CN1709823A - Method for preparing transparent MgAlON ceramic and transparent MgAlON ceramic - Google Patents
Method for preparing transparent MgAlON ceramic and transparent MgAlON ceramic Download PDFInfo
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- CN1709823A CN1709823A CN 200510035301 CN200510035301A CN1709823A CN 1709823 A CN1709823 A CN 1709823A CN 200510035301 CN200510035301 CN 200510035301 CN 200510035301 A CN200510035301 A CN 200510035301A CN 1709823 A CN1709823 A CN 1709823A
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Abstract
The invention relates to the producing method of transparent MgAlON ceramics and the transparent MgAlON ceramics. It makes highly pure magnesiumic compounds, aluminiferous compounds and AlN as raw material, adopts electric discharge plasma sintering technology, through reacting and sintering, directly produce transparent MgAlON ceramics of certain components and specifications. The method has simple craft and is of high efficiency. The weight percentage of nitrogen element of the prepared transparent MgAlON ceramics is 0.5% - 5%, the permeation rate of visible light wave band is 60% - 80%, and the permeation rate at 3.0 - 5.0 mu m infrared wave band is 60% - 85%. It can be widely applied in various high temperature window and various wave permeation assemblies in such fields as national defense science and technology.
Description
Technical field
The invention belongs to the inorganic non-metallic ceramic field, specifically is a kind of method and transparent MgAlON pottery for preparing transparent MgAlON pottery with discharge plasma sintering.
Background technology
Transparent MgAlON pottery is a kind of novel optical ceramics material, has excellent optics, dielectric, physical and mechanical property, and its optical property is than sapphire crystal, silica glass, hot pressing MgF
2More excellent Deng optical material, have good transmitance at ultraviolet, visible light, infrared band.Can be widely used in and make in guided missile head-shield, transparent armor, various high-temperature high-pressure apparatus viewing window, infrared band window material and guidance and the photoelectronic warfare device.But the main problem that transparent MgAlON pottery faces is to be difficult to make.The method that the transparent MgAlON pottery of domestic and international at present preparation is adopted all is a two-step approach: promptly adopt the synthetic high-purity MgAlON powder of solid state reaction sintering or carbothermal reduction-nitridation method earlier, utilizing hot pressed sintering or HIP sintering at high temperature to prepare transparent MgAlON pottery then.The disadvantage of this method is that difficulty is big, and complex process, production process are difficult to control, and the production cycle is long, the production cost height.Because from thermodynamics, the oxygen nitrogen partial pressure scope that MgAlON can stable existence is very little, so composition that must strict controlled atmosphere in the building-up process, and the dividing potential drop of oxygen generally will be controlled at 10
-19About MPa, just might obtain high-purity or single-phase MgAlON powder, reaction sintering and carbothermal reduction-nitridation method all need high temperature and the long reaction times more than 1650 ℃ in addition, are generally more than the several hrs.In the process of this external synthetic MgAlON powder, also follow the generation of these various side reactions, this point is particularly remarkable in the carbothermic reduction process.So strict atmosphere control, so high synthesis temperature, so long reaction times give present MgAlON powder anamorphic zone great difficulty and high production cost.Even synthesize high-purity or monophasic MgAlON ceramic powder; it is also quite difficult to prepare transparent MgAlON pottery; because the coking property of MgAlON powder is very poor, need to carry out under high temperature (more than 1800 ℃), high pressure (nitrogen pressure is about 150MPa) and strict atmosphere (high pure nitrogen) protection.Therefore present this elder generation synthesizes the MgAlON powder, and the method for preparing transparent MgAlON pottery in pressure sintering has very big difficulty.
Summary of the invention
The objective of the invention is to solve the problem that present transparent MgAlON pottery is difficult to prepare, the method for a kind of simple possible, the transparent MgAlON pottery of preparation rapidly and efficiently and the transparent MgAlON pottery that makes in this way are provided.
The method that the present invention prepares transparent MgAlON pottery adopts following steps:
A, get high-purity magnesium-containing compound, high-purity aluminum contained compound and AlN preparation high pure raw material, wherein the quality percentage composition of each component is respectively, high-purity magnesium-containing compound 0.5～25%, high-purity aluminum contained compound 60～90%, high-purity AlN 0.5～15%;
B, described high pure raw material being put into ball grinder, is that medium ground 12～36 hours altogether with ethanol, after the drying mixed powder;
C, described mixed powder is placed graphite jig, put into the discharge plasma sintering stove then, apply 10～100MPa pressure, carry out sintering, temperature rise rate is 50～400 ℃/min, and sintering temperature is 1500～1800 ℃, cool to room temperature after the insulation with the furnace, promptly get transparent MgAlON pottery.
Adopt aforesaid method can make transparent MgAlON pottery, the quality percentage composition of each component is in this transparent MgAlON pottery: MgO 0.5～25%, Al
2O
360～85%, AlN 0.5～15%.The optical property of this transparent MgAlON pottery is: 0.3～0.5 μ m visible light wave range transmitance is that 60～80%, 3.0～5.0 μ m infrared band transmitances are 60～85%.
The inventive method can make another kind of transparent MgAlON pottery, and this transparent MgAlON pottery is made of Mg, Al, O and four kinds of elements of N, and wherein the quality percentage composition of N element is 0.5～5%.The optical property of this transparent MgAlON pottery is: 0.3～0.5 μ m visible light wave range transmitance is that 60～80%, 3.0～5.0 μ m infrared band transmitances are 60～85%.
Discharge plasma sintering technique is a kind of brand-new sintering process, and its outstanding feature is that temperature rise rate is fast, sintering temperature is low, sintering time is short.Its ultimate principle is with the be sintered body of pulse high current by pressurization, make to be sintered the discharge excitation plasma takes place between the body internal particle, thereby make each uniform particles ground self-heating and surface active, mass transfer and heat transfer process are instantaneous to be finished, and makes to be sintered the body densification in the extremely short time.Because the formation of MgAlON is actually MgO, Al
2O
3And the solid solution process between the AlN.Because discharge plasma sintering can be removed the inert coating of powder particle surface, make the particle surface activation, thereby can finish the solid solution process in a short period of time, form monophasic MgAlON pottery.Since discharge plasma sintering be under the high vacuum condition, carry out and the reaction times very short, generally as long as several minutes, therefore can be avoided the atmosphere control strict in the conventional sintering process and the disadvantageous effect of various side reactions effectively to dozens of minutes.Form in the process of MgAlON again densification fully and obtain transparent MgAlON pottery at reaction sintering, this just is combined as a whole the synthetic and densification of MgAlON pottery, thereby avoided the traditional method high-purity MgAlON powder of preparation earlier, and then hot pressed sintering prepares a series of difficult problems that crystalline ceramics brings.
The invention has the advantages that: it is a raw material with high-purity magnesium-containing compound, aluminum contained compound and AlN, adopt discharge plasma sintering technique, by rational sintering process, directly prepare the transparent MgAlON pottery of definite composition and specification through reaction sintering, solve traditional technology and prepared transparent MgAlON ceramic process complexity, the difficult problem that the production cycle is long, production cost is high.Present method technology is simple, efficient, can a step prepare transparent MgAlON pottery.The quality percentage composition of prepared transparent MgAlON pottery N element is 0.5～5%, visible light wave range transmitance 60～80%, in 3.0～5.0 μ m infrared band transmitances is 60～85%, can be widely used in the various parts for wave in the fields such as various high temperature windows and science and techniques of defence.
Embodiment
The present invention is further described below in conjunction with embodiment.
This method for preparing transparent MgAlON pottery is a raw material with high-purity magnesium-containing compound, aluminum contained compound and AlN, adopt discharge plasma sintering technique, by rational sintering process, directly prepare the transparent MgAlON pottery of definite composition and specification through reaction sintering.Concrete grammar is: a, get high-purity magnesium-containing compound, high-purity aluminum contained compound and AlN preparation high pure raw material, wherein the quality percentage composition of each component is respectively, high-purity magnesium-containing compound 5～25%, high-purity aluminum contained compound 60～90%, high-purity AlN 0.5～15%; B, described high pure raw material being put into ball grinder, is that medium ground 12～36 hours altogether with ethanol, after the drying mixed powder; C, described mixed powder is placed graphite jig, put into the discharge plasma sintering stove then, apply the axle pressure of 10～100Mpa, apply the pulsed current of 800～3500A, make the interior temperature of stove rise to 1500～1800 ℃, carry out sintering with the temperature rise rate of 50～400 ℃/min, behind insulation 0～2h, furnace temperature is dropped to below 600 ℃ fast, cool to room temperature then with the furnace, promptly make transparent MgAlON pottery.
Wherein, high-purity magnesium-containing compound can adopt purity to be not less than 99.9% MgO or Mg (OH)
2Or MgCO
3, high-purity aluminum contained compound can adopt purity to be not less than 99.9% Al
2O
3, or Al (OH)
2
The abrading-ball that uses in the ball grinder can adopt high-purity corundum abrading-ball or high-purity Al
2O
3Abrading-ball etc.
Can make the quality percentage composition according to the method described above is MgO 0.5～25%, Al
2O
360～85%, the transparent MgAlON pottery of AlN 0.5～15%.The optical property of this transparent MgAlON pottery is: 0.3～0.5 μ m visible light wave range transmitance is that 60～80%, 3.0～5.0 μ m infrared band transmitances are 60～85%.
The quality percentage composition that also can make the N element according to the method described above is 0.5～5% transparent MgAlON pottery.The optical property of this transparent MgAlON pottery is: 0.3～0.5 μ m visible light wave range transmitance is that 60～80%, 3.0～5.0 μ m infrared band transmitances are 60～85%.
Above-mentioned transparent MgAlON pottery is a sheet structure, and thickness is 0.5～10mm, and cross-sectional area is 100mm
2
Be two specific embodiments below.
Embodiment 1:
With purity 99.99% MgO, Al
2O
3With the AlN powder be MgO10%, Al by the quality percentage composition
2O
380%, the ratio of AlN 10% batching, putting into ball grinder then is to make mixed powder after medium grinds 12h and drying altogether with the dehydrated alcohol.Mixed powder is packed in the graphite jig of discharge plasma sintering stove.With the temperature rise rate of 200 ℃/min temperature is risen to 1750 ℃ and be incubated 60min.Applied pressure is 40MPa in intensification and the insulating process.Insulation is reduced to furnace temperature below 600 ℃ in 6min after finishing.Sample is taken out in the cooling back fully, promptly obtains transparent MgAlON pottery.
Embodiment 2:
With purity 99.99% Mg (OH)
2, Al (OH)
3And the AlN powder is MgO 20%, Al by the quality percentage composition
2O
370%, the ratio of AlN 10% batching, putting into ball grinder then is to make mixed powder after medium grinds 12h and drying altogether with the dehydrated alcohol.Mixed powder is packed in the graphite jig of discharge plasma sintering stove.With the temperature rise rate of 200 ℃/min temperature is risen to 1000 ℃ and be incubated 20min, after insulation finishes temperature risen to 1800 ℃ and be incubated 60min.Applied pressure is 40MPa in intensification and the insulating process.Insulation is reduced to furnace temperature below 600 ℃ in 6min after finishing.Sample is taken out in the cooling back fully, promptly obtains transparent MgAlON pottery.
Embodiment 3:
With purity 99.99% Mg (OH)
2, Al (OH)
3And the AlN powder is MgO 20%, Al by the quality percentage composition
2O
365%, the ratio of AlN 15% batching, putting into ball grinder then is to make mixed powder after medium grinds 24h and drying altogether with the dehydrated alcohol.With the mixed powder sintering in the graphite jig of discharge plasma sintering stove of packing into, adopt embodiment 2 described processing condition, can make transparent MgAlON pottery.
Claims (9)
1, a kind of method for preparing transparent MgAlON pottery is characterized in that may further comprise the steps:
A, get high-purity magnesium-containing compound, high-purity aluminum contained compound and high-purity AlN preparation high pure raw material, wherein the quality percentage composition of each component is respectively, high-purity magnesium-containing compound 0.5～25%, high-purity aluminum contained compound 60～90%, high-purity AlN 0.5～15%;
B, described high pure raw material being put into ball grinder, is that medium ground 12～36 hours altogether with ethanol, after the drying mixed powder;
C, described mixed powder is placed graphite jig, put into the discharge plasma sintering stove then, apply 10～100MPa pressure, carry out sintering, temperature rise rate is 50～400 ℃/min, and sintering temperature is 1500～1800 ℃, cool to room temperature after the insulation with the furnace, promptly get transparent MgAlON pottery.
2, according to the method for the transparent MgAlON pottery of the described preparation of claim 1, it is characterized in that: among the step c, the soaking time during discharge plasma sintering is 0～2 hour, and insulation drops to furnace temperature below 600 ℃ after finishing fast, cools to room temperature then with the furnace.
3, according to the method for the transparent MgAlON pottery of the described preparation of claim 1, it is characterized in that: described high-purity magnesium-containing compound is that purity is not less than 99.9% MgO or Mg (OH)
2, or MgCO
3, high-purity aluminum contained compound is that purity is not less than 99.9% Al
2O
3, or Al (OH)
2, the purity of high-purity AlN raw material is not less than 99.9%.
4, according to the method for the transparent MgAlON pottery of the described preparation of claim 1, it is characterized in that: the pulsed current during sintering is 800～3500A.
5, according to the method for the transparent MgAlON pottery of the described preparation of claim 1, the optical property that it is characterized in that the transparent MgAlON pottery of prepared sheet is: 0.3～0.5 μ m visible light wave range transmitance is that 60～80%, 3.0～5.0 μ m infrared band transmitances are 60～85%.
6, according to the transparent MgAlON pottery of claim 1 method preparation, it is characterized in that: the quality percentage composition of each component is in this transparent MgAlON pottery:
MgO?0.5～25％，Al
2O
3?60～85％，AlN?0.5～15％。
7, according to the transparent MgAlON pottery of claim 1 method preparation, it is characterized in that: this transparent MgAlON pottery is made of Mg, Al, O and four kinds of elements of N, and wherein the quality percentage composition of N element is 0.5～5%.
8, according to claim 6 or 7 described transparent MgAlON potteries, it is characterized in that the optical property of this transparent MgAlON pottery is: 0.3～0.5 μ m visible light wave range transmitance is that 60～80%, 3.0～5.0 μ m infrared band transmitances are 60～85%.
9, according to claim 6 or 7 described transparent MgAlON potteries, it is characterized in that: described transparent MgAlON pottery is sheet structure, and thickness is 0.5～10mm, and cross-sectional area is 100mm
2
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817683A (en) * | 2010-03-30 | 2010-09-01 | 武汉理工大学 | Method for preparing MgAlON transparent ceramic in pressureless sintering way |
| CN106242577A (en) * | 2016-08-08 | 2016-12-21 | 屠秀芬 | The nano oxidized terbium of a kind of MgALON is combined the preparation method of magneto-optic crystalline ceramics |
| TWI579255B (en) * | 2010-10-25 | 2017-04-21 | Ngk Insulators Ltd | A ceramic material, a laminated body, a member for a semiconductor manufacturing apparatus, and a sputtering ring target member |
| WO2017120990A1 (en) * | 2016-01-13 | 2017-07-20 | 广东工业大学 | Process for preparing net-size, complex-shape transparent ceramic piece |
| CN108585878A (en) * | 2018-04-24 | 2018-09-28 | 武汉理工大学 | A kind of high rigidity MgAlON crystalline ceramics and preparation method thereof |
| CN116003156A (en) * | 2022-11-24 | 2023-04-25 | 浙江锦诚新材料股份有限公司 | MgAlON ceramic filter with multiple pore structures for magnesium alloy and preparation method thereof |
-
2005
- 2005-06-21 CN CN 200510035301 patent/CN1709823A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817683A (en) * | 2010-03-30 | 2010-09-01 | 武汉理工大学 | Method for preparing MgAlON transparent ceramic in pressureless sintering way |
| CN101817683B (en) * | 2010-03-30 | 2014-12-03 | 武汉理工大学 | Method for preparing MgAlON transparent ceramic in pressureless sintering way |
| TWI579255B (en) * | 2010-10-25 | 2017-04-21 | Ngk Insulators Ltd | A ceramic material, a laminated body, a member for a semiconductor manufacturing apparatus, and a sputtering ring target member |
| WO2017120990A1 (en) * | 2016-01-13 | 2017-07-20 | 广东工业大学 | Process for preparing net-size, complex-shape transparent ceramic piece |
| CN106242577A (en) * | 2016-08-08 | 2016-12-21 | 屠秀芬 | The nano oxidized terbium of a kind of MgALON is combined the preparation method of magneto-optic crystalline ceramics |
| CN108585878A (en) * | 2018-04-24 | 2018-09-28 | 武汉理工大学 | A kind of high rigidity MgAlON crystalline ceramics and preparation method thereof |
| CN108585878B (en) * | 2018-04-24 | 2021-01-19 | 武汉理工大学 | High-hardness MgAlON transparent ceramic and preparation method thereof |
| CN116003156A (en) * | 2022-11-24 | 2023-04-25 | 浙江锦诚新材料股份有限公司 | MgAlON ceramic filter with multiple pore structures for magnesium alloy and preparation method thereof |
| CN116003156B (en) * | 2022-11-24 | 2023-11-28 | 浙江锦诚新材料股份有限公司 | MgAlON ceramic filter with multiple pore structures for magnesium alloy and preparation method thereof |
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