CN108383486A - A kind of high temperature resistant radiation wave transparent heat-barrier material and preparation method thereof - Google Patents
A kind of high temperature resistant radiation wave transparent heat-barrier material and preparation method thereof Download PDFInfo
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- CN108383486A CN108383486A CN201810220871.2A CN201810220871A CN108383486A CN 108383486 A CN108383486 A CN 108383486A CN 201810220871 A CN201810220871 A CN 201810220871A CN 108383486 A CN108383486 A CN 108383486A
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- wave transparent
- high temperature
- barrier material
- temperature resistant
- transparent heat
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- 239000000463 material Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 230000005855 radiation Effects 0.000 title claims abstract description 24
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000000835 fiber Substances 0.000 claims abstract description 49
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 46
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 28
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000004964 aerogel Substances 0.000 claims abstract description 20
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 20
- 239000011651 chromium Substances 0.000 claims abstract description 20
- 230000032683 aging Effects 0.000 claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 18
- 239000002131 composite material Substances 0.000 claims abstract description 16
- 150000003839 salts Chemical class 0.000 claims abstract description 15
- 239000011159 matrix material Substances 0.000 claims abstract description 14
- 239000012266 salt solution Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 12
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 230000002787 reinforcement Effects 0.000 claims abstract description 10
- 150000001875 compounds Chemical class 0.000 claims abstract description 9
- 238000006073 displacement reaction Methods 0.000 claims abstract description 6
- 239000010453 quartz Substances 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 17
- 230000005540 biological transmission Effects 0.000 claims description 10
- 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 10
- 238000005245 sintering Methods 0.000 claims description 10
- 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
- 238000007598 dipping method Methods 0.000 claims description 6
- 239000013306 transparent fiber Substances 0.000 claims description 6
- 238000005470 impregnation Methods 0.000 claims description 5
- 229910052863 mullite Inorganic materials 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000908 ammonium hydroxide Substances 0.000 claims description 4
- 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 4
- 239000000654 additive Substances 0.000 claims description 3
- 230000000996 additive effect Effects 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims 2
- 239000001569 carbon dioxide Substances 0.000 claims 1
- 229910002092 carbon dioxide Inorganic materials 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 4
- 239000000499 gel Substances 0.000 description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 12
- 239000003605 opacifier Substances 0.000 description 12
- 238000000465 moulding Methods 0.000 description 10
- 239000002245 particle Substances 0.000 description 8
- 230000002209 hydrophobic effect Effects 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- 238000012546 transfer Methods 0.000 description 7
- 238000003483 aging Methods 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 6
- 238000005056 compaction Methods 0.000 description 6
- 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
- 238000003756 stirring Methods 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000002708 enhancing effect Effects 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000009738 saturating Methods 0.000 description 4
- 239000004965 Silica aerogel Substances 0.000 description 3
- 239000003125 aqueous solvent Substances 0.000 description 3
- 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
- 238000012216 screening Methods 0.000 description 3
- -1 Small molecule organic compound Chemical class 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 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
- 238000009413 insulation Methods 0.000 description 2
- 239000011490 mineral wool Substances 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000002210 supercritical carbon dioxide drying Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000036760 body temperature Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000012774 insulation material Substances 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
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000007783 nanoporous material Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 230000000191 radiation effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 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
- 239000011343 solid material 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
- 239000011240 wet gel Substances 0.000 description 1
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- 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
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- 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
- 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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- 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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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- 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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- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
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Abstract
The present invention provides a kind of preparation method of high temperature resistant radiation wave transparent heat-barrier material.Specifically, the method for the present invention includes：Chromic salt is diluted and is dissolved, alkaline reagent is added, obtains chromium complex salt solution；Wave transparent fibre reinforcement is impregnated using chromium complex salt solution, it is dry after collosol and gel, obtain fiber preform；Fiber preform is sintered, the compound fibre reinforced matrix of chrome green is obtained；Fibre reinforced matrix is impregnated using silicon dioxide gel, through collosol and gel, aging, solvent displacement, drying, obtains fibre-reinforced aerogel composite；Damp-proof treatment is carried out to fibre-reinforced aerogel composite, obtains high temperature resistant radiation wave transparent heat-barrier material.The present invention also provides high temperature resistant radiation wave transparent heat-barrier material and its applications.The method of the present invention can control chrome green grain size and crystal form, ensure that material of the present invention has excellent high temperature radiation resistance and dielectric properties.
Description
This case is November 16 2016 applying date, and application number 201611025658.3, " a kind of high temperature resistant radiation is saturating for title
The divisional application of wave heat-barrier material and preparation method thereof ".
Technical field
The present invention relates to a kind of high temperature resistants to radiate wave transparent heat-barrier material and preparation method thereof, belongs to thermal protection technology field.
Background technology
Aerogel material is a kind of novel low density nano-porous materials, is the best solid material of current heat-proof quality,
Aeroge is mutually built up by nano particle and is formed, and has three-dimensional network nano-porous structure, can significantly decrease consolidating for material
Body heat conduction, convection current heat transfer and radiant heat transfer, and the near-infrared wavelength of 2~10 μm of aeroge pair is nearly transparent, and under high temperature, radiation
The effect of heat transfer is fairly obvious, if being not added with any counter infrared ray opacifier, the high temperature insulating effect of aeroge reduces, and opacifier is added
The ratio that each heat transfer path in aeroge can be changed afterwards studies work mostly since the mechanism of radiant heat transfer under high temperature is more complicated
Theoretical qualitative analysis is only rested on, the present inventor is by deep experiment and combines a large amount of theory analysis, it is proposed that a kind of resistance to height
The preparation method and high temperature resistant obtained by this method of temperature radiation wave transparent heat-barrier material radiate wave transparent heat-barrier material.
Research for aeroge high temperature insulating effect is many, the preparation method of opacifier and aerogel composite have with
Under several classes：(1) carbon black, silicon carbide infrared light screening agent are added in aerogel material, preparing can be under 1200 degrees celsius
The high temperature insulating used aerogel composite (referring to CN201410456744.4, a kind of entitled airsetting of high temperature insulating
Glue composite material), but there are preparation method trivial operations, the problems such as needing layering to make and need with a variety of opacifiers.(2)
Infrared light screening agent titanium dioxide is added in aeroge, then composite material (ginseng is prepared by collosol and gel and supercritical drying
See CN200510031952.0, entitled a kind of aerogel heat-insulating composite material and preparation method thereof).(3) in silica aerogel
Middle doping fiber, opacifier etc. be prepared intensity is high and heat-proof quality is good aerogel heat-insulating material (referring to
CN200510012154.3, a kind of entitled preparation method of stephanoporate powder doped silica aerogel heat-insulation material).However,
There is no the chromium complex salts for using high-purity for these patents, and without passing through high temperature sintering step, can not remove in raw material
Small molecule organic compound and metal impurities, opacifier particle diameter difference is excessive and uncontrollable, and it is even more impossible to be formed as expected
It is in the chrome green crystal grain of appropriate particle size range, therefore cannot get expected room temperature thermal conductivity, dielectric constant and loss angle
Tangent so that it is insufficient that high temperature resistant radiates wave transparent heat-proof quality.
Invention content
In order to overcome the shortage of prior art, and a kind of heat insulation stable the present invention provides electrical properties in high temperatures is excellent
High temperature resistant radiates wave transparent heat-barrier material and its preparation method and application.
The present invention provides a kind of preparation method of high temperature resistant radiation wave transparent heat-barrier material, the method packet in first aspect
Include following steps：
(1) preparation of chromium complex salt：Chromic salt is diluted in retarder thinner, alkaline reagent is added, obtains chromic salts
Complex solution；
(2) it impregnates：Wave transparent fibre reinforcement is impregnated using the chromium complex salt solution, it is dry after sol-gel, it obtains
To fiber preform；
(3) it is sintered：The fiber preform is sintered, the compound fibrous matrix of chrome green is obtained；
(4) aeroge is compound：Impregnate the fibre reinforced matrix using silicon dioxide gel, through sol-gel, aging,
Solvent displacement, drying, obtain fibre-reinforced aerogel composite；
(5) damp-proof treatment：Damp-proof treatment is carried out to fibre-reinforced aerogel composite, obtains the high temperature resistant radiation
Wave transparent heat-barrier material.
The present invention provides a kind of high temperature resistant in second aspect and radiates wave transparent heat-barrier material, the high temperature resistant radiation wave transparent every
Hot material includes wave transparent fiber type and chrome green.
The present invention provides a kind of wave transparent heat insulating component in the third aspect, and the wave transparent heat insulating component is by first party of the present invention
High temperature resistant radiation wave transparent heat-barrier material made from method described in face or the high temperature resistant radiation described in second aspect of the present invention are saturating
Wave heat-barrier material is made.
The present invention at least has the advantages that compared with prior art：
(1) high temperature resistant radioresistance wave transparent heat-barrier material prepared by the present invention breaches theoretic analysis, and preparing can
Under the conditions of meeting 1200 DEG C of high temperature, the working time >=2500s；And density is adjustable, range is in 0.25g/cm3~0.4g/cm3；Meet
The requirement that high temperature wave transparent performance is stablized, and heat insulation is substantially better than common aerogel material, can be used as High Mach number and
The thermal protection of wireless device uses in long endurance aircraft.
(2) wave transparent heat insulating component made from the saturating glass heat-barrier material of high temperature resistant radioresistance prepared by the present invention has good
Electrical property, under conditions of 1200 DEG C, dielectric constant is 1.2~1.5, loss angle tangent<5×10-3；Wave transmission rate >=90%.
(3) present invention can be used for preparing the wave transparent heat insulating component of Multiple Type specification, such as hemispherical, class hemispherical, taper
And various large-sized special-shaped surface members have directive significance particularly with the production of special-shaped rigid wave transparent heat insulating component.
Description of the drawings
Fig. 1 is the process flow chart of preparation method of the present invention.
Specific implementation mode
The present invention radiates wave transparent heat-barrier material and preparation method thereof providing a kind of high temperature resistant, and the heat-barrier material includes
Silica aerogel material and infrared light screening agent chrome green.Chrome green chromic salts selected when preparing can
Think selected from the group being made of chromium acetate, chromium sulfate and chromic nitrate；In the preparation method, sintering temperature can be 600~800
DEG C (such as 600,700 or 800 DEG C), sintering time can be 2h~6h (such as 2,3,4,5 or 6 hours)；Grain size can be 2 μm
~5 μm (such as 2,3,4 or 5 μm)；The mass ratio of chrome green and wave transparent fibre reinforcement can be in the heat-barrier material
1：0.05~0.15 (such as 1：0.05、1：0.10 or 1：0.15).
The inventors discovered that chrome green is good opacifier, and the electromagnetic wave transparent material having stable high-temperature performance, in height
Under the conditions of 1200 DEG C of temperature, the dielectric constant and loss angle tangent of the chrome green of cubic are very low, and intracell does not occur
Large change adjusts the synthesis mode, grain size or additive amount of chrome green by the way that chromic salts is formed chromium complex salt,
Chrome green can be made to be evenly distributed in aeroge so that electric performance stablity, and infrared shading performance at high temperature
It is excellent.
In some preferred embodiments, the present invention is by adjusting the content of chrome green, grain size and/or crystal form
Deng making aerogel composite radiation thermal conduction and the efficiency of solid phase heat transfer maximize, ensure that whole high temperature resistant radiation
Effect；Furthermore it is possible to which complexing mode and/or sintering procedure by controlling chrome green, can control chrome green and exist
Being uniformly distributed in aeroge, and then ensure that the stability of electrical property.
Specifically, the present invention provides a kind of preparation method of high temperature resistant radioresistance wave transparent heat-barrier material, the method
Include the following steps：
(1) preparation of chromium complex salt
In the present invention by taking chromic nitrate, chromium phosphate or chromium acetate as an example, but not limited to this, and it is (such as pure that water is added wherein
Water purification) or alcoholic solution dissolved dilution, certain density alkalescent solvent is added later, it is 7~8 to control its pH value, is sufficiently stirred
Uniformly, chromium complex salt solution is obtained；In the present invention adjust chromium complex salt dosage and concentration so that chrome green with thoroughly
The mass ratio of wave fibre reinforcement is 1：0.05~0.15.
(2) it impregnates
Wave transparent fibre reinforcement is impregnated using the chromium complex salt solution；In the present invention, wave transparent fibre reinforcement institute
The saturating glass dimension selected can be selected from the group being made of quartz fibre, mullite fiber and alumina fibre；The dipping of use
Mode can be vacuum impregnation, suppress dipping or vacuum-suppresses dipping.Alkaline reagent can be alkalescent reagent, more preferably
Ammonium hydroxide, further preferably 0.5M are to the ammonium hydroxide of 1.5M, and most preferably, the additive amount of alkaline reagent so that the pH of system is 7
To 8.Drying in the step can be carried out at 100 DEG C, until drying.
(3) it is sintered
Selected high temperature sintering temperature is 600 DEG C~800 DEG C (such as 600,700 or 800 DEG C) in the present invention, total to be sintered
Time is 2h~6h (such as 2,3,4,5 or 6 hours).In some embodiments, different temperature program(me)s, which may be used, to be walked
Suddenly the fiber preform that (2) obtain carries out high temperature sintering, obtains the compound fibrous matrix of chrome green.The temperature programming stage can
Be, for example, 600 DEG C of (a), soaking time be 1h~2h or (b) 700 DEG C of soaking times be 1h~2h or (c) 800 DEG C keep the temperature when
Between to be one or more in 1h~2h so that the grain size of the chrome green formed after sintering be 2 μm~5 μm (such as
2,3,4 or 5 μm).
(4) aeroge is compound
Impregnate the fibrous matrix of compound chrome green using silicon dioxide gel, impregnation method can be vacuum impregnation,
It suppresses dipping or vacuum-suppresses dipping.Through sol gel reaction, after the completion of waiting for its aging, solvent displacement and drying are carried out.Two
Solgel reaction, aging and the solvent displacement of silica sol are all known to the skilled in the art technology.Solvent is replaced
The displacement solvent such as acetone can be used for example to carry out.The present invention is not particularly limited drying mode, it is preferred that using
Supercritical drying mode particularly preferably uses supercritical carbon dioxide drying mode, these drying modes are all known in the art
Technology.
(5) damp-proof treatment
Gas phase hydrophobic treatment is carried out using the high temperature for example at 100 DEG C to 150 DEG C by silicone agent, controls impurity
It introduces, can obtain being capable of moisture-proof and high temperature insulating excellent effect wave transparent heat-barrier material.
For preparation method of the present invention as shown in Figure 1, the present invention uses wave transparent fiber type as reinforcement, inside doping grain size can
The chrome green opacifier of control prepares silica wet gel by sol-gel process, replaced using aging, solvent,
Supercritical drying and damp-proof treatment finally obtain high temperature resistant radioresistance wave transparent heat-barrier material.
The present invention additionally provides a kind of high temperature resistant radiation wave transparent heat-barrier material in second aspect, and the high temperature resistant radiates wave transparent
Heat-barrier material includes wave transparent fiber type and the chrome green that grain size is 2 μm~5 μm (such as 2,3,4 or 5 μm).
In some preferred embodiments, the wave transparent fiber type is quartz fibre or mullite fiber or aluminium oxide
Fiber.
In other preferred embodiment, the high temperature resistant radiates wave transparent heat-barrier material at 25 DEG C to 1200 DEG C
Temperature range, dielectric constant are 1.2~1.5, loss angle tangent<5×10-3And wave transmission rate >=90%；
It is further preferred that the high temperature resistant radiation wave transparent heat-barrier material is made by the method described in first aspect present invention.
The present invention additionally provides a kind of wave transparent heat insulating component in the third aspect, which is characterized in that the wave transparent heat insulating component
Described in the high temperature resistant radiation wave transparent heat-barrier material made from the method described in first aspect present invention or second aspect of the present invention
High temperature resistant radiation wave transparent heat-barrier material be made, it is further preferred that the wave transparent heat insulating component be selected from by hemispherical member, class
The group of hemispherical member, cone-shaped component and Special-Shaped Surface component composition.
Below in conjunction with specific embodiment, the present invention will be described in detail, but protection scope of the present invention is not limited to these implementations
Example.
Embodiment 1
By chromic nitrate according to 1：2 are dissolved into alcohol solvent, are then stirred, mixing time about 20min, make it completely
The ammonia spirit of a concentration of 1M, is slowly added into chromium nitrate solution, is slowly added dropwise, until the pH value of solution is by dissolving later
8, continue to stir 30min, obtains chromium complex salt solution, the mode of vacuumizing will be used to inject density for 0.1g/cm later3Quartz
In fibre reinforced matrix, puts it into 100 DEG C of baking ovens and dry after its sol-gel, be then placed in 600 DEG C of Muffle furnace
Carry out processing 2h, then fiber preform be put into mold, using vacuum compaction molding mode by silicon dioxide gel with it is prefabricated
Bluk recombination is molded, and is carried out aged at room temperature 36 hours, 90 DEG C of high temperature ageings 36 hours later, is carried out acetone solvent after the completion of aging and set
It changes 2 times, then carries out supercritical carbon dioxide drying, then methyltrimethoxysilane is used to carry out the hydrophobic damp-proof treatment of gas phase,
Obtain heat-insulated exemplar.The high temperature resistant wave-permeable heat insulating component density that this example obtains is 0.35g/cm3, 1200 DEG C of heatproof, room temperature heat
Conductance is 0.022W/mK (establishing criteria GB/T 10295-2008), and Ku wave bands room temperature to 1200 DEG C of dielectric constants is less than
1.35, loss angle tangent is less than 5 × 10 in room temperature~1200 DEG C-3, wave transmission rate >=90% of spherical heat shield, size 150mm ×
The back temperature of 1000 DEG C of the exemplar of 150mm × 20mm, the quartz lamp examination of 1000s enhances than the quartz fibre of same specification
Aerogel material is 108 DEG C low.
Embodiment 2
By chromium acetate according to 1：3 are dissolved into aqueous solvent, are then stirred, mixing time about 25min, keep it completely molten
Solution, the ammonia spirit of a concentration of 1M is slowly added into chromium acetate solution later, is slowly added dropwise, until solution pH value be 8,
Continue to stir 30min, obtains chromium complex salt solution, the mode of vacuumizing will be used to inject density for 0.1g/cm later3Mullite
In fibre reinforced matrix, puts it into 100 DEG C of baking ovens and dry after its sol-gel, be then placed in 600 DEG C of Muffle furnace
Carry out processing 2h, then fiber preform be put into mold, using vacuum compaction molding mode by silicon dioxide gel with it is prefabricated
Bluk recombination is molded, and is carried out aged at room temperature 36 hours, 90 DEG C of high temperature ageings 36 hours later, is carried out acetone solvent after the completion of aging and set
It changes 2 times, then carries out supercritical drying, then methyltrimethoxysilane is used to carry out the hydrophobic damp-proof treatment of gas phase, obtained heat-insulated
Exemplar.The high temperature resistant wave-permeable heat insulating component density that this example obtains is 0.30g/cm3, 1200 DEG C of heatproof, room temperature thermal conductivity is
0.022W/mK (establishing criteria GB/T 10295-2008), Ku wave bands room temperature to 1200 DEG C of dielectric constants are less than 1.30, loss
Angle tangent is less than 5 × 10 in room temperature~1200 DEG C-3, wave transmission rate >=94% of spherical heat shield, size 150mm × 150mm ×
The back temperature of 1000 DEG C of the exemplar of 20mm, the quartz lamp examination of 1000s enhances aeroge than the quartz fibre of same specification
Material is 126 DEG C low.
Embodiment 3
By chromium phosphate according to 1：1 is dissolved into aqueous solvent, is then stirred, and mixing time about 20min~30min makes
It is completely dissolved, and the ammonia spirit of a concentration of 1M is slowly added into chromium acetate solution later, is slowly added dropwise, until solution
PH value is 8, continues to stir 30min, obtains chromium complex salt solution, the mode of vacuumizing will be used to inject density for 0.1g/ later
cm3Alumina fibre enhances in matrix, puts it into 100 DEG C of baking ovens and dries after its sol-gel, is then placed in 600 DEG C
Muffle furnace in carry out processing 2h, then fiber preform is put into mold, using vacuum compaction molding mode by silica
Colloidal sol and precast body composite molding, carry out aged at room temperature 36 hours later, and 90 DEG C of high temperature ageings 36 hours carry out after the completion of aging
Acetone solvent is replaced 2 times, then carries out supercritical drying, then methyltrimethoxysilane is used to carry out the hydrophobic moisture-proof place of gas phase
Reason, obtains heat-insulated exemplar.The high temperature resistant wave-permeable heat insulating component density that this example obtains is 0.35g/cm3, 1200 DEG C of heatproof, room temperature
Thermal conductivity is 0.022W/mK (establishing criteria GB/T 10295-2008), and Ku wave bands room temperature to 1200 DEG C of dielectric constants is less than
1.35, loss angle tangent is less than 5 × 10 in room temperature~1200 DEG C-3, wave transmission rate >=92% of spherical heat shield, size 150mm ×
The back temperature of 1000 DEG C of the exemplar of 150mm × 20mm, the quartz lamp examination of 1000s enhances than the quartz fibre of same specification
Aerogel material is 98 DEG C low.
Embodiment 4
By chromium phosphate according to 1：1 is dissolved into aqueous solvent, is then stirred, mixing time about 30min, keeps it completely molten
Solution, the ammonia spirit of a concentration of 1M is slowly added into chromium acetate solution later, is slowly added dropwise, until solution pH value be 8,
Continue to stir 30min, obtains chromium complex salt solution, the mode of vacuumizing will be used to inject density for 0.1g/cm later3It is quartzy fine
Dimension enhancing matrix in, put it into 100 DEG C of baking ovens and dry after its sol-gel, be then placed in 700 DEG C of Muffle furnace into
Row processing 3h, then is put into fiber preform in mold, using vacuum compaction molding mode by silicon dioxide gel and precast body
Composite molding, carries out aged at room temperature 36 hours later, and 90 DEG C of high temperature ageings 36 hours carry out solvent after the completion of aging and replace 2 times,
Supercritical drying is carried out again, then methyltrimethoxysilane is used to carry out the hydrophobic damp-proof treatment of gas phase, is obtained heat-insulated exemplar.This
The high temperature resistant wave-permeable heat insulating component density that example obtains is 0.35g/cm3, 1200 DEG C of heatproof, room temperature thermal conductivity is 0.022W/m
K (establishing criteria GB/T 10295-2008), Ku wave bands room temperature to 1200 DEG C of dielectric constants are less than 1.35, and loss angle tangent is in room
Temperature~1200 DEG C be less than 5 × 10-3, wave transmission rate >=90% of spherical heat shield, the exemplar of size 150mm × 150mm × 20mm
1000 DEG C, the back temperature of the quartz lamp examination of 1000s is 103 DEG C lower than the quartz fibre of same specification enhancing aerogel material.
Embodiment 5
By chromium acetate according to 1：3 are dissolved into alcohol solvent, are then stirred, mixing time about 25min, make it completely
The ammonia spirit of a concentration of 1M, is slowly added into chromium nitrate solution, is slowly added dropwise, until the pH value of solution is by dissolving later
8, continue stir about 30min, obtains chromium complex salt solution, the mode of vacuumizing will be used to inject density for 0.1g/cm later3Not
Come in mineral wool enhancing matrix, puts it into 100 DEG C of baking ovens and dry after its sol-gel, be then placed in 800 DEG C of Muffle
Carry out processing 2h in stove, then fiber preform be put into mold, using vacuum compaction molding mode by silicon dioxide gel with
Precast body composite molding carries out aged at room temperature 36 hours, 90 DEG C of high temperature ageings 36 hours, it is molten to carry out acetone after the completion of aging later
Agent is replaced 2 times, then carries out supercritical drying, then methyltrimethoxysilane reagent is used to carry out the hydrophobic damp-proof treatment of gas phase,
Obtain heat-insulated exemplar.The high temperature resistant wave-permeable heat insulating component density that this example obtains is 0.32g/cm3, 1200 DEG C of heatproof, room temperature heat
Conductance is 0.023W/mK (establishing criteria GB/T 10295-2008), and Ku wave bands room temperature to 1200 DEG C of dielectric constants is less than
1.33, loss angle tangent is less than 5 × 10 in room temperature~1200 DEG C-3, wave transmission rate >=95% of spherical heat shield, size 150mm ×
The back temperature of 1000 DEG C of the exemplar of 150mm × 20mm, the quartz lamp examination of 1000s enhances than the quartz fibre of same specification
Aerogel material is 110 DEG C low.
Embodiment 6
By chromium acetate according to 1：3 are dissolved into alcohol solvent, are then stirred, mixing time about 25min, make it completely
The ammonia spirit of a concentration of 1M, is slowly added into chromium nitrate solution, is slowly added dropwise, until the pH value of solution is by dissolving later
8, continue to stir 30min, obtains chromium complex salt solution, the mode of vacuumizing will be used to inject density for 0.1g/cm later3Mo Lai
In mineral wool matrix, put it into 100 DEG C of baking ovens and dry after its sol-gel, be then placed in 600 DEG C of Muffle furnace into
After row isothermal holding 1h, continue to be warming up to 700 DEG C continuing with 1h, is being warming up to 800 DEG C of heat preservation 1h, then fiber preform
It is put into mold, using vacuum compaction molding mode by silicon dioxide gel and precast body composite molding, it is old to carry out room temperature later
Change 36h, 90 DEG C of high temperature ageing 36h, carrying out acetone solvent after the completion of aging replaces 2 times, then carries out supercritical drying, then uses
Methyltrimethoxysilane carries out the hydrophobic damp-proof treatment of gas phase, obtains heat-insulated exemplar.The high temperature resistant wave-permeable that this example obtains is heat-insulated
Component density is 0.38g/cm3, 1200 DEG C of heatproof, room temperature thermal conductivity is 0.023W/mK (establishing criteria GB/T 10295-
2008), Ku wave bands room temperature to 1200 DEG C of dielectric constants are less than 1.36, and loss angle tangent is less than 5 × 10 in room temperature~1200 DEG C-3,
Wave transmission rate >=91% of spherical heat shield, 1000 DEG C of the exemplar of size 150mm × 150mm × 20mm, the quartz lamp of 1000s is examined
The back temperature of core is 125 DEG C lower than the quartz fibre of same specification enhancing aerogel material.
Embodiment 7
It is carried out using mode substantially the same manner as Example 1, the difference is that directly using the three of same molfraction
It aoxidizes two chromium and replaces chromium complex salt solution, as a result, it has been found that, since chrome green cannot be evenly distributed on silicon dioxide gel
In, cause sample global density uneven, Subsampling dielectric constant is more than 1.4, wave transmission rate 85%, due to solid phase heat transfer
Part aggravation, 1000 DEG C of the exemplar of size 150mm × 150mm × 20mm, the back temperature ratio of the quartz lamp examination of 1000s is same
The quartz fibre enhancing aerogel material back of the body temperature of control gauge lattice is quite.
Embodiment 8
It is carried out using mode substantially the same manner as Example 1, the difference is that, do not suffer from sintering step.As a result, it has been found that
When sampling carries out XRD tests, find exist without stable crystal form, the no radiation-resistant chrome green of wave transparent type generates.
The present inventor has also observed the grain size of opacifier particle in heat-insulated exemplar, as a result as shown in table 1 below.
Opacifier particle average grain diameter (n=5) and maximum particle diameter (μm) in 1 each embodiment of table.
| Embodiment | Opacifier particle average grain diameter (μm) | Opacifier particle maximum particle diameter (μm) |
| 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 | Nothing | Nothing |
Unspecified part of the present invention is known to the skilled person technology.
Claims (10)
1. a kind of high temperature resistant radiates wave transparent heat-barrier material, it is characterised in that：
The chrome green that the high temperature resistant radiation wave transparent heat-barrier material includes wave transparent fiber type and grain size is 2 μm~5 μm；It is preferred that
, the wave transparent fiber type is selected from the group being made of quartz fibre, mullite fiber and alumina fibre.
2. high temperature resistant according to claim 1 radiates wave transparent heat-barrier material, it is characterised in that：
Temperature range of the high temperature resistant radiation wave transparent heat-barrier material at 25 DEG C to 1200 DEG C, dielectric constant is 1.2~1.5, damage
Consume angle tangent<5×10-3And wave transmission rate >=90%.
3. high temperature resistant according to claim 1 radiates wave transparent heat-barrier material, it is characterised in that：The high temperature resistant radiates wave transparent
Heat-barrier material is made by following preparation method, and the preparation method includes the following steps：
(1) preparation of chromium complex salt：Chromic salt is diluted to dissolving in appropriate solvent, alkaline reagent is added, obtains chromic salts
Complex solution；
(2) it impregnates：Wave transparent fibre reinforcement is impregnated using chromium complex salt solution, it is dry after sol-gel, it is pre- to obtain fiber
Body processed；
(3) it is sintered：The fiber preform is sintered, the compound fibre reinforced matrix of chrome green is obtained；
(4) aeroge is compound：The fibre reinforced matrix is impregnated using silicon dioxide gel, through sol-gel, aging, solvent
Displacement, drying, obtain fibre-reinforced aerogel composite；
(5) damp-proof treatment：Damp-proof treatment is carried out to fibre-reinforced aerogel composite, obtains the high temperature resistant radiation wave transparent
Heat-barrier material.
4. high temperature resistant according to claim 3 radiates wave transparent heat-barrier material, it is characterised in that：
In the preparation method, in step (4), the drying is supercritical drying, and preferably supercritical carbon dioxide is dried.
5. high temperature resistant according to claim 3 radiates wave transparent heat-barrier material, it is characterised in that：
In the preparation method,
The chromic salt is selected from the group being made of chromium acetate, chromium sulfate and chromic nitrate；
The retarder thinner is selected from the group being made of second alcohol and water；
Fiber in the fibre reinforcement is quartz fibre, mullite fiber or alumina fibre；
The alkaline reagent is alkalescent reagent, more preferably ammonium hydroxide, the ammonium hydroxide of further preferably 0.5M to 1.5M, most preferably
, the additive amount of alkaline reagent so that the pH of system is 7 to 8.
6. high temperature resistant according to claim 3 radiates wave transparent heat-barrier material, it is characterised in that：
In the preparation method, the temperature of the drying in step (2) is 50~60 DEG C；
The temperature of step (3) described sintering is 600~800 DEG C, and sintering time is 2h~6h.
7. high temperature resistant according to claim 3 radiates wave transparent heat-barrier material, it is characterised in that：
In the preparation method, the grain size of chrome green in the compound fiber preform of chrome green that step (3) obtains
It is 2 μm~5 μm.
8. high temperature resistant according to claim 3 radiates wave transparent heat-barrier material, it is characterised in that：
In the preparation method, the dosage of chromic salt is the mass ratio so that chrome green and the wave transparent fibre reinforcement
It is 1:0.05~0.15.
9. high temperature resistant according to claim 3 radiates wave transparent heat-barrier material, it is characterised in that：
In the preparation method, the impregnation method in step (2) and/or step (4) for vacuum impregnation and/or suppresses dipping.
10. a kind of wave transparent heat insulating component, it is characterised in that：
The wave transparent heat insulating component is made by any one of claim 1 to 9 high temperature resistant radiation wave transparent heat-barrier material；It is more excellent
Choosing, the wave transparent heat insulating component are selected from by hemispherical member, class hemispherical member, cone-shaped component and Special-Shaped Surface component groups
At group.
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| CN109534779A (en) * | 2018-12-27 | 2019-03-29 | 中国建筑材料科学研究总院有限公司 | A kind of high-strength ceramic fibrous insulating material and preparation method thereof |
| CN114560679A (en) * | 2020-11-27 | 2022-05-31 | 航天特种材料及工艺技术研究所 | Efficient hydrophobic wave-transparent aerogel, and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
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| CN108383486B (en) | 2019-12-24 |
| CN107032736B (en) | 2018-02-09 |
| CN107032736A (en) | 2017-08-11 |
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