CN101691138A - Method for preparing heat insulation tile of shuttle - Google Patents
Method for preparing heat insulation tile of shuttle Download PDFInfo
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- CN101691138A CN101691138A CN200910017754A CN200910017754A CN101691138A CN 101691138 A CN101691138 A CN 101691138A CN 200910017754 A CN200910017754 A CN 200910017754A CN 200910017754 A CN200910017754 A CN 200910017754A CN 101691138 A CN101691138 A CN 101691138A
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Abstract
The invention relates to a method for preparing heat insulation tiles of a shuttle, which is mainly used in heat insulation of shuttles and aircraft heat insulation protecting field such as other aerospace, aviation, guided missile and the like, belonging to the special technical field. The method comprises the steps of matrix batching, shaping, sintering and implementing coating, and the matrix batching is prepared from the following components by weight percent: 50-95% of fused quartz glass fiber, 5-50% of alumina fiber, 0-5% of boron nitride and 0-3% of matrix assistant. The heat insulation tile in the invention has the advantages of high-temperature resistance, high strength, low density, low heat conduction and fine heat insulation effect.
Description
Technical field
The present invention relates to a kind of preparation method of heat insulation tile of shuttle, thermal insulation tile is mainly used in the heat insulation protection of aircraft fields such as the heat insulation of space shuttle and other space flight, aviation, guided missile, belongs to the special technology field.
Background technology
The main material of making space shuttle is an aluminium, and is not by a long sight from 1649 degrees centigrade heatproofs requirement, therefore must add a thermal insulation layer to it.Early stage space flight project, what add on the spacecraft is to melt thermal insulation layer, and this thermal insulation layer falls heat exhaustion because of thawing, and it provides the actv. protection to spacecraft, and shortcoming is that it is disposable, can not repeated usage.Space shuttle needs repeated usage, and it is very necessary to equip a kind of new reusable thermal insulation layer.This new material thermal insulation layer must have that density is low, coefficient of thermal conductivity is low, high temperature resistant, intensity is high and the characteristics of high heat-insulating efficiency, the problem that current material exists is: the thermal insulation material that density is lower, resistance to compression, tensile strength are low, perhaps directly are exactly flexible material.The material that intensity is high exists the shortcoming that density is big, heat-insulating efficiency is low, and concerning apparent weight was the Aeronautics and Astronautics aircraft of life, aircraft was light more good more, and thermal insulation material must have lower density and also high strength will be arranged simultaneously thus.
Abroad; the novel space shuttle thermal protection system of the U.S. (TPS) mainly is to be made of several thousand even up to ten thousand blocks of thermal insulation tiles of being attached to the space shuttle belly; because the 80-90% of thermal insulation tile volume is an air; so its weight is extremely light; take just as having taken a plastic foam; the highest can anti-1260 degrees centigrade high temperature, have certain intensity simultaneously, the U.S., Russia are carrying out during constantly research improves this material always.Because this material application value in army is huge, so its manufacture method etc. are holded in close confidence, China since the seventies, carries out constantly exploring the research of this material always, has obtained huge progress in the recent period, has obtained to use in batches.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of heat insulation tile of shuttle, can make the thermal insulation tile of high temperature resistant, high strength, lower density, low heat conduction and good heat-insulation effect.
The preparation method of heat insulation tile of shuttle of the present invention, comprise matrix batching, moulding, burn till and implement coating, the matrix ingredients by weight consists of: fused silica glass fiber 50~95%, alumina fibre 5~50%, boron nitride 0~5% and matrix auxiliary agent 0~3%.
Wherein:
The matrix auxiliary agent is silicasol and methylcellulose according to weight ratio 1: the compound of (0.5~1.5);
The fused silica glass fibre diameter is 1~10 μ m, SiO
2Weight content 〉=95%;
The alumina fibre diameter is 3~20 μ m, Al
2O
3Weight content 〉=80%.
At first, add boron nitride and auxiliary agent dispersed with stirring again, make the matrix blank through under 1100~1400 ℃ high temperature, burning till after the suction filtration moulding with fused silica glass fiber and alumina fibre ball mill grinding.
Blank can heatproof be up to 1700 ℃, can be 600-1200 ℃ of long-term use, and density is low, is 0.20~0.40g/cm
3, coefficient of thermal conductivity is low, the minimum 0.046w/mk that reaches, intensity height, resistance to compression 〉=2MPa, tension 〉=0.5Mpa.
Prepare coating material again:
Coating compounding weight consists of: synthetic borosilicate glass powder 50~80%, beta-eucryptite 5~30%, silica flour 0~5%, four silicon borides 0~20%, black pigment 0~10% and coating aid 1~3%, wherein, coating aid is mixed by carbowax and tributyl phosphate, and the weight blending ratio is 2: (0.5~2).
Wherein:
Synthetic borosilicate glass powder be by boron oxide and silicon dioxide by weight 1: (2~20) are synthetic through 1000~1200 ℃ of fusions of high temperature;
Eucryptite be by lithium carbonate, aluminium oxide and silicon dioxide according to mol ratio 1: 1: (2~5) are synthetic through 1100~1400 ℃ of high temperature;
Black pigment is cobalt black pigment or does not have cobalt black pigment.
Implement coating:
Cleaning matrix blank, with the synthetic borosilicate glass powder of coating compounding, beta-eucryptite, silica flour, four silicon borides and black pigment, disperse through ball milling, add water and coating aid furnishing slip again, can spray or brush on the matrix blank, to make and film, dry after 1100~1400 ℃ high temperature sintering makes the thermal insulation tile product.
The coating resistance to elevated temperatures is good, can have the low bulk performance in long-term use below 1200 ℃, and coefficient of expansion is 1~10 * 10
-6Between the mm/mm.K, good in conjunction with matching performance, high radiation, radiation coefficient is 0.05~0.95, water resistance good (≯ 0.3%), and also any surface finish is smooth.
Experimental results show that, the preparation method of heat insulation tile of shuttle of the present invention, can make the thermal insulation tile of high temperature resistant, high strength, lower density, low heat conduction and good heat-insulation effect, also can prepare other type spare product of different shape specification, be used for space shuttle and the high-speed aircraft surface is heat insulation, also can be widely used in the aircraft such as the space flight that requires high temperature resistant, lower density, low heat conduction, high strength, effectively insulating, aviation, guided missile in the heat insulation protection.
The specific embodiment
The invention will be further described below in conjunction with embodiment.
Synthetic borosilicate glass powder by boron oxide and silicon dioxide by weight 1: (2~20) are synthetic through 1000~1200 ℃ of fusions of high temperature.
Beta-eucryptite by lithium carbonate, aluminium oxide and silicon dioxide according to mol ratio 1: 1: (2~5) are synthetic through 1100~1400 ℃ of high temperature.
Embodiment 1
Quartz fiber composite heat-insulated material of the present invention, ingredients by weight consists of:
Fused silica glass 80%, alumina fibre 15%, boron nitride 3% and matrix auxiliary agent 2%;
Wherein the fused silica glass fibre diameter is 1~10 μ m, SiO
2Weight content 〉=95%;
The alumina fibre diameter is 3~20 μ m, Al
2O
3Weight content 〉=80%;
At first utilize the shears weak point to cut fused silica glass fiber and alumina fibre to 1-3cm;
The matrix auxiliary agent is that silicasol and methylcellulose are according to 1: 1 compound of weight ratio.
With fused silica glass fiber and alumina fibre difference or mixing and ball milling pulverizing, 300 mesh sieves filter, and add matrix auxiliary agent, boron nitride and deionized water medium and carry out dispersed with stirring, pour the suction filtration forming mould into and carry out moulding, burn till after the oven dry and make the matrix blank.
Coating compounding weight consists of: synthetic borosilicate glass powder 65%, beta-eucryptite 15%, fused quartz powder 5%, four silicon boride 8%, cobalt black 6% and coating aid 1%.
Wherein, coating aid is mixed by carbowax and tributyl phosphate, and the weight blending ratio is 2: 1.
Synthetic borosilicate glass powder is synthetic through 1100 ± 15 ℃ of fusions of high temperature by weight 1: 10 by boron oxide and silicon dioxide.
Beta-eucryptite is synthetic through 1150 ± 10 ℃ of high temperature according to mol ratio 1: 1: 3 by lithium carbonate, aluminium oxide and silicon dioxide.
Cleaning matrix blank, with the synthetic borosilicate glass powder of coating compounding, beta-eucryptite, silica flour, four silicon borides and black pigment, disperse through ball milling, add water and coating aid furnishing slip again, can spray or brush on the matrix blank, to make and film, dry after 1150 ℃ high temperature sintering makes the thermal insulation tile product.Sampling records performance figure according to GB: 1200 ℃ of heatproofs, and do not have distortion and shrink density 0.29g/cm in 2 hours
3' coefficient of thermal conductivity 0.049w/mk, normal direction radiation coefficient 0.95, compressive strength 2.8MPa, thickness direction tensile strength 0.79MPa.
Embodiment 2
Quartz fiber composite heat-insulated material of the present invention, ingredients by weight consists of:
Fused silica glass fiber 85%, alumina fibre 10%, boron nitride 3% and matrix auxiliary agent 2%;
Wherein the fused silica glass fibre diameter is 1~10 μ m, Si02 weight content 〉=95%;
The alumina fibre diameter is 3~20 μ m, Al
2O
3Weight content 〉=80%;
At first utilize the shears weak point to cut fused silica glass fiber and alumina fibre to 1-3cm;
The matrix auxiliary agent is that silicasol and methylcellulose are according to 1: 1 compound of weight ratio.
With fused silica glass fiber and alumina fibre difference or mixing and ball milling pulverizing, 300 mesh sieves filter, and add matrix auxiliary agent, boron nitride and deionized water medium and carry out dispersed with stirring, pour the suction filtration forming mould into and carry out moulding, burn till after the oven dry and make the matrix blank.
Coating compounding weight consists of: synthetic borosilicate glass powder 50%, beta-eucryptite 30%, fused quartz powder 5%, four silicon boride 6%, cobalt black 7% and coating aid 2%.
Wherein, coating aid is mixed by carbowax and tributyl phosphate, and the weight blending ratio is 2: 1.5.
Synthetic borosilicate glass powder is synthetic through 1050 ± 30 ℃ of fusions of high temperature by weight 1: 15 by boron oxide and silicon dioxide.
Beta-eucryptite is synthetic through 1200 ± 20 ℃ of high temperature according to mol ratio 1: 1: 2.5 by lithium carbonate, aluminium oxide and silicon dioxide.
Other process is with embodiment 1, molding pressure 0.08MPa, and 1250 ℃ of firing temperatures, 1200 ℃ of coating firing temperatures are prepared thermal insulation tile, and sampling records performance figure according to GB and is: 1200 ℃ of heatproofs, do not have distortion and shrink density 0.27g/cm in 2 hours
3' coefficient of thermal conductivity 0.049w/mk, normal direction radiation coefficient 0.90, compressive strength 2.3MPa, thickness direction tensile strength 0.72MPa.
Embodiment 3
Quartz fiber composite heat-insulated material of the present invention, ingredients by weight consists of:
Fused silica glass fiber 91.5%, alumina fibre 5%, boron nitride 0.5% and matrix auxiliary agent 3%;
Wherein the fused silica glass fibre diameter is 1~10 μ m, SiO
2Weight content 〉=95%;
The alumina fibre diameter is 3~20 μ m, Al
2O
3Weight content 〉=80%;
At first utilize the shears weak point to cut fused silica glass fiber and alumina fibre to 1-3cm;
The matrix auxiliary agent is that silicasol and methylcellulose are according to 1: 1 compound of weight ratio.
With fused silica glass fiber and alumina fibre difference or mixing and ball milling pulverizing, 300 mesh sieves filter, and add matrix auxiliary agent, boron nitride and deionized water medium and carry out dispersed with stirring, pour the suction filtration forming mould into and carry out moulding, burn till after the oven dry and make the matrix blank.
Coating compounding weight consists of: synthetic borosilicate glass powder 80%, beta-eucryptite 5%, fused quartz powder 3%, four silicon boride 5%, cobalt black 6% and coating aid 1%.
Wherein, coating aid is mixed by carbowax and tributyl phosphate, and the weight blending ratio is 2: 1.
Synthetic borosilicate glass powder is synthetic through 1160 ± 10 ℃ of fusions of high temperature by weight 1: 8 by boron oxide and silicon dioxide.
Beta-eucryptite is synthetic through 1300 ± 30 ℃ of high temperature according to mol ratio 1: 1: 4 by lithium carbonate, aluminium oxide and silicon dioxide.
Other process is with embodiment 1, molding pressure 0.08MPa, and 1250 ℃ of firing temperatures, 1100 ℃ of coating firing temperatures are prepared thermal insulation tile, and sampling records performance figure according to GB and is: 1200 ℃ of heatproofs, do not have distortion and shrink density 0.22g/cm in 2 hours
3' coefficient of thermal conductivity 0.046w/mk, normal direction radiation coefficient 0.87, compressive strength 2.0MPa, thickness direction tensile strength 0.59MPa.
Embodiment 4
Quartz fiber composite heat-insulated material of the present invention, ingredients by weight consists of:
Fused silica glass fiber 50%, alumina fibre 45%, boron nitride 2% and matrix auxiliary agent 3%;
Wherein the fused silica glass fibre diameter is 1~10 μ m, SiO
2Weight content 〉=95%;
The alumina fibre diameter is 3~20 μ m, Al
2O
3Weight content 〉=80%;
At first utilize the shears weak point to cut fused silica glass fiber and alumina fibre to 1-3cm;
The matrix auxiliary agent is that silicasol and methylcellulose are according to 1: 1 compound of weight ratio.
With fused silica glass fiber and alumina fibre difference or mixing and ball milling pulverizing, 300 mesh sieves filter, and add matrix auxiliary agent, boron nitride and deionized water medium and carry out dispersed with stirring, pour the suction filtration forming mould into and carry out moulding, burn till after the oven dry and make the matrix blank.
Coating compounding weight consists of: synthetic borosilicate glass powder 63%, beta-eucryptite 19%, fused quartz powder 7%, four silicon boride 8% and coating aid 3%.
Wherein, coating aid is mixed by carbowax and tributyl phosphate, and the weight blending ratio is 2: 1.6.
Synthetic borosilicate glass powder is synthetic through 1150 ± 10 ℃ of fusions of high temperature by weight 1: 13 by boron oxide and silicon dioxide.
Beta-eucryptite is synthetic through 1280 ± 10 ℃ of high temperature according to mol ratio 1: 1: 5 by lithium carbonate, aluminium oxide and silicon dioxide.
Other process is with embodiment 1, molding pressure 0.08MPa, and 1350 ℃ of firing temperatures, 1200 ℃ of coating firing temperatures are prepared thermal insulation tile, and sampling records performance figure according to GB and is: 1200 ℃ of heatproofs, do not have distortion and shrink density 0.40g/cm in 2 hours
3' coefficient of thermal conductivity 0.051w/mk, normal direction radiation coefficient 0.05, compressive strength 3.4MPa, thickness direction tensile strength 0.94MPa.
Embodiment 5
Quartz fiber composite heat-insulated material of the present invention, ingredients by weight consists of:
Fused silica glass fiber 91.5% and alumina fibre 8.5%
Wherein the fused silica glass fibre diameter is 1~10 μ m, SiO
2Weight content 〉=95%;
The alumina fibre diameter is 3~20 μ m, Al
2O
3Weight content 80%;
At first utilize the shears weak point to cut fused silica glass fiber and alumina fibre to 1-3cm;
With fused silica glass fiber and alumina fibre difference or mixing and ball milling pulverizing, 300 mesh sieves filter, and add deionized water medium and carry out dispersed with stirring, pour the suction filtration forming mould into and carry out moulding, burn till after the oven dry and make the matrix blank.
Coating compounding weight consists of: synthetic borosilicate glass powder 78%, beta-eucryptite 12%, four silicon boride 3%, cobalt black 6% and coating aid 1%.
Wherein, coating aid is mixed by carbowax and tributyl phosphate, and the weight blending ratio is 2: 1.
Synthetic borosilicate glass powder is synthetic through 1150 ± 10 ℃ of fusions of high temperature by weight 1: 13 by boron oxide and silicon dioxide.
Beta-eucryptite is synthetic through 1280 ± 10 ℃ of high temperature according to mol ratio 1: 1: 5 by lithium carbonate, aluminium oxide and silicon dioxide.
Other process is with embodiment 1, molding pressure 0.08MPa, and 1250 ℃ of firing temperatures, 1100 ℃ of coating firing temperatures are prepared thermal insulation tile, and sampling records performance figure according to GB and is: 1200 ℃ of heatproofs, do not have distortion and shrink density 0.22g/cm in 2 hours
3' coefficient of thermal conductivity 0.046w/mk, normal direction radiation coefficient 0.87, compressive strength 2.0MPa, thickness direction tensile strength 0.59MPa.
Embodiment 6
Quartz fiber composite heat-insulated material of the present invention, ingredients by weight consists of:
Fused silica glass fiber 50%, alumina fibre 46% and boron nitride 4%;
Wherein the fused silica glass fibre diameter is 1~10 μ m, SiO
2Weight content 〉=95%;
The alumina fibre diameter is 3~20 μ m, Al
2O
3Weight content 〉=80%;
At first utilize the shears weak point to cut fused silica glass fiber and alumina fibre to 1-3cm;
With fused silica glass fiber and alumina fibre difference or mixing and ball milling pulverizing, 300 mesh sieves filter, and add boron nitride and deionized water medium and carry out dispersed with stirring, pour the suction filtration forming mould into and carry out moulding, burn till after the oven dry and make the matrix blank.
Coating compounding weight consists of: synthetic borosilicate glass powder 66%, beta-eucryptite 24%, fused quartz powder 7% and coating aid 3%.
Wherein, coating aid is mixed by carbowax and tributyl phosphate, and the weight blending ratio is 2: 1.6.
Synthetic borosilicate glass powder is synthetic through 1100 ± 20 ℃ of fusions of high temperature by weight 1: 10 by boron oxide and silicon dioxide.
Beta-eucryptite is synthetic through 1350 ± 15 ℃ of high temperature according to mol ratio 1: 1: 3.5 by lithium carbonate, aluminium oxide and silicon dioxide.
Other process is with embodiment 1, molding pressure 0.08MPa, and 1350 ℃ of firing temperatures, 1200 ℃ of coating firing temperatures are prepared thermal insulation tile, and sampling records performance figure according to GB and is: 1200 ℃ of heatproofs, do not have distortion and shrink density 0.40g/cm in 2 hours
3' coefficient of thermal conductivity 0.051w/mk, normal direction radiation coefficient 0.05, compressive strength 3.4MPa, thickness direction tensile strength 0.94MPa.
Claims (10)
1. the preparation method of a heat insulation tile of shuttle, it is characterized in that comprising matrix batching, moulding, burn till and implement coating, the matrix ingredients by weight consists of: fused silica glass fiber 50~95%, alumina fibre 5~50%, boron nitride 0~5% and matrix auxiliary agent 0~3%.
2. the preparation method of heat insulation tile of shuttle according to claim 1 is characterized in that the matrix auxiliary agent is silicasol and methylcellulose according to weight ratio 1: the compound of (0.5~1.5).
3. the preparation method of heat insulation tile of shuttle according to claim 1 is characterized in that the fused silica glass fibre diameter is 1~10 μ m, SiO
2Weight content 〉=95%.
4. the preparation method of heat insulation tile of shuttle according to claim 1 is characterized in that the alumina fibre diameter is 3~20 μ m, Al
2O
3Weight content 〉=80%.
5. according to the preparation method of claim 1,2,3 or 4 described heat insulation tile of shuttle, it is characterized in that fused silica glass fiber and alumina fibre ball mill grinding, add boron nitride and auxiliary agent dispersed with stirring again, make the matrix blank through under 1100~1400 ℃ high temperature, burning till after the suction filtration moulding.
6. the preparation method of heat insulation tile of shuttle according to claim 5, it is characterized in that coating compounding weight consists of: synthetic borosilicate glass powder 50~80%, beta-eucryptite 5~30%, silica flour 0~5%, four silicon borides 0~20%, black pigment 0~10% and coating aid 1~3%, wherein, coating aid is mixed by carbowax and tributyl phosphate, and the weight blending ratio is 2: (0.5~2).
7. the preparation method of heat insulation tile of shuttle according to claim 6, it is characterized in that synthetic borosilicate glass powder be by boron oxide and silicon dioxide by weight 1: (2~20) are synthetic through 1000~1200 ℃ of fusions of high temperature.
8. the preparation method of heat insulation tile of shuttle according to claim 7, it is characterized in that eucryptite be by lithium carbonate, aluminium oxide and silicon dioxide according to mol ratio 1: 1: (2~5) are synthetic through 1100~1400 ℃ of high temperature.
9. the preparation method of heat insulation tile of shuttle according to claim 8 is characterized in that black pigment is a cobalt black pigment.
10. the preparation method of heat insulation tile of shuttle according to claim 9 is characterized in that black pigment is not have the mineral black of boring.
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CN102093066A (en) * | 2010-12-24 | 2011-06-15 | 中国人民解放军国防科学技术大学 | High temperature resistant broadband wave-transparent ceramic matrix composite and preparation method thereof |
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CN107737567A (en) * | 2016-07-26 | 2018-02-27 | 乔治·克劳德方法的研究开发空气股份有限公司 | Mould heat guard |
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CN108127382A (en) * | 2017-12-05 | 2018-06-08 | 北京星航机电装备有限公司 | A kind of assembly method of cover-plate type TPS structures |
CN111114750A (en) * | 2019-12-20 | 2020-05-08 | 山东工业陶瓷研究设计院有限公司 | Thermal protection device and reentry vehicle |
CN111925225A (en) * | 2020-07-21 | 2020-11-13 | 山东工业陶瓷研究设计院有限公司 | Light high-temperature low-heat-conduction crucible and preparation method thereof |
CN114524081A (en) * | 2020-11-23 | 2022-05-24 | 通用电气公司 | Aerospace vehicle with thermal radiation coating and associated methods |
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