CN101880163A - Method for preparing silicon carbide whisker in-situ reinforced aluminum oxide ceramic - Google Patents
Method for preparing silicon carbide whisker in-situ reinforced aluminum oxide ceramic Download PDFInfo
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Abstract
The invention discloses a method for preparing silicon carbide whisker in-situ reinforced aluminum oxide ceramic, which is characterized in that: a four-component assistant is MO (M is one of Mg, Ba, Be and Ca)-SiO2-C-LxOy(L is one of transitional metals of Fe, Ni and Cu); the MO, SiO2 and C account for 0.10 to 0.7 percent of the total weight of the assistant; the LxOy accounts for 0.05 to 0.15 percent of the total assistant; and the granularity of the four-component assistant is between 1 and 10 micrometers. The main raw materials including 70 to 93 weight percent of aluminum oxide powder, 5 to 20 weight percent of the four-component assistant and 2 to 5 weight percent of a bonding agent, and the aluminum oxide ceramic sintered body is formed by steps of ball milling, screening, forming, high-temperature sintering and the like. The method reduces production cost and solves the problems of serious agglomeration of the silicon carbide whiskers and low compatibility with the aluminum oxide ceramic substrate; in addition, the silicon carbide whiskers are generated gradually in the sintering process of the aluminum oxide ceramic, the resistance of mass transfer of the aluminum oxide particles is small, and the influence on the sintering speed of the aluminum oxide ceramic is light. Thus, a good reinforcing effect is formed.
Description
Technical field
The present invention relates to the alumina-ceramic manufacture method, particularly about the toughness reinforcing alumina-ceramic manufacture method of a kind of silicon carbide whisker.
Background technology
Alumina-ceramic has stable chemical performance, physical strength height, hardness is big, high temperature resistant, wear resistance is good, electrical isolation capabilities is high, anti-oxidant, good mechanical properties, raw material are contained many advantages such as abundant, cheap, it is the high-performance multipurpose engineering ceramics that a kind of Application Areas is the widest, consumption is maximum, the application development potentiality are big, be widely used in every field [E.Medvedovski such as mechanical chemical industry, electronics, aviation and national defence, Wear-resistant engineering ceramics, Wear, 249,2001,821-828; Boutin P., Arthroplastie Totale de Hance par Prosthes en Alumine Fritte, Rev.Chir.Orthop., 1972,58:229-246.], the title of " ceramic king " is arranged.
In industrial production, the control valve in the pneumatic element family, distribution valve are the weak links in the pneumatic control system always; Its major cause is because of the easy wear out failure of moving parts.The traditional material of these moving partss is Al alloy materials, though in light weight, corrosion-resistant surface hardness is low, and is easy to wear.If adopt the core components of alumina ceramic material as industrial valve, more corrosion-resistant and wear-resistant than metal, alloy core components, can improve greatly its work-ing life, can reach more than 200,000 times work-ing life after tested.In order to adapt to the deficient day by day challenge of current water resources, stopping property, wearability and erosion resistance to the water tap cock are had higher requirement, traditional plastics spool or Stainless Steel Ball spool are under relatively poor condition of water quality, the comfort, stopping property of operation descends, the wearing and tearing aggravation, be prone to leak, dripping phenomenon.And the water tap hand feel and drape of fine ceramic cartridge, long service life (high-quality ceramic cartridge switch number of times can reach more than 1,000,000 times), Beijing installed the ceramic cartridge water tap as far back as 1996 years with regard to issue regulations Compulsory Feature developer in newly-built residential building.
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, and abrasion resistance properties is good.In addition, 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.The hardness height of alumina-ceramic, frictional coefficient are little, can obtain good sliding properties as the mechanical seal end surface material.At present, alumina-ceramic has obtained a large amount of application in all kinds of mechanical seals (the particularly all kinds of pumps of chemical industry, water conservancy, mechanical industry), makes work-ing life of machinery significantly improve and production cost, maintenance cost descend significantly.Alumina-ceramic also successfully is used as various bearings and cutting tool in mechanical industry, alumina tool has that hardness height, wear resisting property and mechanical behavior under high temperature are good, chemical stability good, be difficult for taking place with metal characteristics such as bonding, and factory is general to be applied to the cutting of hardworking material, superhigh-speed cutting, high-speed dry cutting and to cut firmly etc.The optimum cutting speed of sintex than the high 3-10 of inserted tool doubly can increase substantially machining efficient.Control and multiple toughened and reinforced means by to grain-size, pattern all are greatly improved intensity, toughness, the shock resistance of sintex.Ceramic cutting tool material be considered to 21 century be hopeful most, the most competitive cutter material.
Substitute material for human hard tissues is (as artificial hip joint, knee joint, the repair materials of artificial root of the tooth, middle ear ear bones and other bone injury) requirement on clinical medicine is increasing, requires these materials to have excellent biological compatibility, resistance to abrasion, mechanical stability, very high physical strength.Hydroxylapatite ceramic (HA pottery) biological ceramics has good biological activity, soft or hard tissue energy good combination with human body, fixing reliable, but the resistance to abrasion of HA pottery and physical mechanical index can not reach the standard of hard tissue substituting material, can not use separately in high mechanical load occasion.And alumina-ceramic has higher physical strength, hardness, wear resistance and unreactiveness; in human body, can not be subjected to rejection, chemical property is stable, corrosion-resistant, do not wear out; and alumina surface very thin (＜5um) hydration layer helps to form biological good compatible protective membrane because wetting ability can form one deck.In addition, under the condition that retains in for a long time in the body, this pottery can keep physics and biological chemical performance, thereby constituted the good prerequisite of reactionless implantation and life-time service, therefore alumina-ceramic is very extensive as biological ceramics application clinically, has special application prospect aspect oral cavity and the bone graft.
Yet will further improve the application performance of alumina-ceramic, how solve the fragility problem, be the focus of a concern.The fragility problem also is the common issue with 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.
Because do not exist by endergonic mechanism such as crystal boundary slippage and dislocations in the stupalith, so, in order to improve the toughness of stupalith, must in stupalith, introduce certain endergonic mechanism, to absorb the energy of ceramic crack propagation.Introducing enhancing body formation ceramic matric composite in stupalith is to improve one of stupalith flexible main method [Mah T.I., Mendiratta M.G., Katz A.P., et al.Am.Ceram.Soc.Bull., 1987,66 (2): 304.].It has been generally acknowledged that more effective method for toughening has the zirconium white transformation toughening, particle dispersion is toughness reinforcing and fiber (whisker) strengthening and toughening.Si
3N
4/ nano SiC diphase ceramic material [the refined hero of autumn ancestor, Nippon Seramikkusu Kyokai Gakujutsu Ronbunshi, 1990,98 (5): 424.] is that the exemplary particles disperse is toughness reinforcing.But from result of study, particle dispersion is toughness reinforcing certain limitation, and toughening effect is not remarkable.Transformation toughening is with a kind of additive of zirconium white as pottery, and it will take place by the four directions transformation of monocline phase in opposite directions down stress induced, thereby produces the zone of inelastic deformation around crack tip, and the toughness of stupalith is improved.Yet transformation toughening is a structure and temperature sensitive, at high temperature can lose its toughening effect.Crystal whisker excess weld metal is toughness reinforcing to be to study one of more effective toughness reinforcing means in recent ten years.After the seventies, the appearance of high performance ceramic fiber and whisker has brought excellent opportunity for the development of stupalith.The intensity height of SiC whisker, big, the Heat stability is good of Young's modulus; So, on stupalith toughness reinforcing, become first-selected flexibilizer additive.Its practical application makes the performance of material obtain very big improvement.People are respectively from dispersing technology [the Shalek P.D. of silicon carbide whisker pottery, J.Am.Ceram.Soc., 1998, (2): 65], the sintering method of silicon carbide whisker toughening ceramic and the silicon carbide whisker all many-sides such as toughening mechanism in pottery have been carried out a large amount of research [Kazuo U., J.Ceram.Soc., Japan, 1992,100 (4): 525].Though the crystal whisker toughened aluminum oxide pottery has been obtained certain achievement, yet, this wherein also exists many problems, it at first is the dispersing technology complexity, the SiC whisker is the coacervate state more and exists, and must take adequate measures to make it can be distributed in the toughening effect that just can obtain expection in the ceramic matrix equably.In addition, silicon carbide whisker and alumina-ceramic matrix phase interface are big, and consistency is relatively poor, exists the interface complexcase, and silicon carbide whisker is difficult to be evenly dispersed in the ceramic matrix.Secondly, because the adding of SiC whisker has strengthened the mass transfer path of matrix, particularly when whisker content is higher, form spatial grid structure easily and the rearrangement process of blapharoplast is obstructed, make sintering densification speed reduce [Holm E., Cima M.J., J.Am.Ceram.Soc. greatly, 1989,72 (2): 303].These problems are in the research and development of perplexing the silicon carbide whisker reinforced alumina ceramic in varying degrees.
Summary of the invention
Technical problem to be solved by this invention is a kind of method of introducing silicon carbide whisker in-situ reinforced aluminum oxide ceramic that provides at existing background technology.This method is sneaked into MO (M is Mg, Ba, Be, a kind of among the Ca)-SiO in the sintering precursor powder
2-C-L
xO
y(L is a transition metal, is Fe, Ni, a kind of among the Cu) four component assistant, wherein MO-SiO
2-Al
2O
3Constitute the liquid phase sintering system, under sintering temperature, this component assistant system is in a liquid state, the existence of liquid phase made things convenient for alumina particle rearrangement and by " dissolving-precipitation,, the mechanism acceleration of sintering significantly reduces Al
2O
3The sintering temperature of pottery.And the L in the system
xO
yBe catalyzer, catalysis carbon dust in-situ reducing SiO under suitable temperature
2Form fibrous silicon carbide whisker, increase the effect of alumina-ceramic flexible thereby play.Silicon carbide whisker is reunited serious like this, and the consistency difference between the alumina-ceramic matrix and the problem that can not finely be dispersed in the ceramic matrix has obtained good solution, in addition, silicon carbide whisker progressively forms in alumina-ceramic agglomerating process, resistance to mass transfer to alumina particle is less, and is also less to the influence of the sintering rate of alumina-ceramic.
The present invention solves the problems of the technologies described above the technical scheme that is adopted and is characterised in that main raw material 70-93wt% is alumina powder jointed, 5-25wt%MO (M is Mg, Ba, Be, a kind of among the Ca)-SiO
2-C-L
xO
y(L is a transition metal, be Fe, Ni, a kind of among the Cu) four component assistant, 2-5wt% wedding agent, formed the sintering precursor powder in 1-8 hour by the mixing of high energy ball mill ball milling at normal temperatures, main technique steps such as this precursor powder sieves, moulding, curing, high temperature sintering form silicon carbide whisker in-situ reinforced alumina ceramic product.
Above-mentioned novel four-component auxiliary agent is MO (M is Mg, Ba, Be, a kind of among the Ca)-SiO
2-C-L
xO
y(L is a transition metal, is Fe, Ni, a kind of among the Cu) four mixture, MO, SiO
2, C accounts for the weight percent of whole auxiliary agent between 0.10-0.7.L
xO
yThe weight percent that accounts for whole auxiliary agent is between 0.05-0.15.These component compounds all can be bought on market and obtain.Very useful is under sintering temperature (1300 ℃-1400 ℃), MO-SiO
2-Al
2O
3Form liquid phase, the existence of liquid phase has made things convenient for the rearrangement of alumina particle and by " dissolving-precipitation " mechanism acceleration of sintering, has significantly reduced Al
2O
3The sintering temperature of pottery; This four component assistant granularity is the non-nano yardstick all, between the 1-10 micron, is very easy to reach the state that mixes at short notice by planetary ball mill.
Above-mentioned wedding agent can be a kind of among resol, the PVA (polyvinyl alcohol).
Above-mentioned moulding is that precursor powder is placed in the cylindrical die, under the pressure at 200-250MPa in high tonnage hydropress static 5 minutes again the demoulding obtain.
Above-mentioned high-temperature sintering process is, being evacuated down to vacuum tightness with oil-sealed rotary pump is 4-5Pa, feeds in the temperature programming of minute-pressure Ar gas (0.10-0.13MPa) atmosphere and is warmed up to 1200 ℃-1250 ℃ and insulation 10-20 minute under this temperature with 5-8 ℃/minute speed; With 10-15 ℃/minute speed be warmed up to 1300 ℃-1400 ℃ and under this temperature the insulation 1-3 hour; The process of original position carbon reduction silicon-dioxide takes place also to finish substantially at 1250 ℃ of holding stages.
Compared with prior art, the invention has the advantages that: adopt novel four-component auxiliary agent MO (M is Mg, Ba, Be, a kind of among the Ca)-SiO
2-C-L
xO
y(L is a transition metal, be Fe, Ni, a kind of among the Cu) can be in the process of 1300 ℃ of-1400 ℃ of liquid phase sintering alumina-ceramic of lower temperature, reaction in generates the silicon carbide whisker of nanoscale under the effect of catalyzer, avoided in the sintering precursor powder, adopting physical method to introduce silicon carbide whisker, not only reduced production cost, and silicon carbide whisker reunite serious, and the consistency difference between the alumina-ceramic matrix and the problem that can not finely be dispersed in the ceramic matrix has obtained good solution; In addition, silicon carbide whisker progressively forms in alumina-ceramic agglomerating process, and is less to the resistance to mass transfer of alumina particle, also less to the influence of the sintering rate of alumina-ceramic.Thereby play good toughening effect.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1: get MgO: SiO
2: C: Fe
2O
3Mass ratio=0.4: 0.45: 0.1: 0.05 mixture (account for precursor powder total mass 10%) is alumina powder jointed with 88wt%, 2wt% resol, mix with identical weight ethanol and form suspension at normal temperatures, this suspension is put in the ball grinder of nylon sock to take out after 3 hours through the high energy ball mill ball milling.Through under 80 degree dry 2 hours, after pulverizing, sieving, under 220Mpa, leave standstill in the cylindrical die of packing into and obtained biscuit in 5 minutes.Biscuit 250 ℃ of thermal treatments 20 minutes, is removed phenolic resin binder.Biscuit is placed on is evacuated down to vacuum tightness 4-5Pa in the vacuum carbon tube furnace, the conversion argon gas is to pressure-fired 0.12MPa.The design temperature controller makes the temperature in the furnace chamber rise to 1200 ℃ with 5 ℃/minute, insulation is 15 minutes under this temperature, rise to 1350 ℃ and with 10 ℃/minute speed then, naturally cool to normal temperature with stove and be the toughness reinforcing alumina-ceramic sintered body of original position silicon carbide whisker at the closing temperature controller after 1 hour of insulation under this temperature.
Embodiment 2: get CaO: SiO
2: C: CuO mass ratio=0.4: 0.4: 0.12: 0.08 mixture (account for precursor powder total mass 5%) is alumina powder jointed with 90wt%, the 5wt% PVAC polyvinylalcohol, mix with identical weight ethanol and form suspension at normal temperatures, this suspension is put in the ball grinder of nylon sock to take out after 5 hours through the high energy ball mill ball milling.Through under 80 degree dry 2 hours, after pulverizing, sieving, under 230Mpa, leave standstill in the cylindrical die of packing into and obtained biscuit in 5 minutes.Biscuit 250 ℃ of thermal treatments 20 minutes, is removed the polyvinyl alcohol wedding agent.Biscuit is placed on is evacuated down to vacuum tightness 4-5Pa in the vacuum carbon tube furnace, the conversion argon gas is to pressure-fired 0.12MPa.The design temperature controller makes the temperature in the furnace chamber rise to 1250 ℃ with 5 ℃/minute, insulation is 15 minutes under this temperature, rise to 1350 ℃ with 10 ℃/minute speed then, and, naturally cool to normal temperature with stove and be the toughness reinforcing alumina-ceramic sintered body of original position silicon carbide whisker at 1350 ℃ of following insulation closing temperature controllers after 2 hours.
Embodiment 3: get BaO: SiO
2: C: NiO mass ratio=0.45: 0.3: 0.15: 0.1 mixture (account for precursor powder total mass 15%) is alumina powder jointed with 83wt%, 2wt%PVA, mix with identical weight ethanol and form suspension at normal temperatures, this suspension is put in the ball grinder of nylon sock to take out after 5 hours through the high energy ball mill ball milling.Drying is 2 hours under 80 degree, after pulverizing, sieving, leaves standstill under 250Mpa in the cylindrical die of packing into and obtains biscuit in 5 minutes.Biscuit 250 ℃ of thermal treatments 20 minutes, is removed the PVA wedding agent.Biscuit is placed on is evacuated down to vacuum tightness 4-5Pa in the vacuum carbon tube furnace, the conversion argon gas is to pressure-fired 0.12MPa.The design temperature controller makes the temperature in the furnace chamber rise to 1250 ℃ with 6 ℃/minute, insulation is 20 minutes under this temperature, rise to 1400 ℃ and with 13 ℃/minute speed then, naturally cool to normal temperature with stove and be the toughness reinforcing alumina-ceramic sintered body of original position silicon carbide whisker at the closing temperature controller after 1.5 hours of insulation under this temperature.
Claims (4)
1. the method for an original position silicon carbide whisker reinforced alumina ceramic, this method feature is to sneak into the novel four-component auxiliary agent in the sintering precursor powder, wherein two kinds of auxiliary agents and aluminum oxide constitute the liquid phase sintering system, under sintering temperature, this component assistant system is in a liquid state, the existence of liquid phase has made things convenient for the rearrangement of alumina particle and by " dissolving-precipitation " mechanism acceleration of sintering, has significantly reduced Al
2O
3The sintering temperature of pottery; And another composition is a catalyzer in the system, catalysis and in situ reduction SiO
2Form fibrous silicon carbide whisker, increase the effect of alumina-ceramic flexible thereby play; Silicon carbide whisker is reunited serious like this, and the consistency difference between the alumina-ceramic matrix and the problem that can not finely be dispersed in the ceramic matrix has obtained good solution, in addition, silicon carbide whisker progressively forms in alumina-ceramic agglomerating process, resistance to mass transfer to alumina particle is less, and is also less to the influence of the sintering rate of alumina-ceramic; Main raw material 70-93wt% is alumina powder jointed, 5-25wt% four component assistant, 2-5wt% wedding agent, formed the sintering precursor powder in 1-8 hour by the mixing of high energy ball mill ball milling at normal temperatures, main technique steps such as this precursor powder sieves, moulding, curing, high temperature sintering form silicon carbide whisker in-situ reinforced alumina ceramic product.
2. method according to claim 1 is characterized in that the novel four-component auxiliary agent is MO (M is Mg, Ba, Be, a kind of among the Ca)-SiO
2-C-L
xO
y(L is a transition metal, is Fe, Ni, a kind of among the Cu), MO, SiO
2, C account for whole auxiliary agent weight percent between 0.10-0.7, L
xO
yThe weight percent that accounts for whole auxiliary agent is between 0.05-0.15, and this four component assistant granularity is the non-nano yardstick all, between the 1-10 micron.
3. method according to claim 1 is characterized in that described wedding agent can be a kind of among resol, the PVA (polyvinyl alcohol).
4. method according to claim 1, it is characterized in that high-temperature sintering process is, being evacuated down to vacuum tightness with oil-sealed rotary pump is 4-5Pa, feeds in the temperature programming of minute-pressure Ar gas (0.10-0.13MPa) atmosphere and is warmed up to 1200 ℃-1250 ℃ and insulation 10-20 minute under this temperature with 5-8 ℃/minute speed; With 10-15 ℃/minute speed be warmed up to 1300 ℃-1400 ℃ and under this temperature the insulation 1-3 hour.
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| CN102093067A (en) * | 2010-12-14 | 2011-06-15 | 江苏联能电子技术有限公司 | Nano Al2O3 crystal whisker-toughened ceramic material with high piezoelectric property and preparation method thereof |
| CN104310978A (en) * | 2014-09-30 | 2015-01-28 | 苏州博利迈新材料科技有限公司 | High-temperature-resistant ceramic powder coating material and preparation method thereof |
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| CN106800420A (en) * | 2016-12-30 | 2017-06-06 | 河南工业大学 | A kind of silicon carbide whisker in-situ composite corindon high-temperature ceramic materials and preparation method thereof |
| CN108686524A (en) * | 2018-05-08 | 2018-10-23 | 武汉工程大学 | The preparation method of the silicon carbide ceramics hollow-fibre membrane of silicon carbide whisker strengthening and toughening |
| CN110204333A (en) * | 2019-07-09 | 2019-09-06 | 成都贝施美生物科技有限公司 | A kind of processing technology for the multilayer zirconium oxide porcelain block that can quickly prepare even transition |
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| CN106800420B (en) * | 2016-12-30 | 2021-07-16 | 河南工业大学 | Silicon carbide whisker in-situ composite corundum high-temperature ceramic material and preparation method thereof |
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| CN110204333A (en) * | 2019-07-09 | 2019-09-06 | 成都贝施美生物科技有限公司 | A kind of processing technology for the multilayer zirconium oxide porcelain block that can quickly prepare even transition |
| CN110204333B (en) * | 2019-07-09 | 2021-10-12 | 成都贝施美生物科技有限公司 | Processing technology capable of rapidly preparing multi-layer zirconium oxide ceramic blocks with uniform transition |
| CN110483085A (en) * | 2019-08-01 | 2019-11-22 | 广东工业大学 | A kind of whisker reinforcement alumina composite ceramic and the preparation method and application thereof |
| CN110483085B (en) * | 2019-08-01 | 2022-10-04 | 广东工业大学 | Whisker reinforced alumina composite ceramic and preparation method and application thereof |
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