CN109016722A - A kind of antiscour aerogel composite and preparation method thereof - Google Patents
A kind of antiscour aerogel composite and preparation method thereof Download PDFInfo
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- CN109016722A CN109016722A CN201810688387.2A CN201810688387A CN109016722A CN 109016722 A CN109016722 A CN 109016722A CN 201810688387 A CN201810688387 A CN 201810688387A CN 109016722 A CN109016722 A CN 109016722A
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- 239000002131 composite material Substances 0.000 title claims abstract description 69
- 239000004964 aerogel Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 230000002787 reinforcement Effects 0.000 claims abstract description 41
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 30
- 238000007598 dipping method Methods 0.000 claims abstract description 23
- 238000000280 densification Methods 0.000 claims abstract description 6
- 239000000835 fiber Substances 0.000 claims description 106
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 39
- 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 30
- 229910052863 mullite Inorganic materials 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 27
- 239000000919 ceramic Substances 0.000 claims description 20
- 238000005470 impregnation Methods 0.000 claims description 20
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 13
- 239000010453 quartz Substances 0.000 claims description 13
- 239000000377 silicon dioxide Substances 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 11
- 238000000352 supercritical drying Methods 0.000 claims description 11
- 230000032683 aging Effects 0.000 claims description 9
- 230000002708 enhancing effect Effects 0.000 claims description 9
- 239000002243 precursor Substances 0.000 claims description 9
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 8
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 8
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 8
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 7
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 5
- 239000004917 carbon fiber Substances 0.000 claims description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 5
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 5
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 5
- 239000004890 Hydrophobing Agent Substances 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 230000001680 brushing effect Effects 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000010276 construction Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 2
- -1 methylsiloxane Chemical class 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 238000002386 leaching Methods 0.000 claims 1
- 239000010410 layer Substances 0.000 description 35
- 239000000463 material Substances 0.000 description 23
- 238000009413 insulation Methods 0.000 description 18
- 239000000047 product Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 239000005416 organic matter Substances 0.000 description 7
- 239000004744 fabric Substances 0.000 description 4
- 239000004966 Carbon aerogel Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 239000002196 Pyroceram Substances 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 239000004965 Silica aerogel Substances 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- HPNSNYBUADCFDR-UHFFFAOYSA-N chromafenozide Chemical compound CC1=CC(C)=CC(C(=O)N(NC(=O)C=2C(=C3CCCOC3=CC=2)C)C(C)(C)C)=C1 HPNSNYBUADCFDR-UHFFFAOYSA-N 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000013051 drainage agent Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- LAQFLZHBVPULPL-UHFFFAOYSA-N methyl(phenyl)silicon Chemical compound C[Si]C1=CC=CC=C1 LAQFLZHBVPULPL-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/005—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/16—Drying; Softening; Cleaning
- B32B38/164—Drying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/18—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by features of a layer of foamed material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B9/046—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material of foam
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2266/00—Composition of foam
- B32B2266/12—Gel
- B32B2266/126—Aerogel, i.e. a supercritically dried gel
Landscapes
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Nonwoven Fabrics (AREA)
Abstract
The present invention relates to a kind of preparation methods of antiscour aerogel composite, comprising: (1) the first hydrophobic reinforcement is connected with the second hydrophilic reinforcement, obtains precast body；(2) on precast body including at least the second reinforcement part through it is hydrophilic, for densification first dipping object dipping after be dried, obtain composite material；(3) hydrophilic treated is carried out to the part for including at least the first hydrophobic reinforcement on composite material, obtains antiscour aerogel composite.The invention further relates to a kind of using antiscour aerogel composite made from preparation method as described above.Antiscour aerogel composite of the invention can carry out type face machine and add, and obtain the component in required type face, or carries out overall appearance face machine after assembling aircraft and add, accurately to guarantee the aerodynamic configuration of aircraft.
Description
Technical field
The present invention relates to a kind of preparation methods of antiscour aerogel composite, further relate to a kind of using the preparation side
Antiscour aerogel composite made from method.
Background technique
High velocity of sound aircraft atmosphere or sky back and forth on the way thermal protection system surface and air Pneumatic friction generate it is high
Mild Pneumatic pressure etc., the thermally protective materials that can be born at present are rigid thermal insulation tile and ablator.
Ablator is a kind of widely used solar heat protection method of current reentry vehicle, is mainly inhaled using ablator cracking
Heat and gas diffusion take away heat, reach solar heat protection purpose, but there are density height, and heat-proof quality difference and linear ablation are fairly obvious etc.
Disadvantage.
Rigid ceramic tile is U.S. space shuttle large area thermal protection major programme, by pyroceram fibre high temperature sintering
It forms, technical maturity with higher.However, that there are brittleness is big, deformability is poor, assembly is complicated, the period for the type material
The disadvantages of length, maintenance cost is high, it is difficult to meet the thermal protection demand of the following high velocity of sound aircraft.Aerogel heat-proof composite material by
High-temperature fibre aerogel composite is prepared, and has preferable toughness, strain coordination ability and excellent thermal insulation
Energy.But mechanical strength is lower, causes surface scour resistance poor, it is impossible to be used in aircraft exterior thermal protection.
102642350 A of patent CN " a kind of high temperature resistant heat insulation sandwich structure ceramic composite and preparation method thereof "
And 103101262 A of patent CN " a kind of high temperature resistant heat insulation sandwich structure composite material and preparation method thereof ", refer to one kind three
The anti-heat-barrier material of Mingzhi's sandwich, is made of sandwich layer and upper and lower panel, and sandwich layer is fibre-reinforced aerogel material, and panel is fibre
Dimension enhancing ceramic composite, preparation method is, tiles high-temperature-resistant inorganic fibre cloth or thin sheet fabric in sandwich layer upper and lower surface, into
Hand-manipulating of needle thorn is punctured or is sutured, and is carried out combined processing to fiber cloth or thin sheet fabric, is formed upper and lower surface layer.The type material collection
The functions such as poly- effectively insulating, carrying and wave transparent are integrated, and heat-proof quality is significantly better than ablator, and impact resistance is better than space flight
Thermal insulation tile, application prospect are very extensive.However the sandwich material is related to the processes such as three layers of laying, suture, not only increases
Complex procedures degree also improves cost, and exists and be easily delaminated risk, additionally, due to surface can not machine add, the precision control of type face
Difficulty processed is big.
In view of this, the present invention is specifically proposed.
Summary of the invention
The first object of the present invention is to provide a kind of preparation method of antiscour aerogel composite, to realize optimization
The purpose of heat-proof quality；The second object of the present invention is to provide a kind of using antiscour aeroge made from the preparation method
Composite material.
To realize the first purpose, the present invention adopts the following technical scheme:
A kind of preparation method of antiscour aerogel composite, comprising:
(1) the first hydrophobic reinforcement is connected with the second hydrophilic reinforcement, obtains precast body；
(2) part of the second reinforcement is included at least on precast body through the first dipping hydrophilic, for densification
It is dried after object dipping, obtains composite material；
(3) hydrophilic treated is carried out to the part for including at least the first hydrophobic reinforcement on composite material, obtains antiscour
Aerogel composite.
In step (3), intermediate is obtained after hydrophilic treated, and the part of hydrophobic reinforcement is included at least on intermediate through hydrophilic
, for densification second dipping object dipping after be dried；
Preferably, the first dipping object includes ceramic base presoma；Second dipping object includes aerogel precursor body.
In step (1), the first hydrophobic reinforcement is obtained by carrying out hydrophobic treatment to the first hydrophilic reinforcement；
Preferably, the first reinforcement includes fibre；The raw material of fibre is high silica fiber, quartz fibre, oxygen
Change the combination of one or more of aluminum fiber, Zirconium oxide fibre, mullite fiber, carbon fiber, silicon carbide fibre；
It is furthermore preferred that the first reinforcement is with a thickness of 3-110mm, density 0.05-0.20g/cm3。
Hydrophobing agent used in hydrophobic treatment includes methyltrimethoxysilane, methylsiloxane resin, ethyl organosilicon tree
Rouge, phenyl organic siliconresin.
In step (1), the second reinforcement includes fibre；The raw material of fibre be high silica fiber, quartz fibre,
The combination of one or more of alumina fibre, Zirconium oxide fibre, mullite fiber, carbon fiber, silicon carbide fibre；
Preferably, the second reinforcement in step (1) is with a thickness of 0.2-5mm, density 0.6-2.0g/cm3；
It is furthermore preferred that connection type is to suture to connect using fiber in step (1), suture connects technique used as needle thorn
Technique；Needling density is 4-18 needle/cm2。
Impregnation method includes vacuum impregnation, brushing, spraying.
In step (3), the mode of hydrophilic treated includes hydrophobing agent used in high temperature removal hydrophobic treatment.
Aging is first carried out after dipping, then is dried；Drying mode is supercritical drying；
Preferably, the product after supercritical drying handles 0.5~5h under the conditions of 600~1000 DEG C；
It is furthermore preferred that aerogel precursor body includes one or more of silica sol, alumina sol, carbon sol
Combination.
To realize the second purpose, the present invention adopts the following technical scheme:
It is a kind of to use antiscour aerogel composite made from as above any preparation method.
Antiscour aerogel composite is laminated construction, including the first reinforcement layer and the second reinforcement layer, and first increases
Strong bulk layer thickness is 3-100mm, density 0.2-0.6g/cm3, the second reinforcement layer is 0.2-5mm, density 1.0-2.4g/
cm3；
Preferably, the first enhancing bulk layer thickness is 5-25mm, and the second enhancing bulk layer thickness is 0.5-2mm.
First reinforcement and the second reinforcement not only include fibre, further include by densification at least once
Fibre is such as compounded with the fibre of aeroge.
Specifically, the preparation process of the antiscour aerogel composite is as follows:
The first step prepares above-mentioned the first hydrophobic reinforcement
Hydrophobic treatment is carried out to Low-density high temperature resistant fibrofelt (corresponding above-mentioned first reinforcement) first, is obtained above-mentioned hydrophobic
The first reinforcement, wherein the effect of the hydrophobic treatment are as follows: hydrophilic ceramic base presoma can be prevented in following step to soak
Stain Low-density high temperature resistant fibrofelt；Organic matter used in the hydrophobic treatment is methyltrimethoxysilane or methyl, ethyl, phenyl
Equal organic siliconresins solution.
Second step prepares above-mentioned precast body
Then by Low-density high temperature resistant fibrofelt and the high-density and high-temperature-resistant fibrofelt (corresponding above-mentioned second after hydrophobic treatment
Reinforcement), the high-temperature fibre precast body of monolithic devices density gradient is formed by layer-by-layer continuous needle mode, i.e., it is above-mentioned prefabricated
Body, wherein needling density is 4-18 needle/cm2。
Third step prepares above-mentioned composite material
Hydrophilic ceramic base presoma (corresponding above-mentioned first dipping object) is passed through into vacuum impregnation, brushing or spary technique,
High-density and high-temperature-resistant fibrofelt is impregnated repeatedly, and final high temperature processing prepares surface antiscour panel, obtains above-mentioned composite material.
Wherein, the hydrophilic ceramic presoma can be silica sol, alumina sol, mullite sol；The high-temperature process
Effect are as follows: removal the internal drainage agent of high-density and high-temperature-resistant fibrofelt, be convenient for next step composite aerogel presoma, slab strength
Further strengthen.
4th step prepares above-mentioned antiscour aerogel composite
The precast body that surface has been strengthened passes through sol-gel process impregnating gas Gel Precursor (corresponding above-mentioned second
Impregnate object), the process combinings such as aging, supercritical drying prepare antiscour aerogel composite, obtain the airsetting of density gradient
Glue heat-insulation composite material, wherein before the aerogel precursor body includes siliconoxide precursor, alumina precursor, carbon aerogels
Drive one of body or in which several any combination.The aerogel heat-proof composite material of density gradient is in 600~1000 DEG C of items
0.5~5h is handled under part, is made part ceramic, is obtained antiscour aerogel composite.By material root made from previous step
Machine is carried out according to designed theoretical profile to add, and is processed using numerically-controlled machine tool, the reachable ± 0.2mm of product type face precision.
Antiscour aerogel composite is a kind of gradient-structure surface antiscour aerogel heat-proof composite material, with entirety
The high-temperature fibre precast body of compact density gradient is reinforcement, is divided into surface anti-impact brush layer and thermal insulation layer, table by thickness direction
Face anti-impact brush layer is the ceramic matric composite of high density ceramic fibrofelt enhancing, and thermal insulation layer is the enhancing of low-density ceramic fibrofelt
Aerogel composite.The high-temperature fibre precast body of the integrally formed density gradient is by one layer of Low-density high temperature resistant fibre
It ties up felt and one layer of high-density and high-temperature-resistant fibrofelt is constituted.The high-temperature fibre precast body of the integrally formed density gradient passes through needle
It is integrally formed to pierce technique.Before the needling process, need to carry out Low-density high temperature resistant fibrofelt in hydrophobic type organic matter pre-
Processing.The hydrophobic organic is the organic siliconresins solution such as methyltrimethoxysilane or methyl, ethyl, phenyl.It is described resistance to
High temperature fiber felt can be high silica fiber, quartz fibre, alumina fibre, Zirconium oxide fibre, mullite fiber, carbon fiber, carbon
SiClx fiber is prepared.The Low-density high temperature resistant fibrofelt and high-density and high-temperature-resistant fibrofelt can be same material,
It can be different materials, general high-density and high-temperature-resistant fibrofelt temperature tolerance need to be higher than Low-density high temperature resistant fibrofelt.It is described low close
High-temperature fibre felt is spent with a thickness of 3-110mm, density 0.05-0.20g/cm3.The high-density and high-temperature-resistant fibrofelt with a thickness of
0.2-5mm, density 0.6-2.0g/cm3.With a thickness of 0.2-5mm, preferably 0.5-2mm, density is the surface antiscour layer
1.0-2.4g/cm3, the insulation thickness are 3-100mm, preferably 5-25mm, density 0.2-0.6g/cm3.The pottery
Porcelain based composites are one of silica, aluminium oxide, mullite etc. or in which several any combination ceramic composites.
The aeroge is one of silica aerogel, alumina aerogels, carbon aerogels or in which several any combination.
Compared with prior art, the invention has the following beneficial effects:
1) antiscour aerogel composite of the invention can carry out type face machine and add, and obtain the component in required type face, or
Person carries out overall appearance face machine after assembling aircraft and adds, accurately to guarantee the aerodynamic configuration of aircraft.
2) preparation process of antiscour aerogel composite of the invention is simpler, compared with the prior art, reduces
Punching quilting process, manufacturing cycle shorten, and cost is relatively low.
3) present invention forms surface anti-impact brush layer and thermal insulation layer by composite aerogel using precast body as reinforcement, thus
It is formed in surface anti-impact brush layer and thermal insulation layer in same reinforcement, avoids the risk of the two layering, and preparing aeroge
When thermal insulation layer, surface anti-impact brush layer can also impregnate a certain amount of aerogel material, so that inter-layer bonding force is further enhanced, into
One step improves the globality of the material, reduces the risk of layering.
4) antiscour aerogel composite of the invention surface erosion resistibility with higher is, which is because, table
Surface layer is compounded with high-densit ceramic base presoma not only using high-density fiber felt as reinforcement, while secondary being compounded with
Aerogel precursor body, so that surface strength be made to be further strengthened.
5) antiscour aerogel composite of the invention is provided simultaneously with excellent heat-proof quality, strain coordination performance and resists
Performance of flushing, designability, can machine add ability strong, can be widely applied to the outer heat shield of high-speed aircraft.
Detailed description of the invention
Fig. 1 is the preparation technology flow chart of antiscour aerogel composite of the invention.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be to the technology in embodiment
Scheme is clearly and completely described, and the following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Embodiment 1
1) selecting density is 0.70g/cm3, the mullite fiber felt with a thickness of 1mm is high-density fiber felt, selects density
For 0.10g/cm3, the quartz fiber felt with a thickness of 24mm is low-density fibre felt.
2) first using methyltrimethoxysilane to quartz fiber felt carry out hydrophobic treatment, then by quartz fiber felt with
Mullite fiber felt is prepared into the high-temperature fibre precast body of monolithic devices density gradient, needling density 15 by way of needle thorn
Needle/cm2。
3) precast body is placed in closed container, silica solution is impregnated into composite mullite fiber by vacuum impregnation mode
Felt impregnates 9 times repeatedly, then carries out high-temperature process, removes organic matter.
4) precast body strengthened using silica solution impregnation surface after the techniques such as aging, supercritical drying, obtains density level bands
The aerogel heat-proof composite material of degree.
5) material made from step 4) is handled into 5h under the conditions of 1000 DEG C, makes part ceramic.
6) material made from step 5) is carried out machine according to designed theoretical profile to add, is processed using numerically-controlled machine tool, protected
Demonstrate,prove Product Precision.
Embodiment 2
1) selecting density is 0.70g/cm3, the mullite fiber felt with a thickness of 1mm is high-density fiber felt, selects density
For 0.10g/cm3, the quartz fiber felt with a thickness of 24mm is low-density fibre felt.
2) hydrophobic treatment is carried out to quartz fiber felt using methyl phenyl silicone resin solution first, then by quartz fiber felt
The high-temperature fibre precast body of monolithic devices density gradient, needling density 15 are prepared by way of needle thorn with mullite fiber felt
Needle/cm2。
3) precast body is placed in closed container, silica solution is impregnated into composite mullite fiber by vacuum impregnation mode
Felt impregnates 9 times repeatedly, then carries out high-temperature process, removes organic matter.
4) precast body strengthened using silica solution impregnation surface after the techniques such as aging, supercritical drying, obtains density level bands
The aerogel heat-proof composite material of degree.
5) material made from step 4) is handled into 1h under the conditions of 600 DEG C, makes part ceramic.
6) material made from step 5) is carried out machine according to designed theoretical profile to add, is processed using numerically-controlled machine tool, protected
Demonstrate,prove Product Precision.
Embodiment 3
1) selecting density is 0.70g/cm3, the silicon carbide fibre felt with a thickness of 1mm is high-density fiber felt, selects density
For 0.10g/cm3, the mullite fiber felt with a thickness of 24mm is low-density fibre felt.
2) hydrophobic treatment is carried out to mullite fiber felt using methyltrimethoxysilane first, then by mullite fiber
Felt and silicon carbide fibre felt are prepared into the high-temperature fibre precast body of monolithic devices density gradient by way of needle thorn, and needling density is
15 needles/cm2。
3) precast body is placed in closed container, mullite sol is impregnated into composite mullite fibre by vacuum impregnation mode
Felt is tieed up, is impregnated 9 times repeatedly, high-temperature process is then carried out, removes organic matter.
4) precast body strengthened using mullite sol impregnation surface after the techniques such as aging, supercritical drying, is obtained close
Spend the aerogel heat-proof composite material of gradient.
5) material made from step 4) is handled into 0.5h under the conditions of 700 DEG C, makes part ceramic.
6) material made from step 5) is carried out machine according to designed theoretical profile to add, is processed using numerically-controlled machine tool, protected
Demonstrate,prove Product Precision.
Embodiment 4
1) selecting density is 0.70g/cm3, the silicon carbide fibre felt with a thickness of 1mm is high-density fiber felt, selects density
For 0.10g/cm3, the mullite fiber felt with a thickness of 24mm is low-density fibre felt.
2) hydrophobic treatment is carried out to mullite fiber felt using methyltrimethoxysilane first, then by mullite fiber
Felt and silicon carbide fibre felt are prepared into the high-temperature fibre precast body of monolithic devices density gradient by way of needle thorn, and needling density is
15 needles/cm2。
3) precast body is placed in closed container, silica sol is impregnated into composite mullite fibre by vacuum impregnation mode
Felt is tieed up, is impregnated 9 times repeatedly, high-temperature process is then carried out, removes organic matter.
4) precast body strengthened using silica sol impregnation surface after the techniques such as aging, supercritical drying, is obtained close
Spend the aerogel heat-proof composite material of gradient.
5) material made from step 4) is handled into 3h under the conditions of anaerobic, 800 DEG C, makes part ceramic.
6) material made from step 5) is carried out machine according to designed theoretical profile to add, is processed using numerically-controlled machine tool, protected
Demonstrate,prove Product Precision.
Embodiment 5
1) selecting density is 0.70g/cm3, the alumina fiber blanket with a thickness of 1mm is high-density fiber felt, selects density
For 0.10g/cm3, the mullite fiber felt with a thickness of 24mm is low-density fibre felt.
2) hydrophobic treatment is carried out to mullite fiber felt using methyltrimethoxysilane first, then by mullite fiber
Felt and alumina fiber blanket are prepared into the high-temperature fibre precast body of monolithic devices density gradient by way of needle thorn, and needling density is
15 needles/cm2。
3) precast body is placed in closed container, silica sol is impregnated into composite mullite fibre by vacuum impregnation mode
Felt is tieed up, is impregnated 9 times repeatedly, high-temperature process is then carried out, removes organic matter.
4) precast body strengthened using silica sol impregnation surface after the techniques such as aging, supercritical drying, is obtained close
Spend the aerogel heat-proof composite material of gradient.
5) material made from step 4) is handled into 2h under the conditions of 900 DEG C, makes part ceramic.
6) material made from step 5) is carried out machine according to designed theoretical profile to add, is processed using numerically-controlled machine tool, protected
Demonstrate,prove Product Precision.
Comparative example 1
1) selecting density is 0.70g/cm3, the mullite fiber felt with a thickness of 1mm is high-density fiber felt, selects density
For 0.10g/cm3, the quartz fiber felt with a thickness of 24mm is low-density fibre felt.
2) quartz fiber felt and mullite fiber felt are prepared into the high temperature resistant of monolithic devices density gradient by way of needle thorn
Fiber preform, needling density are 15 needles/cm2。
3) precast body is placed in closed container, silica solution is impregnated into composite mullite fiber by vacuum impregnation mode
Felt is impregnated 9 times repeatedly, is then dried.
4) precast body strengthened using silica solution impregnation surface after the techniques such as aging, supercritical drying, obtains density level bands
The aerogel heat-proof composite material of degree.
5) material made from step 4) is handled into 5h under the conditions of 1000 DEG C, makes part ceramic.
6) material made from step 5) is carried out machine according to designed theoretical profile to add, is processed using numerically-controlled machine tool, protected
Demonstrate,prove Product Precision.
The present invention has carried out performance detection to final product made from above-described embodiment and comparative example, the results are shown in Table 1.
Table 1
As shown in Table 1, the global density of product made from embodiment 1-5, compressive strength are below comparative example 1, thus may be used
Know, in embodiment 1-5, the dipping object for impregnation surface anti-impact brush layer fibrofelt does not immerse to thermal insulation layer fibrofelt, and
In comparative example 1, the dipping object for impregnation surface anti-impact brush layer fibrofelt is immersed to thermal insulation layer fibrofelt.Embodiment 1-5 is made
Room temperature thermal conductivity be lower than comparative example 1, i.e. heat-proof quality is better than comparative example 1, it follows that in embodiment 1-5, for impregnating
The dipping object of surface anti-impact brush layer fibrofelt does not immerse to thermal insulation layer fibrofelt, and in comparative example 1, since there is no hydrophobic place
Step is managed, therefore in impregnation surface anti-impact brush layer fibrofelt, it is fine that thermal insulation layer fibrofelt can be used for impregnation surface anti-impact brush layer
The dipping object dipping for tieing up felt, so as to cause heat-proof quality reduction, even if thermal insulation layer fibrofelt be used to impregnate in subsequent handling
The dipping object of thermal insulation layer fibrofelt impregnates, and can not improve heat-proof quality well.
The present invention is described in detail, of the invention its object is to which those skilled in the art can understand
Content is simultaneously implemented, and it is not intended to limit the scope of the present invention, what all Spirit Essences according to the present invention were done etc.
Changes or modifications are imitated, should be covered by the scope of protection of the present invention.
Claims (10)
1. a kind of preparation method of antiscour aerogel composite characterized by comprising
(1) the first hydrophobic reinforcement is connected with the second hydrophilic reinforcement, obtains precast body；
(2) part of the second reinforcement is included at least on precast body through the first dipping object leaching hydrophilic, for densification
It is dried after stain, obtains composite material；
(3) hydrophilic treated is carried out to the part for including at least the first hydrophobic reinforcement on composite material, obtains antiscour airsetting
Glue composite material.
2. a kind of preparation method of antiscour aerogel composite according to claim 1, which is characterized in that step
(3) in, obtain intermediate after hydrophilic treated, included at least on intermediate the part of hydrophobic reinforcement through it is hydrophilic, for densification
It is dried after changing the second dipping object dipping of processing；
Preferably, the first dipping object includes ceramic base presoma；Second dipping object includes aerogel precursor body.
3. a kind of preparation method of antiscour aerogel composite according to claim 1, which is characterized in that step
(1) in, the first hydrophobic reinforcement is obtained by carrying out hydrophobic treatment to the first hydrophilic reinforcement；
Preferably, the first reinforcement includes fibre；The raw material of fibre is high silica fiber, quartz fibre, aluminium oxide
The combination of one or more of fiber, Zirconium oxide fibre, mullite fiber, carbon fiber, silicon carbide fibre；
It is furthermore preferred that the first reinforcement is with a thickness of 3-110mm, density 0.05-0.20g/cm3。
4. a kind of preparation method of antiscour aerogel composite according to claim 3, which is characterized in that hydrophobic place
Reason hydrophobing agent used includes methyltrimethoxysilane, methylsiloxane resin, ethyl organic siliconresin, phenyl organosilicon tree
Rouge.
5. a kind of preparation method of antiscour aerogel composite according to claim 1, which is characterized in that step
(1) in, the second reinforcement includes fibre；The raw material of fibre be high silica fiber, quartz fibre, alumina fibre,
The combination of one or more of Zirconium oxide fibre, mullite fiber, carbon fiber, silicon carbide fibre；
Preferably, the second reinforcement in step (1) is with a thickness of 0.2-5mm, density 0.6-2.0g/cm3；
It is furthermore preferred that connection type is to suture to connect using fiber, and it is needling process that suture, which connects technique used, in step (1)；
Needling density is 4-18 needle/cm2。
6. a kind of preparation method of antiscour aerogel composite according to claim 1, which is characterized in that dipping side
Formula includes vacuum impregnation, brushing, spraying.
7. a kind of preparation method of antiscour aerogel composite according to claim 1, which is characterized in that step
(3) in, the mode of hydrophilic treated includes hydrophobing agent used in high temperature removal hydrophobic treatment.
8. a kind of preparation method of antiscour aerogel composite according to claim 2, which is characterized in that after dipping
Aging is first carried out, then is dried；Drying mode is supercritical drying；
Preferably, the product after supercritical drying handles 0.5~5h under the conditions of 600~1000 DEG C；
It is furthermore preferred that aerogel precursor body includes the group of one or more of silica sol, alumina sol, carbon sol
It closes.
9. a kind of using antiscour aerogel composite made from any preparation method of claim 1-8.
10. antiscour aerogel composite according to claim 9, which is characterized in that for laminated construction, including first
Reinforcement layer and the second reinforcement layer, the first enhancing bulk layer thickness is 3-100mm, density 0.2-0.6g/cm3, the second enhancing
Body layer is 0.2-5mm, density 1.0-2.4g/cm3；
Preferably, the first enhancing bulk layer thickness is 5-25mm, and the second enhancing bulk layer thickness is 0.5-2mm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113773044A (en) * | 2021-09-27 | 2021-12-10 | 航天特种材料及工艺技术研究所 | High-strength aerogel composite material and preparation method thereof |
| CN117467168A (en) * | 2023-10-31 | 2024-01-30 | 肥城三合工程材料有限公司 | Preparation process of sound-absorbing composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103411098A (en) * | 2013-08-28 | 2013-11-27 | 航天特种材料及工艺技术研究所 | Integrated high-temperature-resistant rigid heat insulation component and production method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103411098A (en) * | 2013-08-28 | 2013-11-27 | 航天特种材料及工艺技术研究所 | Integrated high-temperature-resistant rigid heat insulation component and production method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113773044A (en) * | 2021-09-27 | 2021-12-10 | 航天特种材料及工艺技术研究所 | High-strength aerogel composite material and preparation method thereof |
| CN113773044B (en) * | 2021-09-27 | 2023-07-18 | 航天特种材料及工艺技术研究所 | High-strength aerogel composite material and preparation method thereof |
| CN117467168A (en) * | 2023-10-31 | 2024-01-30 | 肥城三合工程材料有限公司 | Preparation process of sound-absorbing composite material |
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