CN102161594A - SiC whisker reinforced SiC ceramic matrix composite and preparation method thereof - Google Patents

SiC whisker reinforced SiC ceramic matrix composite and preparation method thereof Download PDF

Info

Publication number
CN102161594A
CN102161594A CN 201110122040 CN201110122040A CN102161594A CN 102161594 A CN102161594 A CN 102161594A CN 201110122040 CN201110122040 CN 201110122040 CN 201110122040 A CN201110122040 A CN 201110122040A CN 102161594 A CN102161594 A CN 102161594A
Authority
CN
China
Prior art keywords
sic
prefabricated component
rice husk
product
infiltration
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN 201110122040
Other languages
Chinese (zh)
Other versions
CN102161594B (en
Inventor
高明霞
朱丹
潘颐
潘洪革
刘永锋
巫红燕
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhejiang University ZJU
Original Assignee
Zhejiang University ZJU
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Zhejiang University ZJU filed Critical Zhejiang University ZJU
Priority to CN 201110122040 priority Critical patent/CN102161594B/en
Publication of CN102161594A publication Critical patent/CN102161594A/en
Application granted granted Critical
Publication of CN102161594B publication Critical patent/CN102161594B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Ceramic Products (AREA)

Abstract

The invention belongs to the field of the preparation of ceramic matrix composites, and particularly relates to a SiC whisker reinforced SiC ceramic matrix composite and a preparation method thereof. The SiC whisker reinforced SiC ceramic matrix composite is prepared from a preform through a Si or Si alloy infiltration reaction, and the preform is prepared by compressing and molding a raw material comprising a rice hull SiC whiskerized product. By the method, the preparation process is simple, the temperature of the infiltration reaction is low, external pressure is not required, and the preform can be prepared into complicate shapes and can be used for preparing members with complicated shapes. A main composition phase SiC of the composite comes from rice hull, the raw material is rich, the cost is low, the manufacturing cost of the ceramic matrix composite can be remarkably reduced, the resource is saved and the environment is protected. The SiC ceramic matrix composite has good performance, SiC whiskers have the effect of strengthening materials, and the SiC whisker reinforced SiC ceramic matrix composite can be used for applicable occasions of SiC reaction sintering ceramic material products such as sliding bearings, corrosion-resistant and wear-resistant pipelines, valves and fan blades, military and civil body armors and the like.

Description

SiC ceramic matric composite that a kind of SiC whisker is strengthened and preparation method thereof
Technical field
The invention belongs to the preparation field of ceramic matric composite, relate in particular to SiC ceramic matric composite of a kind of SiC whisker reinforcement and preparation method thereof.
Background technology
Silicon carbide (SiC) stupalith is to be the stupalith of main component with silicon carbide.As a kind of structured material,, be widely used in every field such as modern national defense, nuclear energy, space technology and mechanical industry because it has big, the wear-resisting good characteristic such as resistance to chemical attack that undermines of hot strength height, good in oxidation resistance, thermal conductivity height, hardness.The main preparation methods of SiC stupalith comprises hot pressed sintering, HIP sintering, normal pressure-sintered and reaction sintering etc.Wherein, reaction sintering technology is the wider a kind of preparation technology of present application owing to have that equipment is simple, sintering temperature is low, can prepare the goods of various complicated shapes and realize advantage such as dead size moulding substantially.
In recent years, the research that utilizes natural reproducible resource to prepare thyrite enlivens, and comprises that with timber, bamboo, linen-cotton be raw material etc.As Chinese patent application CN 101434486A(publication number) " a kind of preparation method of SiC wood ceramics " disclosed, it is to be raw material with various timber, pre-treatment and the wood material carbonization of compressing are obtained the carbon template, obtain the SiC wood ceramics by liquid phase or gas phase siliconising then.Chinese patent application CN 101386538A(publication number and for example) " a kind of preparation method of SiC pottery " disclosed, this method be by with behind the bamboo charcoal powder breakdown mill with Si powder, resol etc. by certain mass than mixing, through preheating moulding, the final high temperature sintering obtains the SiC stupalith.
Rice husk is a kind of natural biological raw material, and China is maximum in the world paddy rice plantation country, and the rice husk resource is very abundant.Yet the rice husk surface is hard, and the silicone content height be difficult for by bacterial degradation, and tap density is little, has greatly destroyed environment if do discarded processing, becomes the burden of rice industry enterprise.The development and use of rice husk are for the protection environment, and the economic benefit that improves the paddy rice plantation is significant.Be that raw material is just obtaining research, development and utilization at aspects such as preparation white carbon black, silicon at present with the rice husk.But the utilization to rice husk also is nowhere near.Rice husk is rich in SiC whisker and SiC particulate product through further handling to generate again after the coking under comparatively high temps, but also realizes far away for effective utilization of this product.
Chinese invention patent (application number: the 201010202371.X applying date: 2010-06-18) disclose the method for utilizing rice husk to prepare nanometer-diameter carborundum brief fiber and whisker, this method is in plumbago crucible, rice husk behind the adding cleaning-drying, carbonization at a certain temperature in vacuum oven; Rice husk after the carbonization and one or both catalyzer mechanically mixing is even, or do not add catalyzer; Rice husk after mixing the rice husk after the catalysis or not adding the catalyzer carbonization is put into plumbago crucible, cover graphite cover, put into vacuum sintering furnace, feed protection of inert gas, heat up with given pace, subsequently cool to room temperature; Open sintering oven, cotton-shaped carborundum brief fiber and the whisker of rice husk upper surface adularescent produces in the plumbago crucible, and adularescent to light blue group wadding thing carborundum brief fiber and whisker generates between rice husk.
Chinese invention patent (application number: 200510042708.4 applyings date: 2005-05-24) disclose the method for preparing silicon carbide whisker, this method with rice husk after crushed, in 650 ℃~700 ℃ temperature range, adopt the carbonization technique that closes stove after the first blow-on that rice husk is carried out carbonization, add suitable catalyzer by certain weight ratio, after mixing, compound is packed in the plumbago crucible, carbon fiber is arranged in compound top, builds crucible cover.Plumbago crucible is put into the vertical vacuum furnace that graphite is made heating member, feed argon gas and protect, on carbon fiber, grow silicon carbide whisker.
Above-mentioned method all discloses rice husk and has prepared the method for silicon carbide whisker, but uses for the silicon carbide-containing crystal whisker products of preparation, and still rarer relevant document is announced.
Summary of the invention
Application for the silicon carbide-containing crystal whisker products of expanding rice husk preparation; improve the over-all properties of SiC ceramic matric composite; an object of the present invention is to provide the SiC ceramic matric composite that a kind of SiC whisker is strengthened; this matrix material is main raw material with the rice husk; raw material sources are wide, cost is low, renewable, can save resource and protection environment, improve the economic benefit of paddy rice plantation; the SiC ceramic matric composite of preparation has SiC whisker reinforcing property, over-all properties height.Second purpose of the present invention provides the preparation method of the SiC ceramic matric composite that a kind of above-mentioned SiC whisker strengthens.
In order to realize first above-mentioned purpose, the present invention has adopted following technical scheme:
The SiC ceramic matric composite that a kind of SiC whisker is strengthened, matrix material is obtained by Si or Si alloy infiltration prepared in reaction by prefabricated component, and described prefabricated component is made by the raw material compression molding that comprises rice husk SiC whiskerizing product.
As preferably, also comprise binding agent in the described prefabricated component, binding agent adds when difficult forming, and addition is convenient to moulding and is got final product; As preferred again, described binding agent is selected polyvinyl alcohol or resol for use.
As preferably, also comprise in carbon and the SiC powder body material one or both in the described prefabricated component.As preferred again, described carbon is selected from one or more in graphite, carbon black, decolorizing carbon and the refinery coke.As preferred again, the addition of described carbon is 0~40% of a prefabricated component total amount, and particle size is at 0.1~30 micron; The amount of the SiC powder that adds is in 0~40% of prefabricated component total amount, and particle is at 0.1~30 micron.
As preferably, also comprise Mo in the described prefabricated component, the amount that Mo adds is no more than half of the molar weight that presets infiltration Si or Si alloy.Add a small amount of Mo etc. and can form MoSi with Si 2Etc. high-melting point metal,, improve the hot strength of matrix material with the content of low melting point metals such as Si in the minimizing matrix material.
As preferably, described Si alloy is selected from a kind of among Al-Si, Mo-Si, Fe-Si and the Ni-Si, and wherein the content of Si is at 10~90wt%.
In order to realize second above-mentioned purpose, the present invention has adopted following technical scheme:
A kind of method for preparing the SiC ceramic matric composite of above-mentioned a kind of SiC whisker reinforcement, this method comprises the steps:
1) preparation of prefabricated component
To rice husk SiC whiskerizing product and remove other auxiliary materials of binding agent and grind and disperse, compression molding is prepared into prefabricated component then; When difficult forming, can add an amount of binding agent,, and can carry out the granulation pre-treatment to powder again as polyvinyl alcohol and resol etc.;
2) prefabricated component presintering
Prefabricated component is removed the easy volatile product in 20~120 minutes through 200~500 ℃ of insulations handle (comprise and take off binding agent) under vacuum condition, be directly used in the infiltration reaction then; Perhaps, prefabricated component was carried out presintering in 1~6 hour 1200~1700 ℃ of insulations, to improve the prefabricated component density, the double easy volatile product (comprise and take off binding agent) that removes is handled;
4) infiltration reaction sintering
Will be under vacuum or Ar gas atmosphere through the prefabricated component after taking off adhesive treatment or presintering, with 10~300 ℃ of the Si that is higher than infiltration or Si alloys, be incubated 10~300 minutes and carry out the infiltration reaction, obtain the SiC ceramic matric composite that the SiC whisker is strengthened after the cooling.
Above-mentioned method preparation technology is simple, and the infiltration temperature of reaction is low, need not impressed pressure, and prefabricated component can be made into complicated shape, can be used for preparing the member of complicated shape.
As preferably, the present invention flies the preparation method of rice husk SiC whiskerizing product can be as follows:
1. the cleaning of rice husk: rice husk removes impurity such as earth and floating dust by sieve, washing etc.;
2. the coking of rice husk: will through the rice husk that cleans under Ar atmosphere or vacuum condition, be heated to 700~1000 ℃, coking 1~10 hour;
3. the SiC whiskerizing of rice husk coking product is handled: the rice husk after the coking grinds through pulverizing, and through 1300~1600 ℃ of insulations 1~10 hour, obtains being rich in SiC whisker and SiC particle and a spot of carbon and SiO under Ar atmosphere or vacuum condition 2Product; Or to rice husk through directly under Ar gas atmosphere or vacuum condition, being warming up to 1300~1600 ℃ again after the coking, be incubated 1~10 hour, obtain being rich in SiC whisker and SiC particle and a spot of carbon and SiO 2Product.
As preferably, the dispersion of described rice husk SiC whiskerizing product comprise adopt ultra-sonic dispersion, Ball milling and dispersion agent are a kind of in disperseing in volatile organic liquid.
As preferably, the moulding of described prefabricated component can adopt single shaft directly to use after compression molding, perhaps, carries out using after the isostatic cool pressing again.
As preferably, the infiltrating method of Si or Si alloy can adopt direct infiltration or infiltration indirectly, and wherein directly infiltration is meant the infiltration that melt directly contact with prefabricated component, and indirect infiltration is meant that melt elder generation infiltrates the method for prefabricated component again by infiltration transition body.The transition body has identical component with prefabricated component, but can have different densityes.The Si of infiltration or its alloy can place prefabricated component above or below.The amount that presets Si or its alloy is by determining with prefabricated component component reaction and the needed amount of filling residual pore.If the prefabricated component volume does not shrink in the infiltration process, can put equivalent; If the prefabricated component volume shrinks in the infiltration process, then put and remove a small amount of of volume shrinkage mass, and be optimum principle with the density that improves matrix material.
Enforcement by each step of such scheme of the present invention, SiC whisker and particle in the prefabricated component are carried in the matrix material, carbon in the prefabricated component and Si oxide in the infiltration process each other or and the infiltration body between react, in-situ synthesis of SiC, in original position synthetic SiC particle and the matrix material other forms good binding mutually, remaining a small amount of Si or its alloy are filled the prefabricated component hole, have formed the SiC ceramic matric composite that fine and close SiC whisker is strengthened.
Beneficial effect of the present invention is that the main component SiC of matrix material derives from rice husk, and raw material sources are wide, cost is low, and environment compatibility is good.The utilization ratio height of rice husk coking and silicon carbide (SiC whisker and particle) product does not need extra screening or separating treatment again.And made full use of the strengthening effect of the stupalith that reaction forms to infiltration of SiC whisker in the rice husk product, obtained the SiC ceramic matric composite that high performance SiC whisker is strengthened.The applicable situation of such matrix material and goods thereof is wide, and the preparation method is simple, and cost is low, is expected to obtain good economic and social benefit.
The preparation method of SiC stupalith of the present invention or its goods, except having passed on the advantage of traditional reaction sintering technology, low as preparation temperature, as can to prepare complicated shape, nearly clean shape size member, the SiC whisker that comes from rice husk in the prefabricated component is played effective strengthening effect by fine low remaining in the matrix material to formed matrix material.
The performance of the prepared SiC ceramic matric composite of the present invention is good, can satisfy the corresponding commercial requirement of using.By the present invention preparation a kind of is that the flexural strength of the SiC ceramic matric composite strengthened of the SiC whisker of infiltration body can reach 500 MPa with Si.With the SiC ceramic matric composite of the inventive method preparation, can be used for the applicable situation of commercial SiC reaction sintering goods, as sliding surface bearing, corrosion-resistant, anti abrasive pipeline, valve and fan blade, military-civil flak jackets etc.
Description of drawings
Fig. 1 is the light micrograph of the matrix material of embodiment 1, demonstrates the composite structure densification.
Fig. 2 is the SEM pattern of the matrix material fracture not eroded of embodiment 1, visible SiC whisker extract He Wokou.
Fig. 3 be the matrix material fracture of embodiment 1 through corrosive SEM pattern, visible a large amount of SiC whisker.
Fig. 4 is the XRD figure spectrum of the matrix material of embodiment 1.The main composition of product is SiC mutually, and other contains remaining Si.
Fig. 5 be among the embodiment 3 rice husk through the X-ray diffraction of coking and silicon carbide (SiC whisker and particle) product (XRD figure spectrum.The main composition of product is SiC mutually, and other contains a small amount of SiO 2Carbon in the product exists with amorphous form, does not see obvious diffraction peak on the XRD figure spectrum.
Fig. 6 is that rice husk is handled scanning electron microscope (SEM) pattern of product, visible a large amount of SiC whisker through coking and silicon carbide SiC whiskerizing among the embodiment 4.
Fig. 7 is the SEM pattern of the matrix material that obtains of embodiment 6, Dark grey (comprise SiC particle and SiC whisker, grayish is the Ni-Si alloy phase mutually for the SiC phase mutually.
Embodiment
The present invention may be better understood for following example, but the present invention is not limited to following example.
Embodiment 1
With rice husk sieve earth and other impurity etc., water cleans then, dries.Dried rice husk is placed plumbago crucible in right amount, under Ar atmosphere, carried out coking in 2 hours through 900 ℃ of insulations and handle.To grind through the product that coking is handled, and then place plumbago crucible, in the graphite sintering oven, under Ar atmosphere,, obtain being rich in SiC whisker and particle and part carbon and Si oxide and (be mainly SiO through 1550 ℃ of insulations 6 hours 2) product.This is rich in SiC whisker and the oven dry after disperseing for the medium ball mill pulverizing at dehydrated alcohol of particulate product, crosses 60 mesh sieves, add the polyvinyl alcohol water solution binding agent again, the back oven dry that stirs is carried out granulation to the oven dry powder and is handled.Get an amount of granulation powder at the single shaft of 31 MPa to depressing moulding, isostatic cool pressing obtains size and is about 48 * 48 * 5.5 mm under 180 MPa subsequently 3Prefabricated component.Prefabricated component was carried out presintering in 4 hours and removes easy volatile material (comprise and take off binding agent) processing through 1550 ℃ of insulations under vacuum.Prefabricated component after the presintering is placed on the graphite cake, and on prefabricated component, put a certain amount of silico briquette, in the graphite sintering oven, under vacuum condition, carried out the infiltration reaction sintering in 1 hour through 1550 ℃ of insulations, obtain the SiC ceramic matric composite that the SiC whisker is strengthened behind the furnace cooling.The room temperature flexural strength of this material reaches as high as 550 MPa, and Vickers' hardness can reach 19 GPa, and Young's modulus is 340 GPa.
Embodiment 2
The preparation of prefabricated component is with embodiment 1.Prefabricated component is placed on the graphite cake, and on prefabricated component, put a certain amount of silico briquette, place in the graphite sintering oven, in the graphite sintering oven, it under vacuum condition is 1 hour infiltration reaction sintering through 1450 ℃ of soaking times, cooling obtains the SiC ceramic matric composite that the SiC whisker is strengthened, and the room temperature flexural strength of composite sample is 440~470 MPa.
Embodiment 3
Rice husk through cleaning carried out grinding after coking is handled in 900 ℃ of insulations under the vacuum condition in 2 hours, and the silicon carbide whisker processing was carried out in 1450 ℃ of insulations in 6 hours again.The product that this whiskerizing is handled adds the polyvinyl alcohol water solution binding agent through ball mill pulverizing and after disperseing in right amount, the back oven dry that stirs, and granulation.Again at the single shaft of 80 MPa to depressing moulding, obtain size and be about 48 * 48 * 6 mm 3Prefabricated component was carried out and removes easy volatile material (comprise and take off binding agent) and handle through 400 ℃ of insulations under vacuum in 60 minutes.Then the prefabricated component after taking off adhesive treatment is being placed on the graphite cake, and on prefabricated component, putting a certain amount of Al-55wt.%Si alloy, in the graphite sintering oven, under vacuum condition, carrying out the infiltration reaction in 1 hour through 1300 ℃ of insulations.Prefabricated component obtains being rich in SiC whisker and particulate and residual a small amount of Al, Si SiC based composites is mutually arranged through infiltration reaction postcooling.
Embodiment 4
To carry out coking in 2 hours through 900 ℃ of insulations and handle through cleaning the air dried rice husk under vacuum.To grind through the product that coking is handled, place plumbago crucible, in the graphite sintering oven, in Ar gas atmosphere, carried out the SiC whiskerizing in 6 hours and handle through 1550 ℃ of insulations.This is rich in SiC whisker and particulate product after ball mill pulverizing and Mo powder (10 wt.%, granularity is 7 μ m) mix, and adding polyvinyl alcohol water solution binding agent, the back oven dry stirs, then at the single shaft of 31MPa to depressing premolding, isostatic cool pressing obtains size and is about 48 * 48 * 6 mm under 180 MPa subsequently 3Prefabricated component.Prefabricated component was carried out presintering in 2 hours and removes easy volatile material (comprise and take off binding agent) processing 1550 ℃ of insulations under vacuum.With putting a certain amount of silico briquette on the prefabricated component after the presintering, put into high temperature sintering furnace, under vacuum condition, carried out the infiltration reaction sintering in 1 hour through 1550 ℃ of insulations.Prefabricated component obtains containing the SiC whisker and the particle redoubling contains a small amount of MoSi behind furnace cooling behind the infiltration reaction sintering 2And the SiC ceramic matric composite of Si.
Embodiment 5
Rice husk that will be through cleaning carried out coking in 3 hours through 800 ℃ of insulations in vacuum atmosphere in plumbago crucible, directly be warming up to 1400 ℃ of insulations 3 hours again, obtained being rich in SiC whisker and particle and part carbon and SiO 2Product.This rice husk whiskerizing product is ground and disperse, and the average particle size particle size of adding 10wt.% is that 0.5 micron carbon dust mixes, in this mixed powder, add the oven dry that stirs of polyvinyl alcohol water solution binding agent again.With mixed powder at the single shaft of 96 MPa to depressing moulding, obtain size and be about 48 * 48 * 6mm 3Prefabricated component.Prefabricated component is placed plumbago crucible, in the graphite sintering oven, under vacuum condition, carried out presintering in 3 hours and hold concurrently except that easy volatile material (comprise and take off binding agent) processing through 1450 ℃ of insulations.Prefabricated component is placed on the graphite version again, and put a certain amount of Si piece on prefabricated component, the infiltration reaction was carried out in insulation in 40 minutes under 1480 ℃ condition.Carbon that adds in the prefabricated component and the Si of infiltration reaction generate tiny SiC particle.Tiny original position synthetic SiC particle helps improving the toughness of material.Being added with of tiny carbon granule is beneficial to the density that improves prefabricated component in the prefabricated component, reduces the content of remaining Si in the matrix material.The matrix material that obtains has excellent comprehensive performances.
Embodiment 6
To place plumbago crucible in right amount through the rice husk of cleaning, drying, and under vacuum atmosphere, carry out coking in 2 hours and handle through 900 ℃ of insulations.Product after coking is handled places plumbago crucible again through grinding, and under mobile Ar atmosphere, through 1550 ℃ of insulations reaction in 6 hours cracking, obtains being rich in SiC whisker and particle and part carbon and Si oxide and (is mainly SiO 2) product.This is rich in the SiC whisker and the particulate product is dried after Ball milling, adds the polyvinyl alcohol water solution binding agent again.Get an amount of granulation powder at the single shaft of 96 MPa to depressing moulding, subsequently under 180 MPa isostatic cool pressing to obtain size be the circular prefabricated component of Ф 50 * 4mm.Prefabricated component carried out presintering in 3 hours and removes easy volatile material (comprise and take off binding agent) processing through 1550 ℃ of insulations under vacuum.Prefabricated component after the presintering is placed on the graphite cake that scribbles BN coating, with a certain amount of NiSi 2Alloy places on the prefabricated component, in the graphite sintering oven, carries out the infiltration reaction sintering in 2 hours through 1550 ℃ of insulations under vacuum condition, obtains the SiC ceramic base Ni-Si matrix material that fine and close SiC whisker is strengthened behind the furnace cooling.

Claims (10)

1. the SiC ceramic matric composite that the SiC whisker is strengthened is characterized in that this matrix material is obtained by Si or Si alloy infiltration prepared in reaction by prefabricated component, and described prefabricated component is made by the raw material compression molding that comprises rice husk SiC whiskerizing product.
2. the SiC ceramic matric composite that a kind of SiC whisker according to claim 1 is strengthened is characterized in that: also comprise in carbon and the SiC powder body material one or both in the prefabricated component; As preferably, described carbon is selected from one or more in graphite, carbon black, decolorizing carbon and the refinery coke; As preferred again, the addition of carbon is 0~40% of a prefabricated component total amount, and particle size is at 0.1~30 micron; The amount of the SiC powder that adds is in 0~40% of prefabricated component total amount, and particle is at 0.1~30 micron.
3. the SiC ceramic matric composite that a kind of SiC whisker according to claim 1 and 2 is strengthened is characterized in that: also comprise Mo in the prefabricated component, the amount that Mo adds is no more than half of the molar weight that presets infiltration Si or Si alloy.
4. the SiC ceramic matric composite that a kind of SiC whisker according to claim 1 and 2 is strengthened is characterized in that: the Si alloy is selected from a kind of among Al-Si, Mo-Si, Fe-Si and the Ni-Si, and wherein the content of Si is at 10~90wt%.
5. the SiC ceramic matric composite that a kind of SiC whisker according to claim 1 and 2 is strengthened, it is characterized in that: also comprise binding agent in the prefabricated component, binding agent adds when difficult forming, and addition is convenient to moulding and is got final product; As preferably, described binding agent is selected polyvinyl alcohol or resol for use.
6. a method for preparing the SiC ceramic matric composite of claim 1 or 2 described a kind of SiC whiskers reinforcements is characterized in that this method comprises the steps:
1) preparation of prefabricated component
Rice husk SiC whiskerizing product and auxiliary material are ground and disperse, and add binding agent when difficult forming, compression molding is prepared into prefabricated component then;
2) prefabricated component presintering
Prefabricated component is removed the easy volatile product in 20~120 minutes through 200~500 ℃ of insulations handle under vacuum condition, be directly used in the infiltration reaction then; Perhaps, prefabricated component was carried out presintering in 1~6 hour 1200~1700 ℃ of insulations, to improve the prefabricated component density, the double easy volatile product that removes is handled;
4) infiltration reaction sintering
Will be under vacuum or Ar gas atmosphere through the prefabricated component after taking off adhesive treatment or presintering, with 10~300 ℃ of the Si that is higher than infiltration or Si alloy melting points, be incubated 10~300 minutes and carry out the infiltration reaction, obtain the SiC ceramic matric composite that the SiC whisker is strengthened after the cooling.
7. the method for the SiC ceramic matric composite of strengthening according to the described a kind of SiC whisker of claim 6 is characterized in that the preparation method of rice husk SiC whiskerizing product is as follows:
1. the cleaning of rice husk: rice husk removes impurity such as earth and floating dust by sieve, washing etc.;
2. the coking of rice husk: will through the rice husk that cleans under Ar atmosphere or vacuum condition, be heated to 700~1000 ℃, coking 1~10 hour;
3. the SiC whiskerizing of rice husk coking product is handled: the rice husk after the coking grinds through pulverizing, and through 1300~1600 ℃ of insulations 1~10 hour, obtains being rich in SiC whisker and SiC particle and a spot of carbon and SiO under Ar atmosphere or vacuum condition 2Product; Or to rice husk through directly under Ar gas atmosphere or vacuum condition, being warming up to 1300~1600 ℃ again after the coking, be incubated 1~10 hour, obtain being rich in SiC whisker and SiC particle and a spot of carbon and SiO 2Product.
8. the method for the SiC ceramic matric composite of strengthening according to claim 6 or 7 described a kind of SiC whiskers is characterized in that: the dispersion of rice husk SiC whiskerizing product comprise adopt ultra-sonic dispersion, Ball milling and dispersion agent are a kind of in disperseing in volatile organic liquid.
9. the method for the SiC ceramic matric composite of strengthening according to claim 6 or 7 described a kind of SiC whiskers, it is characterized in that: the moulding of prefabricated component can adopt single shaft directly to use after compression molding, perhaps, carries out using after the isostatic cool pressing again.
10. the method for the SiC ceramic matric composite of strengthening according to claim 6 or 7 described a kind of SiC whiskers, it is characterized in that: the infiltrating method of Si or Si alloy adopts direct infiltration or indirect infiltration, and the amount that presets Si or Si alloy is by determining with prefabricated component component reaction and the needed amount of filling residual pore.
CN 201110122040 2011-05-12 2011-05-12 SiC whisker reinforced SiC ceramic matrix composite and preparation method thereof Expired - Fee Related CN102161594B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 201110122040 CN102161594B (en) 2011-05-12 2011-05-12 SiC whisker reinforced SiC ceramic matrix composite and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 201110122040 CN102161594B (en) 2011-05-12 2011-05-12 SiC whisker reinforced SiC ceramic matrix composite and preparation method thereof

Publications (2)

Publication Number Publication Date
CN102161594A true CN102161594A (en) 2011-08-24
CN102161594B CN102161594B (en) 2013-02-06

Family

ID=44463093

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 201110122040 Expired - Fee Related CN102161594B (en) 2011-05-12 2011-05-12 SiC whisker reinforced SiC ceramic matrix composite and preparation method thereof

Country Status (1)

Country Link
CN (1) CN102161594B (en)

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102874809A (en) * 2012-10-22 2013-01-16 南京工业大学 Silicon carbide composite powder and preparation process thereof
CN104030688A (en) * 2014-06-19 2014-09-10 浙江立泰复合材料有限公司 Preparation method of low-temperature reactive sintered silicon carbide
WO2016037316A1 (en) * 2014-09-09 2016-03-17 南京工业大学 Preparation method of sic porous ceramic material and porous ceramic material manufactured by using same
CN107365168A (en) * 2016-05-11 2017-11-21 航天特种材料及工艺技术研究所 A kind of method for improving SiO 2-ceramic based composites tensile strength
CN107399983A (en) * 2017-08-14 2017-11-28 武汉科技大学 A kind of silicon carbide reaction-sintered foamed ceramics and preparation method thereof
CN109942225A (en) * 2019-03-01 2019-06-28 蒋留平 A kind of preparation method of heat resist modification type retarder
CN110078529A (en) * 2019-05-30 2019-08-02 西安创正新材料有限公司 A kind of silicon carbide whisker reinforced aluminum matrix composites and preparation method thereof
CN110191870A (en) * 2017-01-11 2019-08-30 通用电气公司 Use the infiltration method of SiGa and/or Siln alloy
CN112266257A (en) * 2020-10-29 2021-01-26 中南大学 Low-cost preparation method of reinforced silicon carbide composite material based on hybrid fiber between continuous C and SiC bundles and product thereof
CN112851357A (en) * 2020-12-31 2021-05-28 中核北方核燃料元件有限公司 Preparation method of end plug of SiC composite material cladding tube
CN114230356A (en) * 2022-01-21 2022-03-25 辽宁科技大学 Preparation method of silicon carbide fiber reinforced silicon carbide ceramic through catalytic conversion of glass fiber
WO2024098568A1 (en) * 2022-11-07 2024-05-16 江苏核电有限公司 Composition for main-pump bearing bush and preparation method therefor

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7368405B2 (en) * 2002-12-16 2008-05-06 Council Of Scientific And Industrial Research Process of making silicon—silicon carbide ceramic using biopreform, silicon—silicon carbide ceramic obtained thereby
CN101687251A (en) * 2006-10-24 2010-03-31 瑞锡尼弗莱诺斯可变资本股份公司 permeable annulus
CN101864619A (en) * 2010-06-18 2010-10-20 吉林大学 Method for preparing nanometer-diameter carborundum brief fiber and whisker by utilizing rice hulls

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7368405B2 (en) * 2002-12-16 2008-05-06 Council Of Scientific And Industrial Research Process of making silicon—silicon carbide ceramic using biopreform, silicon—silicon carbide ceramic obtained thereby
CN101687251A (en) * 2006-10-24 2010-03-31 瑞锡尼弗莱诺斯可变资本股份公司 permeable annulus
CN101864619A (en) * 2010-06-18 2010-10-20 吉林大学 Method for preparing nanometer-diameter carborundum brief fiber and whisker by utilizing rice hulls

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
《硅酸盐学报》 20040229 张小立等 反应熔渗烧结法制备MoSi2/SiC复合材料 第162页左栏第1段-第165页右栏最后1段 1-10 第32卷, 第02期 *

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102874809A (en) * 2012-10-22 2013-01-16 南京工业大学 Silicon carbide composite powder and preparation process thereof
CN104030688A (en) * 2014-06-19 2014-09-10 浙江立泰复合材料有限公司 Preparation method of low-temperature reactive sintered silicon carbide
WO2016037316A1 (en) * 2014-09-09 2016-03-17 南京工业大学 Preparation method of sic porous ceramic material and porous ceramic material manufactured by using same
US10287214B2 (en) 2014-09-09 2019-05-14 Nanjing Tech University Preparation method of SiC porous ceramic material and porous ceramic material manufactured by using same
CN107365168A (en) * 2016-05-11 2017-11-21 航天特种材料及工艺技术研究所 A kind of method for improving SiO 2-ceramic based composites tensile strength
CN110191870A (en) * 2017-01-11 2019-08-30 通用电气公司 Use the infiltration method of SiGa and/or Siln alloy
CN107399983A (en) * 2017-08-14 2017-11-28 武汉科技大学 A kind of silicon carbide reaction-sintered foamed ceramics and preparation method thereof
CN109942225A (en) * 2019-03-01 2019-06-28 蒋留平 A kind of preparation method of heat resist modification type retarder
CN110078529A (en) * 2019-05-30 2019-08-02 西安创正新材料有限公司 A kind of silicon carbide whisker reinforced aluminum matrix composites and preparation method thereof
CN112266257A (en) * 2020-10-29 2021-01-26 中南大学 Low-cost preparation method of reinforced silicon carbide composite material based on hybrid fiber between continuous C and SiC bundles and product thereof
CN112851357A (en) * 2020-12-31 2021-05-28 中核北方核燃料元件有限公司 Preparation method of end plug of SiC composite material cladding tube
CN114230356A (en) * 2022-01-21 2022-03-25 辽宁科技大学 Preparation method of silicon carbide fiber reinforced silicon carbide ceramic through catalytic conversion of glass fiber
WO2024098568A1 (en) * 2022-11-07 2024-05-16 江苏核电有限公司 Composition for main-pump bearing bush and preparation method therefor

Also Published As

Publication number Publication date
CN102161594B (en) 2013-02-06

Similar Documents

Publication Publication Date Title
CN102161594B (en) SiC whisker reinforced SiC ceramic matrix composite and preparation method thereof
CN102219536B (en) B4C/SiC whisker/SiC multiphase ceramic matrix composite and preparation method thereof
WO2020042950A1 (en) Short-fiber-reinforced oriented max-phase ceramic-based composite and preparation method therefor
CN103145422B (en) High-hardness ceramic composite material of boron carbide-titanium boride-silicon carbide and preparation method thereof
CN101456737B (en) Boron carbide base composite ceramic and preparation method thereof
CN105130438B (en) A kind of method that boron carbide ceramics composite is prepared based on reaction-sintered
CN101747044B (en) Reactive sintering siliconcarbide ceramics preparation method taking mesocarbon microbead (MCMB) as carbon source
CN110128146B (en) Multifunctional boron carbide-based multiphase ceramic and reactive hot-pressing sintering preparation method thereof
CN108439995B (en) Complex phase ceramic and preparation method thereof
CN103030396A (en) Boron carbide silicon carbide composite ceramic and preparation method thereof
CN103833403A (en) Preparation method of silicon carbide whisker toughened boron carbide (B4C) ceramic composite material and product thereof
CN102731093A (en) Method for low-temperature densification sintering of boron carbide-based ceramic material
CN109439940A (en) A kind of method that hot pressed sintering prepares particle enhanced aluminum-based composite material under air atmosphere
CN108585869A (en) A kind of preparation method of in-situ authigenic MAX phase modified composite materials
WO2009020635A2 (en) Method of preparing pressureless sintered, highly dense boron carbide materials
EP2456733A2 (en) Methods of forming sintered boron carbide
CN102249682B (en) Titanium carbide ceramic composite material reinforced with ferrum and aluminium intermetallic compound and preparation method thereof
CN104593657A (en) Boron carbide-based composite material and preparation method thereof
CN109354504B (en) Boron carbide-based composite ceramic sintering aid and sintering process
CN105483487B (en) A kind of Boral alloy composite materials containing zirconium and preparation method thereof
CN110304933A (en) The preparation method of the crystal whisker toughened reaction sintering silicon carbide ceramic of surface modified carbon SiClx
CN101555136B (en) Titanium silicide carbon/titanium diboride-titanium carbide compound material and preparation method thereof
CN111892414A (en) Short carbon fiber reinforced boron carbide composite material and preparation method thereof
CN100424039C (en) Original position reaction hot pressing synthesis TiB2-NbC-SiC refractory ceramics composite material and preparing method thereof
CN1887796A (en) Process of preparing heterogenous conducting Si3N4/Tin ceramic material tail iron ore

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20130206