CN102718243A - Method for purifying waste sapphire crystals - Google Patents
Method for purifying waste sapphire crystals Download PDFInfo
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- CN102718243A CN102718243A CN2012100103206A CN201210010320A CN102718243A CN 102718243 A CN102718243 A CN 102718243A CN 2012100103206 A CN2012100103206 A CN 2012100103206A CN 201210010320 A CN201210010320 A CN 201210010320A CN 102718243 A CN102718243 A CN 102718243A
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- sapphire crystal
- sapphire
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Abstract
The invention relates a method for purifying sapphire crystals and especially relates to a method for purifying waste sapphire crystals. The method is characterized by comprising the following steps of crushing, organic solvent soaking, high temperature oxidation, high-temperature high-vacuum degassing, wet chemical treatment, cleaning and drying, and through the method, high purity sapphire crystals can be obtained. Compared with the prior art, the method has the advantages that waste sapphire crystals produced by growth and processing processes are recovered and purified so that the requirements of raw materials for growth of high-quality sapphire crystals are fully satisfied.
Description
Technical field
The present invention relates to the sapphire crystal purification process, is exactly the purification process of the discarded brilliant material of a kind of sapphire crystal specifically.Present method through the brilliant material of the discarded sapphire fragmentation that will grow, produce in the process such as processing after through high temperature oxidation, high temperature high vacuum degassing, wet chemical process; The brilliant material of purity is not high, the sapphire that polluted reclaims and purifying in addition, makes it reach the needs of high quality sapphire crystal growth raw material fully.
Background technology
With gan (GaN) be representative broad stopband third generation semiconductor material development in recent years very rapidly; Gan (GaN) base semiconductor material has characteristics such as luminous efficiency height, good thermal conductivity, high temperature resistant, radioprotective, HS and high firmness, can be made into efficient indigo plant, green light LED and laser diode (claiming laser apparatus again).But gan (GaN) material itself can not grow monocrystalline, must be grown on the substrate material with its structure similar.The substrate material of generally acknowledging in the world at present is a sapphire crystal.
The LED substrate generally adopts kyropoulos (Kyropoulos with sapphire crystal growth; Be called for short Ky method or Kjeldahl method, crystal pulling method (Czochralski; Be called for short Cz method or Chai Shi method), heat-exchanging method (Heat Exchanger Method is called for short HEM), guided mode method (Edge Defined Film-Fed Growth is called for short EFG) etc., it is 99.999% alumina raw material that the raw material of use is generally purity.Though adopt the technology of growing sapphire to have nothing in common with each other; But all can in the sapphire growth and the course of processing, produce the brilliant material of a large amount of depleted sapphires; These brilliant material foreign matter content enrichments; And polluted by crucible, the course of processing, generally can not be used for doing the growth of high quality sapphire crystal, caused a lot of waste materials.Sapphire waste material hardness is high, can't clear up at nature, and the generation of a large amount of waste materials brings higher cost to production.Solve in these a large amount of sapphire production processes waste problems to society or enterprise itself all is something highly significant.The present invention focuses on that to The Characteristic Study in the sapphire crystal growth and the course of processing recovery and the purifying that solve the sapphire waste material utilize problem again.
Summary of the invention
The present invention provides a kind of method of the discarded brilliant material of sapphire crystal being carried out purifying in order to overcome the deficiency of prior art.
To achieve these goals, the present invention has designed the purification process of the discarded brilliant material of a kind of sapphire crystal, it is characterized in that: adopt following steps:
(a) carry out break process with producing discarded brilliant material in the sapphire crystal growth process and the course of processing;
(b) the crystalline substance material after the fragmentation is soaked in the organic solvent;
(c) the crystalline substance material is separated oven dry with raw spirit;
(d) the crystalline substance material after will drying places and carries out high temperature oxidation in the oxygen atmosphere stove;
(e) place high-temperature vacuum degassing Reaktionsofen to carry out the high temperature high vacuum degassing in the crystalline substance material after the oxidation and handle, the metallic impurity of some planes of crystal will at high temperature volatilize, and the crystals metallic impurity are expected surface/crystal boundary position migration to crystalline substance;
(f) again with the crystalline substance material after the high-temperature process, by wet chemical process, deionized water filters, and oven dry obtains highly purified sapphire crystal growth and expects with brilliant.
Among the said step a, the crystallographic dimension that obtains after the fragmentation is 5-20mm.
Among the said step b, organic solvent is a kind of in raw spirit, acetone, the gasoline.
In the said steps d, the oxygen atmosphere stove is a kind of in silicon carbide rod furnace, Si-Mo rod stove, the kiln.
In the said steps d, oxidizing temperature is 800-1500oC, and oxidization time is 3-24 hour.
Among the said step e, the vacuum tightness of high-temperature vacuum degassing Reaktionsofen is 5 * 10
-3Below the Pa.
Among the said step f, the metallurgical acid solution of handling employing of wet chemistry is HCl, HF, H
2SO
4, HNO
3In one or more mix acid liquors, soaking temperature is 20-85 oC, soak time is more than 6 hours.
The present invention compares with prior art; Through after the brilliant material of the discarded sapphire fragmentation that will grow, produce in the process such as processing through high temperature oxidation, high temperature high vacuum degassing, wet chemical process; The brilliant material of purity is not high, the sapphire that polluted reclaims and purifying in addition, makes it reach the needs of high quality sapphire crystal growth raw material fully.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
Below in conjunction with accompanying drawing the present invention is further described.
As shown in Figure 1, purification process of the present invention adopts following steps.
A, carry out break process with producing discarded brilliant material in the sapphire crystal growth process and the course of processing, the crystallographic dimension that obtains after the fragmentation is 5-20mm, and preferred size is about 10mm.
B, the crystalline substance material after the fragmentation is soaked in the organic solvent, organic solvent is a kind of in raw spirit, acetone, the gasoline.
C., the crystalline substance material is separated oven dry with raw spirit.
D., the crystalline substance material after will drying places and carries out high temperature oxidation in the oxygen atmosphere stove, the oxygen atmosphere stove is a kind of in silicon carbide rod furnace, Si-Mo rod stove, the kiln, its oxidizing temperature is 800-1500oC, preferred temperature is 1000-1400 oC, oxidization time is 3-24 hour.
E, place high-temperature vacuum degassing Reaktionsofen to carry out the high temperature high vacuum degassing in the crystalline substance material after the oxidation to handle, vacuum tightness is 5 * 10
-3Below the Pa, preferred value is 1 * 10
-3Below the Pa, the metallic impurity of some planes of crystal will at high temperature volatilize, and the crystals metallic impurity are expected surface/crystal boundary position migration to crystalline substance.
F., again with the crystalline substance material after the pyroprocessing, through wet chemical process, wet chemistry is metallurgical, and to handle the acid solution that adopts be HCl, HF, H
2SO
4, HNO
3In one or more mix acid liquors, soaking temperature is 20-85 oC, soak time is more than 6 hours, deionized water filters then, oven dry obtains highly purified sapphire crystal growth with brilliant material.
Compare with prior art; Through after the brilliant material of the discarded sapphire fragmentation that will grow, produce in the process such as processing through high temperature oxidation, high temperature high vacuum degassing, wet chemical process; The brilliant material of purity is not high, the sapphire that polluted reclaims and purifying in addition, makes it reach the needs of high quality sapphire crystal growth raw material fully.
Claims (7)
1. a sapphire crystal is discarded brilliant purification process of expecting, it is characterized in that: adopt following steps:
A, carry out break process with producing discarded brilliant material in the sapphire crystal growth process and the course of processing;
B, the crystalline substance material after the fragmentation is soaked in the organic solvent;
B, the crystalline substance material is separated oven dry with raw spirit;
D, the crystalline substance material after will drying place and carry out high temperature oxidation in the oxygen atmosphere stove;
E, place high-temperature vacuum degassing Reaktionsofen to carry out the high temperature high vacuum degassing in the crystalline substance material after the oxidation to handle, the metallic impurity of some planes of crystal will at high temperature volatilize, and the crystals metallic impurity are expected surface/crystal boundary position migration to crystalline substance;
F, again with the crystalline substance material after the pyroprocessing, through wet chemical process, deionized water filters, oven dry obtains highly purified sapphire crystal growth with brilliant material.
2. the purification process of the discarded brilliant material of sapphire crystal according to claim 1, it is characterized in that: among the said step a, the crystallographic dimension that obtains after the fragmentation is 5-20mm.
3. the purification process of the discarded brilliant material of sapphire crystal according to claim 1 is characterized in that: among the said step b, organic solvent is a kind of in raw spirit, acetone, the gasoline.
4. the purification process of the discarded brilliant material of sapphire crystal according to claim 1 is characterized in that: in the said steps d, the oxygen atmosphere stove is a kind of in silicon carbide rod furnace, Si-Mo rod stove, the kiln.
5. according to the purification process of claim 1 or the discarded brilliant material of 4 described sapphire crystals, it is characterized in that: in the said steps d, oxidizing temperature is 800-1500oC, and oxidization time is 3-24 hour.
6. the purification process of the discarded brilliant material of sapphire crystal according to claim 1 is characterized in that: among the said step e, the vacuum tightness of high-temperature vacuum degassing Reaktionsofen is 5 * 10
-3Below the Pa.
7. the purification process of the discarded brilliant material of sapphire crystal according to claim 1 is characterized in that: among the said step f, the acid solution that the metallurgical processing of wet chemistry is adopted is HCl, HF, H
2SO
4, HNO
3In one or more mix acid liquors, soaking temperature is 20-85 oC, soak time is more than 6 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100103206A CN102718243A (en) | 2012-01-13 | 2012-01-13 | Method for purifying waste sapphire crystals |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100103206A CN102718243A (en) | 2012-01-13 | 2012-01-13 | Method for purifying waste sapphire crystals |
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| CN102718243A true CN102718243A (en) | 2012-10-10 |
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ID=46944153
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| CN2012100103206A Pending CN102718243A (en) | 2012-01-13 | 2012-01-13 | Method for purifying waste sapphire crystals |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104131354A (en) * | 2013-05-02 | 2014-11-05 | 周黎 | Recycling method of residual crystal scrap after processing of sapphire crystal |
| CN113415817A (en) * | 2021-07-22 | 2021-09-21 | 东莞晶驰光电科技有限公司 | Method for regenerating sapphire raw material and regenerated sapphire |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5914024A (en) * | 1994-12-24 | 1999-06-22 | Abb Flaekt Ab | Method for cleaning of aluminum oxide powders |
| CN101588993A (en) * | 2006-12-15 | 2009-11-25 | 日本轻金属株式会社 | Process for producing high-purity alpha-alumina |
| CN102229113A (en) * | 2011-06-07 | 2011-11-02 | 王楚雯 | Method for recovering sapphire powder |
-
2012
- 2012-01-13 CN CN2012100103206A patent/CN102718243A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5914024A (en) * | 1994-12-24 | 1999-06-22 | Abb Flaekt Ab | Method for cleaning of aluminum oxide powders |
| CN101588993A (en) * | 2006-12-15 | 2009-11-25 | 日本轻金属株式会社 | Process for producing high-purity alpha-alumina |
| CN102229113A (en) * | 2011-06-07 | 2011-11-02 | 王楚雯 | Method for recovering sapphire powder |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104131354A (en) * | 2013-05-02 | 2014-11-05 | 周黎 | Recycling method of residual crystal scrap after processing of sapphire crystal |
| CN113415817A (en) * | 2021-07-22 | 2021-09-21 | 东莞晶驰光电科技有限公司 | Method for regenerating sapphire raw material and regenerated sapphire |
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Address after: 200127, room 899, 1009 Dongfang Road, Shanghai, Pudong New Area Applicant after: SHANGHAI YINGBEN OPTOELECTRONICS TECHNOLOGY CO., LTD. Address before: 200127, room 899, 1009 Dongfang Road, Shanghai, Pudong New Area Applicant before: Shanghai Yingben Crystal Technology Co.,Ltd. |
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Free format text: CORRECT: APPLICANT; FROM: SHANGHAI WINSPEED CRYSTALS SCIENCE + TECHNOLOGY CO., LTD. TO: SHANGHAI WINSPEED PHOTOVOLTAICS TECHNOLOGY CO., LTD. |
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Effective date of abandoning: 20170517 |