CN115650754B - SiC coating with dispersed particles on surface of carbon material for strengthening and toughening and preparation method thereof - Google Patents
SiC coating with dispersed particles on surface of carbon material for strengthening and toughening and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a SiC coating with dispersed particles on the surface of a carbon material for strengthening and toughening and a preparation method thereof, wherein Al, si, C, B powder is used for preparing the SiC coating by adopting an embedding method. The SiC coating and the matrix have high bonding strength and compact coating, a large number of particles are dispersed on the surface of the coating, the dispersed particles can play a role in toughening, the problems of incompact, easy cracking and easy falling of the SiC coating in the traditional embedding method can be effectively solved, and the service life of the coating is prolonged. After the prepared dispersion particle toughened SiC coating is subjected to thermal shock for 10 times in static air at 1500 ℃, the mass loss percentage is only 0.49%, meanwhile, the oxidation curve is more gentle, and the oxidation mass loss rate is lower. The percentage of mass loss of the SiC coating which is not toughened by the dispersed particles is as high as 1.50% after 10 times of thermal shock in static air at 1500 ℃, and meanwhile, the oxidation curve is steeper, and the oxidation mass loss rate is higher. It can be seen that the thermal shock resistance of the dispersion particle strengthened SiC coating is remarkably improved.
Description
Technical Field
The invention belongs to the technical field of materials, and relates to a SiC coating with dispersed particles on the surface of a carbon material for strengthening and toughening and a preparation method thereof.
Background
As a thermal structure material, the carbon material has the advantages of small specific gravity, good chemical stability, small thermal expansion coefficient, good thermal shock resistance, ablation resistance and the like, and is widely applied to the fields of metallurgy, machinery, chemical industry, aerospace and the like.
However, to fully exploit the above advantages, it is necessary to ensure that the carbon material is used in an oxygen-free environment, which greatly limits its range of application as a thermostructural material.
In order to solve the problem of high-temperature and easy oxidation of carbon materials, researchers at home and abroad propose a large number of solutions, wherein the preparation of an anti-oxidation coating on the surface of the carbon materials is an effective method. The SiC coating has small thermal expansion coefficient, and the oxidation product is SiO with better oxidation resistance 2 The glass film and the carbon material have good physical and chemical compatibility, and are ideal antioxidation coating of the carbon material.
However, the coefficient of thermal expansion of SiC coatings is still about 4 times that of carbon materials(α SiC ＝4.5×10 -6 K -1 ，α C ＝1.0×10 -6 K -1 ) The mismatch of the thermal expansion coefficients can generate huge thermal stress in the coating during the cooling process of embedding and preparing the SiC coating and in the high-temperature oxidation environment, so that a large number of microcracks are generated in the SiC coating, and the microcracks can be taken as channels for oxidation diffusion to enter the coating to reach a carbon matrix in the high-temperature oxidation environment, so that the service life of the coating is seriously reduced.
In order to solve the problem of cracks in the SiC coating, researchers at home and abroad have made a great deal of researches, wherein the toughening technology is widely used for relieving the problem.
Document one "J.F.Huang, X.R.Zeng, H.J.Li, X.B.Xiong, Y.W.Fu, influence of the preparation temperature on the phase, microstructure and anti-oxidation property of a SiC coating for C/C compositions, carbon 42 (8-9) (2004) 1517-1521," reports an Al prepared by a conventional embedding process 2 O 3 Modified SiC coating. Although the SiC coating is successfully prepared on the surface of the C/C composite material by the technology, the surface of the coating has a plurality of pores, is not compact, has poor toughness and is easy to crack.
Document two, "T.Li, Y.Zhang, J.Zhang, Y.Fu, J.Li, improved antioxidative and mechanical properties of SiC coated C/C composites via a SiO 2 SiC reticulated layer, J.Eur.Ceram.Soc.41 (13) (2021) 6151-6159.) reports that a slurry brushing method is combined with heat treatment and embedding method is used to prepare SiO with SiC nanowires 2 -SiC network toughened SiC coating. The technology firstly prepares SiO with SiC nanowires on the surface of a C/C composite material by a slurry brushing method in combination with heat treatment 2 The SiC reticular structure layer is filled with the reticular structure by adopting an embedding method, and finally the SiO with the SiC nanowire is prepared 2 -SiC network toughened SiC coating. Although the method can effectively toughen the SiC coating and reduce the cracking trend of the coating, an external process is needed to prepare a toughening phase in advance, the process is complex, and the prepared toughening phase can generate particle sintering growth in the subsequent high-temperature sintering process of preparing the coating, so that the method finally really plays a role inThe toughened SiC nanowire has little residue and limited toughening effect.
The three patent CN 105541412A reports a preparation method of a SiC nanowire toughened SiC ceramic coating on the surface of a C/C composite material, wherein the SiC nanowire and the SiC coating are sequentially prepared at 2 different set temperature stages by adopting a chemical vapor deposition process, and finally the SiC nanowire toughened SiC coating with a sandwich structure is prepared in situ by a one-step CVD method. Although the method reduces the cracking trend of the SiC coating, the method has high requirements on equipment, the preparation process is complex, the period is long, and the cost is high.
Document four, "CN 106083206A" reports a method for preparing a SiC inner coating of carbon/carbon composite material, which patent uses SiO 2 The SiC inner coating is prepared by taking Si and C powder as raw materials and adopting an embedding process at 1200-1400 ℃, and the surface of the coating is provided with SiC nanowires and has a network porous structure. According to the method, although the SiC coating is toughened by the SiC nanowire, the cracking tendency of the SiC coating is reduced, the coating is not compact, and the SiC coating has a network porous structure.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a SiC coating with strengthened dispersed particles on the surface of a carbon material and a preparation method thereof, wherein the SiC coating with strengthened dispersed particles is prepared by adopting an embedding method in one step. The invention has the advantages of simple process, low equipment requirement, short preparation period, low cost and safe and controllable preparation process. Meanwhile, the prepared SiC coating has high bonding strength with the matrix, the coating is compact, the surface of the coating macroscopically shows the appearance of molten particles, compared with the SiC coating which is not strengthened and toughened by dispersed particles, the microstructure of the coating is obviously thinned, and microcracks caused by the difference of the thermal expansion coefficients of the SiC coating and the carbon matrix are hardly seen. In addition, a large number of grain boundaries and a large number of grains (average grain diameter is 2.2 mu m) distributed in a dispersing way in the grain boundaries are observed on the surface of the molten coating, the dispersing grains formed in situ on the grain boundaries can play a role in toughening, play a role in pinning phases in the crack propagation process, fully absorb the energy of crack tips, effectively inhibit the unstable propagation of cracks, effectively solve the problems of incompact, easy cracking and easy falling of the SiC coating by the traditional embedding method, and prolong the service life of the coating.
Technical proposal
A SiC coating with strengthened and toughened carbon material surface dispersion particles is characterized in that the surface of the coating macroscopically presents the appearance of molten particles, and the surface of the molten coating has the SiC particles which are dispersed and distributed, have strengthening and toughening effects and play a role of pinning phases in the crack propagation process; after the SiC coating is subjected to thermal shock in static air at 1500 ℃ for 10 times, the mass loss percentage of the SiC coating is only 0.49%.
The average particle diameter of the SiC particles was 2.2. Mu.m.
A method for preparing a SiC coating reinforced by dispersed particles on the surface of a carbon material, which is characterized by comprising the following steps:
step 1: preparing mixed powder, wherein the components are mixed powder with the mass fraction of 1-8% of Al, 50-70% of Si, 10-30% of C and 5-20% of B
Step 2: embedding a carbon material matrix into the mixed powder of a graphite crucible, then placing the graphite crucible in an argon atmosphere to react for 1-3h at 1700-1900 ℃, and preparing a SiC coating on the surface of the carbon material matrix;
the surface of the SiC coating macroscopically presents the appearance of molten particles, and the surface of the molten coating also has pinning phase functions in the crack propagation process, which are distributed in a diffusion way in a grain boundary, so that the energy of the crack tip is fully absorbed, and the unstable and expanded SiC particles of the crack are effectively restrained.
The surface of the carbon material matrix is subjected to polishing treatment before the mixed powder embedded in the graphite crucible.
The carbon material matrix is a graphite material or a C/C composite material.
Advantageous effects
According to the SiC coating and the preparation method for strengthening and toughening the dispersed particles on the surface of the carbon material, the carbon material is used as a matrix sample, the sample is ground and polished, al, si, C, B powder with a certain mass fraction is added, and the SiC coating is prepared by an embedding method. The invention has the advantages of simple process, low equipment requirement, short preparation period, low cost and safe and controllable preparation process. Meanwhile, the prepared SiC coating has high bonding strength with the matrix, the coating is compact, a large number of particles are dispersed on the surface of the coating, the dispersed particles formed in situ can play a role in toughening, the problems of incompact, easy cracking and easy falling of the SiC coating in the traditional embedding method can be effectively solved, and the service life of the coating is prolonged. After the prepared dispersion particle toughened SiC coating is subjected to thermal shock for 10 times in static air at 1500 ℃, the mass loss percentage is only 0.49%, meanwhile, the oxidation curve is more gentle, and the oxidation mass loss rate is lower. The percentage of mass loss of the SiC coating which is not toughened by the dispersed particles is as high as 1.50% after 10 times of thermal shock in static air at 1500 ℃, and meanwhile, the oxidation curve is steeper, and the oxidation mass loss rate is higher. It can be seen that the thermal shock resistance of the dispersion particle strengthened SiC coating is remarkably improved.
Drawings
FIG. 1 is an XRD spectrum of a dispersed particle-toughened SiC coating prepared in example 2 of the invention;
FIG. 2 is an SEM topography of a non-dispersed particle-toughened SiC coating prepared according to comparative example 1;
FIG. 3 is an SEM morphology of a dispersed particle-toughened SiC coating prepared according to example 2 of the invention: (a) Is a low-magnification SEM morphology, and (b) is a partially enlarged SEM morphology.
FIG. 4 is a thermal shock weight loss curve in static air at 1500℃for the dispersion particle-toughened SiC coating prepared in example 2 of the present invention and the non-dispersion particle-toughened SiC coating prepared in comparative example 1.
Detailed Description
The invention will now be further described with reference to examples, figures:
example 1
A preparation method of a SiC coating with dispersed particles on the surface of a carbon material for strengthening and toughening comprises the following steps:
1) C/C composite material is selected as a matrix, 60-mesh SiC sand paper is adopted for polishing treatment, and 400-mesh SiC sand paper is adopted for polishing treatment to obtain a sample;
2) Embedding the sample obtained in the step 1) in the mixed powder of the graphite crucible (mass fraction of the mixed powder: 5% of Al, 60% of Si, 20% of C and 15% of B), and then placing the graphite crucible in an argon atmosphere to react for 3 hours at 1700 ℃ to prepare the SiC coating on the surface of the sample.
Example 2
A preparation method of a SiC coating with dispersed particles on the surface of a carbon material for strengthening and toughening comprises the following steps:
1) Selecting a graphite material as a matrix, firstly adopting 80-mesh SiC abrasive paper for polishing, and then adopting 600-mesh SiC abrasive paper for polishing to obtain a sample;
2) Embedding the sample obtained in the step 1) in the mixed powder of the graphite crucible (mass fraction of the mixed powder: 2% of Al, 63% of Si, 30% of C and 5% of B), and then placing the graphite crucible in an argon atmosphere to react for 2 hours at 1900 ℃ to prepare the SiC coating on the surface of the sample.
Example 3
A preparation method of a SiC coating with dispersed particles on the surface of a carbon material for strengthening and toughening comprises the following steps:
1) Selecting a graphite material as a matrix, firstly adopting 100-mesh SiC abrasive paper for polishing, and then adopting 600-mesh SiC abrasive paper for polishing to obtain a sample;
2) Embedding the sample obtained in the step 1) in the mixed powder of the graphite crucible (mass fraction of the mixed powder: 5% of Al, 55% of Si, 25% of C and 15% of B), and then placing the graphite crucible in an argon atmosphere to react for 2 hours at 1800 ℃ to prepare the SiC coating on the surface of the sample.
Comparative example 1
A preparation method of a SiC coating with no dispersed particle strengthening and toughening on the surface of a carbon material comprises the following steps:
1) Selecting a graphite material as a matrix, firstly adopting 60-mesh SiC abrasive paper for polishing, and then adopting 600-mesh SiC abrasive paper for polishing to obtain a sample;
2) Embedding the sample obtained in the step 1) in the mixed powder of the graphite crucible (mass fraction of the mixed powder: 5% Al, 62.5% Si, 30% C, 2.5% B), and then the graphite crucible was placed in an argon atmosphere and reacted at 1850℃for 2 hours to prepare a SiC coating on the sample surface.
Experimental results and analysis
As can be seen from fig. 1, the SiC coating is prepared according to the present invention. As can be seen from fig. 2 and 3, the SiC coating strengthened and toughened by the non-dispersed particles is not compact, the microstructure of the coating is coarse, the surface of the coating has a plurality of pores and microcracks, and the coating has poor toughness and is easy to crack. The SiC coating toughened by the dispersion particles prepared by the invention is compact, the surface of the coating macroscopically shows the morphology of molten particles, the microstructure of the coating is obviously refined, and microcracks caused by the difference of the thermal expansion coefficients of the SiC coating and a carbon matrix are hardly seen. In addition, a large number of grain boundaries and a large number of particles (average grain diameter is 2.2 mu m) distributed in a dispersing way in the grain boundaries are observed on the surface of the molten coating, the dispersing particles formed in situ in the grain boundaries can play a role in toughening, play a role in pinning phases in the crack propagation process, fully absorb the energy of crack tips, effectively inhibit the unstable propagation of cracks, effectively solve the problems of incompact, easy cracking and easy falling of the SiC coating by the traditional embedding method, and prolong the service life of the coating.
As can be seen from FIG. 4, the mass loss percentage of the prepared dispersion particle toughened SiC coating is only 0.49% after 10 times of thermal shock in static air at 1500 ℃, and the oxidation curve is more gentle, so that the oxidation mass loss rate is lower (see the curve of the dot series connection in FIG. 4). After the SiC coating without dispersion particle strengthening and toughening is subjected to thermal shock for 10 times in static air at 1500 ℃, the mass loss percentage of the SiC coating reaches 1.50%, meanwhile, the oxidation curve is steeper, and the oxidation mass loss rate is higher. Therefore, the thermal shock resistance of the SiC coating strengthened by the dispersed particles is remarkably improved.
Claims (4)
1. A preparation method of a SiC coating with dispersed particles strengthening and toughening on the surface of a carbon material is characterized in that the surface of the coating macroscopically presents the appearance of molten particles, and the surface of the molten coating has dispersed SiC particles which have strengthening and toughening effects and play a role of pinning phases in the crack propagation process; after the SiC coating is subjected to thermal shock in 1500 ℃ static air for 10 times, the mass loss percentage of the SiC coating is only 0.49%; the preparation method comprises the following steps:
step 1: preparing mixed powder, wherein the components of the mixed powder comprise, by mass, 1-8% of Al, 50-70% of Si, 10-30% of C and 5-20% of B;
step 2: embedding a carbon material matrix into the mixed powder of a graphite crucible, then placing the graphite crucible in an argon atmosphere to react for 1-3h at 1700-1900 ℃, and preparing a SiC coating on the surface of the carbon material matrix;
the surface of the SiC coating macroscopically presents the appearance of molten particles, and the surface of the molten coating also has pinning phase functions in the crack propagation process, which are distributed in a diffusion way in a grain boundary, so that the energy of the crack tip is fully absorbed, and the unstable and expanded SiC particles of the crack are effectively restrained.
2. The method for preparing a SiC coating reinforced by dispersed particles on a surface of a carbon material according to claim 1, wherein: the surface of the carbon material matrix is subjected to polishing treatment before the mixed powder embedded in the graphite crucible.
3. The method for preparing a SiC coating reinforced by dispersed particles on a surface of a carbon material according to claim 1, wherein: the carbon material matrix is a graphite material or a C/C composite material.
4. The method for preparing a SiC coating reinforced by dispersed particles on a surface of a carbon material according to claim 1, wherein: the average particle diameter of the SiC particles was 2.2. Mu.m.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5952100A (en) * | 1997-05-21 | 1999-09-14 | General Electric Company | Silicon-doped boron nitride coated fibers in silicon melt infiltrated composites |
| CN115180981A (en) * | 2022-05-12 | 2022-10-14 | 湖北瑞宇空天高新技术有限公司 | Nano-wire cross-scale toughening complex-phase ceramic antioxidant coating and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5952100A (en) * | 1997-05-21 | 1999-09-14 | General Electric Company | Silicon-doped boron nitride coated fibers in silicon melt infiltrated composites |
| CN115180981A (en) * | 2022-05-12 | 2022-10-14 | 湖北瑞宇空天高新技术有限公司 | Nano-wire cross-scale toughening complex-phase ceramic antioxidant coating and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
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| 料浆法制备碳/碳复合材料Al-Si合金抗氧化涂层;黄敏;李克智;王宇;;热加工工艺(18);第94-96页 * |
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