CN101033139A - Technique for preparing transparent aluminum oxynitride ceramic - Google Patents
Technique for preparing transparent aluminum oxynitride ceramic Download PDFInfo
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- CN101033139A CN101033139A CN 200710013606 CN200710013606A CN101033139A CN 101033139 A CN101033139 A CN 101033139A CN 200710013606 CN200710013606 CN 200710013606 CN 200710013606 A CN200710013606 A CN 200710013606A CN 101033139 A CN101033139 A CN 101033139A
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- aluminum oxynitride
- transparent aluminum
- oxynitride ceramic
- sintering
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Abstract
This invention relates to a preparation method for transparent nitrogen alumina ceramics including mixing raw materials, molding blanks and sintering characterizing in mixing Al2O3 in the weight ratio of 80-95% and AlN of 5-20%, adding sintering aids in 0.1-9% of the mixture weight to be ball-milled and dried then pressed and molded, then to get the blank in equal static pressure, then biscuit firing the blank by rising the temperature to 800-1200deg.C for 0.5-3h, then lowering the temperature and firing the second time by sintering at normal pressure under N atmosphere and rises the temperature to 1800-1900deg.C for 0.5-8h to get a transparent nitrogen alumina ceramic material.
Description
Affiliated technical field
The invention provides a kind of preparation technology of transparent aluminum oxynitride ceramic, belong to field of ceramic material preparation.
Background technology
The AlON pottery has good optics, physics, machinery and chemical property, the particularly isotropy that it had, and high temperature sintering can be made into crystalline ceramics, thereby is the preferred material of high temperature resistant infrared window and cover, but domestic research is less.In the paper of " research of the synthetic AlON pottery of hot pressing " that " silicate journal " in January calendar year 2001 delivered, adopt AI as Wang Xidong
2O
3, AIN and AI powder be raw material, at 1800 ℃, 25MPa, N
2Hot pressed sintering 3h has synthesized the high-purity gamma-ALON pottery in the atmosphere.The volume density of obtained AlON sample is 3.63g/cm
3, be about 97.8% of its theoretical value.Its shortcoming is that density is not high, adopts hot-pressing sintering technique, and equipment requirements is higher, and does not reach the crystalline ceramics theoretical density, and crystalline ceramics theoretical density value is more than 99% of ceramic volumetric density theoretical value.For another example: U.S Pat.6995798, Pittsburgh, PA is with AI
2O
3With AI be that raw material prepares the aluminum oxynitride powder under 2000 ℃ of ammonia atmospheres; U.S Pat.7,045,091, Jopa, MD, Northaest, MD adopt overheated sintering process, with high-purity AI
2O
3With AIN be raw material under nitrogen atmosphere, 2050 ℃ of sintering 3 hours are cooled to 2000 ℃ of insulations transmitance transparent aluminum oxynitride ceramic more than 35% behind the preparation 1.25mm more than 16 hours then.The shortcoming of above-mentioned two patented technologies is sintering temperature height, and soaking time is normal, has increased equipment requirements, has strengthened cost.
Summary of the invention
The purpose of this invention is to provide a kind of preparation technology that can overcome above-mentioned defective, technology is simple, firing temperature is low, material property is good transparent aluminum oxynitride ceramic, its technical scheme is:
Comprise proportion of raw materials, blank forming and sintering process, it is characterized in that: be 80～95% AI with weight ratio
2O
3Mix with 5～20% AIN, add sintering aid, ball milling after drying by 0.1～9% of its mixture weight in addition, earlier dry-pressing formed then, in waiting static pressure, be pressed into the acquisition base substrate again, when burning till, first biscuiting, be that vacuum is warmed up to 800～1200 ℃ of insulations 0.5～3 hour, cooling then, twice firing is promptly normal pressure-sintered under nitrogen atmosphere again, be warmed up to 1800～1900 ℃ of insulations 0.5～8 hour, obtain transparent aluminum oxynitride ceramic material.
The preparation method of described transparent aluminum oxynitride ceramic, raw material granularity is AI
2O
30.01～50 μ m, AIN0.01～50 μ m.
The preparation method of described transparent aluminum oxynitride ceramic, sintering aid is by Al powder, Y
2O
3And CaF
2Form, each add-on of forming is AI
2O
3With 0.05～3% of AIN mixture weight.
The preparation method of described transparent aluminum oxynitride ceramic, sintering aid is by Y
2O
3And CaF
2Form, each add-on of forming is AI
2O
3With 0.05～3% of AIN mixture weight.
The preparation method of described transparent aluminum oxynitride ceramic, dry-pressing formed pressure is 20～50MPa.
The preparation method of described transparent aluminum oxynitride ceramic, isostatic pressing pressure is 100～300MPa.
The preparation method of described transparent aluminum oxynitride ceramic, vacuum sintering, atmosphere sintering heat-up rate are 5～15 ℃/min.
The present invention compared with prior art has the following advantages:
1, the present invention adopts normal pressure-sintered forming under the nitrogen atmosphere, has reduced the appointed condition that burns till aluminum oxynitride ceramic, and the adding of sintering aid greatly reduces temperature of reaction and soaking time, and is more simple and easy to do than hot pressing sintering;
2, sintering temperature is below 1900 ℃, with existing more than 2000 ℃ sintering temperature compare, reduce sintering temperature and cost of manufacture greatly, help the utilization and extention of aluminum oxynitride ceramic;
3, the present invention adopts double-firing process, has reduced the distortion of aluminum oxynitride ceramic;
4, the transparent material of Huo Deing in the ultraviolet region (200～470nm) transmitance more than 90%, (800～6000nm) transmitance reaches more than 50% in the near-infrared region, relative density reaches more than 99% of theoretical density, excellent property can be used as high temperature resistant infrared window and cover material.
Embodiment
Embodiment 1
1, batching: the AI that selects 95 grams, 0.01 μ m for use
2O
3Mix with the AIN of 5 grams, 0.01 μ m and the sintering aid of 0.1 gram, ball milling is 8 hours in dehydrated alcohol, wherein the Y that consists of 1 μ m of sintering aid
2O
30.05 the CaF of gram and 1 μ m
20.05 gram;
2, blank forming: with the batching drying of ball milling, first then 20MPa is dry-pressing formed, depresses to base substrate at static pressure such as 200MPa again;
3, sintering process: base substrate is carried out sintering in the chemical vapor infiltration poke, elder generation's biscuiting, temperature rise rate with 6 ℃/min rises to 800 ℃ of insulations 0.5 hour under vacuum state, cool to room temperature, twice firing again, under nitrogen atmosphere, rise to 1850 ℃ of insulations under the atmospheric pressure state after 1 hour with the temperature rise rate of 6 ℃/min, promptly obtain transparent aluminum oxynitride ceramic.
Sample through twin polishing record in the ultraviolet region to 1mm is thick (200～470nm) transmitance more than 95%, (800～6000nm) transmitance reaches more than 50% in the near-infrared region.
Embodiment 2
1, batching: the AI that selects 90 grams, 5 μ m for use
2O
3Mix with the AIN of 10 grams, 5 μ m and the sintering aid of 2 grams, ball milling is 24 hours in dehydrated alcohol, wherein the Y that consists of 1 μ m of sintering aid
2O
3The CaF of 1 gram, 1 μ m
21 gram;
2, blank forming: with the batching drying of ball milling, first then 30MPa is dry-pressing formed, depresses to base substrate at static pressure such as 250MPa again;
3, sintering process: base substrate is carried out sintering in the chemical vapor infiltration poke, elder generation's biscuiting, temperature rise rate with 10 ℃/min rises to 800 ℃ of insulations 0.5 hour under vacuum state, cool to room temperature, twice firing again, under nitrogen atmosphere, rise to 1850 ℃ of insulations under the atmospheric pressure state after 1 hour with the temperature rise rate of 10 ℃/min, obtain transparent aluminum oxynitride ceramic.
Sample through twin polishing record in the ultraviolet region to 1mm is thick (200～470nm) transmitance more than 95%, (800～6000nm) transmitance reaches more than 50% in the near-infrared region.
Embodiment 3
1, batching: the AI that selects 80 grams, 50 μ m for use
2O
3Mix with the AIN of 20 grams, 50 μ m and the sintering aid of 9 grams, ball milling is 48 hours in dehydrated alcohol, wherein the Al powder that consists of 1 μ m 3 grams of sintering aid, the Y of 1 μ m
2O
3The CaF of 3 grams, 1 μ m
23 grams;
2, blank forming: with the batching drying of ball milling, first then 50MPa is dry-pressing formed, depresses to base substrate at static pressure such as 250MPa again;
3, sintering process: base substrate is carried out sintering in the chemical vapor infiltration poke, elder generation's biscuiting, temperature rise rate with 15 ℃/min rises to 800 ℃ of insulations 0.5 hour under vacuum state, cool to room temperature, twice firing again, under nitrogen atmosphere, rise to 1900 ℃ of insulations under the atmospheric pressure state after 0.5 hour with the temperature rise rate of 15 ℃/min, obtain transparent aluminum oxynitride ceramic.
Sample through twin polishing record in the ultraviolet region to 1mm is thick (200～470nm) transmitance more than 95%, (800～6000nm) transmitance reaches more than 50% in the near-infrared region.
Claims (7)
1, a kind of preparation technology of transparent aluminum oxynitride ceramic comprises proportion of raw materials, blank forming and sintering process, it is characterized in that: be 80～95% Al with weight ratio
2O
3Mix with 5～20% AlN, add sintering aid, ball milling after drying by 0.1～9% of its mixture weight in addition, earlier dry-pressing formed then, in waiting static pressure, be pressed into the acquisition base substrate again, when burning till, first biscuiting, be that vacuum is warmed up to 800～1200 ℃ of insulations 0.5～3 hour, cooling then, twice firing is promptly normal pressure-sintered under nitrogen atmosphere again, be warmed up to 1800～1900 ℃ of insulations 0.5～8 hour, obtain transparent aluminum oxynitride ceramic material.
2, the preparation technology of transparent aluminum oxynitride ceramic as claimed in claim 1 is characterized in that: raw material granularity is Al
2O
30.01～50 μ m, AlN 0.01～50 μ m.
3, the preparation technology of transparent aluminum oxynitride ceramic as claimed in claim 1 is characterized in that: sintering aid is by Al powder, Y
2O
3And CaF
2Form, each add-on of forming is Al
2O
3With 0.05～3% of AlN mixture weight.
4, the preparation technology of transparent aluminum oxynitride ceramic as claimed in claim 1, it is characterized in that: sintering aid is by Y
2O
3And CaF
2Form, each add-on of forming is Al
2O
3With 0.05～3% of AlN mixture weight.
5, the preparation technology of transparent aluminum oxynitride ceramic as claimed in claim 1 is characterized in that: dry-pressing formed pressure is 20～50MPa.
6, the preparation technology of transparent aluminum oxynitride ceramic as claimed in claim 1 is characterized in that: isostatic pressing pressure is 100～300MPa.
7, the preparation technology of transparent aluminum oxynitride ceramic as claimed in claim 1 is characterized in that: vacuum sintering, atmosphere sintering heat-up rate are 5～15 ℃/min.
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|---|---|---|---|
| CN 200710013606 CN101033139A (en) | 2007-02-07 | 2007-02-07 | Technique for preparing transparent aluminum oxynitride ceramic |
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|---|---|---|---|
| CN 200710013606 CN101033139A (en) | 2007-02-07 | 2007-02-07 | Technique for preparing transparent aluminum oxynitride ceramic |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103492347A (en) * | 2011-02-28 | 2014-01-01 | 岭南大学校产学协力团 | Method for preparing polycrystalline aluminum oxynitride having enhanced transparency |
| US9287106B1 (en) | 2014-11-10 | 2016-03-15 | Corning Incorporated | Translucent alumina filaments and tape cast methods for making |
| CN107344854A (en) * | 2016-05-06 | 2017-11-14 | 中国科学院上海光学精密机械研究所 | A kind of method for preparing aluminum oxynitride crystalline ceramics |
| CN109109142A (en) * | 2018-09-04 | 2019-01-01 | 北京中材人工晶体研究院有限公司 | A kind of hot pressed sintering AlON crystalline ceramics graphite jig |
| CN110072826A (en) * | 2016-12-21 | 2019-07-30 | 日本碍子株式会社 | Transparent AlN sintered body and its preparation method |
| CN112299861A (en) * | 2020-11-18 | 2021-02-02 | 四川大学 | AlON transparent ceramic pseudo-sintering agent and application thereof, and preparation method of transparent ceramic |
| CN114133252A (en) * | 2021-12-21 | 2022-03-04 | 厦门钜瓷科技有限公司 | AlON transparent ceramic shape-preserving infrared hood and preparation method thereof |
| CN115028458A (en) * | 2022-07-29 | 2022-09-09 | 鲁米星特种玻璃科技股份有限公司 | Preparation technology of aluminum oxynitride transparent ceramic |
-
2007
- 2007-02-07 CN CN 200710013606 patent/CN101033139A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103492347A (en) * | 2011-02-28 | 2014-01-01 | 岭南大学校产学协力团 | Method for preparing polycrystalline aluminum oxynitride having enhanced transparency |
| JP2014508092A (en) * | 2011-02-28 | 2014-04-03 | インダストリー−アカデミック コーペレーション ファンデーション ヨンナム ユニバーシティー | Method for producing polycrystalline aluminum oxynitride with improved transparency |
| CN103492347B (en) * | 2011-02-28 | 2015-10-14 | 岭南大学校产学协力团 | Preparation has the method for the polycrystalline aluminum oxynitride strengthening transparency |
| US9287106B1 (en) | 2014-11-10 | 2016-03-15 | Corning Incorporated | Translucent alumina filaments and tape cast methods for making |
| CN107344854A (en) * | 2016-05-06 | 2017-11-14 | 中国科学院上海光学精密机械研究所 | A kind of method for preparing aluminum oxynitride crystalline ceramics |
| CN110072826A (en) * | 2016-12-21 | 2019-07-30 | 日本碍子株式会社 | Transparent AlN sintered body and its preparation method |
| CN110072826B (en) * | 2016-12-21 | 2022-03-01 | 日本碍子株式会社 | Transparent AlN sintered body and process for producing the same |
| CN109109142A (en) * | 2018-09-04 | 2019-01-01 | 北京中材人工晶体研究院有限公司 | A kind of hot pressed sintering AlON crystalline ceramics graphite jig |
| CN112299861A (en) * | 2020-11-18 | 2021-02-02 | 四川大学 | AlON transparent ceramic pseudo-sintering agent and application thereof, and preparation method of transparent ceramic |
| CN114133252A (en) * | 2021-12-21 | 2022-03-04 | 厦门钜瓷科技有限公司 | AlON transparent ceramic shape-preserving infrared hood and preparation method thereof |
| CN115028458A (en) * | 2022-07-29 | 2022-09-09 | 鲁米星特种玻璃科技股份有限公司 | Preparation technology of aluminum oxynitride transparent ceramic |
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