CN111908932B - Light high-efficiency heat-proof and heat-insulating integrated heat protection material and preparation method thereof - Google Patents
Light high-efficiency heat-proof and heat-insulating integrated heat protection material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a light high-efficiency heat-proof and heat-insulating integrated heat protection material and a preparation method thereof. The high-temperature resistant fiber heat-insulating tile comprises quartz fiber, mullite, alumina fiber or a combination thereof. The organic aerogel comprises resorcinol, formaldehyde, melamine, formaldehyde, phenolic resin, formaldehyde or mixed cresol, formaldehyde. According to the invention, the organic aerogel is added into the heat-insulating matrix, so that the mechanical strength of the heat-insulating material is improved at normal temperature, the material is ensured not to be broken in brittleness in the processing and transportation processes, so that the material is invalid, the heat-insulating performance of the material is improved in a low-temperature application environment, heat is taken away by ablation and volatilization in a high-temperature stage, and the normal use of the heat-protecting material in a service environment is ensured.
Description
Technical Field
The invention relates to the technical field of high-temperature resistant heat insulation materials, in particular to a light high-efficiency heat insulation integrated heat protection material and a preparation method thereof, which are applied to the surface of an aircraft or the environment with serious pneumatic heating in a short time and large heat flux.
Background
When a high-speed aerospace vehicle flies in the atmosphere or reenters the atmosphere, due to a severe pneumatic heating environment, a lightweight, dimensional and efficient heat protection material must be used to prevent heat from being transferred to the interior of the vehicle so as to ensure the safety of the vehicle. In addition to low density and low thermal conductivity, the tensile strength, compressive strength, high temperature linear shrinkage and recyclability of the insulation material are important factors to consider in material selection.
In the process of developing a space shuttle in the United states, a plurality of ceramic heat insulation tiles are developed successively for heat protection of the outer surface of the space shuttle. The first generation rigid ceramic heat insulating tile (Lockheed Insulation, LI) adopts silica sol to bond fused quartz glass fiber, and has the maximum use temperature of 1260 ℃ and the density of 0.14g/cm 3 LI-900 and a density of 0.35g/cm 3 LI-2200 of (B) was applied to the first space shuttle Columbia number. U.S. patent No. 3952083 discloses a process for preparing a rockwell insulation material. The second generation rigid ceramic heat insulating tile-refractory fiber composite material heat insulating tile (Fibrous Refractory Composite Insulation, FRCI) consists of 85 percent of quartz fiber and 15 percent of aluminum borosilicate fiber (Nextel (TM) 312, manufactured by 3M company), has the advantages of low density and high strength when the use temperature is increased to 1320 ℃, and has the density of 0.20g/cm from the third space plane Discovery number (Discovery, 1981) 3 Is replacing most of the LI-2200 rigid insulating tiles. U.S. patent No. 4148962 discloses a process for preparing FRCI. The third generation rigid ceramic insulating tiles are represented by high insulating property materials (High Thermal Performance, HTP) and alumina reinforced thermal barrier materials (Alumina Enhanced Thermal Barrier, AETB) developed in the 80 s. HTP is composed of 60% to 80% quartz fiber, 20% to 40% alumina fiber, and 0.1% to 6% boron nitride sintering agent. U.S. patent No. 5629186 discloses a process for preparing HTP insulation materials. AETB is composed of 68% quartz fiber, 20% alumina fiber and 12% NextelTM312 fiber. Wherein the addition of alumina fibers significantly improves the temperature resistance of the material. The fourth generation rigid heat insulation tile boeing rigid heat insulation material (Boeing Rigid Insulation, BRI) is formed by 60 to 80% by mass of quartz fiber, 20 to 40% by mass of alumina fiber, and 0.1 to 1% by mass of boron carbide powder sintering agent. U.S. patent No. 6716782B2 discloses a preparation process of BRI.
The existing rigid heat-insulating tile and mechanical connection type heat protection system has excellent heat protection and anti-scouring performance, but the overall heat insulation efficiency is low, mainly because the preparation process of the high-temperature-resistant heat-insulating tile developed at present is not mature, and the overall strength of the material is low; on the other hand, the combined heat-proof and heat-proof integrated heat protection material connects the heat insulation material and the heat-proof material together through mechanical connection, wherein the inner layer rigid heat insulation material for heat insulation has low toughness and poor mechanical property, is not easy to process into a high-precision structure, and although the inorganic high-temperature-resistant adhesive can provide partial bonding strength, the rigid heat insulation material has high brittleness, is easy to damage in the assembly process, and influences the reliability of the integral performance of the heat protection material, so the demand of the novel rigid heat insulation material with high toughness and high efficiency is increasingly urgent.
Disclosure of Invention
The invention aims at solving the problems, and provides a light high-efficiency heat-proof and heat-insulating integrated heat protection material and a preparation method thereof, which solve the problems of immature preparation process of a high-temperature-resistant heat-insulating material and low overall strength of the material.
The heat protection material is prepared by impregnating an organic aerogel into a heat insulation matrix, wherein the heat insulation matrix is a high-temperature-resistant fiber heat insulation tile.
The high-temperature resistant fiber heat-insulating tile comprises quartz fiber, mullite or alumina fiber or a combination thereof.
The organic aerogel includes resorcinol+formaldehyde (RF aerogel), melamine+formaldehyde (MF aerogel), phenolic resin+formaldehyde (PM aerogel), or mixed cresol+formaldehyde (JF aerogel).
A preparation method of a light high-efficiency heat-proof and heat-insulating integrated heat protection material comprises the following process steps:
1) Preparing a high-temperature-resistant fiber heat-insulating tile:
adding the pretreated high-temperature resistant fiber into water with the mass of 20-60 times of that of the fiber, adding a high-temperature binder with the mass of 1-10% of that of the fiber, and adding silica sol with the mass of 1-4 times of that of the fiber;
press-filtering the mixed materials to form the materials, wherein the pressure is 3-5 Mpa;
demolding and drying the molded object, wherein the drying temperature is 50-150 ℃;
sintering and shaping the dried substance, wherein the sintering temperature is 1100-1500 ℃;
2) Organic aerogel is compounded with heat insulation matrix:
preparing organic aerogel, and putting the sintered and shaped high-temperature-resistant fiber heat-insulating tile into the organic aerogel for impregnation, wherein the mass of the organic aerogel is 20-95% of the mass of the heat-insulating tile.
The high temperature resistant fiber is quartz fiber, mullite or alumina fiber or the combination thereof, and the fiber length is 30-300 mu m.
Preferably, the high temperature resistant fiber is a combination of any 2 fibers, and the mass ratio is 9:1-5:5.
The quartz fiber is an inorganic fiber prepared from high-purity quartz or natural crystal, and the diameter of the quartz fiber is generally several micrometers to tens of micrometers. It maintains some characteristics and performances of solid quartz, is an excellent high-temperature resistant material, and can be used as a reinforcing phase of advanced composite material. The high-temperature resistance is higher than that of high-silica fiber, the long-term use temperature can reach 1200 ℃, the softening point temperature is up to 1700 ℃, and the high-temperature-resistant high-electrical-insulation high-temperature-resistant high-electrical-insulation high-fiber composite fiber has high electrical insulation performance, ablation resistance, thermal shock resistance, excellent dielectric performance, excellent chemical stability and the like.
Mullite is a good refractory material and is a rare mineral of this type. Mullite is a mineral that aluminosilicates produce at high temperatures and forms mullite when the aluminosilicates are artificially heated. The natural mullite crystals are long and thin needle-shaped and are in radial cluster shape. Mullite ores are used to produce high temperature refractory materials. The C/C composite material is widely used as a thermal barrier coating.
The organic aerogel is resorcinol+formaldehyde (RF aerogel), melamine+formaldehyde (MF aerogel), phenolic resin+formaldehyde (PM aerogel), or mixed cresol+formaldehyde (JF aerogel).
The high-temperature binder is boron nitride or boron carbide powder, and the mass of the high-temperature binder is 1-10% of the mass of the fiber.
The dipping mode is vacuum dipping, and the dipping vacuum degree is controlled to be-0.1-0.05 MPa.
The impregnation mode is gradient impregnation, and the gradient impregnation is formed by repeating sol-gel treatment for a plurality of times and sequentially reducing the density of the organic aerogel used for impregnation.
Compared with the prior art, the light high-efficiency heat-proof and heat-insulating integrated heat protection material and the preparation method thereof have the following outstanding beneficial effects:
according to the invention, the organic aerogel is added into the heat-insulating matrix, so that the mechanical strength of the heat-insulating material is improved at normal temperature, the material is ensured not to be broken in brittleness in the processing and transportation processes, so that the material is invalid, the heat-insulating performance of the material is improved in a low-temperature application environment, heat is taken away by ablation and volatilization in a high-temperature stage, and the normal use of the heat-protecting material in a service environment is ensured.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
A preparation method of a light high-efficiency heat-proof and heat-insulating integrated heat protection material comprises the following process steps:
preparing a high-temperature-resistant heat-insulating tile: adding pretreated quartz fiber and mullite fiber (fiber length is 30-300 mu m) into water with the mass ratio of 20 times of the fiber according to the mass ratio of 9:1, adding boron nitride powder with the mass ratio of 1% of the fiber, adding silica sol with the mass ratio of 1 time of the fiber, performing filter pressing forming, pressing under the pressure of 3MPa, demolding and drying, drying at the temperature of 50 ℃, then sintering at the temperature of 1100 ℃;
the organic aerogel is prepared from resorcinol and formaldehyde (RF aerogel), the mass is 20% of that of the high-temperature-resistant heat-insulating tile, and the sintered high-temperature-resistant heat-insulating tile is subjected to vacuum impregnation, wherein the impregnation vacuum degree is controlled at-0.1 MPa.
Light weight is obtainedHigh-quality efficient heat-proof and insulation integrated heat protection material with density of 0.35g/cm 3 The compression strength is more than 1MPa, the tensile strength is more than 0.35MPa, the normal-temperature heat conductivity coefficient is less than 0.04W/m.K, the heat conductivity coefficient at 300 ℃ is 0.05W/m.K, the service temperature is below 1300 ℃, and the heat insulation material can be used for large-area heat protection and heat insulation requirements of aircrafts.
Example 2
Preparing a high-temperature-resistant heat-insulating tile: the pretreated quartz fiber and alumina fiber (fiber length is 30-300 μm) are adopted, and the mass ratio is 5:5, adding the proportioning into water with the mass being 60 times of that of the fiber, adding boron nitride powder with the mass being 10 percent of that of the fiber, adding silica sol with the mass being 4 times of that of the fiber, performing filter pressing forming, performing demoulding and drying at the drying temperature of 150 ℃ under the pressure of 5MPa, and then sintering at the sintering temperature of 1300 ℃;
the organic aerogel is prepared from melamine and formaldehyde (MF aerogel), the mass is 95% of that of the high-temperature-resistant heat-insulating tile, and the sintered high-temperature-resistant heat-insulating tile is subjected to vacuum impregnation, wherein the impregnation vacuum degree is controlled at 0.05MPa.
To obtain the light high-efficiency heat-proof and heat-insulating integrated heat protection material with the density of 0.8g/cm 3 The compression strength is more than 10MPa, the tensile strength is more than 2.5MPa, the normal-temperature heat conductivity coefficient is less than 0.06W/m.K, the heat conductivity coefficient at 300 ℃ is 0.12W/m.K, the use temperature is more than 1500 ℃, and the heat insulation material can be used for large-area heat protection and heat insulation requirements of aircrafts.
Example 3
Preparing a high-temperature-resistant heat-insulating tile: the pretreated mullite fiber and alumina fiber (fiber length is 30-300 μm) are adopted, and the mass ratio is 7:3, adding the ingredients in proportion into water with 40 times of the fiber mass, adding boron carbide powder with 6% of the fiber mass, adding silica sol with 2.5 times of the fiber mass, performing filter pressing forming, performing demoulding and drying at 100 ℃, and then sintering at 1500 ℃;
the organic aerogel is prepared from melamine and formaldehyde (MF aerogel), the mass is 60% of that of the high-temperature-resistant heat-insulating tile, and the sintered high-temperature-resistant heat-insulating tile is placed into the vacuum for vacuum impregnation, and the impregnation vacuum degree is controlled at 0.01MPa.
To obtain the light high-efficiency heat-proof and heat-insulating integrated heat protection material with the density of 0.6g/cm 3 The compression strength is more than 3MPa, the tensile strength is more than 1MPa, the normal-temperature heat conductivity coefficient is less than 0.08W/m.K, the heat conductivity coefficient at 300 ℃ is 0.2W/m.K, the use temperature is 1500 ℃, and the heat insulation material can be used for large-area heat protection and heat insulation requirements of aircrafts.
Example 4
Preparing a high-temperature-resistant heat-insulating tile: adding pretreated quartz fiber (fiber length of 30-300 μm) into water with 40 times of fiber mass, adding boron carbide powder with 6% of fiber mass, adding silica sol with 2.5 times of fiber mass, press-filtering to form, pressing under 4MPa, demolding and drying at 100deg.C, sintering at 1200deg.C;
the organic aerogel is prepared from phenolic resin and formaldehyde (PM aerogel), the mass is 50% of the mass of the high-temperature-resistant heat-insulating tile, the high-temperature-resistant sintered and formed tile is put into the container for gradient impregnation, and the impregnation vacuum degree is controlled at 0.01MPa.
To obtain the light high-efficiency heat-proof and heat-insulating integrated heat protection material with the density of 0.3g/cm 3 The compression strength is more than 2MPa, the tensile strength is more than 0.85MPa, the normal-temperature heat conductivity coefficient is less than 0.05W/m.K, the heat conductivity coefficient at 300 ℃ is 0.06W/m.K, the service temperature is below 1200 ℃, and the heat insulation material can be used for large-area heat protection and heat insulation requirements of aircrafts.
The mullite fiber and the alumina fiber have similar characteristics when used alone, and can meet the large-area heat protection and heat insulation requirements of the aircraft, and are not repeated here.
The foregoing description of the preferred embodiments of the present application is not intended to limit the invention to the particular embodiments of the present application, but to limit the scope of the invention to the particular embodiments of the present application.
Claims (3)
1. The light high-efficiency heat-proof and heat-insulating integrated heat protection material is characterized in that the heat protection material is prepared by impregnating an organic aerogel heat-insulating matrix, wherein the heat-insulating matrix is a high-temperature-resistant fiber heat-insulating tile; the preparation method comprises the following steps:
1) Preparing a high-temperature-resistant fiber heat-insulating tile:
adding the pretreated high-temperature resistant fiber into water with the mass of 20-60 times of that of the fiber, adding a high-temperature binder with the mass of 1-10% of that of the fiber, and adding silica sol with the mass of 1-4 times of that of the fiber; wherein the high temperature resistant fiber is quartz fiber, mullite or alumina fiber or the combination thereof, and the fiber length is 30-300 mu m;
press-filtering the mixed materials to form the materials, wherein the pressure is 3-5 Mpa;
demolding and drying the molded object, wherein the drying temperature is 50-150 ℃;
sintering and shaping the dried substance, wherein the sintering temperature is 1100-1500 ℃;
2) Organic aerogel is compounded with heat insulation matrix:
preparing organic aerogel, and putting the sintered and shaped high-temperature-resistant fiber heat-insulating tile into the organic aerogel for impregnation, wherein the mass of the organic aerogel is 20-95% of the mass of the heat-insulating tile;
the impregnation mode is gradient impregnation, sol-gelation treatment is repeated for a plurality of times, and the density of organic aerogel used for impregnation is sequentially reduced to form gradient impregnation;
the dipping mode is vacuum dipping, and the dipping vacuum degree is controlled to be-0.1-0.05 MPa.
2. The light-weight efficient heat-proof and heat-insulating integrated heat protection material according to claim 1, wherein the organic aerogel is resorcinol + formaldehyde, melamine + formaldehyde, phenolic resin + formaldehyde or mixed cresol + formaldehyde.
3. The light efficient heat-proof and heat-insulating integrated heat protection material according to claim 1, wherein the high-temperature binder is boron nitride powder or boron carbide powder, and the mass of the high-temperature binder is 1-10% of the mass of the fiber.
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| CN114455978B (en) * | 2022-03-09 | 2023-03-17 | 长沙思云新材料科技有限公司 | Fiber-reinforced mullite-proportioned oxide-modified phenolic resin aerogel composite material and preparation method thereof |
| CN115159954B (en) * | 2022-07-15 | 2023-05-09 | 航天特种材料及工艺技术研究所 | Aerogel heat insulation layer and preparation method thereof |
| CN115521158B (en) * | 2022-10-11 | 2023-08-18 | 南京工业大学 | Preparation method of high-air-permeability ceramic fiber filter tube |
| CN115536415B (en) * | 2022-12-01 | 2023-03-10 | 中南大学 | Ablation-resistant heat-insulation integrated composite material and preparation method thereof |
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