CN106977222A - A kind of preparation method of short fiber reinforced carbon/silicon carbide ceramic matrix composite - Google Patents
A kind of preparation method of short fiber reinforced carbon/silicon carbide ceramic matrix composite Download PDFInfo
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- CN106977222A CN106977222A CN201710256633.2A CN201710256633A CN106977222A CN 106977222 A CN106977222 A CN 106977222A CN 201710256633 A CN201710256633 A CN 201710256633A CN 106977222 A CN106977222 A CN 106977222A
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- silicon carbide
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- C04B35/806—
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- 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
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Abstract
The present invention is a kind of preparation method of silicon carbide fiber reinforced ceramic matric composite, this method is used as reinforcement using chopped carbon fiber or chopped silicon carbide fibre etc., using high viscosity dispersing agent for fibre as chopped strand dispersant and the stabilizer of sintering aid and silicon carbide powder, realize that fiber is mixed with sintering aid, the uniform of silicon carbide powder.Meanwhile, the residual carbon obtained after the carbonization of high viscosity dispersant is as one of sintering aid of silicon carbide powder.Use pressure sintering, hot isostatic pressing method or discharge plasma sintering method for forming method, prepare short fiber reinforced carbon/silicon carbide ceramic matrix composite.This method avoid the shortcoming for disperseing uneven and thus caused poor mechanical property in traditional chopped strand matrix, the Fiber In Composite Material of preparation is evenly distributed, and fiber volume fraction can be in 10%~60% interval interior regulation and control, good mechanical performance.
Description
Technical field
The present invention is a kind of preparation method of short fiber reinforced carbon/silicon carbide ceramic matrix composite, belongs to composite preparation
Technical field.
Background technology
FRCMC has a wide range of applications field.In military domain, due to its have high temperature resistant,
The performances such as good toughness, excellent in oxidation resistance, and it is widely used in aero-engine, sky and space plane and rocket tail spray position；
Civil area, the fields such as sealing ring, brake disc are widely used in due to possessing the performances such as the good, rub resistance of wearability.At present, even
Continuing silicon carbide fiber reinforced ceramics mainly has chemical vapor infiltration, polymer infiltration and pyrolysis method, melting siliconising method and pressure sintering
Prepare.Because Continuous Fiber Reinforced Ceramic Matrix Composites prepare cost height, therefore it is mainly used in military field.Chopped fiber increases
Strong carborundum based material has important value due to possessing the characteristics such as cost is low, the cycle is short in civil area.
Patent CN101314543A describes a kind of preparation method of short carbon fiber toughened silicon carbide composite material, its feature
It is to be modified silicon-carbide particle surface, slurry is prepared using ball-milling technology, dries slurry and granulation processing, mould are carried out to powder
It is molded, hot pressed sintering biscuit.Patent CN101555144B describe a kind of silicon carbide short fiber toughened silicon carbide ceramics and its
The method of preparation.The method of the patent report constitutes main former material using silicon carbide powder, yttrium-aluminium-garnet and carborundum brief fiber
Material, fiber reinforcement short fiber reinforced ceramic base composite wood is prepared using ball milling mixing, granulation, dry-pressing formed and non-pressure sintering technology
Material.Silicon carbide powder is made into slurry and chopped fiber by way of ultrasonic disperse by patent CN1600744A, makes fiber in matrix
In it is fully dispersed, dry after unsticking, prepare short fiber reinforced silicon carbide compound finally by plasma discharging flash sintering method
Material.Patent CN103204693A, which discloses a kind of chopped carbon fiber, strengthens the method for carbon/silicon carbide ceramic matrix composite.First,
Chopped carbon fiber is removed photoresist and is roughened pretreatment, then by chopped carbon fiber, carborundum powder and sintering aid ball mill mixing, after drying
It is molded using discharge plasma sintering instrument.US201313772389 discloses a kind of silicon carbide fiber reinforced based composites and is used in combination
In the method for brake disc, composite is made up of chopped carbon fiber, carbon, silicon and carborundum, and carbon and silicon are rich in the patent matrix.
The above method is using the method sintered silicon carbon of additional sintering aid or infiltration, and due to fiber and powder
Density is different, easily non-uniform phenomenon occurs in mixing process.It is in the above method to use oxide as sintering aid more, and aoxidize
Carbon/silicon carbide ceramic matrix composite corrosion resistance, the heat-resisting quantity prepared when thing is as sintering aid is relatively low.
The content of the invention
The present invention is exactly designed for above-mentioned problems of the prior art there is provided a kind of carbonization of short fiber reinforced
The preparation method of silicon ceramic matric composite, its purpose realizes chopped strand and mixed with the uniform of powder, and prepare it is compound
Material oxide-free, with corrosion-resistant, resistant to elevated temperatures characteristic.
The purpose of the present invention is achieved through the following technical solutions：
The step of preparation method of this kind of silicon carbide fiber reinforced ceramic matric composite, is as follows：
Step 1: dispersing agent for fibre is soluble in water, aqueous dispersant is obtained, the weight of dispersing agent for fibre is water weight
0.3~1.5%；
Step 2: length is scattered in the aqueous dispersant that step one is prepared for 3~20mm chopped fiber, machinery is stirred
1~20h is mixed, fiber aqueous dispersion is obtained, the volume of chopped fiber is whole silicon carbide fiber reinforced ceramic matric composite body
Long-pending 10~60%；
Step 3: being scattered in the fiber point of step 2 preparation using silicon carbide powder and as carbon dust, the boron powder of sintering aid
In aproll solution, chopped strand and powder mixture are obtained, 0.5~2h of mechanical agitation, the weight of carbon dust is carborundum powder body weight
The 0.1~5% of amount, the weight of boron powder is the 0.1~1% of carborundum powder body weight；
Dried Step 4: chopped strand and powder mixture that step 3 is obtained are placed in baking oven, drying temperature is 80
~200 DEG C；
Arranged Step 5: dried chopped strand and powder mixture that step 4 is obtained are placed in inert atmosphere stove
Glue, dump temperature is 500~1200 DEG C, 0.5~2h of soaking time；
Step 6: the chopped strand and powder mixture after dumping are put into graphite jig, 1600~2100 DEG C it
Between, it is molded between 20~40MPa of pressure limit, obtains silicon carbide fiber reinforced ceramic matric composite.
Dispersing agent for fibre described in step one is hydroxymethyl cellulose or hydroxyethyl cellulose.
Forming method described in step 5 is plasma agglomeration method, hot pressing sintering method or hot isostatic pressing method.
Advantages of the present invention and feature：
1. the present invention has the stabilizer function of powder using highly viscous dispersing agent for fibre simultaneously, contribute to fiber and powder
Body it is dispersed；
2. the high viscosity dispersant of the present invention is changed into carbon after inert atmosphere processing, the carbon dust and boron powder with addition are common
It is used as sintering aid, it is to avoid impurity occur in material system；
3. the present invention is helped from carbon and boron as sintering aid, rather than using oxide or Nitride systems as sintering
Agent, is conducive to the raising of matrix high temperature resistant and decay resistance；
4. the chopped strand enhancing carbon/silicon carbide ceramic matrix composite that the present invention is used, with simple production process, production
The free of contamination feature of process, suitable for batch production.
Embodiment
Illustrate the preparation method of short fiber reinforced carbon/silicon carbide ceramic matrix composite below in conjunction with instantiation.
Embodiment 1
The step of preparing the method for silicon carbide fiber reinforced ceramic matric composite is as follows：
Step 1: 0.4g dispersing agent for fibres are dissolved in 400g water, aqueous dispersant is obtained；
Step 2: 3.65g length is scattered in the aqueous dispersant that step one is prepared for 8mm chopped fiber, machinery
10h is stirred, fiber aqueous dispersion is obtained；
Step 3: being scattered in step using 15g silicon carbide powders and as 0.4g graphite powders, the 0.08g boron powder of sintering aid
In the two fiber aqueous dispersions prepared, chopped strand and powder mixture, mechanical agitation 1h are obtained；
Dried Step 4: chopped strand and powder mixture that step 3 is obtained are placed in baking oven, drying temperature is 150
DEG C, drying time 4h；
Arranged Step 5: dried chopped strand and powder mixture that step 4 is obtained are placed in inert atmosphere stove
Glue, dump temperature is 1000 DEG C, heating rate 10 DEG C/min, soaking time 0.5h；
Step 6: the chopped strand and powder mixture after dumping are put into graphite jig, using plasma discharging method,
At 1800 DEG C, soaking time 5min is molded under pressure 35MPa, obtains fiber volume fraction and account for 30% or so fiber increasing
Strong carbon/silicon carbide ceramic matrix composite.
Embodiment 2
The step of preparing the method for silicon carbide fiber reinforced ceramic matric composite is as follows：
Step 1: 4g dispersing agent for fibres are dissolved in 4000g water, aqueous dispersant is obtained；
Step 2: 12.2g length is scattered in the aqueous dispersant that step one is prepared for 12mm chopped fiber, machinery
10h is stirred, fiber aqueous dispersion is obtained；
Step 3: being scattered in step using 210g silicon carbide powders and as 5.2g graphite powders, the 1.1g boron powder of sintering aid
In the two fiber aqueous dispersions prepared, chopped strand and powder mixture, mechanical agitation 1h are obtained；
Dried Step 4: chopped strand and powder mixture that step 3 is obtained are placed in baking oven, drying temperature is 150
DEG C, drying time 4h；
Arranged Step 5: dried chopped strand and powder mixture that step 4 is obtained are placed in inert atmosphere stove
Glue, dump temperature is 1000 DEG C, heating rate 10 DEG C/min, soaking time 0.5h；
Step 6: the chopped strand and powder mixture after dumping are put into graphite jig, using pressure sintering, 1800
DEG C, soaking time 2h is molded under pressure 35MPa, obtain fiber volume fraction account for 10% or so it is silicon carbide fiber reinforced
Ceramic matric composite.
Embodiment 3
The step of preparing the method for silicon carbide fiber reinforced ceramic matric composite is as follows：
Step 1: 0.4g dispersing agent for fibres are dissolved in 400g water, aqueous dispersant is obtained；
Step 2: 1.65g length is scattered in the aqueous dispersant that step one is prepared for 10mm chopped fiber, machinery
10h is stirred, fiber aqueous dispersion is obtained；
Step 3: being scattered in step using 21g silicon carbide powders and as 0.52g graphite powders, the 0.11g boron powder of sintering aid
In the two fiber aqueous dispersions prepared, chopped strand and powder mixture, mechanical agitation 1h are obtained；
Dried Step 4: chopped strand and powder mixture that step 3 is obtained are placed in baking oven, drying temperature is 150
DEG C, drying time 4h；
Arranged Step 5: dried chopped strand and powder mixture that step 4 is obtained are placed in inert atmosphere stove
Glue, dump temperature is 1000 DEG C, heating rate 10 DEG C/min, soaking time 0.5h；
Step 6: the chopped strand and powder mixture after dumping are put into graphite jig, using plasma discharging method,
At 1800 DEG C, soaking time 5min is molded under pressure 35MPa, obtains fiber volume fraction and account for 10% or so fiber increasing
Strong carbon/silicon carbide ceramic matrix composite.
Claims (3)
1. a kind of preparation method of silicon carbide fiber reinforced ceramic matric composite, it is characterised in that：The step of this method, is as follows：
Step 1: dispersing agent for fibre is soluble in water, aqueous dispersant is obtained, the weight of dispersing agent for fibre is water weight
0.3~1.5%；
Step 2: length is scattered in the aqueous dispersant that step one is prepared for 3~20mm chopped fiber, mechanical agitation 1
~20h, obtains fiber aqueous dispersion, the volume of chopped fiber is whole silicon carbide fiber reinforced ceramic matric composite volume
10~60%；
Step 3: being scattered in the fiber disperse water of step 2 preparation using silicon carbide powder and as carbon dust, the boron powder of sintering aid
In solution, chopped strand and powder mixture are obtained, 0.5~2h of mechanical agitation, the weight of carbon dust is carborundum powder body weight
0.1~5%, the weight of boron powder is the 0.1~1% of carborundum powder body weight；
Dried Step 4: chopped strand and powder mixture that step 3 is obtained are placed in baking oven, drying temperature is 80~200
℃；
Step 5: dried chopped strand and powder mixture that step 4 is obtained are placed in dumping in inert atmosphere stove, row
Glue temperature is 500~1200 DEG C, 0.5~2h of soaking time；
Step 6: the chopped strand and powder mixture after dumping are put into graphite jig, between 1600~2100 DEG C, pressure
It is molded between 20~40MPa of power scope, obtains silicon carbide fiber reinforced ceramic matric composite.
2. the preparation method of silicon carbide fiber reinforced ceramic matric composite according to claim 1, it is characterised in that：Step
Dispersing agent for fibre described in rapid one is hydroxymethyl cellulose or hydroxyethyl cellulose.
3. the preparation method of silicon carbide fiber reinforced ceramic matric composite according to claim 1, it is characterised in that：Step
Forming method described in rapid five is plasma agglomeration method, hot pressing sintering method or hot isostatic pressing method.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107778019A (en) * | 2017-10-12 | 2018-03-09 | 华中科技大学 | A kind of method for preparing silicon carbide whisker strengthening and toughening ceramic matric composite |
| CN108672249A (en) * | 2018-04-04 | 2018-10-19 | 北京石墨烯技术研究院有限公司 | A kind of anisotropic graphite alkene composite material and preparation method thereof |
| CN110436955A (en) * | 2019-07-23 | 2019-11-12 | 中国航发北京航空材料研究院 | A kind of modified SiC of yttriumf/ SiC ceramic based composites and preparation method thereof |
| CN111196724A (en) * | 2020-01-19 | 2020-05-26 | 湖南太子新材料科技有限公司 | Modified silicon carbide and preparation method thereof |
| CN112851384A (en) * | 2021-01-29 | 2021-05-28 | 中南大学 | Preparation method of low-temperature sintered ceramic matrix composite based on silicon carbide fiber reinforcement |
| CN115745642A (en) * | 2022-11-21 | 2023-03-07 | 湖南大学 | Chopped fiber reinforced boron carbide ceramic sheet and preparation method and application thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107778019A (en) * | 2017-10-12 | 2018-03-09 | 华中科技大学 | A kind of method for preparing silicon carbide whisker strengthening and toughening ceramic matric composite |
| CN107778019B (en) * | 2017-10-12 | 2021-01-15 | 华中科技大学 | Method for preparing silicon carbide whisker reinforced and toughened ceramic matrix composite |
| CN108672249A (en) * | 2018-04-04 | 2018-10-19 | 北京石墨烯技术研究院有限公司 | A kind of anisotropic graphite alkene composite material and preparation method thereof |
| CN110436955A (en) * | 2019-07-23 | 2019-11-12 | 中国航发北京航空材料研究院 | A kind of modified SiC of yttriumf/ SiC ceramic based composites and preparation method thereof |
| CN110436955B (en) * | 2019-07-23 | 2021-10-15 | 中国航发北京航空材料研究院 | Yttrium modified SiCf/SiC ceramic matrix composite material and preparation method thereof |
| CN111196724A (en) * | 2020-01-19 | 2020-05-26 | 湖南太子新材料科技有限公司 | Modified silicon carbide and preparation method thereof |
| CN112851384A (en) * | 2021-01-29 | 2021-05-28 | 中南大学 | Preparation method of low-temperature sintered ceramic matrix composite based on silicon carbide fiber reinforcement |
| CN112851384B (en) * | 2021-01-29 | 2022-07-08 | 中南大学 | Preparation method of low-temperature sintered ceramic matrix composite based on silicon carbide fiber reinforcement |
| CN115745642A (en) * | 2022-11-21 | 2023-03-07 | 湖南大学 | Chopped fiber reinforced boron carbide ceramic sheet and preparation method and application thereof |
| CN115745642B (en) * | 2022-11-21 | 2023-05-09 | 湖南大学 | Chopped fiber reinforced boron carbide ceramic sheet and preparation method and application thereof |
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Application publication date: 20170725 |