CN101955155A - Technology for preparing germanium hydride by adopting sodium borohydride or potassium borohydride reduction germanium tetrachloride reaction - Google Patents
Technology for preparing germanium hydride by adopting sodium borohydride or potassium borohydride reduction germanium tetrachloride reaction Download PDFInfo
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- CN101955155A CN101955155A CN2010101925656A CN201010192565A CN101955155A CN 101955155 A CN101955155 A CN 101955155A CN 2010101925656 A CN2010101925656 A CN 2010101925656A CN 201010192565 A CN201010192565 A CN 201010192565A CN 101955155 A CN101955155 A CN 101955155A
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Abstract
The invention discloses a technology for preparing germanium hydride by adopting a sodium borohydride or potassium borohydride reduction germanium tetrachloride reaction, which is mainly characterized in that an electromagnetic stirrer is connected with the lower part of a reaction bottle; a No.2 dropping funnel, a No.1 dropping funnel and a condenser are connected with the upper part of the reaction bottle; and the condenser is formed by successively assembling a sampling bottle, a mercury manometer, an air collection bottle and a connecting pipe of a vacuum pump through the connecting pipe. The invention has the advantages of reasonable design and convenient use, and is an ideal technology for preparing high-purity germanium hydride.
Description
Affiliated technical field
The present invention relates to a kind of Chemicals-high-purity germanium hydride preparation method's Technology, particularly a kind of technology that adopts sodium borohydride or potassium borohydride reduction germanium tetrachloride prepared in reaction germanium hydride is suitable for the synthesizing hydrogenated germanium of chemical industry.
Background technology
At present, at present, microelectronics is the main foundation stone of modern information technologies and military technique, is to promote one of scientific-technical progress, industry development, economic liftoff and social progressive key factor.Unicircuit is the core of microelectronics, and its developmental level and industry size have become the important symbol of weighing a national economic strength.Electronics special gas (as germanium hydride), especially high pure electronic gas are the important factors of restriction IC reliability and yield rate as this new class of electronics chemical materials.Along with the develop rapidly of electronic information technology, integrated level is more and more higher, and 5N level (99.999%) has been brought up in the purity requirement of basic raw material (as germanium hydride), even more than the 7N, therefore preparing high pure electronic special gas technology more seems extremely urgent.The technology of preparing of germanium hydride is imperfect as yet, the making method complex process, difficult the grasp, the product of producing still can not satisfy the needs of associated electrical product comprehensively, and of poor quality, problem is many, can only be used to make the product of low specification, therefore, brought bigger trouble to the user, this situation has seriously restricted development of electronic technology.
Summary of the invention
Problem to be solved by this invention is, overcomes the deficiencies in the prior art, and a kind of technology that adopts sodium borohydride or potassium borohydride reduction germanium tetrachloride prepared in reaction germanium hydride is provided.This technology not only technology is reasonable, and preparation is simple, and good product quality, and the germanium hydride purity of production is up to more than the 5N (99.999%), and has solved problem of environmental pollution.
The technical solution used in the present invention is: connection magnetic stirrer under the reaction flask, connect 2# dropping funnel, 1# dropping funnel, condenser on it, condenser by pipe connecting and sampling jug, mercury manometr, air collector, connect the vacuum pump pipe connecting and be assembled into one in proper order and constitute.
The present invention all adopts stainless material to make assembling.
Adopting special pure germanium tetrachloride and purity is 96.5% sodium borohydride or POTASSIUM BOROHYDRIDE, puts into a certain amount of germanium tetrachloride in the 2# dropping funnel, and the aqueous solution of the hydroborate of new preparation is put into homothermic reaction flask and 1# dropping funnel.With vacuum pump the air in the system is taken out.Then the germanium tetrachloride in the 2# dropping funnel is added in the hydroborate solution, use the magnetic stirrer stirred solution simultaneously.The a small amount of germanium tetrachloride that remains on the 2# dropping funnel wall washes with the hydroborate solution in the 1# dropping funnel.Reaction product is collected in the air collector, with mercury manometry pressure.
After reaction finished, the mixing germanium hydride of generation imported in the air collector that soaks in filling the vacuum jacketed flask of liquid nitrogen.Germanium hydride condenses in air collector, and hydrogen is put into atmosphere, and reaction changes germanium hydride the stainless steel cylinder over to from air collector after finishing, and adds and depresses with liquid storage, and technology is reasonable, makes simply, is the desirable technique of germanium hydride preparation.
The invention has the beneficial effects as follows, reasonable in design, easy to use, be ideal germanium hydride fabricating technology.
Description of drawings
The present invention is further described below in conjunction with drawings and Examples.
Fig. 1 is a structural representation of the present invention.
Accompanying drawing number is: 1, reaction flask, 2, magnetic stirrer, 3, the 2# dropping funnel, 4, the 1# dropping funnel, 5, condenser, 6, sampling jug, 7, air collector, 8, mercury manometr, 9, connect the vacuum pump pipe connecting, 10, pipe connecting.
Embodiment
With reference to Fig. 1, reaction flask (1) is connection magnetic stirrer (2) down, connect 2# dropping funnel (3), 1# dropping funnel (4), condenser (5) on it, condenser (5) by pipe connecting (10) and sampling jug (6), mercury manometr (8), air collector (7), connect vacuum pump pipe connecting (9) and be assembled into one in proper order and constitute.
The present invention all adopts stainless material to make assembling.
Adopting special pure germanium tetrachloride and purity is 96.5% sodium borohydride or POTASSIUM BOROHYDRIDE, puts into a certain amount of germanium tetrachloride in 2# dropping funnel (3), and the aqueous solution of the hydroborate of new preparation is put into homothermic reaction flask (1) and 1# dropping funnel (4).With vacuum pump the air in the system is taken out, then the germanium tetrachloride in the 2# dropping funnel (3) is added in the hydroborate solution, use magnetic stirrer (2) stirred solution simultaneously.The a small amount of germanium tetrachloride that remains on 2# dropping funnel (3) wall washes with the hydroborate solution in the 1# dropping funnel (4).Reaction product is collected in the air collector (7), with mercury manometr (8) measuring stress.
After reaction finished, the mixing germanium hydride of generation imported in the air collector that soaks in filling the vacuum jacketed flask of liquid nitrogen (7).Germanium hydride condenses in air collector (7), and hydrogen is put into atmosphere, and reaction changes germanium hydride the stainless steel cylinder over to from air collector (7) after finishing, and adds and depresses with liquid storage, and technology is reasonable, makes simply, is the desirable technique of germanium hydride preparation.
Claims (1)
1. technology that adopts sodium borohydride or potassium borohydride reduction germanium tetrachloride prepared in reaction germanium hydride, it is characterized in that: connection magnetic stirrer under the reaction flask, connect 2# dropping funnel, 1# dropping funnel, condenser on it, condenser by pipe connecting and sampling jug, mercury manometr, air collector, connect the vacuum pump pipe connecting and be assembled into one in proper order and constitute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101925656A CN101955155A (en) | 2010-06-07 | 2010-06-07 | Technology for preparing germanium hydride by adopting sodium borohydride or potassium borohydride reduction germanium tetrachloride reaction |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101925656A CN101955155A (en) | 2010-06-07 | 2010-06-07 | Technology for preparing germanium hydride by adopting sodium borohydride or potassium borohydride reduction germanium tetrachloride reaction |
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| CN101955155A true CN101955155A (en) | 2011-01-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2010101925656A Pending CN101955155A (en) | 2010-06-07 | 2010-06-07 | Technology for preparing germanium hydride by adopting sodium borohydride or potassium borohydride reduction germanium tetrachloride reaction |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249188A (en) * | 2011-05-21 | 2011-11-23 | 南京中锗科技股份有限公司 | Preparation method of germane gas |
| CN102390808A (en) * | 2011-08-12 | 2012-03-28 | 福建博纯材料有限公司 | Purifying and collecting system and method of germane-containing gases |
-
2010
- 2010-06-07 CN CN2010101925656A patent/CN101955155A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249188A (en) * | 2011-05-21 | 2011-11-23 | 南京中锗科技股份有限公司 | Preparation method of germane gas |
| CN102249188B (en) * | 2011-05-21 | 2012-12-26 | 南京中锗科技股份有限公司 | Preparation method of germane gas |
| CN102390808A (en) * | 2011-08-12 | 2012-03-28 | 福建博纯材料有限公司 | Purifying and collecting system and method of germane-containing gases |
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Open date: 20110126 |