CN108383486B - High-temperature-resistant radiation wave-transparent heat-insulating material and preparation method thereof - Google Patents
High-temperature-resistant radiation wave-transparent heat-insulating material and preparation method thereof Download PDFInfo
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- CN108383486B CN108383486B CN201810220871.2A CN201810220871A CN108383486B CN 108383486 B CN108383486 B CN 108383486B CN 201810220871 A CN201810220871 A CN 201810220871A CN 108383486 B CN108383486 B CN 108383486B
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- 230000005855 radiation Effects 0.000 title claims abstract description 46
- 239000011810 insulating material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000000835 fiber Substances 0.000 claims abstract description 66
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000004964 aerogel Substances 0.000 claims abstract description 34
- 150000001844 chromium Chemical class 0.000 claims abstract description 28
- 230000032683 aging Effects 0.000 claims abstract description 24
- 239000002131 composite material Substances 0.000 claims abstract description 24
- 239000002904 solvent Substances 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 21
- 239000011159 matrix material Substances 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 16
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000002787 reinforcement Effects 0.000 claims abstract description 10
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 9
- 238000007865 diluting Methods 0.000 claims abstract description 5
- 238000002791 soaking Methods 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 26
- 239000010453 quartz Substances 0.000 claims description 20
- 238000009413 insulation Methods 0.000 claims description 19
- 239000002245 particle Substances 0.000 claims description 18
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 claims description 14
- 239000012774 insulation material Substances 0.000 claims description 13
- 238000005470 impregnation Methods 0.000 claims description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- 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 10
- 229910052863 mullite Inorganic materials 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- WYYQVWLEPYFFLP-UHFFFAOYSA-K chromium(3+);triacetate Chemical compound [Cr+3].CC([O-])=O.CC([O-])=O.CC([O-])=O WYYQVWLEPYFFLP-UHFFFAOYSA-K 0.000 claims description 9
- 238000000352 supercritical drying Methods 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 239000013306 transparent fiber Substances 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 230000005540 biological transmission Effects 0.000 claims description 4
- 238000002210 supercritical carbon dioxide drying Methods 0.000 claims description 3
- GRWVQDDAKZFPFI-UHFFFAOYSA-H chromium(III) sulfate Chemical compound [Cr+3].[Cr+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRWVQDDAKZFPFI-UHFFFAOYSA-H 0.000 claims description 2
- 238000013329 compounding Methods 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 14
- 239000013078 crystal Substances 0.000 abstract description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 12
- 239000003605 opacifier Substances 0.000 description 11
- 238000003756 stirring Methods 0.000 description 11
- 239000000499 gel Substances 0.000 description 10
- 238000000465 moulding Methods 0.000 description 10
- WGLPBDUCMAPZCE-UHFFFAOYSA-N chromium trioxide Inorganic materials O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 230000002209 hydrophobic effect Effects 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 229910000423 chromium oxide Inorganic materials 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- 229910000151 chromium(III) phosphate Inorganic materials 0.000 description 3
- IKZBVTPSNGOVRJ-UHFFFAOYSA-K chromium(iii) phosphate Chemical compound [Cr+3].[O-]P([O-])([O-])=O IKZBVTPSNGOVRJ-UHFFFAOYSA-K 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000004965 Silica aerogel Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000003471 anti-radiation Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- -1 aging Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 229940117975 chromium trioxide Drugs 0.000 description 1
- GAMDZJFZMJECOS-UHFFFAOYSA-N chromium(6+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Cr+6] GAMDZJFZMJECOS-UHFFFAOYSA-N 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000007783 nanoporous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 238000011160 research 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
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000000475 sunscreen effect Effects 0.000 description 1
- 239000000516 sunscreening agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000012780 transparent material Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 239000011240 wet gel Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/24—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
- C04B28/26—Silicates of the alkali metals
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/42—Coatings containing inorganic materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/02—Treatment
- C04B20/04—Heat treatment
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/46—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
- C04B41/49—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes
- C04B41/4905—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
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- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Thermal Insulation (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention provides a preparation method of a high-temperature-resistant radiation wave-transparent heat-insulating material. Specifically, the method of the present invention comprises: diluting and dissolving trivalent chromium salt, and adding an alkaline reagent to obtain a chromium salt complex solution; soaking the wave-transmitting fiber reinforcement by using a chromium salt complex solution, and drying after sol-gel to obtain a fiber preform; sintering the fiber preform to obtain a chromium sesquioxide composite fiber reinforced matrix; soaking a fiber reinforced matrix by using silica sol, and obtaining a fiber reinforced aerogel composite material through sol-gel, aging, solvent replacement and drying; and carrying out moisture-proof treatment on the fiber-reinforced aerogel composite material to obtain the high-temperature-resistant radiation wave-transparent heat-insulating material. The invention also provides a high-temperature-resistant radiation wave-transparent heat-insulating material and application thereof. The method can control the grain diameter and the crystal form of the chromium sesquioxide, and ensure that the material has excellent high-temperature radiation resistance and dielectric property.
Description
The application is a divisional application with the name of 'a high temperature resistant radiation wave-transparent heat-insulating material and a preparation method thereof' on 2016, 11, 16 and 201611025658.3.
Technical Field
The invention relates to a high-temperature-resistant radiation wave-transparent heat-insulating material and a preparation method thereof, belonging to the technical field of thermal protection.
Background
The aerogel material is a novel low-density nano porous material, is a solid material with the best heat insulation performance at present, is formed by mutually accumulating nano particles, has a three-dimensional network nano porous structure, can obviously reduce the solid heat conduction, the convection heat transfer and the radiation heat transfer of the material, the aerogel is almost transparent to near-infrared wavelength of 2-10 mu m, the radiation heat transfer effect is very obvious at high temperature, if no anti-infrared opacifier is added, the high-temperature heat insulation effect of the aerogel is reduced, the proportion of each heat transfer path in the aerogel can be changed after the opacifier is added, the invention provides a preparation method of a high-temperature-resistant radiation wave-transmitting heat-insulating material and the high-temperature-resistant radiation wave-transmitting heat-insulating material prepared by the method through in-depth experiments and combination of a large number of theoretical analyses.
Aiming at the research on the high-temperature heat insulation effect of the aerogel, the preparation method of the opacifier and aerogel composite material comprises the following steps: (1) carbon black and silicon carbide infrared opacifiers are added into aerogel materials to prepare high-temperature heat-insulating aerogel composite materials (see CN201410456744.4, named as high-temperature heat-insulating aerogel composite materials) which can be used at 1200 ℃, but the preparation method has the problems of being complex in operation, needing to be manufactured in a layered mode, needing to use multiple opacifiers and the like. (2) An infrared opacifier titanium dioxide is added into aerogel, and then the aerogel is subjected to sol-gel and supercritical drying to prepare a composite material (see CN200510031952.0, namely an aerogel thermal insulation composite material and a preparation method thereof). (3) The silica aerogel is doped with fibers, opacifiers and the like to prepare the aerogel heat insulation material with high strength and good heat insulation performance (refer to CN200510012154.3, namely a preparation method of the porous powder doped silica aerogel heat insulation material). However, these patents do not use a high-purity chromium salt complex, and do not go through a high-temperature sintering step, organic small-molecular substances and metal impurities in the raw materials cannot be removed, the particle diameter of the opacifier is too different and uncontrollable, and chromium trioxide grains in a proper particle size range cannot be formed as expected, so that the expected room-temperature thermal conductivity, dielectric constant and loss tangent cannot be obtained, and the high-temperature radiation-resistant wave-transparent heat insulation performance is insufficient.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a high-temperature-resistant radiation wave-transparent heat-insulating material with stable high-temperature electrical property and excellent heat-insulating effect, and a preparation method and application thereof.
The invention provides a preparation method of a high-temperature-resistant radiation wave-transparent heat-insulating material in a first aspect, which comprises the following steps:
(1) preparation of chromium salt complex: diluting trivalent chromium salt in a diluting solvent, and adding an alkaline reagent to obtain a chromium salt complex solution;
(2) dipping: soaking the wave-transparent fiber reinforcement body by using the chromium salt complex solution, and drying after sol-gel to obtain a fiber preform;
(3) and (3) sintering: sintering the fiber preform to obtain a chromium sesquioxide composite fiber matrix;
(4) compounding the aerogel: impregnating the fiber reinforced matrix with silica sol, and carrying out sol-gel, aging, solvent replacement and drying to obtain a fiber reinforced aerogel composite material;
(5) moisture-proof treatment: and carrying out moisture-proof treatment on the fiber-reinforced aerogel composite material to obtain the high-temperature-resistant radiation wave-transparent heat-insulating material.
The invention provides in a second aspect a high temperature resistant radiation transparent and insulating material comprising wave-transparent fibres and chromium oxide.
The present invention provides, in a third aspect, a wave-transparent and heat-insulating member made of the high-temperature radiation-resistant wave-transparent and heat-insulating material obtained by the method of the first aspect of the present invention or the high-temperature radiation-resistant wave-transparent and heat-insulating material of the second aspect of the present invention.
Compared with the prior art, the invention at least has the following beneficial effects:
(1) the high-temperature-resistant radiation-resistant wave-transmitting heat-insulating material prepared by the invention breaks through theoretical analysis, and the prepared high-temperature-resistant radiation-resistant wave-transmitting heat-insulating material can meet the requirement that the working time is more than or equal to 2500s under the condition of high temperature of 1200 ℃; the density is adjustable and is in the range of 0.25g/cm3～0.4g/cm3(ii) a The requirement of stable high-temperature wave-transmitting performance is met, the heat insulation effect is obviously superior to that of a common aerogel material, and the aerogel material can be used for thermal protection of radio equipment in aircrafts with high Mach numbers and long voyages.
(2) The wave-transparent heat-insulating member prepared from the high-temperature-resistant anti-radiation glass heat-insulating material has good electrical property, the dielectric constant is 1.2-1.5 at 1200 ℃, and the loss tangent<5×10-3(ii) a The wave transmission rate is more than or equal to 90 percent.
(3) The invention can be used for preparing wave-transparent heat-insulating components with various types and specifications, such as hemispherical, quasi-hemispherical, conical and various large-scale special-shaped surface components, and has guiding significance for the production of special-shaped rigid wave-transparent heat-insulating components.
Drawings
FIG. 1 is a process flow diagram of the preparation method of the present invention.
Detailed Description
The invention provides a high-temperature-resistant radiation wave-transparent heat-insulating material and a preparation method thereof. The chromium salt selected in the preparation of the chromium sesquioxide can be selected from the group consisting of chromium acetate, chromium sulfate and chromium nitrate; in the preparation method, the sintering temperature can be 600-800 ℃ (for example 600, 700 or 800 ℃), and the sintering time can be 2-6 h (for example 2, 3, 4, 5 or 6 h); the particle size may be 2 μm to 5 μm (e.g., 2, 3, 4, or 5 μm); the mass ratio of the chromium oxide to the wave-transmitting fiber reinforcement in the heat-insulating material can be 1: 0.05-0.15 (e.g., 1:0.05, 1: 0.10, or 1: 0.15).
The inventor finds that the chromium sesquioxide is a good light-shading agent and is also a wave-transmitting material with stable high-temperature performance, the dielectric constant and the loss tangent of the cubic crystal form chromium sesquioxide are very low at the high temperature of 1200 ℃, the interior of a crystal lattice is not greatly changed, the chromium salt is formed into a chromium salt complex, and the synthesis mode, the particle size or the addition amount of the chromium sesquioxide are adjusted, so that the chromium sesquioxide can be uniformly distributed in the aerogel, the electrical performance is stable, and the infrared shading performance is excellent at the high temperature.
In some preferred embodiments, the present invention maximizes the efficiency of radiation heat conduction and solid phase heat conduction of the aerogel composite material by adjusting the content, particle size and/or crystal form of chromium sesquioxide, etc., thereby ensuring the overall high temperature radiation resistant effect; in addition, the uniform distribution of the chromium sesquioxide in the aerogel can be controlled by controlling the complexing mode and/or the sintering procedure of the chromium sesquioxide, and the stability of the electrical property is further ensured.
Specifically, the invention provides a preparation method of a high-temperature-resistant radiation-resistant wave-transparent heat-insulating material, which comprises the following steps:
(1) preparation of chromium salt complexes
Taking chromium nitrate, chromium phosphate or chromium acetate as an example, but not limited thereto, adding water (such as purified water) or an alcohol solution to dissolve and dilute, then adding a weakly alkaline solvent with a certain concentration, controlling the pH value of the solution to be 7-8, and fully and uniformly stirring to obtain a chromium salt complex solution; in the invention, the dosage and concentration of the chromium salt complex are adjusted, so that the mass ratio of the chromium sesquioxide to the wave-transmitting fiber reinforcement is 1:0.05 to 0.15.
(2) Impregnation
Impregnating a wave-transparent fiber reinforcement with the chromium salt complex solution; in the invention, the glass fiber-permeable fiber used for the wave-permeable fiber reinforcement can be selected from the group consisting of quartz fiber, mullite fiber and alumina fiber; the impregnation method can be vacuum impregnation, pressure impregnation or vacuum-pressure impregnation. The alkaline agent may be a weakly alkaline agent, more preferably aqueous ammonia, further preferably 0.5M to 1.5M aqueous ammonia, and most preferably, the alkaline agent is added in an amount such that the pH of the system is 7 to 8. The drying in this step may be carried out at 100 ℃ until drying.
(3) Sintering
The high-temperature sintering temperature selected in the invention is 600-800 ℃ (for example 600, 700 or 800 ℃), and the total sintering time is 2-6 h (for example 2, 3, 4, 5 or 6 h). In some embodiments, the fiber preform obtained in step (2) may be sintered at high temperature using different temperature procedures to obtain a chromium oxide composite fiber matrix. The temperature programming stage may be, for example, one or more of (a)600 ℃ for 1h to 2h, or (b)700 ℃ for 1h to 2h, or (c)800 ℃ for 1h to 2h, such that the particle size of the chromium sesquioxide formed after sintering is 2 μm to 5 μm (e.g., 2, 3, 4, or 5 μm).
(4) Aerogel composites
The fiber matrix of the composite chromium sesquioxide is impregnated by using silica sol, and the impregnation mode can be vacuum impregnation, pressure impregnation or vacuum-pressure impregnation. After the sol-gel reaction and aging, the solvent is replaced and dried. Sol-gel reaction, aging and solvent displacement of silica sols are all techniques known to those skilled in the art. The solvent substitution can be performed using a substitution solvent such as acetone. The drying method is not particularly limited in the present invention, but a supercritical drying method is preferably used, and a supercritical carbon dioxide drying method is particularly preferably used, and these drying methods are known in the art.
(5) Moisture resistant treatment
By subjecting the siloxane reagent to gas phase hydrophobic treatment at a high temperature of, for example, 100 to 150 ℃, introduction of impurities is controlled, and a wave-transmitting and heat-insulating material which is capable of preventing moisture and is excellent in high-temperature heat-insulating effect can be obtained.
The preparation method of the invention is shown in figure 1, the wave-transparent fiber is used as a reinforcement, a chromic oxide opacifier with controllable particle size is doped inside the wave-transparent fiber, silica wet gel is prepared by a sol-gel method, and the high-temperature resistant anti-radiation wave-transparent heat-insulating material is finally obtained by aging, solvent replacement, supercritical drying and damp-proof treatment.
The invention also provides a high-temperature resistant radiation wave-transparent heat-insulating material in a second aspect, which comprises wave-transparent fibers and chromic oxide with the particle size of 2-5 μm (such as 2, 3, 4 or 5 μm).
In some preferred embodiments, the wave-transparent fibers are quartz fibers or mullite fibers, or alumina fibers.
In other preferred embodiments, the high temperature resistant radiation wave-transparent heat-insulating material has a dielectric constant of 1.2-1.5 and a loss tangent in a temperature range of 25 ℃ to 1200 ℃<5×10-3And the sum wave transmission rate is more than or equal to 90 percent;
more preferably, the high temperature resistant radiation wave-transparent thermal insulation material is prepared by the method of the first aspect of the invention.
The invention also provides a wave-transparent and heat-insulating member in a third aspect, which is characterized in that the wave-transparent and heat-insulating member is made of the high-temperature radiation-resistant wave-transparent and heat-insulating material obtained by the method in the first aspect of the invention or the high-temperature radiation-resistant wave-transparent and heat-insulating material in the second aspect of the invention, and more preferably, the wave-transparent and heat-insulating member is selected from the group consisting of a hemispherical member, a quasi-hemispherical member, a conical member and a special-shaped surface member.
The present invention is described in detail below with reference to specific examples, but the scope of the present invention is not limited to these examples.
Example 1
Mixing chromium nitrate according to the weight ratio of 1: 2, dissolving the mixture in an ethanol solvent, stirring the mixture for about 20min to completely dissolve the mixture, slowly adding an ammonia water solution with the concentration of 1M into a chromium nitrate solution, slowly dropwise adding the solution until the pH value of the solution is 8, continuously stirring the solution for 30min to obtain a chromium salt complex solution, and then injecting the solution with the density of 0.1g/cm by adopting a vacuumizing mode3In the quartz fiber-reinforced matrix,after sol-gel, putting the fiber into a drying oven at 100 ℃ for drying, then putting the fiber into a muffle furnace at 600 ℃ for processing for 2h, then putting the fiber preform into a mold, carrying out composite molding on the silica sol and the preform by adopting a vacuum compacting molding mode, then carrying out room-temperature aging for 36h and high-temperature aging at 90 ℃ for 36h, carrying out acetone solvent replacement for 2 times after aging, then carrying out supercritical carbon dioxide drying, and then carrying out gas-phase hydrophobic moisture-proof treatment on methyltrimethoxysilane to obtain a heat-insulating sample. The density of the high-temperature resistant wave-transparent heat-insulation member obtained in the example is 0.35g/cm3The temperature resistance is 1200 ℃, the room temperature thermal conductivity is 0.022W/m.K (according to the standard GB/T10295--3The wave-transmitting rate of the spherical heat-insulating cover is more than or equal to 90 percent, the sample piece with the size of 150mm multiplied by 20mm has the temperature of 1000 ℃, and the temperature of the back surface of a quartz lamp for examination of 1000s is 108 ℃ lower than that of a quartz fiber reinforced aerogel material with the same specification.
Example 2
Mixing chromium acetate according to the weight ratio of 1: 3 dissolving in water solvent, stirring for 25min to dissolve completely, slowly adding 1M ammonia water solution into chromium acetate solution, slowly adding dropwise until pH is 8, stirring for 30min to obtain chromium salt complex solution, and vacuum injecting into solution with density of 0.1g/cm3Putting the mullite fiber reinforced matrix into a 100 ℃ oven for drying after sol-gel treatment, then putting the mullite fiber reinforced matrix into a 600 ℃ muffle furnace for treatment for 2 hours, then putting the fiber preform into a mold, carrying out composite molding on the silica sol and the preform by adopting a vacuum compacting molding mode, then carrying out room temperature aging for 36 hours and high temperature aging at 90 ℃ for 36 hours, carrying out acetone solvent replacement for 2 times after aging, then carrying out supercritical drying, and then carrying out gas phase hydrophobic moisture-proof treatment on methyltrimethoxysilane to obtain a heat-insulating sample. The density of the high-temperature resistant wave-transparent heat-insulation member obtained in the example is 0.30g/cm3The temperature resistance is 1200 ℃, the room temperature thermal conductivity is 0.022W/m.K (according to the standard GB/T10295-200 ℃ below 5X 10-3The wave-transmitting rate of the spherical heat-insulating cover is more than or equal to 94 percent, the sample piece with the size of 150mm multiplied by 20mm has the temperature of 1000 ℃, and the temperature of the back surface of a 1000s quartz lamp for examination is 126 ℃ lower than that of a quartz fiber reinforced aerogel material with the same specification.
Example 3
Mixing chromium phosphate according to the weight ratio of 1: 1 is dissolved in hydrosolvent, then stirred for about 20 min-30 min to be completely dissolved, then ammonia water solution with the concentration of 1M is slowly added into chromium acetate solution, slowly dropwise added until the PH value of the solution is 8, the stirring is continued for 30min to obtain chromium salt complex solution, and then the solution is injected into the solution with the density of 0.1g/cm by adopting a vacuumizing mode3After sol-gel is formed in an alumina fiber reinforced matrix, the alumina fiber reinforced matrix is placed in a 100 ℃ drying oven to be dried, then the alumina fiber reinforced matrix is placed in a 600 ℃ muffle furnace to be processed for 2 hours, then a fiber preform is placed in a mold, silica sol and the preform are compounded and formed in a vacuum compacting forming mode, then room temperature aging is carried out for 36 hours, high temperature aging is carried out for 36 hours at 90 ℃ and is carried out for 2 times through acetone solvent replacement after aging is finished, then supercritical drying is carried out, and then gas phase hydrophobic moisture-proof processing is carried out through methyltrimethoxysilane to obtain a heat insulation sample. The density of the high-temperature resistant wave-transparent heat-insulation member obtained in the example is 0.35g/cm3The temperature resistance is 1200 ℃, the room temperature thermal conductivity is 0.022W/m.K (according to the standard GB/T10295--3The wave-transmitting rate of the spherical heat-insulating cover is more than or equal to 92 percent, the sample piece with the size of 150mm multiplied by 20mm has the temperature of 1000 ℃, and the temperature of the back surface of a 1000s quartz lamp for examination is 98 ℃ lower than that of a quartz fiber reinforced aerogel material with the same specification.
Example 4
Mixing chromium phosphate according to the weight ratio of 1: 1 is dissolved in water solvent, then stirred for about 30min to be completely dissolved, then ammonia water solution with the concentration of 1M is slowly added into chromium acetate solution, slowly dropwise added until the PH value of the solution is 8, the stirring is continued for 30min to obtain chromium salt complex solution, and then the solution is injected into the solution with the density of 0.1g/cm by adopting a vacuumizing mode3In a quartz fiber-reinforced matrix, to be sol-gelAnd then placing the fiber preform into a 100 ℃ drying oven for drying, then placing the fiber preform into a 700 ℃ muffle furnace for processing for 3h, then placing the fiber preform into a mold, carrying out composite molding on the silica sol and the preform by adopting a vacuum compacting molding mode, then carrying out room temperature aging for 36h, carrying out high temperature aging at 90 ℃ for 36h, carrying out solvent replacement for 2 times after aging, then carrying out supercritical drying, and then carrying out gas phase hydrophobic moisture-proof treatment by adopting methyltrimethoxysilane to obtain a heat-insulating sample piece. The density of the high-temperature resistant wave-transparent heat-insulation member obtained in the example is 0.35g/cm3The temperature resistance is 1200 ℃, the room temperature thermal conductivity is 0.022W/m.K (according to the standard GB/T10295--3The wave transmittance of the spherical heat shield is more than or equal to 90 percent, the sample piece with the size of 150mm multiplied by 20mm has the temperature of 1000 ℃, and the temperature of the back surface of a quartz lamp for examination of 1000s is 103 ℃ lower than that of the quartz fiber reinforced aerogel material with the same specification.
Example 5
Mixing chromium acetate according to the weight ratio of 1: 3 dissolving in ethanol solvent, stirring for about 25min to dissolve completely, slowly adding 1M ammonia water solution into chromium nitrate solution, slowly dropwise adding until the pH value of the solution is 8, continuously stirring for about 30min to obtain chromium salt complex solution, and injecting into a container with density of 0.1g/cm by vacuum pumping3Putting the mullite fiber reinforced matrix into a 100 ℃ oven for drying after sol-gel treatment, then putting the mullite fiber reinforced matrix into a 800 ℃ muffle furnace for treatment for 2 hours, then putting the fiber preform into a mold, carrying out composite molding on the silica sol and the preform by adopting a vacuum compacting molding mode, then carrying out room temperature aging for 36 hours and high temperature aging at 90 ℃ for 36 hours, carrying out acetone solvent replacement for 2 times after aging, then carrying out supercritical drying, and then carrying out gas phase hydrophobic moisture-proof treatment by adopting a methyltrimethoxysilane reagent to obtain a heat-insulating sample. The density of the high-temperature resistant wave-transparent heat-insulation member obtained in the example is 0.32g/cm3The temperature resistance is 1200 ℃, the room temperature thermal conductivity is 0.023W/m.K (according to the standard GB/T10295-2008), the dielectric constant of the Ku wave band between room temperature and 1200 ℃ is lower than 1.33, and the loss tangent is lower than 5 multiplied by 10 between room temperature and 1200 DEG C-3The wave transmittance of the spherical heat shield is more than or equal to 95 percent, the sample piece with the size of 150mm multiplied by 20mm has the temperature of 1000 ℃, and the temperature of the back surface of a quartz lamp for 1000s examination is 110 ℃ lower than that of the quartz fiber reinforced aerogel material with the same specification.
Example 6
Mixing chromium acetate according to the weight ratio of 1: 3 dissolving in ethanol solvent, stirring for 25min to dissolve completely, slowly adding 1M ammonia water solution into chromium nitrate solution, slowly dropwise adding until the pH value of the solution is 8, continuously stirring for 30min to obtain chromium salt complex solution, and injecting into a container with density of 0.1g/cm by vacuum pumping3Putting the mullite fiber matrix into a 100 ℃ drying oven after sol-gel treatment, then putting the mullite fiber matrix into a 600 ℃ muffle furnace for heat preservation treatment for 1h, continuing to heat to 700 ℃ for further treatment for 1h, heating to 800 ℃ for heat preservation for 1h, then putting the fiber preform into a mold, carrying out composite molding on the silica sol and the preform by adopting a vacuum compacting molding mode, then carrying out room temperature aging for 36h and 90 ℃ high temperature aging for 36h, carrying out acetone solvent replacement for 2 times after aging is completed, then carrying out supercritical drying, and then carrying out gas phase hydrophobic moisture-proof treatment by adopting methyltrimethoxysilane to obtain a heat-insulating sample piece. The density of the high-temperature resistant wave-transparent heat-insulation member obtained in the example is 0.38g/cm3The temperature resistance is 1200 ℃, the room temperature thermal conductivity is 0.023W/m.K (according to the standard GB/T10295-2008), the dielectric constant of the Ku wave band between room temperature and 1200 ℃ is lower than 1.36, and the loss tangent is lower than 5 multiplied by 10 between room temperature and 1200 DEG C-3The wave transmittance of the spherical heat shield is more than or equal to 91 percent, the sample piece with the size of 150mm multiplied by 20mm has the temperature of 1000 ℃, and the temperature of the back surface of a quartz lamp for 1000s examination is 125 ℃ lower than that of the quartz fiber reinforced aerogel material with the same specification.
Example 7
The procedure was carried out in substantially the same manner as in example 1 except that the same molar part of chromium sesquioxide was directly used in place of the chromium salt complex solution, and as a result, it was found that since chromium sesquioxide was not uniformly distributed in the silica sol, the entire density of the sample was not uniform, the dielectric constant of a part of the sample was more than 1.4, the wave transmittance was 85%, and the temperature of the back surface of the sample examined with a quartz lamp having a size of 150mm × 150mm × 20mm was comparable to the temperature of the back surface of the quartz fiber-reinforced aerogel material having the same specification at 1000 ℃ for 1000s due to local increase in heat conduction through the solid phase.
Example 8
The procedure was carried out in substantially the same manner as in example 1, except that the sintering step was not carried out. As a result, when a sample is sampled and subjected to XRD test, no stable crystal form exists, and no transparent mode radiation-resistant chromium oxide is generated.
The inventors also observed the particle size of the opacifier particles in the insulation samples and the results are shown in table 1 below.
Table 1 shows the average particle diameter (n ═ 5) and the maximum particle diameter (μm) of the light-shading agent particles in each example.
| Examples | Average particle size (μm) of sunscreen particles | Opacifier particle maximum particle size (mum) |
| 1 | 3.25 | 4.94 |
| 2 | 2.37 | 4.12 |
| 3 | 2.22 | 4.78 |
| 4 | 3.56 | 4.23 |
| 5 | 2.48 | 4.86 |
| 6 | 3.47 | 4.88 |
| 7 | 4.21 | 7.62 |
| 8 | Is free of | Is free of |
The invention has not been described in detail and is in part known to those of skill in the art.
Claims (12)
1. A high-temperature-resistant radiation wave-transparent heat-insulating material is characterized in that:
the high-temperature-resistant radiation wave-transparent heat-insulating material comprises wave-transparent fibers and chromium sesquioxide with the particle size of 2 mu m ~ 5 mu m;
the transmission mode fiber is selected from the group consisting of quartz fiber, mullite fiber and alumina fiber;
the high-temperature resistant radiation wave-transmitting heat-insulating material has the dielectric constant of 1.2 ~ 1.5.5 and the loss tangent in the temperature range of 25-1200 DEG C<5×10-3And the sum wave transmission rate is more than or equal to 90 percent;
the high-temperature-resistant radiation wave-transparent heat-insulating material is prepared by the following preparation method, and the preparation method comprises the following steps:
(1) preparation of chromium salt complex: diluting and dissolving trivalent chromium salt in a proper amount of solvent, and adding an alkaline reagent to obtain a chromium salt complex solution;
(2) dipping: soaking the wave-transmitting fiber reinforcement by using a chromium salt complex solution, and drying after sol-gel to obtain a fiber preform;
(3) and (3) sintering: sintering the fiber preform to obtain a chromium sesquioxide composite fiber reinforced matrix;
(4) compounding the aerogel: soaking the chromium sesquioxide composite fiber reinforced matrix by using silica sol, and obtaining a fiber reinforced aerogel composite material through sol-gel, aging, solvent replacement and drying;
(5) moisture-proof treatment: and carrying out moisture-proof treatment on the fiber-reinforced aerogel composite material to obtain the high-temperature-resistant radiation wave-transparent heat-insulating material.
2. The high temperature resistant radiation wave-transparent thermal insulation material of claim 1, wherein:
in the preparation method, in the step (4), the drying is supercritical drying.
3. The high temperature resistant radiation wave-transparent thermal insulation material of claim 1, wherein:
in the preparation method, in the step (4), the drying is supercritical carbon dioxide drying.
4. The high temperature resistant radiation wave-transparent thermal insulation material of claim 3, wherein:
in the preparation method, the raw materials are mixed,
the trivalent chromium salt is selected from the group consisting of chromium acetate, chromium sulfate, and chromium nitrate;
the diluting solvent is selected from the group consisting of ethanol and water;
the fiber in the wave-transmitting fiber reinforcement body is quartz fiber, mullite fiber or alumina fiber;
the alkaline reagent is a weakly alkaline reagent.
5. The high temperature resistant radiation wave-transparent thermal insulation material of claim 4, wherein:
the alkaline reagent is ammonia water.
6. The high temperature resistant radiation wave-transparent thermal insulation material of claim 4, wherein:
the alkaline reagent is 0.5M to 1.5M ammonia water.
7. The high temperature resistant radiation wave-transparent thermal insulation material of claim 4, wherein:
the alkaline agent is added in an amount such that the pH of the system is 7 to 8.
8. The high temperature resistant radiation wave-transparent thermal insulation material of claim 1, wherein:
in the preparation method, the drying temperature in the step (2) is 50 ~ 60 ℃;
the sintering temperature in the step (3) is 600 ~ 800 ℃, and the sintering time is 2h ~ 6 h.
9. The high temperature resistant radiation wave-transparent thermal insulation material of claim 1, wherein:
in the preparation method, the dosage of the trivalent chromium salt is such that the mass ratio of the chromium sesquioxide to the wave-transmitting fiber reinforcement is 1:0.05 ~ 0.15.15.
10. The high temperature resistant radiation wave-transparent thermal insulation material of claim 1, wherein:
in the preparation method, the impregnation mode in the step (2) and/or the step (4) is vacuum impregnation and/or pressure impregnation.
11. A wave-transparent thermal insulation member characterized in that:
the wave-transparent thermal insulation member is made of the high temperature resistant radiation wave-transparent thermal insulation material according to any one of claims 1 to 10.
12. The wave-transparent insulation member according to claim 11, wherein: the wave-transparent thermal insulation member is selected from the group consisting of a hemispherical member, a quasi-hemispherical member, a conical member, and a profiled surface member.
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| CN108383486B (en) * | 2016-11-16 | 2019-12-24 | 航天特种材料及工艺技术研究所 | High-temperature-resistant radiation wave-transparent heat-insulating material and preparation method thereof |
| CN108793984B (en) * | 2018-07-13 | 2021-02-09 | 航天材料及工艺研究所 | High-temperature-resistant heat-insulation wave-transparent function integrated composite material and preparation method thereof |
| CN109607551B (en) * | 2018-12-11 | 2021-07-09 | 航天特种材料及工艺技术研究所 | Silicon dioxide aerogel composite material and preparation method and application thereof |
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| CN111943654B (en) * | 2020-08-18 | 2022-04-12 | 航天特种材料及工艺技术研究所 | High-temperature-resistant and radiation-resistant aerogel composite material and preparation method thereof |
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| CN112522852B (en) * | 2020-12-02 | 2022-05-03 | 航天特种材料及工艺技术研究所 | Heat insulation material with controllable structure and preparation method thereof |
| CN112552064A (en) * | 2020-12-28 | 2021-03-26 | 航天特种材料及工艺技术研究所 | Light wave-transparent ceramic heat-insulating material and preparation method thereof |
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