minimize the filtration of the bulky flocs, and should be long enough to have the greatest possible effect on the thermal and mechanical properties of the resulting composite material. The microfibers may have a thermal conductivity of 200 mW / mK or less to promote the formation of low thermal conductivity aerogel composites.

[0054] When the microfibers are dispersed in the sol, they usually settle rapidly. To overcome this problem, a suspending agent or dispersing agent that does not adversely affect gel formation should be added to the sol. Suitable suspending agents / dispersing agents include solutions of high molecular weight block copolymers with pigment-affinity groups (Disperbyk-184 and 192 from BYK-Chemie), etc. The agent needs to be effective at least during the time period between the dispersion of the microfibers in the gel precursor and the gelation of the sol.

[0055] The number, type and / or size and aspect ratio of the microfibers used in a particular aerogel composite can be varied to meet a particular task. For example, an application may involve using a continuous aerogel composite to isolate zones of different temperatures; the composite may be manufactured such that more microfibers will be present in the areas of the composite that will contact the higher temperature zones. Similarly, different microfibers (e.g., different materials, different aspect ratios, sizes) may be combined in these areas to obtain optimal insulation performance. Such microfiber modifications may be achieved by using various suspending agents and / or microfibers so that the microfibers settle into the composite at different rates and thus settle to different locations.

[0056] Suitable fiber materials for forming the bulky batt and the xy-oriented tensile reinforcement layer include any fiber-forming material. Particularly suitable materials include: glass fiber, quartz, polyester (PET), polyethylene, polypropylene, polybenzimidazole (PBI), polyphenylene benzobisoxazole (PBO), polyetheretherketone (PEEK), polyarylate, polyacrylate, polytetrafluoroethylene (PTFE), polymethylene amine (Nomex), polyparaphenylene terephthalamide (Kevlar), ultra-high molecular weight polyethylene (UHMWPE) such as Spectra TM , phenolic resin (Kynol), polyacrylonitrile (PAN), PAN / carbon and carbon fiber.

[0057] The aerogel composite material may include one or more additives. For example, the aerogel composite material may include boron carbide [B4C], diatomaceous earth, manganese ferrite, MnO, NiO, SnO, Ag2O, Bi2O3, carbon black, titanium oxide, titanium iron oxide, aluminum oxide, zirconium silicate, zirconium oxide, iron (II) oxide, iron (III) oxide, manganese dioxide, titanium iron oxide (ilmenite), chromium oxide, SiC, TiC or WC, TiOSO4, TiOCl2, or mixtures thereof. The concentration of the additive may be in the range of about 0.05 wt % to about 10 wt % of the aerogel composite material or about 1 wt % to about 7 wt % of the aerogel composite material.

[0058] Aerogels processed by simultaneous heating and compression

[0059] In various aspects, the composite material produced by the aerogel composition that is simultaneously heated during compression has a lower thermal conductivity and a more uniform thickness than an equivalent composite material that is not compressed at all and / or is not heated during the compression operation. More specifically, various aspects of the composite aerogel that is heated during compression have a standard deviation of the mean thickness that can be half or one-quarter the standard deviation of the equivalent material that is compressed but not heated. Additionally, in various aspects, the composite material produced by the aerogel composition that is simultaneously heated during compression has a higher maximum stress at 50% strain than an equivalent composite material that is not compressed at all and / or is not heated during the compression operation.

[0060] Additionally, in various aspects, aerogel compositions that are simultaneously heated during compression produce composite materials having higher compressive strain values ​​than equivalent composite materials that are not compressed at all and / or not heated during the compression operation.

[0061] Additionally, in various aspects, aerogel compositions that are simultaneously heated during compression produce composite materials having higher compression set values ​​than equivalent composite materials that are not compressed at all and / or not heated during the compression operation.

[0062] As shown in the Examples, in many applications, the standard deviation of the values ​​obtained is lower than that of a comparative aerogel composite that is only compressed (e.g., not compressed and heated). This means that the resulting aerogel composite can not only have these desired properties, but also have a degree of control over these properties that cannot be achieved through compression alone. This degree of control is beneficial to the general processing and specific applications of aerogel composites, such as electric vehicle battery compartments or other devices with low error tolerances. For example, when using automated assembly systems such as industrial robots to assemble multi-component battery packs, dimensional variations may cause manufacturing system failures. In some examples, poor dimensional control may lead to electrolyte pooling (insufficient external pressure on the lithium-ion battery cell due to the component being too thin) or cell rupture (excessive external pressure on the lithium-ion battery cell due to the component being too thick)

[0063] Aerogel composites can be formed using a hydraulic press.

[0064] Figure 1 A typical hydraulic press is shown, which can be used for mechanical pressing and has two press plates 100, wherein a compressive force F is applied to the press plates by at least one hydraulic press cylinder unit at the location where the cylinder unit is connected to the press plates. The press plates are guided laterally and can be braked by counter-support means. Alternatively, one press plate can be fixed. Thus, the aerogel 102 is positioned between the press plates 100 and is then compressed.

[0065] Densification, on the other hand, is achieved by local compression, which is provided by the continuous action of counter-rotating rollers, the gap (between the rollers) of which is much smaller than the thickness of the uncompressed composite aerogel. Therefore, as the aerogel composite passes through the gap, local compression of the aerogel composite is applied, resulting in a significant increase in density.

[0066] The previously discussed aerogels may also be densified by passing them between at least one pair of rollers to form a sheet having a reduced but more uniform thickness and a generally smoother surface. The term "densification" refers to the process of compressing an aerogel and / or an aerogel composite. In this particular aspect, the compression is performed by passing the aerogel and / or aerogel composite between one or more sets of rollers to densify the resulting product. If a series of rollers is used, the roller pairs have gradually narrowing gaps between them so as to produce gradually denser aerogels and / or aerogel composites, and may also have various patterns on their surfaces.

[0067] The rollers may be treated to prevent adhesion between the aerogel and / or aerogel composite and the rollers. This may be accomplished by coating the rollers with a non-stick substance, polishing the rollers, heating the rollers to form a vapor barrier, cooling the rollers to form a condensation barrier, or a combination of these.

[0068] In one aspect, Figure 2 As shown, it is desirable to "densify" the aerogel or aerogel composite by passing the aerogel or aerogel composite between at least one pair of rollers, with the goal of improving the thermal and / or mechanical properties of the aerogel or aerogel composite by densification. In some aspects, the densification step will only densify the aerogel or aerogel composite by a small amount. In other cases, the densification process will densify the aerogel or aerogel composite substantially. In cases where it is necessary to densify the aerogel or aerogel composite substantially, it is generally necessary to densify the aerogel or aerogel composite in steps, wherein the aerogel or aerogel composite passes through several pairs of rollers, each pair of rollers having a gradually narrowing gap distance between them.

[0069] Should refer to Figure 2 , which shows an example where at least one pair of rollers 202 are used during the densification step. It should be understood that more than one pair of rollers may be needed to achieve the desired densification. When more than one pair of rollers is used, the rollers within each pair may have similar diameters, but in some cases it may be preferable to use a combination of smaller diameter rollers and larger diameter rollers. Figure 2 As shown, a set or pair of rollers generally includes two individual rollers 202 positioned adjacent to each other with a predetermined gap distance therebetween. The gap distance between the two individual rollers corresponds to the desired densification 204 of the aerogel 200 after passing between the set of rollers.

[0070] The pressure applied by the press or roller used can be in the range of about 500 kPa to about 1000 kPa, about 700 kPa to about 1000 kPa, less than, equal to or greater than about 500 kPa, 600 kPa, 700 kPa, 800 kPa, 900 kPa or about 1000 kPa. Throughout the process, the pressure can be constant or can vary. The amount of time for pressing can be about 0.2 hours to about 24 hours, about 2 hours to about 15 hours or about 5 hours to about 10 hours.

[0071] In one aspect of the present disclosure, the aerogel composite is heated during compression. Figure 1 and Figure 2 denoted by "D" in the figure. As non-limiting examples, the aerogel composite material can be heated to a temperature in the range of about 80°C to about 700°C, about 90°C to about 650°C, or 500°C to about 600°C, or even as low as about 90°C to about 110°C. Heating can occur simultaneously with compression or after compression. Heating can also occur at a constant temperature or over a temperature gradient. Heating can be one cycle or multiple heating cycles. Typically, the compression equipment itself is heated, which can transfer heat to the aerogel composite material.

[0072] It has been found that if the aerogel composite is simultaneously heated and compressed as described above, the size of the pores in the aerogel composite can be carefully controlled. Specifically, it has been found that the majority (e.g., greater than 50% of the total number of pores) can have a major (e.g., largest) diameter of less than about 50 nm, less than about 40 nm, less than about 30 nm, less than about 20 nm, in the range of about 10 nm to about 50 nm, or about 20 nm to about 40 nm, as measured perpendicular to a plane of a major surface of the aerogel composite. Pores within these ranges can provide optimal low thermal conductivity. That is, pores within these ranges can rapidly reduce the ability of convective heat transfer through the pores. If the pores are too small, this cannot be achieved. However, if the pores are not small enough, the aerogel must be densified to the extent that one desires to increase conductive heat transfer.

[0073] The individual holes can take many different shapes or profiles. For example, the hole can have an elongated profile. An elongated profile can be understood as a generally non-spherical or elliptical profile. In some aspects, the profile of the individual holes can be circular before compression and then elongate during compression.

[0074] After pressing and heating, the average thickness of the final aerogel composite is in the range of about 0.1 mm to about 1.5 mm, about 0.1 mm to about 0.6 mm, 0.1 mm to about 0.5 mm, or about 0.2 mm to about 0.4 mm. The strain of the aerogel composite after its production is in the range of about 5% to about 40%, about 10% to about 30%, or about 15% to about 20% of the total thickness of the aerogel composite. As understood herein, "strain" refers to the deformation caused by the compression of the heat treated and compressed aerogel composite.

[0075] The thermal conductivity of the final aerogel composite can be in the range of about 13 milliwatts / meter-Kelvin (mW / mK) to about 60 mW / mK, about 15 mW / mK to about 55 mW / mK, about 20 mW / mK to about 50 mW / mK, about 25 mW / mK to about 45 mW / mK, about 30 mW / mK to about 40 mW / mK.

[0076] Without wishing to be bound by any theory, it is believed that heating in addition to compression allows the formation of the disclosed aerogel composites having the disclosed thickness, pore size and thermal conductivity. Specifically, it is believed that it is impossible to achieve these values ​​by simply compressing the aerogel composite without simultaneously applying heat. This is because the reinforcing component (e.g., the fiber reinforcing component) will tend to plastically deform to compensate and / or elastically release some / most of the applied compression in response to the applied stress. The release of compression (equivalent to elasticity in the composite) can come from the resilience caused by twisting in the yarn reinforcement; the natural resilience / elasticity from the available and variable free space between fibers in nonwoven fabrics, which allows the fibers to move in response to the applied compressive stress; and / or the natural resilience / elasticity in woven fabrics. As recognized by the present disclosure, adding a heating step simultaneously with the compressive force can overcome these problems. The benefits of combining heating and compression can include that the thickness of the reinforced aerogel that is heated and compressed at the same time has higher accuracy, consistency and uniformity than the same reinforced aerogel composite compressed without heating.

[0077] Without wishing to be bound by any theory, a mechanism that may contribute to these advantages is that heating the reinforcing component to above the glass transition temperature (for polymers) or other activation temperature may allow the compression state to be maintained after the pressure is released. As an example, the reinforcing component may include a bicomponent fiber (e.g., polyethylene terephthalate) comprising an inner core and an outer core, wherein the melting temperature of the inner core is higher than the melting temperature of the outer core. In such a configuration, the aerogel composite material may be heated to a melting temperature higher than the outer core, so that the inner core remains intact, while the outer core adheres to the gel. Without intending to be bound by any theory, another explanation is that favorable properties may be achieved because heat causes a reaction between surface groups covalently bonded to the aerogel surface (e.g., silanol condensation in a hydrophobe), which prevents the release of the strain applied in the aerogel.

[0078] With specific reference to the improvement in thermal conductivity relative to aerogel composites that are merely compressed, and without wishing to be bound by any theory, the distribution of pore sizes may be altered. By reducing the proportion of macropores (e.g., pores with diameters greater than 50 nm), the ability of gas molecules to diffuse through the porous aerogel structure may be reduced, thereby further reducing the thermal conductivity of the composite. Additionally, compressing aerogel composites (other than as described herein) may result in an undesirable increase in aerogel density, which would increase solid conductive paths in such aerogels.

[0079] As shown in the examples herein, aerogels subjected only to compression can provide suitable properties. However, compression and heating can generally improve the properties of aerogels. As also shown, the thickness of the aerogel can be carefully controlled to produce an aerogel with desired properties. The thickness control and resulting properties of aerogels subjected to both compression and heating are unexpected to those of ordinary skill in the art relative to corresponding aerogels subjected only to compression.

[0080] Example

[0081] Various aspects of the present disclosure may be better understood by reference to the following examples which are provided by way of illustration.The present disclosure is not limited to the examples given herein.

[0082] Example 1

[0083] Composite aerogels with a thickness of 4.5 mm, SiC gels and quartz fiber reinforcement components aged in 0.1 M TMS were prepared. Various properties of the composite aerogels were studied.

[0084] Figure 3 is a graph showing the thermal conductivity of gels used for aerogel composites at different compression levels. As shown, when the aerogel composite is compressed to a density of 0.034 g / cc to 0.079 g / cc, the thermal conductivity at high temperature decreases.

[0085] Figure 4 is a graph showing the relationship between thermal performance and stress for the composite aerogel of Example 1. As shown, the thermal conductivity of the aerogel composite material decreases when exposed to a pressure of 4300 kPa.

[0086] Figure 5 is a graph showing the thermal conductivity at various temperatures of the composite aerogel of Example 1. As shown, the aerogel composite compressed at 11% and 31% strains shows an improvement in thermal conductivity relative to the uncompressed aerogel composite.

[0087] Fig. 6A is a graph showing the reduction in thermal conductivity of composite aerogels having a permanent strain of less than 41%.

[0088] Figure 6B is a graph showing the average pore size at different degrees of permanent strain for the composite aerogel of Example 1. As shown, the pore size can be controlled, however, when the strain exceeds 31%, the pores may become too small.

[0089] Figure 7 is a graph showing the pore size distribution of the composite aerogel under different degrees of permanent strain of Example 1. As shown in the figure, the average pore size decreases as the permanent strain increases.

[0090] Figure 8is a graph showing a finite fraction of the applied strain that remains in an aerogel composite when a compressive strain is applied.

[0091] Fig.9A It is shown that lower silica density and higher compressive strain in aerogel composites are associated with higher plastic strain in aerogel composites.

[0092] Fig. 9B It was shown that the hydrophobic content (covalently bonded to the silica aerogel in the reinforced silica aerogel composite) is another parameter that can change the amount of plastic deformation retained in the aerogel composite in response to compressive strain.

[0093] Example 2

[0094] A composite aerogel was prepared comprising octadecyltrimethoxysilane on partially oxidized polyacrylonitrile. The initial density of the aerogel was 0.0825 g / cc and the initial thickness was 2 mm. Density refers to the grams of silica per unit volume of gel. The target thickness after compression and / or heating was 1.45 mm.

[0095] The aerogels were first compressed without heating to obtain a thickness of 1.716 mm with a thickness standard deviation of 0.0998 mm. In contrast, when the aerogels were compressed and heated, the thickness was 1.62 mm with a thickness standard deviation of 0.05 mm. This shows that compression and heating together can produce a suitable thickness, with a certain degree of control in obtaining the target thickness, and reduced thickness variability, as indicated by the standard deviation, which is about half of the standard deviation of the unheated compressed samples. Reducing dimensional (e.g., thickness) variability is important when using aerogel compositions in precision-manufactured components (such as automotive battery packs), where dimensional tolerances are typically in the millimeter or sub-millimeter range. All of this is unexpected relative to aerogels that have only been compressed. Thickness values ​​were measured 24 hours after formation.

[0096] In order to better understand the physical properties of the formed aerogels, the maximum stress at 50% strain was measured for the compressed aerogel and the compressed and heated aerogel. The value of the compressed aerogel was 1195.67 kPa, and the standard deviation of the maximum stress at 50% strain was 180.8. The value of the compressed and heated aerogel was 1841.33 kPa, and the standard deviation of the maximum stress at 50% strain was 426.08. This shows that both gels can achieve suitable strength, but in particular, the compressed and heated aerogel can show excellent and unexpected strength.

[0097] The compression set values ​​of the compressed aerogel and the compressed and heated aerogel were measured. The results showed that the compression set of the compressed aerogel was 45.3550% with a compression set standard deviation of 5.72, and the compression set of the compressed and heated aerogel was 50.01383% with a compression set standard deviation of 4.64. This shows that the inelastic strain components between the gels are statistically the same, but compression alone does not produce the unexpected benefits mentioned in this article.

[0098] The thermal conductivity of the compressed aerogel and the compressed and heated aerogel was measured. The results showed that the thermal conductivity of the compressed aerogel was 16.011 mW / mK, and the standard deviation of the thermal conductivity was 0.0341. The thermal conductivity of the compressed and heated aerogel was 16.089 mW / mK, and the standard deviation of the thermal conductivity was 0.377. This shows that the thermal conductivity between the gels is statistically the same, but compression alone does not produce the unexpected benefits mentioned in this article.

[0099] Example 3

[0100] A composite aerogel was prepared comprising octadecyltrimethoxysilane on partially oxidized polyacrylonitrile. The initial density of the aerogel was 0.0825 g / cc and the initial thickness was 2 mm. Density refers to the grams of silica per unit volume of gel. The target thickness after compression and / or heating was 0.92 mm.

[0101] The aerogel was first compressed without heating to obtain a thickness of 1.105 mm with a thickness standard deviation of 0.0549 mm. In contrast, when the aerogel was compressed and heated, the thickness was 1.038 mm with a thickness standard deviation of 0.055 mm. This indicates that compression and heating together can produce a suitable thickness that is less than that produced by compression alone. The improvement in dimensional control (producing thinner samples) relative to aerogels that have only been compressed would be unexpected. The thickness values ​​were measured 24 hours after formation.

[0102] In order to better understand the physical properties of the formed aerogels, the maximum stress at 50% strain was measured for the compressed aerogel and the compressed and heated aerogel. The value of the compressed aerogel was 8780.8 kPa, and the standard deviation of the maximum stress at 50% strain was 1107.10. The value of the compressed and heated aerogel was 10689.8 kPa, and the standard deviation of the maximum stress at 50% strain was 1321.21. This shows that both gels can achieve suitable strength, but in particular, the compressed and heated aerogel can show excellent and unexpected strength.

[0103] The compression set values ​​of the compressed aerogels and the compressed and heated aerogels were determined. The results showed that the compression set of the compressed aerogels was 61.7% with a compression set standard deviation of 4.32, and the compression set of the compressed and heated aerogels was 67.5% with a compression set standard deviation of 1.38. This shows that the inelastic strain components between the gels are statistically close to the same, but compression alone does not produce the unexpected benefits mentioned in this article. In fact, it shows that compression and heating together can provide higher compression set values ​​and lower standard deviation values.

[0104] The thermal conductivity of the compressed aerogel and the compressed and heated aerogel was measured. The results showed that the thermal conductivity of the compressed aerogel was 19.45 mW / mk, with a standard deviation of 0.56. The thermal conductivity of the compressed and heated aerogel was 19.67 mW / mk, with a standard deviation of 0.90. This shows that the thermal conductivity between the gels is statistically the same, but compression alone does not produce the unexpected benefits mentioned in this article.

[0105] Example 4

[0106] A composite aerogel was prepared comprising octadecyltrimethoxysilane on partially oxidized polyacrylonitrile. The initial density of the aerogel was 0.0825 g / cc and the initial thickness was 1 mm. Density refers to the grams of silica per unit volume of gel. The target thickness after compression and / or heating was 0.46 mm.

[0107] The aerogels were first compressed without heating, achieving a thickness of 0.60 mm with a thickness standard deviation of 0.041 mm. In contrast, when the aerogels were compressed and heated, the thickness was 0.60 mm with a thickness standard deviation of 0.042 mm. This shows that performing compression and heating together can produce the right thickness, with a degree of control in achieving the target thickness as well as a better standard deviation. All of this was unexpected relative to aerogels that were only compressed. The thickness values ​​were measured 24 hours after formation.

[0108] In order to better understand the physical properties of the formed aerogels, the maximum stress at 50% strain was measured for the compressed aerogel and the compressed and heated aerogel. The value of the compressed aerogel was 20728.7 kPa, and the standard deviation of the maximum stress at 50% strain was 5204.5. The value of the compressed and heated aerogel was 23073.5 kPa, and the standard deviation of the maximum stress at 50% strain was 9828.5. This shows that both gels can achieve suitable strength, but in particular, the compressed and heated aerogel can show excellent and unexpected strength.

[0109] The compression set values ​​of the compressed aerogel and the compressed and heated aerogel were measured. The results showed that the compression set of the compressed aerogel was 56.9%, the standard deviation of the compression set was 17.9, and the compression set of the compressed and heated aerogel was 29.13%, the standard deviation of the compression set was 15.58.

[0110] The thermal conductivity of the compressed aerogel and the compressed and heated aerogel was measured. The results showed that the thermal conductivity of the compressed aerogel was 15mW / mK, with a standard deviation of thermal conductivity of 1.9. The thermal conductivity of the compressed and heated aerogel was 12mWmK, with a standard deviation of thermal conductivity of 2.7. This shows that the thermal conductivity between the gels is statistically the same, but compression alone does not produce the unexpected benefits mentioned in this article.

[0111] Example 5

[0112] A composite aerogel was prepared comprising octadecyltrimethoxysilane on partially oxidized polyacrylonitrile. The initial density of the aerogel was 0.0425 g / cc and the initial thickness was 2 mm. Density refers to the grams of silica per unit volume of gel. The target thickness after compression and / or heating was 0.92 mm.

[0113] The aerogels were first compressed without heating, achieving a thickness of 1.31mm with a thickness standard deviation of 0.095mm. In comparison, when the aerogels were compressed and heated, the thickness was 1.07mm with a thickness standard deviation of 0.056mm. This shows that compressing and heating together can produce the right thickness, with a degree of control in achieving the target thickness as well as better standard deviations, which are an order of magnitude better. All of this is unexpected relative to aerogels that were only compressed. The thickness values ​​were measured 24 hours after formation.

[0114] In order to better understand the physical properties of the aerogels formed, the maximum stress at 50% strain was measured for the compressed aerogel and the compressed and heated aerogel. The value of the compressed aerogel was 800.667 kPa, and the maximum stress at 50% strain standard deviation was 288.70. The value of the compressed and heated aerogel was 413.66 kPa, and the maximum stress at 50% strain standard deviation was 72.67. This shows that both gels can achieve suitable strength, but in particular, the compressed and heated aerogel can show excellent and unexpected strength. In addition, the compressed and heated gel is a less stressed material. In addition, the standard deviation between heating and compression and compression alone is much smaller, indicating a higher degree of control.

[0115] The compression set values ​​of the compressed aerogel and the compressed and heated aerogel were measured. The results showed that the compression set of the compressed aerogel was 30.5% with a compression set standard deviation of 6.048, and the compression set of the compressed and heated aerogel was 13.2% with a compression set standard deviation of 2.4. This shows that compressing and heating together can provide the desired lower compression set values ​​and better control, as indicated by the lower standard deviation.

[0116] The thermal conductivity of the compressed aerogel and the compressed and heated aerogel was measured. The results showed that the thermal conductivity of the compressed aerogel was 19.24 mW / mK, with a standard deviation of thermal conductivity of 0.41. The thermal conductivity of the compressed and heated aerogel was 18.54 mW / mK, with a standard deviation of thermal conductivity of 0.49. This shows that the thermal conductivity between the gels is statistically the same, but compression alone does not produce the unexpected benefits mentioned in this article.

[0117] Example 6

[0118] A composite aerogel was prepared comprising octadecyltrimethoxysilane on partially oxidized polyacrylonitrile. The initial density of the aerogel was 0.0425 g / cc and the initial thickness was 2 mm. Density refers to the grams of silica per unit volume of gel. The target thickness after compression and / or heating was 0.46 mm.

[0119] The aerogels were first compressed without heating to obtain a thickness of 0.85 mm with a thickness standard deviation of 0.011 mm. In contrast, when the aerogels were compressed and heated, the thickness was 0.62 mm with a thickness standard deviation of 0.08 mm. This shows that performing compression and heating together can produce the appropriate thickness, with a degree of control in achieving the target thickness that is unexpected relative to aerogels that have only been compressed. The thickness values ​​were measured 24 hours after formation.

[0120] The thermal conductivity of the compressed aerogel and the compressed and heated aerogel was measured. The results showed that the thermal conductivity of the compressed aerogel was 22.5 mW / mK, and the standard deviation of the thermal conductivity was 0.227. The thermal conductivity of the compressed and heated aerogel was 23.1 mW / mK, and the standard deviation of the thermal conductivity was 0.171. This shows that the thermal conductivity between the gels is statistically the same, but compression alone does not produce the unexpected benefits mentioned in this article.

[0121] In the foregoing examples, thermal conductivity was measured using ASTM C518. In the foregoing examples, stress, strain, and compression were determined using ASTM E3574. Statistical analyses were performed using a computer program called JMP 17 available from JMP Statistical Discovery LLC, Cary NC.

[0122] The terms and expressions used are used as descriptive terms rather than limiting terms, and when using these terms and expressions, it is not intended to exclude any equivalents of the features shown and described or parts thereof, but it is recognized that various modifications can be made within the scope of the various aspects of the present disclosure. Therefore, it should be understood that although the present disclosure has been specifically disclosed through specific aspects and optional features, those of ordinary skill in the art may make modifications and changes to the concepts disclosed herein, and such modifications and changes are considered to be within the scope of the aspects of the present disclosure.

[0123] Exemplary Aspects

[0124] The following exemplary aspects are provided, the numbering of which should not be construed as designating a level of importance:

[0125] Aspect 1 provides a method for preparing an aerogel composite material, the method comprising:

[0126] compressing and heating the aerogel composite, the aerogel composite comprising a gel dispersed around a reinforcing component;

[0127] as well as

[0128] A compressed and heated aerogel composite material is prepared, wherein the prepared aerogel composite material contains a plurality of pores, wherein the diameters of most of the pores are less than 50 nm.

[0129] Aspect 2 provides the method of aspect 1, wherein the gel comprises a metal oxide compound.

[0130] Aspect 3 provides the method of aspect 2, wherein the metal oxide compound comprises silicon dioxide, aluminum oxide, titanium dioxide, ceria, yttrium oxide, or any combination thereof.

[0131] Aspect 4 provides the method of any one of aspects 2 or 3, wherein the metal oxide compound comprises silicon dioxide.

[0132] Aspect 5 provides the method of any one of aspects 1 to 4, wherein the reinforcing component comprises a nonwoven material, a woven material, a fluffy batting, a fibrous batting, or any combination thereof.

[0133] Aspect 6 provides the method of any one of aspects 1 to 5, wherein the reinforcing component comprises inorganic fibers, organic fibers, particles, metal fibers, metal mesh, organic foam, or a mixture thereof.

[0134] Aspect 7 provides the method of aspect 6, wherein the inorganic fiber comprises glass fiber or ceramic fiber.

[0135] Aspect 8 provides the method of any of aspects 6 or 7, wherein the organic fiber comprises polyethylene, oxidized polyacrylonitrile, polyacrylonitrile, polyethylene terephthalate, or a mixture thereof.

[0136] Aspect 9 provides the method of aspect 8, wherein the reinforcing component comprises a biconstituent polyethylene terephthalate fiber comprising an inner core and an outer core, wherein the inner core has a higher melting temperature than the outer core.

[0137] Aspect 10 provides the method of any one of aspects 6 to 9, wherein the organic foam comprises melamine.

[0138] Aspect 11 provides the method of any of aspects 1 to 10, wherein the reinforcing component is in the range of about 5 wt % to about 75 wt % of the aerogel composite.

[0139] Aspect 12 provides the method of any of aspects 1 to 11, wherein the reinforcing component is in the range of about 25 wt % to about 50 wt % of the aerogel composite.

[0140] Aspect 13 provides the method of any one of aspects 1 to 12, wherein the density of the aerogel composite is increased up to 20 times relative to the gel before compression.

[0141] Aspect 14 provides the method of any one of aspects 1 to 13, wherein the density of the aerogel composite is increased up to 10 times relative to the gel before compression.

[0142] Aspect 15 provides the method of any one of aspects 1 to 14, wherein the compressing and heating are performed simultaneously.

[0143] Aspect 16 provides the method of any one of aspects 1 to 14, wherein heating is performed after compressing.

[0144] Aspect 17 provides the method of any one of aspects 1 to 16, wherein the compression comprises mechanical compression or air compression.

[0145] Aspect 18 provides the method of aspect 17, wherein the mechanical compression is performed using a compression device.

[0146] Aspect 19 provides the method of aspect 18, wherein the compression device comprises a press, a roller, or both.

[0147] Aspect 20 provides the method of any of aspects 18 or 19, wherein the compression device is heated.

[0148] Aspect 21 provides the method of any of aspects 1 to 20, wherein the gel dispersed around the reinforcing component is heated to a temperature in the range of about 80°C to about 700°C.

[0149] Aspect 22 provides the method of any of aspects 1 to 21, wherein the gel dispersed around the reinforcing component is heated to a temperature in the range of about 90°C to about 110°C.

[0150] Aspect 23 provides the method of any one of aspects 1 to 22, wherein the heating is performed at a constant temperature.

[0151] Aspect 24 provides the method of any one of aspects 1 to 23, wherein the heating is performed over a temperature gradient.

[0152] Aspect 25 provides the method of any one of aspects 1 to 24, wherein the heating is performed in multiple heating cycles.

[0153] Aspect 26 provides the method of any of aspects 1 to 25, wherein compressing the gel dispersed around the reinforcing component is accomplished at a pressure of up to about 1000 kPa.

[0154] Aspect 27 provides the method of any of aspects 1 to 26, wherein compressing the gel dispersed around the reinforcing component is accomplished at a pressure in the range of about 500 kPa to about 1000 kPa.

[0155] Aspect 28 provides the method of any of aspects 1 to 27, wherein compressing the gel dispersed around the reinforcing component is accomplished at a pressure in the range of about 700 kPa to about 1000 kPa.

[0156] Aspect 29 provides the method of any of aspects 1 to 28, wherein the compression occurs over a period of time in a range from about 0.2 hours to about 24 hours.

[0157] Aspect 30 provides the method of any one of aspects 1 to 29, further comprising distributing an additive throughout the gel.

[0158] Aspect 31 provides the method of aspect 30, wherein the additive is in the range of about 0.05 wt % to about 10 wt % of the aerogel composite.

[0159] Aspect 32 provides the method of any of aspects 30 or 31, wherein the additive is in the range of about 1 wt % to about 7 wt % of the aerogel composite.

[0160] Aspect 33 provides a method as described in any of Aspects 30 to 32, wherein the additive comprises boron carbide [B4C], diatomaceous earth, manganese ferrite, MnO, NiO, SnO, Ag2O, Bi2O3, carbon black, titanium oxide, titanium iron oxide, aluminum oxide, zirconium silicate, zirconium oxide, iron (II) oxide, iron (III) oxide, manganese dioxide, titanium iron oxide (ilmenite), chromium oxide, SiC, TiC or WC, TiOSO4, TiOCl2 or a mixture thereof.

[0161] Aspect 34 provides the method of any one of aspects 1 to 33, further comprising contacting the prepared aerogel composite with a solution comprising ethanol and hexamethyldisiloxane.

[0162] Aspect 35 provides the method of any one of aspects 1 to 34, wherein the compressed aerogel composite material having a thickness of 1 mm to 1.62 mm has a thickness standard deviation of 0.042 mm to 0.056 mm, and in some aspects includes the following:

[0163] 1.62mm, thickness standard deviation is 0.05mm;

[0164] 1.038mm, thickness standard deviation is 0.055mm;

[0165] 0.60mm, thickness standard deviation is 0.042mm;

[0166] 1.07mm, thickness standard deviation is 0.056mm; or

[0167] 0.62mm, thickness standard deviation is 0.08mm.

[0168] Aspect 36 provides the method of any one of aspects 1 to 35, wherein the compressed aerogel composite material having a maximum stress 50% strain value of 413.66 kPa to 23073.5 kPa has a maximum stress standard deviation at 50% strain of 72.67 kPa to 9828.5 kPa, and in some aspects includes the following:

[0169] 1841.33 kPa, the standard deviation of the maximum stress at 50% strain is 426.08;

[0170] 10689.8 kPa, the standard deviation of the maximum stress at 50% strain is 1321.21;

[0171] 23073.5 kPa, with a standard deviation of maximum stress at 50% strain of 9828.5; or

[0172] 413.66 kPa, and the standard deviation of the maximum stress at 50% strain is 72.67.

[0173] Aspect 37 provides the method of any of aspects 1 to 36, wherein the compressed aerogel composite material having a compression set value of 13% to 68% has a standard deviation of a compression set value of 1.38% to 15.58%, and in some aspects can include the following:

[0174] 50.01383%, the standard deviation of compression set is 4.64;

[0175] 67.5%, standard deviation of compression set is 1.38;

[0176] 29.13% with a compression set standard deviation of 15.58; or

[0177] 13.2%, and the standard deviation of compression set is 2.4.

[0178] Aspect 38 provides the method of any of aspects 1 to 37, wherein the compressed aerogel composite material having a thermal conductivity of 16 mW / mK to 23.1 mW / mK has a standard deviation of thermal conductivity of 0.0377 mW / mK to 2.7 mW / mK, and in some aspects can include the following:

[0179] 16.089mW / mK, thermal conductivity standard deviation is 0.0377;

[0180] 19.67mW / mk, thermal conductivity standard deviation is 0.90;

[0181] 12mWmK, thermal conductivity standard deviation is 2.7;

[0182] 18.54mW / mK, with a thermal conductivity standard deviation of 0.49; or

[0183] 23.1mW / mK, and the standard deviation of thermal conductivity is 0.171.

[0184] Aspect 39 provides the method of any of aspects 1 to 38, wherein the thickness of the aerogel composite produced is in the range of about 0.1 mm to about 0.6 mm.

[0185] Aspect 40 provides the method of any of aspects 1 to 39, wherein the thickness of the aerogel composite produced is in the range of about 0.1 mm to about 0.5 mm.

[0186] Aspect 41 provides a method for preparing an aerogel composite material, the method comprising:

[0187] Compressing and heating the aerogel composite material, the aerogel composite material comprising silica gel dispersed around a reinforcing component, the reinforcing component comprising polyethylene, polyacrylonitrile oxide, polyacrylonitrile, polyethylene terephthalate, or a mixture thereof, and the heating is performed at a temperature above the glass transition temperature of the polyethylene, polyacrylonitrile oxide, polyacrylonitrile, polyethylene terephthalate, or a mixture thereof; and

[0188] A compressed and heated aerogel composite material is prepared, wherein the prepared aerogel composite material contains a plurality of pores, wherein the diameters of most of the pores are less than 50 nm.

[0189] Aspect 42 provides the method of aspect 41, wherein the reinforcing component comprises a biconstituent polyethylene terephthalate fiber comprising an inner core and an outer core, wherein the inner core has a higher melting temperature than the outer core.

[0190] Aspect 43 provides the method of any of aspects 41 or 42, wherein the reinforcing component is in the range of about 5 weight percent to about 75 weight percent of the aerogel composite.

[0191] Aspect 44 provides the method of any one of aspects 41 to 43, wherein the density of the aerogel composite is increased up to 20 times relative to the gel before compression.

[0192] Aspect 45 provides the method of any of aspects 41 to 44, wherein the density of the aerogel composite is increased up to 10 times relative to the gel before compression.

[0193] Aspect 46 provides the method of any one of aspects 41 to 45, wherein the compression comprises mechanical compression or air compression.

[0194] Aspect 47 provides the method of aspect 46, wherein the mechanical compression is performed using a compression device.

[0195] Aspect 48 provides the method of aspect 47, wherein the compression device comprises a press, a roller, or both.

[0196] Aspect 49 provides the method of any of aspects 47 or 48, wherein the compression device is heated.

[0197] Aspect 50 provides the method of any one of aspects 41 to 49, wherein the heating is performed at a constant temperature.

[0198] Aspect 51 provides the method of any one of aspects 41 to 50, wherein the heating is performed over a temperature gradient.

[0199] Aspect 52 provides the method of any one of aspects 41 to 51, wherein the heating is performed in multiple heating cycles.

[0200] Aspect 53 provides the method of any of aspects 41 to 52, wherein compressing the gel dispersed around the reinforcing component is accomplished at a pressure of up to about 1000 kPa.

[0201] Aspect 54 provides the method of any of aspects 41 to 53, wherein compressing the gel dispersed around the reinforcing component is accomplished at a pressure in a range of about 500 kPa to about 1000 kPa.

[0202] Aspect 55 provides the method of any of aspects 41 to 54, wherein compressing the gel dispersed around the reinforcing component is accomplished at a pressure in the range of about 700 kPa to about 1000 kPa.

[0203] Aspect 56 provides the method of any of aspects 41 to 55, wherein the compression occurs over a period of time in a range from about 0.2 hours to about 24 hours.

[0204] Aspect 57 provides the method of any of aspects 41 to 56, further comprising distributing an additive around the gel.

[0205] Aspect 58 provides the method of aspect 57, wherein the additive is in the range of about 0.05 wt % to about 10 wt % of the aerogel composite.

[0206] Aspect 59 provides the method of any of aspects 57 or 58, wherein the additive is in the range of about 1 wt % to about 7 wt % of the aerogel composite.

[0207] Aspect 60 provides a method as described in any of Aspects 57 to 59, wherein the additive comprises boron carbide [B4C], diatomaceous earth, manganese ferrite, MnO, NiO, SnO, Ag2O, Bi2O3, carbon black, titanium oxide, titanium iron oxide, aluminum oxide, zirconium silicate, zirconium oxide, iron (II) oxide, iron (III) oxide, manganese dioxide, titanium iron oxide (ilmenite), chromium oxide, SiC, TiC or WC, TiOSO4, TiOCl2 or a mixture thereof.

[0208] Aspect 61 provides the method of any one of aspects 41 to 60, further comprising contacting the prepared aerogel composite with a solution comprising ethanol and bis(trimethylsilyl)amine.

[0209] Aspect 62 provides the method of any one of aspects 41 to 61, wherein the compressed aerogel composite material having a thickness of 1 mm to 1.62 mm has a thickness standard deviation of 0.042 mm to 0.056 mm, and in some aspects includes the following:

[0210] 1.62mm, thickness standard deviation is 0.05mm;

[0211] 1.038mm, thickness standard deviation is 0.055mm;

[0212] 0.60mm, thickness standard deviation is 0.042mm;

[0213] 1.07mm, thickness standard deviation is 0.056mm; or

[0214] 0.62mm, thickness standard deviation is 0.08mm.

[0215] Aspect 63 provides the method of any of aspects 41 to 62, wherein the compressed aerogel composite material having a maximum stress 50% strain value of 413.66 kPa to 23073.5 kPa has a maximum stress standard deviation at 50% strain of 72.67 kPa to 9828.5 kPa, and in some aspects includes the following:

[0216] 1841.33 kPa, the standard deviation of the maximum stress at 50% strain is 426.08;

[0217] 10689.8 kPa, the standard deviation of the maximum stress at 50% strain is 1321.21;

[0218] 23073.5 kPa, with a standard deviation of maximum stress at 50% strain of 9828.5; or

[0219] 413.66 kPa, and the standard deviation of the maximum stress at 50% strain is 72.67.

[0220] Aspect 64 provides the method of any of aspects 41 to 63, wherein the compressed aerogel composite having a compression set value of 13% to 68% has a standard deviation of the compression set value of 1.38% to 15.58%, and in some aspects can include the following:

[0221] 50.01383%, the standard deviation of compression set is 4.64;

[0222] 67.5%, standard deviation of compression set is 1.38;

[0223] 29.13% with a compression set standard deviation of 15.58; or

[0224] 13.2%, and the standard deviation of compression set is 2.4.

[0225] Aspect 65 provides the method of any of aspects 41 to 64, wherein the compressed aerogel composite material having a thermal conductivity of 16 mW / mK to 23.1 mW / mK has a standard deviation of thermal conductivity of 0.0377 mW / mK to 2.7 mW / mK, and in some aspects can include the following:

[0226] 16.089mW / mK, thermal conductivity standard deviation is 0.0377;

[0227] 19.67mW / mk, thermal conductivity standard deviation is 0.90;

[0228] 12mWmK, thermal conductivity standard deviation is 2.7;

[0229] 18.54mW / mK, with a thermal conductivity standard deviation of 0.49; or

[0230] 23.1mW / mK, and the standard deviation of thermal conductivity is 0.171.

[0231] Aspect 66 provides the method of any of aspects 41 to 65, wherein the thickness of the aerogel composite produced is in the range of about 0.1 mm to about 0.6 mm.

[0232] Aspect 67 provides the method of any of aspects 41 to 66, wherein the thickness of the aerogel composite produced is in the range of about 0.1 mm to about 0.5 mm.

[0233] Aspect 68 provides a compressed aerogel composite material, the compressed aerogel composite material comprising:

[0234] A gel comprising a metal oxide compound distributed around a reinforcing component, wherein

[0235] The aerogel composite material comprises a plurality of pores, wherein the diameter of most of the pores is less than 50 nm.

[0236] Aspect 69 provides the compressed aerogel composite material of aspect 68, wherein the compressed aerogel composite material having a thickness of 1 mm to 1.62 mm has a thickness standard deviation of 0.042 mm to 0.056 mm, and in some aspects includes the following:

[0237] 1.62mm, thickness standard deviation is 0.05mm;

[0238] 1.038mm, thickness standard deviation is 0.055mm;

[0239] 0.60mm, thickness standard deviation is 0.042mm;

[0240] 1.07mm, thickness standard deviation is 0.056mm; or

[0241] 0.62mm, thickness standard deviation is 0.08mm.

[0242] Aspect 70 provides a compressed aerogel composite material of any one of aspects 68 or 69, wherein the compressed aerogel composite material having a maximum stress 50% strain value of 413.66 kPa to 23073.5 kPa has a maximum stress standard deviation at 50% strain of 72.67 kPa to 9828.5 kPa, and in some aspects includes the following:

[0243] 1841.33 kPa, the standard deviation of the maximum stress at 50% strain is 426.08;

[0244] 10689.8 kPa, the standard deviation of the maximum stress at 50% strain is 1321.21;

[0245] 23073.5 kPa, with a standard deviation of maximum stress at 50% strain of 9828.5; or

[0246] 413.66 kPa, and the standard deviation of the maximum stress at 50% strain is 72.67.

[0247] Aspect 71 provides a compressed aerogel composite material of any of aspects 68 to 70, wherein the compressed aerogel composite material having a compression set value of 13% to 68% has a standard deviation of compression set values ​​of 1.38% to 15.58%, and in some aspects can include the following:

[0248] 50.01383%, the standard deviation of compression set is 4.64;

[0249] 67.5%, standard deviation of compression set is 1.38;

[0250] 29.13% with a compression set standard deviation of 15.58; or

[0251] 13.2%, and the standard deviation of compression set is 2.4.

[0252] Aspect 72 provides the compressed aerogel composite material of any one of aspects 68 to 71, wherein the compressed aerogel composite material having a thermal conductivity of 16 mW / mK to 23.1 mW / mK has a standard deviation of thermal conductivity of 0.0377 mW / mK to 2.7 mW / mK, and in some aspects can include the following:

[0253] 16.089mW / mK, thermal conductivity standard deviation is 0.0377;

[0254] 19.67mW / mk, thermal conductivity standard deviation is 0.90;

[0255] 12mWmK, thermal conductivity standard deviation is 2.7;

[0256] 18.54mW / mK, with a thermal conductivity standard deviation of 0.49; or

[0257] 23.1mW / mK, and the standard deviation of thermal conductivity is 0.171.

Claims

1. A method for preparing an aerogel composite material, the method comprising: compressing and heating the aerogel composite, the aerogel composite comprising a gel dispersed around a reinforcing component; as well as A compressed and heated aerogel composite material is prepared, wherein the prepared aerogel composite material contains a plurality of pores, wherein the diameters of most of the pores are less than 50 nm.

2. The method of claim 1, wherein the gel comprises a metal oxide compound.

3. The method of claim 2, wherein the metal oxide compound comprises silicon dioxide, aluminum oxide, titanium dioxide, ceria, yttrium oxide, or any combination thereof.

4. The method of any one of claims 2 or 3, wherein the metal oxide compound comprises silicon dioxide.

5. The method of any one of claims 1 to 4, wherein the reinforcing component comprises a nonwoven material, a woven material, a fluffy batting, a fibrous batting, or any combination thereof.

6. The method of any one of claims 1 to 5, wherein the reinforcing component comprises inorganic fibers, organic fibers, particles, metal fibers, metal mesh, organic foam, or mixtures thereof.

7. The method of claim 6, wherein the inorganic fibers comprise glass fibers or ceramic fibers.

8. The method of any one of claims 6 or 7, wherein the organic fibers comprise polyethylene, oxidized polyacrylonitrile, polyacrylonitrile, polyethylene terephthalate, or mixtures thereof.

9. The method of claim 8, wherein the reinforcing component comprises a biconstituent polyethylene terephthalate fiber comprising an inner core and an outer core, wherein the inner core has a higher melting temperature than the outer core.

10. The method of any one of claims 6 to 9, wherein the organic foam comprises melamine.

11. The method of any one of claims 1 to 10, wherein the reinforcing component is in the range of about 5% to about 75% by weight of the aerogel composite.

12. The method of any one of claims 1 to 11, wherein the reinforcing component is in the range of about 25% to about 50% by weight of the aerogel composite.

13. The method of any one of claims 1 to 12, wherein the density of the aerogel composite material is increased up to 20 times relative to the gel before compression.

14. The method of any one of claims 1 to 13, wherein the density of the aerogel composite material is increased up to 10 times relative to the gel before compression.

15. The method of any one of claims 1 to 14, wherein the compressing and heating are performed simultaneously.

16. The method of any one of claims 1 to 14, wherein heating is performed after compressing.

17. The method of any one of claims 1 to 16, wherein the compression comprises mechanical compression or air compression.

18. The method of claim 17, wherein the mechanical compression is accomplished using a compression device.

19. The method of claim 18, wherein the compression device comprises a press, rollers, or both.

20. The method of any one of claims 18 or 19, wherein the compression device is heated.

21. The method of any one of claims 1 to 20, wherein the gel dispersed around the reinforcing component is heated to a temperature in the range of about 80°C to about 700°C.

22. The method of any one of claims 1 to 21, wherein the gel dispersed around the reinforcing component is heated to a temperature in the range of about 90°C to about 110°C.

23. The method of any one of claims 1 to 22, wherein the heating is performed at a constant temperature.

24. The method of any one of claims 1 to 23, wherein the heating is performed over a temperature gradient.

25. The method of any one of claims 1 to 24, wherein the heating is performed in a plurality of heating cycles.

26. The method of any one of claims 1 to 25, wherein compressing the gel dispersed around the reinforcing component is accomplished at a pressure of up to about 1000 kPa.

27. The method of any one of claims 1 to 26, wherein compressing the gel dispersed around the reinforcing component is accomplished at a pressure in the range of about 500 kPa to about 1000 kPa.

28. The method of any one of claims 1 to 27, wherein compressing the gel dispersed around the reinforcing component is accomplished at a pressure in the range of about 700 kPa to about 1000 kPa.

29. The method of any one of claims 1 to 28, wherein compression occurs over a period of time from about 0.2 hours to about 24 hours.

30. The method of any one of claims 1 to 29, further comprising distributing an additive throughout the gel.

31. The method of claim 30, wherein the additive is in the range of about 0.05% to about 10% by weight of the aerogel composite.

32. The method of any one of claims 30 or 31, wherein the additive is in the range of about 1 wt% to about 7 wt% of the aerogel composite.

33. The method of any one of claims 30 to 32, wherein the additive comprises boron carbide [B4C], diatomaceous earth, manganese ferrite, MnO, NiO, SnO, Ag2O, Bi2O3, carbon black, titanium oxide, titanium iron oxide, aluminum oxide, zirconium silicate, zirconium oxide, iron (II) oxide, iron (III) oxide, manganese dioxide, titanium iron oxide (ilmenite), chromium oxide, SiC, TiC or WC, TiOSO4, TiOCl2 or mixtures thereof.

34. The method of any one of claims 1 to 33, further comprising contacting the prepared aerogel composite with a solution comprising ethanol and hexamethyldisiloxane.

35. The method of any one of claims 1 to 34, wherein the compressed aerogel composite material having a thickness of 1 mm to 1.62 mm has a thickness standard deviation of 0.42 mm to 0.55 mm.

36. The method of any one of claims 1 to 35, wherein the compressed aerogel composite has a maximum stress at 50% strain of 413.66 kPa to 23073.5 kPa.

37. The method of any one of claims 1 to 36, wherein the compressed aerogel composite has a compression set value of 13% to 68%.

38. The method of any one of claims 1 to 37, wherein the compressed aerogel composite has a thermal conductivity of 16 mW / mK to 23.1 mW / mK.

39. The method of any one of claims 1 to 38, wherein the thickness of the aerogel composite produced is in the range of about 0.1 mm to about 0.6 mm.

40. The method of any one of claims 1 to 39, wherein the thickness of the aerogel composite produced is in the range of about 0.1 mm to about 0.5 mm.

41. A method for preparing an aerogel composite material, the method comprising: Compressing and heating the aerogel composite material, the aerogel composite material comprising silica gel dispersed around a reinforcing component, the reinforcing component comprising polyethylene, polyacrylonitrile, polyacrylonitrile oxide, polyethylene terephthalate, or a mixture thereof, and the heating is performed at a temperature above the glass transition temperature of the polyethylene, polyacrylonitrile, polyacrylonitrile oxide, polyethylene terephthalate, or a mixture thereof; and A compressed and heated aerogel composite material is prepared, wherein the prepared aerogel composite material contains a plurality of pores, wherein the diameters of most of the pores are less than 50 nm.

42. The method of claim 41, wherein the reinforcing component comprises a biconstituent polyethylene terephthalate fiber comprising an inner core and an outer core, wherein the inner core has a higher melting temperature than the outer core.

43. The method of any one of claims 41 or 42, wherein the reinforcing component is in the range of about 5% to about 75% by weight of the aerogel composite.

44. A method as claimed in any one of claims 41 to 43, wherein the density of the aerogel composite is increased by up to 20 times relative to the gel before compression.

45. A method as claimed in any one of claims 41 to 44, wherein the density of the aerogel composite is increased by up to 10 times relative to the gel before compression.

46. ​​The method of any one of claims 41 to 45, wherein the compression comprises mechanical compression or air compression.

47. The method of claim 46, wherein the mechanical compression is accomplished using a compression device.

48. The method of claim 47, wherein the compression device comprises a press, rollers, or both.

49. The method of any one of claims 47 or 48, wherein the compression device is heated.

50. The method of any one of claims 41 to 49, wherein the heating is performed at a constant temperature.

51. The method of any one of claims 41 to 50, wherein the heating is performed over a temperature gradient.

52. The method of any one of claims 41 to 51, wherein the heating is performed in a plurality of heating cycles.

53. The method of any one of claims 41 to 52, wherein compressing the gel dispersed around the reinforcing component is accomplished at a pressure of up to about 1000 kPa.

54. The method of any one of claims 41 to 53, wherein compressing the gel dispersed around the reinforcing component is accomplished at a pressure in the range of about 500 kPa to about 1000 kPa.

55. The method of any one of claims 41 to 54, wherein compressing the gel dispersed around the reinforcing component is accomplished at a pressure in the range of about 700 kPa to about 1000 kPa.

56. The method of any one of claims 41 to 55, wherein compression occurs over a period of time from about 0.2 hours to about 24 hours.

57. The method of any one of claims 41 to 56, further comprising distributing an additive around the gel.

58. The method of claim 57, wherein the additive is in the range of about 0.05% to about 10% by weight of the aerogel composite.

59. The method of any one of claims 57 or 58, wherein the additive is in the range of about 1 wt% to about 7 wt% of the aerogel composite.

60. The method of any one of claims 57 to 59, wherein the additive comprises boron carbide [B4C], diatomaceous earth, manganese ferrite, MnO, NiO, SnO, Ag2O, Bi2O3, carbon black, titanium oxide, titanium iron oxide, aluminum oxide, zirconium silicate, zirconium oxide, iron (II) oxide, iron (III) oxide, manganese dioxide, titanium iron oxide (ilmenite), chromium oxide, SiC, TiC or WC, TiOSO4, TiOCl2 or mixtures thereof.

61. The method of any one of claims 41 to 60, further comprising contacting the prepared aerogel composite with a solution comprising ethanol and bis(trimethylsilyl)amine.

62. The method of any one of claims 41 to 61, wherein the compressed aerogel composite material having a thickness of 1 mm to 1.62 mm has a thickness standard deviation of 0.42 mm to 0.55 mm.

63. The method of any one of claims 41 to 62, wherein the compressed aerogel composite has a maximum stress at 50% strain of 413.66 kPa to 23073.5 kPa.

64. The method of any one of claims 41 to 63, wherein the compressed aerogel composite has a compression set value of 13% to 68%.

65. The method of any one of claims 41 to 64, wherein the compressed aerogel composite has a thermal conductivity of 16 mW / mK to 23.1 mW / mK.

66. The method of any one of claims 41 to 65, wherein the thickness of the aerogel composite produced is in the range of about 0.1 mm to about 0.6 mm.

67. The method of any one of claims 41 to 66, wherein the thickness of the aerogel composite produced is in the range of about 0.1 mm to about 0.5 mm.

68. A compressed aerogel composite material, comprising: A gel comprising a metal oxide compound distributed around a reinforcing component, wherein The aerogel composite material comprises a plurality of pores, wherein the diameter of most of the pores is less than 50 nm.

69. The compressed aerogel composite of claim 68, wherein the compressed aerogel composite having a thickness of 1 mm to 1.62 mm has a thickness standard deviation of 0.42 mm to 0.55 mm.

70. The compressed aerogel composite material of any one of claims 68 or 69, wherein the compressed aerogel composite material has a maximum stress at 50% strain of 413.66 kPa to 23073.5 kPa.

71. The compressed aerogel composite material of any one of claims 68 to 70, wherein the compressed aerogel composite material has a compression set value of 13% to 68%.

72. The compressed aerogel composite material of any one of claims 68 to 71, wherein the compressed aerogel composite material has a thermal conductivity of 16 mW / mK to 23.1 mW / mK.

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