CN105294143B - Gradient distribution heat insulation material and preparation method thereof - Google Patents
Gradient distribution heat insulation material and preparation method thereof Download PDFInfo
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- CN105294143B CN105294143B CN201510732422.2A CN201510732422A CN105294143B CN 105294143 B CN105294143 B CN 105294143B CN 201510732422 A CN201510732422 A CN 201510732422A CN 105294143 B CN105294143 B CN 105294143B
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Abstract
The invention discloses a kind of gradient distribution heat insulation material, including the face coat being made by the enhanced porous ceramic matrix of Amorphous GaN O, silicon boron glass intermediate layer and by oxidation-resistant material.Its preparation method includes：(1) the enhanced porous ceramic matrix of Amorphous GaN O is prepared；(2) by MoSi2、SiO2With B2O3Powder is mixed, and is obtained mixture, is prepared the suspension of mixture, suspension is sprayed at into matrix surface, quantity for spray is 0.3-1g/cm2；1200-1350 DEG C is warming up to from room temperature with 58 DEG C/min heating rate in air atmosphere, 20-90min is incubated, to prepare the middle product with silicon boron glass intermediate layer；(3) in the surface spraying oxidation-resistant material in silicon boron glass intermediate layer, to form face coat.The heat insulation material density of the present invention is small, and temperature in use is high, can reach more than 2000K, and reusability is high.
Description
Technical field
The present invention relates to spacecraft thermal protection technology, more particularly to a kind of gradient distribution heat insulation material and preparation method thereof.
Background technology
During reentering, spacecraft needs to undergo high enthalpy, the Airflow Environment of high hot-fluid, in the process aircraft master
Bear compression and mechanical shock effect.During reentering, spacecraft maximal rate can reach 25000km/h, now navigate
The temperature in its general ability portion is not less than 1649 DEG C within the 10min times.The length at several centimetres is required for thermal protection system
Interior, the temperature of heat structure drops to 368 DEG C from 1649 DEG C.In order to ensure that the normal work of internal electronic equipment must be to spacecraft
Carry out thermal protection.
Ablating heat shield is thermal protection mode the most frequently used at present.I.e. by the mass loss of heat insulation material heat structure table
The heat that face is produced is taken away.Conventional heat insulation material includes carbon-based heat insulation material and silicon substrate heat insulation material.The anti-hot mode is solved
Return to satellite, the thermal protection problem reentered of spaceship.Using Control System for Reusable Launch Vehicle and re-entry space vehicle as representative
Spacecraft of new generation further provides the requirement such as low-density, reusable to thermal protection.Existing ablating heat shield can not
Corresponding thermal protection demand, is mainly manifested in：
(1) heat insulation material density is high, and launch cost is high.The density of existing carbon-based material is in 1800-2000kg/m3It
Between, more than the thermal protection demand of Control System for Reusable Launch Vehicle and re-entry space vehicle：Heat structure density 300-800kg/m3.High is close
Degree can increase the weight of spacecraft, and then cause launch cost to raise.
(2) greatly, heat structure can not be reused for ablation shape change.Ablating heat shield is damaged by the quality of heat insulation material
Lose what the heat that heat structure surface is produced was taken away.After each, the profile of heat structure can all change, and influence space flight
The aeroperformance of device.Therefore, ablating heat shield does not possess reusability.
The content of the invention
For above-mentioned technical problem, the invention provides a kind of lightweight construction, heat-proof quality is good, reusable ladder
Spend chemoprevention hot material.
Present invention also offers a kind of preparation method of gradient distribution heat insulation material.
The technical scheme is that：
A kind of gradient distribution heat insulation material, including in the middle of the enhanced porous ceramic matrix of Amorphous GaN O, silicon boron glass
Layer and the face coat being made up of oxidation-resistant material.
Preferably, in described gradient distribution heat insulation material, the porous ceramic film material is Al2O3Or ZrO2, averag density
For 0.3-1.0g/cm3。
Preferably, in described gradient distribution heat insulation material, the silicon boron glass intermediate layer is by SiO2、B2O3And MoSi2
Prepare.
Preferably, in described gradient distribution heat insulation material, the thickness in the silicon boron glass intermediate layer is 0.15-0.2mm.
Preferably, in described gradient distribution heat insulation material, the oxidation-resistant material is MoSi2And TaSi2Mixture or
MoSi2Or SiC.
Preferably, in described gradient distribution heat insulation material, the oxidation-resistant material is MoSi2And TaSi2Mixture or
MoSi2When, the thickness of the face coat is 50-100 μm；When the oxidation-resistant material is SiC, the thickness of the face coat
For 100-150 μm.
A kind of preparation method of gradient distribution heat insulation material, including：
(1) the enhanced porous ceramic matrix of Amorphous GaN O is prepared；
(2) by MoSi2、SiO2With B2O3Powder is mixed, and obtains mixture, mixture is sprayed at into matrix surface, quantity for spray is
0.3-1g/cm2, wherein, SiO2And B2O3Mass ratio be 1: 1-1.2, MoSi2Consumption be total weight of the mixture 50-70%；
1200-1350 DEG C is warming up to from room temperature with 5-8 DEG C/min heating rate in air atmosphere, 20-90min is incubated, to prepare
Obtain the middle product with silicon boron glass intermediate layer；
(3) in the surface spraying oxidation-resistant material in silicon boron glass intermediate layer, to form face coat.
Preferably, in the preparation method of described gradient distribution heat insulation material, in step (1), Amorphous GaN O forerunner is prepared
The colloid of body；By porous Al2O3Material is impregnated in certain time in presoma, and certain time is stood in atmosphere, obtains impregnated
Porous Al2O3Material matrix；By impregnated porous Al2O3Material matrix is placed under protective atmosphere and is heated to 1000-1100
DEG C, 1-2h is incubated, the enhanced porous Als of Amorphous GaN O are obtained2O3Material matrix.
Preferably, in the preparation method of described gradient distribution heat insulation material, in step (3), the oxidation-resistant material is
MoSi2And TaSi2Mixture or MoSi2Or SiC.
Preferably, in the preparation method of described gradient distribution heat insulation material, in step (3), the oxidation-resistant material is
MoSi2And TaSi2Mixture or MoSi2When, the thickness of the face coat is 50-100 μm；The oxidation-resistant material is SiC
When, the thickness of the face coat is 100-150 μm.
The advantage of the invention is that：
1st, gradient distribution heat insulation material density of the present invention is small, and temperature in use is high, can reach more than 2000K.
2nd, gradient distribution heat insulation material anti-seismic performance of the present invention is good, and reusability is high.
3rd, in preparation method of the present invention, material technology maturity is high, and preparation technology easily realizes and is engineered journey
Degree is higher.
4th, short preparation period, operation and maintenance cost is low.
Brief description of the drawings
Fig. 1 is the structural representation of gradient distribution heat insulation material of the present invention.
Fig. 2 is gradient distribution heat insulation material and the Contrast on effect analysis chart of prior art.
Fig. 3 (a) is the enhanced porous Als of Amorphous GaN O in embodiment one2O3The infrared spectrogram of matrix, Fig. 3 (b) is implementation
The enhanced porous Als of Amorphous GaN O in example one2O3The total spectrograms of XPS of matrix.
Fig. 4 is small blunt nosed design drawing.
Embodiment
In order to facilitate the understanding of the purposes, features and advantages of the present invention, below in conjunction with the accompanying drawings to the present invention
Embodiment be described in detail.
Referring to Fig. 1, the invention provides a kind of gradient distribution heat insulation material, including by the enhanced porous ceramics of Amorphous GaN O
Material matrix, silicon boron glass intermediate layer and the face coat being made up of oxidation-resistant material.
Please see Figure 2, in order to illustrate the advantage of gradient distribution heat insulation material, using ANSYS softwares to gradient distribution heat insulation material and
The anti-thermal effect of three kinds of traditional solar heat protection+heat insulation schemes is analyzed, and three kinds of existing schemes are respectively C/C+ heat-barrier materials, superelevation
Warm ceramics (UHTC)+heat-barrier material, low-density ceramic+heat-barrier material.Four kinds of materials are processed into small blunt nosed structure (i.e. such as Fig. 4
Shown structure, the structure has cap).The Airflow Environment used is calculated for typical space device reentry environment, corresponding constraint
Condition is：Heat insulation material surface temperature is less than 1700K, and back temperature is less than 350K.The composition of gradient distribution heat insulation material is referring to reality
Apply example one.According to constraint is calculated, Woelm Alumina elects density 450kg/m as3, temperature in use 1900K.Can from Fig. 1
Go out, under identical constraints, C/C+ heat-barrier materials, superhigh temperature ceramics (UHTC)+heat-barrier material, low-density ceramic+heat-insulated material
The gross thickness of material and gradient distribution heat insulation material is respectively 102mm, 67.7mm, 34.3mm and 30.8mm, corresponding density of texture point
Wei not 1653kg/m3、4817kg/m3、768kg/m3And 487kg/m3.I.e. gradient distribution heat insulation material has minimum thickness and most
Low density of texture.I.e. gradient distribution heat insulation material can effectively reduce the weight of thermal protection system, and then reduce the hair of aircraft
Penetrate cost.In addition, from Fig. 2 it can also be seen that in the case of same overall thickness, gradient distribution thermal protection struc ture has highest surface
Heat loss through radiation rate, 821kW/m2.Above analysis shows, relative to traditional solar heat protection+heat insulation schemes, gradient distribution heat insulation material has more
Good anti-thermal effect and relatively low launch cost.Also, relative to cap surface, the temperature at cap side faces and the back side is relatively low, energy
It is enough to realize that structural compatibility is matched with supporter.
The operation principle of gradient distribution heat insulation material is：Under pneumatic thermal environment, material surface produces uniform heating.In heating
During, the stress that silicon boron glass intermediate layer produces temperature change is dispersed, it is to avoid heat insulation material produces hot tearing damage.When
Surface heating reaches after certain temperature that the face coat that oxidation-resistant material is made starts outside radiations heat energy, while preventing pneumatic
Diffusion inside from oxygen in environment to heat insulation material.Silicon boron glass intermediate layer then can effectively reduce heat to inside heat insulation material
Transmission, and pass through MoSi in silicon boron glass2Passive oxidation adsorption and diffusion enter heat insulation material in oxygen.
Further, in described gradient distribution heat insulation material, the porous ceramic film material is Al2O3Or ZrO2, averag density
For 0.3-1.0g/cm3。
Further, in described gradient distribution heat insulation material, the silicon boron glass intermediate layer is by SiO2、B2O3And MoSi2
Prepare.
Further, in described gradient distribution heat insulation material, the thickness in the silicon boron glass intermediate layer is 0.15-0.2mm.
Further, in described gradient distribution heat insulation material, the oxidation-resistant material is MoSi2And TaSi2Mixture or
MoSi2Or SiC.
Further, in described gradient distribution heat insulation material, the oxidation-resistant material is MoSi2And TaSi2Mixture or
MoSi2When, the thickness of the face coat is 50-100 μm；When the oxidation-resistant material is SiC, the thickness of the face coat
For 100-150 μm.
Present invention also offers a kind of preparation method of gradient distribution heat insulation material, including：(1) Amorphous GaN O is prepared enhanced
Porous ceramic matrix；(2) by MoSi2、SiO2With B2O3Powder is mixed, and obtains mixture, mixture is sprayed at into matrix table
Face, quantity for spray is 0.3-1g/cm2, wherein, SiO2And B2O3Mass ratio be 1: 1-1.2, MoSi2Consumption be mixture total weight
The 50-70% of amount；1200-1350 DEG C is warming up to from room temperature with 5-8 DEG C/min heating rate in air atmosphere, 20- is incubated
90min, to prepare the middle product with silicon boron glass intermediate layer；(3) in the surface spraying antioxygen in silicon boron glass intermediate layer
Change material, to form face coat.
Further, in the preparation method of described gradient distribution heat insulation material, in step (1), Amorphous GaN O forerunner is prepared
The colloid of body；By porous Al2O3Material is impregnated in certain time in presoma, and certain time is stood in atmosphere, obtains impregnated
Porous Al2O3Material matrix；By impregnated porous Al2O3Material matrix is placed under protective atmosphere and is heated to 1000-1100
DEG C, 1-2h is incubated, the enhanced porous Als of Amorphous GaN O are obtained2O3Material matrix.Wherein, when preparing presoma, it is preferred to use three
Ethoxy radical siloxane or diethoxy siloxanes.
Further, in the preparation method of described gradient distribution heat insulation material, in step (3), the oxidation-resistant material is
MoSi2And TaSi2Mixture or MoSi2Or SiC.
Further, in the preparation method of described gradient distribution heat insulation material, in step (3), the oxidation-resistant material is
MoSi2And TaSi2Mixture or MoSi2When, the thickness of the face coat is 50-100 μm；The oxidation-resistant material is SiC
When, the thickness of the face coat is 100-150 μm.
Embodiment one
In order to further illustrate the superiority of the present invention, the present invention has carried out Amorphous GaN O enhancing porous Als2O3The system of material
Standby technical study.Density is used for 750kg/m3, temperature in use is that 2200K Woelm Alumina is used as matrix.By vinyl three
Ethoxysilane, absolute ethyl alcohol, distilled water add 1-3at% hydrochloric acid by 1: 3: 1 mixing, with 3-5 points of glass bar stirring
Clock, obtains the organosilicon colloid of homogeneous transparent, i.e. Amorphous GaN O presomas.The presoma is stood into 24h.By size 60mm ×
60mm × 60mm porous Al2O3Taking-up after being impregnated into presoma in 10min, stands 24h in atmosphere, repeated impregnations 3 times,
The porous Al impregnated2O3Matrix.By the pre- modified porous Al in surface2O3Matrix is put into the atmosphere furnace of Ar protections and is heated to
1000 DEG C, 1h is incubated, the enhanced porous Als of Amorphous GaN O are obtained2O3Matrix.Enhanced porous Al2O3Matrix strength improves tool
There is good processability.Fig. 3 (a) and Fig. 3 (b) sets forth the enhanced porous Als of Amorphous GaN O2O3The infrared light of matrix
Spectrogram and XPS score analysis results.
Fig. 4 provides a kind of design drawing of small blunt nosed structure.The preparation process of the small blunt nosed structure is as follows：(1) it will prepare
Obtained Amorphous GaN O enhancing porous Als2O3Matrix is processed into the small blunt configuration of design (see Fig. 4)；(2) it is 200- by granularity
The MoSi of 400 mesh2、SiO2With B2O3Powder in mass ratio 65: 30: 35 adds isometric alcohol ball milling 20-24h after mixing；(3)
Mixed powder is sprayed at porous Al2O3The anti-hot junction of matrix, quantity for spray is 0.3-1g/cm2；(4) sample after spraying is existed
1320 DEG C are heated to from room temperature with 5 DEG C/min heating rate under air atmosphere, 30min is incubated, obtains with silicon boron glass
The middle product of interbed；(5) silicon boron glass intermediate layer 100-150 microns of surface spraying SiC coatings, with formed surface painting
Layer.Measurement shows that the density of heat insulation material is 800kg/m3, less than the density 1800-2000kg/cm of carbon-based heat insulation material3.High temperature
Radiation test shows that the surface emissivity of the gradient distribution heat insulation material is more than 0.9, i.e., in high temperature environments, gradient distribution surface
Its heat can be will act at and be radiated the external space, effectively the anti-thermal pressure of reduction porous matrix.
Embodiment two
VTES, absolute ethyl alcohol, distilled water are added into 1-3at% hydrochloric acid by 1: 3: 1 mixing,
Stirred 3-5 minutes with glass bar, obtain the organosilicon colloid of homogeneous transparent, i.e. Amorphous GaN O presomas.The presoma is stood
24h.By size 60mm × 60mm × 60mm porous Al2O3Taking-up, stands in atmosphere after being impregnated into presoma in 10min
24h, repeated impregnations 3 times, the porous Al impregnated2O3Matrix.By the pre- modified porous Al in surface2O3Matrix is put into Ar protections
1100 DEG C are heated in atmosphere furnace, 2h is incubated, obtains the enhanced porous Als of Amorphous GaN O2O3Matrix.Enhanced porous Al2O3
Matrix strength, which is improved, has good processability.
The preparation process of small blunt nosed structure is as follows：(1) the Amorphous GaN O prepared is strengthened into porous Al2O3Matrix is processed
Into the small blunt configuration of design；(2) by MoSi of the granularity for 200-400 mesh2、SiO2With B2O3Powder in mass ratio 140: 30: 30
Isometric alcohol ball milling 20-24h is added after mixing；(3) mixed powder is sprayed at porous Al2O3The anti-hot junction of matrix, spraying
Measure as 0.3-1g/cm2；(4) sample after spraying is heated to from room temperature with 8 DEG C/min heating rate in air atmosphere
1200 DEG C, 90min is incubated, the middle product with silicon boron glass intermediate layer are obtained；(5) in the surface spraying in silicon boron glass intermediate layer
50-100 microns of MoSi2And TaSi2Mixture, to form face coat.Measurement shows the density and embodiment of heat insulation material
One approaches, the density 1800-2000kg/cm of far smaller than carbon-based heat insulation material3。
Embodiment three
Porous ceramic film material selects ZrO2.Other conditions are consistent with embodiment one.Measurement shows the density of heat insulation material
It is close with embodiment one.
Example IV
Silicon boron glass intermediate layer is by MoSi2Prepare.Other conditions are consistent with embodiment one.Measurement shows solar heat protection material
The density of material is approached with embodiment one.
Although the present invention is disclosed as above with preferred embodiment, it is not for limiting the present invention, any this area skill
Art personnel without departing from the spirit and scope of the present invention, can make possible variation and modification, therefore, guarantor of the invention
The scope that shield scope should be defined by the claims in the present invention is defined.
Claims (8)
1. a kind of gradient distribution heat insulation material, it is characterised in that including by the enhanced porous ceramic matrix of Amorphous GaN O, silicon boron
Glass interlayer and the face coat being made up of oxidation-resistant material, the silicon boron glass intermediate layer are by SiO2、B2O3With
MoSi2Prepare, the oxidation-resistant material is MoSi2And TaSi2Mixture or MoSi2Or SiC.
2. gradient distribution heat insulation material as claimed in claim 1, it is characterised in that the porous ceramic film material is Al2O3Or
ZrO2, averag density is 0.3-1.0g/cm3。
3. gradient distribution heat insulation material as claimed in claim 1, it is characterised in that the thickness in the silicon boron glass intermediate layer is
0.15-0.2mm。
4. gradient distribution heat insulation material as claimed in claim 1, it is characterised in that the oxidation-resistant material is MoSi2And TaSi2
Mixture or MoSi2When, the thickness of the face coat is 50-100 μm；When the oxidation-resistant material is SiC, the surface
The thickness of coating is 100-150 μm.
5. a kind of preparation method of gradient distribution heat insulation material, it is characterised in that including：
(1) the enhanced porous ceramic matrix of Amorphous GaN O is prepared；
(2) by MoSi2、SiO2With B2O3Powder is mixed, and obtains mixture, mixture is sprayed at into matrix surface, quantity for spray is 0.3-
1g/cm2, wherein, SiO2And B2O3Mass ratio be 1: 1-1.2, MoSi2Consumption be total weight of the mixture 50-70%；In sky
1200-1350 DEG C is warming up to from room temperature with 5-8 DEG C/min heating rate under gas atmosphere, 20-90min is incubated, to prepare
Middle product with silicon boron glass intermediate layer；
(3) in the surface spraying oxidation-resistant material in silicon boron glass intermediate layer, to form face coat.
6. the preparation method of gradient distribution heat insulation material as claimed in claim 5, it is characterised in that in step (1), prepare amorphous
The colloid of SiCO presomas；By porous Al2O3Material is impregnated in certain time in presoma, and diel is stood in atmosphere, obtains
Impregnated porous Al2O3Material matrix；By impregnated porous Al2O3Material matrix is placed under protective atmosphere and is heated to 1000-
1100 DEG C, 1-2h is incubated, the enhanced porous Als of Amorphous GaN O are obtained2O3Material matrix.
7. the preparation method of the gradient distribution heat insulation material as described in claim 5 or 6, it is characterised in that described in step (3)
Oxidation-resistant material is MoSi2And TaSi2Mixture or MoSi2Or SiC.
8. the preparation method of gradient distribution heat insulation material as claimed in claim 7, it is characterised in that in step (3), the antioxygen
Change material is MoSi2And TaSi2Mixture or MoSi2When, the thickness of the face coat is 50-100 μm；It is described anti-oxidant
When material is SiC, the thickness of the face coat is 100-150 μm.
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| CN108620298A (en) * | 2017-03-24 | 2018-10-09 | 山东大学 | Electrothermal silicon carbide element surface oxidation-resistant coating and preparation method thereof |
| CN109720016B (en) * | 2017-05-24 | 2020-10-13 | 中国建筑材料科学研究总院有限公司 | Anti-vibration heat insulation layer for engine and preparation method thereof |
| CN109707952A (en) * | 2018-12-27 | 2019-05-03 | 湖北航天技术研究院总体设计所 | A kind of solar heat protection heat insulation structural with Graded Density |
| CN111499414B (en) * | 2020-04-10 | 2022-04-22 | 中国航天空气动力技术研究院 | Light high-strength scouring-resistant ceramic heat-insulation integrated structure and preparation method thereof |
| CN112174698B (en) * | 2020-10-16 | 2022-09-09 | 南京宁贺表面技术有限公司 | Carbon material surface antioxidant protective coating and preparation method thereof |
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