CN103724038A - Preparation method of ceramic matrix hybrid composite material - Google Patents
Preparation method of ceramic matrix hybrid composite material Download PDFInfo
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- CN103724038A CN103724038A CN201310412066.7A CN201310412066A CN103724038A CN 103724038 A CN103724038 A CN 103724038A CN 201310412066 A CN201310412066 A CN 201310412066A CN 103724038 A CN103724038 A CN 103724038A
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Abstract
The invention discloses a preparation method of a ceramic matrix hybrid composite material. The material comprises a nickel coating, SiC foam, a SiC tube and a SiC coating. The preparation method is characterized by sequentially comprising the steps as follows: (1) a carbon fiber framework is woven on the surface of a graphite core; (2) a carbon coating is subjected to pyrolysis on the carbon fiber framework through CVD (chemical vapor deposition), and the thickness of the coating is in a range of 50-150 nm; (3) SiC is deposited on the carbon fiber framework on which a carbon interface layer is deposited with a CVI (chemical vapor infiltration) method, the graphite core is removed, and a semi-finished SiC tube is produced; (4) the SiC is subjected to PIP (precursor impregnation and pyrolysis) to obtain the SiC tube; (5) carbon foam winds around the outer surface of the obtained SiC tube, and then the SiC is subjected to CVI to obtain the SiC tube with SiC foam on the surface; and (6) the nickel coating with a certain thickness is prepared on the outermost layer of the tube with an electroforming method. The tensile breaking strength of the composite material is improved substantially due to the combination of CVI and PIP technologies; layers of the composite material prepared with the method are bonded by atomic power; and the composite material is light in mass, high in strength, excellent in high temperature performance and capable of resisting oxidation and corrosion and can be used as a demanding high-temperature structural part such as an aerospace vehicle spray pipe.
Description
Technical field
The present invention relates to a kind of preparation method of matrix material, particularly relate to a kind of preparation method of ceramic base hybrid composite.
Background technology
High-performance power is the basis of the advanced aerospace device of development, that improves the thrust-weight ratio of aircraft engine and rocket engine rushes matter than being the only way which must be passed that improves advanced aerospace device performance, and these all require constantly to reduce the structural weight of engine and the temperature resistant capability of raising engine component.Therefore, develop high temperature resistant, low-density novel ultrahigh-temperature matrix material and take over superalloy and metallic substance hard to tolerate, become the crucial and basic of development high-performance enginer.The world generally believes, SiC ceramic matric composite is one of technology commanding elevation of engine high-temperature structured material, can reflect Design and manufacture ability prepared by an advanced aerospacecraft of country and advanced weaponry.
On the hot-end component of rocket and guided missile, Cf/SiC ceramic matric composite is for rocket or guided missile thrust chamber, flameholder, the Large Scale Export cone of oxyhydrogen engine, blade, the Fu Bi of advanced turbine engine, solid-rocket Thrust-vectoring Nozzle, guided missile nose cone, the material of main part of the parts such as the leading edge of a wing; At space field, for the base material of space space station, solar collecting device, meanwhile, can be used for the body material of satellite mirror.And these materials are during as hot-end component material, owing to there being multiple thing phase, thermostability and high-temperature oxidation resistance etc. can not reach requirement.Usually adopt at present the method for top coat to alleviate thermal failure and the high temperature oxidation of material.
Publication number is the preparation method that 101265935 Chinese invention patent discloses a kind of ceramic base compound material bolt, its feature comprises the following steps: first by 0/90 ° of positive laying of 1K carbon fiber and ± utilize graphite cake sizing to prepare fiber preform after the oblique laying alternative stacked of θ, on this precast body, deposit RESEARCH OF PYROCARBON interfacial layer, then on the two-dimentional sheet material of RESEARCH OF PYROCARBON interfacial layer of taking advantage of the occasion, depositing silicon carbide matrix is made work in-process ceramic matric composite sheet material, on work in-process ceramic matric composite sheet material, cutting forms bolt blank and uses diamond-impregnated wheel tapping, finally to work in-process bolt infiltration pyrolysis Polycarbosilane continue CVI deposition SiC inoxidzable coating repeatedly, obtain finished product C/SiC compound material bolt.The method is in not completely processing bolt tapping on the work in-process ceramic matric composite precast body of deposition compact, slower to diamond-impregnated wheel wearing and tearing, reduced production cost, CVI makes the tensile break strength of C/SiC compound material bolt in conjunction with PIP technique, by 180～190MPa of prior art, brought up to 210～230MPa.
Publication number is the preparation method that the Chinese invention patent of 101693628A discloses a kind of fiber strengthened ZrC ceramic-matrix composite, for improving the high temperature oxidation resistance of C/C matrix material.First on carbon fabric perform, deposit RESEARCH OF PYROCARBON; to under distilled water and polyvinyl alcohol stirring heating condition, make colloidal sol shape again; then add in proportion after Zr powder; reconcile into thick coating; surface by applying coating at C/C matrix material; at high temperature in protective atmosphere, carry out melt infiltration, make fiber strengthened ZrC ceramic-matrix composite.Owing to adopting melt infiltration method, after highly purified Zr powder and distilled water and polyvinyl alcohol are mixed in proportion, be coated in the surface of C/C matrix material, at high temperature in protective atmosphere, carry out melt infiltration, obtain fiber strengthened ZrC ceramic-matrix composite.The method, by controlling thickness, the heat treated temperature and time of applying coatings, has been prepared fiber strengthened ZrC ceramic-matrix composite, and the thickness of ZrC coating is brought up to several millimeters by tens microns of prior art.
Summary of the invention
The present invention, mainly for the thermal structure pipe fitting of burner, proposes a kind of preparation method of ceramic base hybrid composite.This material has multilayered structure, becomes tubulose, is nickel coating, SiC foam, SiC pipe and SiC coating from outside to inside successively, and thickness is respectively 0.5～3mm, 1～5mm, 0.5～3mm and 0.1mm～0.5mm.By reactive force between atom, combine between layers, can be at steady operation under hot environment, and anti-oxidant, protection against corrosion, can be used as and require the harsh high temperature structural parts such as aerospacecraft jet pipe.
A preparation method for ceramic base hybrid composite, is characterized in that comprising the step of following order:
(1) at graphite core surface weave carbon fiber skeleton, skeleton thickness is 0.8～2.8mm;
(2) CVD pyrocarbon coating on carbon fiber skeleton, coat-thickness is 50～150nm;
(3) method of utilizing CVI deposits SiC depositing on the carbon fiber skeleton of carbon interfacial layer, sloughs graphite core, makes work in-process SiC pipe, porosity residue 10～25%;
(4) PIP SiC, obtains SiC pipe;
The concrete technology condition of described PIP SiC is: first below 1000 ℃, in C fiber, flood Polycarbosilane, then cracking at 1000～1200 ℃ is then heat-treated 2～4h at 1300～1500 ℃; Repeatedly carry out the circulation technology of above-mentioned " dipping-pyrolysis-thermal treatment ", reach the effect to the density of C carbon fabric perform.
(5) at the SiC tube outer surface making, be wound around carbon foam, then CVI SiC3～10 hour, the SiC pipe that surface has SiC foam obtained;
(6) adopt the method for electroforming at the outermost layer of tubing, certain thickness nickel coating is prepared on the surface of SiC foam.
According to above-mentioned preparation method, as the carbon fiber of braiding skeleton, adopt the carbon fiber bundle of 1K, 2K or 3K.
The concrete technology condition of described CVD pyrocarbon coating is: 1300～1400 ℃ of depositing temperatures, methane flow 30～40ml/min; N
2airshed 150～200ml/min; Depositing time 5～20h.
The concrete technology condition of described CVI deposition SiC is: with trichloromethyl silane (CH
3siCl
3, MTS) be precursor raw material, H
2make carrier gas and diluent gas, gas flow is 60～120mL/min, and depositing temperature is 1050～1200 ℃, and pressure is normal pressure, and the time is 40～100h.
The actual conditions of described electroformed nickel coating is: take single nickel salt as main salt, and 40～60 ℃ of temperature, direct current supply, current density is 1.0～3.0A/dm
2.
Major advantage of the present invention is: the hybrid materials that 1. prepared by the method have atomic power combination between layers, and quality is light, and intensity is high, have excellent high-temperature behavior, can anti-oxidant and protection against corrosion; 2. CVI increases substantially the tensile break strength of this matrix material in conjunction with PIP technique; 3. electroplating technology is prepared nickel coating, and technology maturation is simple to operate, and efficiency is high, and coating quality is stable; 4. this material internal is in conjunction with tight, and top coat is anti-oxidant, protection against corrosion, and dependency structure part has long service life, the advantage of good stability.
Accompanying drawing explanation
Be illustrated as a kind of schematic diagram of ceramic base hybrid composite pipe.
Diagram 10 is nickel coating; 20 is SiC foam; 30 is SiC pipe; 40 is SiC coating.
Embodiment
Below in conjunction with specific embodiment, further illustrate the present invention, should understand these embodiment is only not used in and limits the scope of the invention for the present invention is described, after having read the present invention, those skilled in the art all fall within the application's claims to the modification of the various equivalent form of values of the present invention and limit.
Embodiment 1
A preparation method for ceramic base hybrid composite pipe, is characterized in that comprising the step of following order:
(1) adopt the carbon fiber of 1K at graphite core surface weave fiber reinforcement, making skeleton thickness is 1mm;
(2) CVD pyrocarbon coating on carbon fiber skeleton: 1300 ℃ of depositing temperatures, methane flow 30ml/min; N
2airshed 150ml/min; Depositing time 10h;
(3) method of utilizing CVI deposits SiC:CH depositing on the carbon fiber skeleton of carbon interfacial layer
3siCl
3for presoma, H
2make carrier gas and diluent gas, gas flow is 100mL/min, 1050 ℃ of depositing temperatures, and pressure is normal pressure, the time is 40h;
(4) slough graphite core, obtain porosity residue 25%de work in-process SiC pipe;
(5) PIP SiC: the work in-process SiC pipe that surface is had to a residual pore, at 1000 ℃ of infiltration pyrolysis Polycarbosilanes repeatedly, is then heat-treated 2h at 1300 ℃, obtains SiC pipe;
(6) at the SiC tube outer surface making, be wound around the thick carbon foam of 5mm, then CVI SiC8 hour, the SiC pipe that surface has SiC foam obtained;
(7) adopt the method for electroforming at the outermost layer of tubing, the nickel coating of 0.5mm is prepared on the surface of SiC foam.
The ceramic base hybrid composite pipe that aforesaid method makes, has multilayered structure, is nickel coating, SiC foam, SiC pipe and SiC coating from outside to inside successively, and thickness is respectively 0.5mm, 5mm, 1mm and 0.3mm.This preparation method's technology maturation, simple to operate, efficiency is high, and coating quality is stable.
Embodiment 2
A preparation method for ceramic base hybrid composite pipe, is characterized in that comprising the step of following order:
(1) adopt the carbon fiber of 3K at graphite core surface weave fiber reinforcement, making skeleton thickness is 2mm;
(2) CVD pyrocarbon coating on carbon fiber skeleton: 1350 ℃ of depositing temperatures, methane flow 40ml/min; N
2airshed 200ml/min; Depositing time 8h;
(3) method of utilizing CVI deposits SiC:CH depositing on the carbon fiber skeleton of carbon interfacial layer
3siCl
3for presoma, H
2make carrier gas and diluent gas, gas flow is 120mL/min, 1100 ℃ of depositing temperatures, and pressure is normal pressure, the time is 60h;
(4) slough graphite core, obtain the work in-process SiC pipe of porosity residue 20%;
(5) PIP SiC: the work in-process SiC pipe that surface is had to a residual pore, at 1100 ℃ of infiltration pyrolysis Polycarbosilanes repeatedly, is then heat-treated 3h at 1400 ℃, obtains SiC pipe;
(6) at the SiC tube outer surface making, be wound around the thick carbon foam of 4mm, then CVI SiC5 hour, the SiC pipe that surface has SiC foam obtained;
(7) adopt the method for electroforming at the outermost layer of tubing, the nickel coating of 0.8mm is prepared on the surface of SiC foam.
The ceramic base hybrid composite pipe that aforesaid method makes, has multilayered structure, is nickel coating, SiC foam, SiC pipe and SiC coating from outside to inside successively, and thickness is respectively 0.8mm, 4mm, 2mm and 0.2mm.This preparation method's technology maturation, simple to operate, efficiency is high, and coating quality is stable.
Above are only two embodiments of the present invention, but design concept of the present invention is not limited to this, allly utilizes this design to carry out the change of unsubstantiality to the present invention, all should belong to the behavior of invading the scope of protection of the invention.In every case be the content that does not depart from technical solution of the present invention, any type of simple modification, equivalent variations and the remodeling above embodiment done according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (6)
1. a preparation method for ceramic base hybrid composite, comprises nickel coating, SiC foam, SiC pipe and SiC coating, it is characterized in that comprising the step of following order:
(1) at graphite core surface weave carbon fiber skeleton;
(2) CVD pyrocarbon coating on carbon fiber skeleton, coat-thickness is 50～150nm;
(3) method of utilizing CVI deposits SiC depositing on the carbon fiber skeleton of carbon interfacial layer, sloughs graphite core, makes work in-process SiC pipe, porosity residue 10～25%;
(4) PIP SiC, obtains SiC pipe;
(5) at the SiC tube outer surface making, be wound around carbon foam, then CVI SiC3～10 hour, the SiC pipe that surface has SiC foam obtained;
(6) adopt the method for electroforming at the outermost layer of tubing, certain thickness nickel coating is prepared on the surface of SiC foam.
2. preparation method according to claim 1, is characterized in that skeleton thickness is 0.8～2.8mm as carbon fiber employing 1K, the 2K of braiding skeleton or the carbon fiber bundle of 3K.
3. preparation method according to claim 1, is characterized in that the concrete technology condition of described CVD pyrocarbon coating is: 1300～1400 ℃ of depositing temperatures, methane flow 30～40ml/min; N
2airshed 150～200ml/min; Depositing time 5～20h.
4. preparation method according to claim 1, is characterized in that the concrete technology condition of described CVI deposition SiC is: take trichloromethyl silane as precursor raw material, H
2make carrier gas and diluent gas, gas flow is 60～120mL/min, and depositing temperature is 1050～1200 ℃, and pressure is normal pressure, and the time is 40～100h.
5. preparation method according to claim 1, the concrete technology condition that it is characterized in that described PIP SiC is: first below 1000 ℃, in C fiber, flood Polycarbosilane, then cracking at 1000～1200 ℃ is then heat-treated 2～4h at 1300～1500 ℃; Repeatedly carry out the circulation technology of above-mentioned " dipping-pyrolysis-thermal treatment ", reach the effect to the density of C carbon fabric perform.
6. preparation method according to claim 1, is characterized in that the actual conditions of described electroformed nickel coating is: take single nickel salt as main salt, and 40～60 ℃ of temperature, direct current supply, current density is 1.0～3.0A/dm
2.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105220087A (en) * | 2015-07-20 | 2016-01-06 | 西安科技大学 | A kind of high tough Ti (C, N) based ceramic metal matrix material and preparation method thereof |
| TWI602794B (en) * | 2016-03-14 | 2017-10-21 | National Chung-Shan Institute Of Science And Tech | Ceramic composite materials production methods |
| CN107445640A (en) * | 2016-10-12 | 2017-12-08 | 平顺县西沟龙鼎新材料科技有限公司 | A kind of manufacture method of C/SiC novel mechanical sealing rings |
| CN109320275A (en) * | 2018-10-09 | 2019-02-12 | 中国航空工业集团公司基础技术研究院 | A kind of preparation method of anti-oxidant SiC fiber reinforced ceramic matrix composites |
| CN109530491A (en) * | 2018-12-19 | 2019-03-29 | 浙江振兴阿祥集团有限公司 | A kind of non-lubricating rises type rounding die |
| CN109627008A (en) * | 2019-01-17 | 2019-04-16 | 苏州宏久航空防热材料科技有限公司 | A kind of preparation method with laminated composite structure material |
| CN110205811A (en) * | 2019-07-16 | 2019-09-06 | 马鞍山市盈天钢业有限公司 | A kind of preparation method of the fixed protective materials for metal welded tube |
| CN110240489A (en) * | 2019-06-20 | 2019-09-17 | 西北工业大学 | Refractory ceramics based composites torque tube preparation method |
| CN112624784A (en) * | 2020-12-30 | 2021-04-09 | 青岛高泰新材料有限公司 | Manufacturing method of carbon charging frame |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105220087A (en) * | 2015-07-20 | 2016-01-06 | 西安科技大学 | A kind of high tough Ti (C, N) based ceramic metal matrix material and preparation method thereof |
| TWI602794B (en) * | 2016-03-14 | 2017-10-21 | National Chung-Shan Institute Of Science And Tech | Ceramic composite materials production methods |
| CN107445640A (en) * | 2016-10-12 | 2017-12-08 | 平顺县西沟龙鼎新材料科技有限公司 | A kind of manufacture method of C/SiC novel mechanical sealing rings |
| CN109320275A (en) * | 2018-10-09 | 2019-02-12 | 中国航空工业集团公司基础技术研究院 | A kind of preparation method of anti-oxidant SiC fiber reinforced ceramic matrix composites |
| CN109530491A (en) * | 2018-12-19 | 2019-03-29 | 浙江振兴阿祥集团有限公司 | A kind of non-lubricating rises type rounding die |
| CN109530491B (en) * | 2018-12-19 | 2024-06-07 | 浙江振兴阿祥集团有限公司 | Lubrication-free expansion rounding die |
| CN109627008A (en) * | 2019-01-17 | 2019-04-16 | 苏州宏久航空防热材料科技有限公司 | A kind of preparation method with laminated composite structure material |
| CN109627008B (en) * | 2019-01-17 | 2021-04-30 | 苏州宏久航空防热材料科技有限公司 | Preparation method of material with laminated composite structure |
| CN110240489A (en) * | 2019-06-20 | 2019-09-17 | 西北工业大学 | Refractory ceramics based composites torque tube preparation method |
| CN110205811A (en) * | 2019-07-16 | 2019-09-06 | 马鞍山市盈天钢业有限公司 | A kind of preparation method of the fixed protective materials for metal welded tube |
| CN112624784A (en) * | 2020-12-30 | 2021-04-09 | 青岛高泰新材料有限公司 | Manufacturing method of carbon charging frame |
| CN112624784B (en) * | 2020-12-30 | 2022-09-23 | 青岛高泰新材料有限公司 | Manufacturing method of carbon charging frame |
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