CN102924106B - A kind of preparation method of carbon-silicon carbide composite material - Google Patents
A kind of preparation method of carbon-silicon carbide composite material Download PDFInfo
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- CN102924106B CN102924106B CN201210488169.7A CN201210488169A CN102924106B CN 102924106 B CN102924106 B CN 102924106B CN 201210488169 A CN201210488169 A CN 201210488169A CN 102924106 B CN102924106 B CN 102924106B
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 27
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 title abstract description 4
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 47
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 32
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000004917 carbon fiber Substances 0.000 claims abstract description 27
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000011268 mixed slurry Substances 0.000 claims abstract description 10
- 239000006229 carbon black Substances 0.000 claims abstract description 7
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 7
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 7
- 239000004744 fabric Substances 0.000 claims abstract description 4
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 4
- 239000010703 silicon Substances 0.000 claims abstract description 4
- 239000011159 matrix material Substances 0.000 claims description 24
- 239000000835 fiber Substances 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 235000019241 carbon black Nutrition 0.000 claims description 6
- 229920003987 resole Polymers 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 238000005137 deposition process Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 12
- 239000000919 ceramic Substances 0.000 abstract description 8
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 abstract 1
- 239000005011 phenolic resin Substances 0.000 abstract 1
- 229920001568 phenolic resin Polymers 0.000 abstract 1
- 239000002002 slurry Substances 0.000 abstract 1
- 238000009941 weaving Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 8
- 238000005229 chemical vapour deposition Methods 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000009413 insulation Methods 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000011204 carbon fibre-reinforced silicon carbide Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920002430 Fibre-reinforced plastic Polymers 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000011151 fibre-reinforced plastic Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
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- Ceramic Products (AREA)
Abstract
本发明公开一种碳-碳化硅陶瓷复合材料的制备方法及根据该方法所制备的产品，制备步骤包括：首先将碳纤维编织成三维立体织物（下面称为碳纤维预制体）；采用气相沉积技术在碳纤维预制体上沉积一层厚度0.1~2μm的单质硅；将酚醛树脂、炭黑、乙醇、超细碳化硅粉末、聚乙烯吡咯烷酮和四甲基氢氧化铵按比例配制成混合浆料；将浆料在真空环境下加压浸渍到上述碳纤维预制体中得到复合材料坯体；将上述坯体加热固化；将固化后的坯体放在真空炉中，进行高温渗硅反应，得到高致密度、高性能的碳-碳化硅陶瓷复合材料。The invention discloses a method for preparing a carbon-silicon carbide ceramic composite material and a product prepared according to the method. The preparation steps include: first weaving carbon fibers into a three-dimensional fabric (hereinafter referred to as a carbon fiber prefabricated body); A layer of elemental silicon with a thickness of 0.1-2 μm is deposited on the carbon fiber prefabricated body; phenolic resin, carbon black, ethanol, ultrafine silicon carbide powder, polyvinylpyrrolidone and tetramethylammonium hydroxide are prepared in proportion to make a mixed slurry; the slurry The material is pressurized and impregnated into the above-mentioned carbon fiber prefabricated body in a vacuum environment to obtain a composite material body; the above-mentioned green body is heated and solidified; High performance carbon-silicon carbide ceramic composite.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, relate to the preparation technology of matrix material, especially a kind of preparation method of carbon fibre reinforced silicon carbide ceramic composite.
Background technology
In silicon carbide ceramics, add continuous carbon fibre, prepare carbon fibre reinforced silicon carbide (C
f/ SiC) matrix material, carbon fiber the mechanism such as extracts by crack deflection, fiber in ceramic breaking-down process, can strengthen intensity and the toughness of stupalith.
Existing C
fthe preparation technology of/SiC matrix material mainly contains: chemical vapour deposition (CVI) technique, precursor infiltration and pyrolysis (PIP) technique, mud dipping hot pressing (SIHP) technique, liquid impregnation (LSI) technique etc.
The technological process of CVI is that carbon fiber preform is placed in to CVI stove, and reactant gases is delivered to preform backward its internal divergence around by the directed flow being produced by pressure difference, at fiber surface generation chemical reaction in-situ deposition.CVI technique is prepared C
fthe major advantage of/SiC matrix material be can be at the temperature far below body material fusing point synthesize ceramic matrix, reduce the fibre property that the high-temperature chemical reaction between fiber and matrix brings and decline; The integrity that can also keep fibre preforms body structure in preparation process, realizes near-net-shape and prepares complex-shaped goods.But it is very long that CVI technique also exists preparation cycle, along gas diffusion path, there is larger density difference, the defects such as the remaining a large amount of void content of matrix material.
SIHP technological process is that SiC powder, sintering aid powder and organic binder bond etc. are made to mud by solvent, and carbon fiber is spun into non-woven fabrics, the molded rear hot pressed sintering of slice module after mud dipping.The densification of material mainly completes by liquid-phase sintering process.The C manufacturing by SIHP method
f/ SiC matrix material density is higher, and defect is less, is comparatively applicable to preparing unidirectional composite material.But SIHP method has larger difficulty to preparation complex shaped components, and carbon fiber tends to and SiC matrix generation surface reaction under High Temperature High Pressure, cause fibre property to decline, be unfavorable for improving the performance of material.
PIP legal system is for C
fthe conventional process of/SiC matrix material is to adopt organic precursor liquid solution impregnation of carbon fibers preform under certain temperature and pressure, after crosslinking curing, carries out Pintsch process under protection of inert gas, makes precursor be converted into SiC ceramic matrix.The preparation temperature of PIP method is low, can with no pressurely burn till, less to the machinery of fiber and chemical damage, and can prepare the member of large complicated shape.But the shortcoming of this kind of technique also clearly, and material densification needs several dipping-lytic cycles, and the production cycle is longer; And owing to can produce small molecule by-product in Pintsch process process, from matrix, overflow, the porosity of resulting materials is higher, has more difficultly prepared fully dense material; Easily there is the chemical reaction of certain form in precursor and fiber, on the one hand fiber is badly damaged in cracking process, forms on the other hand the interfacial layer of strong combination, causes material toughness not high.
LSI technique comprises three primary processes: first prefabricated carbon fiber part is put into airtight mould, adopt high pressure stamp or resin transfer mold technique to prepare fiber reinforced polymer materials; Then cracking in high temperature inert environment, obtains low density carbon based composites (C
f/ C); Finally adopt melt Si under vacuum by the wicking action processing of infiltrating, Si melt is reacted with carbon base body and generates SiC matrix.This technique can be by adjusting C
fthe volume density of/C and porosity are controlled the density of final matrix material.The preparation cycle of LSI technique is short, cost is low, residual porosity rate is low, can prepare dead size, complex-shaped workpiece; But this technique is Shortcomings also: melt Si, when reacting with carbon base body, inevitably can react with carbon fiber, and fiber is etched and causes degradation.
The present invention has overcome above-mentioned defect.
Summary of the invention
The object of the invention is to overcome the deficiency of above-mentioned prior art, the advantages of three kinds of techniques such as LSI, CVI and PIP is got up, provide a kind of and can either improve C
fthe problem that/SiC matrix material density is low, also can effectively hinder the preparation technology of Si to the erosion action of carbon fiber.
Technical scheme of the present invention is achieved by following processing step:
1) by diameter, be that the carbon fiber knit of 6 ~ 8 μ m becomes three dimension stereo fabric, obtain carbon fabric perform;
2) in vacuum tightness, be 1 * 10
-2~ 5 * 10
-3in the vacuum oven of Pa, at the carbon fiber surface vapour deposition layer of metal silicon of carbon fabric perform;
3) ultra fine silicon carbide powder, carbon black, resol, polyvinylpyrrolidone, Tetramethylammonium hydroxide and ethanol are mixed with to mixed slurry in following ratio after ball milling: 63 ~ 72 parts of silicon carbide powders, 5 ~ 6 parts of carbon blacks, 1.5 ~ 2 parts, resol, 0.5 ~ 1.0 part of Tetramethylammonium hydroxide, 0.1 ~ 0.5 part of polyvinylpyrrolidone, 40 ~ 45 parts of alcohol;
4) carbon fabric perform is positioned in graphite jig, under subatmospheric environment, mixed slurry is applied to the pressure of 0.1 ~ 2.0 MPa, its impregnating by pressure is obtained to composite body in above-mentioned carbon fabric perform;
5) above-mentioned composite body and mould are incubated to 2 hours together under 100 ℃ of temperature condition and carry out baking and curing processing;
6) by above-mentioned, carried out base substrate that baking and curing processes and mould to be placed on together vacuum tightness be 1 * 10
-2~ 1 * 10
-3in the vacuum oven of Pa, be warming up to 1450 ~ 1550 ℃ and carry out high temperature siliconising reaction, make carbon fiber reinforced silicon carbide matrix composite.
With respect to prior art, the present invention has the following advantages:
1. preparation technology provided by the invention carries out at lower temperature, can significantly reduce the damage of reaction process to carbon fiber;
2. with respect to existing technology of preparing, the preparation flow of technique of the present invention is short, and preparation time significantly reduces;
3. the C that prepared by the present invention
f/ SiC matrix material has the high-compactness close to theoretical density.
Embodiment
Below in conjunction with two specific embodiments, the present invention is further understood in exemplary illustration and help.But embodiment detail is only for the present invention is described, do not represent the whole technical schemes of the present invention under conceiving, therefore should not be construed as the restriction to technical scheme of the present invention.Some do not depart from the unsubstantiality of the present invention's design changes, for example, to have simple the change or replacement of technical characterictic of same or similar technique effect, all belong to rights protection scope of the present invention.
Embodiment 1
A preparation method for carbon fiber reinforced silicon carbide matrix composite, preparation technology comprises the following steps:
Step 1, the carbon fiber knit that is 6 ~ 8 μ m by mean diameter becomes three dimension stereo fabric (being called carbon fabric perform below);
Step 2, puts into an airtight container by carbon fabric perform, and in container, places Pure Silicon Metal, and itself and carbon fabric perform are isolated; It is 1 * 10 that material in said vesse and container is positioned over to vacuum tightness together
-2in the vacuum oven of Pa, heat to 1500 ℃, insulation 1h, takes out the carbon fabric perform of processing after furnace cooling;
Step 3, by mean particle size, be silicon carbide powder 72g, carbon black 8g, resol 2g, polyvinylpyrrolidone 0.2g, Tetramethylammonium hydroxide 0.5g and the ethanol 40ml of 0.1 μ m, put into high energy ball mill, and add the agate abrading-ball of 300g, after ball milling 5h, be mixed with mixed slurry;
Step 4, is positioned over carbon fabric perform in graphite jig, and 0.5MPa that mixed slurry is pressurizeed under the vacuum environment of 0.01 MPa, is impregnated in above-mentioned carbon fabric perform and obtains composite body;
Step 5, arises from 100 ℃ of insulation 2h by above-mentioned base substrate and mould one and carries out baking and curing processing;
Step 6, it is 1 * 10 that above-mentioned base substrate and mould are placed on to vacuum tightness together
-3in the vacuum oven of Pa, be warming up to 1500 ℃ and carry out high temperature siliconising reaction, obtain high-compactness, high performance carbon/composite silicon carbide ceramic material.
Embodiment 2
A preparation method for carbon fiber reinforced silicon carbide matrix composite, preparation technology comprises the following steps:
Step 1, the carbon fiber knit that is 6 ~ 8 μ m by mean diameter becomes three-dimensional carbon fiber preform;
Step 2, puts into an airtight container by carbon fabric perform, and in container, places Pure Silicon Metal, and itself and carbon fabric perform are isolated, and it is 5 * 10 that the material in said vesse and container is positioned over to vacuum tightness together
-3in the vacuum oven of Pa, heat to 1500 ℃, insulation 3h, takes out the carbon fabric perform of processing after furnace cooling;
Step 3, by mean particle size, be silicon carbide powder 63g, carbon black 7g, resol 2g, polyvinylpyrrolidone 0.3g, Tetramethylammonium hydroxide 0.5g and the ethanol 40ml of 0.22 μ m, put into high energy ball mill, and add the agate abrading-ball of 300g, after ball milling 5h, be mixed with mixed slurry;
Step 4, is positioned over carbon fabric perform in graphite jig, mixed slurry is applied under the vacuum environment of 0.01 MPa to the pressure of 0.2 MPa, is impregnated in above-mentioned carbon fabric perform and obtains composite body;
Step 5, arises from 100 ℃ of insulation 2h by above-mentioned base substrate and mould one and carries out baking and curing processing;
Step 6, it is 1 * 10 that above-mentioned base substrate and mould are placed on to vacuum tightness together
-3in the vacuum oven of Pa, be warming up to 1480 ℃ and carry out siliconising reaction, obtain high-compactness, high performance carbon-silicon carbide ceramic composite.
Claims (3)
1. a preparation method for carbon fiber reinforced silicon carbide matrix composite, is characterized in that preparation method comprises the steps:
Step 1, the carbon fiber knit that is 6 ~ 8 μ m by diameter becomes three dimension stereo fabric, obtains carbon fabric perform;
Step 2 is 1 * 10 in vacuum tightness
-2~ 5 * 10
-3in the vacuum oven of Pa, at the carbon fiber surface vapour deposition layer of metal silicon of carbon fabric perform;
Step 3 is mixed with mixed slurry by ultra fine silicon carbide powder, carbon black, resol, polyvinylpyrrolidone, Tetramethylammonium hydroxide and ethanol in following ratio after ball milling: 63 ~ 72 parts of silicon carbide powders, 5 ~ 6 parts of carbon blacks, 1.5 ~ 2 parts, resol, 0.5 ~ 1.0 part of Tetramethylammonium hydroxide, 0.1 ~ 0.5 part of polyvinylpyrrolidone, 40 ~ 45 parts of ethanol;
Step 4, is positioned over carbon fabric perform in graphite jig, under subatmospheric environment, mixed slurry is applied to the pressure of 0.1 ~ 2.0 MPa, and its impregnating by pressure is obtained to composite body in above-mentioned carbon fabric perform;
Step 5 is incubated 2 hours together by above-mentioned composite body and mould and carries out baking and curing processing under 100 ℃ of temperature condition;
Step 6, carried out base substrate that baking and curing processes and mould to be placed on together vacuum tightness was 1 * 10 above-mentioned
-2~ 1 * 10
-3in the vacuum oven of Pa, be warming up to 1450 ~ 1550 ℃ and carry out high temperature siliconising reaction, make carbon fiber reinforced silicon carbide matrix composite.
2. according to the preparation method of the carbon fiber reinforced silicon carbide matrix composite described in right 1, it is characterized in that:
In step 2, at the fiber surface of carbon fabric perform, adopting the layer of metal silicon thickness of vapour deposition process deposition is 0.1 ~ 2 μ m.
3. according to the preparation method of the carbon fiber reinforced silicon carbide matrix composite described in right 1 or 2, it is characterized in that:
The granularity of the mixed slurry using in step 3 is 0.05 ~ 0.25 μ m.
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Cited By (1)
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| CN105802580A (en) * | 2016-03-09 | 2016-07-27 | 苏州莱特复合材料有限公司 | Method for preparing carbon/silicon carbide composite friction material |
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| CN103253939B (en) * | 2013-05-15 | 2015-02-25 | 宁波欧翔精细陶瓷技术有限公司 | Preparation method of carbon-silicon carbide composite material |
| CN105174963A (en) * | 2015-07-28 | 2015-12-23 | 江西申山能源科技有限公司 | Composite ceramic material and preparation method thereof |
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| CN115368146B (en) * | 2022-10-24 | 2023-02-21 | 山东红点新材料有限公司 | Non-asphalt-based adhesive for producing carbon products and preparation method thereof |
| CN115594525B (en) * | 2022-10-25 | 2023-08-18 | 崇义恒毅陶瓷复合材料有限公司 | Wear-resistant plate of centrifugal machine and preparation process thereof |
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