CN102390808A - Purifying and collecting system and method of germane-containing gases - Google Patents
Purifying and collecting system and method of germane-containing gases Download PDFInfo
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- CN102390808A CN102390808A CN2011102305320A CN201110230532A CN102390808A CN 102390808 A CN102390808 A CN 102390808A CN 2011102305320 A CN2011102305320 A CN 2011102305320A CN 201110230532 A CN201110230532 A CN 201110230532A CN 102390808 A CN102390808 A CN 102390808A
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Abstract
The invention discloses a purifying and collecting system and method of germane-containing gases. The method comprises the following steps of: condensing the germane-containing gases by using a condensing device; removing gases which are not condensed by the condensing device, by using an evacuating device; and injecting the germane-containing gases which are condensed and purified by the condensing device into a steel cylinder, by using a filling device. The purifying and collecting system and method of the germane-containing gases can be directly applied to purification and collection of gas products, such as germane and the like.
Description
Technical field
The present invention relates to the gas production technology field, particularly relate to a kind of purification gathering system and method that is used for Germane gas.
Background technology
In the process of the manufacturing of photovoltaic device and semiconducter device manufacturing, can use multiple reactant gases, for example when utilizing chemical vapor deposition (CVD) process deposits film.In the manufacturing processed of thin-film solar cells, also can use a large amount of silane (SiH
4) gas and germane (GeH
4) gas, utilize the various non-crystalline silicons of plasma enhanced chemical vapor deposition (PECVD) process deposits, microcrystal silicon and nano-silicon, amorphous germanium and amorphous silicon germanium thin film.
Germane is poisonous, inflammable and colourless gas.Under room temperature and barometric point, has distinctive irritating smell.In the germane production process, through also containing a spot of impurity in the gas after the multiple tracks removal of impurities operation, staple is hydrogen, germane, carbonic acid gas, helium, oxygen and nitrogen etc.In these mixed gass, need germane be separated with other gas, so that purified Germane gas bottling is delivered for use.Separating process should be safe and reliable efficiently controlled again, and how realizing separating safely and effectively is the problem that gas generation producer need solve.
Summary of the invention
The object of the present invention is to provide a kind of purification gathering system and method for Germane gas, the purification that can directly apply to gas products such as germane is collected.
The purification gathering system of Germane gas of the present invention comprises:
Condensing works carries out condensation to containing germane gas; With
Emptier is not with by the air scavenge of said condensing works condensation; And
Filling apparatus will be injected steel cylinder by the Germane gas that said condensing works condensation is purified.
Said condensing works comprises quench liquid storing containers and one or the cold-trap of a plurality of parallel connections being placed in one, and the said germane gas that contains gets into said cold-trap through valve and pipeline.
Series connection again after the cold-trap parallel connection of said a plurality of parallel connections.
Said emptier is a tail gas absorber.
Said filling apparatus comprises quench liquid storing containers and at least one steel cylinder that is placed in one, and said steel cylinder is connected with said condensing works with valve through pipeline.
Said steel cylinder is connected with said cold-trap with valve through pipeline.
Said system also comprises vacuum pump and vacuometer.
Said quench liquid comprises the mixture of liquid argon, liquid nitrogen or dry ice and Hydrocerol A.
The method of utilizing Germane gas purification gathering system that Germane gas is purified and collected of the present invention comprises step:
The mixed gas that will comprise Germane gas feeds in the condensing works, and germane is condensed in condensing works;
Other air scavenge of utilizing emptier not to be condensed;
Connect steel cylinder and steel cylinder is cooled off;
Condensing works is heated up, condensation in germane gasification wherein, and is injected steel cylinder.
Said method also comprises the step that system is vacuumized.
Description of drawings
Through the more specifically explanation of the preferred embodiments of the present invention shown in the accompanying drawing, above-mentioned and other purpose, characteristic and advantage of the present invention will be more clear.Reference numeral identical in whole accompanying drawings is indicated identical part.Painstakingly do not draw accompanying drawing in proportion, focus on illustrating purport of the present invention.
Fig. 1 is the structural representation of explanation core concept of the present invention;
Fig. 2 is the structural representation of optimum system choosing embodiment of the present invention.
Said diagrammatic sketch is schematically, and nonrestrictive, can not excessively limit protection scope of the present invention at this.
Embodiment
For make above-mentioned purpose of the present invention, feature and advantage can be more obviously understandable, does detailed explanation below in conjunction with the accompanying drawing specific embodiments of the invention.A lot of details have been set forth in the following description so that make much of the present invention.But the present invention can implement much to be different from alternate manner described here, and those skilled in the art can do similar popularization under the situation of intension of the present invention.Therefore the present invention does not receive the restriction of following disclosed specific embodiment.
Fig. 1 is the structural representation of explanation core concept of the present invention.As shown in Figure 1, the purification gathering system of Germane gas of the present invention comprises condensing works 10, is used for carrying out condensation to containing germane gas A; With emptier 20, tail gas absorber for example is used for not by the air scavenge of said condensing works condensation; And filling apparatus 30, will be injected steel cylinder by the Germane gas that said condensing works condensation is purified.Wherein, said condensing works comprises quench liquid storing containers and one or the cold-trap of a plurality of parallel connections being placed in one, and the said germane gas that contains gets into said cold-trap through valve and pipeline.
In one embodiment, series connection again after the cold-trap parallel connection of said a plurality of parallel connections.
Said filling apparatus comprises quench liquid storing containers and at least one steel cylinder that is placed in one, and said steel cylinder is connected with said condensing works with valve through pipeline.Said steel cylinder is connected with said cold-trap with valve through pipeline.Said system also comprises vacuum pump and vacuometer.Said quench liquid comprises the mixture of liquid argon, liquid nitrogen or dry ice and Hydrocerol A.
The method of utilizing above-mentioned Germane gas purification gathering system that Germane gas is purified and collected of the present invention, the mixed gas A that at first will comprise Germane gas feeds in the condensing works 10, and germane is condensed in condensing works 10; Other air scavenge of utilizing emptier (tail gas absorber) not to be condensed then; Connect steel cylinder and steel cylinder is cooled off; Condensing works is heated up, condensation in the gasification of wherein germane, and is injected steel cylinder.In one embodiment, said method also comprises the step that system is vacuumized.
Fig. 2 is the structural representation of optimum system choosing embodiment of the present invention.Do bright specifically below in conjunction with Fig. 2 to the present invention.As shown in Figure 2, structure according to a preferred embodiment of the invention comprises quench liquid storing containers 120 and 122, places the cold- trap 110 and 112 of said quench liquid storing containers 120, and the quantity of cold-trap can be one, also can be a plurality of, and present embodiment is two.And placing quench liquid storing containers 122 steel cylinder joining regions 130, the steel cylinder (not shown) is connected in the steel cylinder joining region 130.And tail gas absorber 140, vacuum pump 115, vacuometer 132, valve V1 to V8 and tensimeter 150 etc.Contain germane gas A and can get in cold- trap 110 and 120 through valve V8 and V3, cold-trap 110 is connected with steel cylinder joining region 130 with valve V4, V7 through pipeline with 120, and steel cylinder joining region 130 places quench liquid storing containers 122.Cold-trap 110 is connected with tail gas absorber 140 with valve V4, V5 through pipeline with 120; Vacuum pump 115 is connected with system with pipeline through valve V1; And be connected with vacuometer 132 with pipeline through V2, V6, can vacuumize system, and by vacuometer 132 supervision vacuum tightnesss.
Gas A staple through after the multiple working procedure removal of impurities is a large amount of hydrogen, germane; Traces of carbon dioxide, helium oxygen, nitrogen etc.During the reaction beginning, valve-off V1, V2, V6, V7 open valve V8, V3, V4, V5.Gas A flows via the direction of arrow among the figure, gets in the cold- trap 110 and 112, and germane is cooled, and other non-condensable gas flows to vent gas treatment tower 140 via V4, V5.
After reaction finished, valve-off V3, V5, V7, V8 opened valve V4, V6, V2, V1, and the reading that system is vacuumized up to vacuometer 132 is lower than certain value.
Then, valve-off V8, V1, V2, V5, V6 open valve V3, V4, V7, and open the cylinder valve of steel cylinder joining region 130.Quench liquid is put into quench liquid storing containers 122 to be cooled off steel cylinder.
Remove quench liquid storing containers 120 subsequently; Cold- trap 110 and 112 is exposed in the air, and cold- trap 110 and 112 is heated or ambient air accelerate to be flowed, the germane in the cold- trap 110 and 112 evaporates; Flow to steel cylinder through valve V4, V7, and condensation is in steel cylinder.After collecting end, close cylinder valve.
Cold-trap of the present invention can a plurality of parallel connections, and is as shown in Figure 2, also can carry out the multistage series connection after the parallel connection, to reach better cooling performance.The cold-trap number is decided according to temperature and the flow of gas A.The material of pipeline and valve is 316 stainless steels in the system; Cold-trap can be that 304 or 316 stainless steels etc. can bear certain pressure, again not with the material of germane reaction, and need heat conductivility preferably.The quench liquid of depositing in the quench liquid storing containers can be a liquid argon, the mixture of liquid nitrogen or dry ice and Hydrocerol A etc.The deep length of cold-trap inlet end pipe directly affects cooling performance, and length is relevant with germane output, and is also relevant with the kind of quench liquid in the quench liquid storing containers.If output is too high and pipe gos deep into the oversize pipe obstruction that causes easily, form dangerous; The formed cooling performance of different quench liquids is different, and pipe can be lacked relatively when therefore using the quench liquid of low temperature more.The diameter of cold-trap is relevant with temperature and the flow of gas A with length, and cooling performance is had direct influence.System of the present invention can connect safety guard above cold-trap, system is protected.
The above only is preferred embodiment of the present invention, is not the present invention is done any pro forma restriction.Any those of ordinary skill in the art are not breaking away under the technical scheme scope situation of the present invention, and all the technology contents of above-mentioned announcement capable of using is made many possible changes and modification to technical scheme of the present invention, or is revised as the equivalent embodiment of equivalent variations.Therefore, every content that does not break away from technical scheme of the present invention, all still belongs in the protection domain of technical scheme of the present invention any simple modification, equivalent variations and modification that above embodiment did according to technical spirit of the present invention.
Claims (10)
1. the purification gathering system of a Germane gas comprises:
Condensing works carries out condensation to containing germane gas; With
Emptier is not with by the air scavenge of said condensing works condensation; And
Filling apparatus will be injected steel cylinder by the Germane gas that said condensing works condensation is purified.
2. purification gathering system according to claim 1 is characterized in that: said condensing works comprises quench liquid storing containers and one or the cold-trap of a plurality of parallel connections being placed in one, and the said germane gas that contains gets into said cold-trap through valve and pipeline.
3. purification gathering system according to claim 2 is characterized in that: series connection again after the cold-trap parallel connection of said a plurality of parallel connections.
4. purification gathering system according to claim 1 is characterized in that: said emptier is a tail gas absorber.
5. purification gathering system according to claim 1 is characterized in that: said filling apparatus comprises quench liquid storing containers and at least one steel cylinder that is placed in one, and said steel cylinder is connected with said condensing works with valve through pipeline.
6. according to claim 2 or 5 described purification gathering systems, it is characterized in that: said steel cylinder is connected with said cold-trap with valve through pipeline.
7. purification gathering system according to claim 1 is characterized in that: said system also comprises vacuum pump and vacuometer.
8. according to claim 2 or 5 described purification gathering systems, it is characterized in that: said quench liquid comprises the mixture of liquid argon, liquid nitrogen or dry ice and Hydrocerol A.
9. method of utilizing the described Germane gas purification of claim 1 gathering system that Germane gas is purified and collected comprises step:
The mixed gas that will comprise Germane gas feeds in the condensing works, and germane is condensed in condensing works;
Other air scavenge of utilizing emptier not to be condensed;
Connect steel cylinder and steel cylinder is cooled off;
Condensing works is heated up, condensation in germane gasification wherein, and is injected steel cylinder.
10. method according to claim 9 is characterized in that: said method also comprises the step that system is vacuumized.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102305320A CN102390808A (en) | 2011-08-12 | 2011-08-12 | Purifying and collecting system and method of germane-containing gases |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102305320A CN102390808A (en) | 2011-08-12 | 2011-08-12 | Purifying and collecting system and method of germane-containing gases |
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| CN102390808A true CN102390808A (en) | 2012-03-28 |
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| CN2011102305320A Pending CN102390808A (en) | 2011-08-12 | 2011-08-12 | Purifying and collecting system and method of germane-containing gases |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102628546A (en) * | 2012-04-17 | 2012-08-08 | 南京特种气体厂有限公司 | Cold trap system for purifying and filling silane |
| WO2015084599A1 (en) * | 2013-12-06 | 2015-06-11 | Gelest Technologies, Inc. | Method for producing high purity germane by a continuous or semi-continuous process |
| CN106766675A (en) * | 2016-12-19 | 2017-05-31 | 清远先导材料有限公司 | The method and device of nitrogen is removed from special gas |
| CN108644612A (en) * | 2018-05-10 | 2018-10-12 | 江苏南大光电材料股份有限公司 | The collection device and its method of triethyl-gallium |
| CN111977613A (en) * | 2020-08-18 | 2020-11-24 | 博纯材料股份有限公司 | Digermane collecting and purifying equipment and safety control method, device and system thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723326A (en) * | 2009-12-18 | 2010-06-09 | 浙江理工大学 | Preparation method of germane |
| CN101955155A (en) * | 2010-06-07 | 2011-01-26 | 天津市泰源工业气体有限公司 | Technology for preparing germanium hydride by adopting sodium borohydride or potassium borohydride reduction germanium tetrachloride reaction |
-
2011
- 2011-08-12 CN CN2011102305320A patent/CN102390808A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723326A (en) * | 2009-12-18 | 2010-06-09 | 浙江理工大学 | Preparation method of germane |
| CN101955155A (en) * | 2010-06-07 | 2011-01-26 | 天津市泰源工业气体有限公司 | Technology for preparing germanium hydride by adopting sodium borohydride or potassium borohydride reduction germanium tetrachloride reaction |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102628546A (en) * | 2012-04-17 | 2012-08-08 | 南京特种气体厂有限公司 | Cold trap system for purifying and filling silane |
| WO2015084599A1 (en) * | 2013-12-06 | 2015-06-11 | Gelest Technologies, Inc. | Method for producing high purity germane by a continuous or semi-continuous process |
| US9174853B2 (en) | 2013-12-06 | 2015-11-03 | Gelest Technologies, Inc. | Method for producing high purity germane by a continuous or semi-continuous process |
| CN106766675A (en) * | 2016-12-19 | 2017-05-31 | 清远先导材料有限公司 | The method and device of nitrogen is removed from special gas |
| CN108644612A (en) * | 2018-05-10 | 2018-10-12 | 江苏南大光电材料股份有限公司 | The collection device and its method of triethyl-gallium |
| CN111977613A (en) * | 2020-08-18 | 2020-11-24 | 博纯材料股份有限公司 | Digermane collecting and purifying equipment and safety control method, device and system thereof |
| CN111977613B (en) * | 2020-08-18 | 2021-08-06 | 博纯材料股份有限公司 | Digermane collecting and purifying equipment and safety control method, device and system thereof |
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Address after: 362000, Fujian, Quanzhou province Yongchun County under the town of big glory Village Applicant after: Fujian Bochun Material Co., Ltd. Address before: The South Ring Road in Licheng District of Quanzhou City, Fujian province 362000 No. 1303 Jiangnan Hi-Tech Park of golden sun garden (Bo Chun) Applicant before: Fujian Bochun Material Co., Ltd. |
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Application publication date: 20120328 |