Aerogel composite
The aerogel composite with a fiber substrate and three-dimensional silica structure addresses the issue of insulation deterioration under pressure by maintaining heat transmittance and compression recovery, ensuring effective thermal insulation across varying pressures.
Patent Information
- Application Number
- PCT/KR2024/009125
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2023-11-01
- Filing Date
- 2024-06-28
- Publication Date
- 2025-01-02
AI Technical Summary
Aerogel composites used as thermal insulation materials face significant deterioration in insulation properties when exposed to pressurized environments due to thermal expansion and external pressures, leading to reduced heat transmittance and potential combustion risks.
Development of an aerogel composite with a fiber substrate and a three-dimensional network structure of silica aerogel particles, which maintains its thermal insulation properties by limiting heat transmittance ratio to three times or less under various compression pressures, and exhibits excellent compression recovery rates and mechanical strength.
The aerogel composite maintains excellent thermal insulation performance even under compressed conditions, with heat transmittance ratios within acceptable limits and high compression recovery rates, ensuring effective insulation without significant deterioration across different pressure applications.
Abstract
Description
Aerogel composites
[0001] Cross-citation with related application(s)
[0002] This application claims the benefit of priority to Korean Patent Application No. 10-2023-0083943, filed June 29, 2023, Korean Patent Application No. 10-2023-0097729, filed July 26, 2023, and U.S. Patent Application Nos. 18 / 386,103 and 18 / 386,108, filed November 1, 2023, 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, which are formed by forming hydrophobic silica aerogel on fibers, are widely used in construction and industrial sites as functional insulating materials that prevent corrosion due to moisture, and can also be usefully used as insulating materials, heat retaining materials, or fire retardants for aircraft, ships, automobiles, batteries, etc. However, when such silica aerogel blankets are applied 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 from 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.
[0008] One object of the present invention is to provide an aerogel composite whose insulating properties can be maintained at a constant level without significantly deteriorating even when exposed to a pressurized environment.
[0009] 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.
[0010] According to one embodiment of the present invention, there is provided an aerogel composite comprising a fiber substrate and an aerogel including one or more pores, wherein when the aerogel composite is compressed by applying a pressure of any one of 24 bar, 30 bar, or 33 bar in a horizontal direction (transverse direction) to a cross-section of the aerogel composite, the thermal transmittance after compression is 3 times or less compared to the thermal transmittance before compression.
[0011] When the cross-section of the above aerogel composite is compressed by applying a pressure of 24 bar, 30 bar or 33 bar in the horizontal direction (transverse direction), the thermal transmittance after compression may be more than 1 time and less than 3 times the thermal transmittance before compression.
[0012] When the above aerogel composite is compressed by applying a pressure of 3 bar, 9 bar or 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.
[0013] 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 1.45 times or less than the thermal transmittance before compression. 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 the same as the thermal transmittance before compression, or 1.45 times or less than the thermal transmittance before compression.
[0014] 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 1.85 times or less than the thermal transmittance before compression. 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 the same as the thermal transmittance before compression, or 1.85 times or less than the thermal transmittance before compression.
[0015] When a pressure of 15 bar is applied horizontally (transversely) to the cross-section of the aerogel composite, the thermal transmittance after compression may be 2.35 times or less than the thermal transmittance before compression. When a pressure of 15 bar is applied horizontally (transversely) to the cross-section of the aerogel composite, the thermal transmittance after compression may be the same as the thermal transmittance before compression, or 2.35 times or less than the thermal transmittance before compression.
[0016] When at least one pressure of 9 bar, 15 bar, 24 bar, 30 bar or 33 bar is 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 1 may be 60% or more.
[0017] [Formula 1]
[0018] Compression recovery rate (%) = {(cross-sectional thickness of aerogel composite after compression) / (cross-sectional thickness of aerogel composite before compression)} X 100
[0019] When at least one pressure of 9 bar, 15 bar, 24 bar, 30 bar or 33 bar is applied in the horizontal direction (transverse direction) to the cross-section of the aerogel composite, the compression recovery rate expressed by the above formula 1 may be 60% to 99%, 60% to 98%, 60% to 97%, 60% to 96%, or 60% to 95%.
[0020] 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 above formula 1 may be 60% or more.
[0021] The thermal transmittance obtained after compression at at least one of 3 bar, 9 bar, 15 bar, 24 bar or 30 bar for the above aerogel composite can satisfy the following equation 3:
[0022] [Formula 3]
[0023] (Thermal transmittance after compression (a) - Average value of thermal transmittance after compression (b)) = (Average value of thermal transmittance after compression (b)) XA
[0024] In the above equation 3, the thermal transmittance after compression (a) means the thermal transmittance obtained after compression at a pressure value of 9 bar, 15 bar, 24 bar, or 30 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 (b) means the average value of the thermal transmittances obtained after compression at a pressure value of 9 bar, 15 bar, 24 bar, and 30 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite, and the above A may be a rational number of - 0.15 to + 0.15.
[0025] In the above equation 3, the thermal transmittance after compression (a) means 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, and the average value of the thermal transmittances after compression (b) 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 the above A may be a rational number of -0.25 to +0.25.
[0026] For the above aerogel composite, the thermal transmittance before and after compression can satisfy the following equation 4:
[0027] [Formula 4]
[0028] {(Thermal transmittance before and after compression (c)) - (Average of thermal transmittances before and after compression (d))} = (Average of thermal transmittances before and after compression (d)) XD
[0029] In the above equation 4, the thermal transmittance before and after compression (c) is the thermal transmittance obtained after compression at 0 bar, 3 bar, 9 bar or 24 bar in the transverse direction for the aerogel composite, and the average value of the thermal transmittances before and after compression (d) means the average value of the thermal transmittances obtained after compression at pressure values of 0 bar, 3 bar, 9 bar and 24 bar in the transverse direction for the aerogel composite, and the D may be a rational number of -0.25 to +0.25.
[0030] For the above aerogel composite, the rate of change (B) of the thermal transmittance after compression per unit applied pressure, expressed by Equation 5 below, may be a rational number of - 0.10 to + 0.10:
[0031] [Formula 5]
[0032] B = (Thermal transmittance after compression at pressure x - Thermal transmittance after compression at pressure y) / (x - y)
[0033] In the above equation 5, x and y are each independently a pressure value (unit: bar) of 3 bar, 9 bar, 15 bar or 24 bar, and are different pressure values.
[0034] The 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. The aerogel may include pores having a pore diameter of 0.1 nm or more and 30 nm or less, in an amount of 30% to 45% of the pore volume of the skeletal structure.
[0035] The density of the above aerogel composite is 0.05 to 0.50 g / cm 3 It could be.
[0036]
[0037] According to another embodiment of the present invention, there is provided an insulating member comprising an aerogel composite provided by the present invention.
[0038] 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.
[0039] 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.
[0040] According to one embodiment of the present invention, there is provided an aerogel composite comprising a fiber substrate and an aerogel including one or more pores, wherein when the aerogel composite is compressed by applying pressures of 24 bar, 30 bar, and 33 bar in a horizontal direction (transverse direction) to a cross-section of the aerogel composite, the thermal transmittance after compression is 3 times or less compared to the thermal transmittance before compression.
[0041] 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.
[0042] When the cross-section of the above aerogel composite is compressed by applying pressures of 24 bar, 30 bar, and 33 bar in the horizontal direction (transverse direction), the thermal transmittance after compression may be more than 1 time and less than 3 times the thermal transmittance before compression.
[0043] 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.
[0044] When a pressure of 3 bar is applied in the horizontal direction (transverse direction) to the cross-section of the above aerogel composite, the thermal transmittance after compression may be 1.45 times or less compared to the thermal transmittance before compression.
[0045] When a pressure of 9 bar is applied in the horizontal direction (transverse direction) to the cross-section of the above aerogel composite, the thermal transmittance after compression may be 1.85 times or less compared to the thermal transmittance before compression.
[0046] When a pressure of 15 bar is applied in the horizontal direction (transverse direction) to the cross-section of the above aerogel composite, the thermal transmittance after compression may be 2.35 times or less compared to the thermal transmittance before compression.
[0047] When pressures of 9 bar, 15 bar, 24 bar, 30 bar and 33 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 1 may be 60% or more:
[0048] [Formula 1]
[0049] Compression recovery rate (%) = {(cross-sectional thickness of aerogel composite after compression) / (cross-sectional thickness of aerogel composite before compression)} X 100
[0050] 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 above formula 1 may be 60% or more.
[0051] The thermal transmittance obtained after compression at a pressure of 3 bar, 9 bar, 15 bar, 24 bar or 30 bar for the above aerogel composite can satisfy the following equation 3:
[0052] [Formula 3]
[0053] (Thermal transmittance after compression (a) - Average value of thermal transmittance after compression (b)) = (Average value of thermal transmittance after compression (b)) XA
[0054] In the above equation 3, the thermal transmittance after compression (a) means the thermal transmittance obtained after compression at any one of the pressure values of 9 bar, 15 bar, 24 bar, and 30 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 (b) means the average value of the thermal transmittances obtained after compression at each of the pressure values of 9 bar, 15 bar, 24 bar, and 30 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite, and the above A may be a rational number of - 0.15 to + 0.15.
[0055] In the above equation 3, the thermal transmittance after compression (a) means 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, and the average value of the thermal transmittances after compression (b) 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 the above A may be a rational number of -0.25 to +0.25.
[0056] For the above aerogel composite, the thermal transmittance before and after compression can satisfy the following equation 4:
[0057] [Formula 4]
[0058] {(Thermal transmittance before and after compression (c)) - (Average of thermal transmittances before and after compression (d))} = (Average of thermal transmittances before and after compression (d)) XD
[0059] In the above equation 4, the thermal transmittance before and after compression (c) is 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 aerogel composite, and the average value (d) of the thermal transmittances before and after compression means the average value of the thermal transmittances obtained after compression at pressure values of 0 bar, 3 bar, 9 bar and 24 bar in the horizontal direction (transverse direction) with respect to the aerogel composite, and the D may be a rational number of -0.25 to +0.25.
[0060] For the above aerogel composite, the rate of change (B) of the thermal transmittance after compression per unit applied pressure, expressed by Equation 5 below, may be a rational number of - 0.10 to + 0.10:
[0061] [Formula 5]
[0062] B = (Thermal transmittance after compression at pressure x - Thermal transmittance after compression at pressure y) / (x - y)
[0063] In the above equation 5, x and y are each independently one of 3 bar, 9 bar, 15 bar, and 24 bar pressure values (unit: bar), which are different pressure values.
[0064] The above aerogel may include pores having a pore diameter of 30 nm or less, which account for 30% to 40% of the pore volume of the skeletal structure.
[0065] The density of the above aerogel composite is 0.05 to 0.50 g / cm 3 It could be.
[0066]
[0067] According to another embodiment of the present invention, there is provided an insulating member comprising an aerogel composite provided by the present invention.
[0068] 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.
[0069] 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.
[0070]
[0071] According to one embodiment of the present invention, there is provided an aerogel composite comprising a fiber substrate; and an aerogel including one or more pores.
[0072] The above "aerogel" includes a three-dimensional network structure in which a plurality of aerogel particles having a size of approximately 2 to 20 nm are aggregated or bonded to form a plurality of open pores.
[0073] The aerogel may be an inorganic silica aerogel formed from a silicon alkoxide compound or water glass as a precursor. The aerogel may be composed of silica, methylsilylated silica, dimethylsilylated silica, trimethylsilylated silica, or a mixture thereof. 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. The manufacturing process of the aerogel is described in detail below.
[0074] The above "aerogel particles" are individual solid unit particles that constitute the aerogel, and may be powders, beads, fine particles, granules, pellets, aggregates, fibers, flakes, etc., and the shapes may be spherical, hemispherical, circular, semicircular, polygonal, cubic, rod-shaped, polyhedral, irregular, etc. The aerogel particles may have an average particle diameter of about 10 to 2,000 nm, 10 to 1,500 nm, or 10 to 1,000 nm, but are not limited thereto. The average particle size may be measured by any means known to those skilled in the art, such as, but not limited to, scanning electron microscopy, dynamic light scattering, optical microscopy, or a size exclusion method.
[0075] 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 may include mesopores. In one specific example, the aerogel 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).
[0076] 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.
[0077] Specifically, the aerogel may contain pores having a pore diameter of 30 nm or less, preferably 0.1 nm or more and 30 nm or less, in an amount of 25% or more, 26% or more, 27% or more, 28% or more, 29% or more, 30% or more, or 31% or more 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, and preferably 25% or more and 45% or less, 25% or more and 40% or less, 30% or more and 45% or less, or 30% or more and 40% or less, but is not limited thereto. The aerogel may comprise 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. The aerogel may comprise pores having a pore diameter of 0.1 nm or more and 30 nm or less, in an amount of 30% to 45% of the pore volume of the skeletal structure.
[0078] In addition, the aerogel may contain pores having a pore diameter of 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, and preferably 55% or more but less than 75%, 60% or more but less than 75%, 55% or more but less than 70%, or 60% or more but less than 70%.
[0079] 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.
[0080] 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.
[0081] 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® (manufactured by DuPont), Dyneema® (manufactured by DSM), Spectra® (manufactured by Honeywell), other polypropylene fibers such as Typar®, Xavan® (both manufactured by DuPont), fluoropolymers such as PTFE under the Teflon® trade name (manufactured by DuPont), Gore-tex® (manufactured by WL GORE), silicon carbide fibers such as NICALCON (manufactured by COI Ceramics), ceramic fibers such as NEXTEL (manufactured by 3M), acrylic polymers, wool, silk, hemp, leather, suede fibers, PBO fibers Zylon® (manufactured by Thombo), liquid crystal materials such as VECTAN (manufactured by Hoechst), Cambrel fibers (manufactured by DuPont), polyurethane, polyamide, wool fibers, boron, aluminum, iron, stainless steel fibers or other thermoplastic resins such as PEEK, PES, PET, PEK, PPS, but any fiber that can further improve the insulating performance by including a space or void into which the aerogel can be easily inserted may be used without limitation.
[0082] The thickness of the above fiber substrate may be, but is not limited to, 0.5 to 20 mm.
[0083] The above aerogel composite may have a mixture of fiber substrate and aerogel from the top surface to the bottom surface, but is not limited thereto.
[0084] In addition, at least a portion of the upper or lower surface of the aerogel composite, preferably the entire surface, may have a flat shape. Here, the "flat shape" means that no irregularities are formed by intentional embossing or a coating process. Forming the upper and lower surfaces of the aerogel composite flat increases the ease of work when laminating a support member such as a sheet on the surfaces of the upper and lower surfaces in the future, and can increase the adhesion maintenance rate of the support member. In addition, even if the aerogel composite itself is directly applied as an insulating member without a support member, it is preferable because it can reduce friction with the surface of an adjacent device.
[0085] The above aerogel composite 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 its insulation properties can also be maintained at a high level.
[0086] 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.
[0087] 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% It can be 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.
[0088] The above "compression recovery rate" means 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 1 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.
[0089] [Formula 1]
[0090] Compression recovery rate (%) = {(cross-sectional thickness of aerogel composite after compression) / (cross-sectional thickness of aerogel composite before compression)} X 100
[0091] 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. 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 2 below, but is not limited thereto, and may be calculated differently depending on the specifications of each equipment or manufacturer.
[0092] [Formula 2]
[0093] 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 ))
[0094] In the above equation 2, the unit of the inner diameter of the cylinder may be, for example, cm, and the unit of the area of the specimen may be, for example, cm 2 It can be, and the unit of the set pressure value can be bar or kgf, but is not limited thereto.
[0095] 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.
[0096] Applying transverse pressure to the aerogel composite means applying pressure in a horizontal direction to the cross-section of the aerogel composite, and more specifically, 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.
[0097] When a pressure of 3 bar or more is applied in the horizontal direction (transverse direction) to the cross-section of the above 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.
[0098] 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 above 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.
[0099] When a pressure of 3 bar is applied to the cross-section of the above aerogel composite in the horizontal direction (transverse direction), 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 80% or more, 82% or more, 84% or more, 86% or more, It could be 88% or more, 90% or more, or 92% or more.
[0100] When a pressure of 9 bar is applied to the cross-section of the above 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, 82% or more, It may be 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, 76% or more, or 78% or more.
[0101] When a pressure of 15 bar is applied to the cross-section of the above 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, 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 70% or more, 72% or more, 74% or more, or 76% or more.
[0102] When a pressure of 24 bar is applied to the cross-section of the above 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, 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 70% or more, 72% or more, 74% or more, or 76% or more.
[0103] When a pressure of 30 bar is applied to the cross-section of the above aerogel composite in the horizontal direction (transverse direction), 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, 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 68% or more, 70% or more, 72% or more, 74% or more, or 76% or more.
[0104] When a pressure of 33 bar is applied to the cross-section of the above aerogel composite in the horizontal direction (transverse direction), 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, 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 68% or more, 70% or more, 72% or more, 74% or more, or 76% or more.
[0105] When a pressure of 37 bar is applied to the cross-section of the above aerogel composite in the horizontal direction (transverse direction), 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, 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 55% or more, 60% or more, or 62% or more.
[0106] 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.
[0107] 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 may additionally be 1 times or more or greater than 1 times.
[0108] The above "thermal transmittance" refers to the heat transfer from air layer to air layer through a solid object, and means the amount of heat that flows when there is a temperature difference of 1℃ across a cross-sectional area of 1 m² per unit time. It is the value calculated by dividing the thermal conductivity of an object by the thickness of the object. The amount of heat transfer of an object is affected by its thermal conductivity and the thickness of the object. The higher the thermal conductivity and the thinner the thickness, the greater the amount of 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 object such as an aerogel composite, the thermal conductivity and thickness can change after pressurization. In other words, unless it is a perfectly elastic material, the thickness will inevitably decrease after pressurization. However, 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 deteriorate. Therefore, whether insulation performance is maintained after pressurization cannot be determined simply by post-pressurization thermal conductivity. Rather, it can be determined through the thermal transmittance, which considers both post-pressurization thermal conductivity and post-pressurization thickness. Even if thermal conductivity decreases or is maintained after pressurization, if the post-pressurization thickness is significantly reduced, the thermal transmittance and total heat transfer inevitably increase significantly.
[0109] The above aerogel composite does not show a significant change in thermal conductivity or thickness even after pressurization, so the increase in 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.
[0110] The above "post-compressed thermal transmittance" means 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 a specific level of pressure is applied horizontally (transversely) to the cross-section of the aerogel composite to compress it. 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.
[0111] 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.
[0112] 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 above 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, 1.03 times or less, It can be 1.02 times or less, or 1.01 times or less.
[0113] When pressure is applied to the cross-section of the above 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.
[0114] When pressure is applied to the cross-section of the above 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 compared to the thermal transmittance before compression.
[0115] When pressure is applied to the cross-section of the above 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.
[0116] When pressure is applied to the cross-section of the above 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 compared to the thermal transmittance before compression.
[0117] When pressure is applied to the cross-section of the above 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.
[0118] When pressure is applied to the cross-section of the above 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 compared to the thermal transmittance before compression.
[0119] When pressure is applied to the cross-section of the above aerogel composite in a horizontal direction (transverse direction) at any one of 24 bar to 33 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.
[0120] When pressure is applied to the cross-section of the above 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.
[0121] When pressure is applied to the cross-section of the above 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 compared to the thermal transmittance before compression.
[0122] When a pressure of 3 bar is applied horizontally (transversely) to the cross-section of the above aerogel composite, the thermal transmittance after compression may be 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 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.
[0123] 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 1.45 times or less than the thermal transmittance before compression. 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 the same as the thermal transmittance before compression, or may be 1.45 times or less than the thermal transmittance before compression. 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 greater than the thermal transmittance before compression, and may be 1.45 times or less than the thermal transmittance before compression.
[0124] When a pressure of 9 bar is applied to the cross-section of the above aerogel composite in the horizontal direction (transverse direction), the thermal transmittance after compression may be 1.85 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 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.
[0125] 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 1.85 times or less than the thermal transmittance before compression. 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 the same as the thermal transmittance before compression, or may be 1.85 times or less than the thermal transmittance before compression. 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 greater than the thermal transmittance before compression, and may be 1.85 times or less than the thermal transmittance before compression.
[0126] When a pressure of 15 bar is applied to the cross-section of the above 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 times or less, It may be 1.1 times or less or 1.05 times or less, and more preferably 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.
[0127] When a pressure of 15 bar is applied horizontally (transversely) to the cross-section of the aerogel composite, the thermal transmittance after compression may be 2.35 times or less than the thermal transmittance before compression. When a pressure of 15 bar is applied horizontally (transversely) to the cross-section of the aerogel composite, the thermal transmittance after compression may be the same as the thermal transmittance before compression, or may be 2.35 times or less than the thermal transmittance before compression. When a pressure of 15 bar is applied horizontally (transversely) to the cross-section of the aerogel composite, the thermal transmittance after compression may be greater than the thermal transmittance before compression, and may be 2.35 times or less than the thermal transmittance before compression.
[0128] When a pressure of 24 bar is applied to the cross-section of the above 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 2.3 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, It 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, or 1.05 times or less, and more preferably 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.
[0129] When a pressure of 24 bar is applied horizontally (transversely) to the cross-section of the aerogel composite, the thermal transmittance after compression may be 2.7 times or less than the thermal transmittance before compression. When a pressure of 24 bar is applied horizontally (transversely) to the cross-section of the aerogel composite, the thermal transmittance after compression may be the same as the thermal transmittance before compression, or may be 2.7 times or less than the thermal transmittance before compression. When a pressure of 24 bar is applied horizontally (transversely) to the cross-section of the aerogel composite, the thermal transmittance after compression may be greater than the thermal transmittance before compression, and may be 2.7 times or less than the thermal transmittance before compression.
[0130] When a pressure of 30 bar is applied to the cross-section of the above 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, 2.1 times or less, 2 It may be 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, and more preferably 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.
[0131] When a pressure of 30 bar is applied horizontally (transversely) to the cross-section of the aerogel composite, the thermal transmittance after compression may be 3 times or less than the thermal transmittance before compression. When a pressure of 30 bar is applied horizontally (transversely) to the cross-section of the aerogel composite, the thermal transmittance after compression may be the same as the thermal transmittance before compression, or 3 times or less than the thermal transmittance before compression. When a pressure of 30 bar is applied horizontally (transversely) to the cross-section of the aerogel composite, the thermal transmittance after compression may be greater than the thermal transmittance before compression, and 3 times or less than the thermal transmittance before compression.
[0132] When a pressure of 33 bar is applied to the cross-section of the above 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, 2.1 times or less, 2 It may be 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, and more preferably 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, or 1.2 times or less.
[0133] When a pressure of 33 bar is applied horizontally (transversely) to the cross-section of the aerogel composite, the thermal transmittance after compression may be 3 times or less than the thermal transmittance before compression. When a pressure of 33 bar is applied horizontally (transversely) to the cross-section of the aerogel composite, the thermal transmittance after compression may be the same as the thermal transmittance before compression, or 3 times or less than the thermal transmittance before compression. When a pressure of 33 bar is applied horizontally (transversely) to the cross-section of the aerogel composite, the thermal transmittance after compression may be greater than the thermal transmittance before compression, and 3 times or less than the thermal transmittance before compression.
[0134] When the above aerogel composite is compressed by applying at least one of 3 bar, 9 bar and 24 bar in the transverse direction, the thermal transmittance after compression may be equal to or 1.8 times or less than the thermal transmittance before compression.
[0135] When the above aerogel composite is compressed by applying transverse pressures of 3 bar, 9 bar, and 24 bar, respectively, the thermal transmittance after compression may be the same as or 1.8 times or less than the thermal transmittance before compression.
[0136] When the above aerogel composite is compressed by applying transverse pressures of 3 bar, 9 bar, and 24 bar, respectively, the thermal transmittance after compression may be greater than or 1.8 times less than the thermal transmittance before compression.
[0137] When measuring the recovery rate or thermal transmittance after compression 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 measurement device depending on the measurement 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.
[0138] The above post-compression recovery rate or post-compression thermal transmittance may be measured for a rectangular aerogel composite specimen having a width X length of 20 cm X 20 cm. In this case, if the width or length of the manufactured aerogel composite is each less than 20 cm, two or more specimens may be arranged in parallel adjacent to each other so that the specimens have a size of 20 cm X 20 cm, and then measurements may be performed on these specimens.
[0139] The above aerogel composite can maintain its insulation performance at an excellent level without significant deterioration as the thermal transmittance after compression is maintained within a specific range even when pressurized (or compressed) at any pressure.
[0140] Specifically, the thermal transmittance obtained after compression at at least one pressure value among 3 to 30 bar for the aerogel composite may satisfy the following equation 3:
[0141] [Formula 3]
[0142] (Thermal transmittance after compression (a) - Average value of thermal transmittance after compression (b)) = (Average value of thermal transmittance after compression (b)) XA
[0143] In the above equation 3, the “post-compressed thermal transmittance (a)” means the 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. The post-compressed thermal transmittance (a) may mean the thermal transmittance obtained after compression by applying a pressure of 3 bar, 9 bar, 15 bar, 24 bar, or 30 bar. Alternatively, it may mean the thermal transmittance obtained after compression by applying a pressure of 3 bar, 9 bar, or 24 bar. Alternatively, it may mean the thermal transmittance obtained after compression by applying a pressure of 9 bar, 15 bar, 24 bar, or 30 bar.
[0144] In addition, the above "average value (b) 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. The average value (b) of thermal transmittances after compression may mean an average value of thermal transmittances obtained after compression by applying pressures of 3 bar, 9 bar, and 24 bar, respectively. Alternatively, it may mean an average value of thermal transmittances obtained after compression by applying pressures of 9 bar, 15 bar, 24 bar, and 30 bar, respectively.
[0145] The above A may be a rational number of -0.25 to +0.25, a rational number of -0.24 to +0.24, a rational number of -0.23 to +0.23, a rational number of -0.22 to +0.22, a rational number of -0.21 to +0.21, a rational number of -0.20 to +0.20, a rational number of -0.19 to +0.19, a rational number of -0.15 to +0.15, a rational number of -0.14 to +0.14, a rational number of -0.13 to +0.13, a rational number of -0.12 to +0.12, a rational number of -0.11 to +0.11, or a rational number of -0.10 to +0.10.
[0146] The thermal transmittance obtained after compressing the aerogel composite at a pressure of 9 bar, 15 bar, 24 bar or 30 bar may satisfy the above equation 3. In this case, in the equation 3, the thermal transmittance after compression (a) refers to the thermal transmittance obtained after compressing the aerogel composite at a pressure value of 9 bar, 15 bar, 24 bar or 30 bar in the horizontal direction (transverse direction) with respect to the cross-section, and the average value of the thermal transmittances after compression (b) refers to the average value of the thermal transmittances obtained after compressing the aerogel composite at any two pressure values of 9 bar, 15 bar, 24 bar and 30 bar in the horizontal direction (transverse direction) with respect to the cross-section.
[0147] The thermal transmittance obtained after compressing the aerogel composite at pressures of 9 bar, 15 bar, 24 bar, and 30 bar, respectively, may satisfy Equation 3. In this case, in Equation 3, the thermal transmittance after compression (a) may refer to the thermal transmittance obtained after compressing the aerogel composite at pressure values of 9 bar, 15 bar, 24 bar, and 30 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 (b) may refer to the average value of the thermal transmittances obtained after compressing the aerogel composite at pressure values of 9 bar, 15 bar, 24 bar, and 30 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite. At this time, the above A may be a rational number of - 0.15 to + 0.15, a rational number of - 0.14 to + 0.14, a rational number of - 0.13 to + 0.13, a rational number of - 0.12 to + 0.12, a rational number of - 0.11 to + 0.11, or a rational number of - 0.10 to + 0.10.
[0148] The thermal transmittance obtained after compressing the aerogel composite at a pressure of 3 bar, 9 bar, or 24 bar may satisfy the above equation 3. In this case, in the equation 3, the thermal transmittance after compression (a) refers to the thermal transmittance obtained after compressing the cross-section of the aerogel composite at a pressure value of 3 bar, 9 bar, or 24 bar in the horizontal direction (transverse direction), and the average value of the thermal transmittances after compression (b) may refer to the average value of the thermal transmittances obtained after compressing the cross-section of the aerogel composite at at least two pressure values among 3 bar, 9 bar, and 24 bar in the horizontal direction (transverse direction).
[0149] The thermal transmittance obtained after compression at pressures of 3 bar, 9 bar, and 24 bar for the above aerogel composite can satisfy the above equation 3. At this time, in the above formula 3, the thermal transmittance after compression (a) means the thermal transmittance obtained after compression at 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 (b) means the average value of the thermal transmittances obtained after compression at 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 A may be a rational number of -0.25 to +0.25, a rational number of -0.24 to +0.24, a rational number of -0.23 to +0.23, a rational number of -0.22 to +0.22, a rational number of -0.21 to +0.2, a rational number of -0.20 to +0.20, or a rational number of -0.19 to +0.19.
[0150] In addition, the aerogel composite can maintain its insulation performance at an excellent level without significant deterioration since the thermal transmittance before and after compression is maintained within a specific range even when pressurized (or compressed) at any pressure.
[0151] Specifically, the thermal transmittance obtained after compression at at least one pressure value among 0 to 24 bar for the aerogel composite may satisfy the following equation 4:
[0152] [Formula 4]
[0153] {(Thermal transmittance before and after compression (c)) - (Average of thermal transmittances before and after compression (d))} = (Average of thermal transmittances before and after compression (d)) XD
[0154] In the above equation 4, the “thermal transmittance before and after compression (c)” refers to 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. The thermal transmittance before and after compression (c) may refer to 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 refers to no pressure (no compression), and accordingly, the thermal transmittance obtained after compression by applying a pressure of 0 bar refers to the thermal transmittance of the aerogel composite that is not pressurized.
[0155] In addition, the above "average value (d) of thermal transmittances before and after compression" means the average value of the thermal transmittance of the aerogel composite without applying pressure (or compression) and the average value of the thermal transmittances obtained after compression with at least two pressure values in the range of more than 0 bar and less than 24 bar in the horizontal direction (transverse direction) with respect to the cross-section of the aerogel composite. It may mean the average value of the thermal transmittances obtained after compression by applying pressure to the aerogel composite with at least two pressure values of 0 bar, 3 bar, 9 bar, and 24 bar.
[0156] The above D may be a rational number of -0.30 to +0.30, a rational number of -0.25 to +0.25, a rational number of -0.24 to +0.24, a rational number of -0.23 to +0.23, a rational number of -0.22 to +0.22, a rational number of -0.21 to +0.21, a rational number of -0.20 to +0.20, a rational number of -0.19 to +0.19, a rational number of -0.15 to +0.15, a rational number of -0.14 to +0.14, a rational number of -0.13 to +0.13, a rational number of -0.12 to +0.12, a rational number of -0.11 to +0.11, or a rational number of -0.10 to +0.10. there is.
[0157] The thermal transmittance of the non-pressurized, non-compressed (0 bar compression) aerogel composite can satisfy the above equation 4. At this time, the average value (d) of the thermal transmittances before and after compression can mean the average value of the thermal transmittance of the non-compressed aerogel composite and the thermal transmittance obtained after compression with 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.
[0158] The thermal transmittance obtained after compression at a pressure of 3 bar, 9 bar or 24 bar for the aerogel composite can satisfy the above equation 4. In this case, the average value (d) of the thermal transmittances before and after compression can mean the average value of the thermal transmittance of the non-compressed (0 bar compression) aerogel composite and the thermal transmittances 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.
[0159] The average value (d) of the thermal transmittances before and after the compression refers to 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, the D may be a rational number of -0.30 to +0.30, a rational number of -0.25 to +0.25, a rational number of -0.24 to +0.24, a rational number of -0.23 to +0.23 or a rational number of -0.22 to +0.22.
[0160] The average value (d) of the thermal transmittances before and after the compression refers to 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 D may be a rational number of -0.25 to +0.25, a rational number of -0.24 to +0.24, a rational number of -0.23 to +0.23, a rational number of -0.22 to +0.22, a rational number of -0.21 to +0.21, or a rational number of -0.20 to +0.20.
[0161] The thermal transmittance obtained after compressing the aerogel composite at a pressure of 0 bar, 3 bar, 9 bar or 24 bar can satisfy the above equation 4. Here, 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 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. In this case, the D may be a rational number of -0.25 to +0.25.
[0162] In addition, for the aerogel composite, the rate of change (B) of the thermal transmittance after compression per unit applied pressure expressed by the following equation 5 may be a rational number of - 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 may be a rational number of + 0.10 or less, + 0.09 or less, + 0.08 or less, + 0.07 or less, + 0.06 or less, + 0.05 or less, + 0.04 or less, + 0.03 or less, + 0.02 or less, or + 0.01 or less. Preferably, it may be a rational number of - 0.10 to + 0.10, a rational number of - 0.09 to + 0.09, a rational number of - 0.08 to + 0.08, a rational number of - 0.07 to + 0.07, a rational number of - 0.06 to + 0.06, or a rational number of - 0.05 to + 0.05:
[0163] [Formula 5]
[0164] B = (Thermal transmittance after compression at pressure x - Thermal transmittance after compression at pressure y) / (x - y)
[0165] In the above equation 5, 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.
[0166] In the above equation 5, x and y can each independently be any one of the pressure values of 3 bar, 9 bar, 15 bar, and 24 bar.
[0167] In the above equation 5, x may be 24 bar and y may be 3 bar.
[0168] In the above equation 5, x may be 24 bar and y may be 9 bar.
[0169] In the above equation 5, x may be 15 bar and y may be 9 bar.
[0170] In the above equation 5, x may be 24 bar and y may be 15 bar.
[0171] The rate of change (B) of the thermal transmittance after compression per unit applied pressure may be a rational number of - 0.10 to + 0.10.
[0172] 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.
[0173] 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.
[0174] 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.
[0175] Steps for preparing silica sol;
[0176] In the present invention, a silica sol can be prepared by mixing a silica precursor composition and a catalyst composition.
[0177] The above silica precursor composition may include water and / or a polar organic solvent in the silica precursor.
[0178] 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. More specifically, among these, the silica precursor may be tetramethyl orthosilicate (TMOS), tetraethyl orthosilicate (TEOS), or a mixture thereof.
[0179] 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.
[0180] In addition, the silica precursor may include pre-hydrolyzed TEOS (HTEOS). HTEOS is an ethyl silicate oligomer material having a wide 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.
[0181] 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.
[0182] 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.
[0183] 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 present invention is not limited thereto. The above silica concentration is the concentration of silica contained in the silica precursor composition, and can be appropriately adjusted by varying the contents of the silica precursor, organic solvent, and water.
[0184] 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.
[0185] 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. Among these, when considering miscibility with water and aerogel, the polar organic solvent may be a monohydric alcohol having 1 to 6 carbon atoms such as methanol, ethanol, isopropanol, butanol, for example, ethanol.
[0186] 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.
[0187] When preparing the above silica precursor composition, when preparing a pre-hydrolyzed silica precursor, 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.
[0188] When preparing the above silica precursor composition, when preparing a hydrolyzed silica precursor, the silica precursor and water may be mixed in a molar ratio of 1:0.1 to 10, 1:1 to 8, or 1:2 to 6, but the present invention is not limited thereto.
[0189] In addition, when the silica precursor composition is manufactured, if the silica precursor includes TEOS that has been hydrolyzed, the composition may be manufactured by mixing the hydrolyzed TEOS and the organic solvent in a weight ratio of 1:2 to 10, 1:3 to 8, or 1:3 to 6, but is not limited thereto.
[0190] 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 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.
[0191] 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.
[0192] 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.
[0193] 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.
[0194] The alkoxy silane compound having 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. However, specific examples thereof include, but are not limited to, at least one selected from the group consisting of trimethylethoxysilane (TMES), trimethylsilanol (TMS), trimethylchlorosilane (TMCS), methyltrimethoxysilane (MTMS), methyltriethoxysilane (MTES), dimethyldiethoxysilane (DMDEOS), ethyltriethoxysilane, and phenyltriethoxysilane.
[0195] 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.
[0196] 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.
[0197] 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.
[0198] If necessary, additives may be added to the silica sol. Any known additives that can be added during the manufacture of aerogels may be used, including, for example, opacifiers and flame retardants.
[0199] 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.
[0200] Gelation stage of silica sol
[0201] In the present invention, the silica sol can be gelated after impregnating the substrate with the silica sol.
[0202] 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.
[0203] 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, it is preferable because an appropriate viscosity range of the catalyzed sol can be more easily achieved, and a desired viscosity range can be satisfied even with a relatively short residence time.
[0204] 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 0.7 to 1:1, but is not limited thereto.
[0205] 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.
[0206] The substrate impregnated with the catalyzed sol can be gelled on a moving element such as a conveyor belt.
[0207] The above "gelation" may refer to a sol-gel reaction, and the above "sol-gel reaction" may refer to forming a network structure 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.
[0208] 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 the gelation time can 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.
[0209] Maturation stage of the gelled wet gel complex
[0210] If necessary, an additional maturation step may be included to allow the wet gel composite obtained through gelation as described above to fully undergo chemical changes by allowing it to stand at an appropriate temperature. This maturation step can further solidify the network structure formed through gelation, thereby enhancing the mechanical stability of the aerogel composite.
[0211] 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.
[0212] 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.
[0213] The above maturation step can be performed 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 preventing loss of solvent due to evaporation, thereby preventing an increase in production costs.
[0214] 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%.
[0215] 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.
[0216] 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.
[0217] 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.; preferably, a monohydric alcohol having 1 to 6 carbon atoms such as methanol, ethanol, isopropanol, butanol, etc., such as ethanol, but is not limited thereto.
[0218] 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.
[0219] Surface modification step of the matured wet gel composite
[0220] 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.
[0221] 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.
[0222] 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.
[0223] 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.
[0224] 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.
[0225] Drying stage
[0226] The present invention may include a drying step of drying the surface-modified wet gel composite to obtain an aerogel composite.
[0227] 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.
[0228] 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.
[0229] 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.
[0230] In addition to the above process, the method includes acidifying a basic metal oxide precursor (e.g., sodium silicate) in water to prepare a hydrogel. The salt byproduct can be removed from the silicate 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 in the gel is then at least partially extracted using an innovative processing and extraction technique.
[0231] In addition to the above process, the present invention includes reducing damaging capillary forces at the solvent / pore interface by chemical modification of the matrix material in the wet gel state through conversion of surface hydroxyl groups to hydrophobic trimethylsilyl ethers, thereby enabling liquid phase extraction from the gel material at temperatures and pressures below the critical point of the solvent.
[0232] In addition to the above-described process, the liquid (solvent) within the gel material can 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.
[0233] 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.
[0234]
[0235] According to another embodiment of the present invention, there is provided an insulating member comprising an aerogel composite provided by the present invention.
[0236] 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.
[0237] 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.
[0238] 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).
[0239] 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.
[0240] 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.
[0241] 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).
[0242] 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.
[0243] 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.
[0244]
[0245] 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.
[0246]
[0247] Example
[0248]
[0249] [Example 1]
[0250] A silica precursor solution was prepared by mixing tetraethyl orthosilicate (TEOS) and water in a molar ratio of 1:4 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 3 or lower, and the solution 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. 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 at a volume ratio of 1:1 (catalyzed silica sol: fiber). The fibers, which had passed through the impregnation tank and were infiltrated with the catalyzed sol, were gelled for about 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°C. Thereafter, a solution of 2.9 wt% methyltriethoxysilane (MTES) diluted in ethanol with a moisture content of 10 wt% was added as a maturation solution in an amount of 109 vol% based on the volume of the wet gel composite, and maturation was performed at a temperature of 75°C 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, and then surface modification was performed at a temperature of 75°C for 4 hours. Afterwards, supercritical drying was performed under the conditions of CO2150 bar and 70 ℃ to manufacture an aerogel composite having a density of approximately 0.177 g / cc.
[0251]
[0252] [Example 2]
[0253] 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, acid was added so that the pH of the silica precursor solution became 3 or lower, 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 1:4 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, 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 0.7:1 (catalyzed silica sol: fiber). The fibers, which had passed through the impregnation tank and were infiltrated with the catalyzed sol, were gelled for about 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°C. Thereafter, a solution of 2.9 wt% methyltriethoxysilane (MTES) diluted in ethanol with a moisture content of 10 wt% was added as a maturation solution in an amount of 109 vol% based on the volume of the wet gel composite, and maturation was performed at a temperature of 75°C 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, and then surface modification was performed at a temperature of 75°C for 4 hours. Afterwards, supercritical drying was performed under the conditions of CO2150 bar and 70 ℃ to manufacture an aerogel composite having a density of approximately 0.187 g / cc.
[0254]
[0255] [Example 3]
[0256] A silica precursor composition was prepared by mixing methyltriethoxysilane (MTES) and TEOS in a molar ratio of 97:3. The silica precursor composition and water were mixed in a molar ratio of 1:10, and ethanol in a weight ratio of 1:2 was added to the silica precursor composition to prepare a silica sol. Hydrochloric acid was added so that the pH of the silica sol was 3 or lower to promote hydrolysis. A catalyzed silica sol was prepared by adding a base catalyst solution (10 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 0.5:1 (catalyzed silica sol: fiber). The fibers, which had passed through the impregnation tank and were infiltrated with the catalyzed sol, were gelled for about 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°C. Thereafter, a solution (2.4 wt%) of diluted ammonia water in ethanol was added to the gelled wet gel composite in an amount of 109% based on the volume of the wet gel composite, and maturation was performed at a temperature of 75°C for 1 hour. A hexamethyldisilazane (HMDS) / ethanol solution (5:95 volume ratio) as a surface modifier was added to the matured wet gel composite in an amount of 90% by volume based on the volume of the wet gel composite, and surface modification was performed at a temperature of 75°C for 4 hours. Thereafter, supercritical drying was performed under the conditions of CO2 150 bar and 70°C to produce an aerogel composite having a density of about 0.170 g / cc.
[0257]
[0258] [Example 4]
[0259] A silica precursor composition was prepared by mixing methyltriethoxysilane (MTES) and TEOS at a molar ratio of 97:3. The silica precursor composition and water were mixed at a molar ratio of 1:10, and ethanol at a weight ratio of 1:2 was added to the silica precursor composition to prepare a silica sol. Hydrochloric acid was added so that the pH of the silica sol was 3 or lower to promote hydrolysis. A catalyzed silica sol was prepared by adding a base catalyst solution (10 wt% NaOH aqueous solution) at 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 at a volume ratio of 0.7:1 (catalyzed silica sol: fiber). The fibers, which had been impregnated with the catalyzed sol after passing through the impregnation tank, were gelled for about 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°C. Thereafter, a solution (2.4 wt%) of diluted ammonia water in ethanol was added to the gelled wet gel composite in an amount of 109% based on the volume of the wet gel composite, and maturation was performed at a temperature of 75°C for 1 hour. A hexamethyldisilazane (HMDS) / ethanol solution (5:95 volume ratio) as a surface modifier was added to the matured wet gel composite in an amount of 90% by volume based on the volume of the wet gel composite, and surface modification was performed at a temperature of 75°C for 4 hours. Thereafter, supercritical drying was performed under the conditions of CO2 150 bar and 70°C to produce an aerogel composite having a density of about 0.190 g / cc.
[0260]
[0261] [Example 5]
[0262] A silica precursor composition was prepared by mixing methyltriethoxysilane (MTES) and TEOS at a molar ratio of 97:3. The silica precursor composition and water were mixed at a molar ratio of 1:10, and ethanol at a weight ratio of 1:2 was added to the silica precursor composition to prepare a silica sol. Hydrochloric acid was added so that the pH of the silica sol was 3 or lower to promote hydrolysis. A catalyzed silica sol was prepared by adding a base catalyst solution (10 wt% NaOH aqueous solution) at 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 at a volume ratio of 0.7:1 (catalyzed silica sol: fiber). The fibers, which had been impregnated with the catalyzed sol after passing through the impregnation tank, were gelled for about 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°C. Thereafter, a solution of 2.4 wt% trimethylethoxysilane (TMES) solution diluted in ethanol was added as a maturation solution in an amount of 109 vol% based on the volume of the wet gel composite, and maturation was performed at a temperature of 75°C 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 maturated wet gel composite, and surface modification was performed at a temperature of 75°C for 4 hours. Thereafter, supercritical drying was performed under the conditions of CO2 150 bar and 70°C to produce an aerogel composite having a density of about 0.211 g / cc.
[0263]
[0264] [Example 6]
[0265] A silica precursor composition was prepared by mixing methyltriethoxysilane (MTES) and TEOS in a molar ratio of 97:3. The silica precursor composition and water were mixed in a molar ratio of 1:10, and ethanol in a weight ratio of 1:2 was added to the silica precursor composition to prepare a silica sol. Hydrochloric acid was added so that the pH of the silica sol was 3 or lower to promote hydrolysis. A catalyzed silica sol was prepared by adding a base catalyst solution (10 wt% NaOH aqueous solution) in a volume ratio of 99:1 to the silica sol. After 33.3 L of the catalyzed sol was filled in an impregnation tank, a fiber (Glass fiber, 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 1:1 (catalyzed silica sol: fiber). The fibers, which had passed through the impregnation tank and were infiltrated with the catalyzed sol, were gelled for about 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°C. Thereafter, a solution of 2.4 wt% trimethylethoxysilane (TMES) solution diluted in ethanol 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°C 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°C for 4 hours. Thereafter, supercritical drying was performed under the conditions of CO2 150 bar and 70°C to produce an aerogel composite having a density of about 0.206 g / cc.
[0266]
[0267] [Example 7]
[0268] 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, acid was added so that the pH of the silica precursor solution became 3 or lower, 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 1:4 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, 3 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 0.7:1 (catalyzed silica sol: fiber). Fibers impregnated with the catalyzed sol through the impregnation tank were passed at a constant speed along a conveyor belt and gelled for approximately 10 minutes. During this time, the ambient temperature above 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 mixture of ethanol and ammonia water (volume ratio of 98:2) was prepared and added to the gelled wet gel composite in an amount 1.6 times the volume of silica sol, and secondary maturation was performed in a 70 ℃ oven for 1 hour. A solution (2 vol%) of trimethylethoxysilane (TMES) diluted in ethanol as a surface modifier was added to the aged wet gel composite 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 2 hours. Afterwards, supercritical drying was performed under the conditions of CO2 150 bar and 70 ℃ to manufacture an aerogel composite with a density of approximately 0.189 g / cc.
[0269]
[0270] [Example 8]
[0271] A silica precursor solution was prepared by mixing tetraethylorthosilicate (TEOS) and water in a molar ratio of 1:4 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 3 or lower, and the solution 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. After filling 33.3 L of the catalyzed sol into an impregnation tank, a fiber (glass fiber mat, 3 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 at a volume ratio of 0.7:1 (catalyzed silica sol: fiber). Fibers impregnated with the catalyzed sol through the impregnation tank were passed at a constant speed along a conveyor belt and gelled for approximately 10 minutes. During this time, the ambient temperature above the conveyor belt was maintained at 25°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, followed by secondary maturation in a 75 ℃ oven for 1 hour. A solution (2 vol%) of trimethylethoxysilane (TMES) diluted in ethanol as a surface modifier was added to the aged wet gel composite, and 90 vol% of the wet gel composite volume was added, followed by surface modification at a temperature of 75 ℃ for 2 hours. Afterwards, supercritical drying was performed under the conditions of CO2 150 bar and 70 ℃ to produce an aerogel composite having a density of approximately 0.192 g / cc.
[0272]
[0273] [Example 9]
[0274] A silica precursor solution was prepared by mixing tetraethyl orthosilicate (TEOS) and water in a molar ratio of 1:4 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 3 or lower, and the solution 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. 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 at a volume ratio of 0.7:1 (catalyzed silica sol: fiber). The fibers, which had passed through the impregnation tank and were infiltrated with the catalyzed sol, were gelled for approximately 10 minutes while passing at a constant speed on a conveyor belt. During this time, the ambient temperature on the conveyor belt was maintained at 35°C. After gelation was completed, the fibers were stabilized at room temperature (25°C) for 10 minutes and then subjected to primary maturation in a 70°C oven for 50 minutes. Subsequently, a solution was prepared by diluting 2.9 wt% methyltriethoxysilane (MTES) in ethanol with a moisture content of 10 wt%, and the solution was added to 109% of the volume of the wet gel composite, followed by secondary maturation in a 75°C oven for 1 hour. Subsequently, supercritical drying was performed at 150 bar of CO2 and 70°C to produce an aerogel composite with a density of approximately 0.204 g / cc.
[0275]
[0276] [Comparative Example 1]
[0277] A silica precursor composition was prepared by adding pre-hydrolyzed TEOS (silica content: 20 wt%, HTEOS), ethanol, and distilled water at a weight ratio of 1:2:0.22 and mixing them. A catalyst composition was prepared by adding ethanol, NaOH (5 wt% aqueous solution), and trimethylethoxysilane (TMES) at a weight ratio of 1:0.3:1 and mixing them. The prepared silica precursor composition and the catalyst composition were mixed at a volume ratio of 9:1 in a reactor to prepare a catalyzed silica sol. A fiber (Glass fiber mat, 10 mm) was passed through the fiber as a substrate to infiltrate the catalyzed sol, and the catalyzed silica sol was impregnated at a volume ratio of 1:1 (catalyzed silica sol: glass fiber mat) relative to the volume of the glass fiber mat, and gelling for about 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 left at room temperature for 24 hours to undergo gelation, maturation, and surface modification. Subsequently, supercritical drying was performed under conditions of CO2 150 bar and 70°C, producing an aerogel composite with a density of approximately 0.206 g / cc.
[0278]
[0279] [Comparative Example 2]
[0280] A silica precursor solution was prepared by mixing tetraethyl orthosilicate (TEOS) and water in a molar ratio of 1:4 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 3 or lower, 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 1:4 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, 10 mm) as a substrate by passing the fiber through it, and the catalyzed silica sol was impregnated in a volume ratio of 0.3:1 to the volume of the glass fiber mat (catalyzed silica sol: glass fiber mat). The fibers, which had been impregnated with the catalyzed sol after passing through the impregnation tank, were gelled for about 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, the gelled wet gel composite was left in a chamber at 70℃ for 24 hours to mature. 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 then surface modification was performed at a temperature of 75℃ for 4 hours. Thereafter, supercritical drying was performed under the conditions of CO2 150 bar and 70℃ to produce an aerogel composite having a density of about 0.142 g / cc.
[0281]
[0282] [Comparative Example 3]
[0283] A silica precursor solution was prepared by mixing tetraethyl orthosilicate (TEOS) and water in a molar ratio of 1:4 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 3 or lower, 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 1:4 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, 3 mm) as a substrate by passing the fiber through it, and the catalyzed silica sol was impregnated in a volume ratio of 0.5:1 to the volume of the glass fiber mat (catalyzed silica sol: glass fiber mat). The fibers, which had passed through the impregnation tank and were infiltrated with the catalyzed sol, were passed at a constant speed on a conveyor belt and gelled at room temperature for about 10 minutes. After gelation, they were stabilized at room temperature (25 ℃) for 10 minutes and then subjected to primary maturation in a 70 ℃ oven for 50 minutes. Afterwards, a mixture of ethanol and ammonia water (volume ratio of 98:2) was prepared for the gelled wet gel composite and added in an amount 1.6 times the volume of the silica sol, followed by secondary maturation in a 70 ℃ oven for 1 hour. Afterwards, supercritical drying was performed under the conditions of CO2 150 bar and 70 ℃ to produce an aerogel composite with a density of about 0.168 g / cc.
[0284]
[0285] [Experimental Example 1] Measurement of distribution by density and pore size
[0286] 1. Density
[0287] 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.
[0288] 2. Volume ratio (%) of effective pores with a pore diameter of 30 nm or less
[0289] 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.
[0290] Classification Density (g / cc) Effective Pore Volume Ratio (%) Example 10.17735.6 Example 20.18731.1 Example 30.17040.2 Example 40.19038.7 Example 50.21133.8 Example 60.20637.2 Example 70.18930.3 Example 80.19237.3 Example 90.20438.1 Comparative Example 10.20622.0 Comparative Example 20.14220.9 Comparative Example 30.16820.1
[0291]
[0292] [Experimental Example 2] Measurement of recovery rate and thermal transmittance after compression of aerogel composites
[0293] 1. Compression recovery rate
[0294] Using the aerogel composites obtained in the Examples and Comparative Examples, specimens measuring 20 cm X 20 cm were prepared. If the width or length of the manufactured aerogel composite is less than 20 cm, two or more specimens may be arranged in parallel adjacent to each other so that the specimens measure 20 cm X 20 cm, and then measurements may be performed on these specimens. Each prepared specimen was pressed for 10 minutes under each pressure condition using the QM900A-15T press equipment from QMESYS. The thickness of the aerogel composite was measured using the HFM436 equipment from Netzsch before and after pressing, 1 hour later, and the compression recovery rate was calculated according to Equation 1 below, and the results are shown in Table 2 below. However, the pressure value shown in Table 2 below is the value of the pressure applied per unit area of the specimen, and means the value obtained by dividing the cylinder area of the press equipment by the set pressure value as in Equation 2 below, and dividing by the area of the specimen. 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.
[0295] [Formula 1]
[0296] Compression recovery rate (%) = {(cross-sectional thickness of aerogel composite after compression) / (cross-sectional thickness of aerogel composite before compression)} X 100
[0297] [Formula 2]
[0298] 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 ))
[0299] 2. Evaluation of changes in thermal transmittance after compression (1)
[0300] 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 3 below.
[0301] In addition, in order to confirm the change in thermal transmittance after compression, the average value (b) of the thermal transmittance measured after compression at a pressure of 9 bar to 30 bar was calculated, and as in Equation 3 below, the difference between the thermal transmittance (a) measured after compression at a pressure of 9 bar to 30 bar and the average value (b), and the value A obtained by dividing the difference by the average value (b) of the thermal transmittance were calculated, and the results are shown in Table 4.
[0302] [Formula 3]
[0303] (Thermal transmittance after compression (a) - Average value of thermal transmittance after compression (b)) = (Average value of thermal transmittance after compression (b)) XA
[0304] Each result value shown in Tables 2 to 4 below is rounded to the third decimal place and displayed to the second decimal place.
[0305] Classification Pressure Conditions Thickness after compression (mm) Compression recovery rate (%) Example 1 - 10.4 - 3 bar, 10 min 9.18 7.509 bar, 10 min 8.27 8.85 15 bar, 10 min 8.07 6.9 224 bar, 10 min 8.17 7.88 30 bar, 10 min 7.9 7 5.96 33 bar, 10 min 8.07 6.9 2 Example 2 - 8.6 - 3 bar, 10 min 8.29 5.359 bar, 10 min 8.09 3.02 15 bar, 10 min 7.99 1.86 24 bar, 10 min 7.78 9.53 30 bar, 10 min 7.48 6.05 33 bar, 10 min 6.98 0.23 Example 3 - 3.6 - 3 bar, 10min3.494.449bar, 10min3.391.6715bar, 10min3.288.8924bar, 10min3.288.8930bar, 10min3.186.1133bar, 10min3.083.33Example 4-4.6-3bar, 10min4.495.659bar, 10min4.495.6515bar, 10min4.291.3024bar, 10min4.189.1330bar, 10min4.086.9633bar, 10min3.984.78Example 5-4.7-3bar, 10min4.697.879bar, 10min4.289.3615bar, 10min4.289.3624bar, 10min4.187.2330bar, 10min4.187.2333bar, 10min4.085.11Example 6-5.0-3bar, 10min4.692.009bar, 10min3.978.0015bar, 10min3.774.0024bar, 10min3.774.0030bar, 10min3.672.0033bar, 10min3.672.00Example 7-2.7-3bar, 10min2.696.309bar, 10min2.592.5915bar, 10min2.592.5924bar, 10min2.488.8930bar, 10min2.385.1933bar, 10min2.385.19Example 8-2.7-3bar, 10min2.7100.009bar, 10min2.696.3015bar, 10min2.696.3024bar, 10min2.592.5930bar, 10min2.592.5933bar, 10min2.488.89Example 9-3.9100.003bar, 10min3.589.749bar, 10min3.179.4915bar, 10min3.076.9224bar, 10min2.974.3630bar, 10min2.974.3633bar, 10min2.871.79Comparative example 1-9.5-3bar, 10min6.063.169bar, 10min5.052.6315bar, 10min4.850.5324bar, 10min4.749.4730bar, 10min4.951.5833bar, 10min5.052.63Comparative example 2-6.3-3bar, 10min4.469.849bar, 10min3.758.7315bar, 10min3.352.3824bar, 10min3.149.2130bar, 10min2.946.0333bar, 10min2.946.03Comparative example 3-2.6-3bar, 10min1.765.389bar, 10min1.557.6915bar, 10min1.453.8524bar, 10min1.142.3130bar, 10min1.038.4633bar, 10min0.934.62.
[0306] Thermal transmittance under pressure conditions (W / m) 2K) Increase rate of heat transfer coefficient (times) Example 1 - 2.26 - 3 bar, 10 min 2.59 1.159 bar, 10 min 2.89 1.28 15 bar, 10 min 3.05 1.35 24 bar, 10 min 3.09 1.37 30 bar, 10 min 3.19 1.4 133 bar, 10 min 3.24 1.43 Example 2 - 2.4 2 - 3 bar, 10 min 2.55 1.059 bar, 10 min 2.66 1.10 15 bar, 10 min 2.75 1.14 24 bar, 10 min 2.87 1.19 30 bar, 10 min 3.04 1.26 33 bar, 10 min 3.29 1.36 Example 3 - 6.4 2 - 3 bar, 10min6.851.079bar, 10min7.181.1215bar, 10min7.441.1624bar, 10min7.471.1630bar, 10min7.741.2133bar, 10min8.071.26Example 4-4.30-3bar, 10min4.551.069bar, 10min4.661.0815bar, 10min5.141.1924bar, 10min5.291.2330bar, 10min5.531.2833bar, 10min5.721.33Example 5-4.26-3bar, 10min4.431.049bar, 10min4.931.1615bar, 10min4.981.1724bar, 10min5.121.2030bar, 10min5.151.2133bar, 10min5.331.25Example 6-3.16-3bar, 10min3.481.109bar, 10min4.491.4215bar, 10min4.921.5624bar, 10min4.891.5530bar, 10min5.001.5833bar, 10min5.391.71Example 7-6.93-3bar, 10min7.271.059bar, 10min7.601.1015bar, 10min7.601.1024bar, 10min7.961.1530bar, 10min8.301.2033bar, 10min8.391.21Example 8-8.85-3bar, 10min8.891.009bar, 10min9.231.0415bar, 10min9.271.0524bar, 10min9.881.1230bar, 10min10.001.1333bar, 10min10.461.18Example 9-6.441.003bar, 10min6.751.059bar, 10min7.731.2015bar, 10min8.021.2524bar, 10min8.291.2930bar, 10min8.481.3233bar, 10min8.891.38Comparative example 1-1.84-3bar, 10min2.731.489bar, 10min3.441.8715bar, 10min4.382.3824bar, 10min5.643.0730bar, 10min5.573.0333bar, 10min5.653.07Comparative Example 2-3.89-3bar, 10min6.091.579bar, 10min8.512.1915bar, 10min9.972.5624bar, 10min10.942.8130bar, 10min11.763.0233bar, 10min11.833.04Comparative Example 3-9.38-3bar, 10min16.291.749bar, 10min20.732.2115bar, 10min23.002.4524bar, 10min29.553.1530bar, 10min33.103.5333bar, 10min36.893.93.
[0307] Thermal transmittance under pressure conditions (W / m) 2 K) Average thermal transmittance after compression (W / m) 2 K) Deviation of heat transmittance after compression (W / m) 2K) Deviation of heat transmittance after compression / Average of heat transmittance (A) Example 19 bar, 10 min 2.89 3.05-0.16-0.05 15 bar, 10 min 3.05 0.00 0.00 24 bar, 10 min 3.09 0.04 0.01 30 bar, 10 min 3.19 0.14 0.05 Example 29 bar, 10 min 2.66 2.83-0.17-0.06 15 bar, 10 min 2.75-0.08-0.03 24 bar, 10 min 2.87 0.04 0.01 30 bar, 10 min 3.04 0.21 0.07 Example 39 bar, 10 min 7.18 7.46-0.28-0.04 15 bar, 10min7.44-0.020.0024bar, 10min7.470.010.0030bar, 10min7.740.280.04Example 49bar, 10min4.665.15-0.50-0.1015bar, 10min5.14-0.010.0024bar, 10min5.290.140.0330bar, 10min5.530.370.07Example 59bar, 10min4.935.04-0.11-0.0215bar, 10min4.98-0.07-0.0124bar, 10min5.120.080.0230bar, 10min5.150.100.02Example 69bar, 10min4.494.83-0.34-0.0715bar, 10min4.920.090.0224bar, 10min4.890.060.0130bar, 10min5.000.170.04Example 79bar, 10min7.607.87-0.27-0.0315bar, 10min7.60-0.27-0.0324bar, 10min7.960.090.0130bar, 10min8.300.440.06Example 89bar, 10min9.239.60-0.36-0.0415bar, 10min9.27-0.33-0.0324bar, 10min9.880.290.0330bar, 10min10.000.410.04Example 99bar, 10min7.738.13-0.40-0.0515bar, 10min8.02-0.11-0.0124bar, 10min8.290.160.0230bar, 10min8.480.350.04 Comparative Example 19 bar, 10 min 3.44 4.76-1.32-0.28 15 bar, 10 min 4.38-0.38-0.08 24 bar, 10 min 5.64 0.88 0.19 30 bar, 10 min 5.57 0.81 0.17 Comparative Example 29 bar, 10 min 8.51 10.29-1.78-0.17 15 bar, 10 min 9.97-0.32-0.03 24 bar, 10 min 10.94 0.64 0.06 30 bar, 10 min 11.76 1.46 0.14 Comparative Example 39 bar, 10 min 20.73 26.59-5.86-0.22 15 bar, 10min23.00-3.59-0.1424bar, 10min29.552.950.1130bar, 10min33.106.510.24.
[0308] 3. Evaluation of changes in thermal transmittance after compression (2)
[0309] In addition, in order to confirm the change in thermal transmittance after compression in the range of 3 bar to 24 bar, the average value (b) of the thermal transmittance measured after compression at pressures of 3 bar, 9 bar and 24 bar was calculated, and as in Equation 3, the difference between the thermal transmittance (a) measured after compression at pressures of 3 bar, 9 bar or 24 bar and the average value (b), and the value A obtained by dividing the difference by the average value (b) of the thermal transmittance were calculated, and the results are shown in Table 5. Each result value shown in Table 5 below was rounded to the third decimal place and shown to the second decimal place.
[0310] Thermal transmittance (a) after compression under pressure conditions (W / m) 2 K) Average thermal transmittance after compression (b) (W / m 2 K) Deviation of thermal transmittances after compression (ab) (W / m 2K) Deviation of heat transmittance after compression / Average of heat transmittance (ab / b = A)Example 13 bar, 10 min 2.59 2.86-0.27-0.099 bar, 10 min 2.89 0.03 0.01 24 bar, 10 min 3.09 0.23 0.08Example 23 bar, 10 min 2.55 2.69-0.14-0.059 bar, 10 min 2.66-0.03-0.01 24 bar, 10 min 2.87 0.18 0.07Example 33 bar, 10 min 6.85 7.17-0.32-0.049 bar, 10 min 7.18 0.01 0.00 24 bar, 10 min 7.47 0.30 0.04Example 43 bar, 10min4.554.83-0.28-0.069bar, 10min4.66-0.17-0.0424bar, 10min5.290.460.10Example 53bar, 10min4.434.83-0.40-0.089bar, 10min4.930.100.0224bar, 10min5.120.290.06Example 63bar, 10min3.484.29-0.81-0.199bar, 10min4.490.200.0524bar, 10min4.890.600.14Example 73bar, 10min7.277.61-0.34-0.049bar, 10min7.60-0.010.0024bar, 10min7.960.350.05Example 83bar, 10min8.899.33-0.44-0.059bar, 10min9.23-0.10-0.0124bar, 10min9.880.550.06Example 93bar, 10min6.757.59-0.84-0.119bar, 10min7.730.140.0224bar, 10min8.290.700.09Comparative Example 13bar, 10min2.733.94-1.21-0.319bar, 10min3.44-0.50-0.1324bar, 10min5.641.700.43Comparative example 23bar, 10min6.098.51-2.42-0.289bar, 10min8.510.000.0024bar, 10min10.942.430.29Comparative example 33bar, 10min16.2922.19-5.90-0.279bar, 10min20.73-1.46-0.0724bar, 10min29.557.360.33.
[0311] 4. Evaluation of changes in thermal transmittance before and after compression
[0312] Additionally, in order to confirm the change in the thermal transmittance before and after compression, the average value (d) 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 (c) measured before and after compression at pressures of 0 bar, 3 bar, 9 bar and 24 bar and the average value (d) of these thermal transmittances, and the value D, which is the difference divided by the average value (d) of the thermal transmittances, were calculated, and the results are shown in Table 6. Each result value shown in Table 6 below was rounded to the third decimal place and shown to the second decimal place.
[0313] [Formula 4]
[0314] {(Thermal transmittance before and after compression (c)) - (Average of thermal transmittances before and after compression (d))} = (Average of thermal transmittances before and after compression (d)) XD
[0315] Thermal transmittance (c) before and after compression (W / m) 2 K) Average values of thermal transmittances before and after compression (d) (W / m 2 K) Deviation of thermal transmittance before and after compression (cd) (W / m 2K) Deviation of heat transmittance before and after compression / Average of heat transmittance (cd / d = D)Example 10 bar, 10 min 2.26 2.71-0.45-0.173 bar, 10 min 2.59-0.12-0.049 bar, 10 min 2.89 0.18 0.07 24 bar, 10 min 3.09 0.38 0.14Example 20 bar, 10 min 2.42 2.63-0.21-0.083 bar, 10 min 2.55-0.08-0.039 bar, 10 min 2.66 0.03 0.01 24 bar, 10 min 2.87 0.24 0.09Example 30 bar, 10 min 6.42 6.98-0.56-0.083 bar, 10min6.85-0.13-0.029bar, 10min7.180.200.0324bar, 10min7.470.490.07Example 40bar, 10min4.304.70-0.40-0.083bar, 10min4.55-0.15-0.039bar, 10min4.66-0.04-0.0124bar, 10min5.290.590.13Example 50bar, 10min4.264.69-0.43-0.093bar, 10min4.43-0.26-0.059bar, 10min4.930.240.0524bar, 10min5.120.430.09Example 60bar, 10min3.164.01-0.85-0.213bar, 10min3.48-0.53-0.139bar, 10min4.490.480.1224bar, 10min4.890.880.22Example 70bar, 10min6.937.44-0.51-0.073bar, 10min7.27-0.17-0.029bar, 10min7.600.160.0224bar, 10min7.960.520.07Example 80bar, 10min8.859.21-0.36-0.043bar, 10min8.89-0.32-0.039bar, 10min9.230.020.0024bar, 10min9.880.670.07Example 90bar, 10min6.447.30-0.86-0.123bar, 10min6.75-0.55-0.089bar, 10min7.730.430.0624bar, 10min8.290.990.14Comparative example 10 bar, 10 min 1.84 3.41-1.57-0.463 bar, 10 min 2.73-0.68-0.209 bar, 10 min 3.44 0.03 0.01 24 bar, 10 min 5.64 2.23 0.65Comparative example 20 bar, 10 min 3.89 7.36-3.47-0.473 bar, 10 min 6.09-1.27-0.179 bar, 10 min 8.51 1.15 0.16 24 bar, 10 min 10.94 3.58 0.49Comparative example 30 bar, 10 min 9.38 18.99-9.61-0.513 bar, 10 min 16.29-2.70-0.149 bar, 10min20.731.740.0924bar, 10min33.1010.560.56.
[0316] As shown in Tables 2 to 6 above, it was confirmed that the aerogel composites of Examples 1 to 9 manufactured according to the present invention had higher compression recovery rates than the aerogel composites of Comparative Examples 1 to 3. In addition, it was confirmed that the aerogel composites of Examples 1 to 9 according to the present invention had a smaller increase in thermal transmittance than before compression even after compression, and that even when compressed at various pressure values from low to high pressure, the change in thermal transmittance was small and the insulation performance was maintained at an excellent level.
[0317] From these results, it was confirmed that the aerogel composite of the present invention has excellent elastic flexibility and strength of pores, and thus has excellent resilience even after high-pressure compression, and thus prevents rapid deterioration of insulation performance due to destruction of pores, especially destruction of pores of size less than 30 nm, and maintains excellent insulation performance even after compression.
[0318]
[0319] 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.
[0320]
[0321] The present invention relates to an aerogel composite that maintains excellent thermal insulation properties without significant degradation even when compressed by external pressure, 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 one or more pores, An aerogel composite, wherein when compressed by applying transverse pressures of 24 bar, 30 bar, and 33 bar, the thermal transmittance after compression is 3 times or less compared to the thermal transmittance before compression.
2. In paragraph 1, An aerogel composite, wherein when the aerogel composite is compressed by applying transverse pressures of 24 bar, 30 bar, and 33 bar, respectively, the thermal transmittance after compression is more than 1 time and less than 3 times the thermal transmittance before compression.
3. In paragraph 1, An aerogel composite, wherein the thermal transmittance after compression is 1.45 times or less than the thermal transmittance before compression when a pressure of 3 bar is applied transversely to the aerogel composite.
4. In paragraph 3, An aerogel composite, wherein when a pressure of 3 bar is applied transversely to the above aerogel composite, the thermal transmittance after compression is equal to or 1.45 times or less than the thermal transmittance before compression.
5. In paragraph 1, An aerogel composite, wherein the thermal transmittance after compression is 1.85 times or less than the thermal transmittance before compression when a pressure of 9 bar is applied transversely to the aerogel composite.
6. In paragraph 1, An aerogel composite, wherein when a pressure of 9 bar is applied transversely to the above aerogel composite, the thermal transmittance after compression is equal to or 1.85 times or less than the thermal transmittance before compression.
7. In paragraph 1, An aerogel composite, wherein the thermal transmittance after compression is 2.35 times or less than the thermal transmittance before compression when a pressure of 15 bar is applied transversely to the aerogel composite.
8. In paragraph 7, An aerogel composite, wherein the thermal transmittance after compression is the same as or 2.35 times or less than the thermal transmittance before compression when a pressure of 15 bar is applied transversely to the aerogel composite.
9. In paragraph 1, An aerogel composite having a compression recovery rate expressed by Equation 1 below of 60% or more when pressures of 9 bar, 15 bar, 24 bar, 30 bar and 33 bar are applied transversely to the aerogel composite: [Formula 1] Compression recovery rate (%) = {(cross-sectional thickness of aerogel composite after compression) / (cross-sectional thickness of aerogel composite before compression)} X 100 10. In paragraph 9, An aerogel composite having a compression recovery rate expressed by Equation 1 of 60% or more and 99% or less when pressures of 9 bar, 15 bar, 24 bar, 30 bar and 33 bar are applied transversely to the aerogel composite.
11. In paragraph 1, The thermal transmittance obtained after compression at pressures of 9 bar, 15 bar, 24 bar and 30 bar for the above aerogel composite satisfies the following equation 3: [Formula 3] (Thermal transmittance after compression (a) - Average value of thermal transmittance after compression (b)) = (Average value of thermal transmittance after compression (b)) XA In the above equation 3, the thermal transmittance after compression (a) means the thermal transmittance obtained after compression at any one of the pressure values of 9 bar, 15 bar, 24 bar, and 30 bar in the transverse direction for the aerogel composite, The average value of the thermal transmittances after compression (b) refers to the average value of the thermal transmittances obtained after compression at pressure values of 9 bar, 15 bar, 24 bar and 30 bar in the transverse direction for the aerogel composite. The above A is a rational number between -0.15 and +0.
15.
12. In paragraph 1, When the above aerogel composite was compressed by applying transverse pressures of 3 bar, 9 bar and 24 bar respectively, the thermal transmittance after compression was 1.8 times or less compared to the thermal transmittance before compression. 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 (c)) - (Average of thermal transmittances before and after compression (d))} = (Average of thermal transmittances before and after compression (d)) XD In the above equation 4, the thermal transmittance before and after compression (c) is the thermal transmittance obtained after compression at 0 bar, 3 bar, 9 bar or 24 bar in the transverse direction for the aerogel composite, and the average value of the thermal transmittances before and after compression (d) means the average value of the thermal transmittances obtained after compression at pressure values of 0 bar, 3 bar, 9 bar and 24 bar in the transverse direction for the aerogel composite, The above D is a rational number between -0.25 and +0.
25.
13. In paragraph 1, For the above aerogel composite, the rate of change (B) of the thermal transmittance after compression per unit applied pressure, expressed by the following equation 5, is a rational number of - 0.10 to + 0.10, [Formula 5] B = (thermal transmittance after compression at pressure x - thermal transmittance after compression at pressure y) / (x - y) In the above equation 5, x and y are each independently one of 9 bar, 15 bar, and 24 bar pressure values (unit: bar), and are different pressure values.
14. 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.
15. In paragraph 13, The above aerogel is an aerogel composite comprising pores having a pore diameter of 0.1 nm or more and 30 nm or less, which account for 30% or more and 45% or less of the pore volume of the skeletal structure.
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 is an aerogel composite, which is a silica aerogel.
18. In paragraph 1, An aerogel composite, wherein the thermal transmittance after compression is measured 1 hour after compression.
19. An insulating member comprising an aerogel composite according to any one of claims 1 to 18.
20. In paragraph 19, 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.
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