CN105016759A - Rapid preparation method for C/SiC composite material - Google Patents
Rapid preparation method for C/SiC composite material Download PDFInfo
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- CN105016759A CN105016759A CN201510377418.9A CN201510377418A CN105016759A CN 105016759 A CN105016759 A CN 105016759A CN 201510377418 A CN201510377418 A CN 201510377418A CN 105016759 A CN105016759 A CN 105016759A
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Abstract
The invention relates to a rapid preparation method for a C/SiC composite material. The method is characterized by including the steps of: 1. depositing a pyrolytic carbon interface on a thin layer carbon fiber preform surface by a chemical vapor deposition process; 2. infiltrating the thin layer carbon fiber perform of the deposited PyC interface in a polycarbosilane mixed solution, and then carrying out cross-linking curing and pyrolysis in order under protective atmosphere to obtain a thin layer C/SiC composite material; 3. repeating the previous step 2-3 times; and 4. stacking a plurality of single-layer composite materials in a graphite die to conduct spark plasma sintering (SPS), thus rapidly obtaining a compact C/SiC composite material finally. The method provided by the invention makes full use of the characteristics of short thin layer infiltration time of PIP (precursor infiltration and pyrolysis) method and rapid sintering of SPS method to realize preparation of the C/SiC composite material, is suitable for compaction of small compact components, saves 95% of time than the traditional CVI (chemical vapor infiltration) method and PIP method, also significantly improves the compactness of the composite material, and reduces the making cost of the composite material.
Description
Technical field
The present invention relates to the preparation of Material Field about C/SiC matrix material, particularly a kind of processing method of quick preparation C/SiC matrix material.
Background technology
C/SiC matrix material is a kind of novel super-high temperature structured material emerged with the development of aeronautical and space technology, has low density, high strength, high tenacity, high temperature resistant, resistance to chemical attack, resistance to ablation, antiscour, the feature such as high rigidity and high-wearing feature.The method of the current C/SiC of preparation matrix material has a lot, and chemical vapor infiltration (Chemical vaporinfiltration, CVI) has been used and commercial method.In patent No. 102690124A, disclose a kind of C/SiC ceramic matric composite and preparation method thereof, the method adopts CVI to obtain C/SiC matrix material at carbon fabric perform surface deposition RESEARCH OF PYROCARBON interfacial layer and silicon carbide substrate successively.But it is long that CVI legal system has preparation cycle for C/SiC matrix material, and cost is high, the shortcoming of complex process, document 1 " Xiao Peng, Xu Yongdong, Huang Baiyun, CVI method prepares C/SiC matrix material fast, silicate journal, 2002,30 [2]: 240-243 ".If can production technique be simplified, and shorten the preparation cycle of C/SiC matrix material, will the development and application promoting C/SiC matrix material be further conducive to.
A kind of quick method preparing C/SiC ceramic matric composite is disclosed in patent No. 102795871A.The method is with the liquid Polycarbosilane of low molecule for precursor, and carbon fiber preform is skeleton, adopts the Chemical Liquid-vaporized Infiltration Process of pulsed heating to prepare C/SiC matrix material.
The method of a kind of low cost reaction fusion adhesion legal system for C/SiC matrix material is disclosed in patent No. 103342570A.The method is by carbon felt impregnated carbon/silicon carbide slurry and carry out melting siliconising process, then steeping liq resol carbonization, finally carries out second melting siliconising process and obtains C/SiC.The method technique is more loaded down with trivial details, and high-temperature fusant Si can corrode carbon fiber, and remaining Si can weaken the high-temperature creep resistance of matrix material.
A kind of low temperature preparation method of C/SIC ceramic matric composite is disclosed in the patent No. 101224988.The method adopts precursor infiltration and pyrolysis technique (Precursor Infiltration and Pyrolysis, PIP), by processing steps such as pre-treatment of carbon fiber, vacuum impregnation, Pintsch process, densifications, prepare C/SIC ceramic matric composite under cryogenic.The method repeat cycle is longer, and the matrix of preparation can exist a large amount of shrinkage cracks and hole, and Pintsch process can damage fiber repeatedly.
Utilize Chemical Liquid-vaporized Infiltration Process in conjunction with the preparation method of precursor infiltration and pyrolysis in document 3 " Si'an Chen; Haifeng Hu; Yudi Zhang; Xinbo He; Min Mei.Rapid densificationof C/SiC composites by joint processes of CLVD and PIP.Materials Letters.2011,65 [19-20]: 3137-3139. ".
Discharge plasma sintering (Spark Plasma Sintering, SPS) be a kind of brand new technical preparing functional materials, it has the distinguishing features such as heat-up rate is fast, sintering time is short, weave construction is controlled, energy-conserving and environment-protective, can be used to prepare metallic substance, stupalith, matrix material etc., document 2 " Zhang Jiuxing; Liu Kegao; Zhou Meiling, the development of discharge plasma sintering technique and application, powder metallurgy technology; 2002,20 [3]: 129-134 ".
Document 4 " Alba Centeno, Victoria G.Rocha, Amparo Borrell, Clara Blanco, AdolfoFerna ' ndez.Fabrication of C/SiC composites by combining liquid infiltration process andspark plasma sintering technique.Ceramics International.2012, 38 [3]: 2171-2175. " resin base 2D carbon fabric perform is utilized in, through a series of liquid infiltration technique dipping mesophase pitch, SiC nanowire particle, silica flour then SPS obtains C/SiC, technological process is very complicated.
Summary of the invention
The technical problem solved
Long in order to solve the preparation cycle existed in prior art, the problems such as cost is high, complex process, promote the development and application of C/SiC matrix material further, the present invention proposes a kind of PIP of utilization prepares C/SiC matrix material fast method in conjunction with SPS.
Technical scheme
A fast preparation method for C/SiC matrix material, is characterized in that step is as follows:
Step 1, deposited interfacial layer: adopt thickness to be less than the coating carbon fibre precast body of 0.3mm as composite material reinforcement body, adopt chemical vapor infiltration to deposit RESEARCH OF PYROCARBON PyC interface on coating carbon fibre precast body;
Prepared by step 2, solution: weigh 0 ~ 20wt% sintering aid, mix with Polycarbosilane PCS, uses magnetic agitation 4 ~ 20h to even;
Prepared by step 3, matrix: coating carbon fibre precast body step 1 being deposited PyC interface is immersed in 1 ~ 10h in solution prepared by step 2, then 200 ~ 250 DEG C of crosslinking curing 2 ~ 3h under protective atmosphere, continue cracking 2 ~ 3h at 800 ~ 900 DEG C, obtain thin multilayer composite material: repeat this step, make thin multilayer composite material density more than 80%; Described protective atmosphere is vacuum or argon gas;
Prepared by step 4, matrix material: thin layer composite lay multi-disc step 3 prepared is put into graphite jig and carried out discharge plasma sintering, sintering temperature is 1500 ~ 1900 DEG C, load is 30 ~ 100Mpa, dwell time 2 ~ 10min, prepares fine and close C/SiC matrix material.
This step of repetition in described step 3 is 2 ~ 3 times.
When adopting chemical vapor infiltration to deposit RESEARCH OF PYROCARBON PyC interface in described step 1 on coating carbon fibre precast body, precursor is propylene, methane, acetylene, ethene or other hydrocarbon polymers; Condition is: take argon gas as diluent gas, and depositing temperature is 750 ~ 1100 DEG C, and the time is 10 ~ 20h; Then at 1600 ~ 1800 DEG C of thermal treatment 0.5 ~ 2h.
Described coating carbon fibre precast body is one or more in two-dimentional carbon cloth, two-dimentional half carbon fiber thin layers of woven body, three-dimensional carbon fibre thin layer knitted body and coating carbon fibre Nomex.
The sintering aid that described step 4 uses is one or more in aluminum oxide, magnesium oxide, zirconium white, yttrium oxide, ytterbium oxide, Erbium trioxide, Scium trioxide, cerium oxide and other rare earth oxides.
Described sintering aid total content is 5 ~ 20wt%.
In described step 4, multi-disc thin layer matrix material is 10 ~ 30.
Beneficial effect
The quick method preparing C/SiC matrix material that the present invention relates to, adopts precursor infiltration and pyrolysis (PIP) technique to prepare C/SiC matrix material fast in conjunction with discharge plasma sintering (SPS) technique.Beneficial effect is: the present invention makes full use of the advantage of PIP method and SPS method, fast preparation fiber reinforcement C/SiC matrix material.The method utilizes PIP method to flood thin layer time short and SPS method and sinters feature rapidly, thus realize the preparation of C/SiC matrix material, be applicable to the densification of small-sized fine and close component, 95% can be saved time than traditional C VI method and PIP method, and significantly improve matrix material density, reduce matrix material manufacturing cost.Fig. 2 is the photo of C/SiC matrix material prepared by SPS.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that the present invention prepares C/SiC matrix material fast;
Fig. 2 is the photo of C/SiC matrix material prepared by SPS.
Embodiment
Now in conjunction with the embodiments, the invention will be further described for accompanying drawing:
Embodiment 1
Step one: deposited interfacial layer: adopt thickness to be less than the coating carbon fibre precast body of 0.3mm as composite material reinforcement body, adopts chemical vapor infiltration deposition RESEARCH OF PYROCARBON (PyC) interface.During deposition pyrolysis, precursor is propylene, methane, acetylene, ethene or other hydrocarbon polymers; Condition is: take argon gas as diluent gas, and depositing temperature is 750 ~ 1100 DEG C, and the time is 10 ~ 20h; Then at 1600 ~ 1800 DEG C of thermal treatment 0.5 ~ 2h;
Step 2: prepared by solution: weigh 0 ~ 20wt% aluminum oxide or oxygen soil metal oxide and 0 ~ 20wt% rare earth oxide as sintering aid, mix with Polycarbosilane (PCS).Use magnetic agitation 4 ~ 20h to even.
Step 3: prepared by matrix: the coating carbon fibre precast body dipping mixing solutions 1 ~ 10h at deposition PyC interface, takes out, then 200 ~ 250 DEG C of crosslinking curing 2 ~ 3h under protective atmosphere, 800 ~ 900 DEG C of cracking 2 ~ 3h, obtains thin multilayer composite material.
Repeat this step 2 ~ 3 times, cause thin multilayer composite material density more than 80%.
Step 4: prepared by matrix material: carry out discharge plasma sintering by putting into graphite jig after 10 ~ 30 single layer composite laminations, sintering temperature is 1500 ~ 1900 DEG C, load is 70Mpa, dwell time 2 ~ 10min, finally prepares fine and close C/SiC matrix material fast.
Embodiment 2
Step one: deposited interfacial layer: adopt thickness to be less than the coating carbon fibre precast body of 0.3mm as composite material reinforcement body, adopts chemical vapor infiltration deposition RESEARCH OF PYROCARBON (PyC) interface.During deposition pyrolysis, precursor is propylene, methane, acetylene, ethene or other hydrocarbon polymers; Condition is: take argon gas as diluent gas, and depositing temperature is 750 ~ 1100 DEG C, and the time is 10 ~ 20h; Then at 1600 ~ 1800 DEG C of thermal treatment 0.5 ~ 2h;
Step 2: prepared by solution: weigh 0 ~ 20wt% aluminum oxide or oxygen soil metal oxide and 0 ~ 20wt% rare earth oxide as sintering aid, mix with Polycarbosilane (PCS).Use magnetic agitation 4 ~ 20h to even.
Step 3: prepared by matrix: the coating carbon fibre precast body dipping mixing solutions 1 ~ 10h at deposition PyC interface, takes out, then 200 ~ 250 DEG C of crosslinking curing 2 ~ 3h under protective atmosphere, 800 ~ 900 DEG C of cracking 2 ~ 3h, obtains thin multilayer composite material.
Repeat this step 2 ~ 3 times, cause thin multilayer composite material density more than 80%.
Step 4: prepared by matrix material: carry out discharge plasma sintering by putting into graphite jig after 10 ~ 30 single layer composite laminations, sintering temperature is 1500 ~ 1900 DEG C, load is 80Mpa, dwell time 2 ~ 10min, finally prepares fine and close C/SiC matrix material fast.
Embodiment 3
Step one: deposited interfacial layer: adopt thickness to be less than the coating carbon fibre precast body of 0.3mm as composite material reinforcement body, adopts chemical vapor infiltration deposition RESEARCH OF PYROCARBON (PyC) interface.During deposition pyrolysis, precursor is propylene, methane, acetylene, ethene or other hydrocarbon polymers; Condition is: take argon gas as diluent gas, and depositing temperature is 750 ~ 1100 DEG C, and the time is 10 ~ 20h; Then at 1600 ~ 1800 DEG C of thermal treatment 0.5 ~ 2h;
Step 2: prepared by solution: weigh 0 ~ 20wt% aluminum oxide or oxygen soil metal oxide and 0 ~ 20wt% rare earth oxide as sintering aid, mix with Polycarbosilane (PCS).Use magnetic agitation 4 ~ 20h to even.
Step 3: prepared by matrix: the coating carbon fibre precast body dipping mixing solutions 1 ~ 10h at deposition PyC interface, takes out, then 200 ~ 250 DEG C of crosslinking curing 2 ~ 3h under protective atmosphere, 800 ~ 900 DEG C of cracking 2 ~ 3h, obtains thin multilayer composite material.
Repeat this step 2 ~ 3 times, cause thin multilayer composite material density more than 80%.
Step 4: prepared by matrix material: carry out discharge plasma sintering by putting into graphite jig after 10 ~ 30 single layer composite laminations, sintering temperature is 1500 ~ 1900 DEG C, load is 90Mpa, dwell time 2 ~ 10min, finally prepares fine and close C/SiC matrix material fast.
Claims (7)
1. a fast preparation method for C/SiC matrix material, is characterized in that step is as follows:
Step 1, deposited interfacial layer: adopt thickness to be less than the coating carbon fibre precast body of 0.3mm as composite material reinforcement body, adopt chemical vapor infiltration to deposit RESEARCH OF PYROCARBON PyC interface on coating carbon fibre precast body;
Prepared by step 2, solution: weigh 0 ~ 20wt% sintering aid, mix with Polycarbosilane PCS, uses magnetic agitation 4 ~ 20h to even;
Prepared by step 3, matrix: coating carbon fibre precast body step 1 being deposited PyC interface is immersed in 1 ~ 10h in solution prepared by step 2, then 200 ~ 250 DEG C of crosslinking curing 2 ~ 3h under protective atmosphere, continue cracking 2 ~ 3h at 800 ~ 900 DEG C, obtain thin multilayer composite material: repeat this step, make thin multilayer composite material density more than 80%; Described protective atmosphere is vacuum or argon gas;
Prepared by step 4, matrix material: thin layer composite lay multi-disc step 3 prepared is put into graphite jig and carried out discharge plasma sintering, sintering temperature is 1500 ~ 1900 DEG C, load is 30 ~ 100Mpa, dwell time 2 ~ 10min, prepares fine and close C/SiC matrix material.
2. the fast preparation method of C/SiC matrix material according to claim 1, is characterized in that: this step of repetition in described step 3 is 2 ~ 3 times.
3. the fast preparation method of C/SiC matrix material according to claim 1, is characterized in that: when adopting chemical vapor infiltration to deposit RESEARCH OF PYROCARBON PyC interface in described step 1 on coating carbon fibre precast body, precursor is propylene, methane, acetylene, ethene or other hydrocarbon polymers; Condition is: take argon gas as diluent gas, and depositing temperature is 750 ~ 1100 DEG C, and the time is 10 ~ 20h; Then at 1600 ~ 1800 DEG C of thermal treatment 0.5 ~ 2h.
4. the fast preparation method of C/SiC matrix material according to claim 1, is characterized in that: described coating carbon fibre precast body is one or more in two-dimentional carbon cloth, two-dimentional half carbon fiber thin layers of woven body, three-dimensional carbon fibre thin layer knitted body and coating carbon fibre Nomex.
5. the fast preparation method of C/SiC matrix material according to claim 1, is characterized in that: the sintering aid that described step 4 uses is one or more in aluminum oxide, magnesium oxide, zirconium white, yttrium oxide, ytterbium oxide, Erbium trioxide, Scium trioxide, cerium oxide and other rare earth oxides.
6. the fast preparation method of C/SiC matrix material according to claim 1 or 5, is characterized in that: described sintering aid total content is 5 ~ 20wt%.
7. the fast preparation method of C/SiC matrix material according to claim 1, is characterized in that: in described step 4, multi-disc thin layer matrix material is 10 ~ 30.
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| CN105948775A (en) * | 2016-04-27 | 2016-09-21 | 航天材料及工艺研究所 | Preparation method of high-temperature-resistant and oxidation-resistant lightweight carbon/carbon thermal insulation material |
| CN106064951A (en) * | 2016-06-08 | 2016-11-02 | 中国人民解放军国防科学技术大学 | C/C SiC ceramic matrix composite material and its preparation method and application |
| CN106298398A (en) * | 2016-09-29 | 2017-01-04 | 青岛科技大学 | There is preparation and the application of the situ Al doping SiC nanowire of net shape skin |
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| CN108193325A (en) * | 2017-12-27 | 2018-06-22 | 江西嘉捷信达新材料科技有限公司 | High temperature resistant SiC fibers containing zirconium and preparation method thereof |
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Application publication date: 20151104 |