CN109912316A - A kind of preparation method of the nanowire-toughened coating of C/SiC composite material surface - Google Patents
A kind of preparation method of the nanowire-toughened coating of C/SiC composite material surface Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of silicon carbide nanometer line toughening C/SiC composite material surface coating.It is characterized in that the SiC nanowire growth in situ, in C/SiC composite material surface, with certain depth and nano wire gos deep into internal pore structure, and SiC ceramic particles coat forms fine and close coating in SiC nanowire.Carbon fiber establishment part is placed in tube furnace, with CH3SiCl3It (MTS) is raw material, high-purity H2For carrier gas, high-purity Ar gas is diluent gas, prepares fibre reinforced SiC ceramic based composites using CVI；Then one layer of un-densified SiC nanowire is grown in composite material surface using PPCVD method；Finally use discharge plasma sintering technology (SPS) one layer of SiC coating of plating on nano wire.The present invention can reduce the thermal stress of sintering process using nanowire-toughened coating, increase toughness and the hardness of SiC coating to reduce the cracking of coating, improve coating and substrate combinating strength, improve the anti-oxidant ablation property of composite material.
Description
Technical field
The present invention relates to a kind of preparation method of ceramic matric composite surface covering, in particular to a kind of C/SiC is compound
The preparation method of the nanowire-toughened coating of material surface.
Background technique
In recent years, aerospace vehicle is quickly grown, in the environment of high hot-fluid, high pressure draught and high-velocity particles erosion
Under using more and more, material is also put forward higher requirements, under the background of application demand, resistance to high temperature oxidation composite wood
The development of material is also increasingly mature.In high temperature heat structure field, Cf/ SiC ceramic matrix composite material is comprehensive performance than dystectic gold
Belong to, traditional ceramics material better choice.Cf/ SiC ceramic matrix composite material has excellent comprehensive performance, such as low-density, Gao Biqiang
Degree, high ratio modulus, low thermal coefficient of expansion, heat shock resistance, corrosion-resistant and resistance to ablation etc..The high rigidity of SiC, high intensity, heat-resisting punching
It hits, be broken the characteristics such as just property is low, can overcome the disadvantages that the mechanical property defect of carbon fiber makes Cf/ SiC ceramic matrix composite material has the fracture of metal
Characteristic, averting a calamity property is destroyed, and carbon fiber can also make the crack deflection of SiC ceramic, has the effects that inhibit development of defects,
Two kinds of material interactions make Cf/ SiC material has the comprehensive performances such as excellent high-temperature stability, thermal shock resistance, the material
It is widely used in the fields such as aerospace vehicle high temperature basal seat area, Space Optical System and brake material.
Although CfThe comprehensive performance of/SiC ceramic matrix composite material is extremely excellent, but in air in the environment of 400 DEG C of temperature,
C/SiC composite material will start to aoxidize, and after temperature is more than 500 DEG C, the oxidation rate of C/SiC composite material is with temperature
Degree is increased and is quickly improved, thus largely reduced the service performance of the material at relatively high temperatures, seriously restricts its use.
So the antioxygenic property for improving C/SiC composite material under high temperature is of great significance.
The coating for the carbon fibre reinforced composite developed at present is broadly divided into glass coating, refractory metal and alloy and applies
Several big systems such as layer, ceramic coating and composite coating.Such as glass coating { Jiang F, Cheng L, Zhang J, et
al.Fabrication of barium-strontium aluminosilicate coatings on C/SiC
composites via laser cladding[J].Journal of Materials Science&
Technology.2017,33 (2): 166-171 }；Refractory metal and its alloy coat { Yan Z, Xiong X, Xiao P, et
al.Oxidation behavior of oxidation protective coatings for C/C-SiC composites
1500 DEG C of at [J] .Transactions of Nonferrous Metals Society of China.2009,19 (1):
61-64 } in the C for having SiC transition zonefSi-Mo coating is prepared using slurry method in/C- SiC ceramic matrix composite material, but these are applied
Layer is all oxidizable, and coating brittleness is big, melting and processing difficulties；{ Li Hejun, Xue Hui, Fu Qiangang wait .C/C compound to ceramic coating
Material at high temperature antioxidant coating grinds the status and prospects that make internal disorder or usurp [J] Journal of Inorganic Materials .2010,25 (4): 337-343. } it utilizes
In high temperature aerobic environment, silicon-containing compound is reacted with oxygen forms glassy state SiO in matrix surface2, SiO2Packing hole lacks
It falls into, oxygen is hindered to enter, thus effective protection matrix, but ceramic coating also has certain disadvantage, if the anti-thermal shock service life is short,
It easily cracks after multiple thermal cycle.It is mutually tied using growth in situ SiC nanowire toughening and discharge plasma sintering technology
It closes, bond strength and itself and substrate combinating strength, nano wire, which can be improved between SiC particulate, reduces the heat of sintering process
Stress can reduce coating cracking tendency；Improve the anti-oxidant ablation property of composite material.
Summary of the invention
To solve prior art problem, the present invention proposes a kind of system of nanowire-toughened coating of C/SiC composite material surface
Preparation Method, prepare a kind of smooth, high-compactness, high tenacity, anti-oxidant ablation SiC coating, microstructure is to be coated on C/
SiC ceramic particle in the SiC nanowire of SiC ceramic matrix composite material surface.
A kind of preparation method of the nanowire-toughened coating of C/SiC composite material surface, comprising the following steps:
(1) carbon fiber establishment part is subjected to ultrasonic cleaning, is put into 100 DEG C of drying in baking oven, is then placed in tube furnace
In, it will be vacuumized in furnace, be warming up to 950~1050 DEG C with the rate of 5~10 DEG C/min；
(2) it is passed through reaction gas, with CH3SiCl3It (MTS) is raw material, high-purity H2For carrier gas, high-purity Ar gas is carrier gas
Body, the trichloromethyl silane being passed through, hydrogen, argon gas volume ratio be 1: 10: 10, deposit 300~400h, finally with 3~5 DEG C/
The rate of min is cooled to room temperature and obtains fibre reinforced SiC ceramic based composites；
(3) C/SiC composite material is subjected to ultrasonic cleaning, is put into baking oven 100 DEG C of drying, at the same by Polycarbosilane,
Ferrocene and active carbon powder are mixed to form uniform slurry by 1: 0.01: 1 mass ratio, and slurry is then put into ceramic earthenware
In crucible, and the face that C/SiC composite material needs to grow nano wire is placed on crucible；
(4) crucible is integrally put into tube furnace, as shown in Figure 1, by air displacement in boiler tube being high with oil-sealed rotary pump
Pure Ar gas is then warming up to 1200~1400 DEG C in very low Ar gas velocity protection with the speed of 5~10 DEG C/min, and protects
3~5h of temperature, then cooled to room temperature；
(5) step (4) are repeated until all faces of C/SiC composite material all grow SiC nanowire, by Si powder, graphite powder
And Al2O3Sintering aid keeps the temperature 1h under the conditions of 150 DEG C of temperature in an oven, and granularity is all 300 mesh, and Si powder and graphite powder ratio are
(1.1~1.2): 1, and add 5%Al2O3Sintering aid be mixed into ball mill ball milling for 24 hours, sieving, then with C/SiC composite wood
Material is die-filling together, die-filling as shown in Figure 2；
(6) mold is put on discharge plasma sintering machine and is sintered, 1100 DEG C~1400 DEG C of sintering temperature, protected
Warm time 1min, pressure are (25~30) MPa, and vacuum degree is less than 5 × 10-3Pa finally obtains C/SiC composite material surface and receives
Rice noodles toughening coating.
A kind of preparation method of the nanowire-toughened coating of C/SiC composite material surface of the present invention, including it is following the utility model has the advantages that
1. improving the bond strength of coating and matrix using growth in situ silicon carbide nanometer line toughening coating；2. being carbonized
The presence of silicon nanowires can reduce the thermal stress of sintering process, reduce the tendency of coating cracking；3. nanowire-toughened layer is deposited
In the case where that can avoid high temperature, oxygen penetrates SiC particulate gap oxidic matrix；4. discharge plasma sintering technology can be obtained high-densit
Property coating, and the process time is short, simple process, improves the anti-oxidant ablation property of C/SiC composite material.
Detailed description of the invention
Fig. 1 is that the SPS of C/SiC composite material SiC coating is sintered schematic diagram
Fig. 2 is the nanowire-toughened coating schematic diagram of C/SiC composite material surface
Specific embodiment
Combined with specific embodiments below, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the invention, after the present invention has been read, those skilled in the art are to various equivalences of the invention
It is as defined in the appended claims that the modification of form falls within the application.
Embodiment 1:
(1) carbon fiber establishment part is subjected to ultrasonic cleaning, is put into 100 DEG C of drying in baking oven, is then placed in tube furnace
In, it will be vacuumized in furnace, be warming up to 1000 DEG C with the rate of 7 DEG C/min；
(2) it is passed through reaction gas, with CH3SiCl3It (MTS) is raw material, high-purity H2For carrier gas, high-purity Ar gas is carrier gas
Body, the trichloromethyl silane being passed through, hydrogen, argon gas volume ratio are 1: 10: 10,300h are deposited, finally with the rate of 5 DEG C/min
It is cooled to room temperature and obtains fibre reinforced SiC ceramic based composites；
(3) C/SiC composite material is subjected to ultrasonic cleaning, is put into baking oven 100 DEG C of drying, at the same by Polycarbosilane,
Ferrocene and active carbon powder are mixed to form uniform slurry by 1: 0.01: 1 mass ratio, and slurry is then put into ceramic earthenware
In crucible, and the face that C/SiC composite material needs to grow nano wire is placed on crucible；
(4) crucible is integrally put into tube furnace, as shown in Figure 1, by air displacement in boiler tube being high with oil-sealed rotary pump
Pure Ar gas is then warming up to 1250 DEG C in very low Ar gas velocity protection with the speed of 10 DEG C/min, and keeps the temperature 3h, then
Cooled to room temperature；
(5) step (4) are repeated until all faces of C/SiC composite material all grow SiC nanowire, by Si powder, graphite powder
And Al2O3Sintering aid keeps the temperature 1h under the conditions of 150 DEG C of temperature in an oven, and granularity is all 300 mesh, and Si powder and graphite powder ratio are
1.1: 1, and add 5%Al2O3Sintering aid be mixed into ball mill ball milling for 24 hours, sieving, then together with C/SiC composite material
It is die-filling, it is die-filling as shown in Figure 2；
(6) mold is put on discharge plasma sintering machine and is sintered, 1200 DEG C DEG C of sintering temperature, soaking time
1min, pressure 30MPa, vacuum degree is less than 5 × 10-3Pa finally obtains the nanowire-toughened coating of C/SiC composite material surface.
Embodiment 2:
(1) carbon fiber establishment part is subjected to ultrasonic cleaning, is put into 100 DEG C of drying in baking oven, is then placed in tube furnace
In, it will be vacuumized in furnace, be warming up to 1050 DEG C with the rate of 5 DEG C/min；
(2) it is passed through reaction gas, with CH3SiCl3It (MTS) is raw material, high-purity H2For carrier gas, high-purity Ar gas is carrier gas
Body, the trichloromethyl silane being passed through, hydrogen, argon gas volume ratio are 1: 10: 10,400h are deposited, finally with the rate of 4 DEG C/min
It is cooled to room temperature and obtains fibre reinforced SiC ceramic based composites；
(3) C/SiC composite material is subjected to ultrasonic cleaning, is put into baking oven 100 DEG C of drying, at the same by Polycarbosilane,
Ferrocene and active carbon powder are mixed to form uniform slurry by 1: 0.01: 1 mass ratio, and slurry is then put into ceramic earthenware
In crucible, and the face that C/SiC composite material needs to grow nano wire is placed on crucible；
(4) crucible is integrally put into tube furnace, as shown in Figure 1, by air displacement in boiler tube being high with oil-sealed rotary pump
Pure Ar gas is then warming up to 1400 DEG C in very low Ar gas velocity protection with the speed of 8 DEG C/min, and keeps the temperature 5h, then certainly
So it is cooled to room temperature；
(5) step (4) are repeated until all faces of C/SiC composite material all grow SiC nanowire, by Si powder, graphite powder
And Al2O3Sintering aid keeps the temperature 1h under the conditions of 150 DEG C of temperature in an oven, and granularity is all 300 mesh, and Si powder and graphite powder ratio are
1.15: 1, and add 7%Al2O3Sintering aid be mixed into ball mill ball milling for 24 hours, sieving, then together with C/SiC composite material
It is die-filling, it is die-filling as shown in Figure 2；
(6) mold is put on discharge plasma sintering machine and is sintered, 1400 DEG C of sintering temperature, soaking time
1min, pressure 26MPa, vacuum degree is less than 5 × 10-3Pa finally obtains the nanowire-toughened coating of C/SiC composite material surface.
Embodiment 3:
(1) carbon fiber establishment part is subjected to ultrasonic cleaning, is put into 100 DEG C of drying in baking oven, is then placed in tube furnace
In, it will be vacuumized in furnace, the rate of 10 DEG C/min is warming up to 950 DEG C；
(2) it is passed through reaction gas, with CH3SiCl3It (MTS) is raw material, high-purity H2For carrier gas, high-purity Ar gas is carrier gas
Body, the trichloromethyl silane being passed through, hydrogen, argon gas volume ratio are 1: 10: 10,350h are deposited, finally with the rate of 5 DEG C/min
It is cooled to room temperature and obtains fibre reinforced SiC ceramic based composites；
(3) C/SiC composite material is subjected to ultrasonic cleaning, is put into baking oven 100 DEG C of drying, at the same by Polycarbosilane,
Ferrocene and active carbon powder are mixed to form uniform slurry by 1: 0.01: 1 mass ratio, and slurry is then put into ceramic earthenware
In crucible, and the face that C/SiC composite material needs to grow nano wire is placed on crucible；
(4) crucible is integrally put into tube furnace, as shown in Figure 1, by air displacement in boiler tube being high with oil-sealed rotary pump
Pure Ar gas is then warming up to 1300 DEG C in very low Ar gas velocity protection with the speed of 6 DEG C/min, and keeps the temperature 4h, then certainly
So it is cooled to room temperature；
(5) step (4) are repeated until all faces of C/SiC composite material all grow SiC nanowire, by Si powder, graphite powder
And Al2O3Sintering aid keeps the temperature 1h under the conditions of 150 DEG C of temperature in an oven, and granularity is all 300 mesh, and Si powder and graphite powder ratio are
1.2: 1, and add 5%Al2O3Sintering aid be mixed into ball mill ball milling for 24 hours, sieving, then together with C/SiC composite material
It is die-filling, it is die-filling as shown in Figure 2；
(6) mold is put on discharge plasma sintering machine and is sintered, 1350 DEG C of sintering temperature, soaking time
1min, pressure 28MPa, vacuum degree is less than 5 × 10-3Pa finally obtains the nanowire-toughened coating of C/SiC composite material surface.
Claims (2)
1. a kind of preparation method of the nanowire-toughened coating of C/SiC composite material surface, which is characterized in that the SiC nanometer
Line growth in situ is in C/SiC composite material surface, and with certain depth and nano wire gos deep into internal pore structure, SiC ceramic
Particles coat forms fine and close coating in SiC nanowire；It can be obtained using nanowire-toughened with discharge plasma sintering technology
To smooth, fine and close high rigidity, high tenacity, anti-oxidant SiC coating.
2. the preparation method of the nanowire-toughened coating of C/SiC composite material surface according to claim 1, feature exist
In, comprising the following steps:
(1) carbon fiber establishment part is subjected to ultrasonic cleaning, is put into 100 DEG C of drying in baking oven, is then placed in tube furnace, by furnace
It inside vacuumizes, is warming up to 950~1050 DEG C with the rate of 5~10 DEG C/min；
(2) it is passed through reaction gas, with CH3SiCl3It (MTS) is raw material, high-purity H2 is carrier gas, and high-purity Ar gas is diluent gas, is passed through
Trichloromethyl silane, hydrogen, argon gas volume ratio be 1: 10: 10, deposit 300~400h, finally with the rate of 3~5 DEG C/min
It is cooled to room temperature and obtains fibre reinforced SiC ceramic based composites；
(3) C/SiC composite material is subjected to ultrasonic cleaning, is put into baking oven 100 DEG C of drying, while by Polycarbosilane, two cyclopentadienyls
Iron and active carbon powder are mixed to form uniform slurry by 1: 0.01: 1 mass ratio, and then slurry is put into ceramic crucible,
And the face that C/SiC composite material needs to grow nano wire is placed on crucible；
(4) crucible is integrally put into tube furnace, as shown in Figure 1, by air displacement in boiler tube being high-purity Ar with oil-sealed rotary pump
Gas is then warming up to 1200~1400 DEG C in very low Ar gas velocity protection with the speed of 5~10 DEG C/min, and keep the temperature 3~
5h, then cooled to room temperature；
(5) repeat step (4) until all faces of C/SiC composite material all grow SiC nanowire, by Si powder, graphite powder and
Al2O3Sintering aid keeps the temperature 1h under the conditions of 150 DEG C of temperature in an oven, and granularity is all 300 mesh, and Si powder and graphite powder ratio are
(1.1~1.2): 1, and add 5%Al2O3Sintering aid be mixed into ball mill ball milling for 24 hours, sieving, then with C/SiC composite wood
Material is die-filling together, die-filling as shown in Figure 2；
(6) mold is put on discharge plasma sintering machine and is sintered, 1100 DEG C~1400 DEG C of sintering temperature, soaking time
1min, pressure are (25~30) MPa, and vacuum degree is less than 5 × 10-3It is nanowire-toughened to finally obtain C/SiC composite material surface by Pa
Coating.
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| CN111573678A (en) * | 2020-05-14 | 2020-08-25 | 湖南太子新材料科技有限公司 | Silicon carbide film forming device and preparation method of silicon carbide film |
| CN112030544A (en) * | 2020-08-31 | 2020-12-04 | 北京航空航天大学 | Method for in-situ growth of silicon carbide nanowires on surface of silicon carbide fiber |
| CN114249590A (en) * | 2021-12-21 | 2022-03-29 | 深圳市元亨高新科技高分子材料开发有限公司 | High-strength high-temperature-resistant fireproof heat-insulating material |
| CN114455964A (en) * | 2021-12-30 | 2022-05-10 | 西安超码科技有限公司 | C/SiC composite material crucible containing alumina coating |
| CN114455965A (en) * | 2021-12-30 | 2022-05-10 | 西安超码科技有限公司 | Containing alpha-Al2O3Coated C/SiC composite crucible |
| CN114455981A (en) * | 2021-12-30 | 2022-05-10 | 西安超码科技有限公司 | Containing alpha-Al2O3Coated medium density C/C-SiC composite crucible |
| CN115611660A (en) * | 2022-10-12 | 2023-01-17 | 南京工程学院 | C/C composite material surface 1600-DEG C wind tunnel gas scouring resistant coating and preparation method and application thereof |
| CN116535238A (en) * | 2023-04-27 | 2023-08-04 | 西北工业大学 | Radial SiC nanowire grown on surface of one-dimensional micro-nano silicon-based ceramic substrate in situ and preparation method |
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| CN111253159A (en) * | 2020-01-19 | 2020-06-09 | 中国科学院上海硅酸盐研究所 | Ordered and disordered SiC nanowire/whisker structure and preparation method thereof |
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| CN114249590B (en) * | 2021-12-21 | 2022-07-08 | 深圳市元亨高新科技高分子材料开发有限公司 | High-strength high-temperature-resistant fireproof heat-insulating material |
| CN114455965A (en) * | 2021-12-30 | 2022-05-10 | 西安超码科技有限公司 | Containing alpha-Al2O3Coated C/SiC composite crucible |
| CN114455981A (en) * | 2021-12-30 | 2022-05-10 | 西安超码科技有限公司 | Containing alpha-Al2O3Coated medium density C/C-SiC composite crucible |
| CN114455964A (en) * | 2021-12-30 | 2022-05-10 | 西安超码科技有限公司 | C/SiC composite material crucible containing alumina coating |
| CN114455964B (en) * | 2021-12-30 | 2023-09-05 | 西安超码科技有限公司 | C/SiC composite material crucible containing alumina coating |
| CN114455965B (en) * | 2021-12-30 | 2023-09-05 | 西安超码科技有限公司 | A composition containing alpha-Al 2 O 3 Coated C/SiC composite crucible |
| CN114455981B (en) * | 2021-12-30 | 2023-09-05 | 西安超码科技有限公司 | A composition containing alpha-Al 2 O 3 Medium-density C/C-SiC composite material crucible of coating |
| CN115611660A (en) * | 2022-10-12 | 2023-01-17 | 南京工程学院 | C/C composite material surface 1600-DEG C wind tunnel gas scouring resistant coating and preparation method and application thereof |
| CN116535238A (en) * | 2023-04-27 | 2023-08-04 | 西北工业大学 | Radial SiC nanowire grown on surface of one-dimensional micro-nano silicon-based ceramic substrate in situ and preparation method |
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Application publication date: 20190621 |