CN112899650A - Preparation method of (Ta, Hf, Zr) C composite coating with excellent stability - Google Patents

Preparation method of (Ta, Hf, Zr) C composite coating with excellent stability Download PDF

Info

Publication number
CN112899650A
CN112899650A CN202110052656.8A CN202110052656A CN112899650A CN 112899650 A CN112899650 A CN 112899650A CN 202110052656 A CN202110052656 A CN 202110052656A CN 112899650 A CN112899650 A CN 112899650A
Authority
CN
China
Prior art keywords
temperature
furnace
deposition
heating
tacl
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202110052656.8A
Other languages
Chinese (zh)
Other versions
CN112899650B (en
Inventor
李忠盛
吴护林
丛大龙
何庆兵
陈大军
赵子鹏
田武强
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
No 59 Research Institute of China Ordnance Industry
Original Assignee
No 59 Research Institute of China Ordnance Industry
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by No 59 Research Institute of China Ordnance Industry filed Critical No 59 Research Institute of China Ordnance Industry
Priority to CN202110052656.8A priority Critical patent/CN112899650B/en
Publication of CN112899650A publication Critical patent/CN112899650A/en
Application granted granted Critical
Publication of CN112899650B publication Critical patent/CN112899650B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/32—Carbides

Abstract

The invention relates to a preparation method of a (Ta, Hf, Zr) C composite coating with excellent stability, which sequentially comprises the following steps: (1) in an argon protective glove box, TaCl is prepared and contained5、HfCl4And ZrCl4Mixing the powder; (2) putting the matrix sample in a deposition furnace, removing air, and then heating; (3) putting the mixed powder into a double-temperature-zone gasification furnace, and setting the heating temperature of a low-temperature zone and a high-temperature zone; (4) introduction of H2、CH4And the mixed gas after complete gasification is deposited under normal pressure; (5) after deposition is complete, H is turned off2、CH4，And cooling the deposition furnace and the dual-temperature-zone gasification furnace to take out the sample. The preparation method can accurately control the proportion of the reaction source, can ensure tight and firm combination with the matrix material and excellent stability, and is suitable for ultra-high temperature protection of graphite, carbon-carbon composite materials and the like.

Description

Preparation method of (Ta, Hf, Zr) C composite coating with excellent stability
The application is a divisional application with the application number of 201910242863.2 and the name of 'a method for preparing a multi-component composite carbide coating'.
Technical Field
The invention relates to surface ultra-high temperature protection of materials such as C/C composite materials and graphite, in particular to a preparation method of a (Ta, Hf, Zr) C composite coating with excellent stability.
Background
At present, the carbide coating is widely prepared on the surface of the C/C composite material at home and abroad to improve the high-temperature ablation resistance of the C/C composite material. For example, single coatings such as SiC, TaC, HfC and the like are prepared, the coatings have better high-temperature resistance, and various high-temperature resistant coating materials have different advantages, but are suitable for being used at the high temperature below 2000 ℃; and preparing (Ta, Hf) C, (Hf, Zr) C and other multiphase coatings, and is suitable for high temperature below 3000 ℃. The multiphase coating can enable all phase components in the coating to play a synergistic effect through reasonable component design, and effectively improve the service temperature of the C/C composite material. As an important means for preparing the complex phase coating, the chemical vapor deposition technology has the advantages of strong designability, high coating purity, controllable reaction atmosphere, simple operation and the like. At present, three-component and above composite coatings are prepared by a chemical vapor deposition method, the ablation resistance and the protection capability of the coatings are further improved, and the method becomes a research hotspot of ultrahigh-temperature ceramic coatings.
Disclosure of Invention
The invention aims to provide a preparation method of a (Ta, Hf, Zr) C composite coating with excellent stability, which can accurately control the proportion of reaction sources, can ensure tight and firm combination with a base material and excellent stability, and is suitable for ultra-high temperature protection of graphite, carbon-carbon composite materials and the like.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a (Ta, Hf, Zr) C composite coating with excellent stability is characterized by sequentially comprising the following steps:
(1) in an argon protective glove box, TaCl is added5、HfCl4And ZrCl4Mixing the powder, and filling the powder into an alumina crucible; wherein TaCl5、HfCl4And ZrCl4Prepared according to the mass percentage of 55 percent, 35 percent and 10 percent respectively;
(2) placing the matrix sample on a bracket of a deposition furnace, and introducing argon with the flow rate of 200ml/min into the deposition furnace for 30min to remove air in the furnace; heating the deposition furnace at the heating rate of 5-20 ℃/min to reach the deposition temperature of 1300 ℃;
(3) will contain TaCl5、HfCl4And ZrCl4Placing the crucible of the mixed powder on a lifting support of a low-temperature area in a dual-temperature area gasification furnace, lifting the lifting support to enable the opening of the crucible to be communicated with a high-temperature area, setting the heating temperature of the low-temperature area (gasification area) in the dual-temperature area gasification furnace to be 320 ℃, setting the heating temperature of the high-temperature area (mixing area) to be 550 ℃, and heating to enable the mixed powder to be completely gasified;
(4) h with the flow rate of 500ml/min is introduced into the deposition furnace2CH with a flow rate of 100ml/min4Introducing argon with the flow rate of 180ml/min as carrier gas into the bottom of the high-temperature region in the dual-temperature-region gasification furnace, and completely gasifying to obtain TaCl5、HfCl4And ZrCl4The mixed gas is introduced into a deposition furnace, and the deposition time is 2 hours under the normal pressure condition;
(5) after the coating deposition is complete, H is turned off2、CH4And closing the heating power supplies of the deposition furnace and the dual-temperature-zone gasification furnace under the protection of argon, and taking out the sample when the temperature of the furnace is reduced to be below 200 ℃.
The inventor has found through long-term repeated tests that when the chemical vapor deposition method is adopted to prepare the (Ta, Hf, Zr) C composite coating in the existing method, the powder feeding mode mainly comprises mechanical powder feeding (namely, directly feeding powder into a deposition furnace to perform vapor deposition reaction) and independent gasification powder feeding (namely, each powder raw material is independently gasified in a respective gasification furnace and then fed into the deposition furnace to be mixed and deposited). The powder feeding modes cause that the amount of each raw material powder actually participating in the reaction is not accurate, the proportion of each raw material powder in the obtained mixed raw material powder is not consistent with the proportion of an original design, the obtained mixed raw material powder is not uniformly mixed, and the high temperature resistance of the prepared solid solution coating is influenced by various conditions such as atmosphere conditions, temperature and the like in the preparation process. According to the invention, by combining a specific powder feeding mode and setting conditions such as atmosphere conditions and temperature in the preparation process, accurate stoichiometric ratio of each component in the prepared (Ta, Hf, Zr) C composite coating is realized, accurate control of the proportion of the reaction source is the key for preparing the high-performance (Ta, Hf, Zr) C composite coating, and tight and firm combination of the coating and the base material and excellent stability are ensured.
A preparation method of a (Ta, Hf, Zr) C composite coating with excellent stability is characterized by sequentially comprising the following steps:
(1) adding TaCl5、HfCl4And ZrCl4Mixing the powders, loading into an alumina crucible under nitrogen or argon protection, wherein TaCl is added5、HfCl4And ZrCl4Prepared according to the mass percentage of 55 to 75 percent, 20 to 35 percent and 5 to 10 percent respectively;
(2) placing a substrate sample on a bracket of a deposition furnace, and introducing argon with the flow rate of 100 ml/min-800 ml/min into the deposition furnace for not less than 30min so as to remove air in the furnace; heating the deposition furnace at the heating rate of 5-20 ℃/min to reach the deposition temperature of 1200-1600 ℃;
(3) will contain TaCl5、HfCl4And ZrCl4Placing the crucible of the mixed powder on a lifting support of a low-temperature area in a dual-temperature area gasification furnace, lifting the lifting support to communicate the opening of the crucible with a high-temperature area, setting the heating temperature of the low-temperature area in the dual-temperature area gasification furnace to be 210-450 ℃, the heating temperature of the high-temperature area to be 550-700 ℃, and addingThe mixed powder is completely gasified by heat;
(4) h with the flow rate of 500 ml/min-1200 ml/min is introduced into the deposition furnace2CH with flow rate of 100 ml/min-500 ml/min4Introducing argon with the flow rate of 50-1000 ml/min as carrier gas into the bottom of the high-temperature region in the dual-temperature-region gasification furnace, and completely gasifying to obtain TaCl5、HfCl4And ZrCl4The mixed gas is introduced into a deposition furnace, and the (Ta, Hf, Zr) C composite coating is prepared by deposition under the normal pressure condition, the deposition time is 1-50 h, namely the (Ta, Hf, Zr) C composite coating with the coating thickness of 10-500 mu m is prepared;
(5) after the coating deposition is complete, H is turned off2、CH4And closing the deposition furnace and the double-temperature-zone gasification furnace under the protection of argon, and taking out the sample when the furnace temperature is reduced to be below 200 ℃.
The invention has the following beneficial effects:
the invention provides a preparation method of a (Ta, Hf, Zr) C composite coating with excellent stability. The preparation method realizes the complete gasification of all mixed powder into gaseous state by combining a specific powder feeding mode and setting conditions such as atmosphere conditions, temperature and the like in the preparation process, ensures that the proportion of gaseous reaction sources entering a deposition furnace is the same as the proportion (namely the design proportion) in the powder state, solves the problem of accurate deposition of the reaction sources according to the design proportion, ensures that the stoichiometric ratio of each component in the prepared (Ta, Hf, Zr) C composite coating is accurate, and also ensures that the coating is tightly and firmly combined with a base material and has excellent stability. By adopting the method, the prepared C/C composite material deposited with the (Ta, Hf, Zr) C composite coating meets the use requirement in an ultrahigh temperature environment of more than 3500 ℃, has excellent ultrahigh temperature ablation resistance, has a complete structure of the (Ta, Hf, Zr) C composite coating after being ablated for 38s in a plasma ablation test, has no cracking and falling phenomena, is tightly and firmly combined with the C/C composite material, has excellent stability, and is suitable for ultrahigh temperature protection of graphite, carbon-carbon composite materials and the like.
Drawings
FIG. 1 is a schematic structural view of a chemical vapor deposition system used in a method for producing a (Ta, Hf, Zr) C composite coating layer excellent in stability according to example 1 of the present invention.
FIG. 2 is a cross-sectional structure of a base sample on which a (Ta, Hf, Zr) C composite coating layer was deposited, which was prepared in example 1 of the present invention.
Detailed Description
The invention is further described in the following examples, which are not intended to limit the invention thereto.
Example 1
A preparation method of a (Ta, Hf, Zr) C composite coating with excellent stability sequentially comprises the following steps, wherein the specific structure of a chemical vapor deposition system is shown in the attached figure 1:
(1) in an argon protective glove box, TaCl is added5、HfCl4And ZrCl4Mixing the powder, and filling the powder into an alumina crucible; wherein TaCl5、HfCl4And ZrCl4Prepared according to the mass percentage of 55 percent, 35 percent and 10 percent respectively;
(2) placing the matrix sample on a bracket of a deposition furnace, and introducing argon with the flow rate of 200ml/min into the deposition furnace for 30min to remove air in the furnace; heating the deposition furnace at the heating rate of 5-20 ℃/min to reach the deposition temperature of 1300 ℃;
(3) will contain TaCl5、HfCl4And ZrCl4Placing the crucible of the mixed powder on a lifting support of a low-temperature area in a dual-temperature-area gasification furnace, lifting the lifting support to ensure that the opening part of the crucible is matched and communicated with a conical channel opening on the bottom of a heat insulation layer positioned between the low-temperature area and a high-temperature area, namely, the opening part of the crucible is communicated with the high-temperature area, setting the heating temperature of the low-temperature area (gasification area) in the dual-temperature-area gasification furnace to be 320 ℃, the heating temperature of the high-temperature area (mixing area) to be 550 ℃, and heating to ensure that;
(4) h with the flow rate of 500ml/min is introduced into the deposition furnace2CH with a flow rate of 100ml/min4Introducing argon with the flow rate of 180ml/min as carrier gas into the bottom of the high-temperature region in the dual-temperature-region gasification furnace, and completely gasifying to obtain TaCl5、HfCl4And ZrCl4The mixed gas is introduced into a deposition furnace, and the deposition time is 2 hours under the normal pressure condition;
(5) after the coating deposition is complete, H is turned off2、CH4And closing the heating power supplies of the deposition furnace and the dual-temperature-zone gasification furnace under the protection of argon, and taking out the sample when the temperature of the furnace is reduced to be below 200 ℃.
The bonding strength of the (Ta, Hf and Zr) C composite coating obtained in the example is 12.3MPa, the plasma ablation test method is adopted by referring to GJB323A-96, and after the coating is ablated for 20s, the coating structure is complete and has no cracking and falling phenomena. The cross-sectional structure of the substrate sample deposited with the (Ta, Hf, Zr) C composite coating layer prepared in this example is shown in FIG. 2.
Example 2
A method for preparing a (Ta, Hf, Zr) C composite coating layer having excellent stability, comprising the following steps in order, wherein the structure of the chemical vapor deposition system used is the same as that of example 1:
(1) in an argon protective glove box, TaCl is added5、HfCl4And ZrCl4Mixing the powder, and filling the powder into an alumina crucible; wherein TaCl5、HfCl4And ZrCl4Prepared according to the mass percentages of 75 percent, 20 percent and 5 percent respectively;
(2) placing the matrix sample on a bracket of a deposition furnace, and introducing argon with the flow rate of 200ml/min into the deposition furnace for 30min to remove air in the furnace; heating the deposition furnace at the temperature rise rate of 5-20 ℃/min to reach the deposition temperature of 1400 ℃;
(3) will contain TaCl5、HfCl4And ZrCl4Placing the crucible of the mixed powder on a lifting support of a low-temperature area in a dual-temperature-area gasification furnace, lifting the lifting support to ensure that the opening part of the crucible is matched and communicated with a conical passage opening on the bottom of a heat insulation layer positioned between the low-temperature area and a high-temperature area, namely, the opening part of the crucible is communicated with the high-temperature area, setting the heating temperature of the low-temperature area (gasification area) in the dual-temperature-area gasification furnace to be 400 ℃, the heating temperature of the high-temperature area (mixing area) to be 600 ℃, and heating to ensure that;
(4) h with the flow rate of 800ml/min is introduced into the deposition furnace2CH with a flow rate of 200ml/min4Introducing argon with the flow rate of 300ml/min as carrier gas into the bottom of the high-temperature region in the dual-temperature-region gasification furnace, and completely gasifying to obtain TaCl5、HfCl4And ZrCl4The mixed gas is introduced into a deposition furnace, and the deposition time is 3 hours under the normal pressure condition;
(5) after the coating deposition is complete, H is turned off2、CH4And closing the heating power supplies of the deposition furnace and the dual-temperature-zone gasification furnace under the protection of argon, and taking out the sample when the temperature of the furnace is reduced to be below 200 ℃.
The bonding strength of the (Ta, Hf, Zr) C composite coating obtained in the embodiment is 11.5MPa, and after 30 seconds of ablation, the coating structure is complete and has no cracking or falling-off phenomenon by adopting a plasma ablation test method according to GJB 323A-96.
Example 3
A method for preparing a (Ta, Hf, Zr) C composite coating layer having excellent stability, comprising the following steps in order, wherein the structure of the chemical vapor deposition system used is the same as that of example 1:
(1) in an argon protective glove box, TaCl is added5、HfCl4And ZrCl4Mixing the powder, and filling the powder into an alumina crucible; wherein TaCl5、HfCl4And ZrCl4Prepared according to the mass percentage of 60 percent, 30 percent and 10 percent respectively;
(2) placing the matrix sample on a bracket of a deposition furnace, and introducing argon with the flow rate of 200ml/min into the deposition furnace for 30min to remove air in the furnace; heating the deposition furnace at the temperature rise rate of 5-20 ℃/min to reach the deposition temperature of 1400 ℃;
(3) will contain TaCl5、HfCl4And ZrCl4Placing the crucible of the mixed powder on a lifting support of a low-temperature area in a dual-temperature-area gasification furnace, lifting the lifting support to ensure that the opening part of the crucible is matched and communicated with a conical passage opening on the bottom of a heat insulation layer positioned between the low-temperature area and a high-temperature area, namely, the opening part of the crucible is communicated with the high-temperature area, setting the heating temperature of the low-temperature area (gasification area) in the dual-temperature-area gasification furnace to be 450 ℃, the heating temperature of the high-temperature area (mixing area) to be 650 ℃, and heating to ensure that;
(4) introducing into the deposition furnaceH with a flow rate of 100ml/min2CH with a flow rate of 250ml/min4Introducing argon with the flow rate of 420ml/min as carrier gas into the bottom of the high-temperature region in the dual-temperature-region gasification furnace, and completely gasifying to obtain TaCl5、HfCl4And ZrCl4The mixed gas is introduced into a deposition furnace, and the deposition time is 4 hours under the normal pressure condition;
(5) after the coating deposition is complete, H is turned off2、CH4And closing the heating power supplies of the deposition furnace and the dual-temperature-zone gasification furnace under the protection of argon, and taking out the sample when the temperature of the furnace is reduced to be below 200 ℃.
The bonding strength of the (Ta, Hf, Zr) C composite coating obtained in the embodiment is 10.7MPa, a plasma ablation test method is adopted by referring to GJB323A-96, and after the coating is ablated for 38s, the coating is complete in structure and free of cracking and falling phenomena.

Claims (1)

1. A preparation method of a (Ta, Hf, Zr) C composite coating with excellent stability is characterized by sequentially comprising the following steps:
(1) in an argon protective glove box, TaCl is added5、HfCl4And ZrCl4Mixing the powder, and filling the powder into an alumina crucible; wherein TaCl5、HfCl4And ZrCl4Prepared according to the mass percentage of 55 percent, 35 percent and 10 percent respectively;
(2) placing the matrix sample on a bracket of a deposition furnace, and introducing argon with the flow rate of 200ml/min into the deposition furnace for 30min to remove air in the furnace; heating the deposition furnace at the heating rate of 5-20 ℃/min to reach the deposition temperature of 1300 ℃;
(3) will contain TaCl5、HfCl4And ZrCl4Placing the crucible of the mixed powder on a lifting support of a low-temperature area in a dual-temperature area gasification furnace, lifting the lifting support to enable the opening of the crucible to be communicated with a high-temperature area, setting the heating temperature of the low-temperature area in the dual-temperature area gasification furnace to be 320 ℃, setting the heating temperature of the high-temperature area to be 550 ℃, and heating to enable the mixed powder to be completely gasified;
(4) h with the flow rate of 500ml/min is introduced into the deposition furnace2CH with a flow rate of 100ml/min4And in a dual-temperature zone gasification furnaceArgon with the flow rate of 180ml/min is introduced into the bottom of the high-temperature zone to be used as carrier gas, and TaCl obtained after complete gasification is obtained5、HfCl4And ZrCl4The mixed gas is introduced into a deposition furnace, and the deposition time is 2 hours under the normal pressure condition;
(5) after the coating deposition is complete, H is turned off2、CH4And closing the heating power supplies of the deposition furnace and the dual-temperature-zone gasification furnace under the protection of argon, and taking out the sample when the temperature of the furnace is reduced to be below 200 ℃.
CN202110052656.8A 2019-03-28 2019-03-28 Preparation method of (Ta, hf, zr) C composite coating with excellent stability Active CN112899650B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110052656.8A CN112899650B (en) 2019-03-28 2019-03-28 Preparation method of (Ta, hf, zr) C composite coating with excellent stability

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201910242863.2A CN109972120B (en) 2019-03-28 2019-03-28 Preparation method of multi-element composite carbide coating
CN202110052656.8A CN112899650B (en) 2019-03-28 2019-03-28 Preparation method of (Ta, hf, zr) C composite coating with excellent stability

Related Parent Applications (1)

Application Number Title Priority Date Filing Date
CN201910242863.2A Division CN109972120B (en) 2019-03-28 2019-03-28 Preparation method of multi-element composite carbide coating

Publications (2)

Publication Number Publication Date
CN112899650A true CN112899650A (en) 2021-06-04
CN112899650B CN112899650B (en) 2023-02-03

Family

ID=67081205

Family Applications (2)

Application Number Title Priority Date Filing Date
CN201910242863.2A Active CN109972120B (en) 2019-03-28 2019-03-28 Preparation method of multi-element composite carbide coating
CN202110052656.8A Active CN112899650B (en) 2019-03-28 2019-03-28 Preparation method of (Ta, hf, zr) C composite coating with excellent stability

Family Applications Before (1)

Application Number Title Priority Date Filing Date
CN201910242863.2A Active CN109972120B (en) 2019-03-28 2019-03-28 Preparation method of multi-element composite carbide coating

Country Status (1)

Country Link
CN (2) CN109972120B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113684471A (en) * 2021-08-02 2021-11-23 江苏鎏溪光学科技有限公司 System and method for monitoring reaction atmosphere in chemical vapor deposition process
CN113860917A (en) * 2021-10-09 2021-12-31 航天特种材料及工艺技术研究所 Ablation-resistant ceramic matrix composite and preparation method thereof

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113235066A (en) * 2021-05-19 2021-08-10 重庆大学 Organic platinum group metal chemical vapor deposition device and method

Citations (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1321525A (en) * 1970-11-25 1973-06-27 Sandco Ltd Method of coating sintered hard metal bodies with surface layer of carbide
JPS52147508A (en) * 1976-06-02 1977-12-08 Sumitomo Electric Ind Ltd Multiple coating super hard alloy parts
US4269899A (en) * 1979-05-22 1981-05-26 Hitachi Metals, Ltd. Surface hafnium-titanium carbide coated hard alloy and method
US5238711A (en) * 1990-11-05 1993-08-24 The President And Fellows Of Harvard College Method of coating carbon fibers with a carbide
JPH09228031A (en) * 1996-02-19 1997-09-02 Fuji Electric Co Ltd Production of carbide
CN101791883A (en) * 2009-12-21 2010-08-04 中南大学 Surface erosion-resistant composite coating of carbon/carbon composite, preparation method and application thereof
CN102557703A (en) * 2011-11-07 2012-07-11 中南大学 Method for preparing double-gradient carbide modified C/C composite material
CN102815971A (en) * 2012-08-22 2012-12-12 中南大学 Hf (Ta) C ultra-high-temperature composite coating and preparation method thereof
CN103757603A (en) * 2014-01-07 2014-04-30 哈尔滨工业大学 Method for preparing zirconium diboride coating
CN103834929A (en) * 2014-03-13 2014-06-04 中国兵器工业第五九研究所 Carbide coating containing hafnium and preparation method of carbide coating
US20140287249A1 (en) * 2011-11-25 2014-09-25 Commissariat A L'energie Atomique Et Aux Energies Alternatives Method for coating, using a chemical vapour deposition technique, a part with a coating for protecting against oxidation, and coating and part
CN104775103A (en) * 2015-03-31 2015-07-15 中国人民解放军国防科学技术大学 Method for preparing ZrC coating
CN106478120A (en) * 2016-09-09 2017-03-08 西北工业大学 A kind of preparation method of binary ceramic modification C/C composite
CN106699233A (en) * 2016-11-23 2017-05-24 中南大学 Composite coatings containing chemical vapor codeposition ZrB2/Hf-TaB2 and preparation method of composite coatings
CN109320303A (en) * 2018-10-31 2019-02-12 中国兵器工业第五九研究所 Anti-oxidant ablative-resistant layer of superhigh temperature and preparation method thereof

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101153384B (en) * 2006-09-28 2010-11-10 中南大学 Method for manufacturing unit doublet carbide codeposition fibre-reinforced composite
US7666474B2 (en) * 2008-05-07 2010-02-23 Asm America, Inc. Plasma-enhanced pulsed deposition of metal carbide films
KR101535573B1 (en) * 2014-11-04 2015-07-13 연세대학교 산학협력단 Method for synthesis of transition metal chalcogenide

Patent Citations (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1321525A (en) * 1970-11-25 1973-06-27 Sandco Ltd Method of coating sintered hard metal bodies with surface layer of carbide
JPS52147508A (en) * 1976-06-02 1977-12-08 Sumitomo Electric Ind Ltd Multiple coating super hard alloy parts
US4269899A (en) * 1979-05-22 1981-05-26 Hitachi Metals, Ltd. Surface hafnium-titanium carbide coated hard alloy and method
US5238711A (en) * 1990-11-05 1993-08-24 The President And Fellows Of Harvard College Method of coating carbon fibers with a carbide
JPH09228031A (en) * 1996-02-19 1997-09-02 Fuji Electric Co Ltd Production of carbide
CN101791883A (en) * 2009-12-21 2010-08-04 中南大学 Surface erosion-resistant composite coating of carbon/carbon composite, preparation method and application thereof
CN102557703A (en) * 2011-11-07 2012-07-11 中南大学 Method for preparing double-gradient carbide modified C/C composite material
US20140287249A1 (en) * 2011-11-25 2014-09-25 Commissariat A L'energie Atomique Et Aux Energies Alternatives Method for coating, using a chemical vapour deposition technique, a part with a coating for protecting against oxidation, and coating and part
CN102815971A (en) * 2012-08-22 2012-12-12 中南大学 Hf (Ta) C ultra-high-temperature composite coating and preparation method thereof
CN103757603A (en) * 2014-01-07 2014-04-30 哈尔滨工业大学 Method for preparing zirconium diboride coating
CN103834929A (en) * 2014-03-13 2014-06-04 中国兵器工业第五九研究所 Carbide coating containing hafnium and preparation method of carbide coating
CN104775103A (en) * 2015-03-31 2015-07-15 中国人民解放军国防科学技术大学 Method for preparing ZrC coating
CN106478120A (en) * 2016-09-09 2017-03-08 西北工业大学 A kind of preparation method of binary ceramic modification C/C composite
CN106699233A (en) * 2016-11-23 2017-05-24 中南大学 Composite coatings containing chemical vapor codeposition ZrB2/Hf-TaB2 and preparation method of composite coatings
CN109320303A (en) * 2018-10-31 2019-02-12 中国兵器工业第五九研究所 Anti-oxidant ablative-resistant layer of superhigh temperature and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
JUNHENG XING等: "Facile one-step high-temperature spray pyrolysis route toward metal carbide nanopowders", 《JOURNAL OF THE AMERICAN CERAMIC SOCIETY》 *
宋永忠等: "CVD法制备ZrC涂层与ZrC-TaC共沉积涂层的烧蚀性能", 《粉末冶金材料科学与工程》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113684471A (en) * 2021-08-02 2021-11-23 江苏鎏溪光学科技有限公司 System and method for monitoring reaction atmosphere in chemical vapor deposition process
CN113860917A (en) * 2021-10-09 2021-12-31 航天特种材料及工艺技术研究所 Ablation-resistant ceramic matrix composite and preparation method thereof
CN113860917B (en) * 2021-10-09 2022-11-25 航天特种材料及工艺技术研究所 Ablation-resistant ceramic matrix composite and preparation method thereof

Also Published As

Publication number Publication date
CN112899650B (en) 2023-02-03
CN109972120B (en) 2020-12-01
CN109972120A (en) 2019-07-05

Similar Documents

Publication Publication Date Title
CN112899650B (en) Preparation method of (Ta, hf, zr) C composite coating with excellent stability
CN106699233B (en) Composite coating containing chemical vapor codeposition zirconium boride/hafnium-tantalum boride and preparation method thereof
CN107814591B (en) Preparation method of boride modified silicon-based antioxidant coating on surface of carbon material
CN103409732B (en) A kind of compounding method of diamond surface metallization
CN101445392B (en) Graphite matrix flawless TaC coating and manufacturing method thereof
CN109354506B (en) High-temperature antioxidant carbon-ceramic composite material and preparation method thereof
CN106977223B (en) Ceramic modified C/C composite material with ceramic coating and preparation method thereof
US9085493B2 (en) Process for production of silicon-carbide-coated carbon base material, silicon-carbide-coated carbon base material, sintered (silicon carbide)-carbon complex, ceramic-coated sintered (silicon carbide)-carbon complex, and process for production of sintered (silicon carbide)-carbon complex
CN109970460A (en) A kind of fibre reinforced (carbon -) is silicon carbide-based-ultra-temperature ceramic-based composite material and preparation method thereof
CN110862264A (en) Continuous silicon carbide fiber reinforced silicon carbide ceramic matrix composite material and preparation method and application thereof
CN110963799B (en) Preparation method of liquid-phase silicon-assisted forming thermal protection Z-pins silicide ceramic rod structure
CN109320303B (en) Ultrahigh-temperature oxidation-resistant ablation-resistant layer and preparation method thereof
Ren et al. Influences of deposition temperature, gas flow rate and ZrC content on the microstructure and anti-ablation performance of CVD-HfC-ZrC coating
CN105218102B (en) A kind of method that precursor process prepares SiC/TiC composite ceramics
CN115180981B (en) Nano-wire cross-scale toughening complex-phase ceramic antioxidant coating and preparation method and application thereof
Gu et al. New anti-ablation candidate for carbon/carbon composites: preparation, composition and ablation behavior of Y2Hf2O7 coating under an oxyacetylene torch
CN104451886A (en) Preparation method of composite seed tray for growing A1N single crystals by PVT method
CN101791883A (en) Surface erosion-resistant composite coating of carbon/carbon composite, preparation method and application thereof
CN110723973A (en) Preparation method of SiBCN composite ceramic with high temperature stability
Gai et al. HfB2 coating on C/C composites prepared by chemical vapor deposition: Thermodynamics and experimental investigation
CN109748595B (en) Mixed permeating agent, application and reaction infiltration preparation method
CN105236988B (en) A kind of high-purity high-density recrystallized silicon carbide device and preparation method thereof
EP2933353B1 (en) Method for producing fiber-reinforced composites
CN114908322B (en) Ablation-resistant three-dimensional inlaid ceramic coating and preparation method thereof
CN108218475B (en) Preparation method of boride solid solution modified silicon-based coating on carbon material surface

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant