CN110372346A - A kind of high temperature resistant, lightweight, efficient NEW TYPE OF COMPOSITE heat-barrier material - Google Patents

A kind of high temperature resistant, lightweight, efficient NEW TYPE OF COMPOSITE heat-barrier material Download PDF

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CN110372346A
CN110372346A CN201910651471.1A CN201910651471A CN110372346A CN 110372346 A CN110372346 A CN 110372346A CN 201910651471 A CN201910651471 A CN 201910651471A CN 110372346 A CN110372346 A CN 110372346A
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barrier material
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马桂明
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    • C04B2235/3852Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
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Abstract

The present invention relates to heat-barrier material technical fields, and a kind of high temperature resistant, lightweight, efficient NEW TYPE OF COMPOSITE heat-barrier material are disclosed, the raw material including following parts by weight proportion: 20~30 parts of micron-sized titanium nitride ceramic particles (TiN), 20~30 parts of micron-sized titanium diboride ceramic particle (TiB2), 30~50 parts of micron-sized diatomite, 6~15 parts of silica solution, 10~20 parts of polyethylene glycol hole sealing agent, 100 parts of n-hexane solvent, 200 parts of mannitol (CH2(OH)(CHOH)4CH2OH);Material is made for high latent heat phase-change material, based on the titanium nitride of the high porosity of preparation-titanium diboride porous ceramics by mannitol, NEW TYPE OF COMPOSITE heat-barrier material is prepared using melting method of impregnation.The present invention solves used various glass fibres and fibrous ceramic insulation, and with the raising for using temperature, heat-proof quality decline is very fast, is not able to satisfy the technical issues of certain aerospace crafts and guided missile thermal protection system are to heat-barrier material effectively insulating requirement.

Description

A kind of high temperature resistant, lightweight, efficient NEW TYPE OF COMPOSITE heat-barrier material
Technical field
The present invention relates to heat-barrier material technical field, specially a kind of high temperature resistant, lightweight, the heat-insulated material of efficient NEW TYPE OF COMPOSITE Material.
Background technique
With the development of aerospace craft and guided missile, to prevent long-time high-speed aircraft Aerodynamic Heating to aircraft interior The cause thermal damage of structure and instrument, requirement of the thermal protection system to heat-barrier material are higher.Used heat-barrier material is mainly various Glass fibre and ceramic fibre, with the raising for using temperature, heat-proof quality decline is very fast, is not able to satisfy certain aerospace crafts Requirement with guided missile thermal protection system to heat-barrier material effectively insulating.Therefore, developing has high temperature resistant, lightweight, efficient heat-insulated Material is an urgent demand of novel aerospace craft and guided missile thermal protection system.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of high temperature resistant, lightweight, the heat-insulated materials of efficient NEW TYPE OF COMPOSITE Material, solves used various glass fibres and fibrous ceramic insulation, with the raising for using temperature, heat-proof quality decline Comparatively fast, it is not able to satisfy the technical issues of certain aerospace crafts and guided missile thermal protection system are to heat-barrier material effectively insulating requirement.
(2) technical solution
To achieve the above object, the invention provides the following technical scheme:
A kind of high temperature resistant, lightweight, efficient NEW TYPE OF COMPOSITE heat-barrier material, the raw material including following parts by weight proportion: 20 ~30 parts of micron-sized titanium nitride ceramic particles (TiN), 20~30 parts of micron-sized titanium diboride ceramic particle (TiB2), 30~ 50 parts of micron-sized diatomite, 6~15 parts of silica solution, 10~20 parts of polyethylene glycol hole sealing agent, 100 parts of n-hexane are molten Agent, 200 parts of mannitol;
It is high latent heat phase-change material with mannitol, with the titanium nitride of the high porosity of preparation-titanium diboride porous ceramics is Material is made in basis, and NEW TYPE OF COMPOSITE heat-barrier material is prepared using melting method of impregnation.
Preferably, the average grain diameter of average grain diameter≤10um of the titanium nitride ceramic particle, titanium diboride ceramic particle ≤10um。
Preferably, the mass fraction of the silica in the silica solution is 25~30%.
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 with mannitol for high latent heat phase-change material, porous with titanium nitride-titanium diboride of the high porosity of preparation Material is made based on ceramics, NEW TYPE OF COMPOSITE heat-barrier material, and the heat-insulated material of the NEW TYPE OF COMPOSITE are prepared using melting method of impregnation The density of material is 0.91~0.95g/cm3, infiltration rate be 55.6~56.8%, volume infiltration rate is 63.3~65.6%, phase transformation Temperature is 43.2~44.1 DEG C, and the thermal coefficient at 1000 DEG C is 0.061~0.067W/mK;
To solving used various glass fibres and fibrous ceramic insulation, with the raising for using temperature, every Hot property decline is very fast, is not able to satisfy certain aerospace crafts and guided missile thermal protection system to heat-barrier material effectively insulating requirement Technical problem.
Specific embodiment
Mannitol (CH2(OH)(CHOH)4CH2OH), density 1.521g/cm3, analyze pure, the triumphant logical chemical reagent in Tianjin Co., Ltd;
(1) titanium nitride-titanium diboride porous ceramics preparation
A. 20g average grain diameter≤10um titanium nitride ceramic particle (TiN), two boron of 20g average grain diameter≤10um are weighed Change titanium ceramic particle (TiB2), 30g average grain diameter≤48um diatomite, 6g silica solution, it is spare;Wherein two in silica solution The mass fraction of silica 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 after vacuum degree is 5Pa and carrying out pretreatment 1h, connect By filtering and dry, obtain pretreated diatomite;
C. by titanium nitride ceramic particle, the titanium diboride ceramic particle ball milling together with 20g dehydrated alcohol in step (a) 3h obtains titanium nitride-titanium diboride slurry;
D. the titanium nitride in the silica solution in step (a), the diatomite in step (b), step (c)-titanium diboride is starched Material is together with dehydrated alcohol, under the rate of revolving speed 180rpm, ball milling 3h, later, after drying, hydrostatic profile processing, Titanium nitride-titanium diboride porous ceramics is prepared in heat preservation sintering 2h at 1450 DEG C of temperature;
Using Archimedes principle, it is more that titanium nitride-titanium diboride is measured using electronic balance adapted density measure component The bulk density of hole ceramics is 0.83g/cm3, the porosity of calculating is 71.3%;
(2) by 200g mannitol (CH2(OH)(CHOH)4CH2OH it) is placed in alumina crucible, is put into baking oven, in temperature Melt at 200 DEG C;
Later, the titanium nitride in step (1)-titanium diboride porous ceramics is immersed in mannitol melt, in temperature 200 1h is kept the temperature at DEG C, later takes out alumina porous ceramic out of mannitol melt, is removed the adherency melt on surface, is cooled to room NEW TYPE OF COMPOSITE heat-barrier material is prepared in temperature;
(3) the NEW TYPE OF COMPOSITE heat-barrier material prepared in step (2) is tested for the property, density 0.95g/cm3, leaching Infiltration rate is 55.6%, volume infiltration rate is 63.3%, phase transition temperature is 43.2 DEG C, and the thermal coefficient at 1000 DEG C is 0.067W/m·K。
Embodiment two:
(1) titanium nitride-titanium diboride porous ceramics preparation
A. 30g average grain diameter≤10um titanium nitride ceramic particle (TiN), two boron of 30g average grain diameter≤10um are weighed Change titanium ceramic particle (TiB2), 50g average grain diameter≤48um diatomite, 15g silica solution, it is spare;Wherein in silica solution The mass fraction of silica is 25~30%;
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 titanium nitride ceramic particle, the titanium diboride ceramic particle ball milling together with 20g dehydrated alcohol in step (a) 5h obtains titanium nitride-titanium diboride slurry;
D. the titanium nitride in the silica solution in step (a), the diatomite in step (b), step (c)-titanium diboride is starched Material is together with dehydrated alcohol, under the rate of revolving speed 300rpm, ball milling 3h, later, after drying, hydrostatic profile processing, Titanium nitride-titanium diboride porous ceramics is prepared in heat preservation sintering 5h at 1600 DEG C of temperature;
Using Archimedes principle, it is more that titanium nitride-titanium diboride is measured using electronic balance adapted density measure component The bulk density of hole ceramics is 0.88g/cm3, the porosity of calculating is 71.1%;
(2) by 200g mannitol (CH2(OH)(CHOH)4CH2OH it) is placed in alumina crucible, is put into baking oven, in temperature Melt at 220 DEG C;
Later, the titanium nitride in step (1)-titanium diboride porous ceramics is immersed in mannitol melt, in temperature 220 1h is kept the temperature at DEG C, later takes out alumina porous ceramic out of mannitol melt, is removed the adherency melt on surface, is cooled to room NEW TYPE OF COMPOSITE heat-barrier material is prepared in temperature;
(3) the NEW TYPE OF COMPOSITE heat-barrier material prepared in step (2) is tested for the property, density 0.94g/cm3, leaching Infiltration rate is 56.8%, volume infiltration rate is 65.6%, phase transition temperature is 44.1 DEG C, and the thermal coefficient at 1000 DEG C is 0.065W/m·K。
Embodiment three:
(1) titanium nitride-titanium diboride porous ceramics preparation
A. 25g average grain diameter≤10um titanium nitride ceramic particle (TiN), two boron of 25g average grain diameter≤10um are weighed Change titanium ceramic particle (TiB2), 40g average grain diameter≤48um diatomite, 12g silica solution, it is spare;Wherein in silica solution The mass fraction of silica is 25~30%;
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 titanium nitride ceramic particle, the titanium diboride ceramic particle ball milling together with 20g dehydrated alcohol in step (a) 4h obtains titanium nitride-titanium diboride slurry;
D. the titanium nitride in the silica solution in step (a), the diatomite in step (b), step (c)-titanium diboride is starched Material is together with dehydrated alcohol, under the rate of revolving speed 240rpm, ball milling 3h, later, after drying, hydrostatic profile processing, Titanium nitride-titanium diboride porous ceramics is prepared in heat preservation sintering 4h at 1500 DEG C of temperature;
Using Archimedes principle, it is more that titanium nitride-titanium diboride is measured using electronic balance adapted density measure component The bulk density of hole ceramics is 0.85g/cm3, the porosity of calculating is 71.8%;
(2) by 200g mannitol (CH2(OH)(CHOH)4CH2OH it) is placed in alumina crucible, is put into baking oven, in temperature Melt at 210 DEG C;
Later, the titanium nitride in step (1)-titanium diboride porous ceramics is immersed in mannitol melt, in temperature 210 1h is kept the temperature at DEG C, later takes out alumina porous ceramic out of mannitol melt, is removed the adherency melt on surface, is cooled to room NEW TYPE OF COMPOSITE heat-barrier material is prepared in temperature;
(3) the NEW TYPE OF COMPOSITE heat-barrier material prepared in step (2) is tested for the property, density 0.91g/cm3, leaching Infiltration rate is 55.8%, volume infiltration rate is 64.5%, phase transition temperature is 43.7 DEG C, and the thermal coefficient at 1000 DEG C is 0.061W/m·K。

Claims (4)

1. a kind of high temperature resistant, lightweight, efficient NEW TYPE OF COMPOSITE heat-barrier material, which is characterized in that matched including following parts by weight Raw material: 20~30 parts of micron-sized titanium nitride ceramic particles (TiN), 20~30 parts of micron-sized titanium diboride ceramic particles (TiB2), 30~50 parts of micron-sized diatomite, 6~15 parts of silica solution, 10~20 parts of polyethylene glycol hole sealing agent, 100 parts N-hexane solvent, 200 parts of mannitol (CH2(OH)(CHOH)4CH2OH);
It is high latent heat phase-change material, based on the titanium nitride of the high porosity of preparation-titanium diboride porous ceramics by mannitol Material is made, NEW TYPE OF COMPOSITE heat-barrier material is prepared using melting method of impregnation.
2. NEW TYPE OF COMPOSITE heat-barrier material according to claim 1, which is characterized in that the titanium nitride ceramic particle is averaged Average grain diameter≤10um of partial size≤10um, titanium diboride ceramic particle.
3. NEW TYPE OF COMPOSITE heat-barrier material according to claim 1, which is characterized in that silica in the silica solution Mass fraction is 25~30%.
4. NEW TYPE OF COMPOSITE heat-barrier material according to claim 1, which is characterized in that the average grain diameter of the diatomite≤ 48um。
CN201910651471.1A 2019-07-18 2019-07-18 A kind of high temperature resistant, lightweight, efficient NEW TYPE OF COMPOSITE heat-barrier material Withdrawn CN110372346A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102212729A (en) * 2011-04-17 2011-10-12 山东科技大学 TiB2-TiC-TiN-NiAl porous composite material with combined hole pattern and preparation method thereof
CN106675304A (en) * 2016-12-28 2017-05-17 中南林业科技大学 Decalescence intumescent flame-retardant fireproof waterborne coating and preparation method thereof
CN106738149A (en) * 2016-12-28 2017-05-31 中南林业科技大学 The manufacture method and its expandable flame retardant timber of a kind of expandable flame retardant timber of decalescence
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102212729A (en) * 2011-04-17 2011-10-12 山东科技大学 TiB2-TiC-TiN-NiAl porous composite material with combined hole pattern and preparation method thereof
CN106675304A (en) * 2016-12-28 2017-05-17 中南林业科技大学 Decalescence intumescent flame-retardant fireproof waterborne coating and preparation method thereof
CN106738149A (en) * 2016-12-28 2017-05-31 中南林业科技大学 The manufacture method and its expandable flame retardant timber of a kind of expandable flame retardant timber of decalescence
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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Application publication date: 20191025