CN108395266A - A kind of preparation method of fiber reinforcement multiphase ceramic matrix composite - Google Patents

A kind of preparation method of fiber reinforcement multiphase ceramic matrix composite Download PDF

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CN108395266A
CN108395266A CN201810269910.8A CN201810269910A CN108395266A CN 108395266 A CN108395266 A CN 108395266A CN 201810269910 A CN201810269910 A CN 201810269910A CN 108395266 A CN108395266 A CN 108395266A
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powder
silicon carbide
preparation
obtains
fiber
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杨金华
焦健
姜卓钰
刘虎
焦春荣
吕晓旭
周怡然
杨瑞
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AECC Beijing Institute of Aeronautical Materials
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AECC Beijing Institute of Aeronautical Materials
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    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
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    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
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    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
    • C04B2235/5216—Inorganic
    • C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • C04B2235/5248—Carbon, e.g. graphite

Abstract

The present invention is a kind of preparation method of fiber reinforcement multiphase ceramic matrix composite, this method is using carbon fiber or silicon carbide fibre as reinforcement, fiber prepreg material is prepared in conjunction with slurry process, and then fiber reinforcement multiphase ceramic matrix composite is prepared by hot-forming, charing, infiltration.The present invention directly adds ZrB in slurry2、ZrC、HfB2, the powders such as HfC, to introduce superhigh temperature constituent element, improve the superhigh temperature resistant performance of composite material, this method avoid traditional fibre enhancing ultra-temperature ceramic-based composite material long preparation period, disadvantage of high cost, can short cycle, low cost prepare the ultra-temperature ceramic-based composite material haveing excellent performance.

Description

A kind of preparation method of fiber reinforcement multiphase ceramic matrix composite
Technical field
The present invention is a kind of preparation method of fiber reinforcement multiphase ceramic matrix composite, belongs to composite material technology of preparing Field.
Background technology
Silicon carbide fibre enhancing ceramic matric composite has a wide range of applications field, since it is with high temperature resistant, toughness The performances such as good, excellent in oxidation resistance, and it is widely used in aero-engine, sky and space plane and rocket tail spray position, usually such as Fruit matrix is silicon carbide substrate, and the temperature in use of composite material is no more than 1650 DEG C, and by adding superhigh temperature pottery in the base Porcelain component, such as ZrC, HfC etc., the complex phase ceramic matrix composite prepared can greatly improve the temperature in use of material.
Patent CN10397997A describes a kind of C/SiC-HfB2The preparation method of-HfC multiphase ceramic matrix composites, B is introduced in fibre reinforced composites precast body using vacuum pressure impregnating method first4C and C organic precursors, in conjunction with silicon-hafnium Alloy reacts infiltration method of impregnation and generates SiC, HfB2With HfC.One light of king et al. (Yiguang Wang, Wen Liu, et al.Preparation and properties of 2D C/SiC ultra high temperature ceramic Composites, Materials sciences and engineering, 2009, A524,129-133) ZrB will be coated2 CVD SiC matrix prepares C/SiC-ZrB after grain Polycarbosilane slurry two dimension carbon cloth stacks solidification cracking2It is compound Material, the composite material interlayer binding force for adopting this method preparation are poor.Patent CN102515870A describes a kind of fiber The preparation method for enhancing multiphase ceramic matrix composite, using pressure impregnation method by B4C introduces C/SiC with carbon organic precursor method and answers It in condensation material, is cracked again after solidification, and then C/SiC-ZrB is prepared by silicozirconium reactive melt infiltration method2- ZrC superhigh temperature Composite material.Patent CN104311090A describes a kind of preparation method of multiphase ceramic matrix composite, using hot pressed sintering Method combination polymer infiltration and pyrolysis method prepares Cf/ZrC-SiC composite materials.
In the above-mentioned method for preparing multiphase ceramic matrix composite, if using precast body as raw material, and then using true The generation for phenomena such as empty infusion process is easy to cause plug-hole when introducing powder, causes slurry to be unevenly distributed in precast body, especially It is the core of precast body；Zirconium carbide, zirconium diboride, hafnium carbide or two boronations are introduced by the way of silicozirconium or silicon-hafnium alloy The amount that the mode of hafnium introduces superhigh temperature ceramics component is limited, it is difficult to increase substantially the superelevation temperature characteristics of material；Using presoma When impregnating cracking technology prepares composite material, have the shortcomings that the period is long, inter-layer bonding force is low and of high cost；Using hot pressing legal system When standby composite material, although the introduction volume of ultra-high temperature ceramic powder can be increased substantially, such technique is only applicable in and prepares The composite element of simple shape and hot-forming higher for equipment requirement, therefore cost is higher.Prepreg-infiltration work Skill is a kind of low cost, short cycle and is suitble to prepare the ceramic matric composite preparation method of complex component, and this method at present may be used To prepare silicon carbide fiber reinforced silicon carbide ceramic matrix composite.
Invention content
The present invention exactly for the above-mentioned prior art the problem of and design and provide a kind of fiber reinforcement complex phase pottery The preparation method of porcelain based composites, this method realize the molding of complex component by the form of prepreg overlay, the purpose is to The preparation that complex phase ceramic matrix is realized by the method for being introduced directly into ultra-high temperature ceramic powder in slurry keeps the ceramic base of preparation multiple Condensation material has the effect of superhigh temperature resistant, shortens manufacturing cycle, reduces cost, convenient for preparing large-scale, complex component.
The purpose of the present invention is achieved through the following technical solutions：
The preparation method of this kind of fiber reinforcement multiphase ceramic matrix composite, it is characterised in that：The step of this method, is as follows：
Step 1: carbon fiber or silicon carbide fibre are woven into two-dimentional cloth；
Step 2: preparing boundary layer in fiber surface, boundary layer is two layer interface layer structure, and wherein inner boundary layer is pyrolysis The thickness of carbon boundary layer or boron nitride boundary layer, sublayer boundary layer is 0.1~1 μm, and outer interfacial layer is SiC boundary layers, thickness It is 0.1-5 μm；
Step 3: silicon carbide powder, ultra-high temperature ceramic powder, high carbon residue resin, pore creating material resin and solvent are uniformly mixed It closes, and ball milling 5 hours, obtains slurry, wherein：The mass fraction of silicon carbide powder is 50 parts, the quality of ultra-high temperature ceramic powder Number is 50~200 parts, and the mass fraction of high carbon residue resin is 5~20 parts, and the mass fraction of pore creating material resin is 1~10 part, The mass fraction of solvent is 100~600 parts；
The ultra-high temperature ceramic powder is the mixture of zirconium diboride powder, Zirconium carbide powder or the two, or
The ultra-high temperature ceramic powder is the mixture of hafnium boride powder, hafnium carbide powder or the two；
Step 4: step 3, which is obtained slurry, uniformly brushes the fiber cloth surface prepared to step 2, juxtaposition is at room temperature It is 5~48 hours dry, obtain prepreg；
Step 5: the prepreg that step 4 obtains is placed in laying in mold, and it is molded using press or autoclave, Forming temperature is 100~300 DEG C, and briquetting pressure is 0.1~10MPa, obtains precast body；
It is carbonized Step 6: the precast body that step 5 obtains is placed in high temperature furnace, carbonization temperature is 800~1200 DEG C Between, soaking time 0.2-2h obtains porous body；
Step 7: obtained porous body is placed in graphite crucible, infiltration is carried out to it using metal powder, infiltrating temperature is Between 1350~1800 DEG C, atmosphere is vacuum atmosphere, obtains fiber reinforcement multiphase ceramic matrix composite；
The metal powder is one in silica flour or silicon-base alloy powder, zirconium powder, zirconium-base alloy powder, hafnium powder or hafnium base alloy powder Kind.
Two-dimentional cloth described in step 1 is plain cloth, twills or satin fabric.
High carbon residue resin is one or more of phenolic resin, furane resins or pitch；Mixture.
Pore creating material resin is the mixture of one or more of PVA resins, epoxy resin, PVP resins, PMMA resins.
Solvent is the mixture of one or more of ethyl alcohol, methanol, toluene, dimethylbenzene, furans, acetone.
The advantages and features of the present invention：
1. the present invention directly adds ZrB in slurry preparation process2、ZrC、HfB2, the powders such as HfC, to introduce superelevation Warm constituent element improves the superhigh temperature resistant performance of composite material, and temperature in use is more than 1600 DEG C, which has simple, fast Prompt feature；
2. the present invention prepares composite material flat plate part or composite material complex component by the way of two-dimentional cloth laying, rather than The mode of braiding may be implemented the near-net-shape of flat part or complex component, greatly reduce post-production；
3. the invention avoids traditional fibre enhancing ultra-temperature ceramic-based composite material long preparation period, of high cost lacking Point, can short cycle, low cost prepare the composite material haveing excellent performance, be suitable for batch production fiber reinforcement it is ultra-temperature ceramic-based Composite material.
Specific implementation mode
Illustrate the preparation method of silicon carbide fiber reinforced silicon carbide ceramic matric composite below in conjunction with specific example.
Embodiment 1
The step of preparing the method for fiber reinforcement multiphase ceramic matrix composite is as follows：
Step 1: by carbon fiber fibrage at two-dimentional plain；
Step 2: preparing boundary layer in carbon fiber surface, boundary layer is two layer interface layer structure, and wherein inner boundary layer is nitrogen Change boron boundary layer, the thickness of sublayer boundary layer is 0.5 μm, and outer interfacial layer is SiC boundary layers, and thickness is 0.5 μm；
Step 3: silicon carbide powder, zirconium diboride powder, high carbon residue resin, pore creating material resin are uniformly mixed with solvent, And ball milling 5 hours, wherein silicon carbide powder mass fraction are 50 parts, zirconium diboride powder quality number is 80 parts, high carbon residue tree Fat mass fraction is 10 parts, and pore creating material resin quality number is 10 parts, and solvent quality number is 200 parts；
Step 4: step 3, which is obtained slurry, uniformly brushes the fiber cloth surface prepared to step 2, juxtaposition is at room temperature It is 24 hours dry, obtain prepreg；
Step 5: the prepreg that step 4 obtains is placed in laying in mold, and it is molded using press, forming temperature It it is 200 DEG C, precast body is prepared in briquetting pressure 8MPa；
It is carbonized Step 6: the precast body that step 5 obtains is placed in high temperature furnace, carbonization temperature is 1000 DEG C, heat preservation Time 1h, obtains porous body；
Step 7: obtained porous body is placed in graphite crucible, using ZrSi2- Si alloy powders carry out infiltration to it, Infiltrating temperature is 1500 DEG C, and atmosphere is vacuum atmosphere, obtains fiber reinforcement ultra-temperature ceramic-based composite material.
Embodiment 2
The step of preparing the method for fiber reinforcement multiphase ceramic matrix composite is as follows：
Step 1: by carbon fiber fibrage at two-dimentional plain；
Step 2: preparing boundary layer in carbon fiber surface, boundary layer is two layer interface layer structure, and wherein inner boundary layer is nitrogen Change boron boundary layer, the thickness of sublayer boundary layer is 0.5 μm, and outer interfacial layer is SiC boundary layers, and thickness is 0.5 μm；
Step 3: silicon carbide powder, hafnium boride powder, high carbon residue resin, pore creating material resin are uniformly mixed with solvent, And ball milling 5 hours, wherein silicon carbide powder mass fraction are 50 parts, hafnium boride powder quality number is 80 parts, high carbon residue tree Fat mass fraction is 10 parts, and pore creating material resin quality number is 10 parts, and solvent quality number is 200 parts；
Step 4: step 3, which is obtained slurry, uniformly brushes the fiber cloth surface prepared to step 2, juxtaposition is at room temperature It is 24 hours dry, obtain prepreg；
Step 5: the prepreg that step 4 obtains is placed in laying in mold, and it is molded using press, forming temperature It it is 200 DEG C, precast body is prepared in briquetting pressure 8MPa；
It is carbonized Step 6: the precast body that step 5 obtains is placed in high temperature furnace, carbonization temperature is 1000 DEG C, heat preservation Time 1h, obtains porous body；
Step 7: obtained porous body is placed in graphite crucible, using HfSi2- Si alloy powders carry out infiltration to it, Infiltrating temperature is 1450 DEG C, and atmosphere is vacuum atmosphere, obtains fiber reinforcement ultra-temperature ceramic-based composite material.
Embodiment 3
The step of preparing the method for fiber reinforcement multiphase ceramic matrix composite is as follows：
Step 1: silicon carbide fibre is woven into two-dimentional plain；
Step 2: preparing boundary layer in carbon fiber surface, boundary layer is two layer interface layer structure, and wherein inner boundary layer is nitrogen Change boron boundary layer, the thickness of sublayer boundary layer is 0.5 μm, and outer interfacial layer is SiC boundary layers, and thickness is 0.5 μm；
Step 3: silicon carbide powder, hafnium boride powder, high carbon residue resin, pore creating material resin are uniformly mixed with solvent, And ball milling 5 hours, wherein silicon carbide powder mass fraction are 50 parts, hafnium boride powder quality number is 80 parts, high carbon residue tree Fat mass fraction is 10 parts, and pore creating material resin quality number is 10 parts, and solvent quality number is 200 parts；
Step 4: step 3, which is obtained slurry, uniformly brushes the fiber cloth surface prepared to step 2, juxtaposition is at room temperature It is 24 hours dry, obtain prepreg；
Step 5: the prepreg that step 4 obtains is placed in laying in mold, and it is molded using press, forming temperature It it is 200 DEG C, precast body is prepared in briquetting pressure 8MPa；
It is carbonized Step 6: the precast body that step 5 obtains is placed in high temperature furnace, carbonization temperature is 1000 DEG C, heat preservation Time 1h, obtains porous body；
Step 7: obtained porous body is placed in graphite crucible, using HfSi2- Si alloy powders carry out infiltration to it, Infiltrating temperature is 1450 DEG C, and atmosphere is vacuum atmosphere, obtains fiber reinforcement ultra-temperature ceramic-based composite material.

Claims (5)

1. a kind of preparation method of fiber reinforcement multiphase ceramic matrix composite, it is characterised in that：The step of this method, is as follows：
Step 1: carbon fiber or silicon carbide fibre are woven into two-dimentional cloth；
Step 2: preparing boundary layer in fiber surface, boundary layer is two layer interface layer structure, and wherein inner boundary layer is pyrolytic carbon circle The thickness of face layer or boron nitride boundary layer, sublayer boundary layer is 0.1~1 μm, and outer interfacial layer is SiC boundary layers, and thickness is 0.1-5μm；
Step 3: silicon carbide powder, ultra-high temperature ceramic powder, high carbon residue resin, pore creating material resin are uniformly mixed with solvent, and Ball milling 5 hours, obtains slurry, wherein：The mass fraction of silicon carbide powder is 50 parts, and the mass fraction of ultra-high temperature ceramic powder is 50~200 parts, the mass fraction of high carbon residue resin is 5~20 parts, and the mass fraction of pore creating material resin is 1~10 part, solvent Mass fraction is 100~600 parts；
The ultra-high temperature ceramic powder is the mixture of zirconium diboride powder, Zirconium carbide powder or the two, or
The ultra-high temperature ceramic powder is the mixture of hafnium boride powder, hafnium carbide powder or the two；
Step 4: step 3, which is obtained slurry, uniformly brushes the fiber cloth surface prepared to step 2, juxtaposition dries 5 at room temperature ~48 hours, obtain prepreg；
Step 5: the prepreg that step 4 obtains is placed in laying in mold, and it is molded, is molded using press or autoclave Temperature is 100~300 DEG C, and briquetting pressure is 0.1~10MPa, obtains precast body；
Carbonized Step 6: the precast body that step 5 obtains is placed in high temperature furnace, carbonization temperature be 800~1200 DEG C it Between, soaking time 0.2-2h obtains porous body；
Step 7: obtained porous body is placed in graphite crucible, infiltration, infiltrating temperature 1350 carry out it using metal powder Between~1800 DEG C, atmosphere is vacuum atmosphere, obtains fiber reinforcement multiphase ceramic matrix composite；
The metal powder is one kind in silica flour or silicon-base alloy powder, zirconium powder, zirconium-base alloy powder, hafnium powder or hafnium base alloy powder.
2. the preparation method of silicon carbide fiber reinforced ceramic matric composite according to claim 1, it is characterised in that：Step Two-dimentional cloth described in rapid one is plain cloth, twills or satin fabric.
3. the preparation method of silicon carbide fiber reinforced ceramic matric composite according to claim 1, it is characterised in that：It is high Carbon residue resin is one or more of phenolic resin, furane resins or pitch；Mixture.
4. the preparation method of silicon carbide fiber reinforced ceramic matric composite according to claim 1, it is characterised in that：It makes Agent resin in hole is the mixture of one or more of PVA resins, epoxy resin, PVP resins, PMMA resins.
5. the preparation method of silicon carbide fiber reinforced ceramic matric composite according to claim 1, it is characterised in that：It is molten Agent is the mixture of one or more of ethyl alcohol, methanol, toluene, dimethylbenzene, furans, acetone.
CN201810269910.8A 2018-03-28 2018-03-28 A kind of preparation method of fiber reinforcement multiphase ceramic matrix composite Pending CN108395266A (en)

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Cited By (28)

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CN109485449A (en) * 2019-01-11 2019-03-19 哈尔滨工业大学 A method of density gradient heat insulation material is prepared based on capillarity
CN109704799A (en) * 2019-02-27 2019-05-03 山东工业陶瓷研究设计院有限公司 The preparation method of ceramic matric composite
CN110317073A (en) * 2019-07-09 2019-10-11 中国航发北京航空材料研究院 A kind of preparation method of multistage fiber coordination plasticizing oxidation-resistant ceramic based composites
CN110357648A (en) * 2019-07-09 2019-10-22 中国航发北京航空材料研究院 A method of preparing multistage multiple dimensioned fiber reinforced ceramic matric composite
CN110467473A (en) * 2019-08-02 2019-11-19 中国航发北京航空材料研究院 A kind of preparation method of alumina fibre enhancing alumina ceramic-base composites
CN110563479A (en) * 2019-10-25 2019-12-13 航天特种材料及工艺技术研究所 Ultrahigh-temperature ceramic matrix composite and preparation method thereof
CN111253161A (en) * 2020-01-20 2020-06-09 陕西科技大学 SiCf-ZrC-ZrB2Ceramic composite powder and preparation method thereof
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CN111747764A (en) * 2020-06-10 2020-10-09 中国航发北京航空材料研究院 Preparation method of silicon carbide fiber reinforced silicon carbide composite material capable of generating ZrB2-ZrC in situ
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