Aerogel-based components and systems for thermal management in electric vehicles

Abstract

Aerogel-based components and systems for thermal management in electric vehicles are provided. Exemplary embodiments include thermal control elements. The thermal control elements can include reinforced aerogel compositions that are durable, easy to handle, and have good performance for use as thermal control elements and thermal barriers for batteries, good thermal insulation properties, and good fire, combustion, and flame resistance. Methods for preparing or manufacturing such reinforced aerogel compositions are also provided. In certain embodiments, the compositions have a silica-based aerogel framework reinforced by fibers and containing one or more opacifying additives.

Description

Cross-reference of related applications

[0001] This application claims priority to U.S. Provisional Patent Application No. 62 / 942,495 filed on 2 December 2019, U.S. Provisional Patent Application No. 62 / 958,135 filed on 7 January 2020, U.S. Provisional Patent Application No. 63 / 056,527 filed on 24 July 2020, and U.S. Patent Application No. 17 / 106,940 filed on 30 November 2020, each of which is incorporated herein by reference in its entirety, and any definitions of terms in this application are governed by these. [Technical Field]

[0002] The present invention generally relates to aerogel technology. More specifically, this disclosure relates to thermal control members incorporating aerogel technology. In certain embodiments, this disclosure relates to high-performance thermal control members incorporating aerogel technology for isolating battery cells or for insulating battery components. [Background technology]

[0003] Low-density aerogel materials are widely considered to be the best solid insulators available. Aerogels function as insulators primarily by minimizing conduction (low structural density results in winding pathways for energy transfer through the solid framework), convection (large pore volume and very small pore diameters result in minimal convection), and radiation (having IR absorption or scattering dopants). Aerogels can be used in a wide range of applications, including thermal and cooling insulation, acoustic insulation, electronic dielectrics, aerospace, energy storage and production, and filtration. Furthermore, aerogel materials exhibit many other interesting acoustic, optical, mechanical, and chemical properties that make them highly useful in a variety of insulating and non-insulating applications.

[0004] Insulation suitable for reliably controlling heat flow from heat-generating components in small spaces, thereby providing safety and fire propagation prevention for such products, is needed in the fields of electronics, industrial technology, and automotive technology. Insulation sheets with excellent compression properties can be useful in addressing these needs, for example, as separators in lithium-ion battery modules.

[0005] Safety standards for lithium-ion batteries include fire heating tests. A fire heating test is a test method that determines whether ignition or explosion occurs as a result of heat transfer to other cells, including adjacent cells, after a cell in the battery module has undergone thermal runaway. Safety designs intended to prevent the propagation of thermal runaway to adjacent cells typically include the use of materials with excellent thermal insulation properties between cells.

[0006] Conventional types of insulation materials, such as foam or fiber sheets, can withstand high temperatures, but their capacity for insulation or heat containment is relatively low. For such materials, the thickness of the insulation must be increased to provide effective thermal management. However, the space requirements of battery modules limit the size of the module, as well as the space between cells within the module. Similarly, it is desirable to limit the total weight of the battery module. Therefore, resistance to heat and fire propagation must be achieved while minimizing the thickness and weight of the materials used to provide the required thermal properties. Different types of insulation systems, insulation materials, and insulation methods are needed to provide effective insulation, heat containment, and fire protection.

[0007] Aerogel materials are known to have approximately 2 to 6 times the thermal resistance of other common types of insulating materials, such as foams and fiberglass. Aerogels can increase effective shielding and insulation without substantially increasing the thickness of the insulating material or adding additional weight. Aerogels are known to be a class of structures with low density, an open-cell structure, a large surface area, and nanometer-scale pore sizes.

[0008] Steinke's U.S. Patent Application Publication No. 2012 / 0142802 discloses an open-cell foam filled with aerogel particles. Oikawa's U.S. Patent Application Publication No. 2019 / 0161909 discloses a heat insulating sheet including a nonwoven fabric and an aerogel. However, these documents do not disclose materials having desired thermal, fire, mechanical, and hydrophobic properties, and combinations of many desired properties, for use in a method for manufacturing a thermal barrier for separating a thermal control member or a battery cell or such a material.

[0009] It is desirable to provide a reinforced aerogel composition having improved performance in various aspects including compressibility, compression elasticity, compliance, heat resistance, hydrophobicity, ignition reaction, etc., individually and in one or more combinations. Considering the technology as a whole at the time the present invention was made, it was not obvious to those skilled in the art of the present invention how the disadvantages of the prior art could be solved.

[0010] Certain aspects of the prior art have been discussed to facilitate the disclosure of the present invention, but the applicant does not in any way disclaim these technical aspects, and it is contemplated that the claimed invention may include one or more of the conventional technical aspects described herein.

[0011] The present invention can address one or more of the problems and disadvantages of the prior art. However, it is contemplated that the present invention can be found useful in addressing other problems and deficiencies in some technical fields. Therefore, the claimed invention should not be construed as necessarily limited to addressing any of the specific problems or deficiencies discussed herein.

[0012] In this specification, when an item of literature, act, or knowledge is referenced or discussed, such reference or discussion does not admit that the item of literature, act, or knowledge or any combination thereof was publicly available, known to the public, part of common general knowledge, or constituted prior art under the applicable statutory provisions at the priority date, or that it is known to be relevant to an attempt to solve the problem to which this specification relates.

Prior Art Documents

Patent Documents

[0013]

Patent Document 1

先行技術文献

特許文献

[0013]

特許文献1

特許文献2

発明の概要

[0014] The long-standing but hitherto unmet need for improved aerogel compositions is now satisfied by a new useful and non-obvious invention.

[0015] In a general aspect, the present disclosure provides an aerogel composition, such as a reinforced aerogel composition, that is durable, easy to handle, has good resistance to heat transfer and fire spread while minimizing the thickness and weight of the materials used, and also has good properties for compressibility, compression elasticity, and compliance. In another general aspect, the present disclosure provides a thermal control member that includes an aerogel composition, a reinforced aerogel composition, or a combination thereof. For example, a thermal control member according to an aspect disclosed herein can include at least one layer of an aerogel composition or a reinforced aerogel composition. As another example, a thermal control member according to an aspect disclosed herein can include a plurality of layers of an aerogel composition or a reinforced aerogel composition.

[0016] In exemplary embodiments, the disclosure provides a thermal control member comprising an aerogel composition. In certain embodiments, the thermal control member is substantially flat and has a first main outer surface and a second main outer surface. In exemplary embodiments, the aerogel composition comprises one or more additives. In some embodiments, the additives may be present at a level of about 5 to 20% by weight of the aerogel composition. In some embodiments, the additives may be present at a level of about 10 to 20% by weight of the aerogel composition. In certain embodiments, the thermal control member has a thermal conductivity of less than about 40 mW / mK. In exemplary embodiments, the thermal control member comprises multiple layers of the aerogel composition.

[0017] In another exemplary embodiment, the disclosure provides a thermal control member comprising at least one layer of an aerogel composition, at least one compliant member, and a thermocapacitive material. The aerogel composition comprises one or more additives, which are present at a level of at least about 5 to 20% by weight of the aerogel composition. In some embodiments, the additives may be present at a level of about 10 to 20% by weight of the aerogel composition. In exemplary embodiments, the thermal control member comprises multiple layers of the aerogel composition. In some embodiments, the thermocapacitive material is located between at least two layers of the aerogel composition. The thermocapacitive material has a capacitance of at least about 0.3 J / (g) ·℃ This can be any material having a specific heat capacity of 0.5 J / (g). In some embodiments, the material providing the heat capacity is at least about 0.5 J / (g). ·℃ ) has a specific heat capacity of ). For example, the heat-capacitive material may include at least one layer containing a metal. In exemplary embodiments, at least one compliant member may include a compressible material, i.e., a material that can be compressed to reduce its thickness while providing a desired resistance to compression. For example, the compliant member may be polyolefin, polyurethane, phenol resinThe compliant member may be a material selected from the group consisting of melamine, cellulose acetate, and polystyrene. The compliant member may be positioned adjacent to the aerogel composition or the heat-capacitive material. In exemplary embodiments, the compliant member is located between at least two layers of the aerogel composition. In some embodiments, the compliant member is positioned between both the layer of the aerogel composition and the layer of the heat-capacitive material.

[0018] In some embodiments, the thermal control member has a thermal conductivity in the range of about 30 mW / mK or less, about 25 mW / mK or less, about 20 mW / mK or less, about 18 mW / mK or less, about 16 mW / mK or less, about 14 mW / mK or less, about 12 mW / mK or less, about 10 mW / mK or less, about 5 mW / mK or less, or any combination of the aforementioned thermal conductivity values. In exemplary embodiments, one or more additives include fire-class additives. In exemplary embodiments, one or more additives include opacifiers. In some embodiments, one or more additives include a combination of fire-class additives and opacifiers. For example, one or more additives may include clay minerals, such as kaolin. In another example, one or more additives may be selected from the group consisting of boron carbide, diatomaceous earth, manganese ferrite, MnO, NiO, SnO, Ag2O, Bi2O3, carbon black, graphite, titanium oxide, iron oxide, aluminum oxide, zirconium silicate, zirconium oxide, iron(II) oxide, iron(III) oxide, manganese dioxide, iron oxide (ilmenite), chromium oxide, silicon carbide, titanium carbide, tungsten carbide, or mixtures thereof. In a preferred embodiment, one or more additives include silicon carbide.

[0019] In exemplary embodiments, when the first main outer surface is exposed to a temperature of 650°C or higher, the thermal control member maintains a temperature of 120°C or lower on the second main surface for at least about 1 minute. In some embodiments, when the first main outer surface is exposed to a temperature of 650°C or higher, the thermal control member maintains a temperature of 75°C or lower on the second main outer surface for at least about 30 seconds. In some embodiments, when the first main outer surface is exposed to a temperature of 650°C or higher, the thermal control member maintains a temperature of 150°C or lower on the second main outer surface for at least about 90 seconds. In some embodiments, when the first main outer surface is exposed to a temperature of 650°C or higher, the thermal control member maintains a temperature of 150°C or lower on the second main outer surface for at least about 90 seconds. In some embodiments, when the first main outer surface is exposed to a temperature of 650°C or higher, the thermal control member maintains a temperature of 170°C or lower on the second main outer surface for at least about 90 seconds. In some embodiments, when the first main outer surface is exposed to a temperature of 650°C or higher, the thermal control member maintains a temperature of 180°C or lower on the second main outer surface for at least about 2 minutes, preferably at least about 4 minutes.

[0020] In another embodiment, these thermal profiles are achieved when the thermal control member is incorporated into an electric vehicle system along with other components having various configurations and environments. For example, the thermal control member can be integrated into a system such as a battery system, where the thermal control member and other components are subjected to ambient pressure, temperature, and compression (including from gases other than air).

[0021] In exemplary embodiments, the aerogel composition has an incompressible thickness ranging from about 1 mm to about 10 mm. For example, the aerogel composition may have an incompressible thickness ranging from about 1 mm to about 5 mm. In another example, the aerogel composition may have an incompressible thickness of about 2 mm, about 3 mm, or about 4 mm.

[0022] In certain embodiments, the aerogel composition is approximately 0.60 g / cm³. 3 Below, about 0.50g / cm 3Less than or equal to approximately 0.40 g / cm 3 Less than or equal to approximately 0.30 g / cm 3 Less than or equal to approximately 0.25 g / cm 3 Less than or equal to approximately 0.20 g / cm 3 Less than or equal to approximately 0.18 g / cm 3 Less than or equal to approximately 0.16 g / cm 3 Less than or equal to approximately 0.14 g / cm 3 Less than or equal to approximately 0.12 g / cm 3 Less than or equal to approximately 0.10 g / cm 3 Less than or equal to approximately 0.05 g / cm 3 Less than or equal to approximately 0.01 g / cm 3 Less than or equal to, or having a density within the range between any two of these values. In an exemplary embodiment, the aerogel composition has a density of less than approximately 0.3 g / cm 3 .

[0023] In an exemplary aspect, the present disclosure provides a battery module including a first battery cell, a second battery cell, and a thermal control member according to an embodiment disclosed herein disposed at least between the first battery cell and the second battery cell.

[0024] In an exemplary aspect, the present disclosure provides a battery module or battery pack including at least one battery cell and a thermal control member according to an embodiment disclosed herein disposed on the battery cell or on the battery module, for example, on the surface of at least one battery cell or on the surface of the battery module. For example, the battery module or battery pack has an inner surface and an outer surface. In certain embodiments, the thermal control member is on the inner surface of the battery module or battery pack. In certain embodiments, the thermal control member is on the outer surface of the battery module or battery pack.

[0025] In an exemplary embodiment, the thermal control member includes an aerogel composition. In some embodiments, the thermal control member has an energy absorption capacity in the range of from about 25 J / g to about 225 J / g.

[0026] In embodiments of the aspects disclosed herein, the aerogel composition may include a reinforcing material. For example, the reinforcing material may include fibers. For example, the reinforcing material may be Multiple separate fibers (discrete fibers) The reinforcing material can be selected from the group consisting of woven materials, nonwoven materials, needle nonwovens, battings, webs, mats, felts, and combinations thereof. In some embodiments, the reinforcing material includes open-cell macroporous framework ("OCMF") material. For example, the OCMF material may include melamine foam or urethane polymer foam. In other embodiments, the reinforcing material may include a combination of fibers and OCMF material.

[0027] In embodiments of the features disclosed herein, the thermal control member may have an incompressible thickness ranging from about 2 mm to about 10 mm. For example, the thermal control member may have an incompressible thickness ranging from about 2 mm, about 3 mm, about 4 mm, about 5 mm, about 6 mm, about 7 mm, about 8 mm, about 9 mm, about 10 mm, or any of the aforementioned thicknesses. In exemplary embodiments, the thermal control member may have an incompressible thickness ranging from about 2 mm to about 7 mm.

[0028] In some embodiments of the embodiments disclosed herein, the thermal control member may further include an encapsulation member forming at least one of a first or second outer surface. For example, an aerogel composition may include an encapsulation member. The encapsulation member may include, for example, an encapsulation layer or coating surrounding the aerogel composition and / or the thermal control member. The encapsulation member may include at least one vent to allow air to enter and exit the panel, and in some embodiments, a particulate filter for holding particulate matter within the encapsulation member.

[0029] In exemplary embodiments, the aerogel composition of the thermal control member is hydrophobic. For example, the aerogel composition has a liquid water absorption rate of less than about 15% by weight.

[0030] In exemplary embodiments, the aerogel of the aerogel composition comprises an inorganic, organic, or inorganic / organic hybrid material. For example, the aerogel composition is a silica aerogel composition. In specific embodiments, the aerogel composition comprises alkylated silica.

[0031] In certain embodiments, the aerogel composition taka It's expensive. For the purposes of this patent, taka A high aerogel composition is defined as an aerogel composition that exhibits bulk and some elastic properties (with or without complete bulk recovery). In certain embodiments, taka A high aerogel composition is (i) compressible to at least 50%, preferably at least 65%, most preferably at least 80% of its original thickness or incompressible thickness, and (ii) elastic enough to return to at least 70%, preferably at least 75%, most preferably at least 80% of its original thickness or incompressible thickness after being compressed for several seconds.

[0032] In some embodiments, the reinforcing material may include a reinforcing material comprising multiple material layers. For example, the multiple material layers may be joined to one another. In exemplary embodiments, at least one of the multiple layers may include a first material, and at least one other layer of the multiple layers may include a second material. The first and second materials may have the same or different material properties. For example, the first material may be more compressible than the second material. In another example, the first material may contain closed cells, and the second material may contain open cells.

[0033] In some embodiments of the embodiments disclosed herein, the thermal control member may include multiple layers. For example, the thermal control member may include at least one layer of a thermally conductive material, e.g., a layer comprising a metal, carbon, a thermally conductive polymer, or a combination thereof. As used in the context of these embodiments, the thermally conductive material refers to a material having a thermal conductivity greater than that of the aerogel composition. In certain embodiments, the thermally conductive material has a thermal conductivity at least about an order of magnitude greater than that of the aerogel composition. In some embodiments, the thermal control member may include multiple layers of the aerogel composition. In certain embodiments, the thermal control member may include at least one layer of a conductive material positioned adjacent to the aerogel composition. In certain embodiments, the thermal control member may include at least one layer of a conductive material positioned between at least two of the multiple layers of the aerogel composition. In some embodiments, the thermal control member may include particles of the conductive material positioned within the layers of the thermal control member, e.g., within the layers of the aerogel composition.

[0034] In exemplary embodiments, the thermal control member is a material or material layer that provides heat capacity (i.e., a heat-capacitive material), for example, at least about 0.3 J / (g) ·℃ This may include materials having a specific heat capacity of at least about 0.5 J / (g). In some embodiments, the material providing the heat capacity is at least about 0.5 J / (g). ·℃) has a specific heat capacity. For example, the material providing the heat capacity may include metals such as aluminum, titanium, nickel, steel, iron, or combinations thereof. In some embodiments, the thermal control member may include a layer or coating of the material providing the heat capacity. In some embodiments, the thermal control member may include particles of the material providing the heat capacity disposed within a layer of the thermal control member, for example, within a layer of an aerogel composition. In certain embodiments, the thermal control member may include at least one layer of the material providing the heat capacity disposed adjacent to the aerogel composition. In certain embodiments, the thermal control member may include at least one layer of the material providing the heat capacity disposed between at least two of a plurality of layers of an aerogel composition. In exemplary embodiments, the thermal control member may include both a thermally conductive material and a thermally capacitive material. For example, the thermal control member may include a material that provides both heat capacity and thermal conductivity, for example, metals such as aluminum, titanium, nickel, steel, iron, or combinations thereof. In another example, the thermal control member may include one or more different materials or layers of materials, each providing either heat capacity, thermal conductivity, or a combination thereof, for example, a layer containing a metal and a layer containing a thermally conductive polymer.

[0035] In some embodiments, a thermal paste is used between layers of a thermal control member to ensure uniform and consistent heat conduction between such layers. As used herein, thermal paste refers to a variety of materials also known as thermal compounds, thermal greases, thermal interface materials (TIMs), thermal gels, heat pastes, heat sink compounds, and heat sink pastes. For example, a layer of thermal paste can be placed between an aerogel composition and other layers, such as one or more layers containing a thermally conductive or heat-capacitive material.

[0036] In embodiments of the aspects disclosed herein, the composition may further include at least one opposing layer, as described in more detail below. For example, the opposing layer may be a layer selected from the group consisting of polymer sheets, metal sheets, fiber sheets, and woven fabric sheets. In exemplary embodiments, the opposing layer may include a conductive material, a heat-capacitating material, or a combination thereof. In some embodiments, the opposing layer may be attached to the composition by an adhesive mechanism selected from the group consisting of, for example, aerosol adhesives, urethane adhesives, acrylate adhesives, hot-melt adhesives, epoxy, rubber resin adhesives, polyurethane composite adhesives, and combinations thereof. In some embodiments, the opposing layer may be attached to the composition by a non-adhesive mechanism, for example, a mechanism selected from the group consisting of flame fusion, stitching, sealing bags, rivets, buttons, clamps, wraps, braces, and combinations thereof. In some embodiments, a combination of any of the adhesive and non-adhesive mechanisms described above may be used to attach the opposing layer to the composition. In some embodiments of the above aspects, the thermal control member may further include at least one layer of a conductive material or a heat-capacitating material. For example, at least one layer of conductive or heat-capacitive material may include metal, carbon, conductive polymer, or a combination thereof. In some examples, at least one layer of the carbon-containing conductive material may be a highly oriented graphite material, such as a pyrolysis graphite sheet or a similar material.

[0037] In embodiments of the aspects disclosed herein, one or more additives are selected from the group consisting of boron carbide, diatomaceous earth, manganese ferrite, MnO, NiO, SnO, Ag2O, Bi2O3, carbon black, graphite, 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, silicon carbide, titanium carbide, tungsten carbide, or mixtures thereof. In certain embodiments, one or more additives may include silicon carbide. In certain embodiments, one or more additives may exclude silicon carbide whiskers or fibers.

[0038] In some embodiments, the aerogel composition further comprises one or more additional additives. For example, one or more additional additives include fire-class additives. In these or other embodiments of the above-described aspects, the composition is low-flammability, non-flammability, low-combustibility, or non-combustible. In some embodiments, the additives include clay minerals, such as kaolin. In these or other embodiments, one or more additives include a combination of fire-class additives and an opacifier.

[0039] Furthermore, the aerogel materials or skeletons of various embodiments of the present disclosure are carried out using aerogel particle-based slurries or suspensions impregnated with reinforcing materials described in various embodiments. Various embodiments of the present disclosure can be carried out using non-particulate aerogel materials produced in situ by impregnating a reinforcing material with various gel precursors in a suitable solvent and subsequently using a supercritical fluid, or by removing the solvent at high temperature and ambient or subcritical pressure.

[0040] In a separate embodiment, the present disclosure includes a thermal control member comprising an aerogel composition, for example, an OCMF-reinforced or fiber-reinforced aerogel composition, which comprises one or more, or even all, of the aforementioned features and properties, including various combinations and methods for manufacturing the same.

[0041] Embodiments of thermal barriers and aerogel compositions disclosed herein are useful for isolating, insulating, and protecting battery cells or battery components of batteries of any configuration, such as pouch cells, cylindrical cells, prismatic cells, and packs and modules incorporating or containing any such cells. The thermal barriers and aerogel compositions disclosed herein are useful for lithium-ion batteries, solid-state batteries, and any other energy storage devices or technologies requiring isolation, insulation, and protection.

[0042] These and other important objectives, advantages, and features of the present invention will become apparent as this disclosure progresses.

[0043] Accordingly, the present invention includes features of structures, combinations of elements, and arrangements of components as illustrated in the disclosure described below, and the scope of the present invention is set forth in the claims. [Brief explanation of the drawing]

[0044] [Figure 1] This chart shows a thermal control member for controlling time-temperature behavior according to a specific embodiment disclosed herein. [Figure 2] This chart shows a thermal control member for controlling time-temperature behavior according to a specific embodiment disclosed herein. [Figure 3] This chart shows the relationship between stress and strain in a thermal control member according to a specific embodiment disclosed herein. [Figure 4] This chart shows a thermal control member for controlling time-temperature behavior according to a specific embodiment disclosed herein. [Figure 5] This is an exemplary thermal control member according to a particular embodiment disclosed herein. [Figure 6] A schematic representation of a thermal control member according to a specific embodiment disclosed herein is shown. [Figure 7] A schematic representation of a thermal control member according to a specific embodiment disclosed herein is shown. [Figure 7]A schematic representation of a thermal control member according to a specific embodiment disclosed herein is shown. [Figure 8] A schematic representation of a thermal control member according to a specific embodiment disclosed herein is shown. [Modes for carrying out the invention]

[0045] The following detailed description of preferred embodiments refers to the accompanying drawings, which form part of the present invention and illustrate specific embodiments in which the invention can be carried out. It should be understood that other embodiments may be utilized and structural modifications may be made without departing from the scope of the invention.

[0046] As used herein and in the appended claims, the singular forms “a,” “an,” and “the” refer to multiple subjects unless the content clearly indicates otherwise. As used herein and in the appended claims, the term “or” is generally used to mean “and / or” unless the context otherwise explicitly indicates otherwise.

[0047] As used herein, “about” means approximately or nearly, and in the context of a given number or range, it means ±5% of the number. In embodiments, the term “about” may include conventional rounding by significant figures of a number. Furthermore, the phrase “about “x” to “y”” includes “about “x” to about “y”.”

[0048] As used herein, the terms “composition” and “complex” are interchangeable.

[0049] Aerogels are a class of porous materials having open pores, comprising a framework of interconnected structures, a corresponding network of pores incorporated within the framework, and an interstitial phase within the network of pores primarily composed of gases such as air. Aerogels are typically characterized by low density, high porosity, large surface area, and small pore size. Aerogels can be distinguished from other porous materials by their physical and structural properties.

[0050] In the context of this disclosure, the terms “aerogel” or “aerogel material” mean a gel that includes a framework of interconnected structures, in which a corresponding network of interconnected pores is incorporated within the framework, and which contains a gas such as air as a dispersed interstitial medium, and which is characterized by the following physical and structural properties attributable to aerogels (as determined by nitrogen porosimetry testing): (a) an average pore diameter in the range of about 2 nm to about 100 nm, (b) a porosity of at least 80%, and (c) a surface area of ​​at least 100 m² / g.

[0051] Accordingly, the aerogel materials of this disclosure include any aerogel or other open-cell materials that satisfy the defining elements set forth in the preceding paragraph and can be classified as xerogels, cryogels, ambigels, microporous materials, etc.

[0052] Aerogel materials can also be further characterized by additional physical properties including (d) a pore volume of about 2.0 mL / g or more, particularly about 3.0 mL / g or more; (e) a density of about 0.50 g / cc or less, particularly about 0.3 g / cc or less, and more particularly about 0.25 g / cc or less; and (f) at least 50% of the total pore volume including pores having pore diameters between 2 and 50 nm (although embodiments disclosed herein include aerogel structures and compositions containing pores having pore diameters greater than 50 nm, as will be described in more detail below). However, these additional properties do not need to be met for characterizing a compound as an aerogel material.

[0053] In the context of this disclosure, the term “innovative processing and extraction techniques” refers to methods of replacing the liquid interstitial phase in a wet gel material with a gas such as air in a manner that causes low pore collapse and low shrinkage of the gel's skeletal structure. Drying techniques, such as ambient pressure evaporation, often introduce strong capillary pressure and other mass transfer limitations at the liquid-vapor interface of the interstitial phase being evaporated or removed. The strong capillary forces resulting from the evaporation or removal of the liquid can cause significant pore shrinkage and skeletal collapse within the gel material. The use of innovative processing and extraction techniques during liquid interstitial phase extraction reduces the adverse effects of capillary forces on pores and the gel's skeletal structure during liquid extraction (also known as solvent removal or drying).

[0054] In certain embodiments, innovative processing and extraction techniques utilize near-critical or supercritical fluids, or near-critical or supercritical conditions, to extract the liquid interstitial phase from a wet gel material. This can be achieved by removing the liquid interstitial phase from the gel near or above the critical point of the liquid or mixture of liquids. Cosolvents and solvent exchanges can be used to optimize the near-critical or supercritical fluid extraction process.

[0055] In certain embodiments, the innovative processing and extraction techniques include modifying the gel skeleton to reduce the irreversible effects of capillary pressure and other mass transfer limits at the liquid-vapor interface. This embodiment may include processing the gel skeleton with hydrophobic agents or other functionalizing agents that enable the gel skeleton to withstand or recover from collapse forces during liquid extraction performed below the critical point of the liquid interplasmic phase. This embodiment may also include incorporating functional groups or skeletal elements that provide a skeletal modulus sufficiently high to withstand or recover from collapse forces during liquid extraction performed below the critical point of the liquid interplasmic phase.

[0056] In the context of this disclosure, the term “skeleton” or “skeleton structure” refers to a network of interconnected oligomers, polymers, or particles that form a solid structure of a material. In the context of this disclosure, the term “aerogel skeleton” or “aerogel skeleton structure” refers to a network of interconnected oligomers, polymers, or colloidal particles that form a solid structure of a gel or aerogel. The polymers or particles constituting an aerogel skeleton structure typically have a diameter of about 100 angstroms. However, the skeleton structure in this disclosure may also include a network of interconnected oligomers, polymers, or colloidal particles of all diameter sizes that form a solid structure within a material such as a gel or aerogel. Furthermore, the term “silica-based aerogel” or “silica-based aerogel skeleton” refers to an aerogel skeleton in which silica is at least 50% (by weight) of the oligomers, polymers, or colloidal particles that form a solid skeleton structure within the gel or aerogel.

[0057] In the context of this disclosure, the term “aerogel composition” refers to any composite material that includes an aerogel material as a component of the composite. Examples of aerogel compositions include, but are not limited to, fiber-reinforced aerogel composites, aerogel composites containing additive elements such as opacifiers, aerogel composites reinforced by an open-cell macroporous skeleton, aerogel-polymer composites, and composites incorporating aerogel microparticles, particles, granules, beads, or powders into a solid or semi-solid material in combination with a binder, resin, cement, foam, polymer, or similar solid material. Aerogel compositions are generally obtained after removing the solvent from the various gel materials disclosed herein. The aerogel compositions thus obtained may be subjected to further additional processing or treatment. The various gel materials may also be subjected to additional processing or treatment that is known or useful in the art before being subjected to solvent removal (or liquid extraction or drying).

[0058] In the context of this disclosure, the term “monolithic” refers to an aerogel material in which the majority (by weight) of the aerogel contained in the aerogel material or composition is in the form of a single interconnected aerogel nanostructure. Monolithic aerogel materials include aerogel materials that are initially formed to have a single interconnected gel or aerogel nanostructure but are subsequently cracked, fractured, or divided into non-integrated aerogel nanostructures. Monolithic aerogel materials are distinguished from granular aerogel materials. The term “granular aerogel material” refers to an aerogel material in which the majority (by weight) of the aerogel contained in the aerogel material is in the form of fine particles, particles, granules, beads, or powders, which can be bound together or compressed but lack the interconnected aerogel nanostructure between the individual particles.

[0059] In the context of this disclosure, the term “wet gel” refers to a gel in which the mobile pore phase within an interconnected network of pores is primarily composed of a liquid such as a conventional solvent, a liquefied gas such as liquid carbon dioxide, or a combination thereof. Aerogels typically require the initial generation of a wet gel and subsequent innovative processing and extraction to replace the mobile pore fluid in the gel with air. Examples of wet gels include, but are not limited to, alcohol gels, hydrogels, ketogels, carbonogels, and any other wet gels known to those skilled in the art.

[0060] The aerogel compositions of this disclosure may include reinforced aerogel compositions. In the context of this disclosure, the term “reinforced aerogel composition” refers to an aerogel composition that includes a reinforcing phase within the aerogel material, the reinforcing phase being not part of the aerogel skeleton itself. The reinforcing phase can be any material that imparts high flexibility, elasticity, conformability or structural stability to the aerogel material. Examples of well-known reinforcing materials include open-cell macroporous skeleton reinforcers, closed-cell macroporous skeleton reinforcers, open-cell membranes, honeycomb reinforcers, polymer reinforcers, and Multiple separate This includes, but is not limited to, fiber-reinforced materials such as fibers, woven fabrics, nonwoven fabrics, needle nonwoven fabrics, batting, webs, mats, and felt.

[0061] In the context of this disclosure, the term “fiber-reinforced aerogel composition” refers to a reinforced aerogel composition that includes a fiber-reinforcement material as a reinforcing phase. Examples of fiber-reinforcement materials are: Multiple separateFiber reinforcements include, but are not limited to, fibers, woven materials, nonwoven materials, bats, batting nets, webs, mats, felts, or combinations thereof. Fiber reinforcements include polyester, polyolefin terephthalate, poly(ethylene) naphthalate, polycarbonate (e.g., rayon, nylon), cotton (e.g., Lycra from DuPont), carbon (e.g., graphite), polyacrylonitrile (PAN), PAN oxide, non-carbonized heat-treated PAN (e.g., from SGL carbon), glass or fiberglass-based materials (e.g., S glass, 901 glass, 902 glass, 475 glass, E glass), silica-based fibers such as quartz (e.g., quartz glass from Saint-Gobain), Q felt (Johns Silica fibers such as Manville, Saffil, Durablanket (Unifrax), and other silica fibers; polyaramid fibers such as Duraback (Carborundum), Kevlar, Nomex, Sontera (all from DuPont), and Conex (Taijin); polyolefins such as Tyvek (DuPont), Dyneema (DSM), and Spectra (Honeywell); other polypropylene fibers such as Typar and Xavan (both from DuPont); fluorinated polymers such as PTFE, which has trade names such as Teflon (DuPont) and Goretex (WLGORE); and Nicalon (COI This includes a variety of materials, including but not limited to silicon carbide fibers (such as Ceramics), ceramic fibers (such as Nextel (3M)), acrylic polymers, wool, silk, hemp, leather, suede, liquid crystal materials such as PBO-Zylon fibers (Tyobo) and Vectan (Hoechst), Cambrelle fibers (DuPont), polyurethane, polyamide, wood fibers, boron, aluminum, iron, stainless steel fibers, and other thermoplastic resins such as PEEK, PES, PEI, PEK, and PPS. Glass or glass fiber-reinforced materials can be manufactured using one or more techniques. In certain embodiments, it is preferable to manufacture them using carding and cross-wrapping or air-laid processes.In exemplary embodiments, carded and cross-wrapped glass or glass fiber-based fiber reinforcements offer certain advantages over airlaid materials. For example, carded and cross-wrapped glass or glass fiber-based fiber reinforcements can provide a consistent material thickness for a given basis weight of the reinforcement. In certain additional embodiments, it is desirable to further needle-process the fiber reinforcement, which requires interlacing of the fibers in the z-direction, in order to improve the mechanical and other properties of the final aerogel composition.

[0062] The reinforced aerogel compositions of the present disclosure may include aerogel compositions reinforced with open-cell macroporous framework materials. In the context of the present disclosure, the terms “open-cell macroporous framework” or “OCMF” refer to a porous material comprising a framework of interconnected structures with a substantially uniform composition, in which a corresponding network of interconnected pores is incorporated within the framework, and characterized by an average pore diameter ranging from about 10 μm to about 700 μm. Such an average pore diameter can be measured by known techniques, including but not limited to microscopy using optical analysis. Accordingly, the OCMF materials of the present disclosure include any open-cell material that satisfies the defining elements set forth in this paragraph, including compounds that could otherwise be classified as foams, foam-like materials, macroporous materials, etc. OCMF materials can be distinguished from materials comprising a framework of interconnected structures that have void volumes within the framework and do not have a uniform composition, such as an assembly of fibers and binders having void volumes within a fiber matrix.

[0063] In the context of this disclosure, the term “substantially uniform composition” refers to the uniformity of the composition of the referred material within a 10% tolerance.

[0064] In the context of this disclosure, the term “OCMF-reinforced aerogel composition” refers to a reinforced aerogel composition comprising an open-cell macroporous skeletal material as a reinforcing phase. Suitable OCMF materials for use in this disclosure include, but are not limited to, OCMF materials made from organic polymer materials. Examples include polyolefins, polyurethanes, and phenols. resinThis includes OCMF materials made from melamine, cellulose acetate, and polystyrene. In the context of this disclosure, the term “organic OCMF” refers to OCMF materials having a backbone primarily composed of organic polymer materials. In certain embodiments, OCMF materials made from melamine or melamine derivatives are also preferred. In the context of this disclosure, the term “melamine OCMF” or “melamine-based OCMF” refers to organic OCMF materials having a backbone primarily composed of polymer materials derived from the reaction of melamine with a condensing agent such as formaldehyde. Examples of OCMF materials made from melamine or melamine derivatives for use in this disclosure are presented in U.S. Patent No. 8,546,457, U.S. Patent No. 4,666,948, and International Publication No. 2001 / 094436. The term “inorganic OCMF” refers to OCMF materials having a backbone primarily composed of inorganic materials. Examples of inorganic OCMF include, but are not limited to, cementitious materials, gypsum, and calcium silicate.

[0065] In the context of this disclosure, the term “Foam” refers to a material formed by dispersing a certain proportion of gas in the form of bubbles into a liquid or resin foam material, such that it comprises a framework of interconnected polymer structures of substantially uniform composition, with corresponding networks or pore aggregates incorporated within the framework, and the bubbles are retained as pores as the foam material solidifies into a solid structure. Generally, foams can be manufactured using a wide variety of processes; see, for example, U.S. Patent No. 6,147,134, U.S. Patent No. 5,889,071, U.S. Patent No. 6,187,831, and U.S. Patent No. 5,229,429. Accordingly, the foams of this disclosure include any material that satisfies the defining elements set forth in this paragraph, including compounds that may be classified as OCMF materials, macroporous materials, etc. The foams as defined in this disclosure may be of the types of thermoplastic resins, elastomers, and thermosetting resins (duromers).

[0066] Pores within a solid framework can also be called “bubbles.” Bubbles can be separated by bubble walls or membranes, creating a collection of independent closed pores within a porous material. The term “closed-cell” refers to a porous material in which at least 50% of the pore volume is enclosed by membranes or walls, making it [substantially] closed-cell. Bubbles in a material can also be interconnected through bubble openings, forming a network of interconnected openings within the material. The term “open-cell” refers to a porous material in which at least 50% of the pore volume is open-cell. Open-cell materials can include reticular open-cell materials, non-reticular open-cell materials, or a combination thereof. Reticular materials are open-cell materials produced by a reticularization process that eliminates or punctures bubble membranes within a porous material. Reticular materials typically have a higher concentration of open-cells than non-reticular materials, but tend to be more expensive and difficult to manufacture. In general, porous materials do not have a completely single type of cellular structure (open-cell or closed-cell). Porous materials can be manufactured using a wide variety of processes, including foam manufacturing processes as presented in U.S. Patent No. 6,147,134, U.S. Patent No. 5,889,071, U.S. Patent No. 6,187,831, U.S. Patent No. 5,229,429, U.S. Patent No. 4,454,248, and U.S. Patent Publication No. 2007 / 0213417.

[0067] In the context of this disclosure, the terms “aerogel blanket” or “aerogel blanket composition” refer to an aerogel composition reinforced with a continuous sheet of reinforcing material. Aerogel blanket compositions can be distinguished from other reinforced aerogel compositions reinforced with discontinuous reinforcing material, such as isolated aggregates or lumps of reinforcing material. Aerogel blanket compositions are highly adaptable and can be used like a blanket to cover surfaces of simple or complex geometric shapes while retaining the excellent thermal insulation properties of aerogel, making them particularly useful in applications requiring flexibility.

[0068] In the context of this disclosure, the terms “flexible” and “flexible” refer to the ability of an aerogel material or composition to be bent or flexed without macrostructural fracture. The aerogel compositions of this disclosure can be bent to at least 5°, at least 25°, at least 45°, at least 65°, or at least 85° without macroscopic fracture, and / or have a bending radius of less than 4 feet, less than 2 feet, less than 1 foot, less than 6 inches, less than 3 inches, less than 2 inches, less than 1 inch, or less than 1 / 2 inch without macroscopic fracture. Similarly, the terms “highly flexible” or “highly flexible” refer to an aerogel material or composition that can be bent to at least 90° without macroscopic fracture, and / or have a bending radius of less than 1 / 2 inch. Furthermore, the terms “classified flexible” and “classified as flexible” refer to an aerogel material or composition that can be classified as flexible according to ASTM C1101 (ASTM International, West Consho Hocken, Pennsylvania).

[0069] The aerogel compositions of this disclosure may be flexible, highly flexible, and / or classified as flexible. The aerogel compositions of this disclosure may also be drapeable. In the context of this disclosure, the terms “drapeable” and “drapeable” refer to the ability of an aerogel material or composition to be bent or flexed by 90° or more with a radius of curvature of about 4 inches or less without macroscopic fracture. The aerogel material or composition according to certain embodiments of this disclosure may be non-rigid and flexible so that the composition can be applied to and adapted to a three-dimensional surface or three-dimensional object, or may be pre-formed into various shapes and configurations to simplify installation or application.

[0070] In the context of this disclosure, the terms “additive” or “additive element” refer to materials that can be added to an aerogel composition before, during, or after the manufacture of an aerogel. Additives can be added to modify or improve desirable properties in an aerogel, or to counteract undesirable properties in an aerogel. Additives are typically added to the aerogel material before gelation into a precursor liquid, during gelation into a transition state material, or after gelation into a solid or semi-solid material. Examples of additives include, but are not limited to, microfibers, fillers, reinforcing agents, stabilizers, thickeners, elastic compounds, opacifiers, coloring or pigmenting compounds, radiation-absorbing compounds, radiation-reflecting compounds, fire-class additives, corrosion inhibitors, thermally conductive components, heat-capacitating components, phase-change materials, pH adjusters, redox adjusters, HCN mitigators, off-gas mitigators, conductive compounds, dielectric compounds, magnetic compounds, radar-shielding components, curing agents, shrinkage inhibitors, and other aerogel additives known to those skilled in the art. In some embodiments, the heat-capacitating components provide at least about 0.3 J / (g) ·℃ This may include materials having a specific heat capacity of at least about 0.5 J / (g). In some embodiments, the material providing the heat capacity is at least about 0.5 J / (g). ·℃ It has a specific heat capacity of ). For example, the material that provides the heat capacity may include metals such as aluminum, titanium, nickel, steel, iron, or combinations thereof. In some embodiments, the thermal control member may include a layer or coating of the material that provides the heat capacity. In some embodiments, the thermal control member may include particles of the material that provides the heat capacity disposed within a layer of the thermal control member. In certain embodiments, the thermal control member may include at least one layer of the material that provides the heat capacity disposed adjacent to the aerogel composition. In certain embodiments, the thermal control member may include at least one layer of the material that provides the heat capacity disposed between at least two of a plurality of layers of the aerogel composition.

[0071] In certain embodiments, the aerogel compositions, reinforced aerogel compositions, and thermal control members disclosed herein can function during high-temperature events, for example, to provide thermal protection during high-temperature events disclosed herein. A high-temperature event lasts for at least 2 seconds and at least about 1 cm 2 At least approximately 25 kW / m² over an area 2 , at least approximately 30 kW / m 2 at least approximately 35 kW / m 2 Or at least about 40 kW / m 2 It is characterized by a sustained heat flux of approximately 40 kW / m². 2 The heat flux is related to the heat flux resulting from a typical fire (Behavior of Charring Solids under Fire-Level Heat Fluxes; Milosavljevic, I., Suuberg, EM; NISTIR 5499; September 1994). In special cases, high-temperature events last for at least 1 minute and reach at least about 10 cm. 2 This represents a heat flux of approximately 40 kW / m² over an area.

[0072] In the context of this disclosure, the terms “thermal conductivity” and “TC” refer to a measure of a material or composition’s ability to transfer heat between two surfaces on either side of a material or composition, where there is a temperature difference between the two surfaces. Thermal conductivity is specifically measured as the thermal energy transferred per unit time and per unit surface area divided by the temperature difference. This is typically recorded in SI units as mW / m*K (milliwatts per meter * Kelvin). The thermal conductivity of materials is not limited to these, but includes the following: Test method for steady-state heat transfer characteristics using a heat flow meter (ASTM C518, ASTM International, West Concho Hocken, Pennsylvania), Test method for steady-state heat flux measurement and heat transfer characteristics using a guarded hot plate apparatus (ASTM C177, ASTM International, West Concho Hocken, Pennsylvania), Test method for steady-state heat transfer characteristics of pipe insulation (ASTM C335, ASTM International, West Concho Hocken, Pennsylvania), Thin-film heater thermal conductivity test (ASTM C1114, ASTM International, West Concho Hocken, Pennsylvania), Standard test method for heat transfer characteristics of thermally conductive electrical insulating materials (ASTM D5470, ASTM International, West Concho Hocken, Pennsylvania), Determination of thermal resistance by protected hot plate and heat flow meter method (EN 12667, British Standards Institution), or Determination of steady-state thermal resistance and related characteristics - guarded hot plate apparatus (ISO It can be determined by test methods known in the art, including 8203 (International Organization for Standardization, Switzerland). Since different methods may yield different results, it should be understood that, unless otherwise specified in the context of this disclosure, thermal conductivity measurements are obtained in the ambient environment at atmospheric pressure, at a temperature of approximately 37.5°C, and under a compressive load of approximately 2 psi, in accordance with the ASTM C518 standard (Test method for steady-state heat transfer characteristics using a heat flow meter). Measurements reported in accordance with ASTM C518 typically correlate well with any measurements performed in accordance with EN 12667 with any relevant adjustments to the compressive load.In certain embodiments, the aerogel material or composition of the present disclosure has a thermal conductivity of about 40 mW / mK or less, about 30 mW / mK or less, about 25 mW / mK or less, about 20 mW / mK or less, about 18 mW / mK or less, about 16 mW / mK or less, about 14 mW / mK or less, about 12 mW / mK or less, about 10 mW / mK or less, about 5 mW / mK or less, or in the range of any two of these values.

[0073] Thermal conductivity measurements can also be obtained under compression, at atmospheric pressure, and at a temperature of approximately 10°C. Thermal conductivity measurements at 10°C are generally 0.5 to 0.7 mW / mK lower than the corresponding thermal conductivity measurements at 37.5°C. In certain embodiments, the aerogel material or composition of the present disclosure has a thermal conductivity of approximately 40 mW / mK or less, approximately 30 mW / mK or less, approximately 25 mW / mK or less, approximately 20 mW / mK or less, approximately 18 mW / mK or less, approximately 16 mW / mK or less, approximately 14 mW / mK or less, approximately 12 mW / mK or less, approximately 10 mW / mK or less, approximately 5 mW / mK or less, or in the range between any two of these values ​​at 10°C.

[0074] In the context of this disclosure, the term “density” refers to a measured mass per unit volume of an aerogel material or composition. The term “density” generally refers to the apparent density of an aerogel material, as well as the bulk density of an aerogel composition. Density is typically recorded as kg / m³ or g / cc. The density of an aerogel material or composition can be determined by methods known in the art, including, but not limited to, standard test methods for the dimensions and density of pre-formed blocks and boards—type insulation (ASTM C303, ASTM International, West Concho Hocken, Pennsylvania), standard test methods for the thickness and density of blanket or butt insulation (ASTM C167, ASTM International, West Concho Hocken, Pennsylvania), determination of the apparent density of pre-formed pipe insulation (EN 13470, British Standards Institution), or determination of the apparent density of pre-formed pipe insulation (ISO 18098, International Organization for Standardization, Switzerland). Because different methods may yield different results, it should be understood that, in the context of this disclosure, unless otherwise specified, density measurements are obtained in accordance with ASTM C167 standard (Standard Test Method for Thickness and Density of Blanket or Butt Insulation) with a compression of 2 psi for thickness measurement. In certain embodiments, the aerogel materials or compositions of this disclosure have densities in the range of about 0.60 g / cc or less, about 0.50 g / cc or less, about 0.40 g / cc or less, about 0.30 g / cc or less, about 0.25 g / cc or less, about 0.20 g / cc or less, about 0.18 g / cc or less, about 0.16 g / cc or less, about 0.14 g / cc or less, about 0.12 g / cc or less, about 0.10 g / cc or less, about 0.05 g / cc or less, about 0.01 g / cc or less, or between any two of these values.

[0075] In the context of this disclosure, the term "hydrophobic" refers to a measure of the ability of an aerogel material or composition to repel water.

[0076] The hydrophobicity of an aerogel material or composition can be expressed in relation to liquid water uptake. In the context of this disclosure, the term “liquid water uptake” refers to a measure of the aerogel material or composition’s ability to absorb or retain liquid water. Liquid water uptake can be expressed as the percentage (by weight or volume) of water absorbed or retained by the aerogel material or composition when exposed to liquid water under specific measurement conditions. The liquid water absorption rate of an aerogel material or composition can be determined by methods known in the art, including, but are not limited to, standard test methods for determining the water retention (repellency) properties of fibrous glass insulators (ASTM C1511, ASTM International, West Consho Hocken, Pennsylvania), standard test methods for water absorption by immersion in insulation materials (ASTM C1763, ASTM International, West Consho Hocken, Pennsylvania), and determination of short-term water absorption by partial immersion in insulation products for building applications (EN 1609, British Standards Institution). Because different methods may yield different results, it should be understood that, in the context of this disclosure, unless otherwise specified, measurements of liquid water uptake are obtained under ambient pressure and ambient temperature in accordance with ASTM C1511 standard (Standard test method for determining water retention (repellency) properties of fibrous glass insulators). In certain embodiments, the aerogel materials or compositions of this disclosure may have liquid water uptake in the range of about 50% by weight or less, about 40% by weight or less, about 30% by weight or less, about 20% by weight or less, about 15% by weight or less, about 10% by weight or less, about 8% by weight or less, about 3% by weight or less, about 2% by weight or less, about 1% by weight or less, about 0.1% by weight or less, or in the range between any two of these values. An aerogel material or composition having improved liquid water uptake compared to another aerogel material or composition has a lower percentage of liquid water uptake / retention compared to a reference aerogel material or composition.

[0077] The hydrophobicity of an aerogel material or composition can be expressed in terms of water vapor uptake. In the context of this disclosure, the term “water vapor uptake” refers to a measure of the aerogel material or composition’s ability to absorb water vapor. Water vapor uptake can be expressed as the percentage (by weight) of water absorbed or retained by the aerogel material or composition when exposed to water vapor under specific measurement conditions. The water vapor absorption of an aerogel material or composition can be determined by methods known in the art, including, but are not limited to, standard test methods for determining water vapor sorption of unexposed mineral fiber insulation materials (ASTM C1104, ASTM International, West Consho Hocken, Pennsylvania) and Insulation products for building applications: Determination of long-term water absorption by diffusion (EN 12088, British Standards Institution). Because different methods may yield different results, it should be understood that, in the context of this disclosure, unless otherwise specified, measurements of water vapor absorption are obtained for 24 hours (modified from 96 hours according to ASTM C1104) at ambient pressure, 49°C, and 95% humidity, according to ASTM C1104 standard (Standard test method for determining water vapor absorption of untreated mineral fiber insulation). In certain embodiments, the aerogel materials or compositions of this disclosure may have water vapor absorption in the range of about 50% by weight or less, about 40% by weight or less, about 30% by weight or less, about 20% by weight or less, about 15% by weight or less, about 10% by weight or less, about 8% by weight or less, about 3% by weight or less, about 2% by weight or less, about 1% by weight or less, about 0.1% by weight or less, or between any two of these values. An aerogel material or composition having improved water vapor absorption compared to another aerogel material or composition has lower water vapor absorption / retention compared to a reference aerogel material or composition.

[0078] The hydrophobicity of an aerogel material or composition can be expressed by measuring the equilibrium contact angle of a water droplet at the interface with the surface of the material. The aerogel materials or compositions of this disclosure may have a water contact angle of about 90° or more, about 120° or more, about 130° or more, about 140° or more, about 150° or more, about 160° or more, about 170° or more, about 175° or more, or in the range of any two of these values.

[0079] In the context of this disclosure, the terms “heat of combustion,” “HOC,” and “ΔHC” refer to measured amounts of thermal energy released during the combustion or exothermic pyrolysis of a material or composition. Heat of combustion is typically recorded as calories (cal / g) of thermal energy released per gram of aerogel material or composition, or as megajoules (MJ / kg) of thermal energy released per kilogram of material or composition. The heat of combustion of a material or composition can be determined by methods known in the art, including, but not limited to, the reaction-to-determination of total heat of combustion (calorific value) for combustion tests of products (EN ISO 1716, International Organization for Standardization, Switzerland; adopted by EN). In the context of this disclosure, unless otherwise specified, heat of combustion measurements are obtained in accordance with the EN ISO 1716 standard (reaction-to-combustion tests of products - determination of total heat of combustion (calorific value)). In certain embodiments, the aerogel compositions of the present disclosure may have a heat of combustion of about 750 cal / g or less, about 717 cal / g or less, about 700 cal / g or less, about 650 cal / g or less, about 600 cal / g or less, about 575 cal / g or less, about 550 cal / g or less, about 500 cal / g or less, about 450 cal / g or less, about 400 cal / g or less, about 350 cal / g or less, about 300 cal / g or less, about 250 cal / g or less, about 200 cal / g or less, about 150 cal / g or less, about 100 cal / g or less, about 50 cal / g or less, about 25 cal / g or less, about 10 cal / g or less, or in the range between any two of these values. An aerogel composition having improved heat of combustion compared to another aerogel composition has a lower heat of combustion value compared to a reference aerogel composition. In certain embodiments of this disclosure, the HOC of the aerogel complex is improved by incorporating fire-class additives into the aerogel complex.

[0080] Within the context of this disclosure, all thermal analyses and related definitions refer to measurements performed by starting at 25°C and raising the temperature to 1000°C at a rate of 20°C / min in air at ambient pressure. Therefore, changes in these parameters must be considered (or re-executed under these conditions) when measuring and calculating the onset of pyrolysis, peak heat release temperature, peak sound absorption temperature, etc. Within the context of this disclosure, the terms “onset of pyrolysis” and “TD” refer to the measured ambient temperature at which a rapid exothermic reaction from the decomposition of an organic material appears within the material or composition. The onset of pyrolysis of an organic material within a material or composition can be measured using thermogravimetric analysis (TGA). The TGA curve of a material shows the weight loss (mass%) of the material as it is exposed to an increase in ambient temperature, and thus indicates pyrolysis. The onset of pyrolysis of a material can be correlated with the intersection of the following tangents to the TGA curve: the line tangent to the baseline of the TGA curve, and the line tangent to the TGA curve at the point of maximum gradient during the rapid exothermic decomposition event associated with the decomposition of an organic material. Within the context of this disclosure, unless otherwise specified, measurements of the onset of thermal decomposition of organic materials are obtained using the TGA analysis provided in this paragraph.

[0081] The onset of thermal decomposition of a material can also be measured using differential scanning calorimetry (DSC) analysis. The DSC curve of a material shows the thermal energy (mW / mg) released by the material as it is exposed to a gradual increase in ambient temperature. The onset of thermal decomposition temperature of a material can correlate with the point on the DSC curve where ΔmW / mg (change in thermal energy output) increases most maximally, thus indicating exothermic reaction from aerogel materials. In the context of this disclosure, measurements of the onset of thermal decomposition using DSC, TGA, or both are obtained using a temperature gradient rate of 20°C / min, as further defined in the previous paragraph, unless otherwise specified. DSC and TGA each provide similar values ​​for this onset of thermal decomposition, and often the tests are performed simultaneously, resulting in results from both. In certain embodiments, the aerogel materials or compositions of the Disclosure have an initiation of thermal decomposition at a range of about 300°C or higher, about 320°C or higher, about 340°C or higher, about 360°C or higher, about 380°C or higher, about 400°C or higher, about 420°C or higher, about 440°C or higher, about 460°C or higher, about 480°C or higher, about 500°C or higher, about 550°C or higher, about 600°C or higher, or between any two of these values. In the context of this Spec, for example, a first composition having a higher initiation of thermal decomposition than a second composition is considered an improvement over the second composition. Herein, the initiation of thermal decomposition of a composition or material is intended to increase with the addition of one or more fire-class additives compared to a composition without any fire-class additives.

[0082] In the context of this disclosure, the terms “initiation of endothermic decomposition” and “TED” refer to the measured ambient temperature at which an endothermic reaction from decomposition or dehydration occurs within the material or composition. The initiation of endothermic decomposition of a material or composition can be measured using thermogravimetric analysis (TGA). The TGA curve of a material shows the weight loss (mass%) of the material as it is exposed to an increase in ambient temperature. The initiation of thermal decomposition of a material can be correlated with the intersection of the following tangents to the TGA curve: the line tangent to the baseline of the TGA curve and the line tangent to the TGA curve at the point of maximum gradient during rapid endothermic decomposition or dehydration of the material. In the context of this disclosure, unless otherwise specified, the measured values ​​of the initiation of endothermic decomposition of a material or composition are obtained using the TGA analysis provided in this paragraph.

[0083] In the context of this disclosure, the terms “furnace temperature rise” and “ΔTR” refer to a measured difference between the maximum temperature (TMAX) of a material or composition under pyrolysis conditions and the baseline temperature (usually the final temperature, i.e., TFIN) of that material or composition under pyrolysis conditions. Furnace temperature rises are typically recorded in degrees Celsius or °C. Furnace temperature rises of materials or compositions can be determined by methods known in the art, including, but not limited to, the reaction to fire tests for the construction and transport of products: non-flammability tests (EN ISO 1182, International Organization for Standardization, Switzerland; EN adopted). In the context of this disclosure, unless otherwise specified, furnace temperature rise measurements are obtained in accordance with conditions equivalent to those of the EN ISO 1182 standard (reaction to fire tests for the construction and transport of products: non-flammability tests). In certain embodiments, the aerogel compositions of this disclosure may have furnace temperature rises in the range of about 100°C or less, about 90°C or less, about 80°C or less, about 70°C or less, about 60°C or less, about 50°C or less, about 45°C or less, about 40°C or less, about 38°C or less, about 36°C or less, about 34°C or less, about 32°C or less, about 30°C or less, about 28°C or less, about 26°C or less, about 24°C or less, or between any two of these values. In the context of compositional stability at high temperatures, for example, a first composition having a furnace temperature rise lower than that of a second composition is considered an improvement over the second composition. Herein, the furnace temperature rise of a composition is intended to be reduced by the addition of one or more fire-class additives compared to a composition without any fire-class additives.

[0084] In the context of this disclosure, the terms “flame time” and “TFLAME” refer to the measurement of a sustained flame of a material or composition under thermal decomposition conditions, where “sustained flame” is the persistence of a flame in any part of the visible portion of a specimen lasting for 5 seconds or more. Flame times are typically recorded in seconds or minutes. The flame times of a material or composition can be determined by methods known in the art, including, but not limited to, the reaction to fire tests for the construction and transport of products: non-flammability tests (EN ISO 1182, International Organization for Standardization, Switzerland; EN adopted). In the context of this disclosure, unless otherwise specified, flame time measurements are obtained in accordance with conditions equivalent to those of the EN ISO 1182 standard (reaction to fire tests for the construction and transport of products: non-flammability tests). In certain embodiments, the aerogel compositions of the Disclosure have a flame time in the range of about 30 seconds or less, about 25 seconds or less, about 20 seconds or less, about 15 seconds or less, about 10 seconds or less, about 5 seconds or less, about 2 seconds or less, or any two of these values. In the context of this Spec, for example, a first composition having a lower flame time than a second composition is considered an improvement over the second composition. Herein, the flame time of a composition is intended to be reduced by adding one or more fire-class additives compared to a composition without any fire-class additives.

[0085] In the context of this disclosure, the terms “mass loss” and “ΔM” refer to measured amounts of material, composition, or composite material lost or burned under thermal decomposition conditions. Mass loss is typically recorded as a weight percentage or weight %. The mass loss of a material, composition, or composite material can be determined by methods known in the art, including, but not limited to, the reaction to fire tests for the construction and transport of a product: non-flammability test (EN ISO 1182, International Organization for Standardization, Switzerland; EN adopted). In the context of this disclosure, unless otherwise specified, mass loss measurements are obtained in accordance with conditions equivalent to those of the EN ISO 1182 standard (reaction to fire tests for the construction and transport of a product: non-flammability test). In certain embodiments, the aerogel compositions of this disclosure may have a mass loss of about 50% or less, about 40% or less, about 30% or less, about 28% or less, about 26% or less, about 24% or less, about 22% or less, about 20% or less, about 18% or less, about 16% or less, or a range between any two of these values. In the context of this specification, for example, a first composition having a mass loss lower than that of a second composition is considered an improvement over the second composition. Herein, the mass loss of a composition is intended to be reduced by adding one or more Fire Class additives compared to a composition without any Fire Class additives.

[0086] In the context of this disclosure, the term “peak heat release temperature” refers to a measured value of the ambient heat temperature at which the exothermic heat release from decomposition is maximum. The peak heat release temperature of a material or composition can be measured using TGA analysis, differential scanning calorimetry (DSC), or a combination thereof. DSC and TGA each provide similar values ​​for peak heat release temperature, and often the tests are performed simultaneously, resulting in results from both. In a typical DSC analysis, the heat flow is plotted against the rising temperature, and the peak heat release temperature is the temperature at which the highest peak occurs in such a curve. In the context of this disclosure, unless otherwise specified, measured values ​​of the peak heat release temperature of a material or composition are obtained using the TGA analysis provided in this paragraph.

[0087] In the context of endothermic materials, the term “peak endothermic temperature” refers to a measured value of the ambient heat temperature at which the endothermic reaction from decomposition is minimized. The peak endothermic temperature of a material or composition can be measured using TGA analysis, differential scanning calorimetry (DSC), or a combination thereof. In a typical DSC analysis, the heat flow is plotted against the rising temperature, and the peak heat absorption temperature is the temperature at which the lowest peak of such a curve occurs. In the context of this disclosure, unless otherwise specified, measured values ​​of the peak endothermic temperature of a material or composition are obtained using the TGA analysis provided in this paragraph.

[0088] In the context of this disclosure, the terms “low flammability” and “low flammability” refer to materials or compositions that satisfy the following combinations of properties: i) furnace temperature rise of 50°C or less, ii) flame time of 20 seconds or less, and iii) mass loss rate of 50 wt% or less. In the context of this disclosure, the terms “non-flammability” and “non-flammability” refer to materials or compositions that satisfy the following combinations of properties: i) furnace temperature rise of 40°C or less, ii) flame time of 2 seconds or less, and iii) mass loss rate of 30 wt% or less. As described herein, the flammability of a composition (e.g., a combination of furnace temperature rise, flame time, and mass loss) is intended to be reduced by the inclusion of one or more fire-class additives.

[0089] In the context of this disclosure, the terms “low flammability” and “low flammability” refer to low flammability materials or compositions having a total heat of combustion (HOC) of 3 MJ / kg or less. In the context of this disclosure, the terms “non-flammable” and “non-flammability” refer to non-flammable materials or compositions having a heat of combustion (HOC) of 2 MJ / kg or less. The HOC of a composition is intended to be reduced by including one or more fire-class additives as described herein.

[0090] Aerogels are described as interconnected structural skeletons most commonly composed of interconnected oligomers, polymers, or colloidal particles. Aerogel skeletons can be fabricated from a range of precursor materials, including inorganic precursor materials (such as precursors used in the production of silica-based aerogels), organic precursor materials (such as precursors used in the production of carbon-based aerogels), hybrid inorganic / organic precursor materials, and combinations thereof. In the context of this disclosure, the term “amalgam aerogel” refers to an aerogel fabricated from a combination of two or more different gel precursors, the corresponding precursors being referred to as “amalgam precursors.”

[0091] Inorganic aerogels are generally formed from metal oxide or metal alkoxide materials. These materials can be based on oxides or alkoxides of any metal capable of forming oxides. Such metals include, but are not limited to, silicon, aluminum, titanium, zirconium, hafnium, yttrium, vanadium, and cerium. Inorganic silica aerogels are conventionally produced by hydrolysis and condensation of silica-based alkoxides (such as tetraethoxysilane) or by gelation of silicic acid or water glass. Other relevant inorganic precursor materials for silica-based aerogel synthesis include, but are not limited to, metal silicates such as sodium silicate or potassium silicate, alkoxysilanes, partially hydrolyzed alkoxysilanes, tetraethoxysilane (TEOS), partially hydrolyzed TEOS, condensed polymers of TEOS, tetramethoxysilane (TMOS), partially hydrolyzed condensed polymers of TMOS, condensed polymers of TMOS, tetra-n-propoxysilane, partially hydrolyzed and / or condensed polymers of tetra-n-propoxysilane, polyethylsilicates, partially hydrolyzed polyethylsilicates, monomeric alkylalkoxysilanes, bis-trialkoxyalkyl or arylsilanes, polysilsesquioxanes, or combinations thereof.

[0092] In certain embodiments of this disclosure, a pre-hydrolyzed TEOS, such as Silbond H-5 (SBH5, Silbond Corp.), which is hydrolyzed at a water / silica ratio of about 1.9 to 2, may be used as a commercially available product or may be further hydrolyzed before being incorporated into the gelling process. Partially hydrolyzed TEOS or TMOS, such as polyethyl silicate (Silbond 40) or polymethyl silicate, may also be used as a commercially available product or may be further hydrolyzed before being incorporated into the gelling process.

[0093] Inorganic aerogels may also contain gel precursors comprising at least one hydrophobic group, such as alkyl metal alkoxides, cycloalkyl metal alkoxides, and aryl metal alkoxides, which can impart or improve certain properties in the gel, such as stability and hydrophobicity. Inorganic silica aerogels may particularly contain hydrophobic precursors such as alkylsilanes or arylsilanes. Hydrophobic gel precursors can be used as primary precursor materials for forming the backbone of gel materials. However, hydrophobic gel precursors are more commonly used as co-precursors in combination with simple metal alkoxides in the formation of amalgam aerogels. Hydrophobic inorganic precursor materials for silica-based aerogel synthesis include, but are not limited to, trimethylmethoxysilane (TMS), dimethyldimethoxysilane (DMS), methyltrimethoxysilane (MTMS), trimethylethoxysilane, dimethyldiethoxysilane (DMDS), methyltriethoxysilane (MTES), ethyltriethoxysilane (ETES), diethyldiethoxysilane, dimethyldiethoxysilane (DMDES), ethyltriethoxysilane, propyltrimethoxysilane, propyltriethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane (PhTES), hexamethyldisilazane, and hexaethyldisilazane. Any derivative of any of the above precursors may be used, specifically, certain polymers of other chemical groups may be added to or crosslinked to one or more of the above precursors.

[0094] Aerogels may also be treated to impart or improve hydrophobicity. Hydrophobic treatment can be applied to sol-gel solutions, wet gels before liquid extraction, or aerogels after liquid extraction. Hydrophobic treatment is particularly common in the production of metal oxide aerogels, such as silica aerogels. Examples of hydrophobic treatment of gels are discussed below in more detail, specifically in relation to the treatment of wet gels of silica gel. However, the specific examples and illustrations provided herein are not intended to limit the scope of this disclosure to any particular type of hydrophobic treatment procedure or aerogel substrate. This disclosure may include any gel or aerogel known to those skilled in the art, as well as related methods for hydrophobic treatment of aerogels in either wet gel or dry aerogel form.

[0095] Hydrophobicization is carried out by reacting the hydroxyl moieties on the gel, such as silanol groups (Si-OH) present on the silica gel skeleton, with the functional groups of the hydrophobic agent. The resulting reaction converts the silanol groups and the hydrophobic agent into hydrophobic groups on the silica gel skeleton. Hydrophobic agent compounds can react with hydroxyl groups on the gel according to the following reaction: N MX 4-N (Hydrophobic agent) + MOH (Silanol) → MOMR N (Hydrophobic group) + HX. Hydrophobic treatment can be performed on both the outer macrosurface of silica gel and the inner pore surface within the porous network of the gel.

[0096] The gel can be immersed in a mixture of a hydrophobic agent and any hydrophobic treatment solvent in which the hydrophobic agent is soluble and which is also miscible with the gel solvent in the wet gel. A wide range of hydrophobic treatment solvents can be used, including methanol, ethanol, isopropanol, xylene, toluene, benzene, dimethylformamide, and hexane. Hydrophobicity may also be imparted by directly contacting the gel with the hydrophobic agent in liquid or gaseous form.

[0097] The hydrophobic treatment process may include mixing or stirring to help the hydrophobic agent permeate the wet gel. The hydrophobic treatment process may also include changing other conditions such as temperature and pH to further enhance and optimize the treatment reaction. After the reaction is complete, the wet gel is washed to remove any unreacted compounds or reaction byproducts.

[0098] Hydrophobic agents for the hydrophobic treatment of aerogels are generally given by formula:R N MX 4-N The compound is of the formula: Y(R3M)2; where M is a metal, R is a hydrophobic group such as CH3, CH2CH3, C6H6, or a similar hydrophobic alkyl, cycloalkyl, or aryl moiety, and X is a halogen, usually Cl. Specific examples of hydrophobic agents include, but are not limited to, trimethylchlorosilane (TMCS), triethylchlorosilane (TECS), triphenylchlorosilane (TPCS), dimethylchlorosilane (DMCS), and dimethyldichlorosilane (DMDCS). The hydrophobic agent can be of the formula: Y(R3M)2; where M is a metal, Y is a crosslinking group such as NH or O, and R is a hydrophobic group such as CH3, CH2CH3, C6H6, or a similar hydrophobic alkyl, cycloalkyl, or aryl moite. Specific examples of such hydrophobic agents include, but are not limited to, hexamethyldisilazane [HMDZ] and hexamethyldisiloxane [HMDSO]. Hydrophobic agents are, formula: R N MV 4-N The formula may further include compounds where V is a reactive or leaving group other than a halogen. Specific examples of such hydrophobic agents include, but are not limited to, vinyltriethoxysilane and vinyltrimethoxysilane.

[0099] The hydrophobic treatments of this disclosure may also be carried out during the removal, replacement, or drying of liquid in the gel. In certain embodiments, the hydrophobic treatment may be carried out in a supercritical fluid environment (e.g., supercritical carbon dioxide) and may be combined with a drying or extraction step.

[0100] In the context of this disclosure, the term “hydrophobic-bonded silicon” refers to a silicon atom in a gel or aerogel skeleton containing at least one hydrophobic group covalently bonded to the silicon atom. Examples of hydrophobic-bonded silicon include, but are not limited to, silicon atoms in silica groups in a gel skeleton formed from a gel precursor containing at least one hydrophobic group (such as MTES or DMDS). Hydrophobic-bonded silicon may also include, but are not limited to, silicon atoms in or on the surface of a gel skeleton, which are treated with a hydrophobicizing agent (such as HMDZ) to impart or improve hydrophobicity by incorporating further hydrophobic groups into the composition. Hydrophobic groups in this disclosure include, but are not limited to, methyl, ethyl, propyl, isopropyl, butyl, isobutyl, tert-butyl, octyl, phenyl, or other substituted or unsubstituted hydrophobic organic groups known to those skilled in the art. In the context of this disclosure, the terms “hydrophobic group,” “hydrophobic organic material,” and “hydrophobic organic content” specifically exclude readily hydrolyzable organosilicon-bonded alkoxy groups on the gel material's backbone, which are products of reactions between organic solvents and silanol groups. Such excluded groups can be distinguished from their hydrophobic organic content by NMR analysis. The amount of hydrophobic-bonded silicon contained in the aerogel is determined by CP / MAS 29 Aerogels can be analyzed using NMR spectroscopy, such as Si solid-state NMR. NMR analysis of aerogels allows for the characterization and relative quantification of M-type hydrophobic silicon (monofunctional silica such as TMS derivatives), D-type hydrophobic silicon (bifunctional silica such as DMDS derivatives), T-type hydrophobic silicon (trifunctional silica such as MTES derivatives), and Q-type silicon (tetrafunctional silica such as TEOS derivatives). NMR analysis can also classify specific types of hydrophobic silicon into subtypes (e.g., T-type hydrophobic silicon). 1 seeds, T 2 species and T 3By enabling classification into species, it can be used to analyze the bonding chemistry of hydrophobic silicon contained in aerogels. Specific details regarding the NMR analysis of silica materials can be found in the paper "Applications of Solid-State NMR to the Study of Organic / Inorganic Multicomponent Materials" by Geppi et al., specifically pages 7-9 (Appl.Spec.Rev.(2008),44-1:1-89), which is incorporated herein by reference according to the specifically cited pages.

[0101] CP / MAS 29 The characterization of hydrophobic silicon in Si NMR analysis can be based on the following chemical shift peaks: M 1 (30 to 10 ppm), D 1 (10 to -10 ppm), D 2 (-10 to -20 ppm), T 1 (-30 to -40 ppm), T 2 (-40 to -50 ppm), T 3 (-50 to -70 ppm), Q 2 (-70 to -85 ppm), Q 3 (-85 to -95 ppm), Q 4 (-95 to -110 ppm). These chemical shift peaks are approximate and illustrative, and are not intended to be restrictive or definitive. The exact chemical shift peaks resulting from various silicon species in the material may depend on the specific chemical composition of the material and can generally be deciphered by routine experiments and analyses by those skilled in the art.

[0102] In the context of this disclosure, the terms “hydrophobic organic content” or “hydrophobic substance content” or “hydrophobic content” refer to the amount of hydrophobic organic material bound to the skeleton in an aerogel material or composition. The hydrophobic organic content of an aerogel material or composition can be expressed as a weight percentage of the amount of hydrophobic organic material on the aerogel skeleton relative to the total amount of material in the aerogel material or composition. The hydrophobic organic content can be calculated by those skilled in the art based on the properties and relative concentrations of the materials used in the manufacture of the aerogel material or composition. The hydrophobic organic content can also be measured using thermogravimetric analysis (TGA) of the material in question, preferably in an oxygen atmosphere (however, TGA in an alternative gas environment is also useful). Specifically, the proportion of hydrophobic organic material in the aerogel can be correlated with the proportion of weight loss in the hydrophobic aerogel material or composition when exposed to the heat of combustion temperature during TGA analysis, with adjustments made for water loss, residual solvent loss, and loss of readily hydrolyzable alkoxy groups during TGA analysis. Other alternative techniques known to those skilled in the art, such as differential scanning calorimetry, elemental analysis (particularly carbon), chromatography, nuclear magnetic resonance spectroscopy, and other analytical techniques, can be used to measure and determine the hydrophobic content in the aerogel compositions of this disclosure. In certain examples, a combination of known techniques may be useful or necessary to determine the hydrophobic content of the aerogel compositions of this disclosure.

[0103] The aerogel material or composition of this disclosure may have a hydrophobic organic content of 50% by weight or less, 40% by weight or less, 30% by weight or less, 25% by weight or less, 20% by weight or less, 15% by weight or less, 10% by weight or less, 8% by weight or less, 6% by weight or less, 5% by weight or less, 4% by weight or less, 3% by weight or less, 2% by weight or less, 1% by weight or less, or in a range between any two of these values.

[0104] The term "fuel content" refers to the total amount of flammable material in an aerogel material or composition, which can be correlated with the total percentage of weight loss in the aerogel material or composition when exposed to a flammable thermal temperature during TGA or TG-DSC analysis, with adjustments made for water loss. The fuel content of an aerogel material or composition may include hydrophobic organic content, as well as other flammable residual alcoholic solvents, filler materials, reinforcing materials, and readily hydrolyzable alkoxy groups.

[0105] Organic aerogels are generally formed from carbon-based polymer precursors. Such polymer materials include, but are not limited to, resorcinol formaldehyde (RF), polyimides, polyacrylates, polymethyl methacrylates, acrylate oligomers, polyoxyalkylenes, polyurethanes, polyphenols, polybutadienes, trialkoxysilyl-terminated polydimethylsiloxanes, polystyrene, polyacrylonitriles, polyfurfural, melamine-formaldehyde, cresol formaldehyde, phenol-furfural, polyethers, polyols, polyisocyanates, polyhydroxybenzes, polyvinyl alcohol dialdehydes, polycyanurates, polyacrylamides, various epoxies, agars, chitosans, and combinations thereof. As an example, organic RF aerogels are typically produced from sol-gel polymerization of resorcinol or melamine with formaldehyde under alkaline conditions.

[0106] Organic / inorganic hybrid aerogels are primarily composed of organically modified silica ("ormosyl") aerogels. These ormosyl materials contain organic components covalently bonded to a silica network. Ormosyl is typically formed by the hydrolysis and condensation of an organically modified silane, R-Si(OX)3, with a conventional alkoxide precursor, Y(OX)4. In these formulas, X can represent, for example, CH3, C2H5, C3H7, or C4H9; Y can represent, for example, Si, Ti, Zr, or Al; and R may be any organic fragment such as methyl, ethyl, propyl, butyl, isopropyl, methacrylate, acrylate, vinyl, or epoxide. The organic components in the ormosyl aerogel may also be dispersed throughout the silica network or chemically bonded to the silica network.

[0107] In the context of this disclosure, the term “Ormosil” encompasses the aforementioned materials as well as other organically modified materials sometimes referred to as “Ormocar.” Ormosil is often used as a coating, for example, by casting an ormosil film onto a substrate material by a sol-gel method. Other examples of organic-inorganic hybrid aerogels in this disclosure include, but are not limited to, silica polyethers, silica-PMMA, silica-chitosan, carbides, nitrides, and other combinations of the organic and inorganic aerogel-forming compounds described above. Published U.S. Patent Application Publication No. 20050192367 (paragraphs

[0022] –

[0038] and

[0044] –

[0058] ) contains teachings of such hybrid organic-inorganic materials and is incorporated herein by reference in accordance with the sections and paragraphs cited individually.

[0108] In certain embodiments, the aerogels of the present disclosure are primarily inorganic silica aerogels formed from prepolymerized silica precursors, preferably as oligomers, or hydrolyzed silicates formed from silicon alkoxides in an alcohol solvent. In certain embodiments, such prepolymerized silica precursors or hydrolyzed silicates can be formed in situ from other precursors or silicates, such as alkoxysilanes or water glass. However, the present disclosure as a whole may be carried out using any other aerogel compositions known to those skilled in the art, and is not limited to any one precursor material or amalgam mixture of precursor materials.

[0109] As described above, the aerogel compositions according to embodiments of this disclosure provide desirable properties for compressibility, compressive elasticity, and compliance. When used as separators between cells in a battery module, the insulating sheets formed using the aerogel compositions provide resistance to compressive deformation, allowing them to accommodate cell expansion due to decomposition and swelling of the active material during the battery's charge / discharge cycle. During the initial assembly of the battery module, relatively low loads of 1 MPa or less are typically applied to the cell separator material, e.g., the reinforced aerogel compositions disclosed herein. As cells in the battery module expand or swell during the charge / discharge cycle, loads of up to approximately 5 MPa may be applied to the cell separator material, e.g., the reinforced aerogel compositions disclosed herein. Therefore, compressibility, compressive elasticity, and compliance of the cell separator material are important properties.

[0110] In exemplary embodiments, the Disclosure provides a thermal control member comprising an aerogel composition, which exhibits a compressibility of less than about 25% at about 25 kPa. Optionally, when the compression is released, the thermal control member may have sufficient elasticity to return to at least about 80%, 75%, 65%, 60%, or 50% of its original thickness. In some embodiments, the thermal control member exhibits a compressibility of less than about 25% in the range of about 25 kPa to about 35 kPa, preferably less than about 50% at about 50 kPa. In some embodiments, the thermal control member exhibits a compressibility in the range of about 25% to about 50% at about 50 kPa. In exemplary embodiments, the thermal control member exhibits a compressibility of less than about 80% at about 245 kPa, for example, less than about 70% at about 235 kPa. In exemplary embodiments, the thermal control member exhibits a compressibility of less than about 70% at about 345 kPa. The thermal conductivity of the thermal control member containing the reinforced aerogel composition is preferably maintained at less than about 25 mW / m*K when the thermal control member is compressed.

[0111] As described above, the aerogel compositions according to embodiments of the present disclosure may include an aerogel framework containing macropores. While not bound by any particular operating theory, the presence of macropores within the aerogel framework can allow for compression of the aerogel composition, such as a reinforced aerogel composition, while maintaining or further improving its thermal properties, such as reducing thermal conductivity. For example, macropores can be deformed, crushed, or otherwise reduced in size by compression of the composition, thereby reducing the thickness of the composition under load. However, as the macropores deform, they become more efficient at transferring heat to smaller pores. As a result, the pathways for heat transfer within the aerogel framework may become more winding as the macropores deform, thereby improving the thermal properties, such as reducing thermal conductivity. In the context of the present disclosure, “mesopore” refers to pores with an average pore diameter in the range of about 2 nm to about 50 nm. Aerogel structures are typically mesoporous (i.e., primarily containing pores with an average diameter in the range of about 2 nm to about 50 nm). In certain embodiments, the aerogel skeleton of the aerogel composition of the present disclosure may include macropores. In the context of the present disclosure, “macropore” refers to a pore with an average pore diameter greater than about 50 nm. The aerogel skeleton may include both macropores and mesopores. For example, at least 10% of the pore volume of the aerogel skeleton may consist of macropores, at least 5% of the pore volume of the aerogel skeleton may consist of macropores, at least 75% of the pore volume of the aerogel skeleton may consist of macropores, at least 95% of the pore volume of the aerogel skeleton may consist of macropores, or 100% of the pore volume of the aerogel skeleton may consist of macropores. In some specific embodiments, the aerogel skeleton may be a macroporous aerogel skeleton such that the majority of its pore volume consists of macropores. In some examples, the macroporous aerogel skeleton may also include micropores and / or mesopores.In some embodiments, the average pore diameter (diameter) of the pores in the aerogel framework can be greater than 50 nm, 50 nm to 5000 nm, 250 nm to 2000 nm, 500 nm to 2000 nm, 500 nm to 1400 nm, or greater than 1200 nm. In certain embodiments, the average pore diameter can be greater than 50 nm, greater than 50 nm to 1000 nm, preferably 100 nm to 800 nm, and more preferably 250 nm to 750 nm.

[0112] In some embodiments, variations in pore size within the aerogel framework can be uniformly distributed throughout the aerogel framework. For example, the average pore size can be substantially the same across the entire aerogel framework.

[0113] In other embodiments, variations in pore size within the aerogel framework can be distributed non-uniformly throughout the aerogel framework. For example, the average pore diameter can differ in specific regions of the aerogel framework. In some exemplary embodiments, the average pore diameter can be larger in the upper surface, lower surface, or both upper and lower surfaces of the aerogel framework. For example, macropores can be distributed within the composition such that the ratio of macropores to mesopores is greater on the upper surface than on the lower surface, greater on the lower surface than on the upper surface, or greater on both the upper and lower surfaces than in the central region between the upper and lower surfaces. In another example, macropores can be distributed within the composition such that the ratio of macropores to mesopores is greater near the upper surface than near the upper surface, greater near the lower surface than near the upper surface, or greater near both the upper and lower surfaces than in the central region between the upper and lower surfaces. In other embodiments, the average pore diameter can be larger in the intermediate region between the upper and lower surfaces of the aerogel framework.

[0114] Macropores can be formed during the production of an aerogel composition. For example, macropore formation can be induced in the gel precursor material during the transition to the gel composition. In some embodiments, macropore formation can be achieved, for example, by inducing spinodal decomposition of the gel precursor solution. In another example, macropore formation can be induced by the addition of one or more foaming agents.

[0115] The macropores present in the resulting aerogel framework can be formed by selecting processing conditions that are favorable for the formation of macropores versus mesopores and / or micropores. The amount of macropores can be adjusted by performing any one, any combination, or all of the following variables: (1) polymerization solvent, (2) polymerization temperature, (3) polymer molecular weight, (4) molecular weight distribution, (5) copolymer composition, (6) branching amount, (7) crosslinking amount, (8) branching method, (9) crosslinking method, (10) method used for gel formation, (11) type of catalyst used for gel formation, (12) chemical composition of catalyst used for gel formation, (13) amount of catalyst used for gel formation, (14) gel formation temperature, (15) type of gas flowing over the material during gel formation, (16) velocity of gas flowing over the material during gel formation, (17) atmospheric pressure during gel formation, (18) removal of dissolved gases during gel formation, (19) presence of solid additives in the resin during gel formation, (20) duration of the gel formation process, (21) substrate used for gel formation, (22) type of solvent used in each step of the solvent exchange process, (23) (24) the composition of the solvent used, (25) the time used in each step of the solvent exchange process, (26) the residence time of the portion in each step of the solvent exchange process, (27) the flow rate of the solvent exchange solvent, (28) the type of flow of the solvent exchange solvent, (29) the stirring speed of the solvent exchange solvent, (30) the temperature used in each step of the solvent exchange process, (31) the ratio of the volume of the solvent exchange solvent to the volume of the portion, (32) the drying method, (33) the temperature in each step of the drying process, (34) the composition of the gas used in each step of the drying process, (35) the gas flow rate in each step of the drying process, (36) the gas temperature in each step of the drying process, (37) the temperature of the portion in each step of the drying process, (38) the presence of an enclosure around the portion in each step of the drying process, (39) the type of enclosure surrounding the portion during drying, and / or (40) the solvent used in each step of the drying process.The polyfunctional amine and diamine compounds can be added as solids, either as is or dissolved in a suitable solvent, separately or together in one or more parts. In other embodiments, a method for producing an aerogel may include (a) providing the polyfunctional amine compound and at least one diamine compound in a solvent to form a solution; (b) providing at least one dianhydride compound to the solution of step (a) under conditions sufficient to form a branched polymer matrix solution, wherein the branched polymer matrix is ​​solubilized in the solution; and (c) subjecting the branched polymer matrix solution to conditions sufficient to form an aerogel having an open-cell structure. The macropores present in the resulting aerogel skeleton can be formed by the methods described above. In one preferred non-limiting embodiment, the formation of mesopores and micropores smaller than macropore pairs can be controlled primarily by controlling the polymer / solvent dynamics during gel formation.

[0116] As described above, the aerogel compositions according to embodiments of the present disclosure may include an aerogel skeleton and a reinforcing material in which at least a portion of the reinforcing material is aerogel-free. For example, the aerogel skeleton may extend partially through the thickness of the reinforcing material. In such embodiments, a portion of the reinforcing material, such as OCMF, fibers, or a combination thereof, may include aerogel material and a portion may be aerogel-free. For example, in some embodiments, the aerogel extends through about 90% of the thickness of the reinforcing material, in the range of about 50% to about 90% of the thickness of the reinforcing material, in the range of about 10% to about 50% of the thickness of the reinforcing material, or in the range of about 10% of the thickness of the reinforcing material.

[0117] Without being bound by any particular operating theory, an aerogel composition in which at least a portion of the reinforcing material does not contain aerogel can provide desirable properties for compressibility, compressive elasticity, and compliance. For example, the properties of the reinforcing material can be selected to provide sufficient strengthening and support for thermal properties in the aerogel-containing region and sufficient compressibility, compressive elasticity, and / or compliance in the aerogel-free region. The aerogel-containing portion of the reinforcing aerogel composition can provide a desired thermal conductivity, e.g., less than about 25 mW / m*K, while the aerogel-free portion of the reinforcing material can provide or improve desired physical properties, e.g., compressibility.

[0118] In some embodiments, a reinforced aerogel composition in which at least a portion of the reinforcing material does not contain aerogel can be formed using a method disclosed herein, in which the reinforcing material is combined with a precursor solution in an amount sufficient to partially fill the reinforcing material with the precursor solution. For example, the volume of the precursor can be less than the volume of the reinforcing material, such that the precursor penetrates the reinforcing material only partially. Upon drying, the resulting reinforced aerogel composition contains an aerogel skeleton extending through less than the total thickness of the reinforcing material, as described above. In other embodiments, a reinforced aerogel composition in which at least a portion of the reinforcing material does not contain aerogel can be formed by removing a surface aerogel layer from a reinforced aerogel composition.

[0119] In some embodiments, a reinforced aerogel composition in which at least a portion of the reinforcing material does not contain aerogel can be formed using a reinforcing material having mixed properties throughout its thickness. For example, the reinforcing material may comprise multiple layers, each layer having different properties, e.g., average pore / cell size, material composition, closed-cell, open-cell, surface treatment, or a combination thereof. The multiple layers may be joined together, for example, using an adhesive, by flame fusion, or by other suitable methods or mechanisms as discussed herein. Different properties of the reinforcing material can provide various distributions of aerogel through the layers. For example, the open-cell portions of the reinforcing material may contain an aerogel skeleton, while the closed-cell portions remain substantially aerogel-free. Similarly, other material properties of the reinforcing material or its layers can determine the distribution of aerogel within the reinforcing material and, therefore, within the reinforced aerogel composition.

[0120] In some exemplary embodiments, a reinforced aerogel composition in which at least a portion of the reinforcing material does not contain aerogel can be formed using the methods disclosed herein, wherein the properties of the reinforcing material or layer control or influence the amount of precursor solution used to fill the material or layer, for example, during the casting process, thereby partially filling the reinforcing material with the precursor solution. For example, one layer of the reinforcing material may have open cells, and another layer of the reinforcing material may have closed cells. When the precursor solution is combined with such a reinforcing material, the gel precursor solution can penetrate the closed cells of a layer without substantially penetrating the closed cells of the other layer. When such a composition is dried, the resulting reinforced aerogel composition may contain portions that do not contain aerogel, such as closed-cell layers, while the other portions, such as open-cell layers, contain aerogel.

[0121] In some embodiments, the additives disclosed herein (e.g., endothermic additives, opacifying additives, fire-class additives, or other additives) can be non-uniformly dispersed within the reinforced aerogel composition. For example, the additive material can vary depending on the thickness of the aerogel composition or along the length and / or width of the aerogel composition. For example, the additive can accumulate on one side of the aerogel composition. In some embodiments, the additive material may be concentrated in one layer of the aerogel composite or provided as a separate layer essentially consisting of the additive adjacent to or attached to the composite. For example, a thermal control member may include a layer essentially consisting of an endothermic material such as gypsum, sodium bicarbonate, or magnesia cement.

[0122] In more exemplary embodiments, the aerogel composition may also include at least one additional layer of material, either within the composition or as a counter layer. For example, the layer may be selected from the group consisting of polymer sheets, metal sheets, fiber sheets, highly oriented graphite materials, such as pyrolytic graphite sheets, and woven fabric sheets. In some embodiments, the counter layer may be attached to the composition by an adhesive mechanism selected from the group consisting of, for example, aerosol adhesives, urethane adhesives, acrylate adhesives, hot melt adhesives, epoxy, rubber resin adhesives, polyurethane composite adhesives, and combinations thereof. In some embodiments, the counter layer may be attached to the composition by a non-adhesive mechanism selected from the group consisting of, for example, flame fusion, needlework, stitching, sealing bags, rivets, buttons, clamps, wraps, braces, and combinations thereof. In some embodiments, any combination of the adhesive and non-adhesive mechanisms described above may be used to attach the counter layer to the composition.

[0123] As discussed herein, aerogel compositions or composites may include materials that incorporate aerogel microparticles, particles, granules, beads, or powders into a solid or semi-solid material by combining them with a binder such as an adhesive, resin, cement, foam, polymer, or similar solid or solidifying material. For example, an aerogel composition may include a reinforcing agent, aerogel particles, and optionally a binder. In exemplary embodiments, a slurry containing aerogel particles and at least one wetting agent may be provided. For example, the aerogel particles may be coated or wetted with at least one wetting agent, such as a surfactant or dispersant. The aerogel particles may be completely wetted, partially wetted (e.g., surface wetted), or present in the slurry. Preferred wetting agents may be volatilizable to allow for proper restoration of the hydrophobicity of the hydrophobic aerogel particles. If a wetting agent remains on the surface of the aerogel particles, the remaining wetting agent may contribute to the overall thermal conductivity of the composite. Therefore, preferred wetting agents are removable, such as by volatilization with or without decomposition or other means. In general, any wetting agent compatible with aerogel may be used.

[0124] Slurries or aerogels coated with wetting agents can be useful as a method for easily introducing hydrophobic aerogels into a variety of materials such as other aqueous-containing fluids, slurries, adhesives, and binder materials, which may optionally harden to form solid materials, fibers, metallized fibers, individual fibers, woven materials, nonwoven materials, needle nonwovens, battings, webs, mats, felts, and combinations thereof. Slurries containing aerogels wetted with at least one wetting agent or aerogels containing at least one wetting agent allow for easy introduction and uniform distribution of hydrophobic aerogels. Wet processes, such as those described in U.S. Patent Nos. 9,399,864, 8,021,583, 7,635,411, and 5,399,422, use aqueous slurries to disperse aerogel particles, fibers, and other additives. Next, the slurry can be dewatered to form layers of aerogel particles, fibers, and additives, the aerogel particles, fibers, and additives can be dried, and optionally calendered to produce an aerogel composite.

[0125] In other embodiments, the aerogel composition may include aerogel particles, at least one inorganic matrix material, and optionally fibers, auxiliary materials, additives, and further inorganic binders. In some embodiments, the inorganic matrix material may include phyllosilicates, such as naturally occurring phyllosilicates, such as kaolin, clay, or bentonite; synthetic phyllosilicates, such as magadiite or kenyaite; or mixtures thereof. The phyllosilicate may be calcined or uncalcined, for example, to dry the material and expel crystalline water. In some embodiments, the inorganic matrix material may also include, in combination with the phyllosilicate, an inorganic binder such as cement, lime, gypsum, or a suitable mixture thereof. In some embodiments, the inorganic matrix material may also include other inorganic additives disclosed herein, such as fire-class additives, opacifiers, or combinations thereof. Exemplary methods and aerogel compositions including inorganic matrix materials are disclosed in U.S. Patent No. 6,143,400 and U.S. Patent No. 6,083,619 (each incorporated herein in whole by reference, respectively). In some embodiments, the aerogel composition may include aerogel particles coated or absorbed onto woven materials, nonwoven materials, needle nonwovens, battings, webs, mats, felts, and combinations thereof. Adhesive binders may be included in the composition. Additives such as fire-class additives, opacifiers, or combinations thereof, as disclosed herein, may also be included. Exemplary methods and aerogel compositions coated onto or absorbed onto fabrics are disclosed in U.S. Patent Application Publication 2019 / 0264381, which is incorporated herein by reference in its entirety.

[0126] As discussed herein, aerogel composites can be laminated or opposed with other materials, such as reinforcing layers of opposing materials. In one embodiment, the disclosure provides a multilayer laminate comprising at least one base layer containing a reinforcing aerogel composition and at least one opposing layer. In one embodiment, the opposing layer comprises a reinforcing material. In one embodiment, the reinforcing aerogel composition is reinforced by a fiber-reinforced layer or an open-cell foam-reinforced layer. In one embodiment, the disclosure provides a multilayer laminate comprising a base layer containing a reinforcing aerogel composition and at least two opposing layers containing reinforcing materials, wherein the two opposing layers are on opposing surfaces of the base layer. For example, a multilayer aerogel laminate composite can be manufactured according to the methods and materials described in U.S. Patent Application Publication No. 2007 / 0173157.

[0127] The opposing layer may include materials that help impart specific properties to the final composite structure, such as improved flexibility or reduced dusting. The opposing material may be rigid or flexible. The opposing material may include a conductive layer or a reflective foil. For example, the opposing material may include a metal or a metallized material. The opposing material may include a nonwoven material. The opposing layer may be placed on the surface of the composite structure or the reinforced aerogel composite forming the composite structure, such as a thermal control member. The opposing layer may form a continuous coating or bag around the composite structure or the reinforced aerogel composite forming the composite structure, such as a thermal control member. In some embodiments, one or more opposing layers may encapsulate the composite structure or the reinforced aerogel composite forming the composite structure.

[0128] In one embodiment, the opposing layer comprises a polymer sheet surrounding the composite structure, more specifically, a polymer material including polyester, polyethylene, polyurethane, polypropylene, polyacrylonitrile, polyamide, aramid, more specifically, polyethylene terephthalate, low-density polyethylene, ethylene-propylene copolymer, poly(4-methyl-pentane), polytetrafluoroethylene, poly(1-butene), polystyrene, polyvinyl acetate, polyvinyl chloride, polyvinylidene chloride, polyvinyl fluoride, polyvinyl acrylonitrile, premethyl methacrylate, polyoxymethylene, polyphenylene sulfone, cellulose acetate, polycarbonate, polyethylene naphthalate, polycaprolactam, polyhexamethylene adipamide, polyundecanoamide, polyimide, or a combination thereof. In one embodiment, the polymer sheet comprises or is essentially composed of an expanded polymer material, more specifically, a foamed polymer material including PTFE (ePTFE), expanded polypropylene (ePP), expanded polyethylene (ePE), expanded polystyrene (ePS), or a combination thereof. In a preferred embodiment, the counter material is essentially composed of an expanded polymer material. In one embodiment, the polymer sheet comprises or is essentially composed of a microporous polymer material characterized by pore sizes ranging from 0.1 μm to 210 μm, 0.1 μm to 115 μm, 0.1 μm to 15 μm, or 0.1 μm to 0.6 μm.

[0129] In one embodiment, the counter layer material includes or is essentially composed of a fluoropolymer material. In the context of this disclosure, the terms “fluoropolymer” or “fluoropolymer material” refer to materials that are primarily composed of polymer fluorocarbons. Suitable fluoropolymer counter layer materials include, but are not limited to, polytetrafluoroethylene (PTFE), including microporous PTFE as described in U.S. Patent No. 5,814,405, and expanded PTFE (ePTFE) such as Gore-Tex® (available from WLGore), polyvinyl fluoride (PVF), polyvinylidene fluoride (PVDF), perfluoroalkoxy (PFA), fluorinated ethylene propylene (FEP), polychlorotrifluoroethylene (PCTFE), ethylenetetrafluoroethylene (ETFE), polyvinylidene fluoride (PVDF), ethylene chlorotrifluoroethylene (ECTFE), and combinations thereof. In one preferred embodiment, the counter material is essentially composed of a fluoropolymer material. In one preferred embodiment, the counter material is essentially composed of expanded PTFE (ePTFE) material.

[0130] In one embodiment, the counter layer material includes or is essentially composed of a non-fluoropolymer material. In the context of this disclosure, the terms “non-fluoropolymer” or “non-fluoropolymer material” refer to materials that do not contain fluoropolymer materials. Suitable non-fluoropolymer counter layer materials include, but are not limited to, aluminized mylar, low-density polyethylene such as Tyvek® (available from DuPont), rubber or rubber composites, nonwoven materials, elastic fibers such as spandex, nylon, Lycra or elastane, and combinations thereof. In one embodiment, the counter material is a flexible counter material.

[0131] In some embodiments, the opposing layer material may include automotive resins and polymers having a maximum operating temperature of approximately 100°C, approximately 120°C, or approximately 150°C. For example, the opposing layer material may include acrylonitrile butadiene styrene (ABS) polycarbonate, polypropylene, polyurethane, polystyrene, polyethylene, polycarbonate, polyimide, PVC, or a combination thereof. For example, the aerogel composites and thermal control members according to embodiments disclosed herein may include a layer of automotive resin or automotive polymer, a metal or metallized layer, and an aerogel layer.

[0132] The opposing layer can be attached to the base layer by using an adhesive suitable for fixing an inorganic or organic opposing material to the reinforcing material of the base layer. Examples of adhesives that can be used in this disclosure include, but are not limited to, cement-based adhesives, sodium silicate, latex, pressure-sensitive adhesives, silicone, polystyrene, aerosol adhesives, urethane, acrylate adhesives, hot-melt adhesive systems, adhesive systems commercially available from 3M, epoxy, rubber resin adhesives, and polyurethane adhesive mixtures such as those described in U.S. Patent No. 4,532,316.

[0133] The opposing layer may also be attached to the base layer by using a non-adhesive material or technique suitable for fixing an inorganic or organic opposing material to the reinforcing material of the base layer. Examples of non-adhesive materials or techniques that may be used in this disclosure include, but are not limited to, heat seals, ultrasonic stitches, RF seals, stitches or threads, needlework, seal bags, rivets or buttons, clamps, wraps, or other non-adhesive laminating materials.

[0134] The counter layer can be attached to the base layer at any stage in the manufacture of the aerogel composite. In one embodiment, the counter layer is attached to the base layer after the sol-gel solution has been injected into the base reinforcement but before gelation. In another embodiment, the counter layer is attached to the base layer after the sol-gel solution has been injected into the base reinforcement but after subsequent gelation, but before aging or drying the gel material. In yet another embodiment, the counter layer is attached to the base layer after the gel material has been aged and dried. In a preferred embodiment, the counter layer is attached to the base layer reinforcement before the sol-gel solution has been injected into the base reinforcement. The counter layer can be solid and fluid-impermeable. The counter layer can be porous and fluid-permeable. In a preferred embodiment, the counter layer is porous and fluid-permeable and includes pores or holes having a diameter large enough to allow fluid to diffuse through the counter layer material. In another preferred embodiment, the counter layer is attached to the base layer reinforcement before the sol-gel solution has been injected into the base reinforcement, and the counter layer is porous and fluid-permeable and includes pores or holes having a diameter large enough to allow fluid to diffuse through the counter layer material. In yet another preferred embodiment, the opposing layer is attached to the open-cell foam reinforcer before the sol-gel solution is injected into the foam reinforcer, and the opposing layer is porous and fluid-permeable and includes pores or holes having a diameter large enough to allow the fluid to diffuse through the opposing material.

[0135] In some embodiments, the composite structure or the reinforced aerogel composite forming the composite structure may be encapsulated by an encapsulation member. For example, the encapsulation member may include one or more material layers surrounding the composite structure or the composite structure and / or a coating of the material surrounding the composite structure. For example, the encapsulation member may include a film, layer, envelope, or coating. The encapsulation member may be made from any material suitable for enclosing the composite structure or the reinforced aerogel composite forming the composite structure. For example, the encapsulation member may reduce or eliminate the generation of dust or particulate material released from the composite structure.

[0136] The encapsulating member may include at least one vent that allows air to enter and exit the panel. The encapsulating member may include at least one filter that filters out particulate matter. In an exemplary embodiment, the encapsulating member includes a vent that allows air to enter and exit the panel, and a particulate filter on the vent that holds particulate matter within the encapsulating member. In another embodiment, the encapsulating member includes an edge seal that includes at least one vent and at least one particulate filter. In a further embodiment, the encapsulating member includes an edge seal that includes at least one vent and at least one particulate filter, the vent in the edge seal allowing air to enter and exit the edge of the encapsulating member, and the filter that captures and holds particulate matter in the flowing air, preventing the air outside the encapsulating member from being contaminated with particulate matter. In some embodiments of the above aspects, the thermal control member may include multiple layers. For example, the thermal control member may include layers that include at least one layer of thermally conductive material, e.g., metal, carbon, thermally conductive polymer, or a combination thereof. In the context of these embodiments, the thermally conductive material refers to a material having a thermal conductivity greater than that of the aerogel composition. In certain embodiments, the thermally conductive material has a thermal conductivity at least about an order of magnitude greater than that of the aerogel composition. In some embodiments, the thermal control member may include multiple layers of the aerogel composition. In certain embodiments, the thermal control member may include at least one layer of conductive material positioned adjacent to the aerogel composition. In certain embodiments, the thermal control member may include at least one layer of conductive material positioned between at least two of the multiple layers of the aerogel composition. In some embodiments, the thermal control member may include particles of conductive material positioned within the layers of the thermal control member, for example, within the layers of the aerogel composition.

[0137] In exemplary embodiments, the thermal control member is a material or material layer that provides heat capacity (i.e., a heat-capacitive material), for example, at least about 0.3 J / (g)·℃ This may include materials having a specific heat capacity of at least about 0.5 J / (g). In some embodiments, the material providing the heat capacity is at least about 0.5 J / (g). ·℃ ) has a specific heat capacity. For example, the material providing the heat capacity may include metals such as aluminum, titanium, nickel, steel, iron, or combinations thereof. In some embodiments, the thermal control member may include a layer or coating of the material providing the heat capacity. In some embodiments, the thermal control member may include particles of the material providing the heat capacity disposed within a layer of the thermal control member, for example, within a layer of an aerogel composition. In certain embodiments, the thermal control member may include at least one layer of the material providing the heat capacity disposed adjacent to the aerogel composition. In certain embodiments, the thermal control member may include at least one layer of the material providing the heat capacity disposed between at least two of a plurality of layers of an aerogel composition. In exemplary embodiments, the thermal control member may include both a thermally conductive material and a thermally capacitive material. For example, the thermal control member may include a material that provides both heat capacity and thermal conductivity, for example, metals such as aluminum, titanium, nickel, steel, iron, or combinations thereof. In another example, the thermal control member may include one or more different materials or layers of materials, each providing either heat capacity, thermal conductivity, or a combination thereof, for example, a layer containing a metal and a layer containing a thermally conductive polymer.

[0138] In some embodiments, a thermal paste is used between layers of a thermal control member to ensure uniform and consistent heat conduction between such layers. As used herein, thermal paste refers to a variety of materials also known as thermal compounds, thermal greases, thermal interface materials (TIMs), thermal gels, heat pastes, heat sink compounds, and heat sink pastes. For example, a layer of thermal paste can be placed between an aerogel composition and one or more layers containing thermally conductive or heat-capacitive materials, one or more opposing layers, or any other layer such as an encapsulating member.

[0139] As described herein, a thermal control member may include multiple layers of material, such as an insulating layer, a thermal conductive layer, a thermal capacitance layer, a thermal reflection layer, a compressible layer or a compliant layer, or a combination thereof. The combination of layers within the thermal control member can be selected to obtain a desired combination of properties, such as compressibility, elasticity, thermal performance, fire reactivity, and other properties. In some embodiments, the thermal control member includes at least one compliant member positioned between at least two layers of a reinforced aerogel composition. The compliant member includes a compressible material, i.e., a material that can be compressed to reduce its thickness while providing a desired resistance to compression. For example, the compliant member may be polyolefin, polyurethane, phenol resin The thermal control member may be a foam or other compressible material such as melamine, cellulose acetate, or polystyrene. In certain embodiments, the thermal control member may also include at least one layer of a thermally conductive or heat-capacitive material positioned between at least one compliant member and at least one of a plurality of layers of the reinforced aerogel composition. The thermally conductive or heat-capacitive material can absorb and / or disperse heat within the thermal control member. In some embodiments, the thermal control member may further include a heat-reflective layer. For example, the heat-reflective layer may include a metal foil or sheet.

[0140] In embodiments of a thermal control member comprising several layers, layers can be attached to other layers by an adhesive mechanism selected from the group consisting of, for example, aerosol adhesives, urethane adhesives, acrylate adhesives, hot melt adhesives, epoxy, rubber resin adhesives, polyurethane composite adhesives, and combinations thereof. In some embodiments, layers can be attached by a non-adhesive mechanism selected from the group consisting of, for example, flame fusion, needlework, stitching, sealing bags, rivets, buttons, clamps, wraps, braces, and combinations thereof. In some embodiments, any combination of the aforementioned adhesive and non-adhesive mechanisms can be used to attach the layers to each other.

[0141] Figure 5 shows an exemplary thermal control member according to embodiments disclosed herein. As shown in Figure 6, the exemplary thermal control member 10 includes a layer of reinforced aerogel composition 12. A layer of thermally conductive or heat-capacitive material 14 is disposed adjacent to the layer of reinforced aerogel composition 12. The thermal control member 10 is substantially flat and has a first main outer surface defined by the outer surface of the first layer of reinforced aerogel composition 12 and a second main outer surface defined by the outer surface of the layer of thermally conductive or heat-capacitive material 14. In some embodiments, the thermal control member 10 includes an encapsulation member or layer surrounding all or part of the outer surface of the thermal control member. In some embodiments, the layer of aerogel composition may be surrounded by an encapsulation member or layer surrounding all or part of the layer of aerogel.

[0142] As shown in Figure 7, an exemplary thermal control member 20 includes a first layer of reinforced aerogel composition 22 and a second layer of reinforced aerogel composition 23. A layer of thermally conductive or heat-capacitive material 14 is positioned between the first layer of reinforced aerogel composition 22 and the second layer of reinforced aerogel composition 23. The thermal control member 20 is substantially flat and has a first main outer surface defined by the outer surface of the first layer of reinforced aerogel composition 22 and a second main outer surface defined by the outer surface of the second layer of reinforced aerogel composition 23. In some embodiments, the thermal control member 10 includes an encapsulation member or layer surrounding all or part of the outer surface of the thermal control member. In some embodiments, the layer of aerogel composition may be surrounded by an encapsulation member or layer surrounding all or part of the layer of aerogel.

[0143] As shown in Figure 8, an exemplary thermal control member 30 includes a first layer 32 of a reinforced aerogel composition and a second layer 33 of a reinforced aerogel composition. The thermal control member 30 is substantially flat and has a first main outer surface defined by the outer surface of the first layer 32 of the reinforced aerogel composition and a second main outer surface defined by the outer surface of the second layer 33 of the reinforced aerogel composition. A layer 34 of the corresponding material is placed between the first and second layers of the aerogel composition. A first layer 36 of a thermally conductive or heat-capacitive material is placed between the first layer 32 of the reinforced aerogel composition and the layer 34 of the compliant material. A second layer 37 of a thermally conductive or heat-capacitive material is placed between the second layer 33 of the reinforced aerogel composition and the layer 34 of the compliant material. In some embodiments, the thermal control member 30 includes an encapsulation member or layer surrounding all or part of the outer surface of the thermal control member. In some embodiments, each layer of the aerogel composition may be surrounded by an encapsulating member or layer that surrounds all or part of the aerogel layer.

[0144] As shown in Figure 9, an exemplary thermal control member 40 includes a first layer of reinforced aerogel composition 42 and a second layer of reinforced aerogel composition 43. The thermal control member 40 is substantially flat and has a first main outer surface defined by the outer surface of the first layer of reinforced aerogel composition 42 and a second main outer surface defined by the outer surface of the second layer of reinforced aerogel composition 43. A layer 44 of the corresponding material is located between the first and second layers of the aerogel composition. A first layer 46 of a thermally conductive or heat-capacitive material is located on the main outer surface of the first layer of reinforced aerogel composition 42. A second layer 47 of a thermally conductive or heat-capacitive material is located on the main outer surface of the second layer of reinforced aerogel composition 43. In some embodiments, the thermal control member 40 includes an encapsulation member or layer surrounding all or part of the outer surface of the thermal control member. In some embodiments, each layer of the aerogel composition may be surrounded by an encapsulation member or layer surrounding all or part of the layer of aerogel.

[0145] The production of a multilayer gel or aerogel composition may include the following steps: a) attaching a fluid-permeable counter layer to a sheet of reinforcing material to produce a laminated reinforced sheet, wherein the counter layer includes pores or holes having a diameter large enough to allow fluid to diffuse through the counter material; b) injecting a gel precursor solution into the reinforced sheet via the counter layer; and c) transferring the gel precursor material into a gel material containing a gel structure. A portion of the gel precursor solution is likely to be retained in the pores or holes of the counter layer such that the gel skeleton in the base layer of the reinforcing material extends into at least a portion of the counter layer. The resulting product is a multilayer gel composition comprising: a) at least one base layer including a reinforcing material and a gel skeleton integrated within the reinforcing material; and b) at least one counter layer including a fluid-permeable counter material and a gel skeleton integrated within the fluid-permeable counter material, wherein at least a portion of the gel skeleton of the base layer extends into at least a portion of the gel skeleton of the counter layer and is continuous with at least a portion of the gel skeleton of the counter layer.

[0146] Large-scale production of multilayer aerogel compositions may include a conveyor-based system, the production of which includes a) a step of producing a laminated reinforced sheet by attaching at least one fluid-permeable counter layer to a sheet of reinforcement, wherein the counter layer includes pores or holes having a diameter large enough to allow fluid to penetrate and diffuse; and b) a step of combining a gel precursor solution with a laminated reinforced sheet at one end of a conveyor to produce a continuous reinforced gel sheet laminate, wherein at least a portion of the gel precursor solution is injected into the reinforced sheet via the counter layer, and the gel precursor solution is combined with the laminated reinforced sheet at a rate that allows the gel precursor solution to pass through the counter layer and penetrate into the reinforced sheet. In a preferred embodiment, the reinforcement includes an open-cell foam reinforcement.

[0147] The reinforced laminated gel sheet can be wound in multiple layers (preferably around a mandrel with uniform tension) and then processed in subsequent chemical treatment, aging, and drying steps. Additional separator layers can be co-wound between the gel sheet layers to facilitate aging or drying of the gel material, such as to provide channels for aging agents or desiccants. In a preferred embodiment, the opposing layer provides channels for aging agents or desiccants so that additional separator layers are not required for aging and drying of the gel material.

[0148] Large-scale production of multilayer aerogel compositions may involve a semi-continuous batch-based process commonly known as a gel-in-roll process, which includes a) a mounting step of attaching fluid-permeable opposing layers to a sheet of reinforcing material, wherein the opposing layers include pores or holes having a diameter large enough to allow fluid to penetrate and diffuse; b) a step of rolling the laminated reinforcing material into multiple layers as a preform roll; and c) a step of combining a gel precursor solution with the role of a preform. Additional separator layers may be co-rolled with the reinforcing material in the preform roll to provide channels for the gel precursor solution, aging agent, and desiccant. In a preferred embodiment, the opposing layers provide channels for the gel precursor solution, aging agent, and desiccant so that an additional separator layer is not required. In a preferred embodiment, the reinforcing material includes an open-cell foam reinforcing material.

[0149] The aerogel compositions according to embodiments of this disclosure can be formed into a variety of final products. In the simplest configuration, the reinforced aerogel composition may be in the form of a sheet. The sheet may be formed continuously or semi-continuously, for example, as a rolled product, or by cutting sheets of a desired size and shape, or by forming them from a larger sheet. The sheet material may be used to form a thermal barrier between battery cells. In other configurations, the reinforced aerogel composition may be formed, for example, into a pouch for housing pouch cells of a battery, or into a cylinder for housing cylindrical battery cells.

[0150] The aerogel composites of this disclosure can be molded into a variety of three-dimensional shapes, including panels, pipe preforms, half-shell preforms, elbows, fittings, pouches, cylinders, and other shapes typically required for the application of thermal insulation materials to industrial and commercial applications. In one embodiment, the reinforcing material is formed into the desired shape before the gel precursor material is injected. The gel material is processed to allow the preform to maintain its shape, thus obtaining a reinforced aerogel preform of the desired shape. This technique for forming molded aerogel preforms can be difficult and inefficient due to the difficulties required to process gel materials of various shapes and configurations.

[0151] In exemplary embodiments of the present disclosure, an aerogel can be formed from a gel precursor or combination of gel precursors containing at least one hydrophobic group. Such an aerogel, an inorganic aerogel such as a silica-based aerogel, may contain hydrophobic-bound silicon. For example, the source of hydrophobic-bound silicon in the aerogel may be one or more hydrophobic precursor materials. In embodiments of the present disclosure, an aerogel formed from such precursors may be hydrophobic. In some embodiments, an aerogel formed from such precursors may be inherently hydrophobic.

[0152] In the context of this disclosure, the term “inherently hydrophobic” refers to a material that is hydrophobic without modification by a hydrophobic agent. For example, aerogels can be treated to impart or improve hydrophobicity. Hydrophobic treatment can be applied to sol-gel solutions, wet gels before liquid-phase extraction, or aerogels after liquid-phase extraction. Hydrophobic treatment can be carried out by reacting hydroxyl moieties on the gel, such as silanol groups (Si-OH) present on the silica gel skeleton, with the functional groups of a hydrophobic agent. The resulting reaction converts the silanol groups and the hydrophobic agent into hydrophobic groups on the silica gel skeleton. Hydrophobic agent compounds can react with hydroxyl groups on the gel according to the following reaction: N MX 4-N (Hydrophobic agent) + MOH (Silanol) → MOMR N (Hydrophobic group) + HX. Hydrophobic treatment can be performed on both the outer macrosurface of the silica gel and the inner pore surfaces within the porous network of the gel. Published U.S. Patent Application Publication No. 2016 / 0096949 (paragraphs

[0044] to

[0048] ) teaches hydrophobic treatment and is incorporated herein by reference in accordance with the paragraphs cited individually. However, as stated above, the aerogels according to embodiments of the present disclosure are hydrophobic without hydrophobic treatment, for example, without treatment with a hydrophobic agent.

[0153] The production of aerogels generally includes the steps of i) forming a sol-gel solution, ii) forming a gel from the sol-gel solution, and iii) extracting the solvent from the gel material by innovative processing and extraction to obtain a dry aerogel material. This process is described in more detail below, particularly in relation to the formation of inorganic aerogels such as silica aerogels. However, the specific examples and illustrations provided herein are not intended to limit this disclosure to any particular type of aerogel and / or preparation method. Unless otherwise specified, this disclosure may include any aerogel formed by any relevant preparation method known to those skilled in the art.

[0154] The first step in forming an inorganic aerogel is generally, but not limited to, the formation of a sol-gel solution by hydrolysis and condensation of a silica precursor, such as a metal alkoxide precursor, in an alcoholic solvent. The main variables in the formation of an inorganic aerogel include the type of alkoxide precursor contained in the sol-gel solution, the properties of the solvent, the processing temperature and pH of the sol-gel solution (which can be altered by the addition of an acid or base), and the precursor / solvent / water ratio in the sol-gel solution. Controlling these variables in the formation of the sol-gel solution can enable control of the growth and aggregation of the gel skeleton during the subsequent transition of the gel material from the "sol" state to the "gel" state. The properties of the resulting aerogel are influenced by the pH of the precursor solution and the molar ratio of the reactants, although any pH and molar ratio that enables gel formation can be used in this disclosure.

[0155] A sol-gel solution is formed by combining at least one gelling precursor with a solvent. Suitable solvents for forming sol-gel solutions include lower alcohols with 1 to 6 carbon atoms, particularly 2 to 4 carbon atoms, but other solvents known to those skilled in the art can be used. Examples of useful solvents include, but are not limited to, methanol, ethanol, isopropanol, ethyl acetate, ethyl acetoethyl acetate, acetone, dichloromethane, and tetrahydrofuran. Multiple solvents can also be combined to achieve a desired level of dispersion or to optimize the properties of the gel material. Therefore, the selection of the optimal solvent for the sol-gel formation step and the gel formation step depends on the specific precursors, fillers, and additives incorporated into the sol-gel solution, as well as the target processing conditions for gelation and liquid extraction, and the desired properties of the final aerogel material.

[0156] Water can also be present in the precursor-solvent solution. The water acts to hydrolyze the metal alkoxide precursor to the metal hydroxide precursor. The hydrolysis reaction can be as follows (using TEOS in ethanol solvent as an example): Si(OC2H5)4 + 4H2O → Si(OH)4 + 4(C2H5OH). The resulting hydrolyzed metal hydroxide precursor remains suspended in the solvent solution in a "sol" state, either as individual molecules or as small polymerized (or oligomerized) colloidal clusters of molecules. For example, polymerization / condensation of the Si(OH)4 precursor can occur as follows: 2Si(OH)4 = (OH)3Si-O-Si(OH)3 + H2O. This polymerization can continue until a polymerized (or oligomerized) colloidal cluster of SiO2 (silica) molecules is formed.

[0157] Acids and bases can be incorporated into sol-gel solutions to control the solution's pH and catalyze the hydrolysis and condensation reactions of precursor materials. Any acid can be used to catalyze the precursor reaction and obtain a solution with a lower pH; exemplary acids include HCl, H2SO4, H3PO4, oxalic acid, and acetic acid. Any base can similarly be used to catalyze the precursor reaction and obtain a solution with a higher pH; exemplary bases include NH4OH.

[0158] A strong base can be used to catalyze the precursor reaction, yielding a solution with a higher pH. Using a strong base to catalyze the precursor reaction allows for a significantly higher content of hydrophobic inorganic precursor material, such as MTES or DMDES, than would be possible with a weak base, such as a base containing NH4OH. In the context of this disclosure, the term “strong base” refers to both inorganic and organic bases. For example, the strong bases according to the embodiments herein include cations selected from the group consisting of lithium, calcium, sodium, potassium, rubidium, barium, strontium, and guanidinium. In another example, the basic catalyst used to catalyze the precursor reaction may include catalytic amounts of sodium hydroxide, lithium hydroxide, calcium hydroxide, potassium hydroxide, strontium hydroxide, barium hydroxide, guanidine hydroxide, sodium hydroxide, tetrabutylammonium hydroxide, tetramethylammonium hydroxide, choline hydroxide, phosphonium hydroxide, DABCO, DBU, guanidine derivatives, amidine, or phosphazene.

[0159] The sol-gel solution may contain further co-gelling precursors, as well as filler materials and other additives. The filler materials and other additives may be dispensed into the sol-gel solution at any point before or during gel formation. The filler materials and other additives may also be incorporated into the gel material after gelation by various techniques known to those skilled in the art. In certain embodiments, the sol-gel solution comprising the gelling precursor, solvent, catalyst, water, filler materials, and other additives is a homogeneous solution capable of effective gel formation under appropriate conditions.

[0160] Once a sol-gel solution is formed and optimized, the gel-forming components in the sol-gel can be transferred to the gel material. The process of transferring the gel-forming components to the gel material includes an initial gel-forming step in which the gel solidifies to the gelation point of the gel material. The gelation point of the gel material can be considered the point in which the gelling solution exhibits flow resistance and / or forms a substantially continuous polymer backbone over its entire volume. Various gel-forming techniques are known to those skilled in the art. Examples include, but are not limited to, maintaining the mixture at rest for a sufficient period of time, adjusting the pH of the solution, adjusting the temperature of the solution, directing a form of energy towards the mixture (ultraviolet light, visible light, infrared light, microwaves, ultrasound, particle radiation, electromagnetic radiation), or combinations thereof.

[0161] The process of transferring gel-forming components (gel precursors) to a gel material may also include an aging step (also called curing) before liquid extraction or removal of the solvent from the gel (also called gel drying). Aging the gel material after reaching the gelation point can further strengthen the gel backbone by increasing the number of crosslinks in the network. The duration of gel aging can be adjusted to control various properties in the resulting aerogel material. This aging procedure may be useful in preventing potential volume loss and shrinkage during liquid extraction. Aging may include keeping the gel at rest for a long period (before extraction), keeping the gel at a high temperature, adding crosslinking-promoting compounds, or any combination thereof. Preferred temperatures for aging are typically about 10°C to about 100°C, but other suitable temperatures are also contemplated herein. Aging of the gel material typically continues until liquid extraction of the wet gel material.

[0162] The time required to transfer a gel-forming material (gel precursor) into a gel material includes both the duration of the initial gel formation (from the start of gelation to the gelation point) and the duration of the subsequent hardening and aging of the gel material (from the gelation point to the start of liquid extraction / solvent removal) before liquid extraction or removal of the solvent from the gel (also known as gel drying). The total time required to transfer a gel-forming material into a gel material is typically between about 1 minute and several days, typically less than or equal to about 30 hours, less than or equal to about 24 hours, less than or equal to about 15 hours, less than or equal to about 10 hours, less than or equal to about 6 hours, less than or equal to about 4 hours, less than or equal to about 2 hours, preferably less than or equal to about 1 hour, less than or equal to about 30 minutes, less than or equal to about 15 minutes, or less than or equal to about 10 minutes.

[0163] In another embodiment, the resulting gel material can be washed with a suitable secondary solvent to replace the primary reaction solvent present in the wet gel. Such secondary solvents can be linear monohydric alcohols having one or more aliphatic carbon atoms, dihydric alcohols having two or more carbon atoms, branched alcohols, cyclic alcohols, alicyclic alcohols, aromatic alcohols, polyhydric alcohols, ethers, ketones, cyclic ethers, or derivatives thereof. In yet another embodiment, the resulting gel material may be washed with an additional amount of the same solvent present in the gel material, in particular to remove undesirable by-products or other precipitates in the gel material.

[0164] Once a gel material is formed and processed, the liquid of the gel can be at least partially extracted from the wet gel using extraction methods, including innovative processing and extraction techniques, to form an aerogel material. Liquid extraction plays a crucial role, among other factors, in manipulating the properties of aerogels, such as porosity and density, as well as related properties such as thermal conductivity. Generally, aerogels are obtained by extracting the liquid from the gel in a manner that causes low shrinkage in the porous network and backbone of the wet gel. This liquid extraction is sometimes also called solvent removal or drying.

[0165] One alternative method for forming silica aerogels uses metal oxide salts such as sodium silicate, also known as water glass. First, a water glass solution is prepared by mixing sodium silicate with water and an acid to form a silicate precursor solution. Salt byproducts can be removed from the silicate precursor by ion exchange, surfactant separation, membrane filtration, or other chemical or physical separation techniques. The resulting sol can then be gelled, for example, by adding a base catalyst, to produce a hydrogel. The hydrogel can be washed to remove residual salts or reactants. Water can then be removed from the pores of the gel by exchange with a polar organic solvent such as ethanol, methanol, or acetone. The liquid in the gel is then at least partially extracted using innovative processing and extraction techniques. In embodiments, aerogels are generally formed by removing the liquid mobile phase from the gel material at temperatures and pressures near or above the critical point of the liquid mobile phase. Upon reaching a critical point (i.e., the system's pressure and temperature are above the critical pressure and critical temperature, respectively) or exceeding the critical point (supercritical), a new supercritical phase distinct from the liquid or gas phase appears in the fluid. The solvent can then be removed without introducing any associated mass transfer limitations related to the liquid-vapor interface, capillary pressure, or typically the liquid-vapor boundary. Furthermore, the supercritical phase is generally more miscible with organic solvents and therefore possesses better extraction capabilities. Co-solvents and solvent exchange are also commonly used to optimize supercritical fluid drying processes.

[0166] If evaporation or extraction is well below the critical point, the capillary forces generated by liquid evaporation can cause shrinkage and pore collapse within the gel material. Such adverse effects of capillary forces can be mitigated by maintaining the mobile phase near or above the critical pressure and temperature during the solvent extraction process. In certain embodiments of this disclosure, the use of near-critical conditions just below the critical point of the solvent system allows for the production of aerogel materials or compositions with sufficiently low shrinkage, and thus commercially viable final products.

[0167] Several additional aerogel extraction techniques are known in the art, including various approaches to the use of supercritical fluids in the drying of aerogels. For example, Kistler (J. Phys. Chem. (1932) 36:52-64) describes a simple supercritical extraction process in which the gel solvent is maintained above its critical pressure and critical temperature, thereby reducing the evaporative capillary force and maintaining the structural integrity of the gel network. U.S. Patent No. 4,610,863 describes an extraction process in which the gel solvent is exchanged for liquid carbon dioxide, followed by extraction under conditions in which the carbon dioxide is in a supercritical state. U.S. Patent No. 6,670,402 teaches the extraction of liquid from a gel via rapid solvent exchange by injecting supercritical (not liquid) carbon dioxide into an extractor preheated and pre-pressurized substantially above a supercritical state, thereby generating an aerogel. 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 with a fluid having a critical temperature below the polymer decomposition temperature and extracting the fluid / sol-gel using a supercritical fluid such as supercritical carbon dioxide, supercritical ethanol, or supercritical hexane. U.S. Patent No. 6,315,971 discloses a method for producing a gel composition, comprising drying a wet gel containing a gel solid and a desiccant, and removing the desiccant under sufficiently dry conditions to reduce the shrinkage of the gel during drying. U.S. Patent No. 5,420,168 describes a method by which a resorcinol / formaldehyde aerogel can be produced using a simple air-drying procedure. U.S. Patent No. 5,565,142 describes a drying technique for modifying the gel surface to be stronger and more hydrophobic so that the gel skeleton and pores can withstand collapse during ambient drying or subcritical extraction. Other examples of extracting liquid from aerogel materials can be found in U.S. Patents No. 5,275,796 and 5,395,805. U.S. Patent Application Publication No. 2019 / 0161909 provides an example of a method using alkoxysilane and water glass to produce a high-density aerogel.

[0168] One embodiment of extracting liquid from a wet gel uses a supercritical fluid such as carbon dioxide, which includes, for example, first substantially replacing the primary solvent present in the gel's pore network with liquid carbon dioxide, and then heating the wet gel (typically in an autoclave) above the critical temperature of carbon dioxide (approximately 31.06°C) and raising the system pressure to a pressure higher than the critical pressure of carbon dioxide (approximately 1070 psig). The pressure around the gel material can be slightly varied to facilitate the removal of liquid from the gel. To facilitate the continuous removal of the primary solvent from the wet gel, carbon dioxide can be recirculated through the extraction system. Finally, the temperature and pressure are slowly returned to ambient conditions to produce a dry aerogel material. Carbon dioxide can also be pre-treated to a supercritical state before being injected into the extraction chamber.

[0169] Another example of an alternative method for forming aerogels involves chemically modifying the matrix material in a wet gel state via the conversion of surface hydroxyl groups to hydrophobic trimethylsilyl ethers, thereby reducing the damaging capillary pressure at the solvent / pore interface and allowing liquid extraction from the gel material at temperatures and pressures below the critical point of the solvent.

[0170] In yet another embodiment, the liquid (solvent) in the gel material may be frozen at a lower temperature, followed by a sublimation process to remove the solvent from the gel material. Such removal or drying of the solvent from the gel material is understood to be within the scope of the present disclosure. Such removal largely preserves the gel structure and therefore produces an aerogel with intrinsic properties.

[0171] Large-scale production of aerogel materials or compositions can be complicated by the difficulties associated with the continuous formation of gel materials on a large scale, as well as the difficulties associated with liquid extraction from large volumes of gel materials using innovative processing and extraction techniques. In certain embodiments, the aerogel materials or compositions of the Disclosure are suitable for large-scale production. In certain embodiments, the gel materials of the Disclosure can be produced on a large scale by a continuous casting and gelation process. In certain embodiments, the aerogel materials or compositions of the Disclosure are produced on a large scale and require the use of large-scale extraction vessels. Large-scale extraction vessels of the Disclosure may include extraction vessels having a volume of about 0.1 m³ or more, about 0.25 m³ or more, about 0.5 m³ or more, or about 0.75 m³ or more.

[0172] The aerogel compositions of this disclosure may have thicknesses of 15 mm or less, 10 mm or less, 5 mm or less, 4 mm or less, 3 mm or less, 2 mm or less, 1 mm or less, 0.5 mm or less, 0.3 mm or less, or any combination of the above thicknesses.

[0173] The aerogel composition may be reinforced with various reinforcing materials to achieve a more flexible, resilient, and conformable composite product. Reinforcing materials can be added to the gel at any point in the gelation process to produce a wet-reinforced gel composition. The wet-reinforced gel composition can then be dried to produce a reinforced aerogel composition.

[0174] The aerogel composition may be reinforced with various open-cell macroporous skeletal reinforcing materials to achieve a more flexible, resilient, and conformable composite product. The OCMF reinforcing material can be added to the gel at any point in the gelation process prior to gelation to produce a wet-reinforced gel composition. The wet-reinforced gel composition can then be dried to produce an OCMF-reinforced aerogel composition. The OCMF reinforcing material can be formed from an organic polymer material such as melamine or a melamine derivative and may exist in the form of a continuous sheet or panel.

[0175] Melamine OCMF material can be produced from a melamine-formaldehyde precondensation solution. An aqueous solution of the melamine-formaldehyde condensate is produced by combining the melamine-formaldehyde precondensate with a solvent, emulsifier / dispersant, a curing agent such as an acid, and a blowing agent such as a C5 to C7 hydrocarbon. The melamine-formaldehyde solution or resin is then cured at a high temperature exceeding the boiling point of the blowing agent to produce OCMF containing numerous interconnected three-dimensional branched melamine structures, with corresponding networks of interconnected pores incorporated within the framework. Melamine-formaldehyde precondensates generally have a formaldehyde-to-melamine molar ratio ranging from 5:1 to 1.3:1, typically from 3.5:1 to 1.5:1. The precondensate can be in the form of a powder, spray, resin, or solution. The solvent contained in the melamine-formaldehyde precondensation solution can include alcohols such as methanol, ethanol, or butanol.

[0176] The emulsifier / dispersant contained in the melamine-formaldehyde pre-condensation solution may include anionic surfactants, cationic emulsifiers, or nonionic surfactants. Useful anionic surfactants include, but are not limited to, diphenylene oxide sulfonates, alkane- and alkylbenzene sulfonates, alkylnaphthalene sulfonates, olefin sulfonates, alkyl ether sulfonates, fatty alcohol sulfates, ether sulfates, α-sulfo fatty acid esters, acylaminoalkane sulfonates, acyl isethionates, alkyl ether carboxylates, N-acyl sarcosinates, alkyls, and alkyl ether phosphates. Useful cationic emulsifiers include, but are not limited to, alkyltriammonium salts, alkylbenzyldimethylammonium salts, or alkylpyridinium salts. Useful nonionic surfactants include, but are not limited to, alkylphenol polyglycol ethers, fatty alcohol polyglycol ethers, fatty acid polyglycol ethers, fatty acid alkanolamides, ethylene oxide-propylene oxide block copolymers, amine oxides, glycerol fatty acid esters, sorbitan esters, and alkyl polyglycosides. Emulsifiers / dispersants can be added in amounts from 0.2% to 5% by weight relative to the melamine-formaldehyde precondensate.

[0177] The curing agents contained in the melamine-formaldehyde precondensation solution may include acidic compounds. The amounts of these curing agents are generally in the range of 0.01% to 20% by weight, and typically in the range of 0.05% to 5% by weight, based on the melamine-formaldehyde precondensate. Useful acidic compounds include, but are not limited to, those selected from the group consisting of organic and inorganic acids, such as hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, formic acid, acetic acid, oxalic acid, toluenesulfonic acid, amidosulfonic acid, acid anhydrides, and mixtures thereof.

[0178] The blowing agent contained in the melamine-formaldehyde precondensation solution may include a physical blowing agent or a chemical blowing agent. Useful physical blowing agents include, but are not limited to, hydrocarbons such as pentane and hexane, halogenated hydrocarbons, more specifically chlorinated and / or fluorinated hydrocarbons, such as methylene chloride, chloroform, trichloroethane, chlorofluorocarbons, and hydrochlorofluorocarbons (HCFCs), alcohols, such as methanol, ethanol, n-propanol, or isopropanol, ethers, ketones, and esters, such as methyl formate, ethyl formate, methyl acetate, or ethyl acetate, and gases such as air, nitrogen, or carbon dioxide. In certain embodiments, it is preferable to add a physical blowing agent having a boiling point from 0°C to 80°C. Useful chemical blowing agents include, but are not limited to, isocyanates mixed with water (releasing carbon dioxide as an active blowing agent), carbonates and / or bicarbonates mixed with acids (releasing carbon dioxide as an active blowing agent), and azo compounds, such as azodicarbonamides. The foaming agent is present in the melamine-formaldehyde precondensate solution in amounts ranging from 0.5% to 60% by weight, particularly 1% to 40% by weight, and in specific embodiments, 1.5% to 30% by weight, based on the melamine-formaldehyde precondensate.

[0179] A melamine-formaldehyde precondensation solution can be formed into a melamine OCMF material by heating the solution to a temperature generally exceeding the boiling point of the blowing agent used, thereby forming an OCMF containing numerous interconnected three-dimensional branched melamine structures, with a corresponding network of interconnected open-cell pores incorporated within the framework. The introduction of thermal energy may be carried out via electromagnetic radiation, for example, via high-frequency radiation of 5 to 400 kW per kilogram of the mixture used in the frequency range of 0.2 to 100 GHz, more specifically 0.5 to 10 GHz, e.g., 5 to 200 kW, and in certain embodiments, 9 to 120 kW. A magnetron is a useful dielectric radiation source, and one magnetron may be used, or two or more magnetrons may be used simultaneously.

[0180] The OCMF material can be dried to remove any residual liquid (water, solvent, foaming agent). Post-treatment can also be used to hydrophobize the OCMF material. This post-treatment can use hydrophobic coating agents with high thermal stability and / or low flammability, such as silicones, silicone salts, or fluorinated compounds.

[0181] The density of melamine OCMF is generally in the range of 0.005 to 0.3 g / cc, for example, 0.01 to 0.2 g / cc, in certain embodiments in the range of 0.03 to 0.15 g / cc, or most specifically in the range of 0.05 to 0.15 g / cc. The average pore size of melamine OCMF is generally in the range of 10 μm to about 1000 μm, particularly in the range of 50 to 700 μm.

[0182] In this embodiment, the OCMF reinforcing material is incorporated into the aerogel composition as a continuous sheet. This process first involves producing a continuous sheet of OCMF-reinforced gel by casting or impregnating a gel precursor solution onto a continuous sheet of OCMF reinforcing material, and then forming the material into a reinforced gel composite sheet. The liquid can then be at least partially extracted from the OCMF-reinforced gel composite sheet to produce a sheet-like OCMF-reinforced aerogel composition.

[0183] The aerogel composition may contain opacifying agents to reduce the radiative component of heat transfer. At any point before gel formation, opacifying compounds or their precursors may be dispersed in a mixture containing the gel precursor. Examples of opacifying compounds include, but are not limited to, boron carbide (B4C), diatomaceous earth, manganese ferrite, MnO, NiO, SnO, Ag2O, Bi2O3, carbon black, graphite, titanium oxide, iron oxide, aluminum oxide, zirconium silicate, zirconium oxide, iron(II) oxide, iron(III) oxide, manganese dioxide, iron oxide (ilmenite), chromium oxide, carbides (e.g., SiC, TiC, or WC), or mixtures thereof. Examples of opacifying compound precursors include, but are not limited to, TiOSO4 or TiOCl2. In some embodiments, the opacifying compounds used as additives may exclude silicon carbide whiskers or fibers. When an aerogel composition is intended for use in electrical devices, such as batteries as a barrier layer or other related applications, a composition containing an opacifier can preferably have high dielectric strength with high volume and surface resistivity. In such embodiments, the carbon additive used as the opacifier can be nonconductive or modified to reduce conductivity. For example, the opacifier can be surface-oxidized to reduce conductivity. In some embodiments, a carbonaceous additive having inherent conductivity can be used as an opacifier in an aerogel composition for use in electrical devices. In such embodiments, the conductive carbonaceous additive can be used at a concentration below the percolation threshold to provide a composition with dielectric strength suitable for use in electrical devices.

[0184] The aerogel composition may contain one or more fire-class additives. In the context of this disclosure, the term "fire-class additive" refers to a material that has an endothermic effect in the context of a reaction to fire and can be incorporated into the aerogel composition. Furthermore, in certain embodiments, the fire-class additive may initiate the thermal decomposition (T) of the aerogel composition in which the fire-class additive is present. dThe onset of endothermic decomposition is 100°C or less higher than (E D ) has, in certain embodiments, a fire-class additive is present in the aerogel composition T d E is 50°C lower than D It also has. In other words, the E of the Fire class additive D teeth, From JPEG0007900291000001.jpg1470 It has the range JPEG0007900291000002.jpg1478: JPEG0007900291000003.jpg33125

[0185] Prior to or simultaneously with, or even subsequently with, the fire-class additives may be mixed with, or otherwise dispersed with, a medium containing ethanol and optionally up to 10% by volume of water (e.g., silica sols prepared from alkyl silicates or water glass in various ways as understood in the prior art). The mixture may be mixed and / or stirred as necessary to achieve substantially uniform dispersion of the additives in the medium. While not bound by theory, utilizing the hydrated forms of the clays and other fire-class additives described above can yield additional endothermic effects. For example, halloysite clay (commercially available from Applied Minerals, Inc. under the trade name DRAGONITE, or simply as Halloysite from Imerys), kaolinite clay, are hydrated forms of aluminum silicate clay and have an endothermic effect by releasing hydrated water at high temperatures (gas dilution). As another example, hydrated forms of carbonates can release carbon dioxide when heated or at high temperatures.

[0186] In the context of this disclosure, the term “heat of dehydration” means the amount of heat required to vaporize (and, where applicable, dihydroxylate) water from a material that is in a hydrated form when not exposed to high temperatures. Heat of dehydration is typically expressed on a unit weight basis.

[0187] In certain embodiments, the Fire Class additives of the Disclosure have an onset of thermal decomposition at approximately 100°C or higher, approximately 130°C or higher, approximately 200°C or higher, approximately 230°C or higher, approximately 240°C or higher, approximately 330°C or higher, 350°C or higher, approximately 400°C or higher, approximately 415°C or higher, approximately 425°C or higher, approximately 450°C or higher, approximately 500°C or higher, approximately 550°C or higher, approximately 600°C or higher, approximately 650°C or higher, approximately 700°C or higher, approximately 750°C or higher, approximately 800°C or higher, or in a range between any two of these values. In certain embodiments, the Fire Class additives of the Disclosure have an onset of thermal decomposition at approximately 440°C or 570°C. In certain embodiments, the Fire Class additives of the Disclosure have a T of an aerogel composition (without Fire Class additives) into which the Fire Class additives are incorporated. d The onset of thermal decomposition occurs at a temperature of approximately 50°C or lower, approximately 40°C or lower, approximately 30°C or lower, approximately 20°C or lower, approximately 10°C or lower, approximately 5°C or lower, or within the range of any two of these values.

[0188] The Fire Class additives of this disclosure include phyllosilicate clay (such as illite), kaolin or kaolinite (aluminum silicate; Al2Si2O5(OH)4), metakaolin, halloysite (aluminum silicate; Al2Si2O5(OH)4), endelite (aluminum silicate; Al2Si2O5(OH)4), mica (silica mineral), diaspore (aluminum oxide hydroxide; α-AlO(OH)), gibbsite (aluminum hydroxide), boehmite (aluminum oxide hydroxide; γ-AlO(OH)), montmorillonite, byderite, and pyrophyllite (aluminum silicate; Al2Si4O 10(OH)2), nontronite, brabiite, smectite, lebrierite, letolite, celadonite, attapulgite, chloroparl, volconscoite, alophane, lacévinite, zirnite, severite, mirosilite, cholerite, simolite and newtonite, sodium bicarbonate (NaHCO3), magnesium hydroxide (or magnesium dihydrate, "MDH"), alumina trihydrate ("ATH"), gypsum (calcium sulfate dihydrate; CaSO4·2H2O), barringtonite (MgCO3·2H2O), neskehonite (MgCO3·3H2O), lancefodite (MgCO3·5H2O), hydromagnesite (hydrated magnesium carbonate; Mg5(CO3)4(OH)2·4H2O), dolomite and lithium carbonate, and other carbonates, including but not limited to these, as well as other clay materials. Among clay materials, certain embodiments of the present disclosure use clay materials having at least a partial layered structure. In certain embodiments of the present disclosure, the clay material as a fire-class additive in the aerogel composition has at least some water, such as in a hydrated form. The additive may be in a hydrated crystalline form or may be hydrated during the manufacture / processing of the compositions of the present disclosure. In certain embodiments, the fire-class additive also includes low-melting-point additives that absorb heat without changing the chemical composition. An example of this class is low-melting-point glass, such as inert glass beads. Other additives that may be useful in the compositions of the present disclosure include, but are not limited to, wollastonite (calcium silicate) and titanium dioxide (TiO2). In certain embodiments, other additives may include, but are not limited to, infrared opacifiers such as titanium dioxide or silicon carbide, ceramicizing agents such as low-melting-point glass frit, calcium silicate, or carbides such as phosphates and sulfates. In certain embodiments, the additive may require special processing considerations, such as techniques to ensure that the additive is uniformly distributed and does not aggregate significantly to cause variability in the performance of the product. The processing techniques may include additional static and dynamic mixers, stabilizers, adjustments to process conditions, and other techniques known in the art.

[0189] The amount of additives in the aerogel compositions disclosed herein may depend on the desired properties of the composition. The amount of additives used during the preparation and processing of sol-gel compositions is typically referred to as a weight percentage of the silica content of the sol. The amount of additives in the sol can vary from about 5% to about 70% by weight relative to the silica content. In certain embodiments, the amount of additives in the sol is 10% to 60% by weight relative to the silica content, and in certain preferred embodiments, it is 20% to 40% by weight relative to the silica content. In exemplary embodiments, the amount of additives in the sol relative to the silica content ranges from about 5% to about 20%, about 10% to about 20%, about 10% to about 30%, about 10% to about 20%, about 30% to about 50%, about 35% to about 45%, or about 35% to about 40% by weight relative to the silica content. In some embodiments, the amount of additives in the sol is at least about 10% by weight relative to the silica content or about 10% by weight relative to the silica content. In some embodiments, the amount of additives ranges from about 5% to about 15% by weight relative to the silica content. In certain embodiments, there may be two or more types of additives. One or more Fire-class additives may also be present in the final aerogel composition. In some preferred embodiments, including aluminum fiber-class additives, the additives are present in the aerogel composition at about 60-70% by weight relative to the silica content. For example, in some preferred embodiments, including aluminum Fire-class additives, e.g., kaolin, or a combination of aluminum Fire-class additives, e.g., kaolin and alumina trihydrate ("ATH"), the total amount of additives present in the aerogel composition is about 30-40% by weight relative to the silica content. As another example, in some preferred embodiments, the additives include silicon carbide, the total amount of additives present in the aerogel composition is about 30-40% by weight, e.g., 35% by weight relative to the silica content. As yet another example, in some preferred embodiments, the additives include silicon carbide, the total amount of additives present in the aerogel composition is about 5-15% by weight, e.g., 10% by weight relative to the silica content.

[0190] When referring to a final-strengthened aerogel composition, the amount of additives is typically referred to as a weight percentage of the final-strengthened aerogel composition. The amount of additives in a final-strengthened aerogel composition can vary from about 1% to about 50%, about 1% to about 25%, or about 10% to about 25% of the weight of the strengthened aerogel composition. In exemplary embodiments, the amount of additives in a final-strengthened aerogel composition ranges from about 10% to about 20% by weight of the strengthened aerogel composition. In exemplary embodiments, the amount of additives in a final-strengthened aerogel composition as a weight percentage of the composition is in the range of about 1%, about 2%, about 3%, about 4%, about 5%, about 6%, about 7%, about 8%, about 9%, about 10%, about 11%, about 12%, about 13%, about 14%, about 15%, about 16%, about 17%, about 18%, about 19%, about 20%, or any of the aforementioned percentages. In certain embodiments, the amount of additives in the final strengthened aerogel composition is about 15% by weight of the strengthened aerogel composition. In certain embodiments, the amount of additives in the final strengthened aerogel composition is about 13% by weight of the strengthened aerogel composition. For example, in some preferred embodiments, which include additives such as silicon carbide, the total amount of additives present in the aerogel composition is about 10-20% by weight of the strengthened aerogel composition, for example, about 15% by weight. As another example, in some preferred embodiments, which include silicon carbide as an additive, the total amount of additives present in the aerogel composition is about 3-5% by weight of the strengthened aerogel composition, for example, about 4% by weight.

[0191] In certain embodiments, fire-class additives can be classified or grouped based on their thermal decomposition onset temperature. For example, fire-class additives can be classified or grouped as having thermal decomposition onset temperatures below about 200°C, below about 400°C, or above about 400°C. For example, additives with a thermal decomposition onset temperature below about 200°C include sodium bicarbonate (NaHCO3), neskehonite (MgCO3·3H2O), and gypsum (calcium sulfate dihydrate; CaSO4·2H2O). In another example, additives with a thermal decomposition onset temperature below about 400°C include alumina trihydrate ("ATH"), hydromagnesite (hydrated magnesium carbonate; Mg5(CO3)4(OH)2·4H2O), and magnesium hydroxide (or magnesium dihydrate, "MDH"). In other examples, additives with a thermal decomposition onset temperature of less than approximately 400°C include halloysite (aluminum silicate; Al2Si2O5(OH)4), kaolin or kaolinite (aluminum silicate; Al2Si2O5(OH)4), boehmite (aluminum hydroxide; γ-AlO(OH)), or high-temperature phase change materials (PCMs).

[0192] In certain embodiments of this disclosure, the clay material used as an additive in the aerogel composition, for example, an aluminosilicate clay such as halloysite or kaolinite, is in a dehydrated form, such as metahaloysite or metakaolin. Other additives that may be useful in the compositions of this disclosure include, but are not limited to, wollastonite (calcium silicate) and titanium dioxide (TiO2). In certain embodiments, other additives may include, but are not limited to, infrared opacifiers such as titanium dioxide or silicon carbide, ceramicizing agents such as low-melting-point glass frit, calcium silicate, or carbides such as phosphates and sulfates. In certain embodiments, the additives may require special processing considerations, such as techniques to ensure that the additives are uniformly distributed and do not aggregate significantly to cause variations in the performance of the product. Processing techniques may include additional static and dynamic mixers, stabilizers, adjustments of process conditions, and others known in the art. One or more fire-class additives may also be present in the final aerogel composition.

[0193] In certain exemplary embodiments, improved high-temperature shrinkage properties can be provided by including additives, such as aluminosilicate clay materials, such as halloysite or kaolin, in the aerogel materials and compositions of the Disclosure. An exemplary test method for high-temperature shrinkage is the “Standard Test Method for Linear Shrinkage of Preformed High-Temperature Insulations Subjected to Immersion Heat” (ASTM C356, ASTM International, West Concho Hocken, Pennsylvania). In such a test, called a “thermal soak,” the material is exposed to temperatures exceeding 1000°C for up to 60 minutes. In certain exemplary embodiments, the aerogel materials or compositions of the Disclosure may have high-temperature shrinkage of about 20% or less, about 15% or less, about 10% or less, about 6% or less, about 5% or less, 4% or less, 3% or less, 2% or less, 1% or less, or any combination of linear shrinkage, width shrinkage, thickness shrinkage, or dimensional shrinkage in the range of about two of these values.

[0194] In some exemplary embodiments, certain basic catalysts used to catalyze precursor reactions can introduce trace amounts of alkali metals into the aerogel composition. Trace levels of alkali in aerogel materials, e.g., 100 to 500 ppm, e.g., sodium or potassium, can adversely affect high-temperature shrinkage and thermal durability. However, without being bound by any particular mechanism or theory, aluminosilicate clay materials such as halloysite or kaolin can capture transient alkalis, e.g., sodium or potassium, thereby reducing or eliminating the effect of alkali on shrinkage and thermal durability. In specific embodiments of this disclosure, the aluminosilicate clay material is a dehydrated form, e.g., metahaloysite or metakaolin. For example, an aerogel material or composition containing more than about 0.5% by weight of metakaolin or metahaloysite relative to the silica content can significantly reduce thermal shrinkage and thermal durability. In exemplary embodiments, an aerogel material or composition may contain amounts of metakaolin or metahaloysite ranging from about 0.5% by weight to about 3.0% by weight relative to the silica content.

[0195] Figure 1 shows test data of a sample of a thermal control member material according to an embodiment disclosed herein, in which a temperature of 650°C was applied to one surface of the thermal control member, i.e., the high-temperature side, and the temperature of the other surface of the thermal control member, i.e., the low-temperature side, was measured over time. The control sample corresponds to the composition of Example 1, which is described in more detail below. Samples A, B, and C are embodiments of the thermal control member disclosed herein, comprising kaolin as an additive. Sample A corresponds to the composition of Example 2, which is described in more detail below. Sample B corresponds to the composition of Example 4 below. Sample C corresponds to the composition of Example 3 below. As shown in Figure 1, the composition containing kaolin provides a time to reach a temperature of 75°C on the low-temperature side in about 30 seconds, a time to reach a temperature of 120°C on the low-temperature side in about 1 minute, a time to reach a temperature of 150°C on the low-temperature side in about 90 seconds, and a time to reach a temperature of 180°C on the low-temperature side in about 4 minutes. The exceptionally good performance using kaolin mineral as an additive in the temperature range below 200°C was surprising and unexpected.

[0196] In certain embodiments of this disclosure, methods are provided for preparing reinforced aerogel compositions having fire-class performance. The fire-class compositions of these embodiments also possess sufficient hydrophobicity for use as thermal insulation in industrial environments, as measured by water absorption and low thermal conductivity, to help meet increasingly demanding energy-saving needs. To obtain these combinations of desirable properties, simply adding additives or fire-class additives is not sufficient. While various substitutions and combinations or various additives can be tried to arrive at an optimized solution, such efforts are not always successful and present the risk of viable manufacturing with respect to reproducible quality control of these desired properties. A key aspect of these embodiments is to evaluate the thermal behavior (assessed by thermogravimetric or differential scanning calorimetry) of a composition that would otherwise provide all desirable properties except fire resistance, and to consider fire-class additives that closely match the temperature at which most heat is released with the temperature at which most heat is absorbed, or alternatively, to initiate or alternatively initiate the thermal decomposition of the underlying composition.

[0197] In certain embodiments, the desired combustion characteristics of the final composition may include not only intrinsic characteristics such as combustion heat (ISO 1716), but also system combustion characteristics such as the reaction to combustion performance according to ISO 1182. In the case of ISO 1182, weight loss, furnace temperature rise, and flame time are evaluated when exposed to a furnace at a temperature of approximately 750°C.

[0198] Fiber or OCMF-reinforced aerogel compositions can have various components that add oxidizable organic content (fuel) to the system. Furthermore, they can have various other components that do not contribute as fuel but may hinder combustion when exposed to fire. Therefore, the combustion behavior of such systems cannot be simply predicted based on their components alone. In situations where multiple properties are desired, in certain embodiments, the composition should be achieved regardless of its fire-retardant properties, and the thermal performance of such an achieved composition should be evaluated to find an appropriate class of fire-retardant additive that provides fire-retardant properties without impairing other properties that the starting composition sought to provide.

[0199] In certain embodiments, the initiation of thermal decomposition is an important characteristic of the composition. In certain other embodiments, the peak heat release temperature can be an important characteristic for developing enhanced fire-resistant aerogel compositions. When multiple fuel components are present in a composition identified by multiple peaks in the DSC curve, such compositions function well by matching the peak heat release temperature of the enhanced aerogel composition with a fire-class additive having an endothermic peak heat release temperature of 140°C, 120°C, 100°C, or within 80°C. In many embodiments, the endothermic peak heat release temperature is within 50°C.

[0200] The aerogel materials and compositions of this disclosure have been shown to be highly effective as thermal insulation materials. However, the applications of the methods and materials of this disclosure are not intended to be limited to applications related to thermal insulation. The methods and materials of this disclosure can be applied to any system or application that would benefit from the specific combination of properties or procedures provided by the materials and methods of this disclosure. Examples

[0201] The following embodiments provide various non-limiting embodiments and characteristics of the present disclosure. In the following embodiments, the weight percent of additives is provided on a basis of 100%, which is the total weight of the aerogel composition. Figures 1 and 2 are charts showing thermal control members that control the warm behavior of the following embodiments. Example 1

[0202] A glass fiber-reinforced silica aerogel composition was prepared according to the method disclosed above. The reinforced silica aerogel composition had a thickness of approximately 3 mm and contained 21.7 wt% synthetic amorphous silica, 12.2 wt% methylsilylated silica, 62.27 wt% fibrous glass, and 3.8 wt% iron oxide (Fe2O3). An 8-inch square sample of this composition was evaluated using a high-temperature surface performance test on a high-temperature surface at 650°C. The temperature of the low-temperature surface of the sample composition was measured over a certain period of time. For the sample composition of this example, the time to reach 75°C on the low-temperature surface was approximately 15 seconds, the time to reach 120°C on the low-temperature surface was approximately 30 seconds, the time to reach 150°C on the low-temperature surface was approximately 40 seconds, and the time to reach 180°C on the low-temperature surface was approximately 1 minute. The data for the sample composition of this example corresponds to the "Control" in the table in Figure 1. Example 2

[0203] A glass fiber-reinforced silica aerogel composition was prepared according to the method disclosed above. The reinforced silica aerogel composition had a thickness of approximately 3 mm and contained 15.3 wt% synthetic amorphous silica, 8.6 wt% methylsilylated silica, 37.8 wt% fibrous glass, and 38.3 wt% kaolin. The target silica density was 0.07 g / cc. An 8-inch square sample of this composition was evaluated using a high-temperature surface performance test on a high-temperature surface at 650°C. The temperature of the low-temperature surface of the sample composition was measured over a period of time. For the sample composition of this example, the time to reach 75°C on the low-temperature surface was approximately 32 seconds, the time to reach 120°C on the low-temperature surface was approximately 1 minute, the time to reach 150°C on the low-temperature surface was approximately 90 seconds, and the time to reach 180°C on the low-temperature surface was approximately 4 minutes. The data for the sample composition of this example corresponds to "A" in the table in Figure 1. Example 3

[0204] A glass fiber-reinforced silica aerogel composition was prepared according to the method disclosed above. The reinforced silica aerogel composition had a thickness of approximately 3 mm and contained 15.3 wt% synthetic amorphous silica, 8.6 wt% methylsilylated silica, 37.8 wt% fibrous glass, and 38.3 wt% kaolin. The target silica density was 0.09 g / cc. An 8-inch square sample of this composition was evaluated using a high-temperature surface performance test on a high-temperature surface at 650°C. The temperature of the low-temperature surface of the sample composition was measured over a period of time. For the sample composition of this example, the time to reach 75°C on the low-temperature surface was approximately 38 seconds, the time to reach 120°C on the low-temperature surface was approximately 68 seconds, the time to reach 150°C on the low-temperature surface was approximately 102 seconds, and the time to reach 180°C on the low-temperature surface was approximately 4 minutes. The data for the sample composition of this example corresponds to "C" in the table in Figure 1. Example 4

[0205] A glass fiber-reinforced silica aerogel composition was prepared according to the method disclosed above. The reinforced silica aerogel composition had a thickness of approximately 3 mm and contained 15.3 wt% synthetic amorphous silica, 8.6 wt% methylsilylated silica, 37.8 wt% fibrous glass, and 38.3 wt% kaolin and ATH combination. The target silica density was 0.07 g / cc. An 8-inch square sample of this composition was evaluated using a high-temperature surface performance test on a high-temperature surface at 650°C. The temperature of the low-temperature surface of the sample composition was measured over a period of time. For the sample composition of this example, the time to reach 75°C on the low-temperature surface was approximately 36 seconds, the time to reach 120°C on the low-temperature surface was approximately 1 minute, the time to reach 150°C on the low-temperature surface was approximately 96 seconds, and the time to reach 180°C on the low-temperature surface was approximately 3 minutes and 21 seconds. The data for the sample composition of this example corresponds to "B" in the table in Figure 1. Example 5

[0206] A glass fiber-reinforced silica aerogel composition was prepared according to the method disclosed above. The reinforced silica aerogel composition had a thickness of approximately 3.5 mm and contained 21.7 wt% synthetic amorphous silica, 12.2 wt% methylsilylated silica, 62.27 wt% fibrous glass, and 3.8 wt% iron oxide (Fe2O3). An 8-inch square sample of this composition was evaluated using a high-temperature surface performance test on a high-temperature surface at 650°C. The temperature of the low-temperature surface of the sample composition was measured over a certain period of time. For the sample composition of this example, the time to reach 75°C on the low-temperature surface was approximately 13 seconds, the time to reach 120°C on the low-temperature surface was approximately 22 seconds, the time to reach 150°C on the low-temperature surface was approximately 29 seconds, and the time to reach 180°C on the low-temperature surface was approximately 36 seconds. The data for the sample composition of this example corresponds to the "control" in the table in Figure 2. Example 6

[0207] Sols of methyltriethoxysilane (MTES) and tetraethoxysilane (TEOS) or polyethyl silicate (Silbond 40) were prepared separately by hydrolysis under acidic conditions in ethanol. By adjusting the ratio and concentration of the sol materials, a hydrophobic material content was obtained from approximately 36 wt% MTES, and an aerogel with an organic content of approximately 8.0 wt% was obtained in the aerogel material. Silicon carbide (SiC) was incorporated into the sols at a weight percentage of at least 35 wt% relative to the silica content. The combined sols were then stirred for at least 1 hour.

[0208] Guanidine hydroxide (2M) was added to a sol prepared to a concentration sufficient to target an aerogel density of approximately 0.07–0.085 g / cc. The catalyzed SiC-containing sol was cast onto the fiber-reinforced phase and gelled. Immediately before and after gelling, the fiber-reinforced wet gel was subjected to a series of molding steps using heavy stainless steel rollers. Using a rigid, incompressible gauge block placed at the edge of the wet gel, the wet gel was repeatedly rolled up to four times to a controlled thickness of 3.0 mm. After curing at room temperature for up to one hour, the aerogel material was aged at 68°C for approximately 12 hours in an ethanol aging fluid with a fluid-to-gel ratio of approximately 3:1. The aged gel was solvent-extracted with supercritical CO2 and then dried at 110°C for 2 hours.

[0209] The fiber reinforcement phase is approximately 250 g / m². 2 The resulting material was a uniform nonwoven fabric composed of textile-grade glass fibers (E-glass composition) with a density of approximately 5.6 mm in thickness. The obtained reinforced silica aerogel composition was approximately 2.5 mm thick and consisted of approximately 44% aerogel (containing approximately 28% synthetic amorphous silica and approximately 16% methylsilylated silica), 41% fibrous glass, and 15% silicon carbide, resulting in a predicted material density of approximately 0.20 g / cc (given an aerogel density of 0.085 g / cc).

[0210] An 8-inch square sample of this composition was evaluated using a high-temperature surface performance test on a 650°C surface. The temperature of the low-temperature surface of the sample composition was measured over a certain period of time. In this example, the time to reach 75°C on the low-temperature surface was approximately 13 seconds, the time to reach 120°C was approximately 24 seconds, the time to reach 150°C was approximately 31 seconds, and the time to reach 180°C was approximately 42 seconds. The data for this example's sample composition corresponds to "E" in the table in Figure 2. Example 7

[0211] Sols of methyltriethoxysilane (MTES) and tetraethoxysilane (TEOS) or polyethyl silicate (Silbond 40) were prepared separately by hydrolysis under acidic conditions in ethanol. By adjusting the ratio and concentration of the sol materials, a hydrophobic material content was obtained from approximately 36 wt% MTES, and an aerogel with an organic content of approximately 8.0 wt% was obtained in the aerogel material. Silicon carbide (SiC) was incorporated into the sols at a weight percentage of at least 35 wt% relative to the silica content. The combined sols were then stirred for at least 1 hour.

[0212] Guanidine hydroxide (2M) was added to a sol prepared to a concentration sufficient to target an aerogel density of approximately 0.07–0.085 g / cc. The catalyzed SiC-containing sol was cast onto the fiber-reinforced phase and gelled. Immediately before and after gelling, the fiber-reinforced wet gel was subjected to a series of molding steps using heavy stainless steel rollers. The wet gel was repeatedly rolled up to four times to a controlled thickness of 2.0 mm using a rigid, incompressible gauge block placed at the edge of the wet gel. After curing at room temperature for up to one hour, the aerogel material was aged at 68°C for approximately 12 hours in an ethanol aging fluid with an approximately 3:1 fluid-to-gel ratio. The aged gel was solvent-extracted with supercritical CO2 and then dried at 110°C for two hours.

[0213] The fiber reinforcement phase is approximately 250 g / m². 2The resulting material was a uniform nonwoven fabric composed of textile-grade glass fibers (E-glass composition) with a density of approximately 5.6 mm in thickness. The obtained reinforced silica aerogel composition had a thickness of approximately 2.0 mm and consisted of approximately 36% aerogel (containing approximately 23% synthetic amorphous silica and approximately 13% methylsilylated silica) by weight, 51% fiber, and 13% silicon carbide, resulting in a predicted material density of approximately 0.20 g / cc (given an aerogel density of 0.085 g / cc).

[0214] An 8-inch square sample of this composition was evaluated using a high-temperature surface performance test on a 650°C surface. The temperature of the low-temperature surface of the sample composition was measured over a certain period of time. In the sample composition of this example, the time to reach 75°C on the low-temperature surface was approximately 11 seconds, the time to reach 120°C on the low-temperature surface was approximately 21 seconds, the time to reach 150°C on the low-temperature surface was approximately 31 seconds, and the time to reach 180°C on the low-temperature surface was approximately 39 seconds. The data for the sample composition in this example corresponds to "D" in the table in Figure 2.

[0215] Samples of this composition were evaluated by compression. The deformation of the samples was measured to provide the stress-strain relationship. The data for this analysis are shown in Figure 3. Example 8

[0216] Sols of methyltriethoxysilane (MTES) and tetraethoxysilane (TEOS) or polyethyl silicate (Silbond 40) were prepared separately by hydrolysis under acidic conditions in ethanol. By adjusting the ratio and concentration of the sol materials, a hydrophobic material content was obtained from approximately 36 wt% MTES, and an aerogel with an organic content of approximately 8.0 wt% was obtained in the aerogel material. Silicon carbide (SiC) was incorporated into the sols at a weight percentage of at least approximately 10 wt% relative to the silica content. The combined sols were then stirred for at least 1 hour.

[0217] Guanidine hydroxide (2M) was added to a sol prepared to a concentration sufficient to target an aerogel density of approximately 0.07–0.085 g / cc. The catalyzed SiC-containing sol was cast onto the fiber-reinforced phase and gelled. Immediately before and after gelling, the fiber-reinforced wet gel was subjected to a series of molding steps using heavy stainless steel rollers. Using a rigid, incompressible gauge block placed at the edge of the wet gel, the wet gel was repeatedly rolled up to four times to a controlled thickness of 3.0 mm. After curing at room temperature for up to one hour, the aerogel material was aged at 68°C for approximately 12 hours in an ethanol aging fluid with a fluid-to-gel ratio of approximately 3:1. The aged gel was solvent-extracted with supercritical CO2 and then dried at 110°C for 2 hours.

[0218] The fiber reinforcement phase is approximately 225 g / m². 2 The resulting material was a uniform nonwoven fabric composed of textile-grade glass fibers (E-glass composition) with a density of approximately 4 mm in thickness. The obtained reinforced silica aerogel composition was approximately 2.25 mm thick and consisted of approximately 39% aerogel (containing approximately 25% synthetic amorphous silica and approximately 14% methylsilylated silica), 57% fibrous glass, and 4% silicon carbide, resulting in a predicted material density of approximately 0.16 g / cc (given an aerogel density of 0.075 g / cc).

[0219] An 8-inch square sample of this composition was evaluated using a high-temperature surface performance test on a 650°C surface. The temperature of the low-temperature surface of the sample composition was measured over a certain period of time. In this example, the time to reach 75°C on the low-temperature surface was approximately 9 seconds, the time to reach 120°C was approximately 19 seconds, the time to reach 150°C was approximately 25 seconds, and the time to reach 180°C was approximately 34 seconds. The data for this example sample composition is shown in the chart in Figure 4.

[0220] The advantages described above, and those evident from the above description, are achieved efficiently. Since specific modifications to the above configuration can be made without departing from the scope of the present invention, all matters included in the above description or shown in the accompanying drawings are intended to be construed as illustrative and not as limiting.

[0221] It should also be understood that the following claims are intended to encompass all of the general and specific features of the invention described herein, and all descriptions of the scope of the invention that may be said to lie between them as a matter of language. Some embodiments of the present invention are shown below. [Embodiment 1] A thermal control member, At least one layer of an aerogel composition, wherein the aerogel composition comprises one or more additives, and the additives are present at a level of at least about 5 to 20% by weight of the aerogel composition, At least one compliant member, A thermal control member comprising a heat-capacitive material. [Embodiment 2] The thermal control member according to Embodiment 1, wherein the additive is present in a level of at least about 10 to 20% by weight of the aerogel composition. [Embodiment 3] The thermal control member according to Embodiment 1 or 2, wherein the one or more additives include a fire-class additive. [Embodiment 4] The thermal control member according to Embodiment 1 or 2, wherein the one or more additives include an opaque agent. [Embodiment 5] The one or more additives include a combination of a fire-class additive and an opacifier. A thermal control member according to Embodiment 1 or 2. [Embodiment 6] The battery module according to Embodiment 1 or 2, wherein one or more of the additives include clay minerals. [Embodiment 7] The thermal control member according to Embodiment 1 or 2, wherein one or more of the additives include silicon carbide. [Embodiment 8] A thermal control member according to any one of embodiments 1 to 7, comprising at least two layers of the aerogel composition. [Embodiment 9] The thermal control member according to any one of embodiments 1 to 8, wherein the heat-capacitive material is disposed between at least two layers of the aerogel composition. [Embodiment 10] The thermal control member according to any one of embodiments 1 to 9, wherein the heat-capacitive material includes at least one layer containing a metal. [Embodiment 11] The thermal control member according to any one of embodiments 1 to 10, wherein the at least one compliant member comprises a material selected from the group consisting of polyolefin, polyurethane, phenolic resin, melamine, cellulose acetate, and polystyrene. [Embodiment 12] The thermal control member according to any one of embodiments 1 to 11, wherein the at least one compliant member is disposed between at least two layers of the aerogel composition. [Embodiment 13] A thermal control member according to any one of embodiments 1 to 12, further comprising a thermally conductive material. [Embodiment 14] The thermal control member according to Embodiment 13, wherein the thermal conductive material comprises at least one layer including a metal, carbon, a conductive polymer, or a combination thereof. [Embodiment 15] The thermal control member according to Embodiment 13, wherein the thermal conductive material is disposed between at least two layers of the aerogel composition. [Embodiment 16] The thermal control member according to any one of Embodiments 1 to 15, wherein the aerogel composition has an uncompressible thickness in the range of about 1 mm to about 5 mm. [Embodiment 17] The thermal control member according to Embodiment 16, wherein the aerogel composition has an uncompressible thickness of less than about 3 mm. [Embodiment 18] The thermal control member according to Embodiment 16, wherein the aerogel composition has an uncompressible thickness of less than about 2 mm. [Embodiment 19] The thermal control member according to any one of embodiments 1 to 18, wherein the aerogel composition includes a reinforcing material. [Embodiment 20] The thermal control member according to embodiment 19, wherein the reinforcing material includes fibers. [Embodiment 21] The thermal control member according to Embodiment 20, wherein the fiber is selected from the group consisting of a plurality of separated fibers, woven material, nonwoven material, needle nonwoven, batting, web, mat, felt, and combinations thereof. [Embodiment 22] The thermal control member according to any one of Embodiments 1 to 21, wherein the aerogel of the aerogel composition comprises an inorganic, organic, or inorganic / organic hybrid material. [Embodiment 23] The thermal control member according to any one of Embodiments 1 to 22, wherein the aerogel composition is a silica aerogel composition. [Embodiment 24] The thermal control member according to any one of embodiments 1 to 23, wherein the thermal control member has an incompressible thickness in the range of about 2 mm to about 7 mm. [Embodiment 25] A thermal control member according to any one of embodiments 1 to 24, further comprising an encapsulation member that forms at least one of a first outer surface or a second outer surface. [Embodiment 26] The thermal control member according to any one of Embodiments 1 to 25, wherein the aerogel composition includes an encapsulation member. [Embodiment 27] The thermal control member according to any one of Embodiments 1 to 26, wherein the aerogel composition is bulky. [Embodiment 28] The thermal control member according to any one of embodiments 1 to 27, wherein the aerogel composition is compressible to at least 50% of its incompressible thickness and has sufficient elasticity to return to at least 70% of its incompressible thickness after compression and release. [Embodiment 29] It is a battery module, A first battery cell and a second battery cell, A battery module comprising a thermal control member according to any one of embodiments 1 to 27, wherein the thermal control member is disposed between the first battery cell and the second battery cell. [Embodiment 30] It is a battery module, At least one battery cell, A battery module comprising a thermal control member according to any one of embodiments 1 to 27, wherein the thermal control member is disposed on the surface of at least one battery cell or the surface of the battery module. [Embodiment 31] It is a battery pack, At least one battery cell, A battery pack comprising a thermal control member according to any one of embodiments 1 to 27, wherein the thermal control member is disposed on the surface of at least one battery cell or the surface of the battery pack.

Claims

1. It is a battery module, A first battery cell and a second battery cell, A battery module comprising a thermal control component including the following: A first layer of a fiber-reinforced aerogel composition having a first outer surface and a second outer surface opposite to the first outer surface, wherein the fiber-reinforced aerogel composition contains an opacifying agent present at a level of at least about 5% to about 20% by weight of the fiber-reinforced aerogel composition; A polymer-compliant member disposed on the side of the first layer of the fiber-reinforced aerogel composition corresponding to the first outer surface, comprising one or more of polyolefins, polyurethanes, phenolic resins, melamines, cellulose acetates, and polystyrenes; A first thermally conductive material layer disposed between the first layer of the fiber-reinforced aerogel composition and the polymer-compliant member; The second layer of the fiber-reinforced aerogel composition; and A second thermally conductive material layer disposed between the second layer of the fiber-reinforced aerogel composition and the polymer-compliant member; Here, the second outer surface of the first layer of the fiber-reinforced aerogel composition is positioned adjacent to the first battery cell. The second layer of the fiber-reinforced aerogel composition has a first outer surface and a second outer surface opposite to the first outer surface, The first outer surface of the second layer of the fiber-reinforced aerogel composition is adjacent to the second thermally conductive material layer on the side of the polymer-compliant member opposite to the first layer of the fiber-reinforced aerogel composition, The second outer surface of the second layer of the fiber-reinforced aerogel composition is adjacent to the second battery cell.

2. The battery module according to claim 1, wherein the first layer of the fiber-reinforced aerogel composition has an uncompressible thickness in the range of about 1 mm to about 5 mm.

3. The battery module according to claim 2, wherein the first layer of the fiber-reinforced aerogel composition has an uncompressible thickness of less than about 3 mm.

4. The battery module according to claim 2, wherein the first layer of the fiber-reinforced aerogel composition has an uncompressible thickness of less than about 2 mm.

5. The battery module according to claim 1, wherein the fiber-reinforced aerogel composition comprises an inorganic, organic, or inorganic / organic hybrid aerogel material.

6. The battery module according to claim 1, wherein the fiber-reinforced aerogel composition comprises a silica aerogel composition.

7. The battery module according to claim 1, wherein the thermal control member has an incompressible thickness in the range of about 2 mm to about 7 mm.

8. The battery module according to claim 1, further comprising an encapsulating member that forms at least one of the first outer surface or the second outer surface of the first layer of the fiber-reinforced aerogel composition.

9. The battery module according to claim 1, wherein the milky agent is present in the fiber-reinforced aerogel composition at a level of at least about 10% to about 20% by weight.

10. The milky whitening agent is boron carbide, diatomaceous earth, manganese ferrite, MnO, NiO, SnO, Ag ２ O, Bi ２ O ３ The battery module according to claim 1, selected from the group consisting of carbon black, graphite, titanium oxide, iron oxide, aluminum oxide, zirconium silicate, zirconium oxide, iron(II) oxide, iron(III) oxide, manganese dioxide, iron oxide (ilmenite), chromium oxide, silicon carbide, titanium carbide, tungsten carbide, or mixtures thereof.

11. The battery module according to claim 1, wherein the milky agent contains silicon carbide.

12. The battery module according to claim 1, wherein the first or second thermally conductive material layer comprises at least one layer comprising a metal, carbon, a conductive polymer, or a combination thereof.

13. The battery module according to claim 1, further comprising a heat-capacitive material.

14. Battery system including the following: Battery module housing with an external surface; The battery module according to claim 1, disposed within the battery module housing; and A further thermal control member disposed between the second battery cell and the outer surface of the battery module housing.

15. The battery module according to claim 1, wherein the fiber-reinforced aerogel composition is selected from the group consisting of a plurality of separated fibers, woven materials, nonwoven materials, felt, and combinations thereof.

16. The battery module according to claim 1, wherein the fiber-reinforced aerogel composition is compressible to at least 50% of its incompressible thickness and has sufficient elasticity to return to at least 70% of its incompressible thickness after compression and release.

17. The battery module according to claim 1, wherein the fiber-reinforced aerogel composition has a liquid water absorption rate of less than about 15% by weight.

18. The battery module according to claim 1, wherein the thermal control member has a thermal conductivity of 10 mW / mK to 30 mW / mK.

19. The battery module according to claim 1, wherein when the second outer surface of the first layer of the fiber-reinforced aerogel composition is exposed to a temperature of 650°C or higher, the thermal control member maintains a temperature of 120°C or lower on the first outer surface of the first layer of the fiber-reinforced aerogel composition for at least about 1 minute.

20. The battery module according to claim 1, wherein when the second outer surface of the first layer of the fiber-reinforced aerogel composition is exposed to a temperature of 650°C or higher, the thermal control member maintains a temperature of 180°C or lower on the first outer surface of the first layer of the fiber-reinforced aerogel composition for at least about 4 minutes.

21. It is a battery system, A battery module containing at least one battery cell, Battery system including thermal control components, including the following: A first layer of a fiber-reinforced aerogel composition having a first outer surface and a second outer surface opposite to the first outer surface, wherein the fiber-reinforced aerogel composition contains an opaque agent present at a level of at least about 5% to about 20% by weight of the fiber-reinforced aerogel composition; A polymer-compliant member disposed on the side of the layer of the fiber-reinforced aerogel composition corresponding to the first outer surface, comprising one or more of polyolefins, polyurethanes, phenolic resins, melamines, cellulose acetates, and polystyrenes; A first thermally conductive material layer disposed between the first layer of the fiber-reinforced aerogel composition and the polymer-compliant member; The second layer of the fiber-reinforced aerogel composition; and A second thermally conductive material layer disposed between the second layer of the fiber-reinforced aerogel composition and the polymer-compliant member; Here, The thermally conductive material layer is adjacent to the first outer surface of the layer of the fiber-reinforced aerogel composition, The second outer surface of the layer of the fiber-reinforced aerogel composition is adjacent to the surface of the battery module. The second layer of the fiber-reinforced aerogel composition has a first outer surface and a second outer surface opposite to the first outer surface, The first outer surface of the second layer of the fiber-reinforced aerogel composition is adjacent to the second thermally conductive material layer on the side of the polymer-compliant member opposite to the first layer of the fiber-reinforced aerogel composition, The second outer surface of the second layer of the fiber-reinforced aerogel composition is adjacent to at least one battery cell.

22. It is a battery pack, The outer surface of the battery pack, At least one battery cell is disposed within the space defined by the outer surface of the battery pack, A battery pack comprising a thermal control component including the following: A first layer of a fiber-reinforced aerogel composition having a first outer surface and a second outer surface opposite to the first outer surface, wherein the fiber-reinforced aerogel composition contains an opaque agent present at a level of at least about 5% to about 20% by weight of the fiber-reinforced aerogel composition; A polymer-compliant member disposed on the side of the layer of the fiber-reinforced aerogel composition corresponding to the first outer surface, comprising one or more of polyolefins, polyurethanes, phenolic resins, melamines, cellulose acetates, and polystyrenes; A first thermally conductive material layer existing between the first layer of the fiber-reinforced aerogel composition and the polymer-compliant member; The second layer of the fiber-reinforced aerogel composition; and A second thermally conductive material layer disposed between the second layer of the fiber-reinforced aerogel composition and the polymer-compliant member; Here, The thermally conductive material layer is adjacent to the first outer surface of the layer of the fiber-reinforced aerogel composition, The second outer surface of the layer of the fiber-reinforced aerogel composition is adjacent to the outer surface of the battery pack, The second layer of the fiber-reinforced aerogel composition has a first outer surface and a second outer surface opposite to the first outer surface, The first outer surface of the second layer of the fiber-reinforced aerogel composition is adjacent to the second thermally conductive material layer on the side of the polymer-compliant member opposite to the first layer of the fiber-reinforced aerogel composition, The second outer surface of the second layer of the fiber-reinforced aerogel composition is adjacent to at least one battery cell.

23. The battery pack according to claim 22, wherein the fiber-reinforced aerogel composition includes an encapsulating member.

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