CN100506750C - Process for preparing transparent aluminum oxynitride ceramic - Google Patents
Process for preparing transparent aluminum oxynitride ceramic Download PDFInfo
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- CN100506750C CN100506750C CNB2007100136073A CN200710013607A CN100506750C CN 100506750 C CN100506750 C CN 100506750C CN B2007100136073 A CNB2007100136073 A CN B2007100136073A CN 200710013607 A CN200710013607 A CN 200710013607A CN 100506750 C CN100506750 C CN 100506750C
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- aluminum oxynitride
- transparent aluminum
- preparation
- oxynitride ceramic
- sintering
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Abstract
This invention relates to preparation method for transparent nitrogen alumina including mixing the raw materials, molding the blank and sintering characterizing in mixing Al2O3 with AlN in the weight ratios of 85-95% and 5-20% and adding sinter aids in 0.1-9% weight of the mixture to be ball-milled and dried then pressed and molded then to be pressed to get the blank by equal static pressure, when the blank is finished, the temperature is risen to 800-1200deg.C in vacuum for 0.5-3h then penetrating nitrogen to normal pressure and rising the temperature to 1750-1900deg.C for 0.5-8h to get a transparent nitrogen alumina ceramic material.
Description
Technical field
The invention provides a kind of preparation method 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 Al as Wang Xidong
2O
3, AlN and Al 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 Al
2O
3With Al 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 Al
2O
3With AlN 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 method 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% Al with weight ratio
2O
3Mix with 5～20% AlN, add sintering aid by 0.1～9% of its mixture weight in addition, sintering aid is by Al powder, Y
2O
3Form with MgO, perhaps by Y
2O
3Form with MgO, each add-on of forming is Al
2O
3With 0.05～3% of AlN mixture weight, the ball milling after drying, earlier dry-pressing formed then, in waiting static pressure, be pressed into the acquisition base substrate again, elder generation's vacuum was warmed up to 800～1200 ℃ of insulations 0.5～3 hour when base substrate burnt till, feed nitrogen then and reach normal pressure, be warmed up to 1750～1900 ℃ of insulations 0.5～8 hour again, promptly obtain transparent aluminum oxynitride ceramic material.
The preparation method of described transparent aluminum oxynitride ceramic, raw material granularity is Al
2O
30.01～50 μ m, AlN 0.01～50 μ m.
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 and has burnt till the aluminum oxynitride ceramic appointed condition, 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 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 Al that selects 95 grams, 0.01 μ m for use
2O
3Mix with the AlN 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 MgO 0.05 gram of gram and 1 μ m;
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, temperature rise rate with 5 ℃/min rises to 1000 ℃ of insulations 0.5 hour under vacuum state earlier, feed nitrogen then, temperature rise rate with 5 ℃/min is rising to 1800 ℃ of insulations after 1 hour, the acquisition transparent aluminum oxynitride ceramic under the nitrogen atmospheric pressure state again.
Sample through twin polishing to 1mm thick record in the ultraviolet region (200～470nm) transmitance more than 95%, (800～6000nm) transmitance reaches more than 50% in the near-infrared region.
Embodiment 2
1, batching: the Al that selects 90 grams, 5 μ m for use
2O
3Mix with the AlN 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
3MgO 1 gram of 1 gram, 1 μ m;
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, temperature rise rate with 10 ℃/min rises to 800 ℃ of insulations 1 hour under vacuum state earlier, feed nitrogen then, temperature rise rate with 15 ℃/min is rising to 1850 ℃ of insulations after 1 hour, the acquisition transparent aluminum oxynitride ceramic under the nitrogen atmospheric pressure state again.
Sample through twin polishing to 1mm thick record in the ultraviolet region (200～470nm) transmitance more than 95%, (800～6000nm) transmitance reaches more than 50% in the near-infrared region.
Embodiment 3
1, batching: the Al that selects 80 grams, 50 μ m for use
2O
3Mix with the AlN 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
3MgO 3 grams of 3 grams, 1 μ m;
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, temperature rise rate with 10 ℃/min rises to 800 ℃ of insulations 1 hour under vacuum state earlier, feed nitrogen then, temperature rise rate with 10 ℃/min is rising to 1900 ℃ of insulations after 0.5 hour, the acquisition transparent aluminum oxynitride ceramic under the nitrogen atmospheric pressure state again.
Sample through twin polishing to 1mm thick record in the ultraviolet region (200～470nm) transmitance more than 95%, (800～6000nm) transmitance reaches more than 50% in the near-infrared region.
Claims (5)
1, a kind of preparation method 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 by 0.1～9% of its mixture weight in addition, sintering aid is by Al powder, Y
2O
3Form with MgO, perhaps by Y
2O
3Form with MgO, each add-on of forming is Al
2O
3With 0.05～3% of AlN mixture weight, the ball milling after drying, earlier dry-pressing formed then, in waiting static pressure, be pressed into the acquisition base substrate again, elder generation's vacuum was warmed up to 800～1200 ℃ of insulations 0.5～3 hour when base substrate burnt till, feed nitrogen then and reach normal pressure, be warmed up to 1750～1900 ℃ of insulations 0.5～8 hour again, promptly obtain transparent aluminum oxynitride ceramic material.
2, the preparation method 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 method of transparent aluminum oxynitride ceramic as claimed in claim 1 is characterized in that: dry-pressing formed pressure is 20～50MPa.
4, the preparation method of transparent aluminum oxynitride ceramic as claimed in claim 1 is characterized in that: isostatic pressing pressure is 100～300MPa.
5, the preparation method 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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|---|---|---|---|
| CNB2007100136073A CN100506750C (en) | 2007-02-07 | 2007-02-07 | Process for preparing transparent aluminum oxynitride ceramic |
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|---|---|---|---|
| CNB2007100136073A CN100506750C (en) | 2007-02-07 | 2007-02-07 | Process for preparing transparent aluminum oxynitride ceramic |
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|---|---|
| CN101033140A CN101033140A (en) | 2007-09-12 |
| CN100506750C true CN100506750C (en) | 2009-07-01 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9287106B1 (en) | 2014-11-10 | 2016-03-15 | Corning Incorporated | Translucent alumina filaments and tape cast methods for making |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102875152B (en) * | 2012-09-13 | 2013-10-23 | 大连海事大学 | Low temperature fast preparation method of AlON crystalline ceramics |
| 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 |
| CN106495668A (en) * | 2016-06-03 | 2017-03-15 | 北京晶朗光电科技有限公司 | A kind of manufacture method of non-conventional type ceramic fluorescent tube |
| CN107459354A (en) * | 2017-09-19 | 2017-12-12 | 南京云启金锐新材料有限公司 | High transmittance High Purity Nitrogen alumina transparent ceramic and preparation method thereof |
| CN112225564B (en) * | 2019-07-15 | 2022-01-04 | 中国科学院上海硅酸盐研究所 | Aluminum oxynitride transparent ceramic and preparation method thereof |
| CN114133252B (en) * | 2021-12-21 | 2023-04-28 | 厦门钜瓷科技有限公司 | AlON transparent ceramic conformal infrared head cover and preparation method thereof |
| CN115028458B (en) * | 2022-07-29 | 2023-05-30 | 鲁米星特种玻璃科技股份有限公司 | Preparation method of aluminum oxynitride transparent ceramic |
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2007
- 2007-02-07 CN CNB2007100136073A patent/CN100506750C/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| 影响尖晶石型AlON陶瓷透明性的因素. 魏春城等.现代技术陶瓷，第2006年第4期. 2006 |
| 影响尖晶石型AlON陶瓷透明性的因素. 魏春城等.现代技术陶瓷，第2006年第4期. 2006 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9287106B1 (en) | 2014-11-10 | 2016-03-15 | Corning Incorporated | Translucent alumina filaments and tape cast methods for making |
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| CN101033140A (en) | 2007-09-12 |
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Assignee: Shandong Boyang New Materials Technology Co., Ltd. Assignor: Shandong University of Technology Contract record no.: 2010370000443 Denomination of invention: Process for preparing transparent aluminum oxynitride ceramic Granted publication date: 20090701 License type: Exclusive License Open date: 20070912 Record date: 20100810 |
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