CN109968757A - Ablation-resistant light heat-proof heat-insulation integrated composite material and preparation method thereof - Google Patents

Ablation-resistant light heat-proof heat-insulation integrated composite material and preparation method thereof Download PDF

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CN109968757A
CN109968757A CN201910323696.4A CN201910323696A CN109968757A CN 109968757 A CN109968757 A CN 109968757A CN 201910323696 A CN201910323696 A CN 201910323696A CN 109968757 A CN109968757 A CN 109968757A
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composite material
ablation
heat
fiber cloth
resistance
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CN109968757B (en
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陈思安
胡海峰
陈志华
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National University of Defense Technology
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    • 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
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/12—Layered products comprising a layer of synthetic resin next to a fibrous or filamentary layer
    • 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
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
    • B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
    • 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
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/42—Layered products comprising a layer of synthetic resin comprising condensation resins of aldehydes, e.g. with phenols, ureas or melamines
    • 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
    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • 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
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • 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
    • 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
    • B32B38/08—Impregnating
    • 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
    • B32B5/02—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 structural features of a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B64—AIRCRAFT; AVIATION; COSMONAUTICS
    • B64G—COSMONAUTICS; VEHICLES OR EQUIPMENT THEREFOR
    • B64G1/00—Cosmonautic vehicles
    • B64G1/22—Parts of, or equipment specially adapted for fitting in or to, cosmonautic vehicles
    • B64G1/52—Protection, safety or emergency devices; Survival aids
    • B64G1/58—Thermal protection, e.g. heat shields
    • 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
    • B32B2038/0052—Other operations not otherwise provided for
    • B32B2038/0076—Curing, vulcanising, cross-linking
    • 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
    • B32B2255/00—Coating on the layer surface
    • B32B2255/02—Coating on the layer surface on fibrous or filamentary layer
    • 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
    • B32B2255/00—Coating on the layer surface
    • B32B2255/26—Polymeric coating
    • 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
    • B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
    • B32B2260/02—Composition of the impregnated, bonded or embedded layer
    • B32B2260/021—Fibrous or filamentary layer
    • B32B2260/023—Two or more layers
    • 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
    • B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
    • B32B2260/04—Impregnation, embedding, or binder material
    • B32B2260/046—Synthetic resin
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/304—Insulating
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/306—Resistant to heat
    • B32B2307/3065—Flame resistant or retardant, fire resistant or retardant
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/718—Weight, e.g. weight per square meter

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  • General Health & Medical Sciences (AREA)
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  • Fluid Mechanics (AREA)
  • Laminated Bodies (AREA)
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Abstract

The composite material is of a sandwich structure, the middle layer takes chopped fibers as a reinforcement, phenolic resin as a matrix, hollow microspheres as a heat insulation filler, the upper surface layer and the lower surface layer are laminated by fiber cloth prepreg, and the three layers are co-cured to improve the bearing and anti-scouring capacities; the preparation method comprises eight steps of ceramic powder treatment, short fiber and fiber cloth pretreatment, material mixing, drying, slurry preparation, brushing or dipping, mold filling, curing molding and demolding. The composite material can be applied to ablation working conditions with medium and low heat flow density, is formed at one time, has short preparation period and low cost, can form a stable ablation-resistant ceramic layer on the surface within the temperature range of 800-1300 ℃, and simultaneously realizes the heat insulation function of low-density fillers such as hollow microspheres in the composite material, and the like, and realizes the heat insulation prevention and prevention integrated function under the conditions of medium and low heat flow density and oxidation.

Description

A kind of resistance to ablation lightweight solar heat protection heat-insulation integrative composite material and preparation method
Technical field
The present invention generally belongs to aircraft thermal protection technology field more particularly to a kind of resistance to ablation lightweight solar heat protection heat-insulated one Body composite material and preparation method.
Background technique
Lightweight solar heat protection heat-insulation integrative lightweight thermally protective materials are that the spacecraft that space maneuvering vehicle is representative realizes small Type, high payload ratio, the key technology for quickly passing in and out space, decide the advance, reliability and economy of spacecraft. With the development of the novel spacecraft development work in China, the lightweight thermally protective materials for having solar heat protection heat-insulation integrative function are proposed Urgent demand.
1976,1996 and 2004, the Mars " pirate number " of U.S. NASA, " pioneer number " and " detection ramber number " Successfully land Mars respectively.Above detector windward side heat shield all uses the SLA- of Lockheed Martin Corporation's production 561V Honeycomb low-density thermal-protect ablation material.SLA-561V density is only 0.264g/cm3, with cork powder, silica or Glass microsphere, phenolic aldehyde microballoon, silica and/or carbon fiber etc. are the ultralight heat insulation material of filler, and it is close to be suitable for peak value hot-fluid Spend 0.21MW/m2, reenter time 250s, total amount of heat 1.1MJ/m2, 1727 DEG C of maximum temperature of thermal environment." Galileo " in the U.S. Jupiter probe experience to be that thermal environment condition is the harshest so far reenter, jupiter atmospheric shell is reentered with the speed of 48km/s, Peak heat flux is up to 170MW/m2, stagnation pressure 7MPa, Reentry heating time 70s, highest ablation temperature is 3900 DEG C.Class It is similar to the thermal environment that ballistic reenters and determines heat shield using FM5055 carbon/phenolic materials on strategic missile, density is 1.45g/cm3, thermal protection system weight accounts for the 50% of aircraft gross weight.
The U.S. starts new generation low-density thermal-protect ablation material in the nineties, with phenolic impregnated carbon ablating body (PICA) and the reusable ceramic ablating body (SIRCA) of silicone-impregnated is to represent light ablative material (LCA).SIRCA is used It is less than 3MW/m in hot-fluid2, PICA for hot-fluid be greater than 3MW/m2Environment." the star that lift-off in 2 months 1999, in January, 2006 return Dirt " number return capsule uses entirety PICA material as windward side heat shield, is successfully subjected to aircraft so far and reenters the earth most Fast speed 12.9km/s, peak heat flux reach 12MW/m2Reentry environment.The density of PICA is about 0.24~0.32g/cm3, Using the carbon-based heat-barrier material of threadiness of FMI company, U.S. production as reinforcement, impregnated phenolic resin is formed, and can be considered lighting Carbon/phenolic materials.The high porosity (about 85%) of PICA makes its thermal conductivity be substantially less than high density carbon/phenolic materials, have both compared with Good heat-proof quality.The density of SIRCA is about 0.35g/cm3, the LI-900 and LI-2200 two that are produced using Lockheed Co. Ceramic tile on kind space shuttle is formed through silicone-impregnated, and leeward heat shield, the Mars for Mars Pathfinder number are visited The leading edge and nose cone of the backboard of rope ramber's airship, X-34 aircraft.
The country has developed phenolic aldehyde-terylene thermal-protect ablation material in terms of thermal-protect ablation material and using silicon rubber as base, filling H88, H96 low density ablator made of phenolic aldehyde and glass pellet, and the MD2 enhanced using phenolic aldehyde as base, staple glass fibre Middle density ablator.Wherein, phenolic aldehyde-terylene thermal-protect ablation material is mainly used for retrievable satellite, density 1.280g/cm3, It can be used for heat flow density 3MW/m2Aerodynamic Heating environment；Low density ablator includes two kinds of H88, H96, is flown for Shenzhou Ship leeward, bottom and side wall windward side, density are respectively 0.54g/cm3And 0.71g/cm3；Middle density thermal-protect ablation material MD2 The turning of the Shenzhou airship solar heat protection outsole more serious applied to airflow scouring.
The low-density solar heat protection heat-barrier material of ablative-type protective coating loses to design the ablation in reply use process, the heat-insulated material of solar heat protection Expect that design thickness is necessarily larger, therefore brings superfluous heavy and outer dimension increase to the structure of entire aircraft.It is answered with X-37B TUFROC is representative, and novel non-ablative low-density solar heat protection heat-insulation integrative material becomes the hot spot of research.TUFROC Outer layer is infusibility, oxidation resistant light ceramics/carbon material (ROCCI) nut cap, it is that a kind of surface is complete fully dense highdensity Carbon containing ceramic composite material is realized non-ablative as outer layer.The main component of ROCCI is carbon, silicon and oxygen, is reached using temperature 1200K, after HETC (height radiates low catalysis) coating is added on surface, use temperature of the ROCCI in 10min up to 1931K, The use temperature of 1min is up to 2255K.The internal layer of TUFROC is low-density heat-barrier material, such as AETB (Alumina enhanced Thermal barrier) or FRCI (Fibrous refractory insulation composite), surface TUFI Coating.Its transition region is the binder of 1.2mm thickness.The height that this new ceramics composite construction generates when not only can bear to reenter Temperature (maximum temperature be not less than 1700 DEG C), and also solve ceramic tile hot tearing and anti-oxidant equal bottlenecks are asked in a high temperauture environment Topic, and can reuse.But such heat-insulated non-ablative low-density solar heat protection is multiple layer combination structure, and preparation cost is high. Chopped strand, cenosphere, ceramic packing and resin are mixed post-crosslinking solidification by CN102815958A, are obtained a kind of with anti- Hot heat-insulation integrative function can ceramizable resin matrix composite material.Low density filler drop is added in the material in ceramic resin Low-density and thermal conductivity, while disposal molding, short preparation period, preparation cost are low.But such low-density composite is in height Linear ablative rate is larger under fast airflow scouring, and anti-ablation scouring capability is insufficient, still falls within ablative-type protective coating heat insulation material, cannot achieve non- The solar heat protection heat-insulation integrative of ablation.
Summary of the invention
The technical problem to be solved by the present invention is to, intolerant to ablation, make for heat-insulated heat insulation material used in the prior art With the deficiency that the service life is short, the preparation side of a kind of resistance to ablation lightweight solar heat protection heat-insulation integrative composite material and its simple process is provided Method.
The technical solution adopted by the present invention is that: a kind of resistance to ablation lightweight solar heat protection heat-insulation integrative composite material, it is sandwich Structure, including the first outer layer, the second outer layer and middle layer；Middle layer is that chopped strand is mixed in the phenolic aldehyde for being dispersed with cenosphere The chopped strand prepreg formed in resin, between first outer layer and the second outer layer, i.e. sandwich of layers；First outer layer To brush or impregnating the layer that the slurry containing ceramic powder is formed, i.e. surface erosion-resistant layer in fiber cloth；Second outer layer is fiber cloth The layer that upper brushing or impregnated phenolic resin layer are formed, i.e. bottom surface bearing bed.
The first outer layer in interlayer structure of the present invention plays the role of anti-oxidant ablation, and fiber cloth improves skin-material Globality, and ceramic composition then plays the role of improving anti-oxidant ablation；Sandwich of layers primarily serves heat-blocking action, and cenosphere is just It is to improve the porosity of sandwich material, and realize lighting；Second outer layer is traditional polymer matrix composites, primarily serves and holds The function of load.
Further, the above-mentioned slurry containing ceramic powder is that phenolic aldehyde-ethanol solution of ceramic powder and weight ratio 1:1 is formed Mixture, ceramic powder and phenolic aldehyde-ethanol solution weight ratio 1:1.
Further, in above-mentioned first outer layer each component content with volume percent are as follows: fiber cloth be 25%~40%； Phenolic resin is 25%~35%；Ceramic powder is 25%~35%；Each component content is in middle layer with volume percent are as follows: Chopped strand is 5%~15%；Phenolic resin is 15%~25%；Cenosphere is 60%~80%；Each group in second outer layer Divide content with volume percent are as follows: fiber cloth is 45%~55%；Phenolic resin is 45%~55%.
Further, above-mentioned chopped strand is appointing in high silica fiber, quartz fibre, mullite fiber and SiC fiber The mixing for one or more of anticipating, 5~20mm of length.
Further, above-mentioned cenosphere is one or more mixing of glass microballoon, ceramic microbead and phenolic aldehyde microballon.
Further, above-mentioned fiber cloth be SiC fiber cloth, alumina fibre cloth, quartz fiber cloth, high silica fiber cloth and The mixing of any one or more of mullite fiber cloth.
Further, above-mentioned ceramic powder is SiC, MoSi2、B4C, in glass powder, montmorillonite, mica, feldspar and kaolin Several mixtures.
The present invention also provides the preparation method of above-mentioned resistance to ablation lightweight solar heat protection heat-insulation integrative composite material, including it is following Step:
1) it disperses ceramic powder in the NaOH aqueous solution that NaOH content is 10wt.% and handles 1h, then use distilled water Or deionized water filters cleaning to filtrate neutrality, is scattered in dehydrated alcohol after drying, silane coupling agent is added and changes as surface Property agent stirring, dried in 150 DEG C after suction filtration, obtain pre-treatment ceramic powder；
2) by chopped strand, 300~500 DEG C of 0.5~1h of heat preservation are chopped after obtaining degumming in Muffle furnace with degumming process Fiber；
3) fiber cloth is cut out to being sized, it is spare；
4) by cenosphere be added weight ratio 1:3 phenolic resin-ethanol solution in, stir evenly obtained slurry, then plus Enter chopped strand, is put into mixing tank rotation mixing；
5) the resulting chopped strand prepreg slurry mixed of step 4) is dried in an oven, until ethyl alcohol dries substantially It is dry, obtain chopped strand prepreg；
6) the resulting pre-treatment ceramic powder of step 1) is added in phenolic resin-ethanol solution of weight ratio 1:1, stirring Uniformly obtained ceramic powder slurry；
7) by the brushing of ceramic powder slurry or impregnation steps 3 made from step 6)) in the fiber cloth of resulting half quantity, Laying, which stacks, obtains blank I；By phenolic resin-second of the fiber cloth dipping weight ratio 1:1 of the other half resulting quantity of step 3) Alcoholic solution, then laying, which stacks, obtains blank II；
It 8), successively will the resulting blank I of step 7), step 5) gained in die surface brushing release agent or laying processing release paper Chopped strand prepreg and the resulting blank II of step 7) be fitted into mold；
9) it will be placed in mould test specimen on vulcanizing press and carry out hot-press solidifying；
10) it will be removed with mould test specimen, demoulding obtains resistance to ablation lightweight heat release heat-insulation integrative composite material.
Further, silane coupling agent weight accounts for ceramic powder weight 2wt.% in step 1) described above；Silane is added 1h, mixing speed 150r/min are stirred after coupling agent；The mixing time of the step 4) slurry and chopped strand is for 24 hours；
Further, above-mentioned steps 5) drying temperature is 60 DEG C, drying time 8h；Hot pressing crosslinking curing in step 9) Pressure be 2MP, program curing are as follows: be warming up to 120 DEG C from room temperature with 10 DEG C/min, keep the temperature the 2MPa that pressurizes after 30min, then with 10 DEG C/min heats up 180 DEG C, Temperature fall after heat-insulation pressure keeping 2h.
Compared with the prior art, the advantages of the present invention are as follows:
1, resistance to ablation lightweight solar heat protection heat-insulation integrative composite material of the invention, density 0.5g/cm3~0.9g/cm3, tool There is the characteristics of lightweight.
2, resistance to ablation lightweight solar heat protection heat-insulation integrative composite material of the invention, on 800~1300 DEG C of temperature range surfaces The stable ceramic layer of resistance to ablation can be formed, while heat insulating function, low-heat in realization are realized in the low density fillers such as boring microballoon Current density, it is weak wash away, the solar heat protection heat-insulation integrative function under oxidizing condition；Existing low-density solar heat protection heat-barrier material is compared, and is resisted Ablation property is more excellent, and material is stablized in hot environment dimension shape, optimal to be designed using temperature；And material can be realized it is non-ablative And solar heat protection heat insulating function integration, it is possible to the large area thermally protective materials for middle low-heat stream environment.
3, preparation method of the invention makes composite material disposal molding, with the heat-insulated one of the non-ablative solar heat protection such as Turfroc Change material to compare, have many advantages, such as short preparation period, simple process, at low cost, can be realized aircraft large area prevent it is heat-insulated Integrated molding avoids the technique for sticking of Bulk ceramic watt or Turfroc material, can greatly improve reliability.
Detailed description of the invention
From the detailed description with reference to the accompanying drawing to the embodiment of the present invention, these and/or other aspects of the invention and Advantage will become clearer and be easier to understand, in which:
Fig. 1 is the section macrograph of resistance to ablation lightweight solar heat protection heat-insulation integrative composite material in the embodiment of the present invention 1.
Fig. 2 is the skin-material section SEM of resistance to ablation lightweight solar heat protection heat-insulation integrative composite material in the embodiment of the present invention 1 Figure.
Fig. 3 is the sandwich layer material section of resistance to ablation lightweight solar heat protection heat-insulation integrative composite material in the embodiment of the present invention 1 SEM figure.
After oxy-acetylene flame ablation of the Fig. 4 for resistance to ablation lightweight solar heat protection heat-insulation integrative composite material in the embodiment of the present invention 1 Surface layer macro morphology.
Specific embodiment
In order to make those skilled in the art more fully understand the present invention, with reference to the accompanying drawings and detailed description to this hair It is bright to be described in further detail.
Embodiment 1
A kind of resistance to ablation lightweight solar heat protection heat-insulation integrative composite material, the composite material middle layer is with the high silica fiber that is chopped It is formed using phenolic resin as resin by low density filler of glass microballoon for reinforcement, superficial layer is to increase with high silica fiber cloth Qiang Ti, with B4C powder, montmorillonite powder and carborundum powder are superficial layer ceramic packing.
The preparation of the above-mentioned heat-insulated composite material of resistance to ablation lightweight solar heat protection, including the following steps:
(1) by B4C powder and SiC powder, which are scattered in the NaOH aqueous solution of NaOH content 10wt.%, handles 1h, uses distilled water Or deionized water filters cleaning to filtrate neutrality, 150 DEG C are dried for standby；It disperses montmorillonite powder in dehydrated alcohol, powder is added The silane coupling agent of weight 2% is filtered, 150 DEG C are dried for standby after 1h as surface modifier.
(2) by chopped high silica fiber in Muffle furnace 300~500 DEG C of heat preservation 0.5~1h degumming process.
(3) high silicon oxygen cloth of reinforcement fibers is cut out to 100mm × 100mm, it is totally 15 layers, spare.
(4) be chopped quartz fibre in mass ratio: solution: hollow glass micropearl=6:24:5 weighs chopped quartz fibre, phenol Urea formaldehyde-ethanol solution, hollow glass micropearl, phenolic resin-ethyl alcohol that weight ratio 1:3 is added in hollow glass micropearl filler are molten In liquid, obtained slurry is stirred evenly, chopped strand is then added, is put into mixing tank rotation mixing for 24 hours.
(5) by the chopped strand prepreg mixed 60 DEG C of drying 8h in an oven, until ethyl alcohol is dried substantially.
(6) B in mass ratio4C: montmorillonite: SiC=1:1:2 weighs ceramic powder, and weight ratio 1:1 is added in ceramic powder Phenolic resin-ethanol solution in, ceramic powder and phenolic resin-ethanol solution mass ratio are 1:1, stir evenly obtained slurry Material.
(7) by slurry brushing or impregnation steps 3 made from step 6)) in resulting 8 layers of high silica fiber cloth, laying stacks Obtain blank I；After the resulting 7 layers of high silica fiber cloth dipping 50wt.% phenolic resin-ethanol solution of step 3), laying is folded It puts and obtains blank II.
(8) in die surface brushing release agent or laying processing release paper, successively by blank I, chopped high silica fiber after lamination Prepreg and blank II are fitted into mold.
(9) will be placed in mould test specimen on vulcanizing press and carry out hot-press solidifying, pressure 2MP, curing cycle be from room temperature with 10 DEG C/min is warming up to 120 DEG C, and pressurize 2MPa after heat preservation 30min, is then heated up 180 DEG C with 10 DEG C/min, after heat-insulation pressure keeping 2h Temperature fall.
(10) press will be removed with mould test specimen, demoulding obtains resistance to ablation lightweight solar heat protection heat-insulation integrative composite material.
Resistance to ablation lightweight solar heat protection heat-insulation integrative composite material longitudal section macro morphology such as Fig. 1 institute manufactured in the present embodiment Show.Surface layer microscopic appearance is as shown in Fig. 2, sandwich of layers microscopic appearance is as shown in Figure 3.Material integral thickness 20mm, wherein outside first Thickness degree 3mm, sandwich of layers thickness 15mm, the second outer layer thickness~2mm.Material combined density only 0859g/cm3, compression strength 10.2MP, room temperature thermal conductivity 0.182W/mK.Oxy-acetylene flame presses GJB 323A-96 standard ablation 60s, and linear ablative rate is about 0.03mm/s, macro morphology is as shown in Figure 4 after ablation.
Embodiment 2
A kind of resistance to ablation lightweight solar heat protection heat-insulation integrative composite material, the middle layer of the composite material is with the quartz fibre that is chopped For reinforcement, using Novolac Cyanate Eater Resin as resin, using glass microballoon as low density filler, superficial layer is enhancing with quartz fiber cloth Body, with B4C powder, glass powder, kaolin and carborundum powder are ceramic packing.
The preparation method of above-mentioned resistance to ablation lightweight solar heat protection heat-insulation integrative composite material, including the following steps:
(1) by B4C powder and SiC powder, which are scattered in the NaOH aqueous solution of NaOH content 10wt.%, handles 1h, uses distilled water Or deionized water filters cleaning to filtrate neutrality, 150 DEG C are dried for standby；It disperses glass powder and kaolin in dehydrated alcohol, The silane coupling agent of powder quality 2% is added as surface modifier, is filtered after 1h, 150 DEG C are dried for standby.
(2) by chopped quartz fibre in Muffle furnace 300~500 DEG C of heat preservation 0.5~1h degumming process.
(3) quartzy cloth of reinforcement fibers is cut out to 100mm × 100mm, it is totally 15 layers, spare.
(4) be chopped quartz fibre in mass ratio: phenolic resin-ethanol solution: hollow glass micropearl=8:25:3 weighs short Cut quartz fibre, phenolic resin-ethanol solution, hollow glass micropearl；Then weight ratio 1:3 is added in hollow glass micropearl filler Phenolic resin-ethanol solution in, stir evenly obtained slurry, chopped strand be then added, be put into mixing tank rotation mixing 24h。
(5) by the chopped strand prepreg mixed 60 DEG C of drying 8h in an oven, until ethyl alcohol is dried substantially.
(6) B in mass ratio4C: glass powder: kaolin: SiC=2:1:1:4 weighs ceramic powder, and ceramic powder is added In Novolac Cyanate Eater Resin-butanone solution of weight ratio 4:6, ceramic powder and Novolac Cyanate Eater Resin-butanone solution mass ratio are 1: 1, stir evenly obtained slurry.
(7) by slurry brushing or impregnation steps 3 made from step 6)) in resulting 8 layers of quartz fiber cloth, laying, which stacks, to be obtained Obtain blank I；After phenolic resin-ethanol solution of the resulting other 7 layers of quartz fiber cloth dipping weight ratio 1:1 of step 3), paving Stacking, which is put, obtains blank II.
(8) successively that blank I, the quartz fibre that is chopped after lamination is pre- in die surface brushing release agent or laying processing release paper Leaching material and blank II are fitted into mold.
(9) will be placed in mould test specimen on vulcanizing press and carry out hot-press solidifying, pressure 2MP, curing cycle be from room temperature with 10 DEG C/min is warming up to 120 DEG C, and pressurize 2MPa after heat preservation 30min, is then heated up 180 DEG C with 10 DEG C/min, after heat-insulation pressure keeping 2h Temperature fall.
(10) press will be removed with mould test specimen, demoulding obtains resistance to ablation lightweight solar heat protection heat-insulation integrative composite material.
Resistance to ablation lightweight solar heat protection heat-insulation integrative composite material the first outer layer thickness 3mm manufactured in the present embodiment, sandwich of layers Thickness 20mm, the second outer layer thickness 2mm.Density is only 0.876g/cm3, compression strength 11.9MPa, room temperature thermal conductivity 0.172W/ m·K。
Embodiment 3
The middle layer of a kind of resistance to ablation lightweight solar heat protection heat-insulation integrative composite material, the composite material is fine with the mullite that is chopped Dimension is reinforcement, using phenolic resin as resin, using ceramic microbead as low density filler；Superficial layer is enhancing with alumina fibre cloth Body, with MoSi2Powder, mica, feldspar and carborundum powder are superficial layer ceramic packing.
The preparation method of above-mentioned resistance to ablation lightweight solar heat protection heat-insulation integrative composite material, including the following steps:
(1) by MoSi2Powder and SiC powder, which are scattered in the NaOH aqueous solution of NaOH Han Ling 10wt.%, handles 1h, with distillation Water or deionized water filter cleaning to filtrate neutrality, and 150 DEG C are dried for standby；It disperses mica and feldspar powder in dehydrated alcohol, The silane coupling agent of powder quality 2% is added as surface modifier, is filtered after 1h, 150 DEG C are dried for standby.
(2) by chopped mullite fiber in Muffle furnace 300~500 DEG C of heat preservation 0.5~1h degumming process.
(3) aluminium oxide cloth of reinforcement fibers is cut out to 100mm × 100mm, it is totally 15 layers, spare.
(4) be chopped mullite fiber in mass ratio: solution: ceramic microbead=16:70:9 first fills out hollow ceramic microspheres Material is added in 25wt.% phenolic resin-ethanol solution, stirs evenly obtained slurry, chopped strand is then added, be put into mixing tank Rotation mixing is for 24 hours.
(5) by the chopped strand prepreg mixed 60 DEG C of drying 8h in an oven, until ethyl alcohol is dried substantially.
(6) MoSi in mass ratio2: mica: feldspar: the phenolic aldehyde tree of 1:1 weight ratio is added in ceramic powder by SiC=1:1:2 In rouge-ethanol solution, the mass ratio of ceramic powder and resin is 1:1, stirs evenly obtained slurry.
(7) by slurry brushing or impregnation steps 3 made from step 6)) on resulting 8 layers of alumina fibre cloth, laying stacks Obtain blank I；After phenolic resin-ethanol solution of the resulting 7 layers of alumina fibre cloth dipping 1:1 weight ratio of step 3), paving Stacking, which is put, obtains blank II.
(8) in die surface brushing release agent or laying processing release paper, successively by blank I, chopped mullite fiber after lamination Prepreg and blank II are fitted into mold.
(9) will be placed in mould test specimen on vulcanizing press and carry out hot-press solidifying, pressure 2MP, curing cycle be from room temperature with 10 DEG C/min is warming up to 120 DEG C, and pressurize 2MPa after heat preservation 30min, is then heated up 180 DEG C with 10 DEG C/min, after heat-insulation pressure keeping 2h Temperature fall.
(10) press will be removed with mould test specimen, demoulding obtains resistance to ablation lightweight solar heat protection heat-insulation integrative composite material.
The skin depth 3mm of resistance to ablation lightweight solar heat protection heat-insulation integrative composite material manufactured in the present embodiment, sandwich thickness Spend 20mm, underlayer thickness 2mm.Density only 1.017g/cm3, compression strength 16.8MPa, room temperature thermal conductivity 0.231W/mK.
Embodiment 4
A kind of resistance to ablation lightweight solar heat protection heat-insulation integrative composite material, the composite material are with chopped sic fiber for enhancing Body, using phenolic resin as resin, using phenolic aldehyde microballon as low density filler, using SiC fiber cloth as superficial layer reinforcement, with MoSi2 Powder, glass powder and carborundum powder are superficial layer ceramic packing.
The preparation method of above-mentioned resistance to ablation lightweight solar heat protection heat-insulation integrative composite material, including the following steps:
(1) by MoSi2Powder and SiC powder, which are scattered in the NaOH aqueous solution of NaOH content 10wt.%, handles 1h, with distillation Water or deionized water filter cleaning to filtrate neutrality, and 150 DEG C are dried for standby；It disperses montmorillonite powder in dehydrated alcohol, is added The silane coupling agent of powder quality 2% is filtered, 150 DEG C are dried for standby after 1h as surface modifier.
(2) SiC cloth of reinforcement fibers is cut out to 100mm × 100mm, it is totally 15 layers, spare.
(3) chopped sic fiber in mass ratio: solution: phenolic aldehyde microballon=9:40:2 first adds hollow phenolic aldehyde microballon filler Enter in 25wt.% phenolic resin-ethanol solution, stir evenly obtained slurry, chopped strand is then added, is put into mixing tank rotation Mixing is for 24 hours.
(4) by the chopped strand prepreg mixed 60 DEG C of drying 8h in an oven, until ethyl alcohol is dried substantially.
(5) MoSi in mass ratio2: glass powder: 50wt.% phenolic resin-ethyl alcohol is added in ceramic powder by SiC=1:1:2 In solution, the mass ratio of ceramic powder and resin is 1:1, stirs evenly obtained slurry.
(6) by slurry brushing or impregnation steps 3 made from step 6)) in resulting 8 layers of SiC fiber cloth, laying, which stacks, to be obtained Obtain blank I；After the resulting 7 layers of SiC fiber cloth dipping 50wt.% phenolic resin-ethanol solution of step 3), laying stacks acquisition Blank II.
(7) in die surface brushing release agent or laying processing release paper, successively blank I, chopped sic fiber after lamination are presoaked Material and blank II are fitted into mold.
(8) will be placed in mould test specimen on vulcanizing press and carry out hot-press solidifying, pressure 2MP, curing cycle be from room temperature with 10 DEG C/min is warming up to 120 DEG C, and pressurize 2MPa after heat preservation 30min, is then heated up 180 DEG C with 10 DEG C/min, after heat-insulation pressure keeping 2h Temperature fall.
(9) press will be removed with mould test specimen, demoulding obtains resistance to ablation lightweight solar heat protection heat-insulation integrative composite material.
The skin depth 3mm of resistance to ablation lightweight solar heat protection heat-insulation integrative composite material manufactured in the present embodiment, sandwich thickness Spend 20mm, underlayer thickness 2mm.Density only 0.88g/cm3, compression strength 11.0MPa, room temperature thermal conductivity 0.175W/mK.
Various embodiments of the present invention are described above, above description is exemplary, and non-exclusive, and It is not limited to disclosed each embodiment.Without departing from the scope and spirit of illustrated each embodiment, for this skill Many modifications and changes are obvious for the those of ordinary skill in art field.Therefore, protection scope of the present invention is answered This is subject to the protection scope in claims.

Claims (10)

1. a kind of resistance to ablation lightweight solar heat protection heat-insulation integrative composite material, which is characterized in that it is outside interlayer structure, including first Layer, the second outer layer and middle layer；The middle layer is that chopped strand is mixed in the phenolic resin for be dispersed with cenosphere and is formed Chopped strand prepreg, between first outer layer and the second outer layer；First outer layer is to brush in fiber cloth Or impregnate the layer that the slurry containing ceramic powder is formed；Second outer layer is that brushing or impregnated phenolic resin layer are formed in fiber cloth Layer.
2. resistance to ablation lightweight solar heat protection heat-insulation integrative composite material as described in claim 1, which is characterized in that described containing ceramics The slurry of powder is ceramic powder and phenolic aldehyde-ethanol solution formation mixture, ceramic powder and phenolic aldehyde-ethyl alcohol of weight ratio 1:1 The weight ratio of solution is 1:1.
3. the heat-insulation integrative of resistance to ablative thermal protection composite material as described in claim 1, which is characterized in that
Each component content is in first outer layer with volume percent are as follows: fiber cloth is 25%~40%；Phenolic resin is 25%~35%；Ceramic powder is 25%~35%；
Each component content is in the middle layer with volume percent are as follows: chopped strand is 5%~15%；Phenolic resin is 15% ~25%；Cenosphere is 60%~80%；
Each component content is in second outer layer with volume percent are as follows: fiber cloth is 45%~55%；Phenolic resin is 45%~55%.
4. resistance to ablation lightweight solar heat protection heat-insulation integrative composite material as described in claim 1, which is characterized in that the chopped fibre Dimension is any one or a variety of mixing in high silica fiber, quartz fibre, mullite fiber and SiC fiber, length 5~ 20mm。
5. resistance to ablation lightweight solar heat protection heat-insulation integrative composite material as described in claim 1, which is characterized in that described hollow micro- Pearl is one or more mixing of glass microballoon, ceramic microbead and phenolic aldehyde microballon.
6. resistance to ablation lightweight solar heat protection heat-insulation integrative composite material as described in claim 1, which is characterized in that the fiber cloth For SiC fiber cloth, alumina fibre cloth, quartz fiber cloth, high silica fiber cloth and mullite fiber cloth any one or it is more The mixing of kind.
7. resistance to ablation lightweight solar heat protection heat-insulation integrative composite material as described in claim 1, which is characterized in that the ceramic powder Body is SiC, MoSi2、B4C, mixture several in glass powder, montmorillonite, mica, feldspar and kaolin.
8. a kind of prepare the resistance to ablation lightweight solar heat protection heat-insulation integrative composite material as described in any claim in claim 1-7 Preparation method, which comprises the following steps:
1) it disperses ceramic powder in the NaOH aqueous solution that NaOH content is 10wt.% and handles 1h, then with distilled water or go It is neutrality that ionized water, which filters cleaning to filtrate, is redispersed in dehydrated alcohol after drying, and silane coupling agent is added and changes as surface Property agent stirring, dried at 150 DEG C after suction filtration, obtain pre-treatment ceramic powder；
2) chopped strand is kept the temperature to 0.5~1h in 300~500 DEG C of Muffle furnace to carry out degumming process, obtained short after degumming Cut fiber；
3) fiber cloth is cut out to being sized, it is spare；
4) cenosphere is added in phenolic resin-ethanol solution of weight ratio 1:3, stirs evenly obtained slurry, is then added Through step 2) treated chopped strand, it is put into mixing tank rotation mixing；
5) the resulting chopped strand prepreg slurry mixed of step 4) is dried in an oven, until ethyl alcohol volatilization is completely, is obtained To chopped strand prepreg；
6) the resulting pre-treatment ceramic powder of step 1) is added in phenolic resin-ethanol solution of weight ratio 1:1, is stirred evenly Ceramic powder slurry is made；
7) by the brushing of ceramic powder slurry or impregnation steps 3 made from step 6)) in the fiber cloth of resulting half quantity, laying It stacks and obtains blank I；Phenolic resin-ethyl alcohol of the fiber cloth dipping weight ratio 1:1 of the other half resulting quantity of step 3) is molten Liquid, then laying, which stacks, obtains blank II；
8) successively that the resulting blank I of step 7), step 5) is resulting short in die surface brushing release agent or laying processing release paper It cuts fiber prepreg material and the resulting blank II of step 7) is fitted into mold；
9) it will be placed in mould test specimen on vulcanizing press and carry out hot-press solidifying；
10) it will be removed with mould test specimen, and demould, obtain resistance to ablation lightweight heat release heat-insulation integrative composite material.
9. resistance to ablation lightweight solar heat protection heat-insulation integrative composite material and preparation method thereof as described in claim 8, which is characterized in that The weight of silane coupling agent accounts for the 2wt.% of ceramic powder weight in the step 1)；1h is stirred after silane coupling agent is added, is stirred Mix speed 150r/min；The mixing time of slurry and chopped strand is for 24 hours in the step 4).
10. resistance to ablation lightweight solar heat protection heat-insulation integrative composite material and preparation method thereof as described in claim 8, feature exist In,
Drying temperature is 60 DEG C in the step 5), drying time about 8h；
The pressure of hot pressing crosslinking curing is 2MP, program curing are as follows: be warming up to from room temperature with 10 DEG C/min speed in the step 9) It 120 DEG C, pressurizes 2MPa after keeping the temperature 30min, is then heated up 180 DEG C with 10 DEG C/min speed, Temperature fall after heat-insulation pressure keeping 2h.
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