CN112899650B - 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 PDFInfo
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- CN112899650B CN112899650B CN202110052656.8A CN202110052656A CN112899650B CN 112899650 B CN112899650 B CN 112899650B CN 202110052656 A CN202110052656 A CN 202110052656A CN 112899650 B CN112899650 B CN 112899650B
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- 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
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- 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
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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) Under argonProtecting glove box, preparing and containing TaCl 5 、HfCl 4 And ZrCl 4 Mixing 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 temperatures of a low-temperature zone and a high-temperature zone; (4) Introduction of H 2 、CH 4 And the mixed gas after complete gasification is deposited under normal pressure; (5) After deposition is complete, H is turned off 2 、CH 4， And cooling the deposition furnace and the double-temperature-zone gasification furnace to take out the sample. The preparation method can accurately control the proportion of the reaction sources, can ensure tight and firm combination with the base material and excellent stability, and is suitable for ultra-high temperature protection of graphite, carbon-carbon composite materials and the like.
Description
The application is a divisional application with the application number of 201910242863.2 and the invention name of 'a preparation method of 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, adding TaCl 5 、HfCl 4 And ZrCl 4 Mixing the powder, and filling the powder into an alumina crucible; wherein TaCl 5 、HfCl 4 And ZrCl 4 Prepared according to the mass percent 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; then heating the deposition furnace at the heating rate of 5-20 ℃/min to reach the deposition temperature of 1300 ℃;
(3) Will contain TaCl 5 、HfCl 4 And ZrCl 4 The crucible of the mixed powder is put on a lifting bracket of a low-temperature area in a double-temperature area gasification furnace, and the lifting bracket is liftedCommunicating the opening part of the crucible with a high-temperature area, setting the heating temperature of a low-temperature area (gasification area) in a dual-temperature-area gasification furnace to be 320 ℃, setting the heating temperature of a high-temperature area (mixing area) to be 550 ℃, and heating to completely gasify the mixed powder;
(4) H with the flow rate of 500ml/min is introduced into the deposition furnace 2 CH with a flow rate of 100ml/min 4 Introducing 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 TaCl 5 、HfCl 4 And ZrCl 4 The 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 off 2 、CH 4 And 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 furnace temperature 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 an atmosphere condition and a temperature in the preparation process, the accurate stoichiometric ratio of each component in the prepared (Ta, hf, zr) C composite coating is realized, the accurate control of the reaction source proportion is the key for preparing the high-performance (Ta, hf, zr) C composite coating, and the close and firm combination of the coating and the base material and the excellent stability are also ensured.
The preparation method of the (Ta, hf, zr) C composite coating with excellent stability is characterized by sequentially comprising the following steps of:
(1) Adding TaCl 5 、HfCl 4 And ZrCl 4 Mixing the powders, placing in an alumina crucible under nitrogen or argon protection, wherein TaCl is added 5 、HfCl 4 And ZrCl 4 Prepared according to the mass percentage of 55 to 75 percent, 20 to 35 percent and 5 to 10 percent respectively;
(2) Placing a matrix sample on a bracket of a deposition furnace, and introducing argon with the flow of 100-800 ml/min into the deposition furnace for not less than 30min so as to remove air in the furnace; then heating the deposition furnace at the heating rate of 5-20 ℃/min to reach the deposition temperature of 1200-1600 ℃;
(3) Will contain TaCl 5 、HfCl 4 And ZrCl 4 Placing 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 210-450 ℃, the heating temperature of the high-temperature area to be 550-700 ℃, and heating to enable the mixed powder to be completely gasified;
(4) H with the flow rate of 500 ml/min-1200 ml/min is introduced into the deposition furnace 2 CH with flow rate of 100 ml/min-500 ml/min 4 Introducing argon with the flow rate of 50-1000 ml/min as a carrier gas into the bottom of the high-temperature region in the dual-temperature region gasification furnace, and completely gasifying the obtained TaCl 5 、HfCl 4 And ZrCl 4 The 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 off 2 、CH 4 And 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 that all mixed powder is completely gasified into gas state by combining a specific powder feeding mode and setting the conditions such as the atmosphere condition, the temperature and the like in the preparation process, ensures that the proportion of a gas reaction source 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 source 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 diagram showing the structure of a CVD system used in the method for producing a (Ta, hf, zr) C composite coating having excellent 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 below with reference to examples, without thereby restricting the invention to the described examples.
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, adding TaCl 5 、HfCl 4 And ZrCl 4 Mixing the powder, and filling the powder into an alumina crucible; wherein TaCl 5 、HfCl 4 And ZrCl 4 Prepared according to the mass percent of 55 percent, 35 percent and 10 percent respectively;
(2) Placing a matrix sample on a bracket of a deposition furnace, and introducing argon with the flow of 200ml/min into the deposition furnace for 30min to remove air in the furnace; then heating the deposition furnace at the heating rate of 5-20 ℃/min to reach the deposition temperature of 1300 ℃;
(3) Will contain TaCl 5 、HfCl 4 And ZrCl 4 Placing 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 the mixed powder is completely gasified;
(4) H with the flow rate of 500ml/min is introduced into the deposition furnace 2 CH with a flow rate of 100ml/min 4 Introducing argon with the flow rate of 180ml/min as a carrier gas into the bottom of the high-temperature region in the dual-temperature region gasification furnace, and completely gasifying the obtained TaCl 5 、HfCl 4 And ZrCl 4 The 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 off 2 、CH 4 And 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 according 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 prepared in this example is shown in FIG. 2.
Example 2
A method for preparing a (Ta, hf, zr) C composite coating having excellent stability, comprising the following steps in sequence, wherein the chemical vapor deposition system used has the same structure as in example 1:
(1) In an argon protective glove box, taCl is added 5 、HfCl 4 And ZrCl 4 Mixing the powders, and placing into an alumina crucible(ii) a Wherein TaCl 5 、HfCl 4 And ZrCl 4 Prepared according to the mass percentages of 75 percent, 20 percent and 5 percent respectively;
(2) Placing a matrix sample on a bracket of a deposition furnace, and introducing argon with the flow of 200ml/min into the deposition furnace for 30min to remove air in the furnace; then heating the deposition furnace at the heating rate of 5-20 ℃/min to reach the deposition temperature of 1400 ℃;
(3) Will contain TaCl 5 、HfCl 4 And ZrCl 4 Placing 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 the mixed powder is completely gasified;
(4) H with the flow rate of 800ml/min is introduced into the deposition furnace 2 CH with a flow rate of 200ml/min 4 Introducing 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 TaCl 5 、HfCl 4 And ZrCl 4 Introducing the mixed gas into a deposition furnace, and depositing for 3 hours under the normal pressure condition;
(5) After the coating deposition is complete, H is turned off 2 、CH 4 And 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 furnace temperature 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 30s of ablation, the coating structure is complete and has no cracking or falling-off phenomenon by adopting a plasma ablation test method with reference 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, the argon protective glove box is provided with a gas inlet pipe and a gas outlet pipeTaCl 5 、HfCl 4 And ZrCl 4 Mixing the powder, and filling the powder into an alumina crucible; wherein TaCl 5 、HfCl 4 And ZrCl 4 Prepared according to the mass percent 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; then heating the deposition furnace at the heating rate of 5-20 ℃/min to reach the deposition temperature of 1400 ℃;
(3) Will contain TaCl 5 、HfCl 4 And ZrCl 4 Placing the crucible of the mixed powder on a lifting support of a low-temperature area in a double-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 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 double-temperature-area gasification furnace to be 450 ℃, the heating temperature of the high-temperature area (mixing area) to be 650 ℃, and heating to completely gasify the mixed powder;
(4) H with the flow rate of 100ml/min is introduced into the deposition furnace 2 CH with a flow rate of 250ml/min 4 Introducing 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 TaCl 5 、HfCl 4 And ZrCl 4 The 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 off 2 、CH 4 And 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 furnace temperature 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 according 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 added 5 、HfCl 4 And ZrCl 4 Mixing the powder, and filling the powder into an alumina crucible; wherein TaCl 5 、HfCl 4 And ZrCl 4 Prepared according to the mass percentage of 55 percent, 35 percent and 10 percent respectively;
(2) Placing a matrix sample on a bracket of a deposition furnace, and introducing argon with the flow of 200ml/min into the deposition furnace for 30min to remove air in the furnace; then heating the deposition furnace at the heating rate of 5-20 ℃/min to reach the deposition temperature of 1300 ℃;
(3) Will contain TaCl 5 、HfCl 4 And ZrCl 4 Placing 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 furnace 2 CH with a flow rate of 100ml/min 4 Introducing 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 TaCl 5 、HfCl 4 And ZrCl 4 The 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 off 2 、CH 4 And 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 ℃.
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| BR7007802D0 (en) * | 1970-11-25 | 1973-02-20 | Sandvikens Jernverks Ab | PROCESS TO COVER SYNTHESIZED HARD METAL BODIES |
| JPS52147508A (en) * | 1976-06-02 | 1977-12-08 | Sumitomo Electric Ind Ltd | Multiple coating super hard alloy parts |
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| US5238711A (en) * | 1990-11-05 | 1993-08-24 | The President And Fellows Of Harvard College | Method of coating carbon fibers with a carbide |
| JP3584593B2 (en) * | 1996-02-19 | 2004-11-04 | 富士電機ホールディングス株式会社 | Carbide manufacturing method |
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| US7666474B2 (en) * | 2008-05-07 | 2010-02-23 | Asm America, Inc. | Plasma-enhanced pulsed deposition of metal carbide films |
| CN101791883B (en) * | 2009-12-21 | 2012-07-11 | 中南大学 | Surface erosion-resistant composite coating of carbon/carbon composite, preparation method and application thereof |
| CN102557703B (en) * | 2011-11-07 | 2013-10-09 | 中南大学 | Method for preparing double-gradient carbide modified C/C composite material |
| FR2983192B1 (en) * | 2011-11-25 | 2014-05-23 | Commissariat Energie Atomique | METHOD FOR COATING A COATING OF A COATING AGAINST OXIDATION BY A CHEMICAL VAPOR DEPOSITION TECHNIQUE, AND COATING AND ROOM |
| CN102815971B (en) * | 2012-08-22 | 2013-08-21 | 中南大学 | Hf (Ta) C ultra-high-temperature composite coating and preparation method thereof |
| CN103757603B (en) * | 2014-01-07 | 2016-03-09 | 哈尔滨工业大学 | A kind of preparation method of zirconium diboride coating |
| CN103834929B (en) * | 2014-03-13 | 2016-03-23 | 中国兵器工业第五九研究所 | A kind of carbide coating containing hafnium and preparation method thereof |
| KR101535573B1 (en) * | 2014-11-04 | 2015-07-13 | 연세대학교 산학협력단 | Method for synthesis of transition metal chalcogenide |
| CN104775103B (en) * | 2015-03-31 | 2017-07-07 | 中国人民解放军国防科学技术大学 | The preparation method of ZrC coatings |
| CN106478120B (en) * | 2016-09-09 | 2019-11-05 | 西北工业大学 | A kind of preparation method of the modified C/C composite material of binary ceramic |
| CN106699233B (en) * | 2016-11-23 | 2020-08-25 | 中南大学 | Composite coating containing chemical vapor codeposition zirconium boride/hafnium-tantalum boride and preparation method thereof |
| CN109320303B (en) * | 2018-10-31 | 2021-03-30 | 中国兵器工业第五九研究所 | Ultrahigh-temperature oxidation-resistant ablation-resistant layer and preparation method thereof |
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