CN103232237A - Preparation method of normal-pressure-sintered transparent zirconium oxide ceramic material - Google Patents
Preparation method of normal-pressure-sintered transparent zirconium oxide ceramic material Download PDFInfo
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- CN103232237A CN103232237A CN2013101345620A CN201310134562A CN103232237A CN 103232237 A CN103232237 A CN 103232237A CN 2013101345620 A CN2013101345620 A CN 2013101345620A CN 201310134562 A CN201310134562 A CN 201310134562A CN 103232237 A CN103232237 A CN 103232237A
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Abstract
The invention discloses a preparation method of a normal-pressure-sintered transparent zirconium oxide ceramic material. According to the invention, commercial yttrium-stabilized zirconium oxide powder (xmol% Y2O3-ZrO2, ZrYx for short, and x=6-10) and high-purity Y2O3 and Al2O3 nano-powders are mainly adopted as raw materials; and under a relatively low temperature, a normal-pressure sintering process is adopted, such that the transparent yttrium-stabilized zirconium oxide ceramic material is prepared. The transparent yttrium-stabilized zirconium oxide ceramic material provided by the invention has the advantages of simple preparation process, low cost, normal-pressure sintering, easy molding, and good stability. The material can be widely applied in the fields such as infrared window materials, high-temperature window materials, prisms, polycrystalline zirconium oxide jewelries, radar radomes, infrared fairings, and the like.
Description
Technical field
The present invention is a kind of preparation method of normal pressure-sintered transparent zirconium oxide stupalith, belongs to inorganic non-metallic (pottery) material field.
Background technology
Zirconium white (ZrO
2) pottery is novel texture pottery and the multifunctional ceramic that grows up the seventies in 20th century, it has high tenacity, high strength, high rigidity, high refractive index, low thermal expansivity (close to steel), good abrasion resistance, good high temperature resistant, excellent good characteristics such as high-temperature electric heat performance, be widely used in every field, as mould, abrading-ball, dispersion and grinding medium, wear resistant cutters, parting tool, refractory materials, watchcase and watchband, polycrystal zirconia ornaments, biomedical pottery, oxygen sensor, solid fuel cell, high-temperature electric heat material etc.Wherein the transparent zirconium oxide pottery mainly is used in fields such as material of infrared window, window pyrometer gate material, prism, polycrystal zirconia ornaments, radome and infrared rays nose cone.
1986, first zirconium white transparent block pottery is by the Koji Tsukuma from Toyo Soda Mfg. Co., Ltd. of Japan, by the traditional ceramics molding mode, after the 300MPa isostatic cool pressing under 1450 ~ 1630 ℃ of air atmospheres sintering after 7 ~ 15 hours, behind the hot isostatic pressing (HIP) under 1500 ℃ and 100MPa pressure and argon gas atmosphere again, 1200 ℃ of annealing and the transparent zirconium oxide pottery that obtains; Utilize discharge plasma sintering (SPS) method to utilize the 8Y-ZrO of Tosoh from S.R. Casolco of California, USA university etc.
2Nano powder has successfully prepared the good transparent zirconium oxide pottery of perviousness; Koji Tsukuma had further improved technological measure in 2008, successfully prepared the transparent zirconium oxide pottery with the HIP sintering method, and had analyzed sintering aid, sintering temperature to the influence of crystalline ceramics transmitance; People such as Ulrich Peuchert from German Scott group further improved sintering process on forefathers' basis in 2009, utilized the hot isostatic pressing method sintering successfully to prepare the transparent zirconium oxide pottery; People such as Liwen Lei had prepared the transparent zirconium oxide pottery by the discharge plasma sintering process in 2011, but very low in the transmitance of visible-range.
From above report about the transparent block ceramic of zirconium white, its main method still is prepared from by means of accurate high-end devices, or SPS, or HIP, and these equipment are very expensive, and cost is too high, and preparation technology is also also immature.Therefore up to now, the transparent zirconium oxide pottery still is not extensive use of in market, and relevant report is not also arranged at home.
Summary of the invention
Defectives such as equipment requirements height, the production cost that exists at prior art is big the object of the present invention is to provide a kind of preparation method of normal pressure-sintered transparent zirconium oxide stupalith, by doping Y
2O
3, Al
2O
3Nano powder adopts traditional ceramics preparation technology, formulates suitable sintering schedule, under lower sintering temperature, and normal pressure-sintered preparation transparent zirconium oxide stupalith.
For achieving the above object, the present invention adopts following technical scheme:
A kind of preparation method of normal pressure-sintered transparent zirconium oxide stupalith has following process and step:
A. adopt the commercial powder 10mol% of yttrium stable zirconium oxide Y
2O
3-ZrO
2, be called for short ZrY
10And high-purity Y
2O
3, Al
2O
3Nano powder is raw material, is body material with the commercial powder of yttrium stable zirconium oxide, with Y
2O
3, Al
2O
3Nano powder is dopant material, and incorporation in mass percent is: Y
2O
3: 0 ~ 30wt%, Al
2O
3: 0 ~ 5wt%;
B. will stir by the good body material of above-mentioned formulated and each dopant material mixed, compound mix grinding 24 hours in dehydrated alcohol;
C. compound is dried under 100 ℃ of temperature, carries out granulation then;
D. powder depresses to the sheet sample in 150 ~ 200MPa isostatic cool pressing, subsequently 1100 ~ 1400 ℃ of following pre-burnings 5 hours; Sample after the above-mentioned pre-burning is placed on carries out sintering in the hydrogen furnace, sintering range is 1600～1700 ℃, and sintering time is 24 hours, finally obtains the transparent zirconium oxide stupalith.
Compared with prior art, the present invention has following outstanding substantive distinguishing features and progressive significantly:
The present invention adopts legacy equipment, with normal pressure-sintered prepared the transparent zirconium oxide pottery, preparation technology is simple, cost is low, only sintering gets final product under normal pressure, and easy-formation, good stability can be widely used in fields such as material of infrared window, window pyrometer gate material, prism, polycrystal zirconia ornaments, radome and infrared rays nose cone.
Description of drawings
Fig. 1 is ZrY
10+ 30wt%Y
2O
3+ 0.25wt%Al
2O
3Crystalline ceramics straight line transmittance curve.
Embodiment
After now specific embodiments of the invention being described in.
Embodiment 1
Process and the step of present embodiment are described below:
A. adopt the commercial powder (ZrY of yttrium stable zirconium oxide
10) and high-purity Y
2O
3, Al
2O
3Nano powder is raw material, is body material with the commercial powder of yttrium stable zirconium oxide, with Y
2O
3, Al
2O
3Nano powder is dopant material, and incorporation in mass percent is: Y
2O
3: 20wt%, Al
2O
3: 0. 5wt%;
B. will stir by the good zirconium white matrix material of above-mentioned formulated and each dopant material mixed, compound mix grinding 24 hours in dehydrated alcohol;
C. compound is dried under 100 ℃ of temperature, carries out granulation then;
D. powder depresses to the sheet sample in the 200MPa isostatic cool pressing, subsequently 1400 ℃ of following pre-burnings 5 hours; Sample after the above-mentioned pre-burning is placed on carries out sintering in the hydrogen furnace, sintering range is 1700 ℃, and sintering time is 24 hours, finally obtains the zirconium white crystalline ceramics.
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is Al
2O
3Doping be 0.25wt%.
Embodiment 3
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is Al
2O
3Doping be 2wt%.
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is Al
2O
3Doping be 5wt%.
Embodiment 5
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is Y
2O
3Doping be 30wt%, Al
2O
3Doping be 0.25wt%.
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is Y
2O
3Doping be 30wt%, Al
2O
3Doping be 0.25wt%, sintering temperature is 1650 ℃.
Embodiment 7
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is Y
2O
3Doping be 30wt%, Al
2O
3Doping be 0.25wt%, sintering temperature is 1600 ℃.
Embodiment 8
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is Y
2O
3Doping be 30wt%, Al
2O
3Doping be 3wt%.
Embodiment 9
Identical among the method for the purity of the used powder raw material of present embodiment, pottery preparation and step and the embodiment 1.Difference is Y
2O
3Doping be 30wt%, Al
2O
3Doping be 5wt%.
Be illustrated in figure 1 as the straight line transmittance curve of sample in the embodiment of the invention 5.The composition of ceramics sample is ZrY among the embodiment 5
10+ 30wt%Y
2O
3+ 0.25wt%Al
2O
3, its straight line transmitance reaches as high as 25%.
Claims (1)
1. the preparation method of a normal pressure-sintered transparent zirconium oxide stupalith is characterized in that, has following process and step:
A. adopt the commercial powder 10mol% of yttrium stable zirconium oxide Y
2O
3-ZrO
2, be called for short ZrY
10And high-purity Y
2O
3, Al
2O
3Nano powder is raw material, is body material with the commercial powder of yttrium stable zirconium oxide, with Y
2O
3, Al
2O
3Nano powder is dopant material, and incorporation in mass percent is: Y
2O
3: 0 ~ 30wt%, Al
2O
3: 0 ~ 5wt%;
B. will stir by the good body material of above-mentioned formulated and each dopant material mixed, compound mix grinding 24 hours in dehydrated alcohol;
C. compound is dried under 100 ℃ of temperature, carries out granulation then;
D. powder depresses to the sheet sample in 150 ~ 200MPa isostatic cool pressing, subsequently 1100 ~ 1400 ℃ of following pre-burnings 5 hours; Sample after the above-mentioned pre-burning is placed on carries out sintering in the hydrogen furnace, sintering range is 1600～1700 ℃, and sintering time is 24 hours, finally obtains the transparent zirconium oxide stupalith.
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|---|---|---|---|
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|---|---|---|---|
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ID=48880322
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104613776A (en) * | 2014-12-29 | 2015-05-13 | 临沂临虹无机材料有限公司 | Zirconia ceramic composite material, manufacturing method thereof and method for sintering zirconia ceramic composite material on metal mesh |
| CN104944954A (en) * | 2015-06-19 | 2015-09-30 | 中国科学院上海光学精密机械研究所 | Infrared-transmitted ceramic and preparing method thereof |
| CN105110789A (en) * | 2015-09-02 | 2015-12-02 | 长沙鹏登生物陶瓷有限公司 | Modification method for preparing zirconia powder with super-transparency |
| CN106045505A (en) * | 2016-06-04 | 2016-10-26 | 上海大学 | Preparation method of magnesium oxide doped yttria-stabilized zirconia (5Y-PSZ) ceramic |
| CN106431392A (en) * | 2016-08-26 | 2017-02-22 | 东莞华晶粉末冶金有限公司 | Mobile terminal shell and preparation method thereof, and mobile terminal |
| CN114349500A (en) * | 2022-01-21 | 2022-04-15 | 中国科学院上海硅酸盐研究所 | Medium-wave infrared transparent zirconia ceramic material and preparation method thereof |
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|---|---|---|---|---|
| CN1587199A (en) * | 2004-09-03 | 2005-03-02 | 湖北葛店开发区地大纳米材料制造有限公司 | Aluminium/yttrium zirconium tertiary composite oxide nano structure aggregate powder and its producing method |
| CN1887786A (en) * | 2005-11-03 | 2007-01-03 | 韩敏芳 | Submicron transparent crystal alumina ceramic possessing high linear transmittance |
| CN103044024A (en) * | 2012-12-11 | 2013-04-17 | 北京固圣生物科技有限公司 | Zirconia-based composite ceramic for bone implantation prosthesis and bone implantation prosthesis prepared from same |
-
2013
- 2013-04-18 CN CN2013101345620A patent/CN103232237A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1587199A (en) * | 2004-09-03 | 2005-03-02 | 湖北葛店开发区地大纳米材料制造有限公司 | Aluminium/yttrium zirconium tertiary composite oxide nano structure aggregate powder and its producing method |
| CN1887786A (en) * | 2005-11-03 | 2007-01-03 | 韩敏芳 | Submicron transparent crystal alumina ceramic possessing high linear transmittance |
| CN103044024A (en) * | 2012-12-11 | 2013-04-17 | 北京固圣生物科技有限公司 | Zirconia-based composite ceramic for bone implantation prosthesis and bone implantation prosthesis prepared from same |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104613776A (en) * | 2014-12-29 | 2015-05-13 | 临沂临虹无机材料有限公司 | Zirconia ceramic composite material, manufacturing method thereof and method for sintering zirconia ceramic composite material on metal mesh |
| CN104944954A (en) * | 2015-06-19 | 2015-09-30 | 中国科学院上海光学精密机械研究所 | Infrared-transmitted ceramic and preparing method thereof |
| CN105110789A (en) * | 2015-09-02 | 2015-12-02 | 长沙鹏登生物陶瓷有限公司 | Modification method for preparing zirconia powder with super-transparency |
| CN106045505A (en) * | 2016-06-04 | 2016-10-26 | 上海大学 | Preparation method of magnesium oxide doped yttria-stabilized zirconia (5Y-PSZ) ceramic |
| CN106431392A (en) * | 2016-08-26 | 2017-02-22 | 东莞华晶粉末冶金有限公司 | Mobile terminal shell and preparation method thereof, and mobile terminal |
| CN114349500A (en) * | 2022-01-21 | 2022-04-15 | 中国科学院上海硅酸盐研究所 | Medium-wave infrared transparent zirconia ceramic material and preparation method thereof |
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Application publication date: 20130807 |