CN101767981A - Alumina ceramics composite containing novel four-component sintering adjuvant - Google Patents
Alumina ceramics composite containing novel four-component sintering adjuvant Download PDFInfo
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- CN101767981A CN101767981A CN200910132061A CN200910132061A CN101767981A CN 101767981 A CN101767981 A CN 101767981A CN 200910132061 A CN200910132061 A CN 200910132061A CN 200910132061 A CN200910132061 A CN 200910132061A CN 101767981 A CN101767981 A CN 101767981A
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- alumina
- sintering
- alumina ceramics
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Abstract
The invention discloses an alumina ceramics composite containing a novel four-component sintering adjuvant, which is characterized in that the four-component adjuvant is MO-CaO-SiO2-L2O3, wherein M is one of Mg, Ba and Be, and L is a rare earth element which is one of Ce, La and Lu. The alumina ceramics composite has the following components in percentage by weight: (1), 75%-90% of alumina powder; (2), 3%-6% of nano MO (M is one of Mg, Ba and Be); (3), 2%-6% of nano SiO2; (4), 2%-6% of nano CaO; and (5), 3%-7% of nano L2O3 (L is the rare earth element which is one of Ce, La and Lu). The particle size of the four-component sintering adjuvant is less than 300 nanometers, and the particle size of main alumina powder is at nanometer scale, namely 1-10 nanometers. By forming liquid phase and gradually forming spinel-like matter (the melting point thereof is more than 2100 DEG C) at later sintering stage to eliminate the liquid phase, sintering is promoted and simultaneously the growth of grain is inhibited, air hole elimination is promoted, density is improved and fine and even alumina ceramics grain and grain boundary air hole are formed, thereby ensuring the alumina ceramics material to have better high-temperature mechanical performance and wear resistance.
Description
Technical field
The present invention relates to the alumina-ceramic manufacture method, particularly about a kind of alumina ceramics composite that contains sintering aid.
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, is widely used in the cutting of hardworking material, superhigh-speed cutting, high-speed dry cutting and cuts 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.
The alumina-ceramic sealing member that uses in these occasions, valve spool, high speed sintex, alumina-ceramic grinding medium, component of machine (as the porcelain axle), porcelain great waves etc. have all required the excellent abrasive energy, the alumina-ceramic that wear resistance is good means longer work-ing life, can be applied in more abominable and the environment strict high request.Particularly very high to the requirement of aluminum oxide mill Jie wear resistance in the materials such as substrate, IC encapsulation, cutting tool and liquid-crystal display, television picture tube coating of electronic industry are made, otherwise can produce serious pollution.Yet the wear resisting property of alumina-ceramic is a very complicated factors, with the microcosmic fine structure of alumina surface confidential relation is arranged.There are some researches show that the alumina grain crystallization is tiny, all even crystal boundary micropore of size is less and being evenly distributed is alumina-ceramic toughness and wear resistance microstructure characteristic [Zheng Yuanshan, Peng Jianzhong, Zhang Hongbo, Wang Yimin preferably, the microtexture his-and-hers watches The surface roughness affected of alumina-ceramic, the material Leader, 2000,14,116-118].That is to say that the densification that need be issued to alumina ceramic material in lower temperature for the alumina-ceramic that obtains superior performance (avoids excessively growing up of crystal grain at high temperature, guarantee even and tiny crystal grain, even and small grain boundary porosity) and the control heterogeneous microstructure be transgranular fracture, avoid along the generation of brilliant fracture.This also is the raising Alumina Ceramics, widens its Application Areas, improves the key of value of the product.
The liquid phase sintering of alumina-ceramic is at Al
2O
3Form liquid phase between the blapharoplast, made things convenient for Al
2O
3Particulate is reset, and by " dissolving-precipitation " mechanism acceleration of sintering, significantly reduces Al simultaneously
2O
3The sintering temperature of pottery can make that heterogeneous microstructure is a transgranular fracture under the ultimate load, and the liquid phase sintering auxiliary agent of comparative maturity has CaO+Al at present
2O
3+ SiO2, MgO+Al
2O
3[WU Y.Q. such as+SiO2, ZHANGY.F., HUANG X.X., et al.Microstructural development and mechanicalproperties of self-reinforced alumina with CAS addition[J] .J.Eur.Ceram.Soc., 2000,20:1-7.], be the good preparation method that improves the aluminum oxide wear resisting property.Yet liquid phase sintering also has many shortcomings, and at first liquid phase remains in crystal boundary as glassy phase, makes hot strength, wear resistance descend the application scenario that can not satisfy some comparatively high temps; Secondly particularly cause easily that in the sintering later stage crystal grain grows up unusually [Suzuki is expanded luxuriant chief editor, and Chen Shixing translates, engineering ceramics, Beijing: Science Press, 1989.] and hinder the further raising of performance.Therefore merely promote to reduce the auxiliary agent of sintering temperature effect by mass transfer uniform ceramic crystalline grain is not enough to forming tiny by forming the eutectic liquid phase.The composition of auxiliary agent and form need further screen and consider.
Summary of the invention
Technical problem to be solved by this invention is a kind of alumina ceramics composite that contains four component sintering aids that provides at existing background technology.This nanometer four-component auxiliary agent is MO (M is Mg, Ba, a kind of among the Be)-CaO-SiO
2-L
2O
3(L is a rare earth element, is Ce, La, a kind of among the Lu) four component assistant, wherein MO+Al
2O
3+ SiO
2Constitute the liquid phase sintering system, under sintering temperature, this component assistant system is in a liquid state, and the existence of liquid phase has made things convenient for the rearrangement of alumina particle and by " dissolving-precipitation " mechanism acceleration of sintering, significantly reduced Al
2O
3The sintering temperature of pottery.And the L in the system
2O
3And MO and Al
2O
3Can form spinels material (its fusing point＞2100 ℃) gradually in the agglomerating later stage, this melting point substance is higher to show solid-state under sintering temperature, they are positioned at crystal boundary and suppress grain growth, promote pore to get rid of the density that improves ceramic post sintering, thereby form tiny and uniform alumina-ceramic crystal grain and grain boundary porosity, thereby make the alumina ceramics composite material that high-temperature machinery, wear resisting property preferably be arranged.
The present invention reaches by the following technical solutions, and this technical scheme provides a kind of alumina ceramics composite that contains the novel four-component auxiliary agent, and it is composed as follows:
(1) alumina powder jointed 75%～90% (weight)
(2) nanometer MO (M is Mg, Ba, a kind of among the Be) 3%～6% (weight)
(3) nanometer SiO
22%～6% (weight)
(4) nanometer CaO 2%～6% (weight)
(5) nanometer L
2O
3(L is a rare earth element, is Ce, La, a kind of among the Lu) 3%～7% (weight)
The technical scheme that adopts is characterized in that this four components sintering of nano-material builder granule yardstick below 300 nanometers, but the alumina powder jointed granularity of main body is at micro-meter scale (1-10 micron).These nano assistants all can be bought on market and obtain, and can receive occasion company in Beijing as nano silicon and calcium oxide and buy and obtain or also can prepare voluntarily by methods such as collosol and gels.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; And the L in the system
2O
3And MO and Al
2O
3Can form spinels material (its fusing point＞2100 ℃) gradually in the agglomerating later stage, this melting point substance is higher to show solid-state under sintering temperature, and they have reduced vitreous state eutectic content on the one hand; They are positioned at the density that crystal boundary suppresses grain growth, promotes pore eliminating raising ceramic post sintering on the other hand, thereby form tiny and uniform alumina-ceramic crystal grain and grain boundary porosity, thereby make the alumina ceramics composite material that high-temperature machinery, wear resisting property preferably be arranged.In the sintering precursor powder, main raw material is alumina powder jointed, four component assistant shared weight ratio in integral body is 95-99%, and all the other 1-5wt% are wedding agent, be used in the moulding process of precursor powder bonding powder, keep certain shape.These wedding agents will decompose in follow-up heat treatment process and remove.
Compared with prior art, the invention has the advantages that: adopt novel four-component auxiliary agent MO (M is Mg, Ba, a kind of among the Be)-CaO-SiO
2-L
2O
3(L is a rare earth element, be Ce, La, a kind of among the Lu) can either reduce the sintering temperature to 1300 ℃-1400 ℃ of alumina-ceramic, reduce its content by the sintering aid component in the reaction formation high-melting-point spinel substances of sintering later stage and liquid phase component again simultaneously, improve the hot strength and the antioxidant property of alumina ceramics composite; Suppress grain growth, promote pore to get rid of to improve ceramic composition agglomerating density, thereby form tiny and uniform alumina-ceramic crystal grain and grain boundary porosity make the alumina ceramics composite material that high-temperature machinery, wear resisting property preferably be arranged.Its high strength that is particularly suitable in the severe rugged environment is at high temperature used continuously.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1: get nano-MgO: nanometer La
2O
3: nanometer CaO: nanometer SiO
2Mass ratio=0.15: 0.15: 0.3: 0.4 mixture (account for precursor powder total mass 10%) and 88wt% carborundum powder, 2wt% resol, mix with the water of identical weight and form suspension at normal temperatures, the process electric mixer stirs evenly and insert the 1000W large-power supersonic transducer after 5 minutes in this suspension, stirs evenly through electric mixer and insert the 1000W large-power supersonic transducer after 5 minutes in this suspension.Start ultra-sonic generator, apply the impulse ultrasound field.Work after 20 minutes suspension filtered, the drying that will obtain, pulverize, sieve after, compression molding in the mould of packing into.Biscuit is removed wedding agent temperature programming in vacuum carbon tube furnace through Overheating Treatment, be incubated 1 hour down at 1350 ℃, closing temperature controller after being incubated 30 minutes under 1380 ℃ naturally cools to normal temperature with stove and is the alumina-ceramic sintered body.
Embodiment 2: get nano BeO: nano Ce
2O
3: nanometer CaO: nanometer SiO
2Mass ratio=0.2: 0.2: 0.4: 0.2 mixture (account for precursor powder total mass 5%) and 90wt% carborundum powder, 5wt% resol, mix with the water of identical weight and form suspension at normal temperatures, the process electric mixer stirs evenly and insert the 1500W large-power supersonic transducer after 5 minutes in this suspension, stirs evenly through electric mixer and insert the 1500W large-power supersonic transducer after 5 minutes in this suspension.Start ultra-sonic generator, apply the impulse ultrasound field.Work after 20 minutes suspension filtered, the drying that will obtain, pulverize, sieve after, compression molding in the mould of packing into.Biscuit is removed wedding agent temperature programming in vacuum carbon tube furnace through Overheating Treatment, be incubated 1.5 hours down at 1380 ℃, closing temperature controller after being incubated 20 minutes under 1430 ℃ naturally cools to normal temperature with stove and is the alumina-ceramic sintered body.
Embodiment 3: get nanometer BaO: nanometer Lu
2O
3: nanometer CaO: nanometer SiO
2Mass ratio=0.3: 0.3: 0.2: 0.2 mixture (account for precursor powder total mass 15%) and 83wt% carborundum powder, 2wt%PVA, mix with the water of identical weight and form suspension at normal temperatures, the process electric mixer stirs evenly and insert the 2000W large-power supersonic transducer after 5 minutes in this suspension, stirs evenly through electric mixer and insert the 2000W large-power supersonic transducer after 5 minutes in this suspension.Start ultra-sonic generator, apply the impulse ultrasound field.Work after 20 minutes suspension filtered, the drying that will obtain, pulverize, sieve after, compression molding in the mould of packing into.Biscuit is removed wedding agent temperature programming in vacuum carbon tube furnace through Overheating Treatment, be incubated 1.5 hours down at 1400 ℃, closing temperature controller after being incubated 20 minutes under 1450 ℃ naturally cools to normal temperature with stove and is the alumina-ceramic sintered body.
Claims (3)
1. alumina ceramics composite that contains novel four-component sintering additive, it is composed as follows:
(1) alumina powder jointed 75%～90% (weight)
(2) nanometer MO (M is Mg, Ba, a kind of among the Be) 3%～6% (weight)
(3) nanometer SiO
22%～6% (weight)
(4) nanometer CaO 2%～6% (weight)
(5) nanometer L
2O
3(L is a rare earth element, is Ce, La, a kind of among the Lu) 3%～7% (weight).
2. alumina ceramics composite according to claim 1 it is characterized in that this four components sintering of nano-material builder granule yardstick below 300 nanometers, but the alumina powder jointed granularity of main body is at micro-meter scale (1-10 micron).
3. alumina ceramics composite according to claim 1 is characterized in that in the sintering precursor powder, and main raw material is alumina powder jointed, four component assistant shared weight ratio in integral body is 95-99%, and all the other 1-5wt% are wedding agent.
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| CN200910132061A CN101767981A (en) | 2009-04-10 | 2009-04-10 | Alumina ceramics composite containing novel four-component sintering adjuvant |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030515A (en) * | 2010-10-15 | 2011-04-27 | 广东工业大学 | Low-temperature synthetized aluminum oxide-based ceramic heat dissipation substrate material and preparation method thereof |
| CN102701714A (en) * | 2012-06-27 | 2012-10-03 | 桂林理工大学 | Method for preparing aluminum oxide ceramic with cerium oxide |
| CN102701713A (en) * | 2012-06-27 | 2012-10-03 | 桂林理工大学 | Method for preparing wear-resisting alumina ceramics |
| CN102745978A (en) * | 2012-07-26 | 2012-10-24 | 桂林理工大学 | Method for preparing wear-resistant aluminum oxide ceramic |
| CN105732010A (en) * | 2016-01-14 | 2016-07-06 | 洛阳三睿宝纳米科技有限公司 | High-flexibility 95 ceramic and preparation method thereof |
| CN116265412A (en) * | 2021-12-17 | 2023-06-20 | 辽宁省轻工科学研究院有限公司 | Preparation method of alumina powder for ceramic tube shell |
-
2009
- 2009-04-10 CN CN200910132061A patent/CN101767981A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 陈树江 等: "《相图分析及应用》", 31 August 2007, 冶金工业出版社 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030515A (en) * | 2010-10-15 | 2011-04-27 | 广东工业大学 | Low-temperature synthetized aluminum oxide-based ceramic heat dissipation substrate material and preparation method thereof |
| CN102701714A (en) * | 2012-06-27 | 2012-10-03 | 桂林理工大学 | Method for preparing aluminum oxide ceramic with cerium oxide |
| CN102701713A (en) * | 2012-06-27 | 2012-10-03 | 桂林理工大学 | Method for preparing wear-resisting alumina ceramics |
| CN102745978A (en) * | 2012-07-26 | 2012-10-24 | 桂林理工大学 | Method for preparing wear-resistant aluminum oxide ceramic |
| CN105732010A (en) * | 2016-01-14 | 2016-07-06 | 洛阳三睿宝纳米科技有限公司 | High-flexibility 95 ceramic and preparation method thereof |
| CN116265412A (en) * | 2021-12-17 | 2023-06-20 | 辽宁省轻工科学研究院有限公司 | Preparation method of alumina powder for ceramic tube shell |
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Application publication date: 20100707 |