CN101486574A - Method for preparing YAG transparent ceramic powder by solid-phase reaction - Google Patents
Method for preparing YAG transparent ceramic powder by solid-phase reaction Download PDFInfo
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- CN101486574A CN101486574A CNA2009100213685A CN200910021368A CN101486574A CN 101486574 A CN101486574 A CN 101486574A CN A2009100213685 A CNA2009100213685 A CN A2009100213685A CN 200910021368 A CN200910021368 A CN 200910021368A CN 101486574 A CN101486574 A CN 101486574A
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Abstract
The invention discloses a method for preparing YAG transparent ceramic powder by solid phase reaction. At first, analytically pure Alpha-Al2O3 powder and Y2O3 powder are uniformly mixed and ethyl orthosilicate is added as a sintering addition agent to obtain powder; secondarily, the powder is arranged into a corundum grinding jar provided with a corundum grinding ball; then the grinding jar is ball-ground on a planetary ball mill after absolute ethyl alcohol and Y2O3 are added; the grinded powder material is taken out and dried, and then calcined in a high temperature electric furnace, thus obtaining pure YAG transparent ceramic powder. As a mechanical ball mill only employs the grinding ball and the grinding jar of the corundum material, and does not need to employ a coating material or a high-cost high-pure heterologous material as a grinding ball, the technique device thereof is simple and the purity of the obtained powder is higher; and the YAG transparent ceramic with good light transmission performance can be obtained by carrying out press forming and high temperature sintering to the obtained powder.
Description
Technical field
The present invention relates to a kind of method of the YAG of preparation transparent ceramic powder, be specifically related to a kind of method of preparing YAG transparent ceramic powder by solid-phase reaction.
Background technology
Yttrium aluminum garnet is called for short YAG (yttrium aluminum garnet), have stable chemical properties and good optical property and mechanical behavior under high temperature, obtained using widely in a lot of fields, such as being widely used in laser body material, fluorescent material and fluorescence thermometer etc., also often be used to the resistance to chemical attack structured material of refractory coating, thermal radiation convertor of electronic component and electronic instrument parts etc.The preparation technology of YAG powder has a significant impact the performance of its related products, and the high-property YAG powder can effectively improve the performance of its related products.The YAG powder of excellent property should have good dispersity, thin, the regular shape features such as (being preferably spherical) of particle.Adopt the spherical powder material effectively to lower porosity, be conducive to the preparation of crystalline ceramics.
Preparation YAG powder method is a lot, and methods such as solid reaction process, sol-gel method, combustion synthesis method, spray pyrolysis and chemical precipitation method are arranged.Wherein solid reaction process is that a kind of cost is low, production is easy, efficient is high, the suitable synthetic method of producing in enormous quantities.But still there is the calcining temperature height in solid reaction process, the bad grasp of ball milling time, and mechanical milling process is sneaked into shortcomings such as impurity effect powder characteristic.
The method of being reported at present for preparing the YAG crystalline ceramics with solid reaction process is mainly ball grinder and adopts nylon material to make liner, abrading-ball adopts nylon material parcel [Li Changqing, left side big waves, Zhang Mingfu etc. solid reaction process prepares transparent polycrystalline YAG pottery. silicate journal, 2006,34 (8): 979-984] and abrading-ball adopt high-purity ZrO
2Method [Wen Lei, Sun Xudong, Ma Weimin. solid reaction process prepares the YAG crystalline ceramics. silicate journal, 2003,31 (9): 819-822].No matter these two kinds of methods are to adopt nylon to make liner or lapping or adopt high-purity ZrO
2Make abrading-ball, its main purpose is in order to prevent the pollution of powder body material, but the Ball-milling Time of solid reaction process is all long (tens even tens hours) generally, like this, equipment cost was improved, can't avoid again the wear debris of these lappings or heterogeneous material abrading-ball to pollute powder body material.In order to reach the purpose of practicability, must the low YAG powder solid reaction process preparation technology of Development and Production cost.
Summary of the invention
The object of the present invention is to provide a kind of method of preparing YAG transparent ceramic powder by solid-phase reaction, this method not only processing unit is simple, and cost is low, and can prepare purity height, YAG transparent ceramic powder that printing opacity is good.
For achieving the above object, the technical solution used in the present invention is:
1) at first, with analytically pure α-Al
2O
3Powder and Y
2O
3Powder according to the mixed in molar ratio of 5-7:3 even mixed powder, and the ethyl orthosilicate that adds mixed powder quality 0.3-0.8% in mixed powder gets powder as sintering aid;
2) secondly, powder put into corundum ball grinder that corundum material abrading-ball is housed and mix by the mass ratio of powder: abrading-ball: absolute ethyl alcohol=1:2-5:0.6-0.8, add simultaneously the Y of powder quality percentage 0.2-0.5%
2O
3After with this ball grinder at planetary ball mill ball milling 15-25h;
3) powder body material that ball milling is good takes out and oven dry, namely gets pure YAG transparent ceramic powder in 1300-1500 ℃ of calcining 30-60min then in high-temperature electric resistance furnace.
Because mechanical ball milling directly adopts abrading-ball and the ball grinder of corundum material, need not adopt lapping or expensive high-purity heterogeneous material to make abrading-ball, therefore, its process equipment is simple, gained powder purity is higher, by obtaining the good YAG crystalline ceramics of printing opacity to its compression moulding and high temperature sintering.
Description of drawings
What is Fig. 1 that (horizontal stroke, ordinate zou respectively represent with Japanese D/max2000 type X-ray diffractometer analysis chart of science for the YAG transparent ceramic powder of the embodiment of the invention 1 preparation?).
Embodiment
Embodiment 1: at first, and with analytically pure α-Al
2O
3Powder and Y
2O
3Powder according to the mixed in molar ratio of 5:3 even mixed powder, and the ethyl orthosilicate that adds mixed powder quality 0.5% in mixed powder gets powder as sintering aid; Secondly, powder is put into corundum ball grinder that corundum material abrading-ball is housed by powder: the mass ratio of abrading-ball: absolute ethyl alcohol=1:4:0.6 mixes, and adds simultaneously the Y of powder quality percentage 0.2%
2O
3After with this ball grinder at planetary ball mill ball milling 20h; The powder body material that ball milling is good takes out and oven dry, namely gets pure YAG transparent ceramic powder in 1400 ℃ of calcining 40min then in high-temperature electric resistance furnace.
The YAG powder of gained with Japanese D/max2000 type X-ray diffractometer analytic sample of science, is found that the gained powder is more purified YAG phase (see figure 1).The YAG crystalline ceramics of making of this powder has good light transmission (transmitance at infrared region has reached 70%).
Embodiment 2: at first, and with analytically pure α-Al
2O
3Powder and Y
2O
3Powder according to the mixed in molar ratio of 7:3 even mixed powder, and the ethyl orthosilicate that adds mixed powder quality 0.3% in mixed powder gets powder as sintering aid; Secondly, powder is put into corundum ball grinder that corundum material abrading-ball is housed by powder: the mass ratio of abrading-ball: absolute ethyl alcohol=1:2:0.7 mixes, and adds simultaneously the Y of powder quality percentage 0.3%
2O
3After with this ball grinder at planetary ball mill ball milling 15h; The powder body material that ball milling is good takes out and oven dry, namely gets pure YAG transparent ceramic powder in 1300 ℃ of calcining 60min then in high-temperature electric resistance furnace.
Embodiment 3: at first, and with analytically pure α-Al
2O
3Powder and Y
2O
3Powder according to the mixed in molar ratio of 6:3 even mixed powder, and the ethyl orthosilicate that adds mixed powder quality 0.8% in mixed powder gets powder as sintering aid; Secondly, powder is put into corundum ball grinder that corundum material abrading-ball is housed by powder: the mass ratio of abrading-ball: absolute ethyl alcohol=1:5:0.8 mixes, and adds simultaneously the Y of powder quality percentage 0.5%
2O
3After with this ball grinder at planetary ball mill ball milling 25h; The powder body material that ball milling is good takes out and oven dry, namely gets pure YAG transparent ceramic powder in 1500 ℃ of calcining 30min then in high-temperature electric resistance furnace.
The present invention reunites in mechanical milling process in order to prevent powder, adds an amount of absolute ethyl alcohol as dispersant.Al appears in order to prevent that wearing and tearing because of abrading-ball and ball grinder from causing in the final powder
2O
3Having more than needed of phase added excessive Y when ball milling
2O
3, it acts on except the wear debris with abrading-ball and ball grinder reacts, excessive Y
3+Easier being contained among the YAG is so that prepared YAG powder phase free from foreign meter; The YAG powder purity height that the method makes, homogeneity is good, and is good with the crystalline ceramics light transmission of its making, the sample densification; The YAG powder of technology preparation,
Claims (4)
1, a kind of method of preparing YAG transparent ceramic powder by solid-phase reaction is characterized in that:
1) at first, with analytically pure α-Al
2O
3Powder and Y
2O
3Powder according to the mixed in molar ratio of 5-7:3 even mixed powder, and the ethyl orthosilicate that adds mixed powder quality 0.3-0.8% in mixed powder gets powder as sintering aid;
2) secondly, powder put into corundum ball grinder that corundum material abrading-ball is housed and mix by the mass ratio of powder: abrading-ball: absolute ethyl alcohol=1:2-5:0.6-0.8, add simultaneously the Y of powder quality percentage 0.2-0.5%
2O
3After with this ball grinder at planetary ball mill ball milling 15-25h;
3) powder body material that ball milling is good takes out and oven dry, namely gets pure YAG transparent ceramic powder in 1300-1500 ℃ of calcining 30-60min then in high-temperature electric resistance furnace.
2, the method for preparing YAG transparent ceramic powder by solid-phase reaction according to claim 1 is characterized in that: at first, and with analytically pure α-Al
2O
3Powder and Y
2O
3Powder according to the mixed in molar ratio of 5:3 even mixed powder, and the ethyl orthosilicate that adds mixed powder quality 0.5% in mixed powder gets powder as sintering aid; Secondly, powder is put into corundum ball grinder that corundum material abrading-ball is housed by powder: the mass ratio of abrading-ball: absolute ethyl alcohol=1:4:0.6 mixes, and adds simultaneously the Y of powder quality percentage 0.2%
2O
3After with this ball grinder at planetary ball mill ball milling 20h; The powder body material that ball milling is good takes out and oven dry, namely gets pure YAG transparent ceramic powder in 1400 ℃ of calcining 40min then in high-temperature electric resistance furnace.
3, the method for preparing YAG transparent ceramic powder by solid-phase reaction according to claim 1 is characterized in that: at first, and with analytically pure α-Al
2O
3Powder and Y
2O
3Powder according to the mixed in molar ratio of 7:3 even mixed powder, and the ethyl orthosilicate that adds mixed powder quality 0.3% in mixed powder gets powder as sintering aid; Secondly, powder is put into corundum ball grinder that corundum material abrading-ball is housed by powder: the mass ratio of abrading-ball: absolute ethyl alcohol=1:2:0.7 mixes, and adds simultaneously the Y of powder quality percentage 0.3%
2O
3After with this ball grinder at planetary ball mill ball milling 15h; The powder body material that ball milling is good takes out and oven dry, namely gets pure YAG transparent ceramic powder in 1300 ℃ of calcining 60min then in high-temperature electric resistance furnace.
4, the method for preparing YAG transparent ceramic powder by solid-phase reaction according to claim 1 is characterized in that: at first, and with analytically pure α-Al
2O
3Powder and Y
2O
3Powder according to the mixed in molar ratio of 6:3 even mixed powder, and the ethyl orthosilicate that adds mixed powder quality 0.8% in mixed powder gets powder as sintering aid; Secondly, powder is put into corundum ball grinder that corundum material abrading-ball is housed by powder: the mass ratio of abrading-ball: absolute ethyl alcohol=1:5:0.8 mixes, and adds simultaneously the Y of powder quality percentage 0.5%
2O
3After with this ball grinder at planetary ball mill ball milling 25h; The powder body material that ball milling is good takes out and oven dry, namely gets pure YAG transparent ceramic powder in 1500 ℃ of calcining 30min then in high-temperature electric resistance furnace.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891477A (en) * | 2010-07-23 | 2010-11-24 | 中国科学院上海硅酸盐研究所 | Method for preparing circular rod-shaped RE:YAG laser transparent ceramics |
| CN102115570A (en) * | 2010-12-10 | 2011-07-06 | 吉林大学 | Method for preparing nano fluorescence thermometer |
| CN102173825A (en) * | 2011-01-28 | 2011-09-07 | 中国科学院上海光学精密机械研究所 | Sintering aid for yttrium aluminum garnet-based fluorescent transparent ceramic and using method thereof |
| CN102211942A (en) * | 2010-04-09 | 2011-10-12 | 中国科学院上海硅酸盐研究所 | Preparation method of Er: YAG polycrystal transparent ceramic material |
| CN102976742A (en) * | 2012-11-09 | 2013-03-20 | 航天材料及工艺研究所 | Preparation method of single-phase monolithic ceramic Y4Al2O9 |
| CN106163246A (en) * | 2016-07-12 | 2016-11-23 | 苏州创思得新材料有限公司 | A kind of back cover of digital product |
| CN106631035A (en) * | 2016-12-29 | 2017-05-10 | 广东工业大学 | Composite ceramic and preparation method thereof |
-
2009
- 2009-03-03 CN CNA2009100213685A patent/CN101486574A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102211942A (en) * | 2010-04-09 | 2011-10-12 | 中国科学院上海硅酸盐研究所 | Preparation method of Er: YAG polycrystal transparent ceramic material |
| CN101891477A (en) * | 2010-07-23 | 2010-11-24 | 中国科学院上海硅酸盐研究所 | Method for preparing circular rod-shaped RE:YAG laser transparent ceramics |
| CN101891477B (en) * | 2010-07-23 | 2013-01-02 | 中国科学院上海硅酸盐研究所 | Method for preparing circular rod-shaped RE:YAG laser transparent ceramics |
| CN102115570A (en) * | 2010-12-10 | 2011-07-06 | 吉林大学 | Method for preparing nano fluorescence thermometer |
| CN102173825A (en) * | 2011-01-28 | 2011-09-07 | 中国科学院上海光学精密机械研究所 | Sintering aid for yttrium aluminum garnet-based fluorescent transparent ceramic and using method thereof |
| CN102976742A (en) * | 2012-11-09 | 2013-03-20 | 航天材料及工艺研究所 | Preparation method of single-phase monolithic ceramic Y4Al2O9 |
| CN106163246A (en) * | 2016-07-12 | 2016-11-23 | 苏州创思得新材料有限公司 | A kind of back cover of digital product |
| CN106631035A (en) * | 2016-12-29 | 2017-05-10 | 广东工业大学 | Composite ceramic and preparation method thereof |
| CN106631035B (en) * | 2016-12-29 | 2020-08-11 | 广东工业大学 | Composite ceramic and preparation method thereof |
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