CN109968757B - 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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CN109968757B
CN109968757B CN201910323696.4A CN201910323696A CN109968757B CN 109968757 B CN109968757 B CN 109968757B CN 201910323696 A CN201910323696 A CN 201910323696A CN 109968757 B CN109968757 B CN 109968757B
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heat
fiber cloth
ablation
phenolic resin
ceramic powder
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CN109968757A (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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    • 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
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    • 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
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    • 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
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    • 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
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    • 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
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    • 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
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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

Ablation-resistant light heat-proof heat-insulation integrated composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of thermal protection of aircrafts, and particularly relates to an ablation-resistant light heat-proof heat-insulation integrated composite material and a preparation method thereof.
Background
The light heat-proof and heat-insulating integrated light heat-proof material is a key technology for realizing miniaturization, high effective load ratio and rapid space access of a spacecraft represented by a space motor vehicle, and determines the advancement, reliability and economy of the spacecraft. With the development of the development work of novel spacecrafts in China, urgent needs are provided for light thermal protection materials with the functions of heat prevention and heat insulation.
1976. In 1996 and 2004, mars "sea theft number", "wilderness number" and "probe rover number" by NASA in the united states, respectively, succeeded in landing mars. The heat-proof layer on the windward side of the detector adopts SLA-561V honeycomb reinforced low-density ablation heat-proof materials produced by Rockschid Martin company. The density of SLA-561V is only 0.264g/cm3The super-light heat-proof material taking cork powder, silicon dioxide or glass microspheres, phenolic aldehyde microspheres, silicon dioxide and/or carbon fibers and the like as fillers is suitable for the peak heat flow density of 0.21MW/m2250s of reentry time and 1.1MJ/m of total heat2A maximum temperature of 1727 ℃. The "Galileo" Martian probe in the United states experiences reentry of the most severe thermal environmental conditions to date, with reentry into the Martian atmosphere at a rate of 48km/s and peak heat flux densities of up to 170MW/m2The dwell pressure is 7MPa, the heating time is 70s, and the highest ablation temperature is 3900 ℃. The thermal environment similar to ballistic reentry determined that the thermal protection layer was made of FM5055 carbon/phenolic material used on strategic missiles and had a density of 1.45g/cm3The thermal protection system weight represents 50% of the total weight of the aircraft.
A new generation of low density ablative thermal protective materials was developed in the united states in the nineties, with Phenolic Impregnated Carbon Ablates (PICAs) and Silicone Impregnated Reusable Ceramic Ablates (SIRCA) representing the light weight ablates (LCAs). SIRCA for heat flow less than 3MW/m2PICA for heat flows greater than 3MW/m2The environment of (2). The 'star dust' number re-entry capsule which is lifted off in 2 months in 1999 and returned in 1 month in 2006 adopts the integral PICA material as a heat-proof layer on the windward side, successfully stands the highest speed of an aircraft re-entering the earth of 12.9km/s and the peak heat flux density of 12MW/m2Into the environment. The density of the PICA is about 0.24-0.32 g/cm3A fibrous carbon-based heat insulating material manufactured by FMI corporation of usa is used as a reinforcement and impregnated with a phenolic resin, and thus the material is considered to be a lightweight carbon/phenolic material. The high porosity (about 85%) of PICA makes its thermal conductivity significantly lower than high densityThe carbon/phenolic aldehyde material has better heat-insulating property. SIRCA density of about 0.35g/cm3The heat-proof ceramic tile is prepared by impregnating ceramic tiles used on two space shuttles, namely LI-900 and LI-2200 manufactured by Rockschid company, by silicon resin, and is used for a heat-proof layer on the lee side of a Mars pathfinder, a back plate of a Mars exploration rover airship, and the front edge and the nose cone of an X-34 aircraft.
The aspect of ablation heat-proof materials in China develops phenolic aldehyde-terylene ablation heat-proof materials, H88 and H96 low-density ablation materials which take silicon rubber as a base and are formed by filling phenolic aldehyde and glass beads, and MD2 medium-density ablation materials which take phenolic aldehyde as a base and are reinforced by glass short fibers. Wherein, the phenolic aldehyde-terylene ablation heat-proof material is mainly used for the recoverable satellite and has the density of 1.280g/cm3Can be used for heat flow density of 3MW/m2The pneumatic heating environment of (a); the low-density ablative material comprises two kinds of materials H88 and H96, is used on the leeward side, the bottom and the windward side of the side wall of the Shenzhou airship, and has the density of 0.54g/cm3And 0.71g/cm3(ii) a The medium-density ablation heat-proof material MD2 is applied to the corner of the heat-proof outsole of the Shenzhou airship with serious airflow scouring.
In order to design the ablation-type low-density heat-proof heat-insulating material to cope with ablation loss in the use process, the design thickness of the heat-proof heat-insulating material is inevitably large, so that redundancy and increase of the external dimension are brought to the structure of the whole aircraft. The TUFROC applied by X-37B is taken as a representative, and a novel non-ablative low-density heat-proof and heat-insulation integrated material becomes a hot point of research. The TUFROC outer layer is a refractory, oxidation-resistant, lightweight ceramic/carbon material (ROCCI) cap, which is a high-density carbon-containing ceramic composite material with a fully dense surface, used as the outer layer to achieve non-ablative properties. The main components of ROCCI are carbon, silicon and oxygen, the use temperature reaches 1200K, and after the HETC (high-radiation low-catalysis) coating is added on the surface, the use temperature of ROCCI can reach 1931K within 10min and can reach 2255K within 1 min. The inner layer of TUFROC is a low density thermal insulation material such as AETB (aluminum enhancement thermal barrier) or FRCI (fiber recovery insulation composite) with a TUFI coating on the surface. The transition zone was 1.2mm thick of adhesive. The novel ceramic composite structure can not only bear the high temperature (the highest temperature is not lower than 1700 ℃) generated in reentry, but also solve the bottleneck problems of thermal cracking, oxidation resistance and the like of the ceramic tile in a high-temperature environment, and can be repeatedly utilized. However, the non-ablative low-density heat-proof and heat-insulation structure is a multi-layer combined structure, and the preparation cost is high. CN102815958A mixes chopped fiber, hollow micro-bead, ceramic filler and resin, then cross-links and solidifies, obtains a ceramizable resin matrix composite material with heat-proof and heat-insulation integrated functions. The material is added with low-density filler in ceramic resin to reduce the density and the heat conductivity, and simultaneously, the material is formed at one time, the preparation period is short, and the preparation cost is low. However, the low-density composite material has high ablation rate under high-speed airflow scouring and insufficient ablation resistance, still belongs to an ablation type heat-proof material, and cannot realize non-ablation heat-proof and heat-insulation integration.
Disclosure of Invention
The invention aims to solve the technical problems that a heat-insulating and heat-proof material used in the prior art is not ablation-resistant and short in service life, and provides an ablation-resistant light heat-insulating and heat-proof integrated composite material and a preparation method with a simple process.
The technical scheme adopted by the invention is as follows: an ablation-resistant light heat-proof heat-insulation integrated composite material is of a sandwich structure and comprises a first outer layer, a second outer layer and a middle layer; the middle layer is a chopped fiber prepreg layer formed by mixing chopped fibers in phenolic resin dispersed with hollow microbeads, and is positioned between the first outer layer and the second outer layer, namely a sandwich layer; the first outer layer is a layer formed by brushing or dipping slurry containing ceramic powder on fiber cloth, namely a surface anti-ablation layer; the second outer layer is a layer formed by coating or impregnating phenolic resin layer on the fiber cloth, namely a bottom surface bearing layer.
The first outer layer in the sandwich structure plays a role in resisting oxidation and ablation, the fiber cloth improves the integrity of a surface layer material, and the ceramic component plays a role in improving the oxidation and ablation resistance; the sandwich layer mainly plays a role in heat insulation, and the hollow microspheres improve the porosity of the sandwich material and realize light weight; the second outer layer is made of traditional resin-based composite materials and mainly plays a role in bearing.
Further, the slurry containing the ceramic powder is a mixture of the ceramic powder and a phenolic aldehyde-ethanol solution with the weight ratio of 1:1, and the weight ratio of the ceramic powder to the phenolic aldehyde-ethanol solution is 1: 1.
Further, the content of each component in the first outer layer is as follows by volume percent: 25 to 40 percent of fiber cloth; 25 to 35 percent of phenolic resin; 25 to 35 percent of ceramic powder; the content of each component in the middle layer is calculated by volume percent as follows: 5 to 15 percent of chopped fiber; 15 to 25 percent of phenolic resin; 60% -80% of hollow microspheres; the content of each component in the second outer layer is as follows by volume percent: 45% -55% of fiber cloth; 45 to 55 percent of phenolic resin.
Furthermore, the chopped fibers are one or a mixture of more of high silica fibers, quartz fibers, mullite fibers and SiC fibers, and have a length of 5-20 mm.
Further, the hollow microspheres are one or a mixture of glass microspheres, ceramic microspheres and phenolic microspheres.
Further, the fiber cloth is any one or a mixture of more of SiC fiber cloth, alumina fiber cloth, quartz fiber cloth, high silica fiber cloth and mullite fiber cloth.
Further, the ceramic powder is SiC or MoSi2、B4C. A mixture of several of glass powder, montmorillonite, mica, feldspar and kaolin.
The invention also provides a preparation method of the ablation-resistant light heat-proof heat-insulation integrated composite material, which comprises the following steps:
1) dispersing ceramic powder in a NaOH aqueous solution with the NaOH content of 10 wt.% for treatment for 1h, then carrying out suction filtration and cleaning with distilled water or deionized water until the filtrate is neutral, drying, dispersing in absolute ethyl alcohol, adding a silane coupling agent as a surface modifier, stirring, carrying out suction filtration, and drying at 150 ℃ to obtain pretreated ceramic powder;
2) keeping the temperature of the short-cut fibers in a muffle furnace at 300-500 ℃ for 0.5-1 h for degumming treatment to obtain degummed short-cut fibers;
3) cutting the fiber cloth to a set size for later use;
4) adding the hollow microspheres into a phenolic resin-ethanol solution with the weight ratio of 1:3, uniformly stirring to prepare a slurry, adding the chopped fibers, and putting the mixture into a mixing tank for mixing in a rotating manner;
5) drying the mixed chopped fiber prepreg slurry obtained in the step 4) in an oven until the ethanol is basically dried to obtain a chopped fiber prepreg;
6) adding the pretreated ceramic powder obtained in the step 1) into a phenolic resin-ethanol solution with the weight ratio of 1:1, and uniformly stirring to obtain ceramic powder slurry;
7) coating or dipping the ceramic powder slurry prepared in the step 6) on half of the number of the fiber cloth obtained in the step 3), and stacking to obtain a blank I; dipping the other half of the fiber cloth obtained in the step 3) into a phenolic resin-ethanol solution with the weight ratio of 1:1, and then layering and stacking to obtain a blank II;
8) coating a release agent on the surface of the mould or paving release paper, and sequentially filling the blank I obtained in the step 7), the chopped fiber prepreg obtained in the step 5) and the blank II obtained in the step 7) into the mould;
9) placing the test piece with the mold on a flat vulcanizing machine for hot-pressing solidification;
10) and taking down the test piece with the die, and demolding to obtain the ablation-resistant light heat release and heat insulation integrated composite material.
Further, in the step 1), the weight of the silane coupling agent accounts for 2 wt% of the weight of the ceramic powder; adding a silane coupling agent, and stirring for 1h at a stirring speed of 150 r/min; step 4), mixing the slurry and the chopped fibers for 24 hours;
further, the drying temperature in the step 5) is 60 ℃, and the drying time is 8 hours; the pressure of the hot-pressing crosslinking curing in the step 9) is 2MP, and the curing procedure is as follows: heating from room temperature to 120 deg.C at 10 deg.C/min, maintaining the temperature for 30min, pressurizing to 2MPa, heating to 180 deg.C at 10 deg.C/min, maintaining the temperature for 2 hr, and naturally cooling.
Compared with the prior art, the invention has the advantages that:
1. the ablation-resistant light heat-proof heat-insulation integrated composite material has the density of 0.5g/cm3～0.9g/cm3And has the characteristic of light weight.
2. The ablation-resistant light heat-proof heat-insulation integrated composite material can form a stable ablation-resistant ceramic layer on the surface within the temperature range of 800-1300 ℃, and meanwhile, the heat-insulation function is realized by low-density fillers such as hollow microspheres in the composite material, so that the heat-proof heat-insulation integrated function under the conditions of medium-low heat flow density, weak scouring and oxidation is realized; compared with the existing low-density heat-proof heat-insulating material, the material has more excellent ablation resistance, stable dimension and shape in a high-temperature environment and designable optimal use temperature; and the material can realize integration of non-ablation and heat-proof and heat-insulation functions, and is possibly used for a large-area heat protection material in a medium-low heat flow environment.
3. The preparation method of the invention enables the composite material to be molded at one time, compared with non-ablative heat-proof and heat-insulation integrated materials such as Turfoc and the like, the preparation method has the advantages of short preparation period, simple process, low cost and the like, can realize large-area heat-proof and heat-insulation integrated molding of an aircraft, avoids the bonding process of a blocky ceramic tile or Turfoc material, and can greatly improve the reliability.
Drawings
These and/or other aspects and advantages of the present invention will become more apparent and more readily appreciated from the following detailed description of the embodiments of the invention, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a macroscopic view of a section of an ablation-resistant lightweight thermal-insulation integrated composite material in example 1 of the present invention.
Fig. 2 is a SEM image of a surface layer material section of the ablation-resistant lightweight thermal insulation integrated composite material in example 1 of the present invention.
Fig. 3 is a SEM image of a cross-section of a sandwich layer material of the ablation-resistant lightweight thermal insulation integrated composite material in example 1 of the present invention.
Fig. 4 is a macroscopic view of the surface layer of the ablation-resistant lightweight heat-proof and heat-insulating integrated composite material after the oxyacetylene flame ablation.
Detailed Description
In order that those skilled in the art will better understand the present invention, the following detailed description of the invention is provided in conjunction with the accompanying drawings and the detailed description of the invention.
Example 1
The ablation-resistant light heat-proof heat-insulating integrated composite material is characterized by that its intermediate layer is made up by using short-cut high-silica fibre as reinforcement body, using phenolic resin as resin and using glass microsphere as low-density filler, and its surface layer is made up by using high-silica fibre cloth as reinforcement body and using B4The C powder, the montmorillonite powder and the silicon carbide powder are surface layer ceramic fillers.
The preparation of the ablation-resistant light heat-proof heat-insulation integrated composite material comprises the following steps:
(1) b is to be4Dispersing the C powder and the SiC powder in a NaOH aqueous solution with the NaOH content of 10 wt.% for processing for 1h, carrying out suction filtration and cleaning by using distilled water or deionized water until the filtrate is neutral, and drying at 150 ℃ for later use; dispersing montmorillonite powder in absolute ethyl alcohol, adding silane coupling agent with the mass of 2% of the powder as a surface modifier, filtering after 1h, and drying at 150 ℃ for later use.
(2) And (3) carrying out heat preservation on the short-cut high silica fiber in a muffle furnace at the temperature of 300-500 ℃ for 0.5-1 h for degumming treatment.
(3) The high silica reinforced fiber cloth was cut to 100mm × 100mm for 15 layers for use.
(4) Short-cut quartz fiber according to mass ratio: solution: hollow glass beads 6: 24: 5 weighing the chopped quartz fibers, the phenolic resin-ethanol solution and the hollow glass beads, adding the hollow glass bead filler into the phenolic resin-ethanol solution in a weight ratio of 1:3, uniformly stirring to obtain slurry, adding the chopped fibers, and putting the mixture into a mixing tank to rotate and mix for 24 hours.
(5) And drying the mixed chopped fiber prepreg in an oven at 60 ℃ for 8h until the ethanol is basically dried.
(6) According to the mass ratio B4C: montmorillonite: weighing ceramic powder in a ratio of 1:1:2, adding the ceramic powder into a phenolic resin-ethanol solution in a weight ratio of 1:1, wherein the mass ratio of the ceramic powder to the phenolic resin-ethanol solution is 1:1, and uniformly stirring to obtain slurry.
(7) Coating or dipping the slurry prepared in the step 6) on 8 layers of high silica fiber cloth obtained in the step 3), and stacking to obtain a blank I; and (3) soaking the 7 layers of high silica fiber cloth obtained in the step 3) in 50 wt.% of phenolic resin-ethanol solution, and stacking the layers to obtain a blank II.
(8) And (3) coating a release agent on the surface of the mould or paving release paper, and sequentially filling the laminated blank I, the short-cut high silica fiber prepreg and the blank II into the mould.
(9) And (3) placing the test piece with the die on a flat vulcanizing machine for hot-pressing curing under the pressure of 2MP, wherein the curing system is that the temperature is increased to 120 ℃ from room temperature at the speed of 10 ℃/min, the temperature is kept for 30min, then the pressure is increased to 2MPa, then the temperature is increased to 180 ℃ at the speed of 10 ℃/min, the temperature is kept and the pressure is kept for 2h, and then the temperature is naturally reduced.
(10) And taking the test piece with the die off the press, and demolding to obtain the ablation-resistant light heat-proof heat-insulation integrated composite material.
The macroscopic morphology of the longitudinal section of the ablation-resistant lightweight heat-proof heat-insulation integrated composite material prepared by the embodiment is shown in fig. 1. The surface layer microstructure is shown in FIG. 2 and the sandwich layer microstructure is shown in FIG. 3. The whole thickness of the material is 20mm, wherein the thickness of the first outer layer is 3mm, the thickness of the sandwich layer is 15mm, and the thickness of the second outer layer is 2 mm. The comprehensive density of the material is only 0859g/cm3The compression strength is 10.2MP, and the normal-temperature thermal conductivity is 0.182W/m.K. The oxyacetylene flame was ablated for 60s according to the GJB 323A-96 standard, the line ablation rate was about 0.03mm/s, and the macroscopic morphology after ablation is shown in FIG. 4.
Example 2
An ablation-resistant light-weight heat-proof heat-insulation integrated composite material comprises a middle layer, a surface layer and a heat insulation layer, wherein the middle layer of the composite material takes chopped quartz fibers as a reinforcement, phenolic cyanate ester as resin, glass beads as low-density filler, and quartz fiber cloth as reinforcement and B4The C powder, the glass powder, the kaolin and the silicon carbide powder are ceramic fillers.
The preparation method of the ablation-resistant light heat-proof heat-insulation integrated composite material comprises the following steps:
(1) b is to be4Dispersing the C powder and the SiC powder in a NaOH aqueous solution with the NaOH content of 10 wt.% for processing for 1h, carrying out suction filtration and cleaning by using distilled water or deionized water until the filtrate is neutral, and drying at 150 ℃ for later use; dispersing glass powder and kaolin into absolute ethyl alcohol, adding a silane coupling agent accounting for 2% of the mass of the powder as a surface modifier, performing suction filtration after 1 hour, and drying at 150 ℃ for later use.
(2) And (3) keeping the temperature of the short-cut quartz fiber in a muffle furnace at 300-500 ℃ for 0.5-1 h for degumming treatment.
(3) The quartz reinforced fiber cloth was cut to 100mm × 100mm for 15 layers for use.
(4) Short-cut quartz fiber according to mass ratio: phenolic resin-ethanol solution: hollow glass beads are 8: 25: 3 weighing the short-cut quartz fiber, the phenolic resin-ethanol solution and the hollow glass bead; then adding the hollow glass bead filler into a phenolic resin-ethanol solution in a weight ratio of 1:3, uniformly stirring to prepare slurry, adding the chopped fibers, and putting the mixture into a mixing tank to rotate and mix for 24 hours.
(5) And drying the mixed chopped fiber prepreg in an oven at 60 ℃ for 8h until the ethanol is basically dried.
(6) According to the mass ratio B4C: glass powder: kaolin: weighing ceramic powder according to the weight ratio of SiC to 2:1:1:4, adding the ceramic powder into a phenolic cyanate-butanone solution according to the weight ratio of 4:6, wherein the mass ratio of the ceramic powder to the phenolic cyanate-butanone solution is 1:1, and uniformly stirring to obtain slurry.
(7) Coating or dipping the slurry prepared in the step 6) on the 8 layers of quartz fiber cloth obtained in the step 3), and stacking to obtain a blank I; dipping the other 7 layers of quartz fiber cloth obtained in the step 3) in a phenolic resin-ethanol solution with the weight ratio of 1:1, and stacking to obtain a blank II.
(8) And (3) coating a release agent on the surface of the mould or paving release paper, and sequentially filling the laminated blank I, the chopped quartz fiber prepreg and the blank II into the mould.
(9) And (3) placing the test piece with the die on a flat vulcanizing machine for hot-pressing curing under the pressure of 2MP, wherein the curing system is that the temperature is increased to 120 ℃ from room temperature at the speed of 10 ℃/min, the temperature is kept for 30min, then the pressure is increased to 2MPa, then the temperature is increased to 180 ℃ at the speed of 10 ℃/min, the temperature is kept and the pressure is kept for 2h, and then the temperature is naturally reduced.
(10) And taking the test piece with the die off the press, and demolding to obtain the ablation-resistant light heat-proof heat-insulation integrated composite material.
The ablation-resistant lightweight heat-proof heat-insulation integrated composite material prepared by the embodiment has the advantages that the thickness of the first outer layer is 3mm, the thickness of the sandwich layer is 20mm, and the thickness of the second outer layer is 2 mm. The density is only 0.876g/cm3Compressive strength of 11.9MPa, normal temperatureThe thermal conductivity was 0.172W/m.K.
Example 3
An ablation-resistant light heat-proof heat-insulation integrated composite material, wherein a middle layer of the composite material takes chopped mullite fiber as a reinforcement, phenolic resin as resin and ceramic microspheres as low-density filler; the surface layer takes alumina fiber cloth as a reinforcement and MoSi2The powder, mica, feldspar and silicon carbide powder are used as surface layer ceramic fillers.
The preparation method of the ablation-resistant light heat-proof heat-insulation integrated composite material comprises the following steps:
(1) mixing MoSi2Dispersing the powder and SiC powder in 10 wt.% NaOH aqueous solution of NaOH Hanling for processing for 1h, carrying out suction filtration and cleaning by using distilled water or deionized water until the filtrate is neutral, and drying at 150 ℃ for later use; dispersing mica and feldspar powder in absolute ethyl alcohol, adding a silane coupling agent accounting for 2% of the mass of the powder as a surface modifier, filtering after 1 hour, and drying at 150 ℃ for later use.
(2) And (3) carrying out heat preservation on the chopped mullite fiber in a muffle furnace at the temperature of 300-500 ℃ for 0.5-1 h for degumming treatment.
(3) The alumina reinforced fiber cloth was cut to 100mm × 100mm for 15 layers for use.
(4) Chopping mullite fibers according to the mass ratio: solution: ceramic beads 16: 70: 9, firstly adding the hollow ceramic microbead filler into 25 wt.% of phenolic resin-ethanol solution, uniformly stirring to prepare slurry, then adding the chopped fibers, and putting the mixture into a mixing tank to rotate and mix for 24 hours.
(5) And drying the mixed chopped fiber prepreg in an oven at 60 ℃ for 8h until the ethanol is basically dried.
(6) MoSi in mass ratio2: mica: feldspar: adding the ceramic powder into a phenolic resin-ethanol solution with the weight ratio of 1:1, wherein the mass ratio of the ceramic powder to the resin is 1:1, and uniformly stirring to obtain slurry.
(7) Coating or dipping the slurry prepared in the step 6) on 8 layers of alumina fiber cloth obtained in the step 3), and stacking to obtain a blank I; dipping 7 layers of the alumina fiber cloth obtained in the step 3) in a phenolic resin-ethanol solution with the weight ratio of 1:1, and stacking to obtain a blank II.
(8) And (3) coating a release agent on the surface of the mould or paving release paper, and sequentially filling the laminated blank I, the chopped mullite fiber prepreg and the blank II into the mould.
(9) And (3) placing the test piece with the die on a flat vulcanizing machine for hot-pressing curing under the pressure of 2MP, wherein the curing system is that the temperature is increased to 120 ℃ from room temperature at the speed of 10 ℃/min, the temperature is kept for 30min, then the pressure is increased to 2MPa, then the temperature is increased to 180 ℃ at the speed of 10 ℃/min, the temperature is kept and the pressure is kept for 2h, and then the temperature is naturally reduced.
(10) And taking the test piece with the die off the press, and demolding to obtain the ablation-resistant light heat-proof heat-insulation integrated composite material.
The ablation-resistant light heat-proof heat-insulation integrated composite material prepared by the embodiment has the surface layer thickness of 3mm, the sandwich layer thickness of 20mm and the bottom layer thickness of 2 mm. The density is only 1.017g/cm3The compression strength is 16.8MPa, and the normal-temperature thermal conductivity is 0.231W/m.K.
Example 4
An ablation-resistant light heat-proof heat-insulation integrated composite material takes chopped SiC fibers as a reinforcement, phenolic resin as resin, phenolic microbeads as low-density filler, SiC fiber cloth as a surface layer reinforcement and MoSi2The powder, the glass powder and the silicon carbide powder are surface layer ceramic fillers.
The preparation method of the ablation-resistant light heat-proof heat-insulation integrated composite material comprises the following steps:
(1) mixing MoSi2Dispersing the powder and SiC powder in a NaOH aqueous solution with the NaOH content of 10 wt.% for processing for 1h, carrying out suction filtration and cleaning by using distilled water or deionized water until the filtrate is neutral, and drying at 150 ℃ for later use; dispersing montmorillonite powder in absolute ethyl alcohol, adding silane coupling agent with the mass of 2% of the powder as a surface modifier, filtering after 1h, and drying at 150 ℃ for later use.
(2) The SiC reinforced fiber cloth is cut to 100mm × 100mm, 15 layers in total, and is ready for use.
(3) Chopping SiC fibers according to the mass ratio: solution: phenol formaldehyde microbeads 9: 40: 2, firstly adding the hollow phenolic bead filler into 25 wt.% of phenolic resin-ethanol solution, uniformly stirring to prepare slurry, then adding the chopped fibers, and putting the mixture into a mixing tank to rotate and mix for 24 hours.
(4) And drying the mixed chopped fiber prepreg in an oven at 60 ℃ for 8h until the ethanol is basically dried.
(5) MoSi in mass ratio2: glass powder: adding the ceramic powder into 50 wt.% phenolic resin-ethanol solution with the mass ratio of the ceramic powder to the resin being 1:1:2, and uniformly stirring to obtain slurry.
(6) Coating or dipping the slurry prepared in the step 6) on 8 layers of SiC fiber cloth obtained in the step 3), and stacking to obtain a blank I; and (3) soaking the 7 layers of SiC fiber cloth obtained in the step 3) in 50 wt.% of phenolic resin-ethanol solution, and stacking the layers to obtain a blank II.
(7) And (3) coating a release agent on the surface of the mould or paving release paper, and sequentially filling the laminated blank I, the chopped SiC fiber prepreg and the blank II into the mould.
(8) And (3) placing the test piece with the die on a flat vulcanizing machine for hot-pressing curing under the pressure of 2MP, wherein the curing system is that the temperature is increased to 120 ℃ from room temperature at the speed of 10 ℃/min, the temperature is kept for 30min, then the pressure is increased to 2MPa, then the temperature is increased to 180 ℃ at the speed of 10 ℃/min, the temperature is kept and the pressure is kept for 2h, and then the temperature is naturally reduced.
(9) And taking the test piece with the die off the press, and demolding to obtain the ablation-resistant light heat-proof heat-insulation integrated composite material.
The ablation-resistant light heat-proof heat-insulation integrated composite material prepared by the embodiment has the surface layer thickness of 3mm, the sandwich layer thickness of 20mm and the bottom layer thickness of 2 mm. The density is only 0.88g/cm3The compressive strength is 11.0MPa, and the normal-temperature thermal conductivity is 0.175W/m.K.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (1)

1. An ablation-resistant light heat-proof heat-insulation integrated composite material is characterized by being of a sandwich structure and comprising a first outer layer, a second outer layer and a middle layer; the middle layer is a chopped fiber prepreg layer formed by mixing chopped fibers in phenolic resin dispersed with hollow microbeads and is positioned between the first outer layer and the second outer layer; the first outer layer is formed by coating or dipping slurry containing ceramic powder on a fiber cloth; the second outer layer is formed by coating or dipping phenolic resin on the fiber cloth;
the slurry containing the ceramic powder is a mixture formed by ceramic powder and a phenolic resin-ethanol solution with the weight ratio of 1:1, and the weight ratio of the ceramic powder to the phenolic resin-ethanol solution is 1: 1;
the content of each component in the first outer layer is as follows by volume percent: 40% of fiber cloth; 25 to 35 percent of phenolic resin; 25 to 35 percent of ceramic powder;
the intermediate layer comprises the following components in percentage by volume: 5 to 15 percent of chopped fiber; 15 to 25 percent of phenolic resin; 60% -80% of hollow microspheres;
the content of each component in the second outer layer is calculated by volume percent: 45% -55% of fiber cloth; 45 to 55 percent of phenolic resin;
the chopped fibers are any one or a mixture of more of high silica fibers, mullite fibers and SiC fibers, and the length of the chopped fibers is 5-20 mm;
the hollow microspheres are one or a mixture of glass microspheres, ceramic microspheres and phenolic microspheres;
the fiber cloth is any one or mixture of more of SiC fiber cloth, high silica fiber cloth and mullite fiber cloth;
the preparation method of the ablation-resistant light heat-proof heat-insulation integrated composite material comprises the following steps:
1) dispersing ceramic powder in a NaOH aqueous solution with the NaOH content of 10 wt.% for treatment for 1h, then carrying out suction filtration and cleaning with distilled water or deionized water until the filtrate is neutral, drying, then dispersing in absolute ethyl alcohol, adding a silane coupling agent as a surface modifier for stirring, carrying out suction filtration, and drying at 150 ℃ to obtain pretreated ceramic powder;
2) keeping the temperature of the chopped fibers in a muffle furnace at 300-500 ℃ for 0.5-1 h to carry out degumming treatment to obtain degummed chopped fibers;
3) cutting the fiber cloth to a set size for later use;
4) adding the hollow microspheres into a phenolic resin-ethanol solution in a weight ratio of 1:3, uniformly stirring to obtain slurry, adding the chopped fibers treated in the step 2), and putting the mixture into a mixing tank for rotating and mixing;
5) drying the mixed chopped fiber prepreg slurry obtained in the step 4) in an oven until ethanol is completely volatilized to obtain a chopped fiber prepreg;
6) adding the pretreated ceramic powder obtained in the step 1) into a phenolic resin-ethanol solution with the weight ratio of 1:1, and uniformly stirring to obtain ceramic powder slurry;
7) coating or dipping half of the fiber cloth obtained in the step 3) with the ceramic powder slurry prepared in the step 6), and stacking to obtain a blank I; dipping the other half of the fiber cloth obtained in the step 3) into a phenolic resin-ethanol solution with the weight ratio of 1:1, and then layering and stacking to obtain a blank II;
8) coating a release agent on the surface of the mould or paving release paper, and sequentially filling the blank I obtained in the step 7), the chopped fiber prepreg obtained in the step 5) and the blank II obtained in the step 7) into the mould;
9) placing the test piece with the mold on a flat vulcanizing machine for hot-pressing solidification;
10) taking down the test piece with the mold, and demolding to obtain the ablation-resistant light heat-proof heat-insulation integrated composite material;
in the step 1), the weight of the silane coupling agent accounts for 2 wt% of the weight of the ceramic powder; adding a silane coupling agent, and stirring for 1h at a stirring speed of 150 r/min; the mixing time of the slurry and the chopped fibers in the step 4) is 24 hours;
the drying temperature in the step 5) is 60 ℃, and the drying time is 8 h;
the pressure of hot-pressing curing in the step 9) is 2MPa, and the curing procedure is as follows: heating from room temperature to 120 deg.C at a speed of 10 deg.C/min, maintaining the temperature for 30min, pressurizing to 2MPa, heating to 180 deg.C at a speed of 10 deg.C/min, maintaining the temperature for 2 hr, and naturally cooling.
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