CN105294143A - Gradient heat proof material and preparation method thereof - Google Patents
Gradient heat proof material and preparation method thereof Download PDFInfo
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- CN105294143A CN105294143A CN201510732422.2A CN201510732422A CN105294143A CN 105294143 A CN105294143 A CN 105294143A CN 201510732422 A CN201510732422 A CN 201510732422A CN 105294143 A CN105294143 A CN 105294143A
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- heat insulation
- mosi
- gradient distribution
- insulation material
- distribution heat
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Abstract
The invention discloses a gradient heat proof material which comprises an amorphous SiCO reinforced porous ceramic material base body, a silicon-boron glass middle layer and a surface coating which is prepared from an anti-oxidation material. The preparation method comprises the following steps: (1) preparing the amorphous SiCO reinforced porous ceramic material base body; (2) mixing powder of MoSi2, SiO2 and B2O3 so as to obtain a mixture, preparing suspension of the mixture, spraying the suspension on the surface of the base body, wherein the quantity for spray is 0.3-1g/cm<2>, heating to 1200-1350 DEG C at the heating velocity of 5-8 DEG C/minute from the room temperature at the air atmosphere, keeping the temperature for 20-90 minutes, thereby preparing a middle product with the silicon-boron glass middle layer; (3) spraying the anti-oxidation material on the surface of the silicon-boron glass middle layer, thereby forming the surface coating. The gradient heat proof material disclosed by the invention is small in density, high in use temperature, that is, the use temperature can be greater than 2000K, and high in reusability.
Description
Technical field
The present invention relates to spacecraft thermal protection technology, particularly relate to a kind of gradient distribution heat insulation material and preparation method thereof.
Background technology
Reentering in process, spacecraft needs the Airflow Environment experiencing high enthalpy, high hot-fluid, and aircraft mainly bears stress and mechanical shock effect in the process.Reentering in process, spacecraft top speed can reach 25000km/h, and now the temperature of spacecraft local is not less than 1649 DEG C within the 10min time.Require in the length of several centimetres for thermal protection system, 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 carry out thermal protection to spacecraft.
Ablating heat shield is thermal protection mode the most frequently used at present.Namely by the mass loss of heat insulation material, the heat that heat structure surface produces is taken away.Conventional heat insulation material comprises carbon back heat insulation material and silica-based heat insulation material.This anti-hot mode solves the thermal protection problem reentered returning satellite, spaceship.The spacecraft of new generation being representative with Control System for Reusable Launch Vehicle and re-entry space vehicle further provides low density, the requirement such as reusable to thermal protection.Existing ablating heat shield can not accordingly 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 at 1800-2000kg/m
3between, be greater than the thermal protection demand of Control System for Reusable Launch Vehicle and re-entry space vehicle: heat structure density 300-800kg/m
3.High density can make the weight of spacecraft increase, and then causes launch cost to raise.
(2) ablation shape change greatly, and heat structure can not be reused.Ablating heat shield by the mass loss of heat insulation material, the heat that heat structure surface produces is taken away.After each, the profile of heat structure all can change, and affects the aeroperformance of spacecraft.Therefore, ablating heat shield does not possess reusability.
Summary of the invention
For above-mentioned technical problem, the invention provides a kind of lightweight construction, heat-proof quality is good, reusable gradient distribution heat insulation material.
Present invention also offers a kind of preparation method of gradient distribution heat insulation material.
Technical scheme of the present invention is:
A kind of gradient distribution heat insulation material, comprise strengthened by Amorphous GaN O porous ceramic matrix, silicon boron glass middle layer and the top coat be made up of oxidation-resistant material.
Preferably, in described gradient distribution heat insulation material, described porous ceramic film material is Al
2o
3or ZrO
2, mean density is 0.3-1.0g/cm
3.
Preferably, in described gradient distribution heat insulation material, described silicon boron glass middle layer is by SiO
2, B
2o
3and MoSi
2prepare.
Preferably, in described gradient distribution heat insulation material, the thickness in described silicon boron glass middle layer is 0.15-0.2mm.
Preferably, in described gradient distribution heat insulation material, described oxidation-resistant material is MoSi
2and TaSi
2mixture or MoSi
2or SiC.
Preferably, in described gradient distribution heat insulation material, described oxidation-resistant material is MoSi
2and TaSi
2mixture or MoSi
2time, the thickness of described top coat is 50-100 μm; When described oxidation-resistant material is SiC, the thickness of described top coat is 100-150 μm.
A preparation method for gradient distribution heat insulation material, comprising:
(1) porous ceramic matrix that Amorphous GaN O strengthens is prepared;
(2) by MoSi
2, SiO
2with B
2o
3powder mixes, and obtain mixture, mixture is sprayed at matrix surface, quantity for spray is 0.3-1g/cm
2, wherein, SiO
2and B
2o
3mass ratio be 1: 1-1.2, MoSi
2consumption be the 50-70% of mixture total weight amount; Be warming up to 1200-1350 DEG C from room temperature with the temperature rise rate of 5-8 DEG C/min in air atmosphere, insulation 20-90min, to prepare the middle product with silicon boron glass middle layer;
(3) at the surface spraying oxidation-resistant material in silicon boron glass middle layer, to form top coat.
Preferably, in the preparation method of described gradient distribution heat insulation material, in step (1), prepare the colloid of Amorphous GaN O presoma; By porous Al
2o
3material soaking is certain hour in presoma, leaves standstill certain hour in atmosphere, obtains the porous Al through dipping
2o
3material matrix; By the porous Al through dipping
2o
3material matrix is heated to 1000-1100 DEG C under being placed in protective atmosphere, and insulation 1-2h, obtains the porous Al that Amorphous GaN O strengthens
2o
3material matrix.
Preferably, in the preparation method of described gradient distribution heat insulation material, in step (3), described oxidation-resistant material is MoSi
2and TaSi
2mixture or MoSi
2or SiC.
Preferably, in the preparation method of described gradient distribution heat insulation material, in step (3), described oxidation-resistant material is MoSi
2and TaSi
2mixture or MoSi
2time, the thickness of described top coat is 50-100 μm; When described oxidation-resistant material is SiC, the thickness of described top coat is 100-150 μm.
The invention has the advantages that:
1, gradient distribution heat insulation material density of the present invention is little, and use temperature is high, can reach more than 2000K.
2, gradient distribution heat insulation material anti-seismic performance of the present invention is good, and reusability is high.
3, in preparation method of the present invention, material technology ripening degree is high, and preparation technology easily realizes and through engineering approaches degree is higher.
4, preparation cycle is short, and operation and maintenance cost is low.
Accompanying drawing explanation
Fig. 1 is the structural representation of gradient distribution heat insulation material of the present invention.
Fig. 2 is the effect comparison analysis chart of gradient distribution heat insulation material and prior art.
The porous Al that Fig. 3 (a) strengthens for Amorphous GaN O in embodiment one
2o
3the infrared spectrogram of matrix, the porous Al that Fig. 3 (b) strengthens for Amorphous GaN O in embodiment one
2o
3the total spectrogram of XPS of matrix.
Fig. 4 is little blunt nosed schema.
Embodiment
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, are described in detail the specific embodiment of the present invention below in conjunction with accompanying drawing.
Refer to Fig. 1, the invention provides a kind of gradient distribution heat insulation material, comprise strengthened by Amorphous GaN O porous ceramic matrix, silicon boron glass middle layer and the top coat be made up of oxidation-resistant material.
Please see Figure 2, in order to the advantage of gradient distribution heat insulation material is described, adopt the anti-thermal effect of ANSYS software to gradient distribution heat insulation material and three kinds of traditional solar heat protection+heat insulation schemes to analyze, three kinds of existing schemes are respectively C/C+ lagging material, superhigh temperature ceramics (UHTC)+lagging material, low-density ceramic+lagging material.Four kinds of materials are all processed into little blunt nosed structure (i.e. structure as shown in Figure 4, this structure has cap).Calculating the Airflow Environment adopted is typical space device reentry environment, and 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 see embodiment one.According to calculating constraint, porous alumina elect density 450kg/m as
3, use temperature 1900K.As can be seen from Figure 1, under identical constraint condition, the total thickness of C/C+ lagging material, superhigh temperature ceramics (UHTC)+lagging material, low-density ceramic+lagging material and gradient distribution heat insulation material is respectively 102mm, 67.7mm, 34.3mm and 30.8mm, and corresponding density of texture is respectively 1653kg/m
3, 4817kg/m
3, 768kg/m
3and 487kg/m
3.Namely gradient distribution heat insulation material has minimum thickness and minimum density of texture.Namely gradient distribution heat insulation material can effectively reduce the weight of thermal protection system, and then reduces the launch cost of aircraft.In addition, it can also be seen that from Fig. 2, in same overall thickness situation, gradient distribution thermal protection struc ture has the highest surface emissivity rate of heat dissipation, 821kW/m
2.More than analyze and show, relative to traditional solar heat protection+heat insulation schemes, gradient distribution heat insulation material has better anti-thermal effect and lower launch cost.Further, relative to cap surface, the temperature at cap side faces and the back side is lower, can mate with supporter implementation structure consistency.
The principle of work of gradient distribution heat insulation material is: under Aerodynamic Heating environment, and material surface produces homogeneous heating.In heat-processed, the stress equilibrium dispersion that temperature variation produces by silicon boron glass middle layer, avoids heat insulation material to produce hot tearing damage.After surface heating reaches certain temperature, the top coat that oxidation-resistant material is made starts outside radiations heat energy, stops the oxygen in Airflow Environment to the internal divergence of heat insulation material simultaneously.Silicon boron glass middle layer then effectively can reduce the transmission of heat to heat insulation material inside, and by MoSi in silicon boron glass
2passive oxidation adsorption and diffusion enter oxygen in heat insulation material.
Further, in described gradient distribution heat insulation material, described porous ceramic film material is Al
2o
3or ZrO
2, mean density is 0.3-1.0g/cm
3.
Further, in described gradient distribution heat insulation material, described silicon boron glass middle layer is by SiO
2, B
2o
3and MoSi
2prepare.
Further, in described gradient distribution heat insulation material, the thickness in described silicon boron glass middle layer is 0.15-0.2mm.
Further, in described gradient distribution heat insulation material, described oxidation-resistant material is MoSi
2and TaSi
2mixture or MoSi
2or SiC.
Further, in described gradient distribution heat insulation material, described oxidation-resistant material is MoSi
2and TaSi
2mixture or MoSi
2time, the thickness of described top coat is 50-100 μm; When described oxidation-resistant material is SiC, the thickness of described top coat is 100-150 μm.
Present invention also offers a kind of preparation method of gradient distribution heat insulation material, comprising: (1) prepares the porous ceramic matrix that Amorphous GaN O strengthens; (2) by MoSi
2, SiO
2with B
2o
3powder mixes, and obtain mixture, mixture is sprayed at matrix surface, quantity for spray is 0.3-1g/cm
2, wherein, SiO
2and B
2o
3mass ratio be 1: 1-1.2, MoSi
2consumption be the 50-70% of mixture total weight amount; Be warming up to 1200-1350 DEG C from room temperature with the temperature rise rate of 5-8 DEG C/min in air atmosphere, insulation 20-90min, to prepare the middle product with silicon boron glass middle layer; (3) at the surface spraying oxidation-resistant material in silicon boron glass middle layer, to form top coat.
Further, in the preparation method of described gradient distribution heat insulation material, in step (1), prepare the colloid of Amorphous GaN O presoma; By porous Al
2o
3material soaking is certain hour in presoma, leaves standstill certain hour in atmosphere, obtains the porous Al through dipping
2o
3material matrix; By the porous Al through dipping
2o
3material matrix is heated to 1000-1100 DEG C under being placed in protective atmosphere, and insulation 1-2h, obtains the porous Al that Amorphous GaN O strengthens
2o
3material matrix.Wherein, when preparing presoma, preferably adopt triethoxy silica alkane or diethoxy siloxanes.
Further, in the preparation method of described gradient distribution heat insulation material, in step (3), described oxidation-resistant material is MoSi
2and TaSi
2mixture or MoSi
2or SiC.
Further, in the preparation method of described gradient distribution heat insulation material, in step (3), described oxidation-resistant material is MoSi
2and TaSi
2mixture or MoSi
2time, the thickness of described top coat is 50-100 μm; When described oxidation-resistant material is SiC, the thickness of described top coat is 100-150 μm.
Embodiment one
In order to further illustrate superiority of the present invention, invention has been Amorphous GaN O and strengthening porous Al
2o
3the Study on Preparation of material.Employing density is 750kg/m
3, use temperature is that the porous alumina of 2200K is as matrix.Vinyltriethoxysilane, dehydrated alcohol, distilled water by 1: 3: 1 mixing, and are added the hydrochloric acid of 1-3at%, stirs 3-5 minute with glass stick, obtain the organosilicon colloid of homogeneous transparent, i.e. Amorphous GaN O presoma.This presoma is left standstill 24h.By the porous Al of size 60mm × 60mm × 60mm
2o
3be impregnated into rear in 10min in presoma taking-up, leave standstill 24h in atmosphere, repeated impregnations 3 times, obtain the porous Al of flooding
2o
3matrix.By pre-for surface modified porous Al
2o
3the atmosphere furnace that matrix puts into Ar protection is heated to 1000 DEG C, and insulation 1h, obtains the porous Al that Amorphous GaN O strengthens
2o
3matrix.Porous Al after enhancing
2o
3matrix strength raising has good processability.Fig. 3 (a) and Fig. 3 (b) sets forth the porous Al that Amorphous GaN O strengthens
2o
3the infrared spectrogram of matrix and XPS score analytical results.
Fig. 4 provides a kind of schema of little blunt nosed structure.The preparation process of this little blunt nosed structure is as follows: the Amorphous GaN O prepared is strengthened porous Al by (1)
2o
3matrix is processed into the little blunt configuration (see Fig. 4) of design; (2) be 200-400 object MoSi by granularity
2, SiO
2with B
2o
3powder in mass ratio 65: 30: 35 mixing after add equal-volume alcohol ball milling 20-24h; (3) mixed powder spray is applied to porous Al
2o
3the anti-hot junction of matrix, quantity for spray is 0.3-1g/cm
2; (4) sample after spraying is heated to 1320 DEG C from room temperature with the temperature rise rate of 5 DEG C/min in air atmosphere, insulation 30min, obtains the middle product with silicon boron glass middle layer; (5) the SiC coating of the surface spraying 100-150 micron in silicon boron glass middle layer, to form top coat.The density measuring display heat insulation material is 800kg/m
3, be less than the density 1800-2000kg/cm of carbon back heat insulation material
3.Hyperthermia radiation test shows that the surface emissivity of this gradient distribution heat insulation material is greater than 0.9, and namely in high temperature environments, gradient distribution surface can will act on its heat radiation to the external space, effectively reduces the anti-thermal pressure of porous matrix.
Embodiment two
Vinyltriethoxysilane, dehydrated alcohol, distilled water by 1: 3: 1 mixing, and are added the hydrochloric acid of 1-3at%, stirs 3-5 minute with glass stick, obtain the organosilicon colloid of homogeneous transparent, i.e. Amorphous GaN O presoma.This presoma is left standstill 24h.By the porous Al of size 60mm × 60mm × 60mm
2o
3be impregnated into rear in 10min in presoma taking-up, leave standstill 24h in atmosphere, repeated impregnations 3 times, obtain the porous Al of flooding
2o
3matrix.By pre-for surface modified porous Al
2o
3the atmosphere furnace that matrix puts into Ar protection is heated to 1100 DEG C, and insulation 2h, obtains the porous Al that Amorphous GaN O strengthens
2o
3matrix.Porous Al after enhancing
2o
3matrix strength raising has good processability.
The preparation process of little blunt nosed structure is as follows: the Amorphous GaN O prepared is strengthened porous Al by (1)
2o
3matrix is processed into the little blunt configuration of design; (2) be 200-400 object MoSi by granularity
2, SiO
2with B
2o
3powder in mass ratio 140: 30: 30 mixing after add equal-volume alcohol ball milling 20-24h; (3) mixed powder spray is applied to porous Al
2o
3the anti-hot junction of matrix, quantity for spray is 0.3-1g/cm
2; (4) sample after spraying is heated to 1200 DEG C from room temperature with the temperature rise rate of 8 DEG C/min in air atmosphere, insulation 90min, obtains the middle product with silicon boron glass middle layer; (5) MoSi of the surface spraying 50-100 micron in silicon boron glass middle layer
2and TaSi
2mixture, to form top coat.Density and the embodiment one of measuring display heat insulation material are close, are far smaller than the density 1800-2000kg/cm of carbon back heat insulation material
3.
Embodiment three
Porous ceramic film material selects ZrO
2.Other conditions are all consistent with embodiment one.Density and the embodiment one of measuring display heat insulation material are close.
Embodiment four
Silicon boron glass middle layer is by MoSi
2prepare.Other conditions are consistent with embodiment one.Density and the embodiment one of measuring display heat insulation material are close.
Although the present invention with preferred embodiment openly as above; but it is not for limiting the present invention; any those skilled in the art without departing from the spirit and scope of the present invention; possible variation and amendment can be made; therefore, the scope that protection scope of the present invention should define with the claims in the present invention is as the criterion.
Claims (10)
1. a gradient distribution heat insulation material, is characterized in that, comprise strengthened by Amorphous GaN O porous ceramic matrix, silicon boron glass middle layer and the top coat be made up of oxidation-resistant material.
2. gradient distribution heat insulation material as claimed in claim 1, it is characterized in that, described porous ceramic film material is Al
2o
3or ZrO
2, mean density is 0.3-1.0g/cm
3.
3. gradient distribution heat insulation material as claimed in claim 1 or 2, it is characterized in that, described silicon boron glass middle layer is by SiO
2, B
2o
3and MoSi
2prepare.
4. gradient distribution heat insulation material as claimed in claim 3, it is characterized in that, the thickness in described silicon boron glass middle layer is 0.15-0.2mm.
5. gradient distribution heat insulation material as claimed in claim 3, it is characterized in that, described oxidation-resistant material is MoSi
2and TaSi
2mixture or MoSi
2or SiC.
6. gradient distribution heat insulation material as claimed in claim 5, it is characterized in that, described oxidation-resistant material is MoSi
2and TaSi
2mixture or MoSi
2time, the thickness of described top coat is 50-100 μm; When described oxidation-resistant material is SiC, the thickness of described top coat is 100-150 μm.
7. a preparation method for gradient distribution heat insulation material, is characterized in that, comprising:
(1) porous ceramic matrix that Amorphous GaN O strengthens is prepared;
(2) by MoSi
2, SiO
2with B
2o
3powder mixes, and obtain mixture, mixture is sprayed at matrix surface, quantity for spray is 0.3-1g/cm
2, wherein, SiO
2and B
2o
3mass ratio be 1: 1-1.2, MoSi
2consumption be the 50-70% of mixture total weight amount; Be warming up to 1200-1350 DEG C from room temperature with the temperature rise rate of 5-8 DEG C/min in air atmosphere, insulation 20-90min, to prepare the middle product with silicon boron glass middle layer;
(3) at the surface spraying oxidation-resistant material in silicon boron glass middle layer, to form top coat.
8. the preparation method of gradient distribution heat insulation material as claimed in claim 7, is characterized in that, in step (1), prepare the colloid of Amorphous GaN O presoma; By porous Al
2o
3material soaking is certain hour in presoma, leaves standstill diel in atmosphere, obtains the porous Al through dipping
2o
3material matrix; By the porous Al through dipping
2o
3material matrix is heated to 1000-1100 DEG C under being placed in protective atmosphere, and insulation 1-2h, obtains the porous Al that Amorphous GaN O strengthens
2o
3material matrix.
9. the preparation method of gradient distribution heat insulation material as claimed in claim 7 or 8, it is characterized in that, in step (3), described oxidation-resistant material is MoSi
2and TaSi
2mixture or MoSi
2or SiC.
10. the preparation method of gradient distribution heat insulation material as claimed in claim 9, it is characterized in that, in step (3), described oxidation-resistant material is MoSi
2and TaSi
2mixture or MoSi
2time, the thickness of described top coat is 50-100 μm; When described oxidation-resistant material is SiC, the thickness of described top coat is 100-150 μm.
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Cited By (5)
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| CN107160748A (en) * | 2017-05-24 | 2017-09-15 | 中国建筑材料科学研究总院 | A kind of gradient thermal insulation layer and preparation method thereof and device |
| CN108620298A (en) * | 2017-03-24 | 2018-10-09 | 山东大学 | Electrothermal silicon carbide element surface oxidation-resistant coating 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 |
| CN111499414A (en) * | 2020-04-10 | 2020-08-07 | 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 |
| CN112174698A (en) * | 2020-10-16 | 2021-01-05 | 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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| CN112174698A (en) * | 2020-10-16 | 2021-01-05 | 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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|---|---|
| CN105294143B (en) | 2017-09-05 |
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