CN110256103A - One method of porous alumina ceramics base phase becomes heat-insulation composite material - Google Patents

One method of porous alumina ceramics base phase becomes heat-insulation composite material Download PDF

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CN110256103A
CN110256103A CN201910650757.8A CN201910650757A CN110256103A CN 110256103 A CN110256103 A CN 110256103A CN 201910650757 A CN201910650757 A CN 201910650757A CN 110256103 A CN110256103 A CN 110256103A
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parts
composite material
alumina
insulation composite
heat
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覃向阳
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C—CHEMISTRY; METALLURGY
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    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
    • C04B38/063—Preparing or treating the raw materials individually or as batches
    • C04B38/0635—Compounding ingredients
    • C04B38/0645—Burnable, meltable, sublimable materials
    • C04B38/067—Macromolecular compounds
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    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/08—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding porous substances
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3817—Carbides
    • C04B2235/3826—Silicon carbides
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient

Abstract

The present invention relates to phase transformation heat-insulation composite material technical fields, and disclose a method of porous alumina ceramics base phase and become heat-insulation composite material, the raw material including following parts by weight proportion: 40~60 parts of micron order alumina ceramic grain, 10~30 parts of micron order silicon carbide ceramics particle, 30~50 parts of micron silicon diatomaceous earth, 6~15 parts of micron silicon colloidal sol, 10~20 parts of polyethylene glycol hole sealing agent, 100 parts of n-hexane solvent, 200 parts of stearic acid；Material is made for high latent heat phase-change material, based on the alumina porous ceramic of the high porosity of preparation by stearic acid, alumina porous ceramic base phase is prepared using melting method of impregnation and becomes heat-insulation composite material.The present invention solves in current existing thermal protection system, in the case where integrally-built volume and weight changes less, the technical issues of system heat-insulating capability can not be effectively improved.

Description

One method of porous alumina ceramics base phase becomes heat-insulation composite material
Technical field
The present invention relates to phase transformation heat-insulation composite material technical field, a specially method of porous alumina ceramics base phase becomes heat-insulated Composite material.
Background technique
As increasingly maturation, the flying speed of aircraft of hypersonic aircraft engine technology may reach five times Velocity of sound is more, and the flight time will also be increased to a hour rank, and serious Aerodynamic Heating can make aircraft external skin temperatures fast Speed increases, and temperature ramp-up rate is substantially square directly proportional to speed, such as in sea level altitude, when guided missile is with 8~12 When the speed flight of Mach, aircraft surface temperature will be up to 2400 DEG C, and it is very high in the generation of aircraft outer wall to start heating Heating rate (540~820 DEG C/s), this requires the thermal protection systems of aircraft to have fabulous anti-heat-proof quality, to ensure Its internal temperature will not be excessively high, provides a suitable temperature environment for internal device and load.
The heat-insulating capability for improving thermal protection system at present realizes such as have more mainly by the material structure of comprehensive lower thermal conductivity The Fibrous insulation of lower thermal conductivity, the reflectance coating of high reflectance and main passive heat absorption technology etc..Intrinsically, heat is anti- The effect of protecting system is exactly to pass through to select suitable material system and structure, and system is made to have lesser pyroconductivity or heat logical Rate is crossed, to realize the ability of control system temperature, method is mostly low comprehensive thermal conductivity, energy reflection, energy heat absorption etc..
However phase-change material from a kind of phase into another phase transition process along with a large amount of thermal change, and During phase transformation, material own temperature hardly happens variation, simultaneously because non-chemical variation, has reusable Property, therefore be introduced into insulation system, there is important push away to the breakthrough of the following novel high speed aircraft thermal protection key technology Movement is used.The effect that phase-change material plays in thermal protection system can illustrate that phase-change material can with simplified Equivalent heat path To regard a thermal resistance R as0It connects with hot melt C, before it is not up to phase transition temperature and after undergoing phase transition, just corresponds to a heat Hinder R0Heat transfer, when temperature is raised near phase transition temperature, phase-change material is equivalent to thermal capacitance C heat absorption, and the size of thermal capacitance depends on phase Become the quality and latent heat size of material, so preventing it is, in principle, that existing heat can will be introduced with the phase-change material of high latent heat In watch box system, in the case where integrally-built volume and weight changes less, the heat-insulating capability of system can be substantially improved, is prolonged The long aircraft high-speed flight time or make its at the same time in higher speed can be used fly.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a method of porous alumina ceramics base phases to become heat-insulation composite material, It solves in current existing thermal protection system, it, can not be effective in the case where integrally-built volume and weight changes less The technical issues of improvement system heat-insulating capability.
(2) technical solution
To achieve the above object, the invention provides the following technical scheme:
One method of porous alumina ceramics base phase becomes heat-insulation composite material, the raw material including following parts by weight proportion: 40~ 60 parts of micron order alumina ceramic grain, 10~30 parts of micron order silicon carbide ceramics particle, 30~50 parts of micron silicon Diatomaceous earth, 6~15 parts of micron silicon colloidal sol, 10~20 parts of polyethylene glycol hole sealing agent, 100 parts of n-hexane solvent, 200 parts Stearic acid；
Material is made for high latent heat phase-change material, based on the alumina porous ceramic of the high porosity of preparation by stearic acid Material is prepared alumina porous ceramic base phase using melting method of impregnation and becomes heat-insulation composite material.
Preferably, average grain diameter≤10um of the alumina ceramic grain.
Preferably, average grain diameter≤10um of the silicon carbide ceramics particle.
Preferably, average grain diameter≤48um of the diatomite.
(3) beneficial technical effect
Compared with prior art, the present invention has following beneficial technical effect:
The present invention is by stearic acid for high latent heat phase-change material, based on the alumina porous ceramic of the high porosity of preparation Material is made, alumina porous ceramic base phase is prepared using melting method of impregnation and becomes heat-insulation composite material, and the aluminium oxide is more The infiltration rate of hole ceramic base phase transformation heat-insulation composite material is 51.2~52.4%, volume infiltration rate is 65.6~67.2%, phase transformation Temperature is 42.5~42.8 DEG C, and the thermal coefficient at 1000 DEG C is 0.068~0.073W/mK；
To solve in current existing thermal protection system, change little situation in integrally-built volume and weight Under, the technical issues of system heat-insulating capability can not be effectively improved.
Specific embodiment
Stearic acid (CH3(CH2)16COOH), pure, Tianjin Heng Xing chemical reagent manufacturing company is analyzed；
Embodiment one:
(1) preparation of alumina porous ceramic
A. 40g average grain diameter≤10um alumina ceramic grain, 10g average grain diameter≤10um silicon carbide ceramics are weighed Particle, 30g average grain diameter≤48um diatomite, 6g silica solution, it is spare；The wherein quality of the silica in silica solution point Number is 25%；
B. the polyethylene glycol hole sealing agent of 10g is dissolved in the n-hexane solvent of 100g, obtains pretreatment fluid；First to step (a) diatomite in is vacuumized, until being added in above-mentioned pretreatment fluid and being pre-processed after vacuum degree is 5~10Pa 1h is then passed through filtering and drying, obtains pretreated diatomite；
C. by alumina ceramic grain, the silicon carbide ceramics particle ball milling 3h together with 20g dehydrated alcohol in step (a), Obtain the aluminium oxide ceramics slurry of doped silicon carbide；
D. by the silica solution in step (a), the diatomite in step (b), the aluminium oxide ceramics slurry in step (c) and nothing Water-ethanol together, under the rate of revolving speed 180rpm, ball milling 3h, later, by drying, hydrostatic profile processing after, in temperature Heat preservation sintering 2h at 1450 DEG C, is prepared the alumina porous ceramic of doped silicon carbide；
(2) by 200g stearic acid (CH3(CH2)16COOH it) is placed in alumina crucible, is put into baking oven, at 80 DEG C of temperature Lower thawing；
Later, the alumina porous ceramic of the doped silicon carbide in step (1) is immersed in stearic acid melt, in temperature 1h is kept the temperature at 80 DEG C, later takes out alumina porous ceramic out of stearic acid melt, is removed the adherency melt on surface, is cooled to Room temperature is prepared alumina porous ceramic base phase and becomes heat-insulation composite material；
(3) become heat-insulation composite material to the alumina porous ceramic base phase prepared in step (2) to be tested for the property, soak Infiltration rate is 51.2%, volume infiltration rate is 65.6%, phase transition temperature is 42.5 DEG C, and the thermal coefficient at 1000 DEG C is 0.073W/m·K。
Embodiment two:
(1) preparation of alumina porous ceramic
A. 60g average grain diameter≤10um alumina ceramic grain, 30g average grain diameter≤10um silicon carbide ceramics are weighed Particle, 50g average grain diameter≤48um diatomite, 15g silica solution, it is spare；The wherein quality of the silica in silica solution Score is 30%；
B. the polyethylene glycol hole sealing agent of 20g is dissolved in the n-hexane solvent of 100g, obtains pretreatment fluid；First to step (a) diatomite in is vacuumized, until be added in above-mentioned pretreatment fluid after vacuum degree is 10Pa and carry out pretreatment 1h, It is then passed through filtering and drying, obtains pretreated diatomite；
C. by alumina ceramic grain, the silicon carbide ceramics particle ball milling 5h together with 20g dehydrated alcohol in step (a), Obtain the aluminium oxide ceramics slurry of doped silicon carbide；
D. by the silica solution in step (a), the diatomite in step (b), the aluminium oxide ceramics slurry in step (c) and nothing Water-ethanol together, under the rate of revolving speed 300rpm, ball milling 3h, later, by drying, hydrostatic profile processing after, in temperature Heat preservation sintering 5h at 1600 DEG C, is prepared the alumina porous ceramic of doped silicon carbide；
(2) by 200g stearic acid (CH3(CH2)16COOH it) is placed in alumina crucible, is put into baking oven, at 100 DEG C of temperature Lower thawing；
Later, the alumina porous ceramic of the doped silicon carbide in step (1) is immersed in stearic acid melt, in temperature 1h is kept the temperature at 100 DEG C, later takes out alumina porous ceramic out of stearic acid melt, removes the adherency melt on surface, it is cooling To room temperature, alumina porous ceramic base phase is prepared and becomes heat-insulation composite material；
(3) become heat-insulation composite material to the alumina porous ceramic base phase prepared in step (2) to be tested for the property, soak Infiltration rate is 52.4%, volume infiltration rate is 67.2%, phase transition temperature is 42.8 DEG C, and the thermal coefficient at 1000 DEG C is 0.071W/m·K。
Embodiment three:
(1) preparation of alumina porous ceramic
A. 50g average grain diameter≤10um alumina ceramic grain, 20g average grain diameter≤10um silicon carbide ceramics are weighed Particle, 40g average grain diameter≤48um diatomite, 12g silica solution, it is spare；The wherein quality of the silica in silica solution Score is 30%；
B. the polyethylene glycol hole sealing agent of 15g is dissolved in the n-hexane solvent of 100g, obtains pretreatment fluid；First to step (a) diatomite in is vacuumized, until being added in above-mentioned pretreatment fluid after vacuum degree is 7Pa and carrying out pretreatment 1h, connect By filtering and dry, obtain pretreated diatomite；
C. by alumina ceramic grain, the silicon carbide ceramics particle ball milling 4h together with 20g dehydrated alcohol in step (a), Obtain the aluminium oxide ceramics slurry of doped silicon carbide；
D. by the silica solution in step (a), the diatomite in step (b), the aluminium oxide ceramics slurry in step (c) and nothing Water-ethanol together, under the rate of revolving speed 200rpm, ball milling 3h, later, by drying, hydrostatic profile processing after, in temperature Heat preservation sintering 4h at 1500 DEG C, is prepared the alumina porous ceramic of doped silicon carbide；
(2) by 200g stearic acid (CH3(CH2)16COOH it) is placed in alumina crucible, is put into baking oven, at 90 DEG C of temperature Lower thawing；
Later, the alumina porous ceramic of the doped silicon carbide in step (1) is immersed in stearic acid melt, in temperature 1h is kept the temperature at 90 DEG C, later takes out alumina porous ceramic out of stearic acid melt, is removed the adherency melt on surface, is cooled to Room temperature is prepared alumina porous ceramic base phase and becomes heat-insulation composite material；
(3) become heat-insulation composite material to the alumina porous ceramic base phase prepared in step (2) to be tested for the property, soak Infiltration rate is 52.4%, volume infiltration rate is 67.1%, phase transition temperature is 42.7 DEG C, and the thermal coefficient at 1000 DEG C is 0.073W/m·K。

Claims (4)

1. a method of porous alumina ceramics base phase becomes heat-insulation composite material, which is characterized in that including following parts by weight proportion Raw material: 40~60 parts of micron order alumina ceramic grain, 10~30 parts of micron order silicon carbide ceramics particle, 30~50 parts Micron silicon diatomaceous earth, 6~15 parts of micron silicon colloidal sol, 10~20 parts of polyethylene glycol hole sealing agent, 100 parts of n-hexane are molten Agent, 200 parts of stearic acid；
Material is made for high latent heat phase-change material, based on the alumina porous ceramic of the high porosity of preparation by stearic acid, Alumina porous ceramic base phase is prepared using melting method of impregnation and becomes heat-insulation composite material.
2. alumina porous ceramic base phase according to claim 1 becomes heat-insulation composite material, which is characterized in that the oxidation Average grain diameter≤10um of aluminium ceramic particle.
3. alumina porous ceramic base phase according to claim 1 becomes heat-insulation composite material, which is characterized in that the carbonization Average grain diameter≤10um of silicon ceramic particle.
4. alumina porous ceramic base phase according to claim 1 becomes heat-insulation composite material, which is characterized in that the diatom Average grain diameter≤48um of soil.
CN201910650757.8A 2019-07-18 2019-07-18 One method of porous alumina ceramics base phase becomes heat-insulation composite material Pending CN110256103A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114058338A (en) * 2021-11-19 2022-02-18 航天特种材料及工艺技术研究所 Flexible high-temperature phase-change heat-insulation composite material and preparation method thereof

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CN105837252A (en) * 2015-07-06 2016-08-10 深圳市商德先进陶瓷有限公司 Porous alumina ceramic and preparation method thereof
CN107011868A (en) * 2017-03-08 2017-08-04 北京交通大学 A kind of paraffin/iron tailings Ceramic Composite phase-changing energy storage material and its melting impregnation preparation method
CN108531141A (en) * 2018-06-11 2018-09-14 哈尔滨工业大学 A kind of organic matter fills the preparation method of the composite phase-change energy storage material of orderly porous aluminum oxide template
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CN107011868A (en) * 2017-03-08 2017-08-04 北京交通大学 A kind of paraffin/iron tailings Ceramic Composite phase-changing energy storage material and its melting impregnation preparation method
CN108531141A (en) * 2018-06-11 2018-09-14 哈尔滨工业大学 A kind of organic matter fills the preparation method of the composite phase-change energy storage material of orderly porous aluminum oxide template
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114058338A (en) * 2021-11-19 2022-02-18 航天特种材料及工艺技术研究所 Flexible high-temperature phase-change heat-insulation composite material and preparation method thereof
CN114058338B (en) * 2021-11-19 2023-04-25 航天特种材料及工艺技术研究所 Flexible high-temperature phase-change heat-insulation composite material and preparation method thereof

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