CN114195545A - High-temperature-resistant low-heat-conductivity core-shell-structure nano aluminum heat insulation material and preparation method and application thereof - Google Patents
High-temperature-resistant low-heat-conductivity core-shell-structure nano aluminum heat insulation material and preparation method and application thereof Download PDFInfo
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- 239000012774 insulation material Substances 0.000 title claims abstract description 54
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 46
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 172
- 239000011858 nanopowder Substances 0.000 claims abstract description 107
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 102
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 86
- 239000011258 core-shell material Substances 0.000 claims abstract description 85
- 238000003756 stirring Methods 0.000 claims abstract description 52
- 238000001035 drying Methods 0.000 claims abstract description 50
- 238000010438 heat treatment Methods 0.000 claims abstract description 44
- 238000002156 mixing Methods 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims description 56
- 239000010410 layer Substances 0.000 claims description 52
- 239000012792 core layer Substances 0.000 claims description 51
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 38
- 239000000843 powder Substances 0.000 claims description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 21
- 229920000053 polysorbate 80 Polymers 0.000 claims description 21
- 239000003365 glass fiber Substances 0.000 claims description 20
- 238000009413 insulation Methods 0.000 claims description 20
- 229910052810 boron oxide Inorganic materials 0.000 claims description 19
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 19
- 239000000835 fiber Substances 0.000 claims description 17
- 238000001354 calcination Methods 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 16
- 239000011230 binding agent Substances 0.000 claims description 13
- 239000012783 reinforcing fiber Substances 0.000 claims description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 230000006835 compression Effects 0.000 claims description 6
- 238000007906 compression Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 229910052863 mullite Inorganic materials 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 34
- 230000000694 effects Effects 0.000 abstract description 7
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 238000003980 solgel method Methods 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 16
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 15
- 230000001965 increasing effect Effects 0.000 description 14
- 229910052751 metal Inorganic materials 0.000 description 14
- 239000002184 metal Substances 0.000 description 14
- 239000011810 insulating material Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 239000003605 opacifier Substances 0.000 description 6
- 238000012546 transfer Methods 0.000 description 6
- 230000005855 radiation Effects 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 239000007790 solid phase Substances 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 238000010907 mechanical stirring Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000008033 biological extinction Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000012784 inorganic fiber Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- C04B35/628—Coating the powders or the macroscopic reinforcing agents
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Abstract
The invention discloses a high-temperature-resistant low-heat-conductivity core-shell structure nano aluminum heat insulation material, and a preparation method and application thereof, wherein the method comprises the following steps: preparing core-shell structure nano powder by adopting a sol-gel method; mixing and stirring the materials uniformly; pressure forming; drying; and (4) high-temperature heat treatment. According to the invention, by preparing the alumina/titanium oxide core-shell structure nano-particles, the low heat conduction performance of alumina and the light shielding performance of titanium oxide are comprehensively utilized, the heat conduction performance of the material is effectively reduced, the heat conduction coefficient of the material is reduced, and the actual application effect of the material is improved.
Description
Technical Field
The invention relates to the field of nano powder-based heat insulation materials, in particular to a high-temperature-resistant low-heat-conductivity core-shell structure nano aluminum heat insulation material and a preparation method and application thereof.
Background
The nano powder-based heat insulation material is a heat insulation material with a porous structure formed by stacking and pressing nano powder and fiber in a composite mode, has excellent heat insulation performance, and is a heat insulation material with great application potential.
The nanometer powder-based heat insulation material is mostly prepared from nanometer powder, an opacifier and inorganic fibers. The nanometer powder is used as a heat insulation main body, the opacifier has larger reflectivity and can reduce radiation heat transfer, so that the heat conductivity coefficient is further reduced, and the inorganic fiber is used for enhancing the strength of the material. Common opacifiers are titanium oxide, silicon carbide, zirconium oxide, carbon black and the like. However, the thermal conductivity of the opacifier is generally greater than that of the nanopowder, and increasing the amount of opacifier decreases radiative heat transfer but increases the amount of solid phase heat transfer. On the other hand, the nano powder-based heat insulating material is generally formed by dry powder high-pressure pressing, is reinforced by ceramic fibers, and is generally not high in strength.
Disclosure of Invention
In view of the above, the main objective of the present invention is to provide a high temperature resistant low thermal conductivity core-shell structure nano aluminum thermal insulation material, and a preparation method and an application thereof, and the technical problem to be solved is to prepare alumina/titanium oxide core-shell structure nano particles, comprehensively utilize the low thermal conductivity of alumina and the light shielding performance of titanium oxide, effectively reduce the thermal conductivity of the material, and reduce the thermal conductivity coefficient of the material.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme. The preparation method of the high-temperature-resistant low-heat-conductivity core-shell structure nano aluminum heat insulation material provided by the invention comprises the following steps of:
1) fully and uniformly mixing the raw materials of the alumina nano powder, the core-shell structure nano powder, the reinforced fiber and the inorganic binder;
2) pressure forming: carrying out pressure forming on the mixture obtained in the step 1);
3) and (3) drying: drying the block obtained in step 2) at 50-100 ℃;
4) and (3) heat treatment: carrying out high-temperature heat treatment on the block obtained in the step 3) at the temperature of 500-700 ℃, and then cooling to room temperature.
Preferably, in the preparation method of the high-temperature-resistant low-thermal-conductivity core-shell-structure nano aluminum thermal insulation material, in step 1), the raw materials comprise, by mass: 60-68% of alumina nano powder; 18-25% of core-shell structure nano powder; 8-10% of reinforcing fiber; 4-6% of inorganic binder.
Preferably, in the preparation method of the high-temperature-resistant low-thermal-conductivity core-shell structure nano aluminum thermal insulation material, in the step 1), the core-shell structure nano powder is alumina/titania core-shell structure nano powder; the alumina/titanium oxide core-shell structure nano powder comprises core-layer alumina and shell-layer titanium oxide coated on the core-layer alumina, wherein the grain diameter of the core-layer alumina is 30nm, and the thickness of the shell-layer titanium oxide is 5-8 nm.
Preferably, in the preparation method of the high-temperature-resistant low-thermal-conductivity core-shell-structure nano aluminum thermal insulation material, in step 1), the mass ratio of the core-layer aluminum oxide to the shell-layer titanium oxide is 1: (2-3).
Preferably, in the preparation method of the high-temperature-resistant low-thermal-conductivity core-shell-structure nano aluminum thermal insulation material, in the step 1), the molar ratio of titanium to aluminum in the alumina/titanium oxide core-shell-structure nano powder is 0.7-1.1.
Preferably, in the preparation method of the high-temperature-resistant low-thermal-conductivity core-shell-structure nano aluminum thermal insulation material, in step 1), the alumina/titania core-shell-structure nano powder is prepared by the following steps:
mixing and stirring the alumina nano powder and absolute ethyl alcohol for 0.5-1 hour until the mixture is uniform, adding Tween 80 serving as a surfactant into the solution, stirring and stirring the mixture for 0.5-1 hour until the mixture is uniform again, adding titanium isopropoxide into the solution, stirring and reacting the mixture for 1-2 hours to obtain gel, filtering the gel, drying the product at the temperature of 100-140 ℃ for 6-8 hours, and calcining the product in a muffle furnace at the temperature of 500-600 ℃ for 3-4 hours.
Preferably, in the preparation method of the high-temperature-resistant low-thermal-conductivity core-shell-structure nano aluminum thermal insulation material, the mass ratio of the alumina nano powder to the absolute ethyl alcohol is 1: (40-50).
Preferably, in the preparation method of the high-temperature-resistant low-thermal-conductivity core-shell-structure nano aluminum thermal insulation material, the mass ratio of the tween 80 to the absolute ethyl alcohol is (1-1.5): 1.
Preferably, in the preparation method of the high-temperature-resistant low-thermal-conductivity core-shell-structure nano aluminum thermal insulation material, the mass ratio of the titanium isopropoxide to the alumina nano powder is (2-3): 1.
Preferably, in the preparation method of the high-temperature-resistant low-thermal-conductivity core-shell-structure nano aluminum thermal insulation material, in step 1), the reinforcing fiber is at least one selected from alumina fiber, mullite fiber, alumina silicate fiber, glass fiber and zirconia fiber.
Preferably, in the preparation method of the high-temperature-resistant low-thermal-conductivity core-shell-structure nano aluminum heat insulation material, in step 1), the inorganic binder is selected from boron oxide powder and low-melting-point glass powder.
Preferably, in the preparation method of the high-temperature-resistant low-thermal-conductivity core-shell-structure nano aluminum thermal insulation material, in the step 2), the forming pressure is 1-60MPa, and the dwell time is more than 1 hour, and in the preparation method of the high-temperature-resistant low-thermal-conductivity core-shell-structure nano aluminum thermal insulation material, in the step 3), the drying temperature is 50-100 ℃, and the drying time is more than 12 hours.
Preferably, in the preparation method of the high-temperature-resistant low-thermal-conductivity core-shell-structure nano aluminum thermal insulation material, in the step 4), the heat treatment temperature is 500-700 ℃, and the heat treatment time is more than 4 hours.
The purpose of the invention and the technical problem to be solved can be realized by adopting the following technical scheme. According to the high-temperature-resistant low-heat-conductivity core-shell-structure nano aluminum heat insulation material provided by the invention, the compression strength of the high-temperature-resistant low-heat-conductivity core-shell-structure nano aluminum heat insulation material is 1.38MPa to 1.51MPa, and the density of the high-temperature-resistant low-heat-conductivity core-shell-structure nano aluminum heat insulation material is 0.24 g/cm to 0.28g/cm3The porosity is 89.2% -91.4%, the thermal conductivity at 25 ℃ is 0.018W/mK-0.022W/mK, the thermal conductivity at 400 ℃ is 0.025W/mK-0.030W/mK, the thermal conductivity at 800 ℃ is 0.036W/mK-0.039W/mK, and the thermal conductivity at 1200 ℃ is 0.041W/mK-0.044W/mK.
The purpose of the invention and the technical problem to be solved can be realized by adopting the following technical scheme. According to the heat insulation structure provided by the invention, the heat insulation structure comprises a heat insulation layer, and the heat insulation layer is composed of the high-temperature-resistant low-heat-conduction core-shell structure nano aluminum heat insulation material.
The purpose of the invention and the technical problem to be solved can be realized by adopting the following technical scheme. According to the high-temperature hearth provided by the invention, the high-temperature hearth comprises the heat insulation structure.
The purpose of the invention and the technical problem to be solved can be realized by adopting the following technical scheme. According to the building wall provided by the invention, the building wall comprises the heat insulation structure.
By the technical scheme, the invention at least has the following advantages:
the invention prepares the alumina/titanium oxide core-shell structure nano powder by carrying out surface treatment on the alumina nano powder, effectively utilizes the low heat conduction of alumina and the shading effect of titanium oxide, and further reduces the heat conduction coefficient of the material.
The invention prepares the alumina/titanium oxide core-shell structure nano powder, the core layer alumina has lower heat conductivity coefficient and is a common heat preservation and insulation material, the shell layer titanium oxide is a common opacifier and can absorb or scatter the infrared radiation with the wavelength of 3-8 mu m, and has stronger shielding effect on the infrared radiation heat transfer, thereby reducing the radiation heat transfer; the introduction of the core-shell structure can increase the proportion of alumina, reduce the usage amount of titanium oxide, increase the surface area of the titanium oxide and further reduce the heat conductivity coefficient of the material. In addition, the low-melting-point inorganic binder is added to form inorganic binding on a microenvironment, so that the strength of the material is improved.
The high-temperature-resistant low-heat-conduction core-shell structure nano aluminum heat insulation material has the compression strength of 1.38MPa to 1.51MPa and the density of 0.24 g/cm to 0.28g/cm3The porosity is 89.2% -91.4%, the thermal conductivity at 25 ℃ is 0.018W/mK-0.022W/mK, the thermal conductivity at 400 ℃ is 0.025W/mK-0.030W/mK, the thermal conductivity at 800 ℃ is 0.036W/mK-0.039W/mK, and the thermal conductivity at 1200 ℃ is 0.041W/mK-0.044W/mK.
The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a detailed description of the preferred embodiments of the present invention.
Detailed Description
To further illustrate the technical means and effects adopted by the present invention to achieve the predetermined objects, the following detailed description will be given to specific embodiments, structures, characteristics and effects of the high temperature resistant low thermal conductivity core-shell structure nano aluminum thermal insulation material, the preparation method thereof and the application thereof according to the present invention with reference to the preferred embodiments.
Unless otherwise specified, the following materials, reagents and the like are commercially available products well known to those skilled in the art; unless otherwise specified, all methods are well known in the art. Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. The following procedures or conditions, which are not specifically mentioned, may be performed according to the procedures or conditions of the conventional experimental procedures described in the literature in the art.
The preparation method of the high-temperature-resistant low-heat-conductivity core-shell-structure nano aluminum heat insulation material according to the embodiment of the invention comprises the following steps:
1) fully and uniformly mixing the raw material core-shell structure nano powder, the alumina nano powder, the reinforced fiber and the inorganic binder;
2) pressure forming: carrying out pressure forming on the mixture obtained in the step 1);
3) and (3) drying: drying the block obtained in step 2) at 50-100 ℃;
4) and (3) heat treatment: carrying out high-temperature heat treatment on the block obtained in the step 3) at the temperature of 500-700 ℃, and then cooling to room temperature.
In some embodiments of the present invention, in step 1), the raw materials comprise, by mass: 60-68% of alumina nano powder; 18-25% of core-shell structure nano powder; 8-10% of reinforcing fiber; 4-6% of inorganic binder; within this range, the heat insulating material has a low thermal conductivity and at the same time has high strength. If the content of the alumina nano powder is lower than 60 percent, the heat conductivity coefficient of the heat-insulating material is increased; if the content of the alumina nano powder is higher than 68%, the strength of the heat-insulating material is reduced. The content of the core-shell structure nano powder is lower than 18% or higher than 25%, which can cause the heat conductivity coefficient of the heat-insulating material to be increased. If the content of the reinforcing fibers and the inorganic binder is lower than the lower limit, the strength of the heat-insulating material is too low; above the upper limit, the thermal conductivity of the insulation material increases.
In some embodiments of the present invention, in step 1), the core-shell structure nanopowder is an alumina/titania core-shell structure nanopowder; the alumina/titanium oxide core-shell structure nano powder comprises core-layer alumina and shell-layer titanium oxide coated on the core-layer alumina, wherein the grain diameter of the core-layer alumina is 30nm, and the thickness of the shell-layer titanium oxide is 5-8 nm. The 30nm alumina is selected, and a micro-mesoporous structure can be formed after high-pressure compression, so that the heat-insulating material has a low heat conductivity coefficient. If the particle size of the alumina is larger than 30nm, the thermal conductivity of the heat-insulating material is increased. The thickness of the shell layer titanium oxide is selected to be 5-8nm, so that the extinction performance of the titanium oxide can be utilized, and the low heat conduction characteristic of the aluminum oxide can be utilized. If the thickness of the shell layer is less than 5nm, the shell layer is difficult to completely coat the aluminum oxide; if the thickness of the shell layer is more than 8nm, the thermal conductivity of the heat-insulating material is increased.
In some embodiments of the present invention, in step 1), the mass ratio of the core-layer alumina to the shell-layer titania is 1: (2-3). This is to satisfy the requirement that the thickness of the shell layer titanium oxide is 5 to 8 nm.
In some embodiments of the present invention, in step 1), a molar ratio of titanium to aluminum in the alumina/titania core-shell structured nanopowder is 0.7-1.1. Thus, the thickness of the shell titanium oxide can be 5-8 nm.
In some embodiments of the present invention, in step 1), the alumina/titania core-shell structure nanopowder is prepared by the following steps:
mixing and stirring the alumina nano powder and absolute ethyl alcohol for 0.5-1 hour until the mixture is uniform, adding Tween 80 serving as a surfactant into the solution, stirring and stirring the mixture for 0.5-1 hour until the mixture is uniform again, adding titanium isopropoxide into the solution, stirring and reacting the mixture for 1-2 hours to obtain gel, filtering the gel, drying the product at the temperature of 100-140 ℃ for 6-8 hours, and calcining the product in a muffle furnace at the temperature of 500-600 ℃ for 3-4 hours.
In some embodiments of the present invention, the mass ratio of the alumina nanopowder to the absolute ethyl alcohol is 1: (40-50), the powder has better dispersibility. If the mass ratio of the two is less than 1:50, and the using amount of the absolute ethyl alcohol is too small, the dispersibility of the powder is poor; if the mass ratio of the two is more than 1:40, the excessive use of the absolute ethyl alcohol will result in too dilute concentration of the reactant and too slow chemical reaction.
In some embodiments of the present invention, wherein the mass ratio of tween 80 to absolute ethyl alcohol is (1-1.5):1, the nano powder surface activation is better. If the mass ratio of the two is less than 1:1 and the dosage of the Tween 80 is too small, the surface of the nano powder cannot be completely activated; if the mass ratio of the two is more than 1.5:1, the dosage is too much, and the concentration of the Tween 80 reactant is too thin, the chemical reaction is too slow.
In some embodiments of the present invention, the mass ratio of the titanium isopropoxide to the alumina nanopowder is (2-3):1, which makes the thickness of the shell layer titanium oxide suitable, thereby utilizing both the extinction performance of the titanium oxide and the low thermal conductivity of the alumina. If the mass ratio of the two is less than 2:1, the shell layer is difficult to completely coat the alumina; if the mass ratio of the two is more than 3:1, the thermal conductivity of the heat-insulating material is increased.
In some embodiments of the present invention, in step 1), the reinforcing fibers are at least one selected from alumina fibers, mullite fibers, alumina silicate fibers, glass fibers, and zirconia fibers, and the fibers are resistant to high temperature and have small deformation at high temperature.
In some embodiments of the present invention, wherein in step 1), the inorganic binder is selected from boron oxide powder and low-melting glass powder (melting point about 500 ℃), these powders are easy to disperse uniformly.
In some embodiments of the present invention, wherein in step 2), the pressure of the forming is 1-60MPa, and the dwell time is > 1 h. If the pressure is lower than 1MPa, the strength of the heat-insulating material is too low; if the pressure is higher than 60MPa, the density of the material is too high, and the thermal conductivity is further increased.
In some embodiments of the present invention, in step 3), the drying temperature is 50-100 ℃, the drying time is more than 12h, the material is better formed, and the material is completely dried. The drying temperature is lower than 50 ℃ or the drying time is shorter than 12h, so that the drying temperature is too low or the drying time is too short, and the heat-insulating material is difficult to dry fully; some drying temperatures are above 100 ℃, so that too high a drying temperature reduces the strength of the insulation material.
In some embodiments of the present invention, in step 4), the heat treatment temperature is 500-700 ℃, and the heat treatment time is more than 4h, so that the surface of the alumina can be sufficiently formed with a titanium oxide shell layer. If the temperature is lower than 500 ℃, the heat treatment temperature is too low, the surface of the alumina is difficult to form a titanium oxide shell layer; if the temperature is higher than 700 ℃, the heat conductivity coefficient of the heat-insulating material is increased.
According to the high-temperature-resistant low-heat-conductivity core-shell-structure nano aluminum heat insulation material provided by the embodiment of the invention, the compression strength of the high-temperature-resistant low-heat-conductivity core-shell-structure nano aluminum heat insulation material is 1.38MPa to 1.51MPa, and the density of the high-temperature-resistant low-heat-conductivity core-shell-structure nano aluminum heat insulation material is 0.24 g/cm to 0.28g/cm3The porosity is 89.2-91.4%, the thermal conductivity at 25 ℃ is 0.018W/mK-0.022W/mK, the thermal conductivity at 400 ℃ is 0.025W/mK-0.030W/mK, the thermal conductivity at 800 ℃ is 0.036W/mK-0.039W/mK, and the thermal conductivity at 1200 ℃ is 0.041W/mK-0.044W/mK.
According to the heat insulation structure provided by the embodiment of the invention, the heat insulation structure comprises a heat insulation layer, and the heat insulation layer is composed of the high-temperature-resistant low-heat-conduction core-shell structure nano aluminum heat insulation material.
According to the embodiment of the invention, the high-temperature hearth comprises the heat insulation structure.
According to the embodiment of the invention, the building wall comprises the heat preservation structure.
The present invention will be further described with reference to the following specific examples, which should not be construed as limiting the scope of the invention, but rather as providing those skilled in the art with certain insubstantial modifications and adaptations of the invention based on the teachings of the invention set forth herein.
Example 1
(1) Mixing 50g of alumina nano powder with the particle size of 30nm with 2000g of absolute ethyl alcohol, stirring for half an hour until the mixture is uniform, adding 2000g of Tween 80 into the solution, stirring again for half an hour until the mixture is uniform, adding 100g of titanium isopropoxide into the solution, stirring for reaction for 1h to obtain gel, filtering the gel, drying the product at 120 ℃ for 6h, and calcining in a muffle furnace at 500 ℃ for 3h to obtain alumina/titanium oxide core-shell structure nano powder; the alumina/titanium oxide core-shell structure nano powder comprises core-layer alumina and shell-layer titanium oxide coated on the core-layer alumina, wherein the grain diameter of the core-layer alumina is 30nm, and the thickness of the shell-layer titanium oxide is 5 nm.
(2) Mixing materials: 60g of alumina nano powder with the grain diameter of 30nm, 25g of alumina/titanium oxide nano powder with a core-shell structure, 10g of silica glass fiber (the length is 3-6mm, and the diameter is 4-7 mu m), and 5g of boron oxide powder (the grain diameter is 50-60 mu m) are stirred and mixed evenly by a machine.
(3) Pressure forming: and putting the obtained mixture into a rectangular metal die with the thickness of 150X 50mm, and performing pressure forming under the forming pressure of 4MPa for 1 h.
(4) And (3) drying: the resulting block was dried in an oven at 50 ℃ for 12 h.
(5) And (3) heat treatment: the obtained block was put into a muffle furnace to be subjected to high-temperature heat treatment at 500 ℃ for 4 hours, and then cooled to room temperature.
Example 2
(1) Mixing 50g of alumina nano powder with the particle size of 30nm with 2500g of absolute ethyl alcohol, stirring for half an hour until the mixture is uniform, adding 2000g of Tween 80 into the solution, stirring again for half an hour until the mixture is uniform, adding 100g of titanium isopropoxide into the solution, stirring for reaction for 1h to obtain gel, filtering the gel, drying the product at 120 ℃ for 6h, and calcining in a muffle furnace at 500 ℃ for 3h to obtain alumina/titanium oxide core-shell structure nano powder; the alumina/titanium oxide core-shell structure nano powder comprises core-layer alumina and shell-layer titanium oxide coated on the core-layer alumina, wherein the grain diameter of the core-layer alumina is 30nm, and the thickness of the shell-layer titanium oxide is 5 nm.
(2) Mixing materials: 60g of alumina nano powder with the grain diameter of 30nm, 25g of alumina/titanium oxide nano powder with a core-shell structure, 10g of silica glass fiber (the length is 3-6mm, and the diameter is 4-7 mu m), and 5g of boron oxide powder (the grain diameter is 50-60 mu m) are stirred and mixed evenly by a machine.
(3) Pressure forming: and putting the obtained mixture into a metal rectangular die with the thickness of 50 x 150 x 50mm, and carrying out pressure forming under the forming pressure of 3MPa for 2 h.
(4) And (3) drying: the resulting block was dried in an oven at 60 ℃ for 12 h.
(5) And (3) heat treatment: the obtained block was put into a muffle furnace to be subjected to high-temperature heat treatment at 550 ℃ for 6 hours, and then cooled to room temperature.
Example 3
(1) Mixing 50g of alumina nano powder with the particle size of 30nm with 2000g of absolute ethyl alcohol, stirring for half an hour until the mixture is uniform, adding 2500g of Tween 80 into the solution, stirring again for half an hour until the mixture is uniform, adding 100g of titanium isopropoxide into the solution, stirring for reaction for 1h to obtain gel, filtering the gel, drying the product at 120 ℃ for 6h, and calcining in a muffle furnace at 500 ℃ for 3h to obtain alumina/titanium oxide core-shell structure nano powder; the alumina/titanium oxide core-shell structure nano powder comprises core-layer alumina and shell-layer titanium oxide coated on the core-layer alumina, wherein the grain diameter of the core-layer alumina is 30nm, and the thickness of the shell-layer titanium oxide is 5 nm.
(2) Mixing materials: 60g of alumina nano powder with the grain diameter of 30nm, 25g of alumina/titanium oxide nano powder with a core-shell structure, 10g of silica glass fiber (the length is 3-6mm, and the diameter is 4-7 mu m), and 5g of boron oxide powder (the grain diameter is 50-60 mu m) are stirred and mixed evenly by a machine.
(3) Pressure forming: and putting the obtained mixture into a metal rectangular die with the thickness of 50 x 150 x 50mm, and carrying out pressure forming under the forming pressure of 4MPa for 1 h.
(4) And (3) drying: the resulting block was dried in an oven at 50 ℃ for 12 h.
(5) And (3) heat treatment: the obtained block was put into a muffle furnace to be subjected to high-temperature heat treatment at 600 ℃ for 4 hours, and then cooled to room temperature.
Example 4
(1) Mixing 50g of alumina nano powder with the particle size of 30nm with 2000g of absolute ethyl alcohol, stirring for half an hour until the mixture is uniform, adding 2500g of Tween 80 into the solution, stirring again for half an hour until the mixture is uniform, adding 150g of titanium isopropoxide into the solution, stirring for reaction for 1h to obtain gel, filtering the gel, drying the product at 120 ℃ for 6h, and calcining in a muffle furnace at 500 ℃ for 3h to obtain alumina/titanium oxide core-shell structure nano powder; the alumina/titanium oxide core-shell structure nano powder comprises core-layer alumina and shell-layer titanium oxide coated on the core-layer alumina, wherein the grain diameter of the core-layer alumina is 30nm, and the thickness of the shell-layer titanium oxide is 8 nm.
(2) Mixing materials: 60g of alumina nano powder with the grain diameter of 30nm, 25g of alumina/titanium oxide nano powder with a core-shell structure, 10g of silica glass fiber (the length is 3-6mm, and the diameter is 4-7 mu m), and 5g of boron oxide powder (the grain diameter is 50-60 mu m) are stirred and mixed evenly by a machine.
(3) Pressure forming: and putting the obtained mixture into a metal rectangular die with the thickness of 50 x 150 x 50mm, and carrying out pressure forming under the forming pressure of 3MPa for 3 h.
(4) And (3) drying: the resulting block was dried in an oven at 60 ℃ for 12 h.
(5) And (3) heat treatment: the obtained block was put into a muffle furnace to be subjected to high-temperature heat treatment at 700 ℃ for 3 hours, and then cooled to room temperature.
Example 5
(1) Mixing 50g of alumina nano powder with the particle size of 30nm with 2000g of absolute ethyl alcohol, stirring for half an hour until the mixture is uniform, adding 2000g of Tween 80 into the solution, stirring again for half an hour until the mixture is uniform, adding 150g of titanium isopropoxide into the solution, stirring for reaction for 1h to obtain gel, filtering the gel, drying the product at 120 ℃ for 6h, and calcining in a muffle furnace at 500 ℃ for 3h to obtain alumina/titanium oxide core-shell structure nano powder; the alumina/titanium oxide core-shell structure nano powder comprises core-layer alumina and shell-layer titanium oxide coated on the core-layer alumina, wherein the grain diameter of the core-layer alumina is 30nm, and the thickness of the shell-layer titanium oxide is 8 nm.
(2) Mixing materials: 68g of alumina nano powder with the grain diameter of 30nm, 18g of alumina/titanium oxide nano powder with a core-shell structure, 10g of silica glass fiber (the length is 3-6mm, and the diameter is 4-7 mu m), and 5g of boron oxide powder (the grain diameter is 50-60 mu m) are stirred and mixed evenly by a machine.
(3) Pressure forming: and putting the obtained mixture into a metal rectangular die with the thickness of 50 x 150 x 50mm, and carrying out pressure forming under the forming pressure of 4MPa for 1 h.
(4) And (3) drying: the resulting block was dried in an oven at 50 ℃ for 12 h.
(5) And (3) heat treatment: the obtained block was put into a muffle furnace to be subjected to high-temperature heat treatment at 500 ℃ for 4 hours, and then cooled to room temperature.
Example 6
(1) Mixing 50g of alumina nano powder with the particle size of 30nm with 2000g of absolute ethyl alcohol, stirring for half an hour until the mixture is uniform, adding 2000g of Tween 80 into the solution, stirring again for half an hour until the mixture is uniform, adding 100g of titanium isopropoxide into the solution, stirring for reaction for 1h to obtain gel, filtering the gel, drying the product at 120 ℃ for 6h, and calcining in a muffle furnace at 500 ℃ for 3h to obtain alumina/titanium oxide core-shell structure nano powder; the alumina/titanium oxide core-shell structure nano powder comprises core-layer alumina and shell-layer titanium oxide coated on the core-layer alumina, wherein the grain diameter of the core-layer alumina is 30nm, and the thickness of the shell-layer titanium oxide is 5 nm.
(2) Mixing materials: 62g of alumina nano powder with the grain diameter of 30nm, 25g of alumina/titanium oxide nano powder with a core-shell structure, 8g of silica glass fiber (the length is 3-6mm, and the diameter is 4-7 mu m), and 5g of boron oxide powder (the grain diameter is 50-60 mu m) are stirred and mixed evenly by a machine.
(3) Pressure forming: and putting the obtained mixture into a metal rectangular die with the thickness of 50 x 150 x 50mm, and carrying out pressure forming under the forming pressure of 4MPa for 1 h.
(4) And (3) drying: the resulting block was dried in an oven at 50 ℃ for 12 h.
(5) And (3) heat treatment: the obtained block was put into a muffle furnace to be subjected to high-temperature heat treatment at 500 ℃ for 4 hours, and then cooled to room temperature.
Example 7
(1) Mixing 50g of alumina nano powder with the particle size of 30nm with 2000g of absolute ethyl alcohol, stirring for half an hour until the mixture is uniform, adding 2500g of Tween 80 into the solution, stirring again for half an hour until the mixture is uniform, adding 100g of titanium isopropoxide into the solution, stirring for reaction for 1h to obtain gel, filtering the gel, drying the product at 120 ℃ for 6h, and calcining in a muffle furnace at 500 ℃ for 3h to obtain alumina/titanium oxide core-shell structure nano powder; the alumina/titanium oxide core-shell structure nano powder comprises core-layer alumina and shell-layer titanium oxide coated on the core-layer alumina, wherein the grain diameter of the core-layer alumina is 30nm, and the thickness of the shell-layer titanium oxide is 5 nm.
(2) Mixing materials: uniformly mixing 61g of alumina nano powder with the particle size of 30nm, 25g of alumina/titanium oxide nano powder with a core-shell structure, 10g of silica glass fiber (the length is 3-6mm, and the diameter is 4-7 mu m) and 4g of boron oxide powder (the particle size is 50-60 mu m) by mechanical stirring.
(3) Pressure forming: and putting the obtained mixture into a metal rectangular die with the thickness of 50 x 150 x 50mm, and carrying out pressure forming under the forming pressure of 4MPa for 1 h.
(4) And (3) drying: the resulting block was dried in an oven at 50 ℃ for 12 h.
(5) And (3) heat treatment: the obtained block was put into a muffle furnace to be subjected to high-temperature heat treatment at 500 ℃ for 4 hours, and then cooled to room temperature.
Example 8
(1) Mixing 50g of alumina nano powder with the particle size of 30nm with 2000g of absolute ethyl alcohol, stirring for half an hour until the mixture is uniform, adding 2500g of Tween 80 into the solution, stirring again for half an hour until the mixture is uniform, adding 100g of titanium isopropoxide into the solution, stirring for reaction for 1h to obtain gel, filtering the gel, drying the product at 120 ℃ for 6h, and calcining in a muffle furnace at 500 ℃ for 3h to obtain alumina/titanium oxide core-shell structure nano powder; the alumina/titanium oxide core-shell structure nano powder comprises core-layer alumina and shell-layer titanium oxide coated on the core-layer alumina, wherein the grain diameter of the core-layer alumina is 30nm, and the thickness of the shell-layer titanium oxide is 5 nm.
(2) Mixing materials: 60g of alumina nano powder with the grain diameter of 30nm, 24g of alumina/titanium oxide nano powder with a core-shell structure, 10g of silica glass fiber (the length is 3-6mm, and the diameter is 4-7 mu m), and 6g of boron oxide powder (the grain diameter is 50-60 mu m) are stirred and mixed evenly by a machine.
(3) Pressure forming: and putting the obtained mixture into a metal rectangular die with the thickness of 50 x 150 x 50mm, and carrying out pressure forming under the forming pressure of 4MPa for 1 h.
(4) And (3) drying: the resulting block was dried in an oven at 50 ℃ for 12 h.
(5) And (3) heat treatment: the obtained block was put into a muffle furnace to be subjected to high-temperature heat treatment at 500 ℃ for 4 hours, and then cooled to room temperature.
Example 9
(1) Mixing 50g of alumina nano powder with the particle size of 30nm with 2000g of absolute ethyl alcohol, stirring for half an hour until the mixture is uniform, adding 2000g of Tween 80 into the solution, stirring again for half an hour until the mixture is uniform, adding 150g of titanium isopropoxide into the solution, stirring for reaction for 1h to obtain gel, filtering the gel, drying the product at 120 ℃ for 6h, and calcining in a muffle furnace at 500 ℃ for 3h to obtain alumina/titanium oxide core-shell structure nano powder; the alumina/titanium oxide core-shell structure nano powder comprises core-layer alumina and shell-layer titanium oxide coated on the core-layer alumina, wherein the grain diameter of the core-layer alumina is 30nm, and the thickness of the shell-layer titanium oxide is 8 nm.
(2) Mixing materials: mixing 65g of alumina nano powder with particle size of 30nm, 20g of alumina/titanium oxide nano powder with core-shell structure, 10g of silica glass fiber (length of 3-6mm and diameter of 4-7 μm), and 5g of boron oxide powder (particle size of 50-60 μm) by mechanical stirring.
(3) Pressure forming: and putting the obtained mixture into a metal rectangular die with the thickness of 50 x 150 x 50mm, and carrying out pressure forming under the forming pressure of 4MPa for 1 h.
(4) And (3) drying: the resulting block was dried in an oven at 50 ℃ for 12 h.
(5) And (3) heat treatment: the obtained block was put into a muffle furnace to be subjected to high-temperature heat treatment at 500 ℃ for 4 hours, and then cooled to room temperature.
Example 10
(1) Mixing 50g of alumina nano powder with the particle size of 30nm with 2000g of absolute ethyl alcohol, stirring for half an hour until the mixture is uniform, adding 2000g of Tween 80 into the solution, stirring again for half an hour until the mixture is uniform, adding 150g of titanium isopropoxide into the solution, stirring for reaction for 1h to obtain gel, filtering the gel, drying the product at 120 ℃ for 6h, and calcining in a muffle furnace at 500 ℃ for 3h to obtain alumina/titanium oxide core-shell structure nano powder; the alumina/titanium oxide core-shell structure nano powder comprises core-layer alumina and shell-layer titanium oxide coated on the core-layer alumina, wherein the grain diameter of the core-layer alumina is 30nm, and the thickness of the shell-layer titanium oxide is 8 nm.
(2) Mixing materials: 60g of alumina nano powder with the grain diameter of 30nm, 25g of alumina/titanium oxide nano powder with a core-shell structure, 9g of silica glass fiber (the length is 3-6mm, and the diameter is 4-7 mu m), and 6g of boron oxide powder (the grain diameter is 50-60 mu m) are stirred and mixed evenly by a machine.
(3) Pressure forming: and putting the obtained mixture into a metal rectangular die with the thickness of 50 x 150 x 50mm, and carrying out pressure forming under the forming pressure of 4MPa for 1 h.
(4) And (3) drying: the resulting block was dried in an oven at 50 ℃ for 12 h.
(5) And (3) heat treatment: the obtained block was put into a muffle furnace to be subjected to high-temperature heat treatment at 500 ℃ for 4 hours, and then cooled to room temperature.
Comparative example 1
(1) Mixing materials: 75g of alumina nano powder with the grain diameter of 30nm, 15g of titanium oxide nano powder with the grain diameter of 50nm and 10g of glass fiber are evenly mixed by mechanical stirring.
(2) Pressure forming: and putting the obtained mixture into a mold, and carrying out pressure molding, wherein the molding pressure is 3MPa, and the pressure maintaining time is 3 h.
(3) And (3) drying: the resulting block was dried in an oven at 60 ℃ for 12 h.
(4) And (3) heat treatment: the obtained block was put into a muffle furnace to be heat-treated at 580 ℃ for 3 hours, and then cooled to room temperature.
Comparative example 2
(1) Mixing materials: 62g of alumina nano powder with the grain diameter of 30nm, 30g of titanium oxide nano powder with the grain diameter of 50nm and 8g of silica glass fiber (the length is 3-6mm, and the diameter is 4-7 mu m) are stirred and mixed evenly by a machine.
(2) Pressure forming: and putting the obtained mixture into a metal rectangular die with the thickness of 50 x 150 x 50mm, and carrying out pressure forming under the forming pressure of 4MPa for 1 h.
(3) And (3) drying: the resulting block was dried in an oven at 50 ℃ for 12 h.
(4) And (3) heat treatment: the obtained block was put into a muffle furnace to be subjected to high-temperature heat treatment at 500 ℃ for 4 hours, and then cooled to room temperature.
Comparative example 3
(1) Mixing 50g of alumina nano powder with the particle size of 30nm with 2000g of absolute ethyl alcohol, stirring for half an hour until the mixture is uniform, adding 2000g of Tween 80 into the solution, stirring again for half an hour until the mixture is uniform, adding 100g of titanium isopropoxide into the solution, stirring for reaction for 1h to obtain gel, filtering the gel, drying the product at 120 ℃ for 6h, and calcining in a muffle furnace at 500 ℃ for 3h to obtain alumina/titanium oxide core-shell structure nano powder; the alumina/titanium oxide core-shell structure nano powder comprises core-layer alumina and shell-layer titanium oxide coated on the core-layer alumina, wherein the grain diameter of the core-layer alumina is 30nm, and the thickness of the shell-layer titanium oxide is 5 nm.
(2) Mixing materials: 68g of alumina nano powder with the grain diameter of 30nm, 22g of alumina/titanium oxide nano powder with a core-shell structure and 10g of silica glass fiber (the length is 3-6mm, and the diameter is 4-7 mu m) are stirred and mixed evenly by a machine.
(3) Pressure forming: and putting the obtained mixture into a metal rectangular die with the thickness of 50 x 150 x 50mm, and carrying out pressure forming under the forming pressure of 4MPa for 1 h.
(4) And (3) drying: the resulting block was dried in an oven at 50 ℃ for 12 h.
(5) And (3) heat treatment: the obtained block was put into a muffle furnace to be subjected to high-temperature heat treatment at 500 ℃ for 4 hours, and then cooled to room temperature.
Comparative example 4
(1) Mixing 50g of alumina nano powder with the particle size of 30nm with 2000g of absolute ethyl alcohol, stirring for half an hour until the mixture is uniform, adding 2000g of Tween 80 into the solution, stirring again for half an hour until the mixture is uniform, adding 200g of titanium isopropoxide into the solution, stirring for reaction for 1h to obtain gel, filtering the gel, drying the product at 120 ℃ for 6h, and calcining in a muffle furnace at 500 ℃ for 3h to obtain alumina/titanium oxide core-shell structure nano powder; the alumina/titanium oxide core-shell structure nano powder comprises core-layer alumina and shell-layer titanium oxide coated on the core-layer alumina, wherein the grain diameter of the core-layer alumina is 30nm, and the thickness of the shell-layer titanium oxide is 12 nm.
(2) Mixing materials: 60g of alumina nano powder with the grain diameter of 30nm, 25g of alumina/titanium oxide nano powder with a core-shell structure, 10g of silica glass fiber (the length is 3-6mm, and the diameter is 4-7 mu m), and 5g of boron oxide powder (the grain diameter is 50-60 mu m) are stirred and mixed evenly by a machine.
(3) Pressure forming: and putting the obtained mixture into a metal rectangular die with the thickness of 50 x 150 x 50mm, and carrying out pressure forming under the forming pressure of 4MPa for 1 h.
(4) And (3) drying: the resulting block was dried in an oven at 50 ℃ for 12 h.
(5) And (3) heat treatment: the obtained block was put into a muffle furnace to be subjected to high-temperature heat treatment at 500 ℃ for 4 hours, and then cooled to room temperature.
Comparative example 5
(1) Mixing 50g of alumina nano powder with the particle size of 30nm with 2000g of absolute ethyl alcohol, stirring for half an hour until the mixture is uniform, adding 2000g of Tween 80 into the solution, stirring again for half an hour until the mixture is uniform, adding 50g of titanium isopropoxide into the solution, stirring for reaction for 1h to obtain gel, filtering the gel, drying the product at 120 ℃ for 6h, and calcining in a muffle furnace at 500 ℃ for 3h to obtain alumina/titanium oxide core-shell structure nano powder; the alumina/titanium oxide core-shell structure nano powder comprises core-layer alumina and shell-layer titanium oxide coated on the core-layer alumina, wherein the grain diameter of the core-layer alumina is 30nm, and the thickness of the shell-layer titanium oxide is 2 nm.
(2) Mixing materials: 60g of alumina nano powder with the grain diameter of 30nm, 25g of alumina/titanium oxide nano powder with a core-shell structure, 10g of silica glass fiber (the length is 3-6mm, and the diameter is 4-7 mu m), and 5g of boron oxide powder (the grain diameter is 50-60 mu m) are stirred and mixed evenly by a machine.
(3) Pressure forming: and putting the obtained mixture into a metal rectangular die with the thickness of 50 x 150 x 50mm, and carrying out pressure forming under the forming pressure of 4MPa for 1 h.
(4) And (3) drying: the resulting block was dried in an oven at 50 ℃ for 12 h.
(5) And (3) heat treatment: the obtained block was put into a muffle furnace to be subjected to high-temperature heat treatment at 500 ℃ for 4 hours, and then cooled to room temperature.
Test example
Thermal conductivity was tested according to standard GBT4130-2005 and compressive strength was tested according to standard GBT 4740-1999; the density is tested according to test standard GBT 17911-2006; porosity was tested according to GBT 2998-2015.
The high temperature resistant low thermal conductivity core-shell structure nano aluminum thermal insulation materials prepared in the above examples 1 to 10 and the materials of comparative examples 1 to 5 were tested for their thermal conductivity, compressive strength, density, porosity and other properties at different temperatures, and the test results are shown in tables 1 and 2.
TABLE 1
TABLE 2
As can be seen from the data in Table 1, the thermal insulation material prepared by preparing the alumina/silica nanopowder with the core-shell structure and performing composite pressing with other materials has lower thermal conductivity. The prepared core-shell structure alumina/titanium oxide nano powder not only utilizes the low heat conduction characteristic of alumina, but also has the advantages of shading effect, titanium oxide reduction and solid phase to heat reduction because the titanium oxide is coated on the surface of the alumina. As can be seen from comparative examples 1 and 2, the thermal conductivity of the thermal insulation material is obviously increased without preparing the core-shell structure nano powder. In contrast, the use of an excessive amount of titanium in comparative example 4 resulted in a high titanium oxide content and an increased solid phase heat conductivity; in comparative example 5, too small amount of titanium was used, and radiation heat transfer was not suppressed to the maximum, so that the thermal conductivity was remarkably increased.
As can be seen from the data in table 2, the compressive strength of the material can be increased by adding boron oxide, the material strength is lower in comparative example 3 where no binder is added, and the compressive strength is significantly increased in comparative example 5 where a binder is used. This is because the boron oxide powder produces local solid phase bonding during the high temperature heat treatment process, increasing the strength of the material. The main components in the above examples 1 to 10 and comparative examples 3 to 5 are alumina nano powder and/or alumina/titania core-shell structure nano powder, and the amounts of glass fiber and boron oxide powder are small, so that the density and porosity of the glass fiber and the boron oxide powder are not greatly different.
The high-temperature-resistant low-thermal-conductivity core-shell-structure nano aluminum thermal insulation material prepared in the embodiments 1 to 10 of the invention has the compression strength of 1.38MPa to 1.51MPa and the density of 0.24 to 0.28g/cm3The porosity is 89.2-91.4%, the thermal conductivity at 25 ℃ is 0.018W/mK-0.022W/mK, the thermal conductivity at 400 ℃ is 0.025W/mK-0.030W/mK, the thermal conductivity at 800 ℃ is 0.036W/mK-0.039W/mK, and the thermal conductivity at 1200 ℃ is 0.041W/mK-0.044W/mK.
In conclusion, the high-temperature-resistant low-heat-conductivity core-shell-structure nano aluminum thermal insulation material prepared by the invention has high temperature resistance, low heat conductivity coefficient and high strength, can be applied to high-temperature hearth thermal insulation, building material external wall thermal insulation and other places, and has an energy-saving effect.
In the description of the present invention, numerous specific details are set forth. It is understood, however, that embodiments of the invention may be practiced without these specific details. In some embodiments, well-known methods, structures and techniques have not been shown in detail in order not to obscure an understanding of this description.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are still within the scope of the technical solution of the present invention.
Claims (10)
1. A preparation method of a high-temperature-resistant low-heat-conductivity core-shell structure nano aluminum heat insulation material is characterized by comprising the following steps of:
1) fully and uniformly mixing the raw material core-shell structure nano powder, the alumina nano powder, the reinforced fiber and the inorganic binder;
2) pressure forming: carrying out pressure forming on the mixture obtained in the step 1);
3) and (3) drying: drying the block obtained in step 2) at 50-100 ℃;
4) and (3) heat treatment: carrying out high-temperature heat treatment on the block obtained in the step 3) at the temperature of 500-700 ℃, and then cooling to room temperature.
2. The preparation method of the high temperature resistant low thermal conductivity core-shell structure nano aluminum thermal insulation material according to claim 1, characterized in that in step 1), the raw materials comprise, by mass: 60-68% of alumina nano powder; 18-25% of core-shell structure nano powder; 8-10% of reinforcing fiber; 4-6% of inorganic binder.
3. The preparation method of the high temperature resistant low thermal conductivity core-shell structure nano aluminum thermal insulation material according to claim 1, wherein in the step 1), the core-shell structure nano powder is alumina/titania core-shell structure nano powder; the alumina/titanium oxide core-shell structure nano powder comprises core-layer alumina and shell-layer titanium oxide coated on the core-layer alumina, wherein the grain diameter of the core-layer alumina is 30nm, and the thickness of the shell-layer titanium oxide is 5-8 nm; the mass ratio of the nuclear layer alumina to the shell layer titanium oxide is 1: (2-3).
4. The preparation method of the high temperature resistant low thermal conductivity core-shell structure nano aluminum thermal insulation material according to claim 1, wherein in the step 1), the core-shell structure nano powder is prepared through the following steps:
mixing and stirring the alumina nano powder and absolute ethyl alcohol for 0.5-1 hour until the mixture is uniform, adding Tween 80 serving as a surfactant into the solution, stirring and stirring the mixture for 0.5-1 hour until the mixture is uniform again, adding titanium isopropoxide into the solution, stirring and reacting the mixture for 1-2 hours to obtain gel, filtering the gel, drying the product at the temperature of 100-140 ℃ for 6-8 hours, and calcining the product in a muffle furnace at the temperature of 500-600 ℃ for 3-4 hours.
5. The preparation method of the high-temperature-resistant low-thermal-conductivity core-shell-structure nano aluminum thermal insulation material as claimed in claim 4, wherein the mass ratio of the alumina nano powder to the absolute ethyl alcohol is 1: (40-50); the mass ratio of the Tween 80 to the absolute ethyl alcohol is (1-1.5) to 1; the mass ratio of the titanium isopropoxide to the alumina nano powder is (2-3) to 1.
6. The preparation method of the high temperature resistant low thermal conductivity core-shell structure nano aluminum thermal insulation material according to claim 1, wherein in the step 1), the reinforcing fiber is at least one selected from alumina fiber, mullite fiber, alumina silicate fiber, glass fiber and zirconia fiber; the inorganic binder is at least one selected from boron oxide powder and low-melting-point glass powder; in the step 2), the forming pressure is 1-60MPa, and the pressure maintaining time is more than 1 h; in the step 3), the drying temperature is 50-100 ℃, and the drying time is more than 12 hours; in the step 4), the heat treatment temperature is 500-700 ℃, and the heat treatment time is more than 4 h.
7. The high-temperature-resistant low-heat-conduction core-shell-structure nano aluminum heat insulation material is characterized in thatThe compression strength of the high-temperature-resistant low-heat-conduction core-shell structure nano aluminum heat insulation material is 1.38MPa to 1.51MPa, and the density of the high-temperature-resistant low-heat-conduction core-shell structure nano aluminum heat insulation material is 0.24 g/cm to 0.28g/cm3The porosity is 89.2% -91.4%, the thermal conductivity at 25 ℃ is 0.018W/mK-0.022W/mK, the thermal conductivity at 400 ℃ is 0.025W/mK-0.030W/mK, the thermal conductivity at 800 ℃ is 0.036W/mK-0.039W/mK, and the thermal conductivity at 1200 ℃ is 0.041W/mK-0.044W/mK; the high-temperature-resistant low-thermal-conductivity core-shell-structure nano aluminum thermal insulation material is prepared by the method of any one of claims 1 to 6.
8. The heat insulation structure comprises a heat insulation layer, and is characterized in that the heat insulation layer is made of the high-temperature-resistant low-heat-conductivity core-shell-structure nano aluminum heat insulation material disclosed by claim 7.
9. A high temperature furnace comprising the insulation structure of claim 8.
10. A building wall comprising the insulation structure of claim 8.
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