CN101445381B - Al core/Al2O-based ceramic sheath self-healing composite foam thermal protection structure simulating capillary plexus and manufacture method thereof - Google Patents
Al core/Al2O-based ceramic sheath self-healing composite foam thermal protection structure simulating capillary plexus and manufacture method thereof Download PDFInfo
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- 238000004519 manufacturing process Methods 0.000 title abstract description 4
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- 239000004480 active ingredient Substances 0.000 description 1
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- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
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Abstract
An Al core/Al2O-based ceramic sheath self-healing composite foam thermal protection structure simulating capillary plexus and a manufacture method thereof belong to a low-melting-point metal core/high-temperature-resistant ceramic sheath composite material open-cell foam biomimetic structure with biomimetic self-healing function and the manufacture method thereof. The Al2O3-based high-temperature-resistant ceramic sheath simulates the capillary, and can keep foam shape at normal and high temperature; the low-melting-point metal core can be Al or other alloys with the function of blood incrustation and wound healing of similar capillary and the function of phase-change heat absorption by volatilization cooling of sweat in sweat gland. The Al core/Al2O3-based ceramic sheath composite foam structure can be manufactured from open-cell foam aluminum by microarc oxidation. The structure has the characteristics of light weight, high toughness, self healing, phase-change heat absorption and the like, and can be used for self-healing high-efficiency thermal protection system in hypersonic aerospace vehicles, reusable space launch vehicle, and relative industries.
Description
Technical field
A kind of decalescence that imitates the capillary vessel clump that the present invention relates to that the reusable elevated temperature heat protective material of aerospace field uses, high temperature self-healing Al core/Al2O3 based ceramic sheath composite foam structure and preparation method thereof.
Background of invention
The flight environment of vehicle situation that reenters of spacecraft is very extreme and harsh.Bore at least 15 minutes, temperature is returned smoothly up to the environmental test of 2000K, and the thermal protection system of spacecraft has been proposed strict more requirement.Yet existing multiple factor might damage the heat insulation material structure.The ice cube that falls when for example collision in terrestrial operation, spacecraft emission or bump of other objects and micrometeor in the space and space junk or the like all can cause the heat insulation material structure is damaged.Under extremely abominable spacecraft reentry environment, even atomic little crack in the thermal protection struc ture or hole all can cause the inefficacy of whole heat-protection system, and then cause huge disaster and loss.In February, 2003, U.S.'s shuttle Columbia has an accident in the Returning ball process, and all crews are all wrecked, makes whole world shock.And " arch-criminal " that cause this disaster just space shuttle strengthen place breakage in the carbon-carbon composite thermal protection struc ture.Thereafter, NASA and European Aeronautics and Space Administration have successively carried out the research of bionical self-healing material and mechanism.
In many kind materials, the crackle self-healing progress of polymer matrix composites is the fastest.The crackle self-healing of polymer matrix composites research at present is about to store the s-generation self-healing structural research stage that the first-generation self-healing structure of repairing medium and solidifying agent enters imitation capillary vessel clump in advance from microcapsule, hollow fiber, and the research of polymer matrix composites s-generation self-healing structure has begun to start.
The self-healing behavior of ceramic matric composite and polymer matrix composites a great difference arranged.At first, the service temperature of ceramic matric composite is far above polymer matrix composites; Secondly, the reparation medium in the resin base self-healing material needs and solidifying agent meets crosslinking curing could take place and self-healing, and ceramic self-healing often realizes by the high temperature oxidation of some active ingredient wherein; And ceramic matric composite preparation temperature height, the preparation difficulty is big.Thereby crackle high temperature self-healing research lags far behind the resin base self-healing material in the stupalith both at home and abroad, still is in the starting stage at present.Current stupalith self-healing few in number research also more to be confined to add SiC, B4C and MoSi2 micro-nano granules in strengthening carbon-carbon composite, form SiO2 by the micro-nano granules oxidation and wait to heal and strengthen tiny crack in the carbon carbon material, and among the TiC/Si3N4, Mullite/ZrO2/SiCp diphase ceramic material because the caused crack healing behavioral study of micro-nano granules.Still there is not the report that the first-generation, s-generation self-healing structure applications are used in the stupalith, particularly ceramic base thermally protective materials.Increasingly mature along with the emission successively of China divine boat series space shuttle and manned spaceflight technology in recent years, repeated use of realization spacecraft and guarantee spacecraft and cosmonaut's safety are returned, and the applied research in comprising the ceramic base thermally protective materials of rigid foams ceramic insulation tile of self-healing structure seems particularly urgent.
In view of the above, the present invention introduces s-generation self-healing structure in the ceramic high temperature thermally protective materials, proposes a kind of decalescence, the high temperature self-healing Al core/bionical composite foam structure of Al2O3 based ceramic sheath perforate that imitates the capillary vessel plex structure, and the preparation method is provided.
It is raw material that Chinese patent ZL87106360.3 " producing the method for foamed ceramics " once adopted open celled foam aluminium, by the high-temperature thermal oxidation method, before the Al fusing, can form one deck Al2O3 base pottery on the surface of raw material open celled foam Al metal branch and support coating, when foams are heated to above the Al fusing point, this support coating can roughly keep the integrity of open foamy structure, and make the Al of fusing and oxidizing reaction further takes place, thereby increase the thickness of supporting coating, final formation has the compound open mesh foamy structure of Al core/Al2O3 based ceramic sheath.But because the Al of the high-temperature fusion liquid state in process of cooling shrinks and solidification shrinkage, can make Al core after solidifying can not fill up the duct in the Al2O3 based ceramic sheath, cause this foamy structure mechanical property discreteness bigger.This method is not suitable for preparing the bionical composite foam structure of Al core/Al2O3 based ceramic sheath perforate of this purposes.
And the appearance of differential arc oxidization technique in recent years; the membrane of oxide ceramics that synthesizes the densification of protectiveness for metallic surfaces such as Al, Ti, Mg provides new thinking; be that metals such as Al, Ti, Mg or its alloy are placed electrolyte solution promptly by micro-plasma oxidation; impose high-voltage; utilize recombining process such as electric physics and electrochemistry to make material surface produce the spark discharge spot; generate the method for corrosion-proof wear ceramic film at workpiece surface in thermochemistry, plasma chemistry and electrochemistry jointly down.Rete and basal body binding force that this method obtains are strong, have greatly improved wear-resisting, the corrosion resisting property on Al alloy parts surface.But, adopt the differential arc oxidation legal system to be equipped with the compound open mesh foamy structure of Al core/Al2O3 based ceramic sheath and still do not have report at present at open celled foam aluminium.
Summary of the invention
The present invention is directed to spacecraft and reenter the harsh requirement of thermal environment, in the ceramic high temperature thermally protective materials, introduce s-generation self-healing structure, propose a kind of decalescence, the high temperature self-healing Al core/bionical composite foam structure of Al2O3 based ceramic sheath perforate that imitates the capillary vessel plex structure, and the preparation method is provided.
Al core/Al2O3 the based ceramic sheath self-healing composite foam thermal protection structure of the thin plexus vasculosus of a kind of simulate wool, it is characterized in that: whole for being similar to the three-dimensional branch network of capillary vessel clump open-cell foam structure, specifically comprise monolateral thickness be 20-300 μ m the Al2O3 based ceramic sheath, and the airtight Al2O3 of being wrapped in based ceramic sheath in the low melting point metal core, this low melting point metal core is Al or its alloy, above-mentioned Al2O3 based ceramic sheath has determined the normal temperature and the high temperature shape of foamy structure, and wherein metal-cored diameter is 0.5-12 with the monolateral thickness ratio of ceramic sheath.
The preparation method of the Al core/Al2O3 based ceramic sheath self-healing composite foam thermal protection structure of the thin plexus vasculosus of above-mentioned simulate wool is characterized in that:
(1), employing has the three-dimensional foam aluminum or aluminum alloy in open duct that connects as raw material;
(2), above-mentioned raw materials is carried out neutral oil removal treatment, after distilled water cleans up, put into the electrolyzer that electrolytic solution is housed, adopt constant current to carry out differential arc oxidation and form the Al2O3 based ceramic sheath on the top layer; Wherein the differential arc oxidation parameter is to change in the temperature of electrolytic solution: the 20-50 ℃ scope, and average current density is 4-10A/dm
2, be 10-120 minute conduction time, voltage is 200-600V.
Above-mentioned electrolytic solution is the mixed aqueous solution of 3-10g/L NaSiO3 and 0.5-2g/L KOH.Above-mentioned electrolytic solution is the mixed aqueous solution of 4-30g/L NaSiO3,2-10g/L KF, 1-10g/L KOH, 5-30ml ethylene glycol or glycerol.Above-mentioned electrolytic solution is for being the mixed aqueous solution of 4-30g/LNaAlO2,2-10g/L KF.Above-mentioned electrolytic solution is the mixed aqueous solution for 4-10g/L NaSiO3,1-3g/L NaAlO2,1-5g/L KOH.
In the above-mentioned constant current differential arc oxidation process, the foamed aluminium workpiece that is immersed in the electrolytic solution applies down at higher anode voltage, make the initial one deck rete that generates in its surface, when the insulating film layer part breakdown, produce minute-pressure plasma arc light discharge, under the high-energy effect of plasma micro-arc discharge generation, form moment high temperature between foamed aluminium parts and the electrolyte interface, the high pressure differential of the arc forms the foamed aluminium oxidation and sinter on the alumina-ceramic layer of outside.The Al core of raw material A l that present method adopted or aluminium alloy foam and prepared imitation capillary vessel clump/Al2O3 based ceramic sheath composite foam structural section synoptic diagram as shown in Figure 1.
The present invention is that presoma is equipped with the bionical composite foam structure of Al core/Al2O3 based ceramic sheath perforate with the differential arc oxidation legal system with open celled foam aluminium, avoided thermal oxidation method to make the ununiformity of Al2O3 based ceramic sheath thickness and the shortcoming that the Al core can not be full of duct in the ceramic sheath, and these goods not only can be by adjusting the micro-arc oxidation process parameter, control Al/Al
2O
3Relative proportion, the density of regulating foam materials.
The present invention proposes a kind of decalescence, high temperature self-healing Al core/Al2O3 based ceramic sheath composite foam structure that imitates the capillary vessel plex structure, and the low melting point Al with the three-dimensional branch network structure that is similar to the capillary vessel plex structure is metal-cored/the bionical foamy structure of refractory ceramics sheath matrix material perforate.With high temperature resistant Al2O3 based ceramic sheath imitation capillary vessel, its outside surface constitutes the open celled foam shape under normal temperature and high temperature, and the airtight parcel low melting point of ceramic sheath Al is metal-cored.
Aluminium core in the composite structure is full of all ducts in the ceramic sheath, can also improve the low-temperature flexibility of material greatly, the aluminium of composite inner fusing heat absorption can also be played the effect of cooling under high-temperature condition, and more than the molten point of aluminium to 1400 ℃ of scopes, blood in the metal-cored imitation capillary vessel of the Al of high temperature melting, cracks at ceramic sheath shell directly contacts with oxygen, high temperature oxidation taking place directly generate fine and close alumina-based ceramic and form a scab mutually and cover crackle " wound ", thereby realizes self-healing.Low melting point Al core in ceramic sheath heat absorption in a large number in melting process simultaneously, the temperature of ceramic sheath in the reduction system promptly has the function of the decalescence of sweat volatilization cooling in the similar sweat gland.
This Al core/Al2O3 based ceramic sheath composite foam structure can be applicable to possessing of hypersonic empty day aircraft, reusable space launch vehicle and the relevant industries efficient thermal protection system of characteristics such as lightweight, tough, self-healing, decalescence.
Description of drawings
Fig. 1 is former strand foam Al and Al core/Al2O3 based ceramic sheath composite foam structural section synoptic diagram of imitation capillary vessel clump, the number in the figure title: 1, the branch cross-sectional shape synoptic diagram of former strand foam Al, 2, Al core/Al2O3 based ceramic sheath schematic cross-section.
Fig. 2 is Al core/Al2O3 based ceramic sheath composite foam structure photomacrograph of imitation capillary vessel clump, composite foam structural integrity among the figure.
Fig. 3 is the precrack on the Al2O3 layer incrustation healing Al2O3 based ceramic sheath that 1400 ℃ of fusion Al ooze out and the oxidation generation is fine and close, left side figure is the photomacrograph that marks the precrack position, right figure is a precrack self-healing photo, wherein can see because 1400 ℃ of Al oxidizing reactions and rapid, " scab " of zone of oxidation is formed on the subsurface of crackle, and healed cracks.
Embodiment
Example 1
The foamed metal that uses as raw material is 6101 aluminium alloys of 10mm * 10mm * 10mm.The main component of this metal is silicon 0.3-0.7%, and the maximum level 0.5% of magnesium 0.35-0.8% and iron is gone back amount and is 0.1% and just or less than 0.1% element comprises copper, zinc, boron, manganese and chromium.Foamed aluminium is made up of the metal strip that three-dimensional random connects, and this metal strip has constituted open microvoid structure, and the outside surface of this band defines the open duct of three-dimensional random UNICOM.
Place temperature to contain 8g/L NaSiO3 for 25 ℃ the foamed aluminium after the neutral oil removing, in the electrolytic solution of 2g/L KOH, open and regulate electric current behind the power supply and make its current density at 7A/dm
2, voltage is 200-600V, and after 60 minutes processing, disconnected power down source is taken out after washing with it and is dried up that can to obtain aluminium be core, and aluminum oxide is the foamed ceramics matrix material of sheath package structure.The Al core of prepared imitation capillary vessel clump/Al2O3 based ceramic sheath composite foam structure photomacrograph as shown in Figure 2, its microscopic appearance has the described constitutional features of Fig. 1.Adopt compression set precrack in above-mentioned foamy structure, then it is incubated 0.5 hour at 1400 ℃, cooling back finds by sem observation (as shown in Figure 3), and 1400 ℃ of fused Al ooze out and oxidation generates precrack on the fine and close Al2O3 layer incrustation healing Al2O3 based ceramic sheath.
Example 2
Other steps are with example 1, and only electrolytic solution becomes 26g/L NaSiO3,10g/L KF, 8g/L KOH, 24ml ethylene glycol or glycerol, current density 8A/dm
2, voltage is 300V.
The Al core of prepared imitation capillary vessel clump/Al2O3 based ceramic sheath composite foam structure microscopic appearance has the described constitutional features of Fig. 1.Adopt compression set precrack in above-mentioned foamy structure, then with it 1100 ℃ of insulations after 1 hour, 1400 ℃ of fused Al ooze out and oxidation generates precrack on the fine and close Al2O3 layer incrustation healing Al203 based ceramic sheath.
Example 3
Other steps are with example 1, and only electrolytic solution becomes 20g/L NaAlO2,6g/L KF, current density 7A/dm
2, voltage is 240V.
The Al core of prepared imitation capillary vessel clump/Al2O3 based ceramic sheath composite foam structure microscopic appearance has the described constitutional features of Fig. 1.Adopt compression set precrack in above-mentioned foamy structure, then with it 1200 ℃ of insulations after 0.5 hour, 1400 ℃ of fused Al ooze out and oxidation generates precrack on the fine and close Al2O3 layer incrustation healing Al2O3 based ceramic sheath.
Example 4
Other steps are with example 1, and only electrolytic solution becomes 8g/L NaSiO3,3g/L NaAlO2,5g/LKOH, current density 8A/dm
2, voltage is 300V.
The Al core of prepared imitation capillary vessel clump/Al2O3 based ceramic sheath composite foam structure microscopic appearance has the described constitutional features of Fig. 1.Adopt compression set precrack in above-mentioned foamy structure, then with it 1300 ℃ of insulations after 0.5 hour, 1400 ℃ of fused Al ooze out and oxidation generates precrack on the fine and close Al2O3 layer incrustation healing Al2O3 based ceramic sheath.
The above-mentioned bionical thermal protection struc ture of high temperature self-healing composite ceramics foam and four preparation embodiments thereof of having enumerated imitation capillary vessel clump of the present invention, but bionical thermal protection struc ture proposed by the invention and above-mentioned embodiment all can only be thought can not limit the present invention to explanation of the present invention, and claims have been pointed out scope of the present invention.Therefore, under the situation of not violating the invention basic thought, as long as the ceramic heat insulation material that adopts the s-generation to have capillary vessel clump self-healing structure as long as adopted micro-arc oxidation process in the preparation production process, all should be thought to belong to protection scope of the present invention.
Claims (6)
1. the Al of the thin plexus vasculosus of simulate wool core/Al2O3 based ceramic sheath self-healing composite foam thermal protection structure, it is characterized in that: whole for being similar to the three-dimensional branch network of capillary vessel clump open-cell foam structure, specifically comprise monolateral thickness be 20-300 μ m the Al2O3 based ceramic sheath, and the airtight Al2O3 of being wrapped in based ceramic sheath in the low melting point metal core, this low melting point metal core is Al or its alloy, above-mentioned Al2O3 based ceramic sheath has determined the normal temperature and the high temperature shape of foamy structure, and wherein metal-cored diameter is 0.5-12 with the monolateral thickness ratio of ceramic sheath.
2. the preparation method of the Al core/Al2O3 based ceramic sheath self-healing composite foam thermal protection structure of the thin plexus vasculosus of simulate wool according to claim 1 is characterized in that:
(1), employing has the three-dimensional foam aluminum or aluminum alloy in open duct that connects as raw material;
(2), above-mentioned raw materials is carried out neutral oil removal treatment, after distilled water cleans up, put into the electrolyzer that electrolytic solution is housed, adopt constant current to carry out differential arc oxidation and form the Al2O3 based ceramic sheath on the top layer; Wherein the differential arc oxidation parameter is to change in the temperature of electrolytic solution: the 20-50 ℃ scope, and average current density is 4-10A/dm
2, be 10-120 minute conduction time, voltage is 200-600V.
3. the preparation method of the Al core/Al2O3 based ceramic sheath self-healing composite foam thermal protection structure of the thin plexus vasculosus of simulate wool according to claim 2 is characterized in that: described electrolytic solution is the mixed aqueous solution of 3-10g/L NaSiO3 and 0.5-2g/LKOH.
4. the preparation method of the Al core/Al2O3 based ceramic sheath self-healing composite foam thermal protection structure of the thin plexus vasculosus of simulate wool according to claim 2 is characterized in that: described electrolytic solution is for being-the mixed aqueous solution of 30g/LNaSiO3,2-10g/LKF, 1-10g/L KOH, 5-30ml ethylene glycol or glycerol.
5. the preparation method of the Al core/Al2O3 based ceramic sheath self-healing composite foam thermal protection structure of the thin plexus vasculosus of simulate wool according to claim 2 is characterized in that: described electrolytic solution is the mixed aqueous solution of 4-30g/LNaAlO2,2-10g/LKF.
6. the preparation method of the Al core/Al2O3 based ceramic sheath self-healing composite foam thermal protection structure of the thin plexus vasculosus of simulate wool according to claim 2 is characterized in that: described electrolytic solution is the mixed aqueous solution of 4-10g/L NaSiO3,1-3g/LNaAlO2,1-5g/L KOH.
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| CN111205826A (en) * | 2020-01-08 | 2020-05-29 | 哈尔滨工业大学（威海） | Multi-sphere coupling phase change heat storage material structure simulating alveolus layout and heat storage tank |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1026687C (en) * | 1986-09-16 | 1994-11-23 | 兰克西敦技术公司 | Ceramic foams |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1026687C (en) * | 1986-09-16 | 1994-11-23 | 兰克西敦技术公司 | Ceramic foams |
Non-Patent Citations (12)
| Title |
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| 刘永胜 |
| 容敏智 |
| 张兴才 |
| 张兴才;容敏智;章明秋.自修复材料研究进展.《宇航材料工艺》.2003,(第1期),1-4. * |
| 张立同 |
| 张立同;成来飞;徐永东;刘永胜;曾庆丰;董宁;栾新刚.自愈合碳化硅陶瓷基复合材料研究及应用进展.《航空材料学报》.2006,第26卷(第3期),226-228. * |
| 徐永东 |
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| 栾新刚.自愈合碳化硅陶瓷基复合材料研究及应用进展.《航空材料学报》.2006,第26卷(第3期),226-228. |
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