Aerogel composite

The integration of a fiber substrate with a specific aerogel composite in the silica aerogel blankets addresses the issue of insulation reduction under pressure, maintaining effective insulation even at high compression levels.

WO2025075429A1PCT designated stage expired Publication Date: 2025-04-10LG CHEM LTD
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Patent Information

Application Number
PCT/KR2024/015088
Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Priority Date
2024-02-07
Filing Date
2024-10-04
Publication Date
2025-04-10

AI Technical Summary

Technical Problem

Silica aerogel blankets experience a significant reduction in insulation when exposed to pressurized environments due to continuous heat expansion or during installation, where high pressure is applied.

Method used

A fiber substrate integrated with an aerogel composite that features a plurality of open pores and silica aerogel particles, characterized by a specific X-ray scattering pattern, which maintains its insulation properties even under compression.

Benefits of technology

The aerogel complex maintains an excellent level of insulation without significant decrease, as evidenced by a heat pipeline rate that is 1.8 times or less than the pre-compression rate when subjected to pressures up to 24 bars.

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Abstract

The present invention relates to an aerogel composite, which maintains insulation properties at excellent levels even under compression deformation resulting from pressure exerted by various reasons when applied as an insulation material to a battery, an electronic device, a vehicle, an industrial device, a structure, or the like.
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Description

Aerogel composites

[0001] Cross-citation with related application(s)

[0002] This application claims the benefit of priority to Korean Patent Application No. 10-2023-0132930, filed October 5, 2023, and U.S. Patent Application No. 18 / 435,481, filed February 7, 2024, the entire contents of which are incorporated herein by reference.

[0003] The present invention relates to an aerogel composite and its use as an insulating material.

[0004] Aerogels are ultraporous, high surface area (≥500 m) materials with a porosity of approximately 90.0% to 99.9% and pore sizes in the range of 1 nm to 100 nm. 2 / g) is a material with excellent ultra-lightness, ultra-insulation, and ultra-low dielectric properties. Accordingly, research is being actively conducted on the development of aerogel materials, as well as on applications such as transparent and environmentally friendly high-temperature insulators, ultra-low dielectric thin films for highly integrated devices, catalysts and catalyst carriers, electrodes for supercapacitors, and electrode materials for seawater desalination.

[0005] The biggest advantage of aerogel is that it is a super-insulator with a thermal conductivity of less than 0.300 W / m·K, which is lower than that of conventional organic insulation materials such as Styrofoam, and that it can solve the fatal weakness of organic insulation materials, such as vulnerability to fire and the generation of harmful gases in case of fire.

[0006] Typically, aerogels are manufactured by manufacturing hydrogels from silica precursors such as water glass and alkoxysilanes (TEOS, TMOS, MTMS, etc.) and removing the liquid component inside the hydrogel without destroying the microstructure.

[0007] In particular, hydrophobic silica aerogel blankets formed with hydrophobic silica aerogel on fibers are widely used in construction or industrial sites as functional insulating materials that prevent corrosion due to moisture, and can also be usefully used as insulating materials, heat-insulating materials, or fire-retardant materials in aircraft, ships, automobiles, batteries, etc.

[0008] However, when applying such silica aerogel blankets for the above-mentioned purposes, there was a problem in that the insulating properties were significantly reduced, such as when a pressurized environment was provided due to continuous thermal expansion in a neighboring device, or when a large pressure was applied from the surroundings during the installation of the aerogel insulation, causing the aerogel structure to collapse.

[0009] One object of the present invention is to provide an aerogel composite or an insulating member including the same, which can maintain a constant level of insulating properties without significantly deteriorating even when exposed to a pressurized environment.

[0010] However, the technical problems to be solved by the present invention are not limited to the problems mentioned above, and other problems not mentioned can be clearly understood by those skilled in the art from the description below.

[0011] According to one embodiment of the present invention, there is provided an aerogel composite comprising a fiber substrate; and an aerogel having a plurality of open pores formed therein, wherein the aerogel comprises a plurality of silica aerogel particles, and in a small angle X-ray scattering (SAXS) graph in which scattering intensity versus wave number is expressed logarithmically for the aerogel particles, a slope in a wave number range of 0.015 / Å to 0.035 / Å is -2.80 to -2.20.

[0012] The above-mentioned incineration X-ray scattering graph may be for aerogel particles detached from the aerogel composite.

[0013] The above-mentioned incineration X-ray scattering graph may be for aerogel particles within the aerogel composite.

[0014] When the cross-section of the above aerogel composite is compressed by applying pressures of 3 bar, 9 bar, and 24 bar in the horizontal direction (transverse direction), the thermal transmittance after compression may be 1.8 times or less compared to the thermal transmittance before compression.

[0015] When the cross-section of the above aerogel composite is compressed by applying a pressure of 3 bar, 9 bar, and 24 bar in the horizontal direction (transverse direction), the thermal transmittance after compression may be more than 1 time and less than 1.8 times the thermal transmittance before compression.

[0016] For the above aerogel composite, the thermal transmittance before and after compression can satisfy the following equation 4:

[0017] [Formula 4]

[0018] {(Thermal transmittance before and after compression (a)) - (Average of thermal transmittances before and after compression (b))} = (Average of thermal transmittances before and after compression (b)) XA

[0019] In the above equation 4, the thermal transmittance before and after compression (a) refers to the thermal transmittance obtained after compression at 0 bar, 3 bar, 9 bar, or 24 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite, and the average value of the thermal transmittances before and after compression (b) refers to the average value of the thermal transmittance of the unpressurized aerogel composite and the thermal transmittances obtained after compression at pressure values ​​of 3 bar, 9 bar, and 24 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite, and A is a real number of -0.40 to +0.40.

[0020] For the above aerogel composite, the thermal transmittance before and after compression can satisfy the following equation 4:

[0021] [Formula 4]

[0022] {(Thermal transmittance before and after compression (a)) - (Average of thermal transmittances before and after compression (b))} = (Average of thermal transmittances before and after compression (b)) XA

[0023] In the above equation 4, the thermal transmittance before and after compression (a) refers to the thermal transmittance obtained after compression at 0 bar, 3 bar, or 9 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite, and the average value of the thermal transmittances before and after compression (b) refers to the average value of the thermal transmittances obtained after compression at pressure values ​​of 0 bar, 3 bar, and 9 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite, and A is a real number of - 0.23 to + 0.23.

[0024] The thermal transmittance obtained after compression at pressures of 3 bar, 9 bar, and 24 bar in the horizontal direction (transverse direction) for the cross-section of the above aerogel composite can satisfy the following equation 5:

[0025] [Formula 5]

[0026] {(Thermal transmittance after compression (c) - Average value of thermal transmittances after compression (d))} = (Average value of thermal transmittances after compression (d)) XB

[0027] In the above equation 5, the thermal transmittance after compression (c) means the thermal transmittance obtained after compression with a pressure of 3 bar, 9 bar or 24 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite, and the average value of the thermal transmittances after compression (d) means the average value of the thermal transmittances obtained after compression by applying a pressure of 3 bar, 9 bar and 24 bar, respectively, in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite, and B is a real number of -0.30 to +0.30.

[0028] For the above aerogel composite, the rate of change (C) of the thermal transmittance after compression per unit applied pressure, expressed by Equation 6 below, can be a real number from - 0.15 to + 0.15:

[0029] [Formula 6]

[0030] C = {(thermal transmittance after compression at pressure x - thermal transmittance after compression at pressure y)} / (x - y)

[0031] In the above equation 6, x and y are each independently 3 bar or 24 bar, but are different pressure values.

[0032] When pressures of 3 bar, 9 bar, and 24 bar are applied in the horizontal direction (transverse direction) to the cross-section of the above aerogel composite, the compression recovery rate expressed by the following Equation 2 may be 60% or more:

[0033] [Formula 2]

[0034] Compression recovery rate (%) = {(cross-sectional thickness of aerogel composite after compression) / (cross-sectional thickness of aerogel composite before compression)} X 100

[0035] The above aerogel may include pores having a pore diameter of 30 nm or less, in an amount of 30% to 45% of the pore volume of the skeletal structure.

[0036] The above aerogel may be composed of silica, methylsilylated silica, dimethylsilylated silica, trimethylsilylated silica, or a mixture thereof.

[0037] The above aerogel particles may include particles in which multiple aerogel particles having a particle size of greater than 0 and less than or equal to 5 nm are aggregated or bonded.

[0038] The average particle diameter of the above-mentioned aggregated or combined particles may be 5 to 2,000 nm.

[0039] The above fiber substrate may include at least one selected from the group consisting of polyester, polyolefin terephthalate, poly(ethylene) naphthalate, polycarbonate, cotton, carbon, polyacrylonitrile (PAN), oxidized PAN, non-carbonized heat-treated PAN, glass fiber, silica fiber, polyaramid fiber, polyolefin fiber, fluoropolymer fiber, silicon carbide fiber, ceramic paper, ceramic fiber, acrylic polymer fiber, basalt fiber, wool, silk, hemp, leather, suede fiber, PBO-xylon fiber (made of Tobo), liquid crystal material fiber, polyurethane fiber, polyamide fiber, wool fiber, boron, aluminum, iron, stainless steel fiber, or PEEK, PES, PET, PEK, and PPS.

[0040] The thickness of the above aerogel composite may be from 0.5 mm to 20 mm.

[0041] The density of the above aerogel composite is 0.05 to 0.50 g / cm 3 It could be.

[0042] The above aerogel composite has a compressive strength of 20 kPa to 80 kPA at 10% strain and a tensile strength of 30 N / cm. 2 Up to 60 N / cm 2 It could be.

[0043] According to another embodiment of the present invention, there is provided an insulating member comprising an aerogel composite provided by the present invention.

[0044] The above insulating member may further include a support member positioned on at least one of the upper and lower surfaces of the aerogel composite.

[0045] The aerogel composite provided in the present invention, when applied as an insulating material to batteries, electronic devices, automobiles, industrial devices, or structures, can maintain excellent levels of insulating properties without significantly reducing them even when pressure is applied to the aerogel composite due to expansion of various devices or structures located adjacent thereto or other causes, thereby causing compression deformation.

[0046] Figure 1 shows a graph according to small-angle X-ray diffraction (SAXS) analysis of aerogel powder (particles) detached from the aerogel composites of Examples 1 and 3 in Experimental Example 2, and the aerogel composite of Example 1.

[0047] Figure 2 shows a graph according to small-angle X-ray diffraction (SAXS) analysis of aerogel powder (particles) detached from the aerogel composites of Comparative Examples 1 and 2 in Experimental Example 2.

[0048] According to one embodiment of the present invention, there is provided an aerogel composite comprising a fiber substrate; and an aerogel having a plurality of open pores formed therein, wherein the aerogel comprises a plurality of silica aerogel particles, and in a small angle X-ray scattering (SAXS) graph in which scattering intensity versus wave number is expressed logarithmically for the silica aerogel particles, a slope in a wave number range of 0.015 / Å to 0.035 / Å is -2.80 to -2.20.

[0049] The above-mentioned incineration X-ray scattering graph may be for silica aerogel particles detached from the aerogel composite.

[0050] The above-mentioned small-angle X-ray scattering graph may be for silica aerogel particles within the aerogel composite.

[0051] When the cross-section of the above aerogel composite is compressed by applying pressures of 3 bar, 9 bar, and 24 bar in the horizontal direction (transverse direction), the thermal transmittance after compression may be 1.8 times or less compared to the thermal transmittance before compression.

[0052] When the cross-section of the above aerogel composite is compressed by applying a pressure of 3 bar, 9 bar, and 24 bar in the horizontal direction (transverse direction), the thermal transmittance after compression may be more than 1 time and less than 1.8 times the thermal transmittance before compression.

[0053] For the above aerogel composite, the thermal transmittance before and after compression can satisfy the following equation 4:

[0054] [Formula 4]

[0055] {(Thermal transmittance before and after compression (a)) - (Average of thermal transmittances before and after compression (b))} = (Average of thermal transmittances before and after compression (b)) XA

[0056] In the above equation 4, the thermal transmittance before and after compression (a) refers to the thermal transmittance obtained after compression at 0 bar, 3 bar, 9 bar, or 24 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite, and the average value of the thermal transmittances before and after compression (b) refers to the average value of the thermal transmittance of the unpressurized aerogel composite and the thermal transmittances obtained after compression at pressure values ​​of 3 bar, 9 bar, and 24 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite, and A is a real number of -0.40 to +0.40.

[0057] For the above aerogel composite, the thermal transmittance before and after compression can satisfy the following equation 4:

[0058] [Formula 4]

[0059] {(Thermal transmittance before and after compression (a)) - (Average of thermal transmittances before and after compression (b))} = (Average of thermal transmittances before and after compression (b)) XA

[0060] In the above equation 4, the thermal transmittance before and after compression (a) refers to the thermal transmittance obtained after compression at 0 bar, 3 bar, or 9 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite, and the average value of the thermal transmittances before and after compression (b) refers to the average value of the thermal transmittance of the unpressurized aerogel composite and the thermal transmittances obtained after compression at pressure values ​​of 3 bar and 9 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite, and A is a real number of - 0.23 to + 0.23.

[0061] The thermal transmittance obtained after compression at pressures of 3 bar, 9 bar, and 24 bar in the horizontal direction (transverse direction) for the cross-section of the above aerogel composite can satisfy the following equation 5:

[0062] [Formula 5]

[0063] {(Thermal transmittance after compression (c) - Average value of thermal transmittances after compression (d))} = (Average value of thermal transmittances after compression (d)) XB

[0064] In the above equation 5, the thermal transmittance after compression (c) means the thermal transmittance obtained after compression with a pressure of 3 bar, 9 bar or 24 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite, and the average value of the thermal transmittances after compression (d) means the average value of the thermal transmittances obtained after compression by applying a pressure of 3 bar, 9 bar and 24 bar, respectively, in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite, and B is a real number of -0.30 to +0.30.

[0065] For the above aerogel composite, the rate of change (C) of the thermal transmittance after compression per unit applied pressure, expressed by Equation 6 below, can be a real number from - 0.15 to + 0.15:

[0066] [Formula 6]

[0067] C = {(thermal transmittance after compression at pressure x - thermal transmittance after compression at pressure y)} / (x - y)

[0068] In the above equation 6, x and y are each independently 3 bar or 24 bar, but are different pressure values.

[0069] When pressures of 3 bar, 9 bar, and 24 bar are applied in the horizontal direction (transverse direction) to the cross-section of the above aerogel composite, the compression recovery rate expressed by the following Equation 2 may be 60% or more:

[0070] [Formula 2]

[0071] Compression recovery rate (%) = {(cross-sectional thickness of aerogel composite after compression) / (cross-sectional thickness of aerogel composite before compression)} X 100

[0072] The above aerogel may include pores having a pore diameter of 30 nm or less, in an amount of 30% to 45% of the pore volume of the skeletal structure.

[0073] The above aerogel may be composed of silica, methylsilylated silica, dimethylsilylated silica, trimethylsilylated silica, or a mixture thereof.

[0074] The above silica aerogel particles may include particles in which multiple aerogel particles having a particle size of more than 0 and less than or equal to 5 nm are aggregated or bonded.

[0075] The average particle diameter of the above-mentioned aggregated or combined particles may be 5 to 2,000 nm.

[0076] The above fiber substrate may include glass fibers.

[0077] The thickness of the above aerogel composite may be from 0.5 mm to 20 mm.

[0078] The density of the above aerogel composite is 0.05 to 0.50 g / cm 3 It could be.

[0079] The above aerogel composite has a compressive strength of 20 kPa to 80 kPA at 10% strain and a tensile strength of 30 N / cm. 2Up to 60 N / cm 2 It could be.

[0080] According to another embodiment of the present invention, there is provided an insulating member comprising an aerogel composite provided by the present invention.

[0081] The above insulating member may further include a support member positioned on at least one of the upper and lower surfaces of the aerogel composite.

[0082] Hereinafter, the present invention will be described in more detail to facilitate understanding. The terms and words used in this specification and claims should not be interpreted based on their conventional or dictionary meanings. Based on the principle that the inventor can appropriately define the concepts of terms to best explain his or her invention, they should be interpreted in a way that aligns with the technical spirit of the present invention.

[0083] According to one embodiment of the present invention, there is provided an aerogel composite comprising a fiber substrate; and an aerogel comprising a plurality of open pores.

[0084] The above "aerogel" includes a plurality of primary aerogel particles having a size of approximately 0 to 10 nm or more and 0 to 5 nm or less, and secondary aerogel particles formed by agglomeration or bonding of these primary aerogel particles, and a plurality of open pores are formed between the primary aerogel particles and between the secondary aerogel particles to form aggregates, thereby forming a three-dimensional network structure of the aerogel.

[0085] The aerogel may be an inorganic silica aerogel formed from a silicon alkoxide compound or water glass as a precursor. As an example, the aerogel may be composed of silica, methylsilylated silica, dimethylsilylated silica, trimethylsilylated silica, or a mixture thereof. As another example, the aerogel may have at least a portion of the SiO2 on the surface of the SiO2 network having a bonding structure of Si-O-SiO2(CH3), Si-O-SiO(CH3)2, or Si-O-Si(CH3)3. A specific silica aerogel manufacturing process is described in detail below.

[0086] Aerogel particles may be positioned on the fiber substrate and in the gaps between adjacent fiber substrates. The "aerogel particles" are individual solid unit particles forming an aerogel, and may include both primary aerogel particles having a size of approximately 0 to 10 nm or less, or approximately 0 to 5 nm or less, preferably approximately 1 nm, and secondary aerogel particles formed by agglomeration of these particles. However, the aerogel in the aerogel composite is mostly secondary aerogel particles or a form in which these are agglomerated and combined, and a trace amount of primary aerogel particles that do not form secondary aerogel particles may be mixed in. The secondary aerogel particles may have an average particle diameter of approximately 5 to 2,000 nm, 5 to 1,000 nm, 5 to 500 nm, 5 to 100 nm, or 5 to 50 nm, but is not limited thereto. The above average particle size may be measured by any means known to those skilled in the art, including, but not limited to, scanning electron microscopy, dynamic light scattering, optical microscopy, or size exclusion methods.

[0087] In general, aerogel particles (secondary aerogel particles) can be manufactured in a shape such as a disk, sphere, cocoon, rod, or irregular shape. However, the aerogel composite provided by the present invention contains a high proportion of oblate disk-shaped secondary aerogel particles having a convex disk shape in the center, thereby increasing the pore ratio within the aerogel composite and improving both strength and elastic recovery rate in the three-dimensional network structure of the aerogel, so that when the aerogel composite is applied as an insulating material in a battery module or the like, it can have excellent recovery ability and insulation retention ability even when compressed due to expansion of the surrounding device.

[0088] In order to analyze the structural characteristics of the aerogel particles of the present invention, small angle X-ray scattering (SAXS) analysis was performed.

[0089] The above "Small Angle X-ray Scattering (SAXS)" is an analytical method that obtains structural information of a material by irradiating the target material with X-rays and measuring the scattered X-rays at small scattering angles. This is achieved by analyzing the elastic scattering behavior of X-rays as they pass through the material and recording the scattering at small angles (typically 0.1 to 10°, hence the name "small angle"). It belongs to the small-angle scattering (SAS) technology family along with small-angle neutron scattering and is typically performed using hard X-rays with a wavelength of 0.07 to 0.2 nm. Depending on the angular range over which a clear scattering signal can be recorded, SAXS can provide structural information on the order of 1 to 100 nm and a repeat distance for partially ordered systems of up to 150 nm.

[0090] In addition, the above "small-angle X-ray scattering (SAXS) graph" is a graph showing the wavenumber dependence of the scattering intensity I (intensity) among the scattered X-rays scattered by the aerogel particles when X-rays are incident on the aerogel composite or aerogel particles, in a range where the scattering angle 2θ is 10° or less. The above scattering angle 2θ can be adjusted by the separation distance between the sample and the detector. In addition, the above small-angle X-ray scattering graph is expressed as the scattering intensity I for the wavenumber Q (unit: Å-1), where the wavenumber Q is calculated from 4πsinθ / λ, and λ represents the wavelength of the X-ray.

[0091] As a result of performing small-angle X-ray scattering (SAXS) analysis on the aerogel composite of the present invention, preferably on the aerogel particles included in the aerogel composite, a graph in which the scattering intensity is expressed logarithmically with respect to the wave number can be obtained, and in this graph, the slope in the wave number range of 0.015 / Å to 0.035 / Å is characterized by being -2.80 to -2.20, -2.70 to -2.20, -2.60 to -2.20, -2.55 to -2.20, or -2.50 to -2.20. In this case, the slope is expressed by calculating the change value of the scattering intensity according to the change in the wave number in the linear regression obtained in the wave number range of 0.015 / Å to 0.035 / Å using the least square method. As an example, the slope in the wave number range of 0.015 / Å to 0.035 / Å in the above graph may be -2.80 to -2.20.

[0092] FIG. 1 is a graph showing the scattering intensity against the wave number obtained by performing small-angle X-ray scattering (SAXS) analysis on aerogel powder (aerogel particles) or an aerogel composite detached from an aerogel composite according to one embodiment of the present invention, expressed logarithmically. It can be seen that the aerogel particles according to the present invention or the aerogel composite including the same have a slope in the range of -2.80 to -2.20 in the wave number range of 0.015 / Å to 0.035 / Å.

[0093] The aerogel composite according to the present invention contains a high proportion of secondary aerogel particles having a structure such as an oblate shape, compared to a conventional aerogel composite, so that the absolute value of the slope in the wavenumber range of 0.015 / Å to 0.035 / Å of a small-angle X-ray scattering (SAXS) graph is larger than that of a conventional aerogel composite. The aerogel composite according to the present invention has a high void ratio for the above reasons and, as described below, has high strength, elastic recovery rate, and compressive recovery rate in the three-dimensional network structure of the aerogel, and has the characteristics of not significantly increasing the thermal transmittance after compression.

[0094] The above small-angle X-ray scattering (SAXS) analysis can be performed on the aerogel composite provided in the present invention or the aerogel powder (aerogel particles) detached from the aerogel composite. In this case, when the small-angle X-ray scattering (SAXS) analysis is performed on the aerogel composite, the small-angle X-ray scattering (SAXS) graph according to the analysis may be for aerogel particles substantially included in the aerogel composite, attached or bonded to a fiber substrate, or included in an aerogel network structure.

[0095] As an example, the small-angle X-ray scattering (SAXS) graph may be obtained as a result of performing small-angle X-ray scattering (SAXS) analysis on aerogel powder (aerogel particles) detached from an aerogel composite.

[0096] At this time, the aerogel powder may be obtained from an aerogel composite manufactured in a rectangular shape (for example, a size of 60 cm X 12 cm in length X width, but is not limited thereto) or a piece of a specimen obtained by cutting a portion thereof.

[0097] The aerogel powder used in the above small-angle X-ray scattering (SAXS) analysis can be prepared through the following process: An aerogel composite measuring 60 cm X 12 cm in length X width was placed in a sealed container, and then repeatedly shaken up and down to induce the detachment of the aerogel powder. To remove the fiber substrate mixed in the detached aerogel powder, the fiber substrate that was visible to the naked eye was first removed using tweezers. Afterwards, the aerogel powder was placed in a 100 ml vial, distilled water was added at a weight ratio of approximately 1:130 (powder:distilled water), and the vial was shaken vigorously 50 times. This removed the fiber substrate that had settled to the bottom layer of the vial and the agglomerates formed by the fiber substrate and the aerogel powder, and carefully obtained only the aerogel powder floating on the upper layer of the distilled water. The obtained aerogel powder was dried at 120°C for 1 hour and used in the experiments of this specification. At this time, for sufficient analysis, at least 10 mg of the final obtained aerogel powder sample is required.

[0098] As an example, the small-angle X-ray scattering (SAXS) graph may be obtained as a result of performing small-angle X-ray scattering (SAXS) analysis on a specimen of an aerogel composite. At this time, the specimen may have a square shape with a size of 1 cm X 1 cm in length X width. In the present invention, when performing small-angle X-ray scattering (SAXS) analysis on a specimen of an aerogel composite as described above, the slope of the small-angle X-ray scattering (SAXS) graph may be expressed as an average value of the slopes measured in the wavenumber range of 0.015 / Å to 0.035 / Å in the graph obtained for each specimen after obtaining 5 specimens from the same aerogel composite and performing small-angle X-ray scattering (SAXS) analysis on all 5 specimens. At this time, the five specimens are manufactured in a rectangular shape (for example, the size may be 60 cm X 12 cm in length and width), and the position 10 cm apart from each corner in the center direction is positioned at the exact center of the specimen, thereby obtaining four specimens. The center portion of the aerogel composite is also positioned at the exact center of the specimen, thereby obtaining one specimen.

[0099] As an example, the small-angle X-ray scattering (SAXS) graph is obtained as a result of small-angle X-ray scattering (SAXS) analysis on aerogel powder detached from the aerogel composite of the present invention, and the slope in the wave number range of 0.015 / Å to 0.035 / Å may be -2.80 to -2.20, -2.70 to -2.20, or -2.60 to -2.20.

[0100] As an example, the small-angle X-ray scattering (SAXS) graph is obtained as a result of small-angle X-ray scattering (SAXS) analysis of aerogel particles included in the aerogel composite of the present invention or a part of the specimen thereof, and the slope in the wave number range of 0.015 / Å to 0.035 / Å may be -2.80 to -2.20, -2.70 to -2.20, or -2.60 to -2.20.

[0101] The above small-angle X-ray scattering (SAXS) analysis was performed by transmitting X-rays through the sample using an Xeuss 2.0 X-ray scattering device from Xenocs, and measuring the scattering intensity (I(q)) according to the scattering wavenumber (Q). More specifically, the small-angle X-ray scattering (SAXS) analysis was performed by placing the sample 2.5 m away from the detector and irradiating X-rays to measure the sample, and a Pilatus3 300K (2D detector) was used as the detector. Then, the scattered 2D diffraction pattern was obtained as an image, and this was calibrated using the sample-to-detector distance obtained through the standard sample, and then the 2D diffraction pattern obtained through the specimen analysis was circularly averaged to convert the scattering intensity (I(q)) according to the scattering wavenumber (Q).

[0102] [Formula 1]

[0103] Q = 4πsinθ / λ

[0104] In the above general formula 1,

[0105] Q is the scattering wavenumber (vector), θ is half the scattering angle, and λ is the wavelength of the irradiated X-ray.

[0106] The aerogel composite having the above characteristics has excellent elasticity, flexibility, and strength, so that even when the aerogel composite is compressed and deformed under a pressurized environment, it has excellent elastic recovery and its insulation properties can also be maintained at a high level.

[0107] The aerogel may have a skeletal structure including mesopores, and may also include micropores or macropores in addition to the mesopores. Here, the "mesopores" are pores having an average pore diameter in a range of about 2 nm to about 50 nm, the "macropores" are pores having an average pore diameter in a range exceeding about 50 nm, and the "micropores" are pores having an average pore diameter in a range less than about 2 nm. The aerogel may include mesopores in an amount of at least 50%, at least 60%, at least 70%, at least 80%, at least 90%, at least 95%, at least 96%, at least 97%, at least 98%, at least 99%, or 100% of the pore volume of the skeletal structure. In one specific example, the aerogel of the present invention may include mesopores. In one specific example, the aerogel of the present invention may include mesopores and micropores. The pore size may be measured by any means known to those skilled in the art, such as, but not limited to, gas adsorption experiments, mercury intrusion, capillary flow porometry, or positron annihilation lifetime spectroscopy (PALS).

[0108] In aerogels, pores with a pore diameter of 30 nm or less are not destroyed or are destroyed at a low rate even when the aerogel is compressed under high pressure (e.g., 37 bar or less, 33 bar or less, or 30 bar or less). Accordingly, in the present invention, by including a certain proportion of pores with a pore diameter of 30 nm or less in the aerogel, the thermal transmittance of the aerogel composite is maintained within a certain range compared to before pressurization even under a pressurized environment.

[0109] Specifically, the aerogel may contain pores having a pore diameter of greater than 0 nm and less than or equal to 30 nm, in an amount of 25%, 26%, 27%, 28%, 29%, 30%, or 31% of the pore volume of the skeletal structure, and may contain 50% or less, 49% or less, 48% or less, 47% or less, 46% or less, 45% or less, 44% or less, 43% or less, 41% or less, or 40% or less, preferably 25% or more but less than 45%, 25% or more but less than 40%, 30% or more but less than 45%, or 30% or more but less than 40%, more preferably 30% or more but less than 45%, or 30% or more but less than 40%, but is not limited thereto. As an example, the skeletal structure may include pores having a pore diameter of greater than 0 and less than or equal to 30 nm, which account for more than 30% and less than or equal to 45% of the pore volume.

[0110] In addition, the aerogel may contain pores having a pore diameter greater than 30 nm, which are 50% or more, 51% or more, 52% or more, 53% or more, 54% or more, 55% or more, 56% or more, 57% or more, 58% or more, 59% or more, or 60% or more of the pore volume of the skeletal structure, and may contain 75% or less, 74% or less, 73% or less, 72% or less, 71% or less, 70% or less, or 69% or less, preferably 55% or more but 75% or less, 60% or more but 75% or less, 55% or more but 70% or less, 60% or more but 70% or less, more preferably 55% or more but 70% or less, or 60% or more but 70% or less, but is not limited thereto.

[0111] The porosity of the above aerogel may be 80% or more, 85% or more, 88% or more, 89% or more, 90% or more, 91% or more, 92% or more, 93% or more, 94% or more, 95% or more, 96% or more, 97% or more, 98% or more, or 99% or more, and preferably 80% or more and 99.9% or less, but is not limited thereto.

[0112] The above aerogel composite has a structure in which at least some of a plurality of aerogel particles are dispersed, preferably bonded, on the surface of a substrate including fibers, and at the same time, at least some of the plurality of aerogel particles are dispersed, preferably positioned, in the empty spaces between the fibers within the substrate. Examples of the substrate may include discrete fibers, films, sheets, nets, fibers, porous bodies, foams, non-woven fabrics, or laminates of two or more layers thereof. In addition, depending on the intended use, the surface may be formed with surface roughness or patterned.

[0113] The above fiber substrate is selected from the group consisting of polyester, polyolefin terephthalate, poly(ethylene) naphthalate, polycarbonate (e.g., rayon, nylon), cotton (e.g., Lycra® from DuPont), carbon (e.g., graphite), polyacrylonitrile (PAN), oxidized PAN, non-carbonized heat-treated PAN (e.g., from SGL Carbon), glass fiber-based materials (S-glass, 901 glass, 902 glass, 475 glass, E-glass, etc.), silica-based fibers such as quartz (e.g., Quartzel® from Saint-Gobain), Q-Fiber® felt (from Johns Manville), Saffil (from Saffil), Durablanket (from Unifrax) and other silica fibers, Duraback® (from carborundum), polyaramid fibers such as Kevlar®, Nomex®, Sontera® (all from DuPont), Conex (from Tyjin), polyolefins such as Tyvek® (from DuPont) (DSM), Dyneema® (DSM), Spectra® (Honeywell), other polypropylene fibers such as Typar®, Xavan® (both from DuPont), fluoropolymers such as PTFE under the Teflon® brand name (DuPont), Goretex® (WL GORE), silicon carbide fibers such as Nicalcon (COI Ceramics), ceramic paper, ceramic fibers such as Nextel (3M), acrylic polymers, basalt fibers, wool, silk, hemp, leather, suede fibers, PBO-Xylon® fibers (Topbo), liquid crystal materials such as Vectan (Hoekst), Cambrel fibers (DuPont), polyurethane, polyamide, wool fibers, boron, aluminum, iron, stainless steel fibers or other thermoplastic resins such as PEEK, PES, PET, PEK, PPS, but without limitation, as long as the fiber can further improve the insulating performance by including spaces or voids into which the aerogel can be easily inserted. Can be used. As an example, the fiber substrate may be made of glass fiber.

[0114] The thickness of the above fiber substrate may be, but is not limited to, 0.5 to 20 mm.

[0115] The density of the above aerogel composite is 0.05 to 0.50 g / cm 3 , 0.05 to 0.35 g / cm 3 , 0.05 to 0.30 g / cm 3 , 0.10 to 0.30 g / cm 3 or 0.15 to 0.30 g / cm 3 It may include, but is not limited to.

[0116] As described above, the aerogel composite provided by the present invention has excellent elasticity, flexibility, and strength, so that even when the aerogel composite is compressed and deformed under a pressurized environment, it has excellent elastic recovery ability and can also maintain a high level of insulation.

[0117] When a pressure of 1 bar or more, 2 bar or more, 3 bar or more, 4 bar or more, 5 bar or more, 6 bar or more, 7 bar or more, 8 bar or more, 9 bar or more, 10 bar or more, 15 bar or more, 20 bar or more, 25 bar or more, 30 bar or more, 35 bar or more, or 40 bar or more, and 50 bar or less, 45 bar or less, 40 bar or less, 35 bar or less, 30 bar or less, 25 bar or less, 20 bar or less, 15 bar or less, 10 bar or less, 9 bar or less, 8 bar or less, 7 bar or less, 6 bar or less, 5 bar or less, 4 bar or less, 3 bar or less, or 2 bar or less is applied to the cross section of the aerogel composite, the compression recovery rate is 45% or more, 50% or more, 55% or more, 60% or more, 62% or more, or 64% The compression recovery can be greater than, or equal to, 66%, greater than, 68%, greater than, 70%, greater than, 72%, greater than, 74%, greater than, 76%, greater than, 78%, greater than, 80%, greater than, 82%, greater than, 84%, greater than, 86%, greater than, 88%, greater than, 90%, greater than, 92%, greater than, 94%, greater than, 95%, greater than, 96%, greater than, 97%, greater than, 98%, or greater than, 99%. As an example, the compression recovery can be greater than, or equal to, 60%.

[0118] The above "compression recovery rate" refers to the percentage of the cross-sectional thickness of the aerogel composite after a predetermined period of time has elapsed after compression compared to the cross-sectional thickness of the aerogel composite before compression, as shown in Equation 2 below. Here, the predetermined period of time may be, for example, 1 second or more, 5 seconds or more, 10 seconds or more, 30 seconds or more, 1 minute or more, 5 minutes or more, 10 minutes or more, 20 minutes or more, 30 minutes or more, 40 minutes or more, 50 minutes or more, 1 hour or more, 2 hours or more, 4 hours or more, 6 hours or more, 8 hours or more, 10 hours or more, 12 hours or more, 24 hours or more, 48 hours or more, or 96 hours or more, but is not limited thereto. As an example, the post-compression recovery rate may be measured 60 minutes (1 hour) after compressing the aerogel composite.

[0119] [Formula 2]

[0120] Compression recovery rate (%) = {(cross-sectional thickness of aerogel composite after compression) / (cross-sectional thickness of aerogel composite before compression)} X 100

[0121] The above "pressure" value refers to the pressure value actually applied to the unit area of ​​the aerogel composite when applying pressure in the horizontal direction (transverse direction) to the cross-section of the aerogel composite using a press device, etc. As an example, when applying pressure in the horizontal direction (transverse direction) to the cross-section of the aerogel composite using a press device including a cylinder, the actual pressure value may refer to a value obtained by dividing the product of the cross-sectional area of ​​the cylinder and the set pressure value by the area of ​​the specimen, as shown in Equation 3 below, but is not limited thereto, and may be calculated differently depending on the specifications of each equipment or manufacturer.

[0122] [Formula 3]

[0123] Actual pressure value = (Inner cylinder radius of press equipment (cm) X Inner cylinder radius of press equipment (cm) X 3.14 X Set pressure value) / (Area of ​​specimen (cm)2 ))

[0124] Applying pressure in a horizontal direction (transverse direction) to the cross-section of the above aerogel composite means applying pressure to the aerogel composite in the direction from the upper surface to the lower surface or from the lower surface to the upper surface, i.e., in the thickness direction.

[0125] The time for applying pressure to the above aerogel composite is not particularly limited, but may be, for example, 1 second or more, 5 seconds or more, 10 seconds or more, 30 seconds or more, 1 minute or more, 5 minutes or more, 10 minutes or more, 20 minutes or more, 30 minutes or more, 40 minutes or more, 50 minutes or more, 1 hour or more, or 2 hours or more, and 24 hours or less, 12 hours or less, 10 hours or less, 8 hours or less, 6 hours or less, 4 hours or less, 2 hours or less, 1 hour or less, 50 minutes or less, 40 minutes or less, 30 minutes or less, 20 minutes or less, 10 minutes or less, 5 minutes or less, 1 minute or less, 30 seconds or less, 10 seconds or less, or 5 seconds or less, but is not limited thereto. As an example, the time for applying pressure may be 10 minutes.

[0126] For example, when a pressure of 3 bar, 9 bar, 15 bar, 24 bar, 30 bar or 33 bar is applied horizontally (transversely) to the cross-section of the aerogel composite, the compression recovery rate may be 45% or more, 50% or more, 55% or more, 60% or more, 62% or more, 64% or more, 66% or more, 68% or more, 70% or more, 72% or more, 74% or more, 76% or more, 78% or more, 80% or more, 82% or more, 84% or more, 86% or more, 88% or more, 90% or more, 92% or more, 94% or more, 95% or more, 96% or more, 97% or more, 98% or more or 99% or more.

[0127] For example, when a pressure of 3 bar or more is applied in the horizontal direction (transverse direction) to the cross-section of the aerogel composite, the compression recovery rate may be 70% or more, 72% or more, 74% or more, 76% or more, 78% or more, 80% or more, 82% or more, 84% or more, 86% or more, 88% or more, 90% or more, 92% or more, 94% or more, 95% or more, 96% or more, 97% or more, 98% or more, or 99% or more.

[0128] For example, when a pressure of 5 bar or more, 10 bar or more, 15 bar or more, 20 bar or more, 25 bar or more, 30 bar or more, or 35 bar or more is applied in the horizontal direction (transverse direction) to the cross-section of the aerogel composite, the compression recovery rate may be 60% or more, 62% or more, 64% or more, 66% or more, 68% or more, 70% or more, 72% or more, 74% or more, 76% or more, 78% or more, 80% or more, 82% or more, 84% or more, 86% or more, 88% or more, 90% or more, 92% or more, 94% or more, 95% or more, 96% or more, 97% or more, 98% or more, or 99% or more.

[0129] For example, when a pressure of 3 bar is applied horizontally (transversely) to the cross-section of the aerogel composite, the compression recovery rate may be 70% or more, 72% or more, 74% or more, 76% or more, 78% or more, 80% or more, 82% or more, 84% or more, 86% or more, 88% or more, 90% or more, 92% or more, 94% or more, 95% or more, 96% or more, 97% or more, 98% or more, or 99% or more, and preferably 70% or more, 72% or more, 74% or more, 76% or more, 78% or more, 80% or more, 82% or more, 84% or more, 86% or more, 88% or more, 90% or more, or 92% or more, and more preferably 84% or more or 86% or more.

[0130] For example, when a pressure of 9 bar is applied to the cross-section of the aerogel composite in the horizontal direction (transverse direction), the compression recovery rate may be 60% or more, 62% or more, 64% or more, 66% or more, 68% or more, 70% or more, 72% or more, 74% or more, 76% or more, 78% or more, 80% or more, 82% or more, 84% or more, 86% or more, 88% or more, 90% or more, 92% or more, 94% or more, 95% or more, 96% or more, 97% or more, 98% or more, or 99% or more, and preferably 60% or more, 62% or more, 64% or more, 66% or more, 68% or more, 70% or more, 72% or more, 74% or more, 76% or more, 78% or more, 80% or more, It may be 82% or more, 84% or more, 86% or more, 88% or more, 90% or more, or 92% or more, and more preferably 72% or more, 74% or more, 76% or more, or 78% or more.

[0131] For example, when a pressure of 15 bar is applied to the cross-section of the aerogel composite in the horizontal direction (transverse direction), the compression recovery rate may be 55% or more, 60% or more, 62% or more, 64% or more, 66% or more, 68% or more, 70% or more, 72% or more, 74% or more, 76% or more, 78% or more, 80% or more, 82% or more, 84% or more, 86% or more, 88% or more, 90% or more, 92% or more, 94% or more, 95% or more, 96% or more, 97% or more, 98% or more, or 99% or more, and preferably 60% or more, 62% or more, 64% or more, 66% or more, 68% or more, 70% or more, 72% or more, 74% or more, 76% or more, 78% or more, It may be 80% or more, 82% or more, 84% or more, 86% or more, 88% or more, 90% or more, or 92% or more, and more preferably 70% or more, 72% or more, 74% or more, or 76% or more.

[0132] For example, when a pressure of 24 bar is applied to the cross-section of the aerogel composite in the horizontal direction (transverse direction), the compression recovery rate may be 55% or more, 60% or more, 62% or more, 64% or more, 66% or more, 68% or more, 70% or more, 72% or more, 74% or more, 76% or more, 78% or more, 80% or more, 82% or more, 84% or more, 86% or more, 88% or more, 90% or more, 92% or more, 94% or more, 95% or more, 96% or more, 97% or more, 98% or more, or 99% or more, and preferably 60% or more, 62% or more, 64% or more, 66% or more, 68% or more, 70% or more, 72% or more, 74% or more, 76% or more, 78% or more, It may be 80% or more, 82% or more, 84% or more, 86% or more, 88% or more, 90% or more, or 92% or more, and more preferably 70% or more or 72% or more.

[0133] For example, when a pressure of 30 bar is applied in the horizontal direction (transverse direction) to the cross-section of the aerogel composite, the compression recovery rate may be 53% or more, 55% or more, 60% or more, 62% or more, 64% or more, 66% or more, 68% or more, 70% or more, 72% or more, 74% or more, 76% or more, 78% or more, 80% or more, 82% or more, 84% or more, 86% or more, 88% or more, 90% or more, 92% or more, 94% or more, 95% or more, 96% or more, 97% or more, 98% or more, or 99% or more, and preferably 60% or more, 62% or more, 64% or more, 66% or more, 68% or more, 70% or more, 72% or more, 74% or more, 76% or more, It may be 78% or more, 80% or more, 82% or more, 84% or more, 86% or more, 88% or more, 90% or more, or 92% or more, and more preferably 68% or more, 70% or more, 72% or more, 74% or more, or 76% or more.

[0134] For example, when a pressure of 33 bar is applied in the horizontal direction (transverse direction) to the cross-section of the aerogel composite, the compression recovery rate may be 53% or more, 55% or more, 60% or more, 62% or more, 64% or more, 66% or more, 68% or more, 70% or more, 72% or more, 74% or more, 76% or more, 78% or more, 80% or more, 82% or more, 84% or more, 86% or more, 88% or more, 90% or more, 92% or more, 94% or more, 95% or more, 96% or more, 97% or more, 98% or more, or 99% or more, and preferably 60% or more, 62% or more, 64% or more, 66% or more, 68% or more, 70% or more, 72% or more, 74% or more, 76% or more, It may be 78% or more, 80% or more, 82% or more, 84% or more, 86% or more, 88% or more, 90% or more, or 92% or more, and more preferably 68% or more, 70% or more, 72% or more, 74% or more, or 76% or more.

[0135] For example, when a pressure of 37 bar is applied horizontally (transversely) to the cross-section of the aerogel composite, the compression recovery rate may be 50% or more, 55% or more, 60% or more, 62% or more, 64% or more, 66% or more, 68% or more, 70% or more, 72% or more, 74% or more, 76% or more, 78% or more, 80% or more, 82% or more, 84% or more, 86% or more, 88% or more, 90% or more, 92% or more, 94% or more, 95% or more, 96% or more, 97% or more, 98% or more, or 99% or more, and preferably 55% or more, 60% or more, 62% or more, 64% or more, 66% or more, 68% or more, 70% or more, 72% or more, 74% or more, It may be 76% or more, 78% or more, 80% or more, 82% or more, 84% or more, 86% or more, 88% or more, 90% or more, or 92% or more, and more preferably 55% or more, 60% or more, or 62% or more.

[0136] The thickness of the above aerogel composite before compression may be 20 mm or less, 15 mm or less, 14 mm or less, 13 mm or less, 12 mm or less, 11 mm or less, 10 mm or less, 9 mm or less, 8 mm or less, 7 mm or less, 6 mm or less, 5 mm or less, 4 mm or less, 3 mm or less, 2 mm or less, or 1 mm or less, and 0.5 mm or more, 1 mm or more, or 2 mm or more, and can be appropriately controlled by controlling the thickness of the substrate or the amount of aerogel sol impregnated into the substrate depending on the application purpose of the aerogel composite.

[0137] When a pressure of 1 bar or more, 2 bar or more, 3 bar or more, 4 bar or more, 5 bar or more, 6 bar or more, 7 bar or more, 8 bar or more, 9 bar or more, 10 bar or more, 15 bar or more, 20 bar or more, 25 bar or more, 30 bar or more, 35 bar or more, or 40 bar or more, and 50 bar or less, 45 bar or less, 40 bar or less, 35 bar or less, 30 bar or less, 25 bar or less, 20 bar or less, 15 bar or less, 10 bar or less, 9 bar or less, 8 bar or less, 7 bar or less, 6 bar or less, 5 bar or less, 4 bar or less, 3 bar or less, or 2 bar or less is applied to the cross-section of the aerogel composite, the thermal transmittance after compression is 3 times or less, 2.9 times or less, 2.8 times or less, or 2.7 times the thermal transmittance before compression. It may be less than, 2.6 times or less, 2.5 times or less, 2.4 times or less, 2.3 times or less, 2.2 times or less, 2.1 times or less, 2 times or less, 1.9 times or less, 1.8 times or less, 1.7 times or less, 1.6 times or less, 1.5 times or less, 1.4 times or less, 1.3 times or less, 1.2 times or less, 1.1 times or less, 1.05 times or less, 1.04 times or less, 1.03 times or less, 1.02 times or less, or 1.01 times or less, and additionally may be 1 times or more, or greater than 1 times.

[0138] The above "thermal transmittance" refers to the heat transfer from air layer to air layer through a solid object, and is 1 m in unit time. 2It refers to the amount of heat that flows when there is a 1 ℃ temperature difference through the cross-sectional area of ​​a material, and it is the value obtained by dividing the thermal conductivity of a material by the thickness of the material. The amount of heat transfer of a material is affected by its thermal conductivity and the thickness of the material. The higher the thermal conductivity and the thinner the thickness, the greater the heat transfer. Therefore, in order to have excellent insulation performance, the thermal conductivity must be low and the thickness must be large. However, when pressure is applied to an elastic material such as an aerogel composite, the thermal conductivity and thickness may change after pressurization. In other words, unless it is a perfectly elastic material, the thickness will inevitably decrease after pressurization, but if the thermal conductivity does not change, the total heat transfer will increase due to the decrease in thickness. In other words, the insulation performance will inevitably decrease. Therefore, whether the insulation performance is maintained after pressurization cannot be confirmed simply by the thermal conductivity after pressurization, but can be confirmed through the thermal transmittance that considers both the thermal conductivity after pressurization and the thickness after pressurization. Even if the thermal conductivity decreases or is maintained after pressurization, if the thickness is greatly reduced after pressurization, the thermal transmittance and total heat transfer are bound to increase significantly.

[0139] The aerogel composite provided in the present invention does not significantly change in thermal conductivity and thickness even after pressurization, so the increase rate of thermal transmittance compared to before pressurization is not high, and the insulation performance can be maintained at an excellent level without a significant decrease in performance due to pressurization.

[0140] The above "post-compressed thermal transmittance" refers to the ratio of thermal conductivity to the thickness of the cross-section of the aerogel composite after a predetermined period of time has elapsed after compressing the cross-section of the aerogel composite by applying a specific level of pressure in the horizontal direction (transverse direction). Here, the predetermined period of time may be, for example, 1 second or more, 5 seconds or more, 10 seconds or more, 30 seconds or more, 1 minute or more, 5 minutes or more, 10 minutes or more, 20 minutes or more, 30 minutes or more, 40 minutes or more, 50 minutes or more, 60 minutes or more, 2 hours or more, 4 hours or more, 6 hours or more, 8 hours or more, 10 hours or more, 12 hours or more, 24 hours or more, 48 hours or more, or 96 hours or more, but is not limited thereto. As an example, the post-compressed thermal transmittance may be measured 60 minutes (1 hour) after compressing the aerogel composite.

[0141] The time for applying pressure to the above aerogel composite is not particularly limited, but may be, for example, 1 second or more, 5 seconds or more, 10 seconds or more, 30 seconds or more, 1 minute or more, 5 minutes or more, 10 minutes or more, 20 minutes or more, 30 minutes or more, 40 minutes or more, 50 minutes or more, 1 hour or more, or 2 hours or more, and 24 hours or less, 12 hours or less, 10 hours or less, 8 hours or less, 6 hours or less, 4 hours or less, 2 hours or less, 1 hour or less, 50 minutes or less, 40 minutes or less, 30 minutes or less, 20 minutes or less, 10 minutes or less, 5 minutes or less, 1 minute or less, 30 seconds or less, 10 seconds or less, or 5 seconds or less, but is not limited thereto. As an example, the time for applying pressure may be 10 minutes.

[0142] For example, when a pressure of 3 bar or more, 5 bar or more, 10 bar or more, 15 bar or more, 20 bar or more, 25 bar or more, 30 bar or more, or 35 bar or more is applied in the horizontal direction (transverse direction) to the cross-section of the aerogel composite, the thermal transmittance after compression is 3 times or less, 2.9 times or less, 2.8 times or less, 2.7 times or less, 2.6 times or less, 2.5 times or less, 2.4 times or less, 2.3 times or less, 2.2 times or less, 2.1 times or less, 2 times or less, 1.9 times or less, 1.8 times or less, 1.7 times or less, 1.6 times or less, 1.5 times or less, 1.4 times or less, 1.3 times or less, 1.2 times or less, 1.1 times or less, 1.05 times or less, 1.04 times or less, or 1.03 times the thermal transmittance before compression. It may be less than, 1.02 times or less, or 1.01 times or less.

[0143] For example, when a pressure of 3 bar, 9 bar, 15 bar, 24 bar, 30 bar or 33 bar is applied to the cross-section of the aerogel composite in the horizontal direction (transverse direction), the thermal transmittance after compression is 3 times or less, 2.9 times or less, 2.8 times or less, 2.7 times or less, 2.6 times or less, 2.5 times or less, 2.4 times or less, 2.3 times or less, 2.2 times or less, 2.1 times or less, 2 times or less, 1.9 times or less, 1.8 times or less, 1.7 times or less, 1.6 times or less, 1.5 times or less, 1.4 times or less, 1.3 times or less, 1.2 times or less, 1.1 times or less, 1.05 times or less, 1.04 times or less, 1.03 times or less, 1.02 times or less, or 1.01 times or less compared to the thermal transmittance before compression. Can be.

[0144] For example, when pressure is applied to the cross-section of the aerogel composite in a horizontal direction (transverse direction) at any one of 3 bar to 33 bar, the thermal transmittance after compression may be 2.0 times or less, 1.9 times or less, 1.8 times or less, 1.7 times or less, 1.6 times or less, 1.5 times or less, 1.4 times or less, 1.3 times or less, 1.2 times or less, 1.1 times or less, 1.05 times or less, 1.04 times or less, 1.03 times or less, 1.02 times or less, or 1.01 times or less compared to the thermal transmittance before compression.

[0145] For example, when pressure is applied to the cross-section of the aerogel composite in a horizontal direction (transverse direction) at any one of 3 bar to 24 bar, the thermal transmittance after compression may be 1.8 times or less, 1.7 times or less, 1.6 times or less, 1.5 times or less, 1.4 times or less, 1.3 times or less, 1.2 times or less, 1.1 times or less, 1.05 times or less, 1.04 times or less, 1.03 times or less, 1.02 times or less, or 1.01 times or less than the thermal transmittance before compression.

[0146] For example, when pressure is applied to the cross-section of the aerogel composite in a horizontal direction (transverse direction) at any one of 3 bar to 9 bar, the thermal transmittance after compression may be 1.7 times or less, 1.6 times or less, 1.5 times or less, 1.45 times or less, 1.4 times or less, 1.3 times or less, 1.2 times or less, 1.1 times or less, 1.05 times or less, 1.04 times or less, 1.03 times or less, 1.02 times or less, or 1.01 times or less compared to the thermal transmittance before compression.

[0147] For example, when pressure is applied to the cross-section of the aerogel composite in a horizontal direction (transverse direction) at any one of 9 bar to 33 bar, the thermal transmittance after compression may be 1.8 times or less, 1.7 times or less, 1.6 times or less, 1.5 times or less, 1.4 times or less, 1.3 times or less, 1.2 times or less, 1.1 times or less, 1.05 times or less, 1.04 times or less, 1.03 times or less, 1.02 times or less, or 1.01 times or less than the thermal transmittance before compression.

[0148] For example, when pressure is applied to the cross-section of the aerogel composite in a horizontal direction (transverse direction) at any one of 9 bar to 24 bar, the thermal transmittance after compression may be 1.7 times or less, 1.6 times or less, 1.5 times or less, 1.4 times or less, 1.3 times or less, 1.2 times or less, 1.1 times or less, 1.05 times or less, 1.04 times or less, 1.03 times or less, 1.02 times or less, or 1.01 times or less compared to the thermal transmittance before compression.

[0149] For example, when pressure is applied to the cross-section of the aerogel composite in a horizontal direction (transverse direction) at any one of 15 bar to 33 bar, the thermal transmittance after compression may be 2.3 times or less, 2.2 times or less, 2.1 times or less, 2 times or less, 1.9 times or less, 1.8 times or less, 1.7 times or less, 1.6 times or less, 1.5 times or less, 1.4 times or less, 1.3 times or less, 1.2 times or less, 1.1 times or less, or 1.05 times or less compared to the thermal transmittance before compression.

[0150] For example, when pressure is applied to the cross-section of the aerogel composite in a horizontal direction (transverse direction) at any one of 15 bar to 30 bar, the thermal transmittance after compression may be 2.3 times or less, 2.2 times or less, 2.1 times or less, 2 times or less, 1.9 times or less, 1.8 times or less, 1.7 times or less, 1.6 times or less, 1.5 times or less, 1.4 times or less, 1.3 times or less, 1.2 times or less, 1.1 times or less, or 1.05 times or less than the thermal transmittance before compression.

[0151] For example, when a pressure of any one of 24 bar to 33 bar is applied to the cross-section of the aerogel composite in the horizontal direction (transverse direction), the thermal transmittance after compression may be 2.7 times or less, 2.6 times or less, 2.5 times or less, 2.4 times or less, 2.3 times or less, 2.2 times or less, 2.1 times or less, 2 times or less, 1.9 times or less, 1.8 times or less, 1.7 times or less, 1.6 times or less, 1.5 times or less, 1.4 times or less, 1.3 times or less, 1.2 times or less, or 1.1 times or less than the thermal transmittance before compression.

[0152] For example, when pressure is applied to the cross-section of the aerogel composite in a horizontal direction (transverse direction) at any one of 24 bar to 30 bar, the thermal transmittance after compression may be 2.7 times or less, 2.6 times or less, 2.5 times or less, 2.4 times or less, 2.3 times or less, 2.2 times or less, 2.1 times or less, 2 times or less, 1.9 times or less, 1.8 times or less, 1.7 times or less, 1.6 times or less, 1.5 times or less, 1.4 times or less, 1.3 times or less, 1.2 times or less, or 1.1 times or less than the thermal transmittance before compression.

[0153] For example, when pressure is applied to the cross-section of the aerogel composite in a horizontal direction (transverse direction) at any one of 30 bar to 33 bar, the thermal transmittance after compression may be 3 times or less, 2.9 times or less, 2.8 times or less, 2.7 times or less, 2.6 times or less, 2.5 times or less, 2.4 times or less, 2.3 times or less, 2.2 times or less, 2.1 times or less, 2 times or less, 1.9 times or less, 1.8 times or less, 1.7 times or less, 1.6 times or less, 1.5 times or less, 1.4 times or less, 1.3 times or less, 1.2 times or less, or 1.1 times or less than the thermal transmittance before compression.

[0154] For example, when a pressure of 3 bar is applied horizontally (transversely) to the cross-section of the aerogel composite, the thermal transmittance after compression may be 1.8 times or less, 1.24 times or less, 1.2 times or less, 1.15 times or less, 1.1 times or less, 1.05 times or less, 1.04 times or less, 1.03 times or less, 1.02 times or less, or 1.01 times or less than the thermal transmittance before compression, and preferably 1.2 times or less, 1.1 times or less, 1.05 times or less, 1.04 times or less, 1.03 times or less, 1.02 times or less, or 1.01 times or less.

[0155] For example, when a pressure of 9 bar is applied horizontally (transversely) to the cross-section of the aerogel composite, the thermal transmittance after compression may be 1.8 times or less, 1.7 times or less, 1.6 times or less, 1.5 times or less, 1.4 times or less, 1.3 times or less, 1.2 times or less, 1.1 times or less, 1.05 times or less, 1.04 times or less, 1.03 times or less, 1.02 times or less, or 1.01 times or less than the thermal transmittance before compression, and preferably may be 1.5 times or less, 1.4 times or less, 1.3 times or less, 1.2 times or less, 1.1 times or less, 1.05 times or less, 1.04 times or less, 1.03 times or less, 1.02 times or less, or 1.01 times or less.

[0156] For example, when a pressure of 15 bar is applied to the cross-section of the aerogel composite in the horizontal direction (transverse direction), the thermal transmittance after compression may be 2.35 times or less, 2.3 times or less, 2.2 times or less, 2.1 times or less, 2 times or less, 1.9 times or less, 1.8 times or less, 1.7 times or less, 1.6 times or less, 1.5 times or less, 1.4 times or less, 1.3 times or less, 1.2 times or less, 1.1 times or less, 1.05 times or less, 1.04 times or less, 1.03 times or less, 1.02 times or less, or 1.01 times or less, and preferably 2 times or less, 1.9 times or less, 1.8 times or less, 1.7 times or less, 1.6 times or less, 1.5 times or less, 1.4 times or less, 1.3 times or less, 1.2 It may be less than 1.1 times, less than 1.05 times, and more preferably less than 1.7 times, less than 1.6 times, less than 1.5 times, less than 1.4 times, less than 1.3 times, less than 1.2 times, or less than 1.1 times.

[0157] For example, when a pressure of 24 bar is applied to the cross-section of the aerogel composite in the horizontal direction (transverse direction), the thermal transmittance after compression may be 2.7 times or less, 2.6 times or less, 2.5 times or less, 2.4 times or less, 2.3 times or less, 2.2 times or less, 2.1 times or less, 2 times or less, 1.9 times or less, 1.8 times or less, 1.7 times or less, 1.6 times or less, 1.5 times or less, 1.4 times or less, 1.3 times or less, 1.2 times or less, 1.1 times or less, 1.05 times or less, 1.04 times or less, 1.03 times or less, 1.02 times or less, or 1.01 times or less, and preferably 2 times or less, 1.9 times or less, 1.8 times or less, 1.7 times or less, 1.6 times or less, or 1.5 times or less. It may be less than, 1.4 times, 1.3 times, 1.2 times, 1.1 times, or 1.05 times, and more preferably less than, 1.7 times, 1.6 times, 1.5 times, 1.4 times, 1.3 times, 1.2 times, or 1.1 times.

[0158] For example, when a pressure of 30 bar is applied to the cross-section of the aerogel composite in the horizontal direction (transverse direction), the thermal transmittance after compression may be 3 times or less, 2.9 times or less, 2.8 times or less, 2.7 times or less, 2.6 times or less, 2.5 times or less, 2.4 times or less, 2.3 times or less, 2.2 times or less, 2.1 times or less, 2 times or less, 1.9 times or less, 1.8 times or less, 1.7 times or less, 1.6 times or less, 1.5 times or less, 1.4 times or less, 1.3 times or less, 1.2 times or less, 1.1 times or less, 1.05 times or less, 1.04 times or less, 1.03 times or less, 1.02 times or less, or 1.01 times or less, and preferably 2.3 times or less, 2.2 times or less, or 2.1 times or less, compared to the thermal transmittance before compression. It may be less than, 2 times less than, 1.9 times less than, 1.8 times less than, 1.7 times less than, 1.6 times less than, 1.5 times less than, 1.4 times less than, 1.3 times less than, 1.2 times less than, 1.1 times less than, or 1.05 times less than, and more preferably, it may be less than, 1.7 times less than, 1.6 times less than, 1.5 times less than, 1.4 times less than, 1.3 times less than, 1.2 times less than, or 1.1 times less than.

[0159] For example, when a pressure of 33 bar is applied to the cross-section of the aerogel composite in the horizontal direction (transverse direction), the thermal transmittance after compression may be 3 times or less, 2.9 times or less, 2.8 times or less, 2.7 times or less, 2.6 times or less, 2.5 times or less, 2.4 times or less, 2.3 times or less, 2.2 times or less, 2.1 times or less, 2 times or less, 1.9 times or less, 1.8 times or less, 1.7 times or less, 1.6 times or less, 1.5 times or less, 1.4 times or less, 1.3 times or less, 1.2 times or less, 1.1 times or less, 1.05 times or less, 1.04 times or less, 1.03 times or less, 1.02 times or less, or 1.01 times or less, and preferably 2.3 times or less, 2.2 times or less, or 2.1 times or less. It may be less than, 2 times less than, 1.9 times less than, 1.8 times less than, 1.7 times less than, 1.6 times less than, 1.5 times less than, 1.4 times less than, 1.3 times less than, 1.2 times less than, or 1.1 times less than, and more preferably, 2.0 times less than, 1.9 times less than, 1.8 times less than, 1.7 times less than, 1.6 times less than, 1.5 times less than, 1.4 times less than, 1.3 times less than, or 1.2 times less than.

[0160] For example, when pressures of 3 bar, 9 bar, and 24 bar are applied horizontally (transversely) to the cross-section of the aerogel composite, the thermal transmittance after compression may be 1.8 times or less or 1.7 times or less than the thermal transmittance before compression, and preferably, it may be more than 1 time, 1.8 times or less, or more than 1 time and 1.7 times or less. For example, the thermal transmittance after compression may be 1.8 times or less than the thermal endurance coefficient before compression. For example, the thermal transmittance after compression may be more than 1 time and 1.8 times or less than the thermal transmittance before compression.

[0161] The aerogel composite provided in the present invention can maintain its insulation performance at an excellent level without significant deterioration, as the thermal transmittance before and after compression is maintained within a specific range, regardless of the pressure applied (or compressed) at any intensity.

[0162] Specifically, the thermal transmittance obtained after compression at at least one pressure value of 0 to 24 bar for the aerogel composite of the present invention can satisfy the following equation 4:

[0163] [Formula 4]

[0164] {(Thermal transmittance before and after compression (a)) - (Average of thermal transmittances before and after compression (b))} = (Average of thermal transmittances before and after compression (b)) XA

[0165] In the above equation 4, the “thermal transmittance before and after compression (a)” means the thermal transmittance obtained after compression at at least one pressure value in the range of 0 to 24 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite, and as an example, may mean the thermal transmittance obtained after compression by applying a pressure of 0 bar, 3 bar, 9 bar, or 24 bar to the aerogel composite. Here, the pressure of 0 bar means no pressure (no compression), and accordingly, the thermal transmittance obtained after compression by applying a pressure of 0 bar means the thermal transmittance of the aerogel composite that is not pressurized.

[0166] In addition, the above "average value (b) of thermal transmittances before and after compression" means the average value of the thermal transmittance of an aerogel composite without pressurization (or compression) and the average value of the thermal transmittances obtained after compression with at least two pressure values ​​in the range of 0 bar or more and 24 bar or less in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite. As an example, it may mean the average value of the thermal transmittance of an aerogel composite without pressurization (non-compressed) and the average value of the thermal transmittances obtained after compression by applying pressure to the aerogel composite with at least two pressure values ​​of 3 bar, 9 bar, and 24 bar.

[0167] The above A is a real number of - 0.40 to + 0.40, a real number of - 0.35 to + 0.35, a real number of - 0.34 to + 0.34, a real number of - 0.33 to + 0.33, a real number of - 0.32 to + 0.32, a real number of - 0.31 to + 0.31, a real number of - 0.30 to + 0.30, a real number of - 0.25 to + 0.25, a real number of - 0.24 to + 0.24, a real number of - 0.23 to + 0.23, a real number of - 0.22 to + 0.22, a real number of - 0.21 to + 0.21, a real number of - 0.20 to + 0.20, a real number of - 0.19 to + 0.19, a real number of - 0.15 to + 0.15, - It can be a real number between 0.14 and + 0.14, a real number between - 0.13 and + 0.13, a real number between - 0.12 and + 0.12, or a real number between - 0.11 and + 0.11.

[0168] As an example, the thermal transmittance of an uncompressed (0 bar compression) aerogel composite may satisfy the above equation 4. In this case, the average value (b) of the thermal transmittances before and after compression may mean the average value of the thermal transmittance of the uncompressed aerogel composite and the thermal transmittance obtained after compression at at least two pressure values ​​among 3 bar, 9 bar, and 24 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite.

[0169] As an example, the thermal transmittance obtained after compressing the aerogel composite at a pressure of 3 bar, 9 bar, or 24 bar may satisfy Equation 4. In this case, the average value (b) of the thermal transmittances before and after compression may mean the average value of the thermal transmittance of the non-compressed (0 bar compressed) aerogel composite and the thermal transmittances obtained after compressing the aerogel composite at at least two pressure values ​​among 3 bar, 9 bar, and 24 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite.

[0170] As an example, the thermal transmittance of an uncompressed (0 bar compression) aerogel composite may satisfy the above equation 4. In this case, the average value (b) of the thermal transmittances before and after compression may mean the average value of the thermal transmittance of the uncompressed aerogel composite and the thermal transmittance obtained after compression at pressure values ​​of 3 bar, 9 bar, and 24 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite.

[0171] As an example, the thermal transmittance obtained after compressing the aerogel composite at a pressure of 3 bar, 9 bar, or 24 bar may satisfy Equation 4. In this case, the average value (b) of the thermal transmittances before and after compression may mean the average value of the thermal transmittance of the non-compressed (0 bar compressed) aerogel composite and the average value of the thermal transmittances obtained after compressing the aerogel composite at pressures of 3 bar, 9 bar, and 24 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite.

[0172] As an example, the thermal transmittance of an uncompressed (0 bar compression) aerogel composite may satisfy the above equation 4. In this case, the average value (b) of the thermal transmittances before and after compression may mean the average value of the thermal transmittance of the uncompressed aerogel composite and the thermal transmittances obtained after compression at pressure values ​​of 3 bar and 9 bar, respectively, in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite.

[0173] As an example, the thermal transmittance obtained after compressing the aerogel composite at a pressure of 3 bar or 9 bar may satisfy Equation 4. In this case, the average value (b) of the thermal transmittances before and after compression may mean the average value of the thermal transmittance of the non-compressed (0 bar compressed) aerogel composite and the average value of the thermal transmittances obtained after compressing the aerogel composite at pressures of 3 bar and 9 bar, respectively, in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite.

[0174] As an example, the average value (b) of the thermal transmittances before and after the compression means the average value of the thermal transmittance of the non-compressed (0 bar compression) aerogel composite and the thermal transmittances obtained after compression by applying pressures of 3 bar, 9 bar and 24 bar in the horizontal direction (transverse direction) to the cross-section of the aerogel composite, and at this time, A may be a real number of -0.40 to +0.40, a real number of -0.35 to +0.35, a real number of -0.30 to +0.30 or a real number of -0.25 to +0.25.

[0175] As an example, the average value (b) of the thermal transmittances before and after the compression means the average value of the thermal transmittance of the non-compressed (0 bar compression) aerogel composite and the thermal transmittances obtained after compression by applying pressures of 3 bar and 9 bar in the horizontal direction (transverse direction) to the cross-section of the aerogel composite, and at this time, the above A may be a real number of -0.23 to +0.23, a real number of -0.22 to +0.22, a real number of -0.21 to +0.21, or a real number of -0.20 to +0.20.

[0176] As an example, the thermal transmittance obtained after compressing the aerogel composite at a pressure of 0 bar, 3 bar, 9 bar, or 24 bar may satisfy the above equation 4. At this time, the average value (b) of the thermal transmittances before and after compression may mean the average value of the thermal transmittance of the non-compressed (0 bar compressed) aerogel composite and the thermal transmittances obtained after compressing the aerogel composite at pressures of 3 bar, 9 bar, and 24 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite. Here, A may be a real number of -0.40 to +0.40.

[0177] As an example, the thermal transmittance obtained after compressing the aerogel composite at a pressure of 3 bar, 9 bar, or 24 bar may satisfy Equation 4. At this time, the average value (b) of the thermal transmittances after compression may mean the average value of the thermal transmittances obtained after compressing the cross-section of the aerogel composite at pressure values ​​of 3 bar, 9 bar, and 24 bar in the horizontal direction (transverse direction). Here, A may be a real number of -0.23 to +0.23.

[0178] The average value (b) of the thermal transmittances before and after compression means the average value of the thermal transmittance of the non-compressed (0 bar compression) aerogel composite and the thermal transmittances obtained after compression by applying pressures of 3 bar and 9 bar in the horizontal direction (transverse direction) to the cross-section of the aerogel composite, and in this case, A may be a real number of -0.23 to +0.23, a real number of -0.22 to +0.22, a real number of -0.21 to +0.21, or a real number of -0.20 to +0.20.

[0179] In addition, the aerogel composite provided in the present invention can maintain its insulation performance at an excellent level without significant deterioration since the thermal transmittance after compression is maintained within a specific range even when pressurized (or compressed) at any pressure.

[0180] Specifically, the thermal transmittance obtained after compression at at least one pressure value of 3 to 30 bar for the aerogel composite of the present invention can satisfy the following equation 5:

[0181] [Formula 5]

[0182] {(Thermal transmittance after compression (c) - Average value of thermal transmittances after compression (d))} = (Average value of thermal transmittances after compression (d)) XB

[0183] In the above formula 5, the “thermal transmittance after compression (c)” means a thermal transmittance obtained after compression at at least one pressure value in the range of 3 to 30 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite, and as an example, it may mean a thermal transmittance obtained after compression by applying a pressure of 3 bar, 9 bar, 15 bar, 24 bar or 30 bar, and as another example, it may mean a thermal transmittance obtained after compression by applying a pressure of 3 bar, 9 bar or 24 bar.

[0184] In addition, the above "average value (d) of thermal transmittances after compression" means an average value of thermal transmittances obtained after compression at at least two pressure values ​​in the range of 3 to 30 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite, and as an example, may mean an average value of thermal transmittances obtained after compression by applying pressures of 3 bar, 9 bar, and 24 bar, respectively.

[0185] The above B is a real number of - 0.30 to + 0.30, a real number of - 0.29 to + 0.29, a real number of - 0.28 to + 0.28, a real number of - 0.27 to + 0.27, a real number of - 0.26 to + 0.26, a real number of - 0.25 to + 0.25, a real number of - 0.24 to + 0.24, a real number of - 0.23 to + 0.23, a real number of - 0.22 to + 0.22, a real number of - 0.21 to + 0.21, a real number of - 0.20 to + 0.20, a real number of - 0.19 to + 0.19, a real number of - 0.15 to + 0.15, a real number of - 0.14 to + 0.14, a real number of - 0.13 to + 0.13, - It can be a real number between 0.12 and + 0.12, a real number between - 0.11 and + 0.11, or a real number between - 0.10 and + 0.10.

[0186] As an example, the thermal transmittance obtained after compressing the aerogel composite at a pressure of 3 bar, 9 bar, or 24 bar may satisfy Equation 5. In this case, in Equation 5, the thermal transmittance after compression (c) refers to the thermal transmittance obtained after compressing the aerogel composite at a pressure value of 3 bar, 9 bar, or 24 bar in the horizontal direction (transverse direction) with respect to the cross-section, and the average value of the thermal transmittances after compression (d) refers to the average value of the thermal transmittances obtained after compressing the aerogel composite at at least two pressure values ​​among 3 bar, 9 bar, and 24 bar in the horizontal direction (transverse direction) with respect to the cross-section.

[0187] As an example, the thermal transmittance obtained after compression at a pressure of 3 bar, 9 bar or 24 bar for the aerogel composite can satisfy Equation 5 above. At this time, in the above formula 5, the thermal transmittance after compression (c) means the thermal transmittance obtained after compression with a pressure value of 3 bar, 9 bar or 24 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite, and the average value of the thermal transmittances after compression (d) means the average value of the thermal transmittances obtained after compression with a pressure value of 3 bar, 9 bar and 24 bar, respectively, in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite, and the above B is a real number of - 0.30 to + 0.30, a real number of - 0.29 to + 0.29, a real number of - 0.28 to + 0.28, a real number of - 0.27 to + 0.27, a real number of - 0.26 to + 0.26, a real number of - 0.25 to + 0.25, a real number of - 0.24 to + 0.24, or a real number of - 0.23 to + 0.23. It could be a mistake.

[0188] As an example, the thermal transmittance obtained after compression at pressures of 3 bar, 9 bar, and 24 bar for the aerogel composite can satisfy Equation 5 above. At this time, in the above formula 5, the thermal transmittance after compression (c) means the thermal transmittance obtained after compression with any one of the pressure values ​​of 3 bar, 9 bar and 24 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite, and the average value of the thermal transmittances after compression (d) means the average value of the thermal transmittances obtained after compression with each of the pressure values ​​of 3 bar, 9 bar and 24 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite, and the above B is a real number of - 0.30 to + 0.30, a real number of - 0.29 to + 0.29, a real number of - 0.28 to + 0.28, a real number of - 0.27 to + 0.27, a real number of - 0.26 to + 0.26, a real number of - 0.25 to + 0.25, a real number of - 0.24 to + 0.24, or a real number of - 0.23 to + It could be a real number of 0.23.

[0189] In addition, for the aerogel composite, the rate of change (C) of the thermal transmittance after compression per unit applied pressure expressed by the following equation 6 may be a real number of - 0.15 or more, - 0.14 or more, - 0.13 or more, - 0.12 or more, - 0.11 or more, - 0.10 or more, - 0.09 or more, - 0.08 or more, - 0.07 or more, - 0.06 or more, - 0.05 or more, - 0.04 or more, - 0.03 or more, - 0.02 or more, or - 0.01 or more, and + 0.15 or less, + 0.14 or less, + 0.13 or less, + 0.12 or less, + 0.11 or less, + 0.10 or less, + 0.09 or less, + 0.08 or less, + 0.07 or less, + 0.06 or less, + It can be a real number of 0.05 or less, + 0.04 or less, + 0.03 or less, + 0.02 or less, or + 0.01 or less. Preferably, it can be a real number of - 0.15 to + 0.15, a real number of - 0.14 to + 0.14, a real number of - 0.13 to + 0.13, a real number of - 0.12 to + 0.12, a real number of - 0.11 to + 0.11, or a real number of - 0.10 to + 0.10:

[0190] [Formula 6]

[0191] C = {(thermal transmittance after compression at pressure x - thermal transmittance after compression at pressure y)} / (x - y)

[0192] In the above equation 6, x and y are each independently a pressure value (unit: bar) within a pressure range of 3 to 24 bar, and are different pressure values.

[0193] As an example, in the above equation 6, x and y can each independently be any one of the pressure values ​​of 3 bar, 9 bar, 15 bar and 24 bar.

[0194] As an example, in Equation 6 above, x may be 24 bar and y may be 3 bar.

[0195] As an example, in Equation 6 above, x may be 24 bar and y may be 9 bar.

[0196] As an example, in Equation 6 above, x may be 15 bar and y may be 9 bar.

[0197] As an example, in Equation 6 above, x may be 24 bar and y may be 15 bar.

[0198] When measuring the recovery rate or thermal transmittance after compression of an aerogel composite using a press device, etc. as described above, a single specimen can be prepared from the aerogel composite and measured. However, if the width or length of the aerogel composite is smaller than the pressure-applying portion of the measuring device depending on the measuring device, the aerogel composite is cut into two or more pieces and rearranged so that both the width and length are larger than the pressure-applying device. Then, the compression recovery rate or thermal transmittance, etc. are measured. The measured values ​​are considered to be substantially the same as for a single specimen.

[0199] As an example, the post-compression recovery rate or post-compression thermal transmittance may be measured for a rectangular aerogel composite specimen having a width X length of 30 cm X 24 cm. In this case, if the width or length of the manufactured aerogel composite is less than 30 cm or 24 cm, respectively, two or more specimens may be arranged in parallel adjacent to each other so that the specimens have a size of 30 cm X 24 cm, and then measurements may be performed on these specimens.

[0200] The above aerogel composite may have excellent mechanical strength, with a compressive strength at 10% strain of 20 kPa to 80 kPA, 20 kPa to 70 kPA, 30 kPa to 80 KPa, 30 kPa to 70 kPA, 35 kPa to 80 kPA, or 35 kPa to 70 kPA. Here, the compressive strength may be measured by manufacturing a specimen according to the ASTM C165 standard.

[0201] The above aerogel composite has a tensile strength of 30 N / cm. 2 Up to 60 N / cm 2 , 40 N / cm 2 Up to 55 N / cm 2 , or 45 N / cm 2 Up to 55 N / cm 2 As such, it may have excellent flexibility. Here, the tensile strength may be measured by manufacturing a specimen according to the ASTM D638 standard.

[0202] The above aerogel composite can generally be formed by a step of preparing a silica sol; a gelation step after impregnating a fiber substrate with the silica sol; and a drying step. Each step is described below. However, the specific manufacturing process or examples described herein are not intended to be limited to any specific type of aerogel or its manufacturing method. The present disclosure may include any aerogel formed by any related manufacturing method known to those skilled in the art.

[0203] Steps for preparing silica sol

[0204] In the present invention, a silica sol can be prepared by mixing a silica precursor composition and a catalyst composition.

[0205] The above silica precursor composition may include water and / or a polar organic solvent in the silica precursor.

[0206] The above silica precursor can be any precursor that can be used to form a silica aerogel without limitation, and may be, for example, a silicon-containing alkoxide compound. Specifically, tetramethyl orthosilicate (TMOS), tetraethyl orthosilicate (TEOS), methyl triethyl orthosilicate, dimethyl diethyl orthosilicate, tetrapropyl orthosilicate, tetraisopropyl orthosilicate, tetrabutyl orthosilicate, tetra secondary butyl orthosilicate, tetra tertiary butyl orthosilicate, tetrahexyl orthosilicate, and tetracyclohexyl orthosilicate. It may be a tetraalkyl silicate such as tetracyclohexyl orthosilicate, tetradodecyl orthosilicate, etc. Among these, more specifically, in the case of the present invention, the silica precursor may be tetramethyl orthosilicate (TMOS), tetraethyl orthosilicate (TEOS), or a mixture thereof.

[0207] Additionally, the silica precursor may be a water glass solution. Here, the water glass solution may refer to a diluted solution obtained by adding distilled water to water glass and mixing it, and the water glass may be sodium silicate (Na2SiO3), which is an alkaline silicic acid salt obtained by melting silicon dioxide (SiO2) and an alkali.

[0208] In addition, the silica precursor may include pre-hydrolyzed TEOS (HTEOS). HTEOS is an ethyl silicate oligomer material having a broad molecular weight distribution. Since the properties such as gelation time can be controlled when synthesizing it in the form of an oligomer from a TEOS monomer, it can be easily applied according to the user's reaction conditions. In addition, it has the advantage of producing reproducible properties of the final product. The HTEOS may be synthesized by a condensation reaction of TEOS that has undergone a partial hydration step under acidic conditions. That is, the HTEOS may be in the form of an oligomer manufactured by condensing TEOS, and the oligomer may be a partially hydrated form.

[0209] The above silica precursor composition may further include a silicate containing a hydrophobic group. The silicate containing the hydrophobic group is not limited in type as long as it is an alkyl silane compound containing an alkyl group that induces hydrophobicity and a silane functional group that can react with the -Si-O- functional group of the wet gel. For example, the silicate containing the hydrophobic group may be at least one selected from the group consisting of methyltriethoxysilane (MTES), trimethylethoxysilane (TMES), trimethylsilanol (TMS), methyltrimethoxysilane (MTMS), dimethyldiethoxysilane (DMDEOS), ethyltriethoxysilane (ETES), and phenyltriethoxysilane (PTES), but is not limited thereto.

[0210] When the silica precursor composition includes a silicate containing the hydrophobic group, it may be included in a molar ratio of 2:98 to 98:2 with the tetraalkyl silicate (molar ratio of the hydrophobic group-containing silicate: tetraalkyl silicate). Within this range, the strength and insulating performance of the aerogel can be efficiently secured, while shrinkage during atmospheric pressure drying can be prevented, thereby preventing a decrease in the insulating performance.

[0211] The silica concentration of the above silica precursor composition is 10 kg / m 3 Up to 100 kg / m 3 , 20 kg / m 3 Up to 80 kg / m 3 , 30 kg / m 3 Up to 70 kg / m 3 , 30 kg / m 3 Up to 60 kg / m 3 , or 35 kg / m 3 Up to 45 kg / m 3 However, the silica concentration may be, but is not limited to, the concentration of silica contained in the silica precursor composition, and may be appropriately adjusted by varying the contents of the silica precursor, organic solvent, and water.

[0212] The above silica precursor may be used in an amount such that the silica content contained in the silica sol is 0.1 wt% to 30 wt%, but is not limited thereto. When the silica content satisfies the above range, it is preferable in terms of securing excellent mechanical properties, particularly flexibility, of the aerogel composite while also having an improved insulating effect.

[0213] The polar organic solvent may include an alcohol, and specific examples thereof include monohydric alcohols such as methanol, ethanol, isopropanol, butanol, etc.; polyhydric alcohols such as glycerol, ethylene glycol, propylene glycol, diethylene glycol, dipropylene glycol, and sorbitol, etc.; or combinations thereof; however, other solvents known to those skilled in the art may also be used without limitation. In the present invention, the polar organic solvent may be, among these, a monohydric alcohol having 1 to 6 carbon atoms such as methanol, ethanol, isopropanol, butanol, etc., for example, ethanol, considering miscibility with water and aerogel.

[0214] The above polar organic solvent can be used in an appropriate amount by a person skilled in the art, taking into account the degree of hydrophobicity in the final aerogel composite to be manufactured while promoting the surface modification reaction.

[0215] In order to prepare a pre-hydrolyzed silica precursor when preparing the above-described silica precursor composition, the silica precursor and the organic solvent may be mixed in a weight ratio of 1:0.1 to 1.5, 1:0.5 to 1.5, or 1:0.5 to 1.2, but the present invention is not limited thereto.

[0216] In addition, in order to prepare a pre-hydrolyzed silica precursor when preparing the silica precursor composition, the silica precursor and water may be mixed in a molar ratio of 1:0.5 to 10, 1:1 to 8, or 1:3 to 6, but the present invention is not limited thereto.

[0217] In addition, when the silica precursor composition is manufactured, if a pre-hydrolyzed silica precursor (e.g., pre-hydrolyzed TEOS) is included as the silica precursor, the pre-hydrolyzed silica precursor (e.g., pre-hydrolyzed TEOS) and the organic solvent may be mixed in a weight ratio of 1:2 to 10, 1:3 to 8, or 1:3 to 6 to satisfy the silica concentration, but the present invention is not limited thereto.

[0218] The above silica precursor composition may further comprise an acid catalyst, and specifically, when an alkoxy silane compound other than a hydrolyzate is used as a precursor, an acid catalyst may be further comprised. At this time, the acid catalyst may be used without limitation as long as it makes the pH 3 or lower, and particularly, the pH approximately 3, and examples thereof include hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, oxalic acid, or acetic acid. At this time, the acid catalyst may be added in an amount such that the pH of the sol becomes 3 or lower, and may be added in the form of an aqueous solution dissolved in an aqueous solvent.

[0219] The above catalyst composition may include an inorganic base such as sodium hydroxide or potassium hydroxide as a base catalyst; or an organic base such as ammonium hydroxide. Specific examples include sodium hydroxide (NaOH), potassium hydroxide (KOH), calcium hydroxide (Ca(OH)2), ammonia (NH3), ammonium hydroxide (NH4OH; ammonia water), tetramethylammonium hydroxide (TMAH), tetraethylammonium hydroxide (TEAH), tetrapropylammonium hydroxide (TPAH), tetrabutylammonium hydroxide (TBAH), methylamine, ethylamine, isopropylamine, monoisopropylamine, diethylamine, diisopropylamine, dibutylamine, trimethylamine, triethylamine, triisopropylamine, tributylamine, choline, monoethanolamine, diethanolamine, 2-aminoethanol, 2-(ethyl amino)ethanol, 2-(methyl amino)ethanol, N-methyl diethanolamine, dimethylaminoethanol, diethylaminoethanol, nitrilotriethanol, It may be, but is not limited to, 2-(2-aminoethoxy)ethanol, 1-amino-2-propanol, triethanolamine, monopropanolamine, dibutanolamine, pyridine, or a combination thereof.

[0220] The above base catalyst may be included in an amount such that the pH of the sol is 5 to 9. If the pH of the sol is outside the above range, gelation may not be easy or the gelation speed may be excessively slow, which may lower the processability. In addition, since the base may precipitate when introduced in a solid state, it may be preferable to add it in the form of a solution diluted with an aqueous solvent or the above organic solvent. In this case, the dilution ratio of the base catalyst and the organic solvent, specifically, alcohol, may be 1:4 to 1:100 by volume, but is not limited thereto.

[0221] The above catalyst composition further includes an alkoxy silane compound having a hydrophobic group, so that the hydrophobic agent and the silica wet gel can react to strengthen the structure and perform surface modification.

[0222] The alkoxy silane compound having the hydrophobic group is not limited in type as long as it includes an alkyl silane compound having an alkyl group that induces hydrophobicity and a silane functional group that can react with the -Si-O- functional group of the wet gel. However, specific examples thereof include at least one selected from the group consisting of trimethylethoxysilane (TMES), trimethylsilanol (TMS), trimethylchlorosilane (TMCS), methyltrimethoxysilane (MTMS), methyltriethoxysilane (MTES), dimethyldiethoxysilane (DMDEOS), ethyltriethoxysilane, and phenyltriethoxysilane, but are not limited thereto.

[0223] The alkoxy silane compound having the hydrophobic group may be included in an amount of 3 to 15 parts by weight, 5 to 10 parts by weight, or 6 to 8 parts by weight based on 100 parts by weight of silica sol, but is not limited thereto.

[0224] However, when the catalyst composition includes an alkoxy silane compound having a hydrophobic group, water may be included to promote the surface modification reaction. The catalyst composition may include 3 to 8 equivalents, 4 to 8 equivalents, or 5 to 6 equivalents of water based on 1 equivalent of the hydrophobic agent.

[0225] In order to prepare the silica sol, the silica precursor composition and the catalyst composition may be mixed in a volume ratio of 1:0.01 to 10.0, 1:0.01 to 5.0, or 1:0.01 to 2.0, but is not limited thereto.

[0226] In the present invention, additives may be added to the silica sol as needed. Any known additives that can be added during the manufacture of aerogels may be used. For example, additives such as opacifiers and flame retardants may be used.

[0227] The above additive may be added in an amount of 0.1 wt% to 10 wt%, 0.1 wt% to 7 wt%, 0.5 wt% to 7 wt%, or 0.5 wt% to 5 wt% relative to the silica content of the aerogel, but is not limited thereto.

[0228] Gelation stage of silica sol

[0229] In the present invention, the silica sol can be gelated after impregnating the substrate with the silica sol.

[0230] The above impregnation process is a process for allowing the catalyzed silica sol to penetrate the internal pores of the substrate, and can be performed by placing the catalyzed silica sol and the substrate into a reaction vessel, or by spraying the catalyzed silica sol onto the substrate moving on a conveyor belt according to a roll-to-roll process. At this time, the substrate can be lightly pressed to ensure sufficient impregnation to improve the bonding between the substrate and the silica sol. Afterwards, the material can be pressed to a certain thickness at a certain pressure to remove excess silica sol, thereby reducing the drying time.

[0231] The temperature of the silica sol in the reaction vessel may be 1 to 40° C., 20 to 40° C., 25 to 40° C., 30 to 40° C., or 35 to 45° C. When the temperature of the silica sol in the reaction vessel satisfies the above range, the aforementioned viscosity range of the catalyzed sol can be more easily achieved, and the desired viscosity range can be satisfied even with a relatively short residence time, which is preferable.

[0232] The above catalyzed silica sol can be impregnated into the substrate at a volume ratio of 0.1 to 10:1 (catalyzed silica sol:substrate), 0.1 to 1:1, 0.3 to 1:1, 0.5 to 1:1, or 0.6 to 1:1, but is not limited thereto.

[0233] The silica sol impregnated into the substrate can be gelled simultaneously with the impregnation process of the above silica sol or sequentially after the impregnation process.

[0234] In the present invention, a substrate impregnated with a catalyzed sol can be gelled on a moving element such as a conveyor belt.

[0235] The above "gelation" may refer to a sol-gel reaction, and the above "sol-gel reaction" may be a network structure formed from a silicon unit precursor material. Here, the network structure may refer to a planar net-shaped structure in which a specific polygon having one or more types of atomic arrangements is connected, or a structure in which a three-dimensional skeletal structure is formed by sharing vertices, edges, faces, etc. of a specific polyhedron.

[0236] The above gelation can be performed under an ambient temperature of 20 to 40°C, 20 to 30°C, 25 to 40°C, 30 to 40°C or 35 to 40°C, and preferably performed under an ambient temperature of 30 to 40°C or 35 to 40°C, which can strengthen the pore structure.

[0237] Additionally, the gelation time may be performed for, but is not limited to, 1 to 120 minutes, 1 to 100 minutes, 1 to 60 minutes, 5 to 60 minutes, 5 to 40 minutes, 10 to 40 minutes, 10 to 30 minutes, or 10 to 20 minutes.

[0238] Maturation stage of the gelled wet gel complex

[0239] The present invention may further include, if necessary, a maturation step in which the wet gel composite obtained through gelation as described above is left at an appropriate temperature to ensure complete chemical change. The maturation step further strengthens the network structure formed through gelation, thereby enhancing the mechanical stability of the aerogel composite.

[0240] The above maturation step can be performed by leaving the gelled wet gel complex at an appropriate temperature as is or by adding a cross-linking promoting compound.

[0241] In addition, in the presence of the wet gel complex during the maturation step, a solution of a base catalyst such as sodium hydroxide (NaOH), potassium hydroxide (KOH), ammonium hydroxide (NH4OH), triethylamine, or pyridine diluted in an organic solvent at a concentration of 1 to 10% may be added. In this case, there is an effect of maximally inducing Si-O-Si bonds within the aerogel, thereby making the network structure of the silica gel more solid, thereby facilitating the maintenance of the pore structure in the subsequent drying process. At this time, the organic solvent may be the aforementioned alcohol, and specifically, may include ethanol.

[0242] The above maturation step can be carried out by leaving the mixture at a temperature of 30°C to 80°C, 40°C to 80°C, or 50°C to 80°C for 0.1 to 20 hours, 0.5 to 15 hours, 0.5 to 10 hours, 0.5 to 7 hours, or 1 to 5 hours to strengthen the pore structure, and within this range, a decrease in productivity can be prevented, while loss of solvent due to evaporation can be prevented, thereby preventing an increase in production costs.

[0243] In addition, the above aging step may be performed firstly by leaving the mixture at 30°C to 80°C for 0.1 to 5 hours to strengthen the pore structure, and then secondly by aging the mixture at 30°C to 80°C for 0.1 to 20 hours, 0.5 to 15 hours, 0.5 to 10 hours, 0.5 to 7 hours, or 1 to 5 hours in the presence of a solution in which a base catalyst is diluted in an organic solvent at a concentration of 1 to 10%.

[0244] In addition, during the maturation step (second maturation when performed in two stages), a mixed solution of an alkoxy silane compound and an alcohol may be added to provide an additional sol precursor source as well as unreacted sol, thereby inducing additional gelation in the silica gel network structure, thereby further strengthening the gel structure. At this time, the alkoxy silane compound may be included in an amount of 0.5 parts by weight to 9.5 parts by weight, 1.0 parts by weight to 9.5 parts by weight, or 1.5 parts by weight to 9.5 parts by weight relative to 100 parts by weight of the total maturation solution.

[0245] The above alkoxy silane compounds include tetramethyl orthosilicate (TMOS), tetraethyl orthosilicate (TEOS), methyl triethyl orthosilicate, dimethyl diethyl orthosilicate, tetrapropyl orthosilicate, tetraisopropyl orthosilicate, tetrabutyl orthosilicate, tetra secondary butyl orthosilicate, tetra tertiary butyl orthosilicate, tetrahexyl orthosilicate, and tetracyclohexyl. It may include at least one selected from the group consisting of tetracyclohexyl orthosilicate, tetradodecyl orthosilicate, methyltrimethoxysilane (MTMS), methyltriethoxysilane (MTES), trimethylethoxysilane (TMES), trimethylsilanol (TMS), trimethylchlorosilane (TMCS), ethyltriethoxysilane (ETES), dimethyldiethoxysilane (DMDEOS), and phenyltriethoxysilane.

[0246] In addition, the alcohol may be a monohydric alcohol such as methanol, ethanol, isopropanol, butanol, etc.; or a polyhydric alcohol such as glycerol, ethylene glycol, propylene glycol, diethylene glycol, dipropylene glycol, and sorbitol, etc.; and preferably a monohydric alcohol having 1 to 6 carbon atoms such as methanol, ethanol, isopropanol, butanol, etc., for example, ethanol, but is not limited thereto.

[0247] The above maturation step may be performed in a separate reaction vessel after recovering the gelled wet gel composite, or may be performed inside the reaction vessel in which the gelling step was performed.

[0248] Surface modification step of the matured wet gel composite

[0249] In the present invention, if necessary, a surface modification step may be further included to hydrophobize the surface of the wet gel composite obtained by gelation as described above or the matured wet gel composite in the presence of a surface modifier.

[0250] The above surface modifier may be applied without limitation to any compound that hydrophobicizes the wet gel surface, and may be, for example, a silane-based compound, a siloxane-based compound, a silanol-based compound, a silazane-based compound, or a combination thereof. Specific examples include silane compounds including trimethylchlorosilane (TMCS), dimethyldimethoxysilane, dimethyl diethoxysilane, methyltrimethoxysilane (MTMS), methyltriethoxysilane (MTES), trimethylethoxysilane (TMES), vinyltrimethoxysilane, ethyltriethoxysilane, phenyltriethoxysilane, phenyltrimethoxysilane, tetraethoxysilane, dimethyldichlorosilane, 3-aminopropyltriethoxysilane, etc.; siloxane compounds including polydimethyl siloxane, polydiethyl siloxane, or octamethyl cyclotetrasiloxane, etc.; Silanol compounds including trimethylsilanol, triethylsilanol, triphenylsilanol, and t-butyldimethylsilanol; Silazane compounds including 1,2-diethyldisilazane, 1,1,2,2-tetramethyldisilazane, 1,1,3,3-tetramethyl disilazane, 1,1,1,2,2,2-hexamethyldisilazane (HMDS), 1,1,2,2-tetraethyldisilazane, or 1,2-diisopropyldisilazane; or a combination thereof, but is not limited thereto.

[0251] The above surface modifier may be used in the form of a solution diluted in an organic solvent. Here, the organic solvent may be alcohol (organic solvent), and the surface modifier may be diluted to 1 to 15% by volume based on the total volume of the diluted solution.

[0252] In addition, the surface modifier may be added in an amount of 0.01 to 90 volume% to the wet gel composite to achieve a sufficient surface modification effect, but is not limited thereto.

[0253] The above surface modification step may be performed at a temperature of 50 to 90°C or 50 to 80°C for 1 to 24 hours, but is not limited thereto.

[0254] Drying stage

[0255] The present invention may include a drying step of drying the surface-modified wet gel composite to obtain an aerogel composite.

[0256] The above drying is performed by a process of removing only the solvent while maintaining the pore structure of the matured gel, and can be performed by, for example, supercritical drying or atmospheric pressure drying.

[0257] The above supercritical drying process is performed using supercritical carbon dioxide. For example, a matured wet gel composite is placed in a supercritical drying reactor, then liquid CO2 is filled, and a solvent substitution process is performed to replace the alcohol solvent inside the wet gel with CO2. Then, the temperature is increased to a temperature of 40 to 70°C at a constant temperature increase rate, for example, 0.1 to 1°C / min, and then a pressure higher than the pressure at which carbon dioxide becomes supercritical, for example, a pressure of 100 to 150 bar, is maintained so that the carbon dioxide can be maintained in the supercritical state for a certain period of time, specifically, 20 minutes to 1 hour. Generally, carbon dioxide becomes supercritical at a temperature of 31°C and a pressure of 73.8 bar. An aerogel composite can be manufactured by maintaining the carbon dioxide at a certain temperature and pressure at which it becomes supercritical for 2 to 12 hours, more specifically, 2 to 6 hours, and then gradually removing the pressure to complete the supercritical drying process, but is not limited thereto.

[0258] In addition, the above atmospheric pressure drying process can be performed according to a conventional method such as hot air drying or IR drying at a temperature of 70 to 200°C and atmospheric pressure (1±0.3 atm), but is not limited thereto.

[0259] In addition to the aforementioned process, the present invention also includes acidification of a basic metal oxide precursor (e.g., sodium silicate) in water to prepare a hydrogel. Salt byproducts can be removed from the silica precursor by ion exchange and / or by subsequent washing of the formed gel with water. Removal of water from the pores of the gel can be accomplished by exchange with a polar organic solvent, such as ethanol, methanol, or acetone. The liquid phase within the gel is then at least partially extracted using innovative processing and extraction techniques.

[0260] In addition to the above-described process, the present invention includes reducing damaging capillary forces at the solvent / pore interface by chemically modifying the matrix material in a wet gel state through conversion of surface hydroxyl groups into hydrophobic trimethylsilyl ether, thereby enabling liquid phase extraction from the gel material at a temperature and pressure below the critical point of the solvent.

[0261] In addition to the aforementioned process, the present invention allows the liquid (solvent) within the gel material to 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, resulting in an aerogel with unique properties.

[0262] The aerogel composite provided by the present invention can be usefully used as an insulating material, heat-insulating material, or fire-retardant material for various industrial facilities, such as pipes or industrial furnaces, as well as for heat-insulating plant facilities, such as aircraft, ships, automobiles, electronic devices, and batteries.

[0263]

[0264] According to another embodiment of the present invention, there is provided an insulating member comprising an aerogel composite provided by the present invention.

[0265] The above insulating member may include the above-described aerogel composite and a support member positioned on at least one of the upper and lower surfaces of the aerogel composite.

[0266] Examples of the above-mentioned support member include a film-like support member, a sheet-like support member, a thin support member, a porous support member, and the like.

[0267] The above film-shaped support member is formed into a thin film from a polymer raw material, and examples thereof include organic films such as PET and polyimide, glass films, etc. (including metal deposition films).

[0268] The above sheet-like support member is formed from a fiber-like raw material of organic, inorganic or metallic origin, and may include paper, non-woven fabric (including glass mat), organic fiber fabric, glass cloth, etc.

[0269] The above-mentioned thin support member is formed by forming a metal raw material into a thin film, and examples thereof include aluminum foil, copper foil, etc.

[0270] The above porous support member has a porous structure made of organic, inorganic or metal raw materials, and examples thereof include porous organic materials (e.g., polyurethane foam), porous inorganic materials (e.g., zeolite sheets), and porous metal materials (e.g., porous metal sheets, porous aluminum sheets).

[0271] The thickness of the above-mentioned support member is not particularly limited and may be, for example, 0.1 to 100 μm, or 1 to 50 μm.

[0272] The above insulating material can also be applied as an insulating material, heat-insulating material, or fire-retardant material in the fields of construction, aviation, automobiles, batteries, home appliances, semiconductors, and industrial equipment.

[0273]

[0274] Hereinafter, the present invention will be described in detail with reference to the following examples. However, the following examples are merely illustrative of the present invention, and the content of the present invention is not limited to the following examples.

[0275]

[0276] Example

[0277]

[0278] [Example 1]

[0279] A silica precursor solution was prepared by mixing tetraethyl orthosilicate (TEOS) and water in a molar ratio of 1:6 and adding ethanol in a weight ratio of 1:1 to TEOS. To promote hydrolysis of the silica precursor solution, an aqueous HCl solution was added such that the pH of the silica precursor solution became approximately 3, and the mixture was stirred for more than 2 hours to prepare a hydrated TEOS solution. A silica sol was prepared by adding ethanol in a weight ratio of 1:4 to the hydrated TEOS solution. A catalyzed sol was prepared by adding a base catalyst solution (5 wt% NaOH aqueous solution) in a volume ratio of 99:1 to the silica sol. After filling 33.3 L of the catalyzed sol into an impregnation tank, a fiber (glass fiber mat, 5 mm) was passed through the substrate to infiltrate the fiber with the catalyzed sol, such that the catalyzed silica sol was impregnated into the fiber mat in a volume ratio of 0.6:1 (catalyzed silica sol: fiber). The fibers, which had been impregnated with the catalyzed sol after passing through the impregnation tank, were gelled for 10 minutes while passing at a constant speed on a conveyor belt. At this time, the ambient temperature on the conveyor belt was maintained at 35℃. Thereafter, a solution of 2.9 wt% methyltriethoxysilane (MTES) diluted in ethanol with a moisture content of 10 wt% was added as a maturing solution in an amount of 109 vol% based on the volume of the wet gel composite, and maturing was performed at a temperature of 75℃ for 1 hour. A hexamethyldisilazane (HMDS) / ethanol solution (5:95 volume ratio) was added as a surface modifier in an amount of 90 vol% based on the volume of the wet gel composite to the maturing wet gel composite, and surface modification was performed at a temperature of 75℃ for 4 hours. Afterwards, the silica wet gel was placed in a 7.2 L supercritical extractor and CO2 was injected. Afterwards, the temperature inside the extractor was increased to 70°C over 1 hour and 20 minutes, and when it reached 70°C and 150 bar, CO2 was injected and discharged at a rate of 0.5 L / min for 20 minutes, and the CO2 injection was stopped for 20 minutes. This process was repeated 4 times.Ethanol was recovered through the bottom of the separator during CO2 injection and discharge. CO2 was then vented over a period of two hours to produce a hydrophobic silica aerogel composite.

[0280]

[0281] [Example 2]

[0282] A silica precursor solution was prepared by mixing tetraethyl orthosilicate (TEOS) and water in a molar ratio of 1:6 and adding ethanol in a weight ratio of 1:1 to TEOS. To promote hydrolysis of the silica precursor solution, an aqueous HCl solution was added such that the pH of the silica precursor solution became approximately 3, and the mixture was stirred for more than 2 hours to prepare a hydrated TEOS solution. A silica sol was prepared by adding ethanol in a weight ratio of 1:3 to the hydrated TEOS solution. A catalyzed sol was prepared by adding a base catalyst solution (5 wt% NaOH aqueous solution) in a volume ratio of 99:1 to the silica sol. After filling 33.3 L of the catalyzed sol into an impregnation tank, a fiber (glass fiber mat, 5 mm) was passed through the substrate to infiltrate the fiber with the catalyzed sol, such that the catalyzed silica sol was impregnated into the fiber mat in a volume ratio of 0.6:1 (catalyzed silica sol: fiber). The fibers, which had been impregnated with the catalyzed sol after passing through the impregnation tank, were gelled for 10 minutes while passing at a constant speed on a conveyor belt. At this time, the ambient temperature on the conveyor belt was maintained at 35℃. Thereafter, a solution of 2.9 wt% methyltriethoxysilane (MTES) diluted in ethanol with a moisture content of 10 wt% was added as a maturing solution in an amount of 109 vol% based on the volume of the wet gel composite, and maturing was performed at a temperature of 75℃ for 1 hour. A solution of 2 vol% trimethylethoxysilane (TMES) diluted in ethanol as a surface modifier was added in an amount of 90 vol% based on the volume of the wet gel composite, and surface modification was performed at a temperature of 75℃ for 12 hours. Afterwards, the silica wet gel was placed in a 7.2 L supercritical extractor and CO2 was injected. Afterwards, the temperature inside the extractor was increased to 70 ℃ over 1 hour and 20 minutes, and when it reached 70 ℃ and 150 bar, it was cooled to 0 for 20 minutes.The process of injecting and discharging CO2 at a rate of 5 L / min and maintaining the CO2 injection at a standstill for 20 minutes was repeated four times. Ethanol was recovered through the bottom of the separator during CO2 injection and discharging. Afterwards, CO2 was vented over a period of 2 hours to produce a hydrophobic silica aerogel composite.

[0283]

[0284] [Example 3]

[0285] A silica precursor solution was prepared by mixing tetraethyl orthosilicate (TEOS) and water in a molar ratio of 1:5 and adding ethanol in a weight ratio of 1:1 to TEOS. To promote hydrolysis of the silica precursor solution, an HCl aqueous solution was added such that the pH of the silica precursor solution became approximately 3, and the mixture was stirred for more than 2 hours to prepare a hydrated TEOS solution. A silica sol was prepared by adding the hydrated TEOS solution and ethanol in a weight ratio of 1:5. A catalyzed sol was prepared by adding the silica sol and a base catalyst solution (5 wt% NaOH aqueous solution) in a volume ratio of 99:1. After filling 33.3 L of the catalyzed sol into an impregnation tank, a fiber (Glass fiber mat, 10 mm) was passed through the substrate to infiltrate the fiber with the catalyzed sol, such that the catalyzed silica sol was impregnated into the fiber mat in a volume ratio of 1:1 (catalyzed silica sol: fiber). The fibers, which had been impregnated with the catalyzed sol after passing through the impregnation tank, were gelled for 10 minutes while passing at a constant speed on a conveyor belt. At this time, the ambient temperature on the conveyor belt was maintained at 40℃. Thereafter, a solution of 2.9 wt% methyltriethoxysilane (MTES) diluted in ethanol with a moisture content of 10 wt% was added as a maturing solution in an amount of 109 vol% based on the volume of the wet gel composite, and maturing was performed at a temperature of 75℃ for 1 hour. A hexamethyldisilazane (HMDS) / ethanol solution (5:95 volume ratio) was added as a surface modifier in an amount of 90 vol% based on the volume of the wet gel composite to the maturing wet gel composite, and surface modification was performed at a temperature of 75℃ for 4 hours. Afterwards, the silica wet gel was placed in a 7.2 L supercritical extractor and CO2 was injected. Afterwards, the temperature inside the extractor was increased to 70°C over 1 hour and 20 minutes, and when it reached 70°C and 150 bar, CO2 was injected and discharged at a rate of 0.5 L / min for 20 minutes, and the CO2 injection was stopped for 20 minutes. This process was repeated 4 times.Ethanol was recovered through the bottom of the separator during CO2 injection and discharge. CO2 was then vented over a period of two hours to produce a hydrophobic silica aerogel composite.

[0286]

[0287] [Example 4]

[0288] A silica precursor solution was prepared by mixing tetraethyl orthosilicate (TEOS) and water in a molar ratio of 1:6 and adding ethanol in a weight ratio of 1:1 to TEOS. To promote hydrolysis of the silica precursor solution, an aqueous HCl solution was added such that the pH of the silica precursor solution became approximately 3, and the mixture was stirred for more than 2 hours to prepare a hydrated TEOS solution. A silica sol was prepared by adding ethanol in a weight ratio of 1:3 to the hydrated TEOS solution. A catalyzed sol was prepared by adding a base catalyst solution (5 wt% NaOH aqueous solution) in a volume ratio of 99:1 to the silica sol. After filling 33.3 L of the catalyzed sol into an impregnation tank, a fiber (glass fiber mat, 10 mm) was passed through the substrate to infiltrate the fiber with the catalyzed sol, such that the catalyzed silica sol was impregnated into the fiber mat in a volume ratio of 1:1 (catalyzed silica sol: fiber). The fibers, which had been impregnated with the catalyzed sol after passing through the impregnation tank, were gelled for 10 minutes while passing at a constant speed on a conveyor belt. At this time, the ambient temperature on the conveyor belt was maintained at 40℃. Thereafter, a solution of 2.9 wt% methyltriethoxysilane (MTES) diluted in ethanol with a moisture content of 10 wt% was added as a maturing solution in an amount of 109 vol% based on the volume of the wet gel composite, and maturing was performed at a temperature of 75℃ for 1 hour. A solution of 2 vol% trimethylethoxysilane (TMES) diluted in ethanol as a surface modifier was added in an amount of 90 vol% based on the volume of the wet gel composite, and surface modification was performed at a temperature of 75℃ for 12 hours. Afterwards, the silica wet gel was placed in a 7.2 L supercritical extractor and CO2 was injected. Afterwards, the temperature inside the extractor was increased to 70 ℃ over 1 hour and 20 minutes, and when it reached 70 ℃ and 150 bar, it was cooled to 0 for 20 minutes.The process of injecting and discharging CO2 at a rate of 5 L / min and maintaining the CO2 injection at a standstill for 20 minutes was repeated four times. Ethanol was recovered through the bottom of the separator during CO2 injection and discharging. Afterwards, CO2 was vented over a period of 2 hours to produce a hydrophobic silica aerogel composite.

[0289]

[0290] [Example 5]

[0291] A silica precursor solution was prepared by mixing tetraethyl orthosilicate (TEOS) and water in a molar ratio of 1:6 and adding ethanol in a weight ratio of 1:1 to TEOS. To promote hydrolysis of the silica precursor solution, an aqueous HCl solution was added such that the pH of the silica precursor solution became approximately 3, and the mixture was stirred for more than 2 hours to prepare a hydrated TEOS solution. A silica sol was prepared by adding ethanol in a weight ratio of 1:3 to the hydrated TEOS solution. A catalyzed sol was prepared by adding a base catalyst solution (5 wt% NaOH aqueous solution) in a volume ratio of 99:1 to the silica sol. After filling 33.3 L of the catalyzed sol into an impregnation tank, a fiber (glass fiber mat, 5 mm) was passed through the substrate to infiltrate the fiber with the catalyzed sol, such that the catalyzed silica sol was impregnated into the fiber mat in a volume ratio of 0.6:1 (catalyzed silica sol: fiber). Fibers impregnated with the catalyzed sol through the impregnation tank were passed at a constant speed over a conveyor belt and gelled for 10 minutes. During this time, the ambient temperature over the conveyor belt was maintained at 35°C. After gelation, it was stabilized at room temperature (25 ℃) for 10 minutes, and then primary maturation was performed in a 70 ℃ oven for 50 minutes. Afterwards, a solution of 2.9 wt% methyltriethoxysilane (MTES) diluted in ethanol with a moisture content of 10 wt% was prepared for the gelled wet gel composite, and 109% of the wet gel composite volume was added thereto, and secondary maturation was performed in a 75 ℃ oven for 1 hour. A solution (2 vol.%) of trimethylethoxysilane (TMES) diluted in ethanol as a surface modifier was added thereto, and 90 vol.% of the wet gel composite volume was added thereto, and surface modification was performed at a temperature of 75 ℃ for 6 hours. Afterwards, the silica wet gel was placed in a 7.2 L supercritical extractor and CO2 was injected. Afterwards, the temperature inside the extractor was raised to 70 ℃ over 1 hour and 20 minutes. 0 for 20 minutes when reaching 70 ℃, 150 bar.The process of injecting and discharging CO2 at a rate of 5 L / min and maintaining the CO2 injection at a standstill for 20 minutes was repeated four times. Ethanol was recovered through the bottom of the separator during CO2 injection and discharging. Afterwards, CO2 was vented over a period of 2 hours to produce a hydrophobic silica aerogel composite.

[0292]

[0293] [Comparative Example 1]

[0294] A silica precursor solution was prepared by mixing tetraethyl orthosilicate (TEOS) and water in a molar ratio of 1:4 and adding ethanol in a weight ratio of 1:1 to TEOS. To promote hydrolysis of the silica precursor solution, an HCl aqueous solution was added so that the pH of the silica precursor solution became approximately 2, and the solution was stirred for more than 2 hours to prepare a hydrated TEOS solution. A silica sol was prepared by adding ethanol in a weight ratio of 1:3 to the hydrated TEOS solution. A catalyzed sol was prepared by mixing the silica sol and ammonia water (30 wt%) in a volume ratio of 99.5:0.5. After filling 33.3 L of the catalyzed sol into an impregnation tank, a fiber (Glass fiber mat, 10 mm) was passed through the substrate to infiltrate the fiber with the catalyzed sol, such that the catalyzed silica sol was impregnated into the fiber mat in a volume ratio of 1:1 (catalyzed silica sol: fiber). The fibers, which had been impregnated with the catalyzed sol after passing through the impregnation tank, were gelled for 10 minutes while passing at a constant speed on a conveyor belt. At this time, the ambient temperature on the conveyor belt was maintained at 30°C. Thereafter, the gelled wet gel composite was left to mature at 25°C for 24 hours. To the matured wet gel composite, a surface modifier, hexamethyldisilazane (HMDS) / ethanol solution (5:95 volume ratio), was added in an amount of 90% by volume based on the volume of the wet gel composite, and the surface was modified at a temperature of 75°C for 4 hours. Afterwards, the silica wet gel was placed in a 7.2 L supercritical extractor and CO2 was injected. Afterwards, the temperature inside the extractor was increased to 70 ℃ over 1 hour and 20 minutes, and when 70 ℃ and 150 bar were reached, CO2 was injected and discharged at a rate of 0.5 L / min for 20 minutes, and the CO2 injection was stopped for 20 minutes. This process was repeated 4 times. Ethanol was recovered through the bottom of the separator during the CO2 injection and discharge. Thereafter, CO2 was vented over 2 hours to produce a hydrophobic silica aerogel composite.

[0295]

[0296] [Comparative Example 2]

[0297] A silica precursor solution was prepared by mixing tetraethyl orthosilicate (TEOS) and water in a molar ratio of 1:5 and adding ethanol in a weight ratio of 1:1 to TEOS. To promote hydrolysis of the silica precursor solution, an aqueous HCl solution was added so that the pH of the silica precursor solution became approximately 2, and the solution was stirred for more than 2 hours to prepare a hydrated TEOS solution. A silica sol was prepared by adding ethanol in a weight ratio of 1:3 to the hydrated TEOS solution. A catalyzed sol was prepared by mixing the silica sol and ammonia water (30 wt%) in a volume ratio of 99.5:0.5. After filling 33.3 L of the catalyzed sol into an impregnation tank, a fiber (glass fiber mat, 10 mm) was passed through the substrate to infiltrate the fiber with the catalyzed sol, such that the catalyzed silica sol was impregnated into the fiber mat in a volume ratio of 0.4:1 (catalyzed silica sol: fiber). The fibers, which had been impregnated with the catalyzed sol after passing through the impregnation tank, were gelled for 10 minutes while passing at a constant speed on a conveyor belt. At this time, the ambient temperature on the conveyor belt was maintained at 25℃. Thereafter, a solution of 2.9 wt% methyltriethoxysilane (MTES) diluted in ethanol with a moisture content of 10 wt% was added as a maturing solution in an amount of 109 vol% based on the volume of the wet gel composite, and maturing was performed at a temperature of 75℃ for 1 hour. A hexamethyldisilazane (HMDS) / ethanol solution (5:95 volume ratio) was added as a surface modifier in an amount of 90 vol% based on the volume of the wet gel composite to the maturing wet gel composite, and surface modification was performed at a temperature of 75℃ for 4 hours. Afterwards, the silica wet gel was placed in a 7.2 L supercritical extractor and CO2 was injected. Afterwards, the temperature inside the extractor was increased to 70°C over 1 hour and 20 minutes, and when it reached 70°C and 150 bar, CO2 was injected and discharged at a rate of 0.5 L / min for 20 minutes, and the CO2 injection was stopped for 20 minutes. This process was repeated 4 times.Ethanol was recovered through the bottom of the separator during CO2 injection and discharge. CO2 was then vented over a period of two hours to produce a hydrophobic silica aerogel composite.

[0298]

[0299] [Comparative Example 3]

[0300] A silica precursor solution was prepared by mixing tetraethyl orthosilicate (TEOS) and water in a molar ratio of 1:3 and adding ethanol having a weight ratio of 1:1 to TEOS. To promote hydrolysis of the silica precursor solution, acid was added so that the pH of the silica precursor solution became approximately 3, and the mixture was stirred for more than 2 hours to prepare a hydrated TEOS solution. A silica sol was prepared by adding ethanol having a weight ratio of 1:6 to the hydrated TEOS solution. A catalyzed sol was prepared by adding a base catalyst solution (5 wt% NaOH aqueous solution) having a volume ratio of 99:1 to the silica sol. The catalyzed sol was impregnated into a fiber (glass fiber mat, 5 mm) as a substrate by passing the fiber through the fiber, and the catalyzed silica sol was impregnated in a volume ratio of 0.6:1 (catalyzed silica sol: glass fiber mat) to the volume of the glass fiber mat, and gelled after 10 minutes to prepare a wet gel composite. The fibers, which had been impregnated with the catalyzed sol after passing through the impregnation tank, were gelled for 10 minutes while passing at a constant speed on a conveyor belt. At this time, the ambient temperature on the conveyor belt was maintained at 25℃. Thereafter, a solution of 2.9 wt% methyltriethoxysilane (MTES) diluted in ethanol with a moisture content of 10 wt% was added as a maturing solution in an amount of 109 vol% based on the volume of the wet gel composite, and maturing was performed at a temperature of 75℃ for 1 hour. A hexamethyldisilazane (HMDS) / ethanol solution (5:95 volume ratio) was added as a surface modifier in an amount of 90 vol% based on the volume of the wet gel composite to the maturing wet gel composite, and surface modification was performed at a temperature of 75℃ for 4 hours. Afterwards, the silica wet gel was placed in a 7.2 L supercritical extractor and CO2 was injected. Afterwards, the temperature inside the extractor was increased to 70°C over 1 hour and 20 minutes, and when it reached 70°C and 150 bar, CO2 was injected and discharged at a rate of 0.5 L / min for 20 minutes, and the CO2 injection was stopped for 20 minutes. This process was repeated 4 times.Ethanol was recovered through the bottom of the separator during CO2 injection and discharge. CO2 was then vented over a period of two hours to produce a hydrophobic silica aerogel composite.

[0301]

[0302] [Experimental Example 1] Measurement of distribution by density and pore size

[0303] 1. Density

[0304] For each silica aerogel composite manufactured in each example and comparative example, five specimens measuring 10 cm X 10 cm were prepared, and their weights were measured, and the thicknesses of the specimens were measured using NETZSCH's HFM436 equipment. The density was calculated using the measured weight, thickness, and size, and the average density of the five specimens was determined as the final density, and the results are shown in Table 1 below.

[0305] 2. Volume ratio (%) of effective pores with a pore diameter of 30 nm or less

[0306] For each silica aerogel composite manufactured in each example and comparative example, partial pressure (0.11) was measured using ASAP 2010 equipment from Micrometrics Co. <p / p0<1)에 따른 질소의 흡 / 탈착량으로 분석하여, 비표면적, 기공 부피 및 기공 직경을 측정하였다. 측정된 기공 부피에서 기공 직경이 30 nm 이하의 수치범위를 갖는 기공(유효 기공)의 부피 비율을 산출하여 그 결과를 하기 표 1에 나타내었다.

[0307] Density (g / cc) Effective pore volume ratio (%) Example 10.17733.5 Example 20.18532.8 Example 30.18939.2 Example 40.19830.1 Example 50.18833.2 Comparative Example 10.19122.1 Comparative Example 20.16221.5 Comparative Example 30.16924.5

[0308]

[0309] [Experimental Example 2] SAXS Analysis of Aerogel Particles

[0310] In order to perform small-angle X-ray diffraction (SAXS) analysis on the aerogel particles included in the aerogel composites obtained in Examples 1 to 5 and Comparative Examples 1 to 3, first, the aerogel composites of Examples 1 to 5 and Comparative Examples 1 to 3, which were manufactured to a size of 60 cm X 12 cm (width X length), were prepared. Each aerogel composite was placed in a sealable vinyl container and then repeatedly shaken up and down to intentionally induce the detachment of the aerogel powder (aerogel particles). The fibrous substrate mixed in the obtained aerogel powder and identifiable with the naked eye was removed using tweezers. Thereafter, in order to further remove the fibrous substrate finely mixed in the detached powder for more precise analysis, the aerogel powder was placed in a 100 ml vial, distilled water was added so that the weight ratio of powder:distilled water was approximately 1:130, and the vial was shaken vigorously up and down 50 times. Afterwards, the fiber substrate that had settled to the bottom layer of the vial was removed, and the lumps formed by the fiber substrate and aerogel powder agglomeration were also removed. Only the aerogel powder that did not form agglomerates was carefully obtained and dried at 120 ° C. The small-angle X-ray scattering (SAXS) analysis below was performed by taking 10 mg of the final obtained aerogel powder. The aerogel powder sample was placed at a distance of about 2.5 m from the detector using Xeuss 2.0 X-ray scattering equipment from Xenocs, and X-rays were incident on the detector to measure the results. Pilatus3 300K (2D detector) was used as the detector. Then, the scattered 2D diffraction pattern was obtained as an image, and this was calibrated using the sample-to-detector distance obtained through the standard sample, and the scattering intensity (I(q)) according to the scattering wavenumber (Q) was converted through the circular average, and a graph was obtained that displayed the scattering intensity logarithmically against the scattering wavenumber (Q).In the small-angle X-ray diffraction (SAXS) graphs obtained for the aerogel powders of Examples 1 to 5 and Comparative Examples 1 to 3, linear regression was obtained by considering all measured values ​​(q, Intensity I(q)) in the wave number range of 0.015 / Å to 0.035 / Å according to the least square method, and then the slope obtained by calculating the change in scattering intensity according to the change in wave number of 0.015 / Å to 0.035 / Å is shown in Table 2. Among these, the small-angle X-ray diffraction (SAXS) graphs obtained for the aerogel powders of Examples 1 and 3 and Comparative Examples 1 and 2 are shown in FIGS. 1 and 2. However, in order to confirm whether it is possible to analyze aerogel particles located within a fiber substrate by performing small-angle X-ray diffraction (SAXS) on an aerogel composite rather than on detached aerogel powder, a square specimen measuring 1 cm X 1 cm was obtained from the center of the aerogel composite of Example 1, and the graph obtained by performing small-angle X-ray diffraction (SAXS) analysis using the same method is shown in Fig. 1.

[0311] SAXS graph slope Example 1 - 2.22 Example 2 - 2.37 Example 3 - 2.46 Example 4 - 2.58 Example 5 - 2.32 Comparative Example 1 - 1.88 Comparative Example 2 - 2.07 Comparative Example 3 - 2.12

[0312] As shown in Table 2 above and FIGS. 1 and 2, it was confirmed that the aerogel powders derived from the aerogel composites of Examples 1 to 5 according to the present invention had slopes measured in the wavenumber range of 0.015 / Å to 0.035 / Å in the small-angle X-ray scattering (SAXS) graph, which fell within the range of -2.80 to -2.20. Through this, it was found that the aerogel powders of Examples 1 to 5 according to the present invention contained a high proportion of secondary aerogel particles having an oblate disk-shaped structure in the center, whereas the aerogel powders of Comparative Examples 1 to 3 contained a high proportion of secondary aerogel particles having a disk shape closer to a two-dimensional shape (i.e., a disk shape with a flat center). In addition, as shown in Fig. 1, the slope of the small-angle X-ray scattering (SAXS) graph for the aerogel powder of Example 1 was -2.22, and the slope of the small-angle X-ray scattering (SAXS) graph for the aerogel composite specimen of Example 1 was measured to be -2.25 for the same wavenumber range, indicating that information on the shape of the aerogel particles included in the aerogel composite itself can be obtained through small-angle X-ray scattering (SAXS) analysis.

[0313]

[0314] [Experimental Example 3] Measurement of recovery rate and thermal transmittance after compression of aerogel composites

[0315] The aerogel composites obtained in Examples 1 to 5 and Comparative Examples 1 to 3 were manufactured in a rectangular shape with a size of 60 cm X 12 cm (width X length). However, in the following experiments, considering the specifications of the measuring equipment, each aerogel composite was cut at half the width to obtain two specimens with a size of 30 cm X 12 cm, and these were then arranged in parallel adjacent to each other to rearrange the specimens to have a size of 30 cm X 24 cm, and then analysis was performed on these specimens.

[0316] 1. Compression recovery rate

[0317] As described above, the aerogel composite specimens obtained in Examples 1 to 5 and Comparative Examples 1 to 3 were pressed for 10 minutes under each pressure condition using the QM900A-15T press equipment of QMESYS Co., Ltd. Before pressing and 1 hour after the end of pressing, the thickness of the aerogel composite was measured using the HFM436 equipment of Netzsch Co., Ltd., and the compression recovery rate was calculated according to Equation 2 below, and the results are shown in Table 3 below. However, the pressure value shown in Table 3 below means the value of the pressure applied per unit area of ​​the specimen, and means the value obtained by dividing by the area of ​​the specimen obtained by multiplying the cylinder area of ​​the press equipment by the set pressure value as in Equation 3 below. The cylinder radius of the QM900A-15T press equipment used in this experiment is 6.25 cm, and the cylinder size is 12.5 cm.

[0318] [Formula 2]

[0319] Compression recovery rate (%) = {(cross-sectional thickness of aerogel composite after compression) / (cross-sectional thickness of aerogel composite before compression)} X 100

[0320] [Formula 3]

[0321] Actual pressure value = (Inner cylinder radius of press equipment (cm) X Inner cylinder radius of press equipment (cm) X 3.14 X Set pressure value) / (Area of ​​specimen (cm) 2 ))

[0322] 2. Thermal transmittance

[0323] After conducting an experiment using the same method as in 1 above, the thermal conductivity of the aerogel composite was measured using Netzsch HFM436 equipment before compression and after 1 hour had passed after the end of compression, and the thermal transmittance was calculated, and the increase rate of the thermal transmittance compared to before compression was evaluated, and the results are shown in Table 4 below.

[0324] In addition, in order to confirm the change in thermal transmittance before and after compression, the average value (b) of the thermal transmittance measured after compression at pressures of no compression (0 bar), 3 bar, 9 bar and 24 bar was calculated, and as in Equation 4 below, the difference between the thermal transmittance (a) measured after compression at pressures of 0 bar, 3 bar, 9 bar and 24 bar and the average value (b) of these thermal transmittances, and the value A obtained by dividing the difference by the average value (b) of the thermal transmittances were calculated, and the results are shown in Table 5.

[0325] [Formula 4]

[0326] {(Thermal transmittance before and after compression (a)) - (Average of thermal transmittances before and after compression (b))} = (Average of thermal transmittances before and after compression (b)) XA

[0327] In addition, in order to confirm the change in thermal transmittance after compression, the average value (d) of the thermal transmittance measured after compression at pressures of 3 bar, 9 bar and 24 bar was calculated, and as in Equation 5 below, the difference between the thermal transmittance (c) measured after compression at pressures of 3 bar, 9 bar or 24 bar and the average value (d), and the value B obtained by dividing the difference by the average value (d) of the thermal transmittance were calculated, and the results are shown in Table 6.

[0328] [Formula 5]

[0329] (Thermal transmittance after compression (c) - Average value of thermal transmittance after compression (d)) = (Average value of thermal transmittance after compression (d)) XB

[0330] Each result value shown in Tables 3 to 6 below is rounded to the third decimal place and displayed to the second decimal place.

[0331] Classification Pressure Conditions Thickness after compression (mm) Compression recovery rate (%) Example 1 - 3.6 100.003 bar 10 min 3.49 4.449 bar 10 min 38 3.33 24 bar 10 min 2.67 2.22 Example 2 - 3.7 100.003 bar 10 min 3.59 4.599 bar 10 min 3.28 6.49 24 bar 10 min 2.87 5.68 Example 3 - 10.2 100.003 bar 10 min 8.98 7.259 bar 10 min 8.17 9.41 24 bar 10 min 7.97 7.45 Example 4 - 9.8 100.003 bar 10 min 8.78 8.789 bar 10 min 88 1.63 24 bar 10min7.879.59Example 5-3.7100.003bar 10min3.697.309bar 10min3.389.1924bar 10min2.978.38Comparative Example 1-9.1100.003bar 10min7.279.129bar 10min5.156.0424bar 10min4.852.75Comparative Example 2-5.5100.003bar 10min4.683.649bar 10min3.970.9124bar 10min2.545.45Comparative Example 3-3.9100.003bar 10min3.282.059bar 10min2.564.1024bar 10min251.28

[0332] Thermal transmittance under pressure conditions (W / m) 2K) Increase rate of heat transfer coefficient (times)Example 1 - 6.89 - 3 bar 10 min 7.03 1.029 bar 10 min 7.87 1.14 24 bar 10 min 9.04 1.31Example 2 - 5.00 - 3 bar 10 min 5.46 1.099 bar 10 min 6.3 11.26 24 bar 10 min 8.14 1.63Example 3 - 2.26 - 3 bar 10 min 2.62 1.169 bar 10 min 2.9 11.29 24 bar 10 min 3.10 1.37Example 4 - 1.58 - 3 bar 10 min 1.87 1.189 bar 10 min 2.23 1.41 24 bar 10 min 2.36 1.49Example 5 - 4.84 - 3 bar 10min5.031.049bar 10min5.611.1624bar 10min6.621.37Comparative example 1-1.85-3bar 10min2.571.399bar 10min4.692.5424bar 10min5.883.18Comparative example 2-3.60-3bar 10min4.981.389bar 10min6.281.7424bar 10min10.482.91Comparative example 3-6.44-3bar 10min8.721.359bar 10min13.122.0424bar 10min18.402.86

[0333] Thermal transmittance (a) before and after compression (W / m) 2 K) Average values ​​of thermal transmittances before and after compression (b) (W / m 2 K) Deviation of thermal transmittance before and after compression (ab) (W / m 2K) Deviation of heat transmittance before and after compression / Average of heat transmittance (ab / b = A)Example 10 bar, 10 min 6.89 7.71-0.82-0.113 bar, 10 min 7.03-0.68-0.099 bar, 10 min 7.87 0.16 0.02 24 bar, 10 min 9.04 1.33 0.17Example 20 bar, 10 min 5.00 6.23-1.23-0.203 bar, 10 min 5.46-0.77-0.129 bar, 10 min 6.31 0.08 0.01 24 bar, 10 min 8.14 1.9 10.31Example 30 bar, 10 min 2.26 2.72-0.46-0.173 bar, 10min2.62-0.10-0.049bar, 10min2.910.190.0724bar, 10min3.100.380.14Example 40bar, 10min1.582.01-0.43-0.213bar, 10min1.87-0.14-0.079bar, 10min2.230.220.1124bar, 10min2.360.350.17Example 50bar, 10min4.845.53-0.69-0.123bar, 10min5.03-0.5-0.099bar, 10min5.610.080.0124bar, 10min6.621.090.20Comparative Example 10bar, 10min1.853.75-1.9-0.513bar, 10min2.57-1.18-0.319bar, 10min4.690.940.2524bar, 10min5.882.130.57Comparative example 20bar, 10min3.606.34-2.74-0.433bar, 10min4.98-1.36-0.219bar, 10min6.28-0.06-0.0124bar, 10min10.484.140.65Comparative example 30bar, 10min6.4411.67-5.23-0.453bar, 10min8.72-2.95-0.259bar, 10min13.121.450.1224bar, 10min18.406.730.58

[0334] Thermal transmittance (c) after compression under pressure conditions (W / m) 2 K) Average thermal transmittance after compression (d) (W / m 2K) Deviation of thermal transmittances after compression (cd) (W / m 2 K) Deviation of heat transmittance after compression / Average of heat transmittance (cd / d = B)Example 13 bar, 10 min 7.03 7.98-0.95-0.129 bar, 10 min 7.87-0.11-0.01 24 bar, 10 min 9.04 1.06 0.13Example 23 bar, 10 min 5.46 6.64-1.18-0.18 9 bar, 10 min 6.31-0.33-0.05 24 bar, 10 min 8.14 1.50 0.23Example 33 bar, 10 min 2.62 2.88-0.26-0.099 bar, 10 min 2.91 0.03 0.01 24 bar, 10 min 3.10 0.22 0.08Example 43 bar, 10 min 1.87 2.15-0.28-0.139 bar, 10 min 2.23 0.08 0.03 24 bar, 10 min 2.36 0.21 0.10 Example 53 bar, 10 min 5.03 5.75-0.72-0.139 bar, 10 min 5.61-0.14-0.03 24 bar, 10 min 6.62 0.87 0.15 Comparative example 13 bar, 10 min 2.57 4.38-1.81-0.419 bar, 10 min 4.69 0.31 0.07 24 bar, 10 min 5.88 1.50 0.34 Comparative example 23 bar, 10 min 4.98 7.25-2.27-0.319 bar, 10min6.28-0.97-0.1324bar, 10min10.483.230.45Comparative example 33bar, 10min8.7213.41-4.69-0.359bar, 10min13.12-0.29-0.0224bar, 10min18.404.990.37

[0335] As shown in Tables 4 to 6 above, it was confirmed that the aerogel composites of Examples 1 to 5 manufactured according to the present invention had higher compression recovery rates than the aerogel composites of Comparative Examples 1 to 3, and even after compression, the degree of increase in the thermal transmittance of the aerogel composite was small compared to before compression, and it was confirmed that the degree of change in the thermal transmittance was small and the insulation performance was maintained at an excellent level even when compressed at various pressure values ​​from low pressure to high pressure. From these results, it was confirmed that the aerogel composite of the present invention has both excellent elastic flexibility and strength of the pores, so that it has excellent recovery power even after high-pressure compression, and accordingly, a rapid decrease in insulation performance due to destruction of the pores, especially destruction of pores with a size of 30 nm or less, is prevented, and excellent insulation performance is maintained even after compression.

[0336]

[0337] While specific aspects of the present invention have been described in detail above, it should be apparent to those skilled in the art that these specific descriptions are merely preferred implementation examples and do not limit the scope of the present invention. Therefore, the substantial scope of the present invention is defined by the appended claims and their equivalents.

[0338] The present invention relates to an aerogel composite that maintains excellent thermal insulation properties without significant degradation even when compressed by external pressure for various reasons, and to its application as an insulating material. The insulating material can also be applied to batteries, electronic devices, automobiles, industrial equipment, or structures.

Claims

1. An aerogel composite comprising a fiber substrate and an aerogel having a plurality of open pores, wherein the aerogel comprises a plurality of silica aerogel particles; An aerogel composite, wherein in a small angle X-ray scattering (SAXS) graph in which the scattering intensity versus wave number is expressed logarithmically for the silica aerogel particles, the slope in the wave number range of 0.015 / Å to 0.035 / Å is -2.80 to -2.

20.

2. In paragraph 1, The above-mentioned incineration X-ray scattering graph is for silica aerogel particles detached from the aerogel composite, an aerogel composite.

3. In paragraph 1, The above-mentioned small-angle X-ray scattering graph is for silica aerogel particles within the aerogel composite.

4. In paragraph 1, An aerogel composite, wherein when compressed by applying a pressure of 3 bar, 9 bar, and 24 bar in the horizontal direction (transverse direction) to the cross-section of the above aerogel composite, the thermal transmittance after compression is 1.8 times or less compared to the thermal transmittance before compression.

5. In paragraph 1, An aerogel composite, wherein when compressed by applying a pressure of 3 bar, 9 bar, and 24 bar in the horizontal direction (transverse direction) to the cross-section of the above aerogel composite, the thermal transmittance after compression is more than 1 time and less than 1.8 times the thermal transmittance before compression.

6. In paragraph 1, For the above aerogel composite, the thermal transmittance before and after compression satisfies the following equation 4: [Formula 4] {(Thermal transmittance before and after compression (a)) - (Average of thermal transmittances before and after compression (b))} = (Average of thermal transmittances before and after compression (b)) XA In the above equation 4, The thermal transmittance before and after compression (a) refers to the thermal transmittance obtained after compression at 0 bar, 3 bar, 9 bar or 24 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite. The average value of the thermal transmittances before and after compression (b) refers to the average value of the thermal transmittance of the unpressurized aerogel composite and the thermal transmittances obtained after compression at pressure values ​​of 3 bar, 9 bar and 24 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite. A is between -0.40 and +0.

40.

7. In paragraph 1, For the above aerogel composite, the thermal transmittance before and after compression satisfies the following equation 4: [Formula 4] {(Thermal transmittance before and after compression (a)) - (Average of thermal transmittances before and after compression (b))} = (Average of thermal transmittances before and after compression (b)) XA In the above equation 4, The thermal transmittance before and after compression (a) refers to the thermal transmittance obtained after compression at 0 bar, 3 bar, or 9 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite. The average value of the thermal transmittances before and after compression (b) refers to the average value of the thermal transmittance of the unpressurized aerogel composite and the thermal transmittances obtained after compression at pressure values ​​of 3 bar and 9 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite. A is between -0.23 and +0.

23.

8. In paragraph 1, The thermal transmittance obtained after compression at pressures of 3 bar, 9 bar and 24 bar in the horizontal direction (transverse direction) for the cross-section of the above aerogel composite satisfies the following equation 5: [Formula 5] {(Thermal transmittance after compression (c) - Average value of thermal transmittances after compression (d))} = (Average value of thermal transmittances after compression (d)) XB In the above equation 5, The thermal transmittance after compression (c) refers to the thermal transmittance obtained after compression at a pressure of 3 bar, 9 bar or 24 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite. The average value of the thermal transmittances after compression (d) refers to the average value of the thermal transmittances obtained after compression by applying pressures of 3 bar, 9 bar, and 24 bar in the horizontal direction (transverse direction) to the cross-section of the aerogel composite. B is between -0.30 and +0.30, 9. In paragraph 1, For the above aerogel composite, the rate of change (C) of the thermal transmittance after compression per unit applied pressure, expressed by the following equation 6, is - 0.15 to + 0.15, the aerogel composite: [Formula 6] C = {(thermal transmittance after compression at pressure x - thermal transmittance after compression at pressure y)} / (x - y) In the above equation 6, x and y are independently 3 bar or 24 bar, but are different pressure values.

10. In paragraph 1, An aerogel composite having a compression recovery rate of 60% or more, expressed by Equation 2 below, when pressures of 3 bar, 9 bar, and 24 bar are applied in the horizontal direction (transverse direction) to the cross-section of the aerogel composite: [Formula 2] Compression recovery rate (%) = {(cross-sectional thickness of aerogel composite after compression) / (cross-sectional thickness of aerogel composite before compression)} X 100 11. In paragraph 1, The above aerogel is an aerogel composite comprising pores having a pore diameter of 30 nm or less, which account for 30% to 45% of the pore volume of the skeletal structure.

12. In paragraph 1, An aerogel composite, wherein the aerogel comprises silica, methylsilylated silica, dimethylsilylated silica, trimethylsilylated silica, or a mixture thereof.

13. In paragraph 1, An aerogel composite, wherein the silica aerogel particles include a plurality of aerogel particles having a particle size of more than 0 and less than or equal to 5 nm, which are aggregated or bonded together.

14. In paragraph 13, An aerogel composite wherein the average particle diameter of the above-mentioned aggregated or bonded particles is 5 to 2,000 nm.

15. In paragraph 1, An aerogel composite, wherein the thickness of the aerogel composite is 0.5 mm to 20 mm.

16. In paragraph 1, The density of the above aerogel composite is 0.05 to 0.50 g / cm 3 In, aerogel composite.

17. In paragraph 1, The above aerogel composite has a compressive strength of 20 kPa to 80 kPA at 10% strain and a tensile strength of 30 N / cm. 2 Up to 60 N / cm 2 An aerogel composite.

18. An insulating member comprising an aerogel composite according to any one of claims 1 to 17.

19. In paragraph 18, An insulating member, wherein the insulating member further includes a support member positioned on at least one of the upper and lower surfaces of the aerogel composite.

Citation Information

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