CN110483055B - SiC containing codeposition complex phase interfacefPreparation method of/SiC composite material - Google Patents
SiC containing codeposition complex phase interfacefPreparation method of/SiC composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 12
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 130
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 114
- 239000001257 hydrogen Substances 0.000 claims abstract description 47
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 47
- 230000008021 deposition Effects 0.000 claims abstract description 46
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 230000005501 phase interface Effects 0.000 claims abstract description 38
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000835 fiber Substances 0.000 claims abstract description 30
- 238000002360 preparation method Methods 0.000 claims abstract description 25
- 239000007789 gas Substances 0.000 claims abstract description 24
- 239000012159 carrier gas Substances 0.000 claims abstract description 21
- 229910052786 argon Inorganic materials 0.000 claims abstract description 16
- 239000003085 diluting agent Substances 0.000 claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 12
- 239000011159 matrix material Substances 0.000 claims abstract description 11
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims abstract description 8
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 6
- DWAWYEUJUWLESO-UHFFFAOYSA-N trichloromethylsilane Chemical compound [SiH3]C(Cl)(Cl)Cl DWAWYEUJUWLESO-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001764 infiltration Methods 0.000 claims abstract description 5
- 230000008595 infiltration Effects 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 5
- 239000002296 pyrolytic carbon Substances 0.000 claims abstract description 4
- 238000000151 deposition Methods 0.000 claims description 43
- 239000002159 nanocrystal Substances 0.000 claims description 9
- 238000005229 chemical vapour deposition Methods 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 4
- 239000013078 crystal Substances 0.000 abstract 1
- 239000012495 reaction gas Substances 0.000 description 3
- 238000009941 weaving Methods 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000002679 ablation Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
The invention discloses SiC containing codeposition complex phase interfacefThe preparation method of the/SiC composite material comprises the following steps: performing interface deposition on the SiC fiber preform by adopting a CVI (chemical vapor infiltration) process, and performing codeposition by taking propylene as a carbon source gas and trichloromethylsilane as a silicon carbide source gas; the carrier gas is hydrogen, and the diluent gas is argon and hydrogen; and performing SiC matrix deposition on the SiC fiber preform subjected to interface deposition by using a CVI (chemical vapor infiltration) process, wherein the silicon carbide source gas is trichloromethylsilane, the carrier gas is hydrogen, and the diluent gas is argon and hydrogen. Preparation of the obtained SiCfthe/SiC composite material has PyC-SiC complex phase interface between the fiber and the matrix, and the PyC-SiC complex phase interface is formed through codeposition and consists of SiC nanometer crystal and pyrolytic carbon phase PyC. The preparation method provided by the invention mainly comprises two main steps of preparing a PyC-SiC complex phase interface by using CVI codeposition and densifying the SiC matrix, the preparation of the interface is easier to control, and the preparation efficiency is higher; prepared SiCfThe toughness of the/SiC composite material is further improved.
Description
Technical Field
The invention relates to the technical field of nuclear industry composite materials, in particular to SiC containing codeposition complex phase interfacefA preparation method of a/SiC composite material.
Background
SiCf/The SiC composite material has a plurality of excellent performances such as high strength, high modulus, low density, high temperature resistance, impact resistance, oxidation resistance, creep resistance, ablation resistance, irradiation resistance and the like, and has wide application prospect in the fields of aerospace, nuclear energy and the like. The interface between the fiber and the matrix is the key factor determining the performance of the composite material, and the optimization of the interface is still to improve the SiCfThe main means of the mechanical property of the/SiC composite material.
At present, SiCfThe interface phase of the/SiC composite material mainly comprises BN, PyC/SiC and BN/SiC multilayer interfaces. However, under neutron irradiation conditions, B can be rapidly transmuted to 10B, and therefore, the BN interface phase cannot be applied to nuclear application environments. The PyC interface can well improve SiCfFracture behavior of the/SiC composite, but the radiation stability of PyC is extremely limited, which can be attributed to SiCfThe radiation resistance of the/SiC composite is adversely affected. Because the irradiation stability of SiC is much higher than that of PyC, the (PyC/SiC) n multilayer composite interface is adopted, so that the oxidation resistance of the composite material can be improved, and the composite material can have better mechanical property and fracture behavior under the neutron irradiation environment. For example, Nozawa and Snead et al have shown SiC with (PyC/SiC) n interfaces after neutron irradiationfThe strength retention rate of the/SiC composite material is higher, and the research of Kishioto et al also shows that the (PyC/SiC) n interface has better dimensional stability after irradiation.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the invention provides a method for preparing SiC containing (PyC-SiC) complex phase interface by using a CVI process to solve the problems that the toughening efficiency of a (PyC/SiC) n multilayer interface is not high and the preparation is not easy to controlfA preparation method of a/SiC composite material.
The invention is realized by the following technical scheme:
a preparation method of a composite material containing a codeposition complex phase interface comprises the following steps:
setp.1, interfacial deposition: performing interface deposition on the SiC fiber preform by adopting a CVI (chemical vapor infiltration) process, and performing codeposition by taking propylene as a carbon source gas and trichloromethylsilane as a silicon carbide source gas; the carrier gas is hydrogen, and the diluent gas is argon and hydrogen; the deposition temperature is 950-1200 ℃, and the deposition pressure is 100-1000 Pa;
setp.2, matrix deposition: performing SiC matrix deposition on the SiC fiber preform subjected to interface deposition by using a CVI (chemical vapor deposition) process, wherein the silicon carbide source gas is trichloromethylsilane, the carrier gas is hydrogen, and the diluent gas is argon and hydrogen; the deposition temperature is 950-1200 ℃, and the deposition pressure is 100-2000 Pa.
Furthermore, in the Setp.1, the flow ratio of propylene to carrier gas hydrogen is 5-10, the flow ratio of diluted hydrogen to carrier gas hydrogen is 3-10, and the flow ratio of diluted argon to diluted hydrogen is 1-5.
Furthermore, in the Setp.2, the flow ratio of the diluted hydrogen to the carrier gas hydrogen is 6-10, and the flow ratio of the diluted argon to the diluted hydrogen is 1-5.
SiC prepared by the preparation method of the composite material containing the codeposition complex phase interfacefa/SiC composite material in SiCfThe composite material comprises a substrate and/or a fiber, wherein a PyC-SiC complex phase interface is arranged between the fiber and the substrate of the/SiC composite material, and the PyC-SiC complex phase interface is a complex phase interface which is formed by codeposition and consists of SiC nanocrystals and pyrolytic carbon phase PyC.
Further, the SiC nanocrystals are dispersed and embedded in the PyC phase, and the grain size of the SiC nanocrystals is 1-100 nm.
Further, the thickness of the PyC-SiC complex phase interface is 200-1000 nm.
The invention has the following advantages and beneficial effects:
1. SiC provided by the inventionfPreparation method of/SiC composite material, and SiC containing (PyC/SiC) complex phase interface prepared by preparation methodfThe invention provides a/SiC composite material, which is based on a (PyC/SiC) n multilayer composite interface, wherein the PyC and SiC codeposit complex phase interface is provided, namely the interface layer is (PyC/SiC) complex phase ceramic; compared with a (PyC/SiC) n multilayer composite interface, in the (PyC/SiC) complex phase interface, SiC nanocrystals are dispersed and distributed and embedded in the pyrolytic carbon phase PyC, and the (PyC/SiC) complex phase interface has a multi-dimensional interface structure and can better play a role in deflecting cracks, so that the (PyC/SiC) complex phase interface can improve SiCfThe toughness of the/SiC composite material is higher in efficiency;
2. SiC provided by the inventionfThe preparation method of the/SiC composite material mainly comprises the steps of preparing a PyC-SiC complex phase interface by utilizing a chemical vapor infiltration process and densifying a SiC matrixThe (PyC/SiC) complex phase interface can be subjected to one-time codeposition, and multiple alternate depositions are not required like a (PyC/SiC) n multilayer composite interface, so that the preparation is easier to control and the preparation efficiency is higher.
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. In the drawings:
FIG. 1 is an SEM image of the present invention;
FIG. 2 is a partial enlarged view of the SEM image of FIG. 1;
FIG. 3 shows the tensile mechanical property characterization results of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.
Example 1
Preparation of PyC-SiC-containing complex phase interface SiCfThe preparation method of the/SiC composite material comprises the following steps:
step 1, preparing a SiC fiber preform: weaving the composite material preform by using SiC fibers to obtain the SiC fiber preform which meets the structural form required by the sample;
step 2, interface deposition: placing the SiC fiber preform in a chemical vapor deposition furnace to start codeposition to obtain a complex phase interface, wherein the adopted reaction gas system is as follows: SiCl3CH3-H2-C3H6-Ar，SiCl3CH3As a silicon carbide source gas, C3H6The carbon source gas is used as a carbon source gas, the flow ratio of propylene to carrier gas hydrogen is 5, the flow ratio of diluent hydrogen to carrier gas hydrogen is 4, the flow ratio of diluent argon to diluent hydrogen is 2, the deposition temperature is 1000 ℃, the deposition pressure is 100-150 Pa, and the deposition time is 40-45 min;
and 3, placing the prepared SiC fiber preform with the complex phase interface in a chemical vapor deposition furnace again, and performing SiC matrix deposition, wherein the flow ratio of the diluted hydrogen to the carrier gas hydrogen is 6, the flow ratio of the diluted argon to the diluted hydrogen is 2, the deposition temperature is 1050 ℃, the deposition pressure is 200-260 Pa, and the deposition time is 350-400 h. The thickness of the finally obtained complex phase interface is 200-300 nm.
Example 2
Preparation of PyC-SiC-containing complex phase interface SiCfThe preparation method of the/SiC composite material comprises the following steps:
step 1, preparing a SiC fiber preform: weaving the composite material preform by using SiC fibers to obtain the SiC fiber preform which meets the structural form required by the sample;
step 2, interface deposition: placing the SiC fiber preform in a chemical vapor deposition furnace to start codeposition to obtain a complex phase interface, wherein the adopted reaction gas system is as follows: SiCl3CH3-H2-C3H6-Ar，SiCl3CH3As a silicon carbide source gas, C3H6The carbon source gas is used as a carbon source gas, the flow ratio of propylene to carrier gas hydrogen is 7, the flow ratio of diluent hydrogen to carrier gas hydrogen is 6, the flow ratio of diluent argon to diluent hydrogen is 4, the deposition temperature is 950 ℃, the deposition pressure is 250-300 Pa, and the deposition time is 50-55 min;
and 3, placing the prepared SiC fiber preform with the complex phase interface in a chemical vapor deposition furnace again for SiC matrix deposition, wherein the flow ratio of the diluted hydrogen to the carrier gas hydrogen is 8, the flow ratio of the diluted argon to the diluted hydrogen is 3, the deposition temperature is 950 ℃, the deposition pressure is 220-270 Pa, and the deposition time is 330-360 h. The thickness of the finally obtained complex phase interface is 400-500 nm.
Example 3
Preparation of PyC-SiC-containing complex phase interface SiCfThe preparation method of the/SiC composite material comprises the following steps:
step 1, preparing a SiC fiber preform: weaving the composite material preform by using SiC fibers to obtain the SiC fiber preform which meets the structural form required by the sample;
step 2, interface deposition: placing the SiC fiber preform in a chemical vapor deposition furnace to start coprecipitationAnd obtaining a complex phase interface by accumulation, wherein the adopted reaction gas system is as follows: SiCl3CH3-H2-C3H6-Ar，SiCl3CH3As a silicon carbide source gas, C3H6The carbon source gas is used as a carbon source gas, the flow ratio of propylene to carrier gas hydrogen is 10, the flow ratio of diluent hydrogen to carrier gas hydrogen is 9, the flow ratio of diluent argon to diluent hydrogen is 5, the deposition temperature is 1200 ℃, the deposition pressure is 850-900 Pa, and the deposition time is 55-60 min;
and 3, placing the prepared SiC fiber preform with the complex phase interface in a chemical vapor deposition furnace again, and performing SiC matrix deposition, wherein the flow ratio of the diluted hydrogen to the carrier gas hydrogen is 10, the flow ratio of the diluted argon to the diluted hydrogen is 5, the deposition temperature is 2000 ℃, the deposition pressure is 1500-1600 Pa, and the deposition time is 300-350 h. The thickness of the finally obtained complex phase interface is 900-1000 nm.
And (3) performance characterization and analysis:
the sample provided in example 2 was examined and shown in fig. 1 and 2 as a TEM photograph of a carbon-coated interface in which PyC in the carbon-coated interface had a turbostratic structure, a low degree of orientation, and a distinct amorphous diffraction pattern. In the carbon-coated interface, SiC uniformly exists in the form of nanocrystals, and the SiC nanocrystals are coated with PyC of a turbostratic structure. Fig. 3 is a tensile stress strain curve of the SiC fiber bundle composite material containing different interfaces, and it can be seen from the graph that the tensile strength and the failure strain value of the SiC fiber bundle composite material containing the PyC-SiC complex phase interface are larger than those of the SiC fiber bundle composite material containing the PyC/SiC multilayer interface, which indicates that the PyC-SiC complex phase interface has a better toughening effect.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (6)
1. SiC containing codeposition complex phase interfacefThe preparation method of the/SiC composite material is characterized by comprising the following steps:
setp.1, interfacial deposition: performing interface deposition on the SiC fiber preform by adopting a CVI (chemical vapor infiltration) process, and performing codeposition by taking propylene as a carbon source gas and trichloromethylsilane as a silicon carbide source gas; the carrier gas is hydrogen, and the diluent gas is argon and hydrogen; the deposition temperature is 950-1200 ℃, and the deposition pressure is 100-1000 Pa;
setp.2, matrix deposition: performing SiC matrix deposition on the SiC fiber preform subjected to interface deposition by using a CVI (chemical vapor deposition) process, wherein the silicon carbide source gas is trichloromethylsilane, the carrier gas is hydrogen, and the diluent gas is argon and hydrogen; the deposition temperature is 950-1200 ℃, and the deposition pressure is 100-2000 Pa.
2. The SiC containing codeposited complex phase interface as claimed in claim 1fThe preparation method of the/SiC composite material is characterized in that in Setp.1, the flow ratio of propylene to carrier gas hydrogen is 5-10, the flow ratio of diluted hydrogen to carrier gas hydrogen is 3-10, and the flow ratio of diluted argon to diluted hydrogen is 1-5.
3. The SiC containing codeposited complex phase interface as claimed in claim 1fThe preparation method of the/SiC composite material is characterized in that in Setp.2, the flow ratio of diluted hydrogen to carrier gas hydrogen is 6-10, and the flow ratio of diluted argon to diluted hydrogen is 1-5.
4. SiC containing codeposition complex phase interfacefA/SiC composite material using a SiC composite material comprising a co-deposited complex phase interface as claimed in any one of claims 1 to 3fThe preparation method of the/SiC composite material is characterized in that the SiC is preparedfThe composite material comprises a substrate and/or a fiber, wherein a PyC-SiC complex phase interface is arranged between the fiber and the substrate of the/SiC composite material, and the PyC-SiC complex phase interface is a complex phase interface which is formed by codeposition and consists of SiC nanocrystals and pyrolytic carbon phase PyC.
5. A process according to claim 4SiC containing codeposited complex phase interfacefthe/SiC composite material is characterized in that the SiC nanocrystals are dispersed and embedded in a PyC phase, and the grain size of the SiC nanocrystals is 1-100 nm.
6. The SiC containing codeposited complex phase interface as claimed in claim 4fthe/SiC composite material is characterized in that the thickness of a PyC-SiC complex phase interface is 200-1000 nm.
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| CN113004051A (en) * | 2019-12-20 | 2021-06-22 | 中核北方核燃料元件有限公司 | SiCfInterface layer structure of/SiC composite material fuel cladding and preparation method |
| CN112028657A (en) * | 2020-08-03 | 2020-12-04 | 杭州卓导新材料有限公司 | Preparation method of carbon/carbon composite material crucible |
| CN112876257B (en) * | 2021-01-27 | 2022-05-17 | 中国核动力研究设计院 | SiCfTwo-layer composite cladding tube made of/SiC composite material and preparation method thereof |
| CN114315395A (en) * | 2021-10-20 | 2022-04-12 | 中国航发沈阳黎明航空发动机有限责任公司 | SiCfSiC nanowire toughened PyC/SiC composite interface of/SiC composite material and preparation method thereof |
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| US8980434B2 (en) * | 2011-12-16 | 2015-03-17 | Wisconsin Alumni Research Foundation | Mo—Si—B—based coatings for ceramic base substrates |
| CN106966742A (en) * | 2016-06-03 | 2017-07-21 | 北京航空航天大学 | Alumina fibre enhancing mullite ceramic of the phase containing interface and preparation method thereof |
| CN108395279A (en) * | 2018-02-08 | 2018-08-14 | 西北工业大学 | The method that chemical gaseous phase co-electrodeposition method prepares HfC-SiC complex phase gradient coatings |
| CN108484190A (en) * | 2018-03-22 | 2018-09-04 | 陕西科技大学 | A kind of preparation method of the multiphase carbide ceramics based composites of fibre reinforced |
| CN109970460A (en) * | 2018-11-23 | 2019-07-05 | 中国科学院金属研究所 | A carbon fiber reinforced (carbon-) silicon carbide-based ultra-high temperature ceramic matrix composite material and preparation method thereof |
| CN109485423A (en) * | 2018-11-29 | 2019-03-19 | 西北工业大学 | The preparation method of SiC nanowire toughening chemical gaseous phase co-deposition HfC-SiC duplex heat treatment |
| CN109721377A (en) * | 2019-01-30 | 2019-05-07 | 湖南兴晟新材料科技有限公司 | Ceramic Matrix Composites Reinforced by Carbon Fibers and preparation method thereof |
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