CN101164998B - Method for preparing silicon carbide ceramic composition containing silicon carbide whisker - Google Patents
Method for preparing silicon carbide ceramic composition containing silicon carbide whisker Download PDFInfo
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Abstract
The present invention relates to silicon carbide ceramic, and is especially preparation process of silicon carbide ceramic composition containing silicon carbide crystal whisker. The present invention features that rod shaped alumina grain and flaky alumina grain easily mixed with other materials are introduced to toughen silicon carbide ceramic together with silicon carbide crystal whisker as powerful toughening material. The silicon carbide ceramic has less dependence on hard-to-disperse silicon carbide crystal whisker and less negative effect caused by inhomogeneous material mixing.
Description
Technical field
The present invention relates to process for preparing ceramic, is about method for manufacturing silicon carbide ceramics, particularly about a kind of method for preparing silicon carbide ceramic composition of silicon carbide-containing whisker.
Background technology
Good characteristics such as thyrite has that hot strength is big, high-temperature oxidation resistance is strong, abrasion resistance properties is good, thermostability is good, thermal expansivity is little, thermal conductivity is big, hardness is high, anti-thermal shock and resistance to chemical attack; in fields such as automobile, mechanical chemical industry, environment protection, space technology, information electronics, the energy increasingly extensive application is arranged, become a kind of irreplaceable structural ceramics of other materials at a lot of industrial circle excellent performances.
Dynamic seal in the mechanical means is to be undertaken by the rotational slide of two seal face materials, as the seal face material, requires the hardness height, has wearability.Suitable height of the hardness of silicon carbide ceramics and frictional coefficient are little, so silicon carbide ceramics can obtain sliding properties that other material is beyond one's reach as the mechanical seal end surface material.On the other hand, two mechanical seal materials can produce certain heat owing to rub in rotary movement, thereby the local temperature of seal face is raise, so the end face material also must can tolerate certain temperature.In the rotational slide process, produce thermal strain and hot tearing for fear of the mechanical seal material, require thermal conductivity height, the good thermal shock of end face material.At present, silicon carbide ceramics has obtained a large amount of application in all kinds of mechanical seals, and for the laborsaving of mechanical means with energy-conservationly made very big contribution, demonstrate other materials incomparable superiority.Silicon carbide ceramics also successfully is used as various bearings, cutting tool in mechanical industry.
What need in the occasion of needs such as aerospace, nuclear industry tolerances ultra high temp such as nuclear fission and the fusion reactor bears 2000 degree left and right sides pyritous heat-stable materials; Rocket and aerospacecraft surface are used for tolerating the thermal insulation tile up to thousands of K temperature that produces with the violent friction of atmosphere; Rocket combustion chamber's larynx lining and inner lining material, gas-turbine blade; The top board of High Temperature Furnaces Heating Apparatus, support, and the high temperature members such as jig of high temperature experiment usefulness also generally adopt the silicon carbide ceramics member.Silicon carbide ceramics also is widely used as various corrosion-resistant with container and pipeline in petrochemical industry.
Will further improve the performance of silicon carbide ceramics, how solve the fragility problem, be the focus of a concern.The fragility problem is the common problem that all kinds of potteries face.The Zhou Zhenjun of China's University Of Tianjin's high-temperature structural ceramics and key lab of the engineering ceramics processing technology the Ministry of Education etc., be published in be entitled as " the Research on Toughening progress of high reliability structural ceramics " of " silicate circular " the 3rd phase p57-61 in 2003, and, the Hao Chuncheng of Shandong University etc., be published in be entitled as " progress of particulate reinforcement pottery " of the 16th volume the 2nd phase p28-30 in " material Leader " February in 2002, and, the Guo Jingkun of Shanghai Silicate Inst., Chinese Academy of Sciences's high-performance ceramic and ultrastructure National Key Laboratory, be published in be entitled as " about the fragility problem of stupalith " of the 42nd volume the 6th phase p822-827 in " Fudan Journal (natural science edition) " December in 2003, and, the Liu Hanlian of the advanced jet Engineering Technical Research Centre of School of Mechanical Engineering of Shandong University etc., be published in being entitled as in the papers such as " the toughened and reinforced mechanism progress of nanocomposite ceramic material " of the 22nd volume the 2nd phase p98-103 in " powder metallurgy technology " April in 2004, ceramic toughening theory problem and practice are had detailed introduction.
The malleableize mode of pottery mainly contains that transformation toughening, fiber (whisker) are toughness reinforcing, particulate reinforcement and composite toughening.Wherein, particulate reinforcement is the simplest a kind of method of ceramic toughening, and it has many advantages such as improving intensity and toughness simultaneously.The principal element that influences the second phase particulate composite toughening effect is a matrix and second particulate elastic modulus E, thermalexpansioncoefficient and the biphase chemical compatibility mutually.Wherein chemical compatibility is the compound prerequisite, and two alternately can not exist too much chemical reaction, must have suitable interface comprehensive strength simultaneously again.Utilize the mismatch of thermalexpansioncoefficient, thereby, be the toughened and reinforced main root of complex phase ceramic in the second phase particle and the residual stress field of the inner generation of matrix on every side.Suppose between the second phase particle and the matrix chemical reaction not to take place, if having the mismatch of thermal expansivity, i.e. Δ α=α between the second phase particle and the matrix
p-α
m≠ 0 (p, m represent particle and matrix), when Δ α＞0, the second phase particle is in tensile stress state, and matrix radially is in stretched state, tangentially is in compressed state, and at this moment crackle tends to walk around particle and continues expansion; When Δ α＜0, the second phase particle is in compressive stress state, tangentially is subjected to tensile stress, and at this moment crackle tends at particle place pinning or passes particle.Thereby the appearance of tiny crack can absorb energy and reach toughness reinforcing purpose, one of tiny crack toughening mecha-nism operating is a crack deflection, crack deflection is a kind of crack tip effect, is meant the inclination and the deflection that are taken place when crack tip runs into deflection thing (particle, fiber, whisker, interface etc.) in the crack propagation process; Two of tiny crack toughening mecha-nism operating is crackle bridgings, bridging thing (particle, fiber, whisker etc.) connects near two surfaces of two crackles of bridging thing and provides one to make two crack surfaces close stress mutually, be closure stress, cause stress intensity factor to increase like this with crack propagation.When crack propagation ran into bridging agent, the possible grain failure of bridging thing also the interlocking phenomenon may occur, and promptly crackle is walked around the bridging thing along crystal boundary development and formation friction bridge.Letter is local to be said, and the second mutually heterogeneous phase particulate introducing will bring a large amount of tiny cracks, and a large amount of dominance or recessive tiny crack help to dissipate or dissolve or absorb external destructive tension stress.In addition, adopting whisker to carry out also existing and extracting effect when toughness reinforcing, extracting effect also is a kind of toughness reinforcing factor that helps.When the second mutually heterogeneous phase particle of introducing is nano particle, also help and suppress growing up of ceramic base material crystal grain, the microminiaturization of ceramic base material crystal grain also is an important toughening mecha-nism operating in the Low fire ceramic, from fracture toughness property value and displaing microstructure observing result, the sample microcosmic is the nano level microscopic structure, then macro manifestations goes out the highest fracture toughness property, can think, the particulate refinement makes weave construction more even, reduced the size of stress concentration and micro-flaw, simultaneously, the particulate refinement also makes micro-flaw quantity increase, that is to say, fine crystalline-granular texture can cause the crystal boundary volume fraction to increase, and in this case, the new crack surfaces of the dissipativeness that generates in the ceramic breaking-down process is long-pending to be increased, need the outside energy that absorbs in the process before the pottery fracture thereby increase considerably, show as ceramic fracture toughness on the macroscopic view and improve.
It is toughness reinforcing to adopt the tabular crystal particle that stupalith is carried out, and also is an effective ceramic toughening approach.The Li Shaochun of China Qingdao Technological University, wear Changhong and be published in being entitled as in " silicon-carbide particle, whisker, wafer toughening ceramic composite study present situation " literary composition of " silicate circular " the 6th phase p63-65 in 2004, silicon-carbide particle, whisker, wafer are applied to the toughness reinforcing situation of non-silicon carbide base material, a detailed introduction is arranged, this article relates to the toughening technology of non-silicon carbide base material, and for example: silicon-carbide particle, silicon carbide whisker, silicon carbide wafer are used for (BaO-Al
2O
3-SiO
2) glass-ceramic, silicon nitride ceramics, TOUGHENING OF ALUMINA CERAMICS.Wherein, the toughening mechanism of silicon carbide wafer is considered to extract mechanism because of crackle bridging mechanism, crack deflection mechanism and wafer after deliberation.
In the silicon carbide ceramics system, present more report be that to adopt silicon carbide whisker to carry out toughness reinforcing, and, adopt the charcoal fiber to carry out toughness reinforcing.Silicon carbide whisker toughening technology scheme is for example: Tian Jiemo etc. invent (design), Tsing-Hua University's application, and application number is the patent application case " reinforcing of carbon-ceramics composite material with flexibilizer for coystal whiskers " of CN91101684.8; And, the big J Pai Qike invention of A Lishan (design), Tang Chemical Corporation's application, application number is the patent application case " silicon carbide whisker reinforced ceramic composites and manufacture method thereof " of CN90110427.2; And, inventions such as Cheng Laifei, Zhang Litong, Xu Yongdong, Liu Yongsheng, Li Zhen, Wang Xiaoming (design), the application of NW China polytechnical university, application number is the patent application case " a kind of whisker and particulate reinforcement ceramic matric composite preparation method " of CN200410026337.6.The fiber reinforced technical scheme of charcoal is for example: Geng Haoran etc. invent (design), University Of Ji'nan's application, and application number is the patent application case " a kind of device and technology for preparing carbon fibre reinforced silicon carbide composite material " of CN03138926.0.
Introducing silicon carbide whisker or charcoal fiber carries out toughness reinforcing, silicon carbide ceramics toughness is increased substantially, but, the silicon carbide whisker preparation cost is higher, bring the production cost of whole toughening ceramic finished product to rise, in addition, silicon carbide whisker that length-to-diameter ratio is very high and charcoal fiber are generally speaking difficult to mix with other silicon carbide ceramics raw materials for production, and this has influenced the quality homogeneity of ceramics of silicon carbide toughened finished product to a certain extent.
Summary of the invention
Purpose of the present invention, provide a kind of new toughness reinforcing scheme, the objective of the invention is to utilize the toughness reinforcing advantage of silicon carbide whisker, when being used in combination silicon carbide whisker, introduce the plasticizing substance of other suitable cheapnesss, with silicon carbide whisker silicon carbide ceramics is carried out combined plasticizing, in the hope of reducing for the dependence that is difficult to the dispersive silicon carbide whisker relatively, and the negative impact that may bring of reduction batch mixing inequality.This solution will be taken into account the various useful toughening effect of above addressing as far as possible, and the plasticizing substance of described other suitable cheapnesss should be easy and the mixed uniformly material of other silicon carbide ceramics raw materials for production as far as possible.
The objective of the invention is to reach by the following technical solutions, this technical scheme is a kind of method for preparing silicon carbide ceramic composition of silicon carbide-containing whisker, the main raw material of this manufacture method is a carborundum powder, sintering aid, toughness reinforcing material and wedding agent, through mixing, moulding, solidify, main technique steps such as high temperature sintering, form the silicon carbide ceramics product, the toughness reinforcing material that contains in the raw material is the material that adds for the toughness that increases silicon carbide ceramics, the sintering processing of described high-sintering process step is not have to press solidly phase sintering or do not have the hydraulic fluid phase sintering, it is characterized in that, the toughness reinforcing material that is adopted is made up of rod-like aluminum oxide particle and sheet-shaped alpha-alumina particles and three kinds of plasticizing substances of silicon carbide whisker, described rod-like aluminum oxide particle is that granule-morphology is bar-shaped aluminum oxide powder, described sheet-shaped alpha-alumina particles is a granule-morphology aluminum oxide powder in the form of sheets, and the ratio value of the usage quantity (weight) of usage quantity of each described plasticizing substance (weight) and described toughness reinforcing material integral body is between 0.1 and 0.8.The usage quantity of described rod-like aluminum oxide particle and sheet-shaped alpha-alumina particles and silicon carbide whisker is all non-vanishing.The art-recognized meanings that described nothing presses solidly phase sintering and do not have a hydraulic fluid phase sintering is known at the silicon carbide ceramics production field.Described sintering aid is for example: C-B, C-rare earth metal compound, AlN+Y
2O
3, B, BN, Al
4C
3-B
4C, Al
8B
4C
7, Al
2O
3+ Y
2O
3, Al
4SiC
4, Al-C.Described wedding agent is with the material of helping the blank typing, for example: PVB (phenolic resin), PVA (polyvinyl alcohol).The raw material that is used to produce silicon carbide ceramics also can comprise softening agent, and, lubricant.Described softening agent is used to reduce the moulding difficulty, and described softening agent is glycerine for example.Described lubricant is used to reduce demoulding difficulty, and described lubricant is oleic acid for example.Can also contain some other processing step in the production process, for example, dry materials; Granulation for powders; Blank after solidifying is carried out mechanical cutting roughing; Base behind high temperature sintering pottery is carried out mechanical ground finish etc.Described hybrid technique step can adopt general hybrid technique.Described moulding process step can adopt die press technology for forming or extruding-out process.Described curing process step is by at 100 ℃ of-300 ℃ of processing steps of heating described wedding agent being played a role.Described high-sintering process step is 1700 ℃ of-2100 ℃ of heat-treating process steps.
About the technology of preparing or the tailor-made product of rod-like aluminum oxide particle and sheet-shaped alpha-alumina particles, Hi-tech Industry Development portion of Chinese Wuhan University, Wuhan University productivity promotion center can provide.Wherein, the preparation method of described sheet-shaped alpha-alumina particles (tabular alumina powder just) can also find in the prior art, described prior art is for example: (1) contriver is: Sai Ersi R Xibe spy, Ai Tehua L Ge Lawen, Jr, the applicant is: Sheng Geben/promise industrial enamel company limited of pausing, application number is: CN94100796.0, being entitled as: the application for a patent for invention case of " tabular alumina ". (2) contriver is: new Tian Shengjiu, Chen Mingshou, villous themeda is former pure, the applicant is: Merck Patent GmbH, application number is: CN96112590.X is entitled as: the application for a patent for invention case of " flake aluminum oxide and pearly pigment and manufacture method thereof ".In addition, Chinese Zhejiang Province enterprise supply from stock (this thing mainly was the substrate as pearly pigment originally) in a large number.In addition, Chinese Aluminium Co., Ltd Zhengzhou research institute also can provide the technology of preparing of multiple special appearance alumina particle.
Sintering process in the described method for manufacturing silicon carbide ceramics can be not have to press solidly phase sintering technology, also can be no hydraulic fluid phase sintering technology.Have multiple sintering aid available, when adopting no hydraulic fluid phase sintering technology, one of alternative sintering aid scheme is: yttrium oxide adds aluminum oxide.
Adopting no hydraulic fluid phase sintering technology, and add with yttrium oxide under the situation of combination as sintering aid of aluminum oxide, that part of alumina raw material as sintering aid can certainly be the combination of adopting described rod-like aluminum oxide particle and described sheet-shaped alpha-alumina particles, and the ratio value of total usage quantity (weight) of the usage quantity of each described alumina particle (weight) and two kinds of described alumina particles is between 0.1 and 0.9.The usage quantity of each described alumina particle is all non-vanishing.That is to say, in this scheme, the part of the described alumina particle that adds as one of raw material, in the high temperature sintering step, promptly in 1700 ℃ of-2100 ℃ of warm area heat-treating process steps, yttrium aluminum garnet liquation with yttrium oxide reaction generation molten, and becoming plasticizing substance, the unreacted described alumina particle of remainder is trapped in the silicon carbide ceramics, because described alumina particle undertakes dual role in this scheme, it certainly will be above the aluminium in the yttrium aluminum garnet chemical formula and the element mol ratio of yttrium with the reinforced proportioning (the element mol ratio of aluminium and yttrium) of yttrium oxide.
Can also contain magnesium elements in the raw material of described method for manufacturing silicon carbide ceramics.The adding form of described magnesium elements in raw material be for example: magnesium oxide, magnesium nitrate, magnesiumcarbonate, magnesium oxalate.The introducing of magnesium elements helps to suppress growing up of carborundum grain.As mentioned before, the refinement of carborundum grain helps toughness reinforcing.
No matter whether contain magnesium elements in the described raw material, also allow to contain lanthanum element in the described raw material.The adding form of described lanthanum element in raw material be for example: lanthanum trioxide, lanthanum nitrate, Phosbloc, lanthanum oxalate.The adding of lanthanum element also helps suppressing carborundum grain and grows up.
When adopting no hydraulic fluid phase sintering technology, simultaneously, add the combination of aluminum oxide as sintering aid with yttrium oxide, and, that part of alumina raw material as sintering aid also is the combination of adopting described rod-like aluminum oxide particle and described sheet-shaped alpha-alumina particles, preamble is addressed, in this case, because described alumina particle undertakes dual role in this scheme, it certainly will be above the aluminium in the yttrium aluminum garnet chemical formula and the element mol ratio of yttrium with the reinforced proportioning (the element mol ratio of aluminium and yttrium) of yttrium oxide.The further feature of this kind scheme is, the raw material mixed processes comprises following processing step: a: described rod-like aluminum oxide particle and described sheet-shaped alpha-alumina particles are mixed with yttrium oxide, carry out ball milling, form difunctional prefabricated material, in described difunctional prefabricated material, aluminium element mixes mol ratio greater than seven to three with yttrium.B: described difunctional prefabricated material is mixed with carborundum powder and silicon carbide whisker and wedding agent etc.What explain is, the aluminium in the yttrium aluminum garnet chemical formula is 5 to 3 with the element mol ratio of yttrium, is used for toughness reinforcingly if expect to have remaining described alumina particle, and then aluminium element should be greater than seven to three with the appropriate mol ratio of mixing of yttrium in the raw material.This process program is divided into two sections with the raw material mixed processes exactly, wherein, step a, just described rod-like aluminum oxide particle and described sheet-shaped alpha-alumina particles are mixed with yttrium oxide, carry out ball milling, form the step of described difunctional prefabricated material, its effect, be to utilize mechanochemical reaction to make the described alumina particle and the yttrium oxide generation reaction to a certain extent of a part, form a certain amount of yttrium aluminum garnet presoma.The generation of a certain amount of yttrium aluminum garnet presoma helps sintering.Contain simultaneously in the described difunctional prefabricated material and be useful on toughness reinforcing excessive described rod-like aluminum oxide particle and described sheet-shaped alpha-alumina particles.
Described difunctional prefabricated material and carborundum powder and silicon carbide whisker and wedding agent etc. are being carried out in the blended processing step, and its hybrid mode can adopt ball milling method.Though comprise in the material and be difficult to the blended silicon carbide whisker relatively, mixed effect is useful to the ball milling hybrid mode for reaching preferably.
The hybrid mode of described difunctional prefabricated material and carborundum powder and silicon carbide whisker and wedding agent etc. also can adopt churned mechanically mode, and its operation is to add liquid to form pasty material, and described pasty material is applied mechanical stirring.Described liquid is for example: the mixing solutions of water, ethanol, methyl alcohol or their any ratio.Because the particle diameter of carborundum powder that is used for non-pressure sintering technology is mostly between the 0.1-0.9 micron, particle is less, and it is also less through the described difunctional prefabricated material particle diameter of ball milling generation, thereby, although comprise in the material and be difficult to the blended silicon carbide whisker relatively, adopting adding liquid to be made into pasty material and to apply churned mechanically mode is of value to mixing of materials.
And, the hybrid mode of described difunctional prefabricated material and carborundum powder and silicon carbide whisker and wedding agent etc., can also be in conjunction with applying mechanical stirring and hyperacoustic mode:, described pasty material is applied ultrasonic wave applying churned mechanically while or intermittence.In conjunction with applying the uniform mixing that mechanical stirring and hyperacoustic mode help promoting being mixed with the material of silicon carbide whisker.
The radial width of described rod-like aluminum oxide particle distributes, the distribution of the plate width distribution of the aspect ratio distribution of rod-like aluminum oxide particle, sheet-shaped alpha-alumina particles and plate width and the ratio of sheet, in fact allowed band broad; But, reasonable range of choice is: the aspect ratio distribution of described rod-like aluminum oxide particle is between 3 and 5, the radial width of described rod-like aluminum oxide particle is distributed between 0.1 micron and 0.8 micron, the plate width of described sheet-shaped alpha-alumina particles is between 0.3 micron and 6.0 microns, and the plate width of described sheet-shaped alpha-alumina particles and the ratio of sheet are between 3 and 10.Nano level insert particle helps to suppress growing up of carborundum grain, carborundum grain refinement be an important toughening mecha-nism operating.
Characteristics of the present invention are toughness reinforcing advantages of utilizing silicon carbide whisker, being used in combination under the situation of silicon carbide whisker, introduce rod-like aluminum oxide particle and sheet-shaped alpha-alumina particles simultaneously, with silicon carbide whisker silicon carbide ceramics are carried out combined plasticizing; Described rod-like aluminum oxide particle and sheet-shaped alpha-alumina particles are easy to and other material uniform mixing; The solution of the present invention has reduced for the degree of dependence that is difficult to the dispersive silicon carbide whisker relatively, and the negative impact that the batch mixing inequality may be brought that weakened.The solution of the present invention is taken into account and is utilized thermal expansion mismatch to bring out that tiny crack, crack deflection, crackle bridging, rod-like aluminum oxide particle are extracted effect, sheet-shaped alpha-alumina particles extracts effect and silicon carbide whisker is extracted useful toughening mecha-nism operating such as effect.
Embodiment
Embodiment 1: get rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, the ratio of ratio value between 0.1 and 0.9 in total usage quantity (weight) of the usage quantity (weight) of each described alumina particle and two kinds of described alumina particles, take by weighing rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, simply be mixed into dimorphism looks alumina particle powder.
C-B sintering aid with 0.5%-3.0% (weight), PVA with 1.0%-5.0% (weight), and, the described dimorphism looks alumina particle powder of 2.0%-12.0% (weight), and, the carborundum powder of 70.0%-94.5% (weight), and, the silicon carbide whisker of 2.0%-10.0% (weight) carries out dry ball milling and mixes compression molding, solidify 100 ℃ of-300 ℃ of temperature ranges, afterwards, 1700 ℃ of-2100 ℃ of temperature range sintering 0.5-3.0 hour, form the silicon carbide ceramics product.
Embodiment 2: get rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, the ratio of ratio value between 0.1 and 0.9 in total usage quantity (weight) of the usage quantity (weight) of each described alumina particle and two kinds of described alumina particles, take by weighing rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, simply be mixed into dimorphism looks alumina particle powder.
C-B sintering aid with 0.5%-3.0% (weight), PVA with 1.0%-5.0% (weight), and, the described dimorphism looks alumina particle powder of 2.0%-12.0% (weight), and, the carborundum powder of 70.0%-94.5% (weight), and, the silicon carbide whisker of 2.0%-10.0% (weight), and, an amount of water, be made into pasty material, carry out wet ball grinding and mix drying, granulation, compression molding is solidified 100 ℃ of-300 ℃ of temperature ranges, afterwards, 1700 ℃ of-2100 ℃ of temperature range sintering 0.5-3.0 hour, form the silicon carbide ceramics product.
Embodiment 3: get rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, the ratio of ratio value between 0.1 and 0.9 in total usage quantity (weight) of the usage quantity (weight) of each described alumina particle and two kinds of described alumina particles, take by weighing rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, simply be mixed into dimorphism looks alumina particle powder.
C-B sintering aid with 0.5%-3.0% (weight), PVA with 1.0%-5.0% (weight), and, the described dimorphism looks alumina particle powder of 2.0%-12.0% (weight), and, the carborundum powder of 70.0%-94.5% (weight), and, the silicon carbide whisker of 2.0%-10.0% (weight), and, an amount of water, be made into pasty material, carry out mechanical stirring and mix drying, granulation, compression molding is solidified 100 ℃ of-300 ℃ of temperature ranges, afterwards, 1700 ℃ of-2100 ℃ of temperature range sintering 0.5-3.0 hour, form the silicon carbide ceramics product.
Embodiment 4: get rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, the ratio of ratio value between 0.1 and 0.9 in total usage quantity (weight) of the usage quantity (weight) of each described alumina particle and two kinds of described alumina particles, take by weighing rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, simply be mixed into dimorphism looks alumina particle powder.
With the C-B sintering aid of 0.5%-3.0% (weight), with the PVA of 1.0%-5.0% (weight), and, the described dimorphism looks alumina particle powder of 2.0%-12.0% (weight), and, the carborundum powder of 70.0%-94.5% (weight), and, the silicon carbide whisker of 2.0%-10.0% (weight), and an amount of water is made into pasty material, carrying out mechanical stirring mixes, simultaneously pasty material is applied ultrasonic wave, after so handling, drying, granulation, compression molding is solidified 100 ℃ of-300 ℃ of temperature ranges, afterwards, 1700 ℃ of-2100 ℃ of temperature range sintering 0.5-3.0 hour, form the silicon carbide ceramics product.
Embodiment 5: get rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, the ratio of ratio value between 0.1 and 0.9 in total usage quantity (weight) of the usage quantity (weight) of each described alumina particle and two kinds of described alumina particles, take by weighing rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, simply be mixed into dimorphism looks alumina particle powder.
AlN+Y with 2.0%-8.0% (weight)
2O
3Sintering aid, PVA with 1.0%-5.0% (weight), and, the described dimorphism looks alumina particle powder of 2.0%-12.0% (weight), and, the carborundum powder of 65.0%-93.0% (weight), and, the silicon carbide whisker of 2.0%-10.0% (weight), and, an amount of water, be made into pasty material, carry out wet ball grinding and mix drying, granulation, compression molding is solidified 100 ℃ of-300 ℃ of temperature ranges, afterwards, 1700 ℃ of-2100 ℃ of temperature range sintering 0.5-3.0 hour, form the silicon carbide ceramics product.
Embodiment 6: get rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, the ratio of ratio value between 0.1 and 0.9 in total usage quantity (weight) of the usage quantity (weight) of each described alumina particle and two kinds of described alumina particles, take by weighing rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, simply be mixed into dimorphism looks alumina particle powder.
Press the element mol ratio 8～17 to 3 of aluminium and yttrium, described dimorphism looks alumina particle powder is mixed with yttrium oxide, carry out ball milling, make difunctional prefabricated material.With the difunctional prefabricated material of 5.0%-20.0% (weight), with the PVA of 1.0%-5.0% (weight), and, the carborundum powder of 65.0%-92.0% (weight), and, the silicon carbide whisker of 2.0%-10.0% (weight), and an amount of water is made into pasty material, carry out wet ball grinding and mix drying, granulation, compression molding is solidified 100 ℃ of-300 ℃ of temperature ranges, afterwards, 1700 ℃ of-2100 ℃ of temperature range sintering 0.5-3.0 hour, form the silicon carbide ceramics product.
Embodiment 7: get rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, the ratio of ratio value between 0.1 and 0.9 in total usage quantity (weight) of the usage quantity (weight) of each described alumina particle and two kinds of described alumina particles, take by weighing rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, simply be mixed into dimorphism looks alumina particle powder.
Press the element mol ratio 8～17 to 3 of aluminium and yttrium, described dimorphism looks alumina particle powder is mixed with yttrium oxide, carry out ball milling, make difunctional prefabricated material.With the difunctional prefabricated material of 5.0%-20.0% (weight), with the PVA of 1.0%-5.0% (weight), and, the carborundum powder of 65.0%-92.0% (weight), and, the silicon carbide whisker of 2.0%-10.0% (weight), and an amount of water is made into pasty material, carry out mechanical stirring and mix drying, granulation, compression molding is solidified 100 ℃ of-300 ℃ of temperature ranges, afterwards, 1700 ℃ of-2100 ℃ of temperature range sintering 0.5-3.0 hour, form the silicon carbide ceramics product.
Embodiment 8: get rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, the ratio of ratio value between 0.1 and 0.9 in total usage quantity (weight) of the usage quantity (weight) of each described alumina particle and two kinds of described alumina particles, take by weighing rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, simply be mixed into dimorphism looks alumina particle powder.
Press the element mol ratio 8～17 to 3 of aluminium and yttrium, described dimorphism looks alumina particle powder is mixed with yttrium oxide, carry out ball milling, make difunctional prefabricated material.Difunctional prefabricated material with 5.0%-18.0% (weight), PVA with 1.0%-5.0% (weight), the magnesium oxide of 0.1%-2.0% (weight), and, the carborundum powder of 65.0%-91.9% (weight), and, the silicon carbide whisker of 2.0%-10.0% (weight), and an amount of water is made into pasty material, carrying out mechanical stirring mixes, drying, granulation, compression molding, solidify 100 ℃ of-300 ℃ of temperature ranges, afterwards, 1700 ℃ of-2100 ℃ of temperature range sintering 0.5-3.0 hour, form the silicon carbide ceramics product.
Embodiment 9: get rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, the ratio of ratio value between 0.1 and 0.9 in total usage quantity (weight) of the usage quantity (weight) of each described alumina particle and two kinds of described alumina particles, take by weighing rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, simply be mixed into dimorphism looks alumina particle powder.
Press the element mol ratio 8～17 to 3 of aluminium and yttrium, described dimorphism looks alumina particle powder is mixed with yttrium oxide, carry out ball milling, make difunctional prefabricated material.Difunctional prefabricated material with 5.0%-20.0% (weight), PVA with 1.0%-5.0% (weight), the magnesium oxide of 0.1%-2.0% (weight), the lanthanum trioxide of 0.1%-2.0% (weight), and, the carborundum powder of 61.0%-91.8% (weight), and, the silicon carbide whisker of 2.0%-10.0% (weight), and, an amount of water, be made into pasty material, carry out mechanical stirring and mix drying, granulation, compression molding is solidified 100 ℃ of-300 ℃ of temperature ranges, afterwards, 1700 ℃ of-2100 ℃ of temperature range sintering 0.5-3.0 hour, form the silicon carbide ceramics product.
Embodiment 10: get rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, the ratio of ratio value between 0.1 and 0.9 in total usage quantity (weight) of the usage quantity (weight) of each described alumina particle and two kinds of described alumina particles, take by weighing rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, simply be mixed into dimorphism looks alumina particle powder.
C-B sintering aid with 0.5%-3.0% (weight), with the PVA of 1.0%-5.0% (weight), the described dimorphism looks alumina particle powder of 2.0%-12.0% (weight), the magnesium oxide of 0.1%-2.0% (weight), the lanthanum trioxide of 0.1%-2.0% (weight), and, the carborundum powder of 66.0%-94.3% (weight), and, the silicon carbide whisker of 2.0%-10.0% (weight), and an amount of water is made into pasty material, carrying out wet ball grinding mixes, drying, granulation, compression molding, solidify 100 ℃ of-300 ℃ of temperature ranges, afterwards, 1700 ℃ of-2100 ℃ of temperature range sintering 0.5-3.0 hour, form the silicon carbide ceramics product.
Embodiment 11: get rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, the ratio of ratio value between 0.1 and 0.9 in total usage quantity (weight) of the usage quantity (weight) of each described alumina particle and two kinds of described alumina particles, take by weighing rod-like aluminum oxide particle raw material and sheet-shaped alpha-alumina particles raw material, simply be mixed into dimorphism looks alumina particle powder.
C-B sintering aid with 0.5%-3.0% (weight), PVA with 1.0%-5.0% (weight), the described dimorphism looks alumina particle powder of 2.0%-12.0% (weight), the magnesium oxide of 0.1%-2.0% (weight), the lanthanum trioxide of 0.1%-2.0% (weight), the glycerine of 0.1%-2.0% (weight), the oleic acid of 0.1%-2.0% (weight), and, the carborundum powder of 62.0%-94.1% (weight), and, the silicon carbide whisker of 2.0%-10.0% (weight), and an amount of water is made into pasty material, carrying out wet ball grinding mixes, drying, granulation, compression molding, solidify 100 ℃ of-300 ℃ of temperature ranges, afterwards, 1700 ℃ of-2100 ℃ of temperature range sintering 0.5-3.0 hour, form the silicon carbide ceramics product.
For making things convenient for the technician outside this area to understand and enforcement the present invention, it is norbide that the embodiment of all relating in the embodiment of the invention " C-B sintering aid ", " C-B sintering aid " all specify, i.e. B
4C.
For making things convenient for the technician outside this area to understand and enforcement the present invention all " AlN+Y that relates in the embodiment of the invention
2O
3Sintering aid " embodiment, " AlN+Y
2O
3Sintering aid " all to specify be AlN and Y
2O
3Mol ratio is 2 to 1 mixture.
In the various embodiments of the present invention, the consumption of related raw material all provides with range format, implements by listed amount ranges, all can realize purpose of the present invention in varying degrees; For making things convenient for the technician outside this area to understand and enforcement the present invention, the intermediate value that can specify the listed amount ranges of each raw material is an optimum amount enforcement value.
For making things convenient for the technician outside this area to understand and enforcement the present invention, it is vacuum carbon tube furnace or hot-pressed sintering furnace that agglomerating plant can be specified; Can find the supplier of many these kind equipments on the internet.
Testing method and dependence test instrument about ceramic performance, for making things convenient for the technician outside this area to go and find out what's going on, be described as follows: key in retrieval with suitable keyword,, can find many relevant informations by Chinese periodical net and foreign language periodicals net and each large search instrument of internet.
Claims (1)
1. the method for preparing silicon carbide ceramic composition of a silicon carbide-containing whisker, the main raw material of this manufacture method is a carborundum powder, sintering aid, toughness reinforcing material and wedding agent, the main technique step is to mix, moulding, solidify, high temperature sintering, through above-mentioned main technique step, form the silicon carbide ceramics product, the toughness reinforcing material that contains in the raw material is the material that adds for the toughness that increases silicon carbide ceramics, the sintering processing of described high-sintering process step is not have to press solidly phase sintering or do not have the hydraulic fluid phase sintering, it is characterized in that, the toughness reinforcing material that is adopted is made up of rod-like aluminum oxide particle and sheet-shaped alpha-alumina particles and three kinds of plasticizing substances of silicon carbide whisker, described rod-like aluminum oxide particle is that granule-morphology is bar-shaped aluminum oxide powder, described sheet-shaped alpha-alumina particles is a granule-morphology aluminum oxide powder in the form of sheets, and, the ratio value of the weight of the weight of each described plasticizing substance and described toughness reinforcing material integral body is between 0.1 and 0.8, the aspect ratio distribution of described rod-like aluminum oxide particle is between 3 and 5, the radial width of described rod-like aluminum oxide particle is distributed between 0.1 micron and 0.8 micron, the plate width of described sheet-shaped alpha-alumina particles is between 0.3 micron and 6.0 microns, the plate width of described sheet-shaped alpha-alumina particles and the ratio of sheet are between 3 and 10, and, the weight percent of each raw material is respectively: norbide 0.5%～3.0%, polyvinyl alcohol 1.0%～5.0%, dimorphism looks alumina particle powder 2.0%～12.0%, carborundum powder 70.0%～94.5%, silicon carbide whisker 2.0%～10.0%, described dimorphism looks alumina particle powder is the simple mixtures of described rod-like aluminum oxide particle and described sheet-shaped alpha-alumina particles, wherein, the ratio of the weight of the weight of described rod-like aluminum oxide particle and described dimorphism looks alumina particle powder is between 0.1 and 0.9, and the ratio of the weight of the weight of described sheet-shaped alpha-alumina particles and described dimorphism looks alumina particle powder is between 0.1 and 0.9.
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| C.S.MONTROSS.Conductivity and strengh behaviour of alumina-zirconia composites.JOURNAL OF MATERIALS SCIENCE 30.1995,(30),3285-3290. |
| C.S.MONTROSS.Conductivity and strengh behaviour of alumina-zirconia composites.JOURNAL OF MATERIALS SCIENCE 30.1995,(30),3285-3290. * |
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