CN100549227C - A kind of method for processing internal wall of ultrapure silane gas cylinder - Google Patents

A kind of method for processing internal wall of ultrapure silane gas cylinder Download PDF

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Publication number
CN100549227C
CN100549227C CNB2008100246805A CN200810024680A CN100549227C CN 100549227 C CN100549227 C CN 100549227C CN B2008100246805 A CNB2008100246805 A CN B2008100246805A CN 200810024680 A CN200810024680 A CN 200810024680A CN 100549227 C CN100549227 C CN 100549227C
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gas cylinder
inwall
qualified
silane
days
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CNB2008100246805A
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CN101250704A (en
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林培川
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NANJING SPECIAL GAS FACTORY CO Ltd
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NANJING SPECIAL GAS FACTORY CO Ltd
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Abstract

The invention discloses a kind of method for processing internal wall of ultrapure silane gas cylinder, its step is as follows: the inwall polishing: add the deionized water polishing with quartz sand; With splanchnoscopy gas cylinder inwall, rust scar and rough surface can not be arranged.Adopt washed with de-ionized water gas cylinder internal surface, the specific conductivity≤0.1uS/cm after cleaning is qualified; Be inverted gas cylinder, pour out a bottle interior residual water; The zinc-plated nickel composite deposite of inwall; Clean inwall again; With the gas cylinder oven dry, gas cylinder is evacuated to≤10Pa; Charge into 6N High Purity Hydrogen to 3~4MPa, place the water content of measuring gas in the gas cylinder after 24 hours ,≤0.5ppm is qualified; Bleed off hydrogen, be evacuated to≤1Pa, can silane was placed more than 10 days, analyzed every foreign matter content, particularly water content≤2ppm in the silane; 30 days, analyze once more after 60 days, as every impurity index no change, then dispose.

Description

A kind of method for processing internal wall of ultrapure silane gas cylinder
Technical field
The present invention relates to a kind of method for processing internal wall of gas cylinder of splendid attire electronic gas, the method for processing internal wall of especially ultrapure silane gas cylinder.
Technical background
Gas cylinder has multiple material to make, and the most frequently used have carbon steel and aluminium alloy gas cylinder, a gas cylinder that also has stainless steel to make.The gas cylinder that is used for the splendid attire electronic gas abroad relates to the gas cylinder through special processing of patented technology more, such as the steel cylinder of the ULTRAPURE high pressure of Praxair and the stainless steel cylinder of low pressure, ULTRACLEAN special processing, FIBRALUME aluminium alloy bottle etc.; The UNIQUAL steel cylinder of method liquid air etc.The domestic wall anode oxidation that also grown up, nickel-zinc plating alloy layer, be coated with fluorine material, bonderizing or the like, but major part is used for the splendid attire of various calibrating indicating instrument gases, does not see the method for processing internal wall that is used for electronic gas splendid attire gas cylinder in the prior art.The wall anode oxidation is primarily aimed at aluminium alloy gas cylinder, and is not suitable for steel tank; Being coated with the fluorine material mainly is to be coated with fluorine-containing material, can bring fluoride pollution; Though bonderizing can be used for the surface protection of steel material, bring phosphide to pollute equally, and because the porousness of its phosphate coating, the planar water activity gas that grades can bring new source of pollution easily.So, adopting electronic gas such as steel tank splendid attire silane, " ion " impurity of gas cylinder inwall is mainly to consider the object removed.
Summary of the invention
Technical problem to be solved by this invention is to fill up the blank of prior art, and a kind of method for processing internal wall of ultrapure silane gas cylinder is provided.
The method for processing internal wall of a kind of ultrapure silane gas cylinder of the present invention, its step is as follows:
1, inwall polishing: the gas cylinder of handling is removed cylinder valve, be positioned on the gas cylinder roller press of rotation, add the deionized water polishing with quartz sand; Pour out quartz sand and deionized water;
2, inwall inspection: with splanchnoscopy gas cylinder inwall, clean rust scar and the rough surface of polishing, end can not be arranged, if any then returning step 1, otherwise enter step 3.
3, inwall cleans: adopt washed with de-ionized water gas cylinder internal surface, the specific conductivity≤0.1uS/cm after cleaning is qualified; Be inverted gas cylinder, pour out a bottle interior residual water;
4, inwall nickel plating: the zinc-plated nickel composite deposite of inwall; 3 clean inwall set by step again;
5, gas cylinder oven dry: inwall is cleaned qualified gas cylinder load onto cylinder valve, put into 105~110 ℃ vacuum drying oven, gas cylinder is evacuated to≤10Pa;
6, result inspection: the gas cylinder that vacuum-drying is qualified, charge into 6N High Purity Hydrogen to 3~4MPa, place the water content of measuring gas in the gas cylinder after 24 hours ,≤0.5ppm is qualified; Defective, bleed off hydrogen, return step 4 operation, qualified till;
7, bleed off hydrogen, be evacuated to≤1Pa, can silane was placed more than 10 days, and every foreign matter content, particularly water content are wanted≤2ppm in the analysis silane; 30 days, analyze once more after 60 days, as every impurity index no change, then dispose; Otherwise, return step 5.
The inventive method, the gas cylinder splendid attire high purity silane that adopts this law to handle, can not introduce " ion " sources such as metallic compound, adopt washed with de-ionized water, can avoid bringing into above-mentioned " ion " said, inwall polishing, nickel plating alloy layer can be avoided foreign gases such as gas cylinder inwall planar water, guarantee the purity and the permanent stability of high purity silane.
Description of drawings
Fig. 1 is the inventive method schematic process flow diagram;
Embodiment
Below in conjunction with accompanying drawing the present invention is described in further details.
Embodiment: as shown in Figure 1, the method for processing internal wall of a kind of ultrapure silane gas cylinder of the present invention, its step is as follows:
1, inwall polishing: the gas cylinder of handling is removed cylinder valve, be positioned on the gas cylinder roller press of rotation, put into gas cylinder, add deionized water 10~15kg and rotate gas cylinder, polished 3~4 hours with quartz sand 4~6kg of diameter 6~8mm.Pour out quartz sand and deionized water (as being the oil-containing gas cylinder, after then cleaning with benzene, acetone, alcohol solvent in advance, clean up with deionized water, the oil-containing gas cylinder that suggestion does not clean up does not use).
2, inwall inspection: with splanchnoscopy gas cylinder inwall, the rust scar and the rough surface of not polishing clean can not be arranged, if any, polishing is again checked once more.
3, inwall cleans: adopt washed with de-ionized water gas cylinder internal surface, the specific conductivity≤0.1uS/cm after cleaning is qualified (noting the influence of Carbon Dioxide in Air during measurement).Be inverted gas cylinder 30~60 minutes, and poured out a bottle interior residual water.
4, inwall nickel plating: the zinc-plated nickel composite deposite of inwall.3 clean inwall set by step again.
5, gas cylinder oven dry: inwall is cleaned qualified gas cylinder load onto cylinder valve, put into 105~110 ℃ vacuum drying oven, gas cylinder is evacuated to≤10Pa.
6, result inspection: the gas cylinder that vacuum-drying is qualified, charge into 6N High Purity Hydrogen to 3~4MPa, place the water content of measuring gas in the gas cylinder after 24 hours ,≤0.5ppm is qualified.Defective, bleed off hydrogen, return step 4 operation, qualified till.
7, bleed off hydrogen, be evacuated to≤1Pa, can silane was placed more than 10 days, and every foreign matter content, particularly water content are wanted≤2ppm in the analysis silane.30 days, analyze once more after 60 days, there is not considerable change as every impurity index, prove that gas cylinder inwall treatment effect is good, gas cylinder can be used for the splendid attire high purity silane.Otherwise, return step 5, handle again.

Claims (2)

1, a kind of method for processing internal wall of ultrapure silane gas cylinder, its step is as follows:
A, inwall polishing: the gas cylinder of handling is removed cylinder valve, be positioned on the gas cylinder roller press of rotation, add the deionized water polishing with quartz sand; Pour out quartz sand and deionized water;
B, inwall inspection: with splanchnoscopy gas cylinder inwall, the rust scar and the rough surface of not polishing clean can not be arranged, if any then returning steps A, otherwise enter step C.
C, inwall clean: adopt washed with de-ionized water gas cylinder internal surface, the specific conductivity≤0.1uS/cm after cleaning is qualified; Be inverted gas cylinder, pour out a bottle interior residual water;
D, inwall nickel plating: the zinc-plated nickel composite deposite of inwall; C cleans inwall set by step again;
E, gas cylinder oven dry: inwall is cleaned qualified gas cylinder load onto cylinder valve, put into 105~110 ℃ vacuum drying oven, gas cylinder is evacuated to≤10Pa;
F, result inspection: the gas cylinder that vacuum-drying is qualified, charge into 6N High Purity Hydrogen to 3~4MPa, place the water content of measuring gas in the gas cylinder after 24 hours ,≤0.5ppm is qualified; Defective, bleed off hydrogen, return step D operation, qualified till;
G, bleed off hydrogen, be evacuated to≤1Pa, can silane was placed more than 10 days, analyzed every foreign matter content, particularly water content≤2ppm in the silane; 30 days, analyze once more after 60 days, as every impurity index no change, then dispose; Otherwise, return steps A.
2, according to the method for processing internal wall of the described a kind of ultrapure silane gas cylinder of claim 1, it is characterized in that: steps A, inwall polishing: the gas cylinder of handling is removed cylinder valve, be positioned on the gas cylinder roller press of rotation, quartz sand 4~6kg with diameter 6~8mm puts into gas cylinder, add deionized water 10~15kg rotation gas cylinder, polished 3~4 hours; Pour out quartz sand and deionized water.
CNB2008100246805A 2008-04-01 2008-04-01 A kind of method for processing internal wall of ultrapure silane gas cylinder Expired - Fee Related CN100549227C (en)

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Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101922004A (en) * 2010-08-20 2010-12-22 南京特种气体厂有限公司 Method for treating inner wall of high-pressure seamless steel gas cylinder
CN102218705B (en) * 2011-04-01 2012-10-31 苏州金宏气体股份有限公司 Treatment method of gas cylinder used for storing electronic grade ultra-pure gas
CN104458145B (en) * 2014-12-22 2017-03-01 洛阳双瑞特种装备有限公司 A kind of gas cylinder inner surface cleaning filling high-purity gas and quality determining method
CN106002640A (en) * 2016-06-06 2016-10-12 洛阳双瑞特种装备有限公司 Forming method of large-volume high-purity industrial gas bottle type steel container
CN106002644A (en) * 2016-06-06 2016-10-12 洛阳双瑞特种装备有限公司 Treatment method for inner surface of steel high pressure gas cylinder for high purity gas

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
低浓度SO2标准气包装容器的研究. 金花子等.低温与特气,第21卷第2期. 2003
低浓度SO2标准气包装容器的研究. 金花子等.低温与特气,第21卷第2期. 2003 *

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