CN103965226A - Triethyl gallium production method - Google Patents
Triethyl gallium production method Download PDFInfo
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- CN103965226A CN103965226A CN201310036444.6A CN201310036444A CN103965226A CN 103965226 A CN103965226 A CN 103965226A CN 201310036444 A CN201310036444 A CN 201310036444A CN 103965226 A CN103965226 A CN 103965226A
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- gallium
- triethyl
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Abstract
The invention provides a triethyl gallium synthesis method. The triethyl gallium synthesis method comprises the following steps of adding a gallium source and ethyl aluminum into an inert atmosphere-containing reactor, keeping a mixed system temperature of 0-150 DEG C, and carrying out distillation in mixing or after mixing to obtain triethyl gallium. The triethyl gallium synthesis method does not adopt any solvent, has the advantages of high efficiency, high yield and high selectivity, has simple reaction processes and substantially reduces a production cost.
Description
Technical field
The present invention relates to a kind of preparation method of triethyl-gallium.
Background technology
Along with the development of semiconductor manufacturing industry, in recent years, the development of the III A group-III nitride taking gan as representative is very fast, becomes the focus of semi-conductor industry area research and exploitation.The Semiconductor Microstructure Materials being formed by it, the electronic drift saturating speed that brings its broad stopband is high, specific inductivity is little and the feature such as good heat conductivity,
Make it aspect luminescent device of making short wavelength, high brightness, there is good prospect.MOCVD technology is compared with other any epitaxy technology, and it can make more big area, more uniform film, also more easily realizes industrialization.In the growth of current III A group nitride material, MOCVD is also one of the most successful growing technology.In MOCVD grows the technology of the III A group-III nitride taking GaN as representative, the selection in gallium source plays conclusive effect for the growth properties of III A group-III nitride, on on the impact of device performance, gallium source is important more than aluminium source, and different selections directly has influence on a series of critical natures such as microstructure, configuration of surface, electrical properties and the optical property of the thin-film material growing.For the consideration of the source to MO source, purity and performance, trimethyl-gallium and triethyl-gallium are current the most frequently used gallium sources.
Triethyl-gallium is the extraordinary presoma starting material of growing gallium nitride, and also there is no the more report about triethyl-gallium synthetic method at present, is particularly applicable to the method report of the triethyl-gallium of suitability for industrialized production.Conventional synthetic method has: 1, react in ether solvent with gallium trichloride and Grignard reagent, react that not only productive rate is lower, and to use a large amount of lower boiling ether be solvent, have larger potential safety hazard; 2, gallium-magnesium alloy and monobromethane or iodoethane react in ether solvent, also have the shortcoming that productive rate is not high and use ether is solvent, need to use the source that the expensive iodoethane of price comparison is ethyl simultaneously, have increased cost; 3, carry out transalkylation reaction with gallium trichloride and triethyl aluminum, the raw material triethyl aluminum that reaction is used is inflammable, has used a large amount of solvents in reaction, and this has just proposed higher requirement to production unit etc., has also increased cost simultaneously.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of synthetic method of triethyl-gallium of applicable suitability for industrialized production, the above-mentioned defect existing to overcome prior art.
For solving the problems of the technologies described above, the present invention realizes by the following technical solutions:
A synthetic method for triethyl-gallium, comprises the steps: in the reactor of inert atmosphere, to add gallium source and aluminium triethyl, maintains the temperature of mixed system at 0～150 DEG C, in mixing process or after finishing, distills and can obtain triethyl-gallium.
Described gallium source can be selected from least one in gallium trichloride, tribromide gallium, triiodide gallium or tonsilon gallium;
Described aluminium triethyl is at least one in triethyl aluminum or diethylaluminum chloride;
Described inert atmosphere is at least one in nitrogen, argon gas or helium atmosphere;
The mol ratio of gallium source and aluminium triethyl is 1:1.05
-9.0, preferably 1:3～6;
Reaction times is 0.5～24 hour, preferably 4～8 hours;
Taking gallium as benchmark, the selectivity of triethyl-gallium is greater than 90%, and described triethyl-gallium purity is 80
-99.995%.
The present invention has following unusual effect compared with existing synthetic method:
(1) this synthetic method is not used any solvent, and two kinds of raw materials directly contact, and efficiency is high.
(2) in the process of mixing or after finishing, directly separate, selectivity and the yield of triethyl-gallium are high.
(3) this synthetic method adopts one-step synthesis, simplifies operational path, raises the efficiency.
(4) adopt present method can directly synthesize the triethyl-gallium of purity more than 95.0%.
Embodiment
Embodiment 1
Under nitrogen atmosphere, in reactor, add 880 grams of gallium trichlorides and 1710 grams of triethyl aluminums, maintain the temperature of mixed system at 80-90 DEG C, mix and directly distill after 1.0 hours, obtain 706 grams of triethyl-galliums, taking gallium as calculating benchmark, molar yield 90.1%.
Embodiment 2
Under helium atmosphere, in reactor, add 1547 grams of tribromide galliums and 3420 grams of triethyl aluminums, maintain the temperature of mixed system at 30-40 DEG C, mix and directly distill after 15.0 hours, obtain 721 grams of triethyl-galliums, taking gallium as calculating benchmark, molar yield 92.0%.
Embodiment 3
Under argon gas atmosphere, in reactor, add 880 grams of gallium trichlorides and 723 grams of diethylaluminum chlorides, maintain the temperature of mixed system at 120-130 DEG C, mix and directly distill after 9.0 hours, obtain 635 grams of triethyl-galliums, taking gallium as calculating benchmark, molar yield 81.0%.
Embodiment 4
Under argon gas atmosphere, in reactor, add 2252 grams of triiodide galliums and 1710 grams of triethyl aluminums, maintain the temperature of mixed system at 60-70 DEG C, mix and directly distill after 3.0 hours, obtain 604 grams of triethyl-galliums, taking gallium as calculating benchmark, molar yield 77.0%.
Embodiment 5
Under nitrogen atmosphere, in reactor, add 1547 grams of tribromide galliums and 2412 grams of diethylaluminum chlorides, maintain the temperature of mixed system at 10-20 DEG C, mix and directly distill after 24.0 hours, obtain 651 grams of triethyl-galliums, taking gallium as calculating benchmark, molar yield 83%.
Comparative example
Under argon gas atmosphere, in reactor, add 880 grams of gallium trichlorides, and add solvent dry toluene, under agitation condition, in reactor, drip 2850 grams of triethyl aluminums, control the speed dripping and make temperature of reaction system remain on 100 DEG C, after dropping finishes, continue reaction 4 hours.First normal pressure steams toluene, then carries out underpressure distillation, obtains 567 grams of triethyl-galliums, taking gallium trichloride as calculating benchmark, productive rate 72.3%.
Claims (8)
1. the synthetic method of a triethyl-gallium, it is characterized in that, comprise the steps: in the reactor of inert atmosphere, to add gallium source and aluminium triethyl, maintain the temperature of mixed system at 0～150 DEG C, in mixing process or after finishing, distill and can obtain triethyl-gallium.
2. the synthetic method of triethyl-gallium as claimed in claim 1, is characterized in that, described gallium source is selected from least one in gallium trichloride, tribromide gallium, triiodide gallium or tonsilon gallium.
3. the synthetic method of triethyl-gallium as claimed in claim 1, is characterized in that, described aluminium triethyl is at least one in triethyl aluminum or diethylaluminum chloride.
4. the synthetic method of triethyl-gallium as claimed in claim 1, is characterized in that, described inert atmosphere is at least one in nitrogen, argon gas or helium atmosphere.
5. the synthetic method of the triethyl-gallium as described in claim 1-4 any one, is characterized in that, the mol ratio of described gallium source and aluminium triethyl is 1:1.05
-9.0.
6. the synthetic method of triethyl-gallium as claimed in claim 1, is characterized in that, the reaction times is 0.5～24 hour.
7. the synthetic method of triethyl-gallium as claimed in claim 1, is characterized in that, described triethyl-gallium purity is 80
-99.995%.
8. the synthetic method of triethyl-gallium as claimed in claim 1, is characterized in that, taking gallium as benchmark, the selectivity of triethyl-gallium is greater than 90%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310036444.6A CN103965226A (en) | 2013-01-30 | 2013-01-30 | Triethyl gallium production method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310036444.6A CN103965226A (en) | 2013-01-30 | 2013-01-30 | Triethyl gallium production method |
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| CN103965226A true CN103965226A (en) | 2014-08-06 |
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| CN201310036444.6A Pending CN103965226A (en) | 2013-01-30 | 2013-01-30 | Triethyl gallium production method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105175438A (en) * | 2015-09-30 | 2015-12-23 | 江西佳因光电材料有限公司 | Preparation method of trimethylgallium |
| CN108822142A (en) * | 2018-09-03 | 2018-11-16 | 上海芯渊光电科技有限公司 | A kind of preparation method of triethyl-gallium |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040122248A1 (en) * | 2002-10-18 | 2004-06-24 | Shipley Company, L.L.C. | Preparation of organometal compounds |
| CN1572902A (en) * | 2003-06-19 | 2005-02-02 | 信越化学工业株式会社 | Preparation of high purity alkyl gallium |
| JP2009126835A (en) * | 2007-11-27 | 2009-06-11 | Ube Ind Ltd | High-purity trialkylgallium and method for producing the same |
-
2013
- 2013-01-30 CN CN201310036444.6A patent/CN103965226A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040122248A1 (en) * | 2002-10-18 | 2004-06-24 | Shipley Company, L.L.C. | Preparation of organometal compounds |
| CN1572902A (en) * | 2003-06-19 | 2005-02-02 | 信越化学工业株式会社 | Preparation of high purity alkyl gallium |
| JP2009126835A (en) * | 2007-11-27 | 2009-06-11 | Ube Ind Ltd | High-purity trialkylgallium and method for producing the same |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105175438A (en) * | 2015-09-30 | 2015-12-23 | 江西佳因光电材料有限公司 | Preparation method of trimethylgallium |
| CN108822142A (en) * | 2018-09-03 | 2018-11-16 | 上海芯渊光电科技有限公司 | A kind of preparation method of triethyl-gallium |
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Application publication date: 20140806 |
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