CN102618735B - Method for removing impurity bismuth in metal gallium - Google Patents
Method for removing impurity bismuth in metal gallium Download PDFInfo
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- CN102618735B CN102618735B CN 201210119811 CN201210119811A CN102618735B CN 102618735 B CN102618735 B CN 102618735B CN 201210119811 CN201210119811 CN 201210119811 CN 201210119811 A CN201210119811 A CN 201210119811A CN 102618735 B CN102618735 B CN 102618735B
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Abstract
The invention discloses a method for removing impurity bismuth in metal gallium, which adopts a partial crystallization purification technique to implement the operation for four times. The technical condition is set as: a temperature gradient is 1.1 to 1.4 DEG C/cm, an average crystallization speed is 3.2 to 4.2g/min, and the solid-liquid ratio is 75 to 85 percent. Compared with the prior art, the method can effectively lower the bismuth content in the gallium metal to the limit (5ppb) or less detected by a glow discharge mass spectrometry (GDMS), so that a good condition can be created for preparing high-purity gallium with the purity of 99.9999 percent.
Description
Technical field
The present invention relates to a kind of method of purification, relate in particular to a kind of method that adopts partial crystallization method purifying technique to remove impurity bismuth in gallium.
Background technology
In modern high-tech field, use a lot of highly purified materials.High-purity gallium is exactly one of extremely important material in the electronics science development.For this reason, a lot of purifying substances have been developed, the method for the element of especially purifying metals.The gallium of purifying metals is exactly give prominence in the development of high purity electronic material a kind of.The method of gallium of purifying metals has: chemical extraction method, the preferential chlorination process of impurity, electrolytic refining process, vertical temperature gradient freezing method (VGF), algan single crystal drawing and compound purification reduction method etc.But aforesaid method is all undesirable to removing impurity bismuth effect, so that when in the raw material gallium, the impurity bi content is too high, reaches 49ppm as bi content, is difficult to get in order to the top legal system high purity gallium of purity 99.9999%.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, and a kind of method that adopts the longitudinal temperature gradient solidification purifying technique to remove impurity bismuth in gallium is provided.
The technical scheme that the present invention takes is:
A kind of method of removing impurity bismuth in gallium adopts partial crystallization method purifying technique to carry out four operations, and processing condition are: 1.1 ~ 1.4 ℃/cm of thermograde, average crystallite speed is 3.2 ~ 4.2g/min, solid-to-liquid ratio 75 ~ 85%.
Through four partial crystallization operations, can be reduced to the content of bismuth in gallium below 5ppb from 11ppm, namely in gallium, the content of bismuth is reduced to the content requirement of 6N from 4N.Adopt method of the present invention, bi content is that 49ppm raw material gallium operates through four partial crystallizations, and bismuth is enriched in the liquid phase gallium, and in the liquid phase gallium, bi content reaches 3370ppm.
Compared with prior art, the method that the present invention adopts can be effectively be reduced to the content of bismuth in gallium below the limit＜5ppb that glow discharge spectrometry (GDMS) detects, for the high purity gallium of producing purity 99.9999% creates good conditions.
Embodiment
The present invention is further described in more detail below in conjunction with subordinate list and specific embodiment.
Embodiment 1: a kind of method of removing impurity bismuth in gallium, adopt the longitudinal temperature gradient solidification purifying technique to carry out adding for four times a partial crystallization operation, the processing condition of partial crystallization are: 1.1 ~ 1.4 ℃/cm of longitudinal temperature gradient, average crystallite speed is 3.2 ~ 4.2g/min, solid-to-liquid ratio 75 ~ 85%.
Adopt above-mentioned processing condition, 3 groups of samples are carried out 5 partial crystallization operations separately, refining effect is referring to table 1.S wherein
0Be raw material gallium, S
3Be the solid phase of the 3rd partial crystallization output, S
4Be the solid phase of the 4th partial crystallization output, S
5Solid phase for the 5th partial crystallization output.
Table 1, impurity bismuth element content unit: ppm.wt.
The enrichment condition of impurity bismuth element is referring to table 2.L wherein
1: represent remaining liquid gallium after crystallization for the first time; L
2: represent L
1Remaining liquid gallium after crystallization again; L
2S: represent L
2The solid phase of output after crystallization; L
3: represent L
2Remaining liquid gallium after crystallization; L
3S: represent L
3The solid phase of output after crystallization; L
4: represent L
3Remaining liquid gallium after crystallization.
Table 2, the enrichment of impurity bismuth element content unit: ppm.wt.
After four partial crystallization operations, can be reduced to the content of bismuth in gallium below 5ppb from 11ppm.Adopt method of the present invention, bi content is that after 49ppm raw material gallium operates through four partial crystallizations, bismuth is enriched in the liquid phase gallium, and in the liquid phase gallium, bi content reaches 3370ppm.
In addition to the implementation, the present invention can also have other embodiments, and all employings are equal to the technical scheme of replacement or equivalent transformation formation, within all dropping on the protection domain of requirement of the present invention.
Claims (2)
1. method of removing impurity bismuth in gallium is characterized in that: adopt the longitudinal temperature gradient solidification purifying technique to operate, processing condition are: thermograde is 1.1-1.4 ℃/cm, and average crystallite speed is 3.2-4.2g/min, solid-to-liquid ratio 75-85%.
2. the method for impurity bismuth in removal gallium according to claim 1 is characterized in that: through four longitudinal temperature gradient solidification purifying techniques operations, the content of bismuth in gallium is reduced to the content requirement of 6N from 4N.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210119811 CN102618735B (en) | 2012-04-23 | 2012-04-23 | Method for removing impurity bismuth in metal gallium |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201210119811 CN102618735B (en) | 2012-04-23 | 2012-04-23 | Method for removing impurity bismuth in metal gallium |
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| CN102618735A CN102618735A (en) | 2012-08-01 |
| CN102618735B true CN102618735B (en) | 2013-05-08 |
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| CN 201210119811 Active CN102618735B (en) | 2012-04-23 | 2012-04-23 | Method for removing impurity bismuth in metal gallium |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108611500B (en) * | 2018-06-27 | 2019-10-25 | 东南大学 | A kind of low-melting-point metal method of purification |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0349449B1 (en) * | 1988-07-01 | 1992-05-13 | Aluminium Pechiney | Process for purifying gallium by partial solidification |
| CN101082086A (en) * | 2007-06-22 | 2007-12-05 | 东南大学 | Preparation method of high-purity gallium |
| CN101413068A (en) * | 2008-10-29 | 2009-04-22 | 南京金美镓业有限公司 | Metal gallium longitudinal temperature gradient solidification purification apparatus and method |
| JP4916203B2 (en) * | 2006-03-31 | 2012-04-11 | Ｄｏｗａホールディングス株式会社 | Purification method of gallium |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63270430A (en) * | 1987-04-24 | 1988-11-08 | Chiyoda Chem Eng & Constr Co Ltd | Vacuum thermal decomposition method for gallium-containing material |
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2012
- 2012-04-23 CN CN 201210119811 patent/CN102618735B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0349449B1 (en) * | 1988-07-01 | 1992-05-13 | Aluminium Pechiney | Process for purifying gallium by partial solidification |
| JP4916203B2 (en) * | 2006-03-31 | 2012-04-11 | Ｄｏｗａホールディングス株式会社 | Purification method of gallium |
| CN101082086A (en) * | 2007-06-22 | 2007-12-05 | 东南大学 | Preparation method of high-purity gallium |
| CN101413068A (en) * | 2008-10-29 | 2009-04-22 | 南京金美镓业有限公司 | Metal gallium longitudinal temperature gradient solidification purification apparatus and method |
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| CN102618735A (en) | 2012-08-01 |
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Effective date of registration: 20221024 Address after: 122304 Kazuo Economic Development Zone, Chaoyang City, Liaoning Province Patentee after: Chaoyang Jinmei gallium Industry Co.,Ltd. Address before: 211165 No. 718, Jiangjun Avenue, Jiangning Development Zone, Nanjing, Jiangsu Patentee before: NANJING JINMEI GALLIUM Ltd. |