CN102093083B - Preparation method for ablation-resistant coating made of carbon/carbon composite material HfC - Google Patents
Preparation method for ablation-resistant coating made of carbon/carbon composite material HfC Download PDFInfo
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- CN102093083B CN102093083B CN201010575008A CN201010575008A CN102093083B CN 102093083 B CN102093083 B CN 102093083B CN 201010575008 A CN201010575008 A CN 201010575008A CN 201010575008 A CN201010575008 A CN 201010575008A CN 102093083 B CN102093083 B CN 102093083B
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Abstract
The invention discloses a preparation method of an ablation-resistant made of a carbon/carbon composite material HfC. The method comprises the following steps of: I, polishing the carbon/carbon composite material, cleaning and drying; II, mixing by ball-milling to prepare slurry; III, uniformly brushing or spraying the slurry onto the surface of the carbon/carbon composite material; and IV, sintering under the protection of inert gas to prepare the ablation-resistant made of the carbon/carbon composite material HfC. By adopting the method, damage on carbon fibers caused by the reaction of HfO2 and C in a substrate modification process is overcame, the permeation capability of Hf is enhanced due to the addition of a rare earth metal oxide and AlN, and the coating is uniform, compact and flawless; in addition, a constituent transition gradient coating is formed between the coating and the carbon/carbon composite material, so that the residue stress of the coating is reduced, the bonding strength between the HfC coating and the carbon/carbon composite material is enhanced, and the high-temperature intensity of the HfC is enhanced.
Description
Technical field
The invention belongs to the high temperature material technical field, be specifically related to the preparation method of the anti-ablative coating of a kind of carbon/carbon composite HfC.
Background technology
Carbon/carbon composite be at present unique can be at the material that keeps higher mechanical property more than 2000 ℃; A series of excellent properties such as it has that low density, height ratio are strong, height ratio mould, low thermal coefficient of expansion and heat shock resistance; Especially have the special performance that intensity raises and goes up not down with temperature, use as the ultrahigh-temperature thermal structure material to have unique advantage.Yet, to wash away under the environment at high temperature oxidation, high velocity air and high-velocity particles stream, the anti-ablation property of carbon/carbon composite is relatively poor.The main method that improves the anti-ablation property of carbon/carbon composite is: (1) matrix modification, promptly add refractory carbides in matrix of carbon/carbon composite materials; (2) prepare anti-ablative coating, promptly at carbon/carbon composite surface preparation refractory carbides, silicide or boride compound coating.
People such as Li Shuping (Li Shuping, Li Kezhi, Guo Lingjun and hilllock forever, the ablation property research of the whole larynx lining of HfC modification C/C matrix material, Journal of Inorganic Materials, 2008,23 (6): 1155~1158) employing HfOCl
28H
2O ethanolic soln impregnated carbon precast body utilizes thermal treatment to make HfOCl
2Be converted into HfO earlier
2Be converted into HfC again, realize modification, improved the anti-ablation property of C/C matrix material carbon matrix.Yet, HfO
2Damage the charcoal fiber with the process of charcoal reaction generation HfC, reduced the mechanical property of C/C matrix material.
Marquis's root very waits people (Hou Genliang, Su Xunjia, Wang Yanbin, Zhou Xiaobo, the preparation of the anti-ablation HfC of C/C matrix material coating, aeronautical material journal, 2009,29 (1): 77~80) adopt HfOCl
2Solution applies matrix material, and 1800 ℃ of thermal treatment 2h under argon atmospher form the HfC coating then.Yet not only there is crackle in the HfC coating of this method preparation but also is porous, can not effectively improve the anti-ablation property of carbon/carbon composite.
People such as Wang Depeng (Wang Depeng, Su Xunjia, Hou Genliang, the preparation of HfC ceramic coating and performance analysis, Guangdong non-ferrous metal journal, 2006,16 (1): 19~21) adopt plasma spraying method to prepare the HfC coating.Yet; Because HfC generating gasification more than fusing point is decomposed and do not melted, adopt plasma spraying method to prepare HfC coating preparation metal bonding coating earlier, and metal bonding coating can not be used under the hot conditions more than 1650 ℃; In addition, the HfC coating exists micropore and bonding strength low.
U.S. Ultramet company adopts the chemical vapor deposition (CVD) method to prepare the HfC coating.Yet, adopt this method to prepare the HfC coating, reaction product HCl is serious to equipment corrosion, and coating and high base strength are low.
Summary of the invention
Technical problem to be solved by this invention is the deficiency to above-mentioned prior art, and a kind of carbon/carbon composite HfC is provided the preparation method of anti-ablative coating.The anti-ablative coating of the HfC of preparation is evenly fine and close, and is high with the carbon/carbon composite bonding strength.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: the preparation method of the anti-ablative coating of a kind of carbon/carbon composite HfC is characterized in that this method may further comprise the steps:
(1) with behind the carbon/carbon composite sanding and polishing, clean 20min~60min at the organic solvent for ultrasonic ripple, put into baking oven then and dry;
(2) obtain mixture with mixing in Hf powder, rare-earth oxide powder, AlN powder and the Graphite Powder 99 adding ball grinder, in ball grinder, add ETHYLE ACETATE and zapon varnish then, ball mill mixing 24h~72h prepares slip; The mass percent of Hf powder is 70%~89% in the said mixture, and the mass percent of rare-earth oxide powder is 5%~15%, and the mass percent of AlN powder is 1%~5%, and Graphite Powder 99 is a surplus; The quality sum of said ETHYLE ACETATE and zapon varnish is 50%~150% of a mixture quality; The mass ratio of said ETHYLE ACETATE and zapon varnish is 1~2: 1;
(3) slip described in the step (2) is evenly brushed or is sprayed at the surface of the carbon/carbon composite after the oven dry in the step (1), and form the coating that thickness is not less than 50 μ m, place baking oven to dry then on the surface;
(4) carbon/carbon composite after the oven dry in the step (3) is put into plumbago crucible; Together place vacuum oven again; Under protection of inert gas; Temperature rise rate with 5 ℃/min~25 ℃/min is warming up to 1550 ℃~1900 ℃ sintering, is incubated 2h~3h then, and outage is cooled to room temperature and obtains the anti-ablative coating of carbon/carbon composite HfC.
The system of sanding and polishing is described in the above-mentioned steps (1): use the SiC silicon carbide paper successively No. 400, No. 800 SiC silicon carbide papers, No. 1200 SiC silicon carbide paper sanding and polishings.
Organic solvent is an acetone or alcohol described in the above-mentioned steps (1); Temperature of oven described in the above-mentioned steps (1) is 100 ℃~200 ℃.
The rare-earth oxide powder is Y described in the above-mentioned steps (2)
2O
3Powder, Er
2O
3Powder, Sc
2O
3Powder, Lu
2O
3Powder, La
2O
3Powder, Yb
2O
3Powder, Ce
2O
3Powder and Gd
2O
3In the powder one or more.
Ball grinder described in the above-mentioned steps (2) is aluminum oxide ball milling jar or urethane ball grinder.
The thickness of coating described in the above-mentioned steps (3) is 50 μ m~1500 μ m; Temperature of oven described in the step (3) is 100 ℃~200 ℃.
Rare gas element described in the above-mentioned steps (4) is that quality purity is not less than 99.9% argon gas.
The present invention compared with prior art has the following advantages: the present invention makes Hf and C be reflected at carbon/carbon composite surface preparation HfC coating through slip coating, inert atmosphere protection sintering, has overcome HfO in the matrix modification process
2Damage with C reaction pair charcoal fiber; Ability is oozed in the expansion that the adding of rare-earth oxide and AlN has improved Hf; Make coating evenly, densification and flawless, make the gradient cladding that forms the composition transition between coating and the matrix simultaneously, reduced the unrelieved stress of coating; Improve HfC coating and high base strength, also improved the hot strength of HfC coating simultaneously.
Below in conjunction with accompanying drawing and embodiment the present invention is done further detailed description.
Description of drawings
Fig. 1 is the X-ray diffracting spectrum of the anti-ablative coating of carbon/carbon composite HfC of the embodiment of the invention 1 preparation.
Fig. 2 is the profile scanning electromicroscopic photograph of the anti-ablative coating of carbon/carbon composite HfC of the embodiment of the invention 1 preparation.
Fig. 3 is the surface scan electromicroscopic photograph of the anti-ablative coating of carbon/carbon composite HfC of the embodiment of the invention 1 preparation.
Embodiment
Embodiment 1
(1) carbon/carbon composite is used SiC silicon carbide paper sanding and polishing successively No. 400, No. 800, No. 1200, ultrasonic cleaning 20min in acetone then, the baking oven of putting into temperature and be 100 ℃ is dried;
(2) obtain mixture with mixing in Hf powder, rare-earth oxide powder, AlN powder and the Graphite Powder 99 adding aluminum oxide ball milling jar, in ball grinder, add ETHYLE ACETATE and zapon varnish then, ball mill mixing 24h prepares slip; The mass percent of Hf powder is 70% in the said mixture, and the mass percent of rare-earth oxide powder is 15%, and the mass percent of AlN powder is 5%, and Graphite Powder 99 is a surplus, and said rare-earth oxide powder is La
2O
3Powder, the quality sum of said ETHYLE ACETATE and zapon varnish is 50% of a mixture quality; The mass ratio of said ETHYLE ACETATE and zapon varnish is 2: 1;
(3) slip is evenly brushed the surface of carbon/carbon composite after oven dry, and form the coating of thickness 50 μ m on the surface, placing temperature then is that 150 ℃ baking oven is dried;
(4) carbon/carbon composite after will drying is put into plumbago crucible; Together place vacuum oven again; Be not less than at quality purity under 99.9% the argon shield; Temperature rise rate with 5 ℃/min is warming up to 1550 ℃ of sintering, is incubated 3h then, and outage is cooled to room temperature and obtains the anti-ablative coating with high, fine and close even, the flawless HfC of carbon/carbon composite bonding strength.
X-ray diffracting spectrum such as Fig. 1 of the anti-ablative coating of carbon/carbon composite HfC of present embodiment preparation, the crystal face of diffraction peak corresponds respectively to (111), (200), (220), (311), (222), (400) crystal face of HfC among the figure.
Profile scanning electromicroscopic photograph such as Fig. 2 of the anti-ablative coating of carbon/carbon composite HfC of present embodiment preparation, the anti-ablative coating of HfC combines well with matrix of carbon/carbon composite materials.
Surface scan electromicroscopic photograph such as Fig. 3 of the anti-ablative coating of carbon/carbon composite HfC of present embodiment preparation, fine and close, the flawless of the anti-ablative coating of HfC.
Embodiment 2
Present embodiment is identical with embodiment 1, and wherein difference is: used rare-earth oxide powder is Er
2O
3, Sc
2O
3, Lu
2O
3, La
2O
3, Yb
2O
3, Ce
2O
3And Gd
2O
3In a kind of, perhaps be Y
2O
3, Er
2O
3, Sc
2O
3, Lu
2O
3, La
2O
3, Yb
2O
3, Ce
2O
3And Gd
2O
3In at least two kinds.
The anti-ablative coating of HfC and the carbon/carbon composite bonding strength of present embodiment preparation are high, and coating is fine and close evenly, flawless.
Embodiment 3
(1) carbon/carbon composite is used SiC silicon carbide paper sanding and polishing successively No. 400, No. 800, No. 1200, ultrasonic cleaning 40min in ethanol then, the baking oven of putting into temperature and be 200 ℃ is dried;
(2) obtain mixture with mixing in Hf powder, rare-earth oxide powder, AlN powder and the Graphite Powder 99 adding urethane ball grinder, in ball grinder, add ETHYLE ACETATE and zapon varnish then, ball mill mixing 48h prepares slip; The mass percent of Hf powder is 89% in the said mixture, and the mass percent of rare-earth oxide powder is 5%, and the mass percent of AlN powder is 1%, and Graphite Powder 99 is a surplus, and said rare-earth oxide powder is Sc
2O
3Powder, the quality sum of said ETHYLE ACETATE and zapon varnish is 100% of a mixture quality; The mass ratio of said ETHYLE ACETATE and zapon varnish is 1: 1;
(3) slip is evenly brushed the surface of carbon/carbon composite after oven dry, and form the coating of thickness 1500 μ m on the surface, placing temperature then is that 200 ℃ baking oven is dried;
(4) carbon/carbon composite after will drying is put into plumbago crucible; Together place vacuum oven again; Be not less than at quality purity under 99.9% the argon shield; Temperature rise rate with 25 ℃/min is warming up to 1900 ℃ of sintering, is incubated 2h then, and outage is cooled to room temperature and obtains the anti-ablative coating with high, fine and close even, the flawless HfC of carbon/carbon composite bonding strength.
Embodiment 4
Present embodiment is identical with embodiment 3, and wherein difference is: used rare-earth oxide powder is Y
2O
3, Er
2O
3, Lu
2O
3, La
2O
3, Yb
2O
3, Ce
2O
3And Gd
2O
3In a kind of, perhaps be Y
2O
3, Er
2O
3, Sc
2O
3, Lu
2O
3, La
2O
3, Yb
2O
3, Ce
2O
3And Gd
2O
3In at least two kinds.
The anti-ablative coating of HfC and the carbon/carbon composite bonding strength of present embodiment preparation are high, and coating is fine and close evenly, flawless.
Embodiment 5
(1) carbon/carbon composite is used SiC silicon carbide paper sanding and polishing successively No. 400, No. 800, No. 1200, ultrasonic cleaning 60min in acetone then, the baking oven of putting into temperature and be 150 ℃ is dried;
(2) obtain mixture with mixing in Hf powder, rare-earth oxide powder, AlN powder and the Graphite Powder 99 adding aluminum oxide ball milling jar, in ball grinder, add ETHYLE ACETATE and zapon varnish then, ball mill mixing 72h prepares slip; The mass percent of Hf powder is 80% in the said mixture, and the mass percent of rare-earth oxide powder is 10%, and the mass percent of AlN powder is 3%, and Graphite Powder 99 is a surplus, and said rare-earth oxide powder is Ce
2O
3Powder, the quality sum of said ETHYLE ACETATE and zapon varnish is 150% of a mixture quality; The mass ratio of said ETHYLE ACETATE and zapon varnish is 1.5: 1;
(3) slip is evenly brushed the surface of carbon/carbon composite after oven dry, and form the coating of thickness 800 μ m on the surface, placing temperature then is that 100 ℃ baking oven is dried;
(4) carbon/carbon composite after will drying is put into plumbago crucible; Together place vacuum oven again; Be not less than at quality purity under 99.9% the argon shield; Temperature rise rate with 15 ℃/min is warming up to 1725 ℃ of sintering, is incubated 2.5h then, and outage is cooled to room temperature and obtains the anti-ablative coating with high, fine and close even, the flawless HfC of carbon/carbon composite bonding strength.
Embodiment 6
Present embodiment is identical with embodiment 5, and wherein difference is: used rare-earth oxide powder is Y
2O
3, Er
2O
3, Sc
2O
3, Lu
2O
3, La
2O
3, Yb
2O
3And Gd
2O
3In a kind of, perhaps be Y
2O
3, Er
2O
3, Sc
2O
3, Lu
2O
3, La
2O
3, Yb
2O
3, Ce
2O
3And Gd
2O
3In at least two kinds.
The anti-ablative coating of HfC and the carbon/carbon composite bonding strength of present embodiment preparation are high, and coating is fine and close evenly, flawless.
Claims (7)
1. the preparation method of the anti-ablative coating of carbon/carbon composite HfC is characterized in that, this method may further comprise the steps:
(1) with behind the carbon/carbon composite sanding and polishing, clean 20min~60min at the organic solvent for ultrasonic ripple, put into baking oven then and dry;
(2) obtain mixture with mixing in Hf powder, rare-earth oxide powder, AlN powder and the Graphite Powder 99 adding ball grinder, in ball grinder, add ETHYLE ACETATE and zapon varnish then, ball mill mixing 24h~72h prepares slip; The mass percent of Hf powder is 70%~89% in the said mixture, and the mass percent of rare-earth oxide powder is 5%~15%, and the mass percent of AlN powder is 1%~5%, and Graphite Powder 99 is a surplus; The quality sum of said ETHYLE ACETATE and zapon varnish is 50%~150% of a mixture quality; The mass ratio of said ETHYLE ACETATE and zapon varnish is 1~2: 1;
(3) slip described in the step (2) is evenly brushed or is sprayed at the surface of the carbon/carbon composite after the oven dry in the step (1), and form the coating that thickness is not less than 50 μ m, place baking oven to dry then on the surface;
(4) carbon/carbon composite after the oven dry in the step (3) is put into plumbago crucible; Together place vacuum oven again; Under protection of inert gas; Temperature rise rate with 5 ℃/min~25 ℃/min is warming up to 1550 ℃~1900 ℃ sintering, is incubated 2h~3h then, and outage is cooled to room temperature and obtains the anti-ablative coating of carbon/carbon composite HfC.
2. the preparation method of the anti-ablative coating of carbon/carbon composite HfC according to claim 1; It is characterized in that; The system of sanding and polishing is described in the step (1): use the SiC silicon carbide paper successively No. 400, No. 800 SiC silicon carbide papers, No. 1200 SiC silicon carbide paper sanding and polishings.
3. the preparation method of the anti-ablative coating of carbon/carbon composite HfC according to claim 1 is characterized in that organic solvent is an acetone or alcohol described in the step (1); Temperature of oven described in the step (1) is 100 ℃~200 ℃.
4. the preparation method of the anti-ablative coating of carbon/carbon composite HfC according to claim 1 is characterized in that the rare-earth oxide powder is Y described in the step (2)
2O
3Powder, Er
2O
3Powder, Sc
2O
3Powder, Lu
2O
3Powder, La
2O
3Powder, Yb
2O
3Powder, Ce
2O
3Powder and Gd
2O
3In the powder one or more.
5. the preparation method of the anti-ablative coating of carbon/carbon composite HfC according to claim 1 is characterized in that, ball grinder described in the step (2) is aluminum oxide ball milling jar or urethane ball grinder.
6. the preparation method of the anti-ablative coating of carbon/carbon composite HfC according to claim 1 is characterized in that, the thickness of coating described in the step (3) is 50 μ m~1500 μ m; Temperature of oven described in the step (3) is 100 ℃~200 ℃.
7. the preparation method of the anti-ablative coating of carbon/carbon composite HfC according to claim 1 is characterized in that, rare gas element described in the step (4) is that quality purity is not less than 99.9% argon gas.
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CN102515850B (en) * | 2011-12-22 | 2013-07-24 | 西北有色金属研究院 | Carbon/carbon composite material ultrahigh temperature oxidation resistant coating and preparation method thereof |
CN102674892B (en) * | 2012-05-31 | 2014-03-19 | 西北有色金属研究院 | Carbon/carbon composite ultrahigh temperature anti-oxidation coating and preparation process thereof |
CN102659452B (en) * | 2012-05-31 | 2014-01-01 | 西北有色金属研究院 | Carbon/carbon composite ultra-high-temperature oxidation-resistant coating layer and preparation method thereof |
CN102730685B (en) * | 2012-07-03 | 2014-04-02 | 西北工业大学 | Method for preparing one-dimensional hafnium carbide nanometer material |
CN105541416B (en) * | 2016-01-18 | 2018-01-12 | 西北工业大学 | A kind of preparation method of C/C composite material surfaces HfC SiC coatings |
CN107021787A (en) * | 2017-05-26 | 2017-08-08 | 广东省新材料研究所 | A kind of preparation method of anti-yaw damper coating |
CN108395279B (en) * | 2018-02-08 | 2021-09-17 | 西北工业大学 | Method for preparing HfC-SiC complex phase gradient coating by chemical vapor codeposition method |
CN109678560B (en) * | 2019-03-08 | 2019-12-10 | 航天特种材料及工艺技术研究所 | High-temperature anti-ablation coating formed on base material and preparation method and application thereof |
CN111116228A (en) * | 2019-11-18 | 2020-05-08 | 中南大学 | Preparation method of ablation-resistant ZrC-HfC/SiC double-layer complex phase ceramic coating |
CN112794734B (en) * | 2021-04-14 | 2021-06-18 | 中国人民解放军国防科技大学 | Multi-metal carbide modified carbon-based material and preparation method thereof |
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