CN102218705B - Treatment method of gas cylinder used for storing electronic grade ultra-pure gas - Google Patents
Treatment method of gas cylinder used for storing electronic grade ultra-pure gas Download PDFInfo
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Abstract
The invention relates to a treatment method of a gas cylinder used for storing pure or ultra-pure gas, which has a strict demand upon the cleanness inside the gas cylinder. The method comprises the steps of: gas cylinder cleaning and drying, internal rust removing, re-cleaning, inner wall grinding, third-time cleaning, deionizing, and deep vacuuming and displacing. With the method provided by the present invention, impurities inside the gas cylinder can be removed, internal cleanness and draught of the gas cylinder can be maintained, and the gas cylinder satisfies the requirements of electronic grade ultra-pure gas storing.
Description
Technical field
The present invention relates to a kind of processing method of gas cylinder, such gas cylinder is mainly used in and fills high-purity, the ultra-pure gas of electron level, and processing finishes can be used to fill high-purity, the ultra-pure gas of electron level of 99.9999% above purity.
Background technology
Along with the continuous development of modern industry, all trades and professions to the demand of gas purity in continuous increase, industries such as light emitting semiconductor device LED, LCD LCD, photovoltaic SOLAR and integrated circuit microelectronics particularly.One of critical material that needs like electronics industry is exactly various high-purity, ultra-pure gas of based on very high purity; Because development ultra-large, ULSI; Requirement high-purity to these, ultra-pure gas is also more and more stricter; Not only require high-purityly, ultrapure, even also require ultra-clean in some special links.In the integrated circuit industry, from the preparation polysilicon to final annealing process, equal using gases in the whole process that IC makes, wide in variety and consumption is big.With the epitaxy technique is example, and the gas of use just comprises and contains Si gas, impurity gas, carries gas, reducing gas and drive gas.If contain the hydrocarbon of a few millionths or the impurity of oxygen in the gas, just on wafer, cause pit, influence the quality of later process.If contain the beavy metal impurity of parts per billion in the gas, will generate deposit, thereby cause the variation of circuit performance.The influence that very little spacing can increase impurity between the active circuit element reduces yield rate.Be to adapt to the megabit development of integrated circuits, need the circuit structure of micron and sub-micron, the total amount of trace impurity should be limited in 1ppm or still less in the gas.These gases generally all use gas cylinder to store, and the pollution of gas cylinder itself is very big to influence high-purity, ultra-pure gas purity.The contaminating impurity of gas cylinder comprises infiltration, absorption and chemical action etc.; And cleaning and degree of drying that gas cylinder is inner; Influence to gaseous mass also is very direct, thoroughly or with external environment has taken place to contact, has not perhaps cleaned for a long time if gas cylinder cleans, and obviously gas is stained easily.Such gas cylinder even charged into the high gas of purity, also can make the gas purity of output reduce because of the influence of gas cylinder internal contamination, even become substandard product to a certain extent.For this reason, produce qualified high-purity, ultra-pure gas, the processing that stores the gas cylinder of these gases is a precondition.
Summary of the invention
Goal of the invention of the present invention is to improve a kind of processing method of gas cylinder; Certain processing is carried out in inside to the gas cylinder of high-purity, ultra-pure gas to be filled; Thereby make it satisfy requirements such as bright and clean, clean, the no attachment of inner wall surface, drying, ion concentration be low, reduce gas cylinder greatly pollution high-purity, ultra-pure gas.
Goal of the invention of the present invention realizes through following technical scheme.
A kind of processing method that fills the gas cylinder of the ultra-pure gas of electron level, this method comprises the steps:
1) cleaning of gas cylinder, dried: the steel seamless gas cylinder that will newly buy uses the high pressure running water to wash processing; Mainly be to remove the inner corrosion thing of gas cylinder etc.; Utilize vapours to purge then the gas cylinder inwall is carried out dried, and remove the greasy dirt that inwall adheres to;
2) the inner impeller blasting of gas cylinder: utilize high pressure draught that the shot in the rust remover impeller head is sprayed in the gas cylinder inner surface, thereby remove gas cylinder inner wall oxide layer, field trash;
3) clean once more: the method for using step 1) is cleaning-drying once more, removes step 2) dirt that produces;
4) inwall grinds: utilize high density material, in its gas cylinder of packing into, the gas cylinder inwall is ground, thereby reach the purpose of best bright finish;
5) clean: utilize water under high pressure to clean, remove the dirt that step 4) produces.
6) deionization processing: use the high-purity de-ionized water that gas cylinder inside is cleaned, reduce the high problem of the inner ion concentration of gas cylinder thereby reach;
7) inner dry: as to use vapours to purge and carries out preliminarily dried, re-use heating constant-temperature equipment and gas cylinder is carried out inside dry processing, thereby reach the purpose of removing the inner traces of moisture of gas cylinder;
8) vacuum displacement is handled: the dry gas cylinder that finishes uses molecular pump vacuum unit that it is vacuumized processing; It is residual to extract the inner air of gas cylinder; And use the corresponding ultra-high purity dielectric gas that will fill to carry out replacement Treatment, thereby reach the purpose of removing inner other gaseous impurities of gas cylinder.
The invention has the beneficial effects as follows: removed inner impurity through the above-mentioned steps cylinder treated, guaranteed the clean and tidy and dry of its inside, satisfied the condition that fills gas cylinder as the ultra-pure gas of electron level.
The specific embodiment
Existing through the next better description of specific embodiment the present invention.
A kind of processing method that fills the gas cylinder of the ultra-pure gas of electron level, this method comprises the steps:
1) inner cleaning, the dried of gas cylinder: working pressure 6kg/cm
2Running water washes the steel seamless gas cylinder inside of newly buying, on one side flushing, rotate gas cylinder on one side; And use endoscope to check, till interior flushing to non-corroding thing, after flushing finishes; Utilize vapours to purge its inwall is carried out dried, make its inwall not have free profit and exist.Wherein said vapours purging needs to use following equipment: electric furnace, leaf formula air blast, hot blow support, endoscope and corresponding pipeline and temperature control instrument; When using vapours to purge gas cylinder, gas cylinder must be inverted, and the steel pipe that hot blow is used should insert gas cylinder l/2～2/3 place; The hot blow time is no less than 60min; The hot blow temperature is 70～80 ℃, and the vapours temperature is controlled at about 70～80 ℃, drives vapours with 2kg/cm with leaf formula air blast
2Pressure purges gas cylinder inside, and uses endoscope to check, till inner dry no water stain, oil stain.
2) the inner impeller blasting of gas cylinder: utilize high pressure draught that the shot in the rust remover impeller head is sprayed in the gas cylinder inner surface, thereby remove gas cylinder inner wall oxide layer, field trash; Rust remover must adopt bottom ball blast structure, and complete machine mainly is made up of body, impeller head, transmission device and four parts of dust arrester.Gas cylinder is rotation in a clockwise direction in shot-blasting machine, is applicable to oxide layer, the cleaning of powder sprayed coating, the rust cleaning of the various gas cylinders of diameter phi 220-φ 420mm.The rust remover important technological parameters:
Be suitable for the gas cylinder diameter range: φ 220 ~ φ 420mm
Bullet specification: φ 1.2 ~ φ 1.5mm, the about 120Kg of loadings.
Motor general power: 15.5KW
Driving motor: Y100L2-43KW
Ball blast motor: Y132S--4 2*5.5KW
Dedusting fan motor: Y90S one 2 1.5KW
Transmit road rotating speed: 47r/min
Impeller diameter: φ 320mm
Wheel speed: 2440r/min
3) clean once more: the method for using step 1) is cleaning-drying once more, removes step 2) dirt that produces.
4) gas cylinder is inner grinds: step is following:
1. before this gas cylinder inside was roughly ground: the cubical high-density milling material of packing in the gas cylinder, above-mentioned grinding-material are the porcelain bodies that purity reaches the artificial sintering of aluminium oxide more than 99.9%; This grinding-material is of a size of about 2mm, and the ratio of gas cylinder container and this grinding-material use amount is the grinding-material that every 1L volume needs 0.5kg, and corresponding volume is the gas cylinder of 40L, and use amount is 20kg; The gas cylinder that installs abrasive is placed on the gas cylinder tourelle, and gas cylinder moves in the direction of the clock earlier on tourelle, and the time is 2 hours, rotation counter clockwise again, and the time also is 2 hours, accomplishes corase grind.
2. fine grinding is carried out in gas cylinder inside: corase grind finishes the back fine grinding is being carried out in gas cylinder inside, and the grinding-material that uses during fine grinding is the porcelain ball that purity reaches the artificial sintering of silica more than 99.9%; The diameter of the porcelain ball of the artificial sintering of this silica is about 2mm, and the ratio of gas cylinder container and this grinding-material use amount is the grinding-material that every 1L volume needs 0.75kg, is the gas cylinder of 40L for volume; Use amount 30kg is placed on the gas cylinder of the porcelain ball that installs the artificial sintering of this silica on the gas cylinder tourelle, and gas cylinder moves in the direction of the clock earlier on tourelle; Time is 2 hours; Rotation counter clockwise again, the time also is 2 hours, accomplishes fine grinding.Fineness through the gas cylinder inwall after grinding can reach 0.2 μ m;
1. step packs into behind the gas cylinder with the grinding-material of step described in 2., uses thread forms as the Plastic cap of PZ27.8 the gas cylinder valve seat to be stopped up, and prevents that grinding-material from spilling; Step 1. with the gas cylinder tourelle of step described in 2. can by clockwise with rotation counterclockwise; Motor drives is arranged, slow down through decelerator, speed reducing ratio is 1:30; The rotating speed of gas cylinder tourelle is 40r/min, and each tourelle can be placed 4～8 gas cylinders simultaneously.
5) to clean gas cylinder inner for water under high pressure: with the high pressure running water gas cylinder inside being washed once more, mainly is to clean above-mentioned steps 4) metal dust and the impurity of generation when grinding.
6) deionization processing: use the high-purity de-ionized water that gas cylinder inside is cleaned, solve the high problem of the inner ion concentration of gas cylinder thereby reach, this high-purity deionized water resistivity should reach 18M Ω;
7) inner dry: the gas cylinder that uses de-ionized water to clean should drain free water, re-uses the vapours purging and carries out drying, and the drying that vapours purges is preliminary drying; In order to reach high dry, must put into temperature drying device to gas cylinder and carry out long time drying processing, temperature should be controlled at about 110 ℃; Drying time generally continues about 4 hours, because the gas cylinder of handling mainly is used to fill high-purity, ultra-pure gas, gas cylinder valve is all selected diaphragm valve for use; The valve of this valve and other types relatively; Air-tightness is best, and mounted diaphragm valve causes the damage of valve diaphragm easily under the temperature about 110 ℃; Gas cylinder is when needs carry out high dry; Temperature drying device should partly expose gas cylinder valve, and uses low power fan to aim at the valve position and lower the temperature, and prevents the damage of diaphragm valve.
8) vacuum displacement is handled: the gas cylinder of process high dry is after the oven dry certain hour; The operation that must carry out is to vacuumize and use to fill gas medium displacement three times; The device that uses is a molecular pump vacuum unit, and it carries out vacuum " slightly taking out " by preposition sliding vane rotary pump, and the vacuum limit of this moment can reach 10pa; And then open molecular pump and carry out " carefully taking out ", the vacuum limit of " carefully taking out " through molecular pump can reach 10
-5Pa, the purpose that vacuumizes is the hot-air that extracts in the gas cylinder, keeps the inner vacuum of gas cylinder, avoid airborne oxygen and moisture entrapment to fill " pollution " of eminence, ultra-pure gas.And be about about 110 ℃ through the oven dry gas cylinder temperature of certain hour, the vacuum that under this higher temperature, is extracted is about 10
-5Pa, when the temperature of gas cylinder was reduced to environment temperature, the limit of its vacuum one magnitude that can descend again at least reached 10
-6Pa, thus air pollution better avoided.But because air has certain " viscosity ", though handle through high vacuum, appointing so has the air-polluting space; Therefore need to use the ultra-high purity dielectric gas that will fill that it is replaced; The displacement number of times is 3 times, displacement pressure position 0.5Mpa, and replacement procedure is following:
1. use and treat that accordingly the ultra-high purity dielectric gas that will fill is forced into 0.5Mpa to gas cylinder, should purge application of vacuum to connecting pipeline earlier this moment;
2. emptying is carried out application of vacuum to gas cylinder and connection pipeline again to normal pressure;
3. reuse and treat that accordingly the ultra-high purity dielectric gas that will fill is forced into 0.5Mpa to gas cylinder;
4. emptying is carried out application of vacuum to gas cylinder and connection pipeline again to normal pressure once more;
5. use for the third time and treat that accordingly the ultra-high purity dielectric gas that will fill is forced into 0.5Mpa to gas cylinder;
6. emptying is for the third time carried out application of vacuum to gas cylinder and connection pipeline again to normal pressure;
7. be forced into 0.5Mpa the 4th time, promptly we are referred to as pressurize, and it is to be filled that such gas cylinder gets final product etc.;
Through above step 1)～8) processing, it is whole that to be used to fill gas cylinder treatment process high-purity, ultra-pure gas just complete, real satisfy filling needs high-purity, ultra-pure gas.
Claims (1)
1. a processing method that fills the gas cylinder of the ultra-pure gas of electron level is characterized in that this method comprises the steps:
1) cleaning of gas cylinder, dried: the steel seamless gas cylinder that will newly buy uses the high pressure running water to wash processing; Mainly be to remove the inner corrosion thing of gas cylinder; Utilize vapours to purge then the gas cylinder inwall is carried out dried, and remove the greasy dirt that inwall adheres to;
2) the inner impeller blasting of gas cylinder: utilize high pressure draught that the shot in the rust remover impeller head is sprayed in the gas cylinder inner surface, thereby remove gas cylinder inner wall oxide layer, field trash;
3) clean once more: the method for using step 1) is cleaning-drying once more, removes step 2) dirt that produces;
4) inwall grinds: utilize high density material, in its gas cylinder of packing into, the gas cylinder inwall is ground, thereby reach the purpose of best bright finish;
5) clean: utilize water under high pressure to clean, remove the dirt that step 4) produces;
6) deionization processing: use the high-purity de-ionized water that gas cylinder inside is cleaned, reduce the high problem of the inner ion concentration of gas cylinder thereby reach;
7) inner dry: as to use vapours to purge and carries out preliminarily dried, re-use heating constant-temperature equipment and gas cylinder is carried out inside dry processing, thereby reach the purpose of removing the inner traces of moisture of gas cylinder;
8) vacuum displacement is handled: the dry gas cylinder that finishes uses molecular pump vacuum unit that it is vacuumized processing; It is residual to extract the inner air of gas cylinder; And use the corresponding ultra-high purity dielectric gas that will fill to carry out replacement Treatment, thereby reach the purpose of removing inner other gaseous impurities of gas cylinder.
2. the processing method that fills the gas cylinder of the ultra-pure gas of electron level as claimed in claim 1; When it is characterized in that using in the described step 1) vapours to purge the gas cylinder inwall, gas cylinder must be inverted, and the steel pipe that hot blow is used should insert gas cylinder l/2～2/3 place; The hot blow time is no less than 60min; The hot blow temperature is 70～80 ℃, and the vapours temperature is controlled at 70～80 ℃, and vapours is with 2kg/cm
2Pressure purges gas cylinder inside, and uses endoscope to check, till inner dry no water stain, oil stain.
3. the processing method that fills the gas cylinder of the ultra-pure gas of electron level as claimed in claim 1 is characterized in that the gas cylinder inwall is ground described in the step 4) comprised following two steps:
1. gas cylinder inside is roughly ground: the cubical high-density milling material of packing in the gas cylinder; This grinding-material is the porcelain body that purity reaches the artificial sintering of aluminium oxide more than 99.9%, and this grinding-material is of a size of 2mm, and the ratio of gas cylinder container and this grinding-material use amount is the grinding-material that every 1L volume needs 0.5kg; The gas cylinder that installs this grinding-material is placed on the gas cylinder tourelle; Gas cylinder moves in the direction of the clock earlier on tourelle, and the time is 2 hours, again rotation counter clockwise; Time also is 2 hours, accomplishes corase grind;
2. fine grinding is carried out in gas cylinder inside: corase grind carries out fine grinding to gas cylinder inside after finishing again, and the grinding-material that uses during fine grinding is the porcelain ball that purity reaches the artificial sintering of silica more than 99.9%, and the diameter of the porcelain ball of the artificial sintering of this silica is 2mm; The ratio of gas cylinder container and this grinding-material use amount is this grinding-material that every 1L volume needs 0.75kg; The gas cylinder of the porcelain ball that installs the artificial sintering of this silica is placed on the gas cylinder tourelle, and gas cylinder moves in the direction of the clock earlier on tourelle, and the time is 2 hours; Rotation counter clockwise again; Time also is 2 hours, accomplishes fine grinding, and the fineness of the gas cylinder inwall after process is ground reaches 0.2 μ m.
4. the processing method that fills the gas cylinder of the ultra-pure gas of electron level as claimed in claim 1 is characterized in that described the vacuumizing with the dielectric gas replacement Treatment of step 8) need carry out three times at least, and replacement procedure is following:
1. use and treat that accordingly the ultra-high purity dielectric gas that will fill is forced into 0.5Mpa to gas cylinder, should purge application of vacuum to connecting pipeline earlier this moment;
2. emptying is carried out application of vacuum to gas cylinder and connection pipeline again to normal pressure;
3. reuse and treat that accordingly the ultra-high purity dielectric gas that will fill is forced into 0.5Mpa to gas cylinder;
4. emptying is carried out application of vacuum to gas cylinder and connection pipeline again to normal pressure once more;
5. use for the third time and treat that accordingly the ultra-high purity dielectric gas that will fill is forced into 0.5Mpa to gas cylinder;
6. emptying is for the third time carried out application of vacuum to gas cylinder and connection pipeline again to normal pressure;
7. be forced into 0.5Mpa the 4th time, promptly we are referred to as pressurize, and it is to be filled that such gas cylinder gets final product etc.
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| 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 |
| CN105215835A (en) * | 2015-09-07 | 2016-01-06 | 浙江陶特容器科技有限公司 | The grinding technics of high-purity and ultrapure electronic chemical product container |
| 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 |
| KR102012794B1 (en) * | 2018-03-07 | 2019-11-04 | 주식회사 엔케이 | Cylinder treatment method for ultra-high purity gas filling |
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| CN111469042A (en) * | 2020-04-16 | 2020-07-31 | 浙江西亚特电子材料有限公司 | Gas cylinder processing system and processing method for ultrapure gas |
| CN114737180A (en) * | 2022-04-21 | 2022-07-12 | 苏州金宏气体股份有限公司 | Treatment process for high-purity deuterium gas storage steel cylinder |
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| US5759360A (en) * | 1995-03-13 | 1998-06-02 | Applied Materials, Inc. | Wafer clean sputtering process |
| US5779807A (en) * | 1996-10-29 | 1998-07-14 | Applied Materials, Inc. | Method and apparatus for removing particulates from semiconductor substrates in plasma processing chambers |
| JPH11286023A (en) * | 1998-04-03 | 1999-10-19 | Ulvac Corp | Method and apparatus for plasma cleaning |
| TW503123B (en) * | 2000-09-08 | 2002-09-21 | Boc Group Inc | Plasma drying and passivation of compressed gas cylinders |
| CN100549227C (en) * | 2008-04-01 | 2009-10-14 | 南京特种气体厂有限公司 | A kind of method for processing internal wall of ultrapure silane gas cylinder |
| CN101913581B (en) * | 2010-07-15 | 2012-05-30 | 首钢总公司 | Method for preparing ultra-high purity gas by combining liquid pump with raw material gas cylinder |
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Address after: 215152 Anmin Road, Panyang Industrial Park, Huangdai Town, Xiangcheng District, Suzhou City, Jiangsu Province Patentee after: Jinhong Gas Co.,Ltd. Address before: No. 6, Anmin Road, Panyang Industrial Park, Huangdai Town, Xiangcheng District, Suzhou City, Jiangsu Province, 215000 Patentee before: SUZHOU JINHONG GAS Co.,Ltd. |