CN104086203B - Preparation method of crystal whisker/fiber synergic reinforced ceramic-base composite material - Google Patents
Preparation method of crystal whisker/fiber synergic reinforced ceramic-base composite material Download PDFInfo
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- CN104086203B CN104086203B CN201410333870.0A CN201410333870A CN104086203B CN 104086203 B CN104086203 B CN 104086203B CN 201410333870 A CN201410333870 A CN 201410333870A CN 104086203 B CN104086203 B CN 104086203B
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Abstract
The invention discloses a preparation method of a crystal whisker/fiber synergic reinforced ceramic-base composite material, which is used for solving the technical problem of poor bending strength in the material prepared by the existing C/SiC composite material preparation method. The technical scheme is as follows: the preparation method comprises the following steps: uniformly dispersing pretreated crystal whiskers by ball milling, uniformly brushing the crystal whiskers onto every carbon fiber cloth layer by a slurry brushing process, naturally drying, laminating, puncturing and sewing the lamination together with carbon fibers to prepare a crystal whisker fiber precast body, depositing a pyrolytic carbon interface layer on the crystal whisker fiber precast body by a gas-phase permeation process, and finally, depositing the SiC base for compaction. The introduced crystal whiskers are uniformly distributed in the lamination direction, and the binary synergic enhancement effect is utilized to enhance the strength and toughness of the C/SiC composite material. The test proves that the bending strength of the C/SiC composite material is enhanced from 235 MPa in the background art to 381-466 MPa under identical conditions.
Description
Technical field
The present invention relates to a kind of preparation method of ceramic matric composite, particularly relate to the preparation method of a kind of whisker and fiber cooperative reinforcing ceramic matric composite.
Background technology
Silicon carbide whisker is that a kind of defect is less, there is the single crystal fibre of certain length-to-diameter ratio, having high-melting-point, low density, high strength, high elastic coefficient, low-thermal-expansion rate and wear-resisting, corrosion-resistant, the characteristic such as high temperature resistant property is strong, is a kind of desirable reinforcing and toughening material.The effects such as the crack deflection utilizing whisker to produce, whiosker pullout and bridging, can significantly improve the mechanical property of crystal whisker toughened matrix material.
Document " CVI-C/SiC composite preform structure and mechanical property [D]. Xi'an: Northwestern Polytechnical University; 2009 05 month " disclose one and utilize chemical vapor infiltration (CVI) to prepare the method for C/SiC matrix material, first multilayer plain weave carbon fiber cloth superposes by the method, then with carbon fiber, lamination puncture is stitched together, deposit RESEARCH OF PYROCARBON interfacial layer again, finally deposit SiC matrix, obtain C/SiC matrix material.Although the method can avoid direct high-temperature heat treatment to cause damage to carbon fiber performance, the bending strength of the C/SiC material of preparation reduces, when density is 2.0 ~ 2.1g/cm
3time, its bending strength is only 235MPa, can not meet the requirement of high-end field to material property.
Silicon carbide whisker has excellent performance, but is introduced in continuous carbon fibre precast body, improves the mechanical property of C/SiC matrix material, yet there are no open report.
Summary of the invention
In order to overcome the deficiency of material bending strength difference prepared by existing C/SiC composite material and preparation method thereof, the invention provides the preparation method of a kind of whisker and fiber cooperative reinforcing ceramic matric composite.First the method adopts ball milled by dispersed for the whisker that pre-treatment is good, then slurry squeegee process is adopted to be brushed to by whisker on every one deck carbon cloth equably, seasoning lamination, with carbon fiber, lamination puncture is stitched together and is prepared into whisker fibre precast body again, chemical vapor infiltration (CVI) is adopted to deposit RESEARCH OF PYROCARBON interfacial layer on this basis on whisker fibre precast body, finally deposit SiC matrix and carry out densification, complete SiC
wthe preparation of-C/SiC matrix material.The SiC of enhancing worked in coordination with by whisker prepared by the method and fiber
w-C/SiC matrix material, the whisker of introducing distributes equably on laying direction, can give full play to the crack deflection of whisker, whiosker pullout and bridge linking effect, utilizes binary to work in coordination with the effect of enhancing, can improve the obdurability of C/SiC matrix material.
The technical solution adopted for the present invention to solve the technical problems is: the preparation method of a kind of whisker and fiber cooperative reinforcing ceramic matric composite, is characterized in adopting following steps:
Step one, take first volume fraction as the alcohol of 20% be solution, adopt the method dispersion SiC of ultrasonic disperse and magnetic agitation
wwhisker, wherein ultrasonic 30 minutes, magnetic agitation 2 hours, dried;
Step 2, with Virahol and toluene for solvent, through the SiC that step one processes
wwhisker is solute, and triethyl phosphate, as dispersion agent ball milling 10h, makes slurry.SiC
wwhisker control 5 ~ 15%.
Step 3, in the slurry made, add polyvinyl butyral acetal as binding agent, glycerol as softening agent, ball milling 8h, obtains stable SiC
wslurry.
Step 4, the SiC that brushing one deck step 3 prepares on several 2D [0 °/90 °] carbon cloth
wslurry, seasoning;
Step 5, be with SiC by step 4
w2D [0 °/90 °] carbon cloth lamination successively;
Step 6, by the sizing graphite template of two pieces of porous by the carbon cloth lamination clamping in step 5, adopt relay-type needle-punching method template and middle lamination carbon cloth to be sewed up, obtain scribbling SiC
wthe precast body of fiber;
Step 7, adopt chemical Vapor deposition process to obtain in step 6 precast body on deposit RESEARCH OF PYROCARBON interfacial layer, processing condition are: depositing temperature 800 ~ 900 DEG C, pressure 0.2 ~ 0.4kPa, propylene flow 25 ~ 35ml/min, Ar airshed 250 ~ 350ml/min, depositing time 40 ~ 60h;
Step 8, employing CVI deposit SiC matrix, processing condition are as follows: trichloromethyl silane is source material, argon gas is diluent gas, argon flow amount 300 ~ 400ml/min, hydrogen is carrier gas, hydrogen flowing quantity 200 ~ 350ml/min, and the mol ratio of hydrogen and trichloromethyl silane is 10:1, depositing temperature is 1000 ~ 1100 DEG C, depositing time 160 ~ 200h;
Repeating step eight after step 9, form removal, obtains fine and close SiC
wafter-C/SiC matrix material, roughing is carried out to material surface, reduce hole of holding one's breath;
Step 10, again repeating step eight, obtain SiC
wwith the SiC based composites of continuous carbon fibre cooperative reinforcing.
By controlling the number of plies control SiC of brushing whisker carbon cloth
wthe number of plies of-C/SiC matrix material and thickness, the volume fraction controlling whisker slurry controls Whisker Content.
The invention has the beneficial effects as follows: first the method adopts ball milled by dispersed for the whisker that pre-treatment is good, then slurry squeegee process is adopted to be brushed to by whisker on every one deck carbon cloth equably, seasoning lamination, with carbon fiber, lamination puncture is stitched together and is prepared into whisker fibre precast body again, chemical vapor infiltration (CVI) is adopted to deposit RESEARCH OF PYROCARBON interfacial layer on this basis on whisker fibre precast body, finally deposit SiC matrix and carry out densification, complete SiC
wthe preparation of-C/SiC matrix material.The SiC of enhancing worked in coordination with by whisker prepared by the method and fiber
w-C/SiC matrix material, the whisker of introducing distributes equably on laying direction, can give full play to the crack deflection of whisker, whiosker pullout and bridge linking effect, utilizes binary to work in coordination with the effect of enhancing, improves the obdurability of C/SiC matrix material.After tested, under the same terms, C/SiC matrix material flexural strength brings up to 381 ~ 466MPa by the 235MPa of background technology.
Below in conjunction with the drawings and specific embodiments, the present invention is elaborated.
Accompanying drawing explanation
Fig. 1 is the schema of the preparation method of whisker of the present invention and fiber cooperative reinforcing ceramic matric composite.
Fig. 2 is SiC prepared by the inventive method embodiment 1
w-C/SiC fracture of composite materials surface microstructure figure.
Fig. 3 is SiC prepared by the inventive method embodiment 1
w-C/SiC fracture of composite materials surface SiC
wwhiosker pullout schematic diagram.
Embodiment
Following examples are with reference to Fig. 1-3.
Embodiment 1:(1) adopt length-to-diameter ratio be 8 ~ 11 SiC
wwhisker as reinforcement, using volume fraction be 20% alcohol as solution, ultrasonic 30 minutes, magnetic agitation 2 hours, dry;
(2) with Virahol and toluene for solvent, SiC in step (1)
wwhisker is solute, and triethyl phosphate is as dispersion agent ball milling 10h, and whisker controls 5%.
(3) in the slurry of step (2), add polyvinyl butyral acetal (PVB) as binding agent, glycerol as softening agent, ball milling 8h, obtains stable SiC
wslurry.
(4) 5wt%SiC prepared in brushing one deck step (3) on 25 2D [0 °/90 °] carbon cloth
wwhisker slurry, seasoning;
(5) by step (4) with 5wt%SiC
w2D [0 °/90 °] the carbon cloth lamination successively of whisker; SiC as seen from Figure 2
wwhisker layer and carbon cloth layer are alternately folded mutually.
(6) by the sizing graphite template of two pieces of porous, above-mentioned carbon cloth lamination is clamped, adopt relay-type needle-punching method template and middle lamination carbon cloth to be sewed up, obtain scribbling 5wt%SiC
wthe fiber preform of whisker;
(7) precast body adopting chemical Vapor deposition process (CVD) to obtain in step (6) deposits RESEARCH OF PYROCARBON interfacial layer, processing condition are: depositing temperature 800 DEG C, pressure 0.4kPa, propylene flow 25ml/min, Ar airshed 250ml/min, depositing time 60h;
(8) CVI is adopted to deposit SiC matrix, processing condition are as follows: trichloromethyl silane is source material, argon gas is diluent gas (flow 300ml/min), hydrogen is carrier gas (flow 200ml/min), the mol ratio of hydrogen and trichloromethyl silane is 10:1, depositing temperature is 1000 DEG C, depositing time 200h;
(9) repeating step (8) after form removal, after obtaining finer and close C/SiC matrix material, carries out roughing to material surface, reduces hole of holding one's breath;
(10) repeating step (8) again, obtains 5wt%SiC
wthe SiC based composites of whisker and continuous carbon fibre cooperative reinforcing.As can be seen from Figure 3, the extracting of fracture surface of sample pattern place whisker.
SiC prepared by the present embodiment
w-C/SiC matrix material, compared with carbon/silicon carbide ceramic matrix (C/SiC) matrix material of the continuous lod prepared in background technology, flexural strength brings up to 466MPa by 235MPa, improves 98.5%.
Embodiment 2:(1) adopt length-to-diameter ratio be 8 ~ 11 SiC
wwhisker as reinforcement, using volume fraction be 20% alcohol as solution, ultrasonic 30 minutes, magnetic agitation 2 hours, dry;
(2) with Virahol and toluene for solvent, SiC in step (1)
wwhisker is solute, and triethyl phosphate is as dispersion agent ball milling 10h, and whisker controls 15%.
(3) in the slurry of step (2), add polyvinyl butyral acetal (PVB) as binding agent, glycerol as softening agent, ball milling 8h, obtains stable SiC
wslurry.
(4) 15wt%SiC prepared in brushing one deck step (3) on 25 2D [0 °/90 °] carbon cloth
wwhisker slurry, seasoning;
(5) by step (4) with 15wt%SiC
w2D [0 °/90 °] the carbon cloth lamination successively of whisker.
(6) by the sizing graphite template of two pieces of porous, above-mentioned carbon cloth lamination is clamped, adopt relay-type needle-punching method template and middle lamination carbon cloth to be sewed up, obtain scribbling 15wt%SiC
wthe fiber preform of whisker;
(7) precast body adopting chemical Vapor deposition process (CVD) to obtain in step (6) deposits RESEARCH OF PYROCARBON interfacial layer, processing condition are: depositing temperature 900 DEG C, pressure 0.2kPa, propylene flow 35ml/min, Ar airshed 350ml/min, depositing time 40h;
(8) CVI is adopted to deposit SiC matrix, processing condition are as follows: trichloromethyl silane is source material, argon gas is diluent gas (flow 400ml/min), hydrogen is carrier gas (flow 350ml/min), the mol ratio of hydrogen and trichloromethyl silane is 10:1, depositing temperature is 1100 DEG C, depositing time 160h;
(9) repeating step (8) after form removal, after obtaining finer and close C/SiC matrix material, carries out roughing to material surface, reduces hole of holding one's breath;
(10) repeating step (8) again, obtains 15wt%SiC
wthe SiC based composites of whisker and continuous fiber C cooperative reinforcing.
SiC prepared by the present embodiment
w-C/SiC matrix material, compared with carbon/silicon carbide ceramic matrix (C/SiC) matrix material of the continuous lod prepared in background technology, flexural strength brings up to 381MPa by 235MPa, improves 64.3%.
Claims (2)
1. a preparation method for whisker and fiber cooperative reinforcing ceramic matric composite, is characterized in that comprising the following steps:
Step one, take first volume fraction as the alcohol of 20% be solution, adopt the method dispersion SiC of ultrasonic disperse and magnetic agitation
wwhisker, wherein ultrasonic 30 minutes, magnetic agitation 2 hours, dried;
Step 2, with Virahol and toluene for solvent, through the SiC that step one processes
wwhisker is solute, and triethyl phosphate, as dispersion agent ball milling 10h, makes slurry; SiC
wwhisker control 5 ~ 15%;
Step 3, in the slurry made, add polyvinyl butyral acetal as binding agent, glycerol as softening agent, ball milling 8h, obtains stable SiC
wslurry;
Step 4, the SiC that brushing one deck step 3 prepares on several 2D [0 °/90 °] carbon cloth
wslurry, seasoning;
Step 5, be with SiC by step 4
w2D [0 °/90 °] carbon cloth lamination successively;
Step 6, by the sizing graphite template of two pieces of porous by the carbon cloth lamination clamping in step 5, adopt relay-type needle-punching method template and middle lamination carbon cloth to be sewed up, obtain scribbling SiC
wthe precast body of fiber;
Step 7, adopt chemical Vapor deposition process to obtain in step 6 precast body on deposit RESEARCH OF PYROCARBON interfacial layer, processing condition are: depositing temperature 800 ~ 900 DEG C, pressure 0.2 ~ 0.4kPa, propylene flow 25 ~ 35ml/min, Ar airshed 250 ~ 350ml/min, depositing time 40 ~ 60h;
Step 8, employing CVI deposit SiC matrix, processing condition are as follows: trichloromethyl silane is source material, argon gas is diluent gas, argon flow amount 300 ~ 400ml/min, hydrogen is carrier gas, hydrogen flowing quantity 200 ~ 350ml/min, and the mol ratio of hydrogen and trichloromethyl silane is 10:1, depositing temperature is 1000 ~ 1100 DEG C, depositing time 160 ~ 200h;
Repeating step eight after step 9, form removal, obtains fine and close SiC
wafter-C/SiC matrix material, roughing is carried out to material surface, reduce hole of holding one's breath;
Step 10, again repeating step eight, obtain SiC
wwith the SiC based composites of continuous carbon fibre cooperative reinforcing.
2. the preparation method of whisker according to claim 1 and fiber cooperative reinforcing ceramic matric composite, is characterized in that: by controlling the number of plies control SiC of brushing whisker carbon cloth
wthe number of plies of-C/SiC matrix material and thickness, the volume fraction controlling whisker slurry controls Whisker Content.
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| CN104446589B (en) * | 2014-12-24 | 2016-05-18 | 中南大学 | A kind of preparation method of whisker modified carbon/carbon compound material |
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| CN115536416B (en) * | 2022-08-28 | 2023-07-28 | 西北工业大学 | High-temperature high-strength high-density SiC/SiC composite material and preparation method thereof |
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| CN102964145A (en) * | 2012-12-04 | 2013-03-13 | 西北工业大学 | Method for preparing coating reinforced C/SiC composite material |
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