CN100460745C - Method of storing nitrogen trifluoride - Google Patents

Method of storing nitrogen trifluoride Download PDF

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Publication number
CN100460745C
CN100460745C CNB2005100482999A CN200510048299A CN100460745C CN 100460745 C CN100460745 C CN 100460745C CN B2005100482999 A CNB2005100482999 A CN B2005100482999A CN 200510048299 A CN200510048299 A CN 200510048299A CN 100460745 C CN100460745 C CN 100460745C
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China
Prior art keywords
container
gas
chrome
molybdenum
steel container
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Expired - Fee Related
Application number
CNB2005100482999A
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Chinese (zh)
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CN1880830A (en
Inventor
饭久保佑一
张香子
金大铉
金哲虎
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Ulsan Chemical Co Ltd
Foosung Co Ltd
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Foosung Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L5/00—Gas handling apparatus
    • B01L5/02—Gas collection apparatus, e.g. by bubbling under water
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/22—Ferrous alloys, e.g. steel alloys containing chromium with molybdenum or tungsten
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L5/00—Gas handling apparatus
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
    • C01B21/083—Compounds containing nitrogen and non-metals and optionally metals containing one or more halogen atoms
    • C01B21/0832—Binary compounds of nitrogen with halogens
    • C01B21/0835—Nitrogen trifluoride

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Clinical Laboratory Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Filling Or Discharging Of Gas Storage Vessels (AREA)
  • Packging For Living Organisms, Food Or Medicinal Products That Are Sensitive To Environmental Conditiond (AREA)
  • Nitrogen Condensed Heterocyclic Rings (AREA)

Abstract

The method of storing nitrogen trifluoride includes storing nitrogen trifluoride in a chromium-molybdenum steel vessel manufactured through a deep drawing ironing process. Nitrogen trifluoride stored in this way according to the method of this invention does not deteriorate even after two years or more have passed.

Description

The method of storing nitrogen trifluoride
Technical field
A kind of storing nitrogen trifluoride (NF of relate generally to of the present invention 3) method, particularly, the present invention relates to a kind of use and flatten moulding by deep-draw (deep drawing ironing, DDI) the chrome-molybdenum steel container of explained hereafter is stored NF 3The method of gas.
Background technique
In the sheet metal forming field, a kind of technology of using Production of Stamping Die to have the hydrostatic column of airtight bottom is called DDI technology.
Press tool is a kind of machining tool, and it comprises the element up and down (drift and mould) that a pair of tool carbon steel or alloy tool steel are made.Mould is installed on the press bed, and with sheet material location be fixed on the press bed.Then, when drift was pressed to sheet material, sheet material was stamped, and was shaped to the cylindrical shell of cup-shaped hydrostatic column thus, and is as a whole thereby bottom surface and sidewall surfaces are combined into.The open top of the container that the sealing said method is produced, and injection port place mounted valve thereon, thus a high-pressure bottle that is used for gas storage finished.
DDI technology is also referred to as plug drawing.
As a kind of etchant that is used to produce semiconductor devices, NF 3Gas is a kind of chemical product of costliness.Direct reaction by fluorine gas and ammonia can prepare NF 3Gas also can pass through hydrofluorination ammonium (NF 4HF 2) and the reaction of fluorine gas, or electrolyzing fused hydrofluorination ammonium prepares NF 3Gas.In general, provide NF to the user 3Be by it being prepared into highly purified liquid, in the container of the 20～50L that packs into then, making it be in the pressurized gas state.
In addition, because NF 3As the etchant of producing semiconductor devices, must be highly purified therefore, purity is 99.99% or higher.
At present, semiconductor technology needs NF 3The purity level that gas has is 3ppm or N still less 2, 3ppm or O still less 2, 1ppm or CO still less 2, 20ppm or CF still less 4, 1ppm or H still less 2O, 1ppm or N still less 2O and 1ppm or HF still less.
Therefore, as a kind of high reaction activity gas, NF 3Should be stored in the special container, to avoid at storage or cyclic process mesometamorphism.
As storing NF 3Gas containers is used the manganese steel container usually.The manganese steel container is the manganese steel pipe experience hot briquetting that contains 0.5～1.5% manganese element by making, and with production cylindrical seal container, the container that will produce like this polishes and cleaning then.
NF as routine 3Storage container will be through the polishing treatment of inner surface of container so that the roughness of internal surface (Ra) be less than or equal to after the 10 μ m, and through cleaning-drying in a vacuum so that after inner impurity removed fully, the manganese steel container just can be used.
Yet roughness is less than or equal to 10 μ m and inside does not have impurity even the manganese steel container is processed into, if overlong time is stored in NF wherein 3Still can show acidity, cause NF 3Rotten.
Although not clear NF 3The rotten reason of cutter really, but can infer that this comes from the negative effect of impurity, this impurity are the oxide (Fe of the iron that exists in the container xO y), water and oxygen.Can determine that acidifying is mainly caused by nitric acid.
Following reaction equation has shown NF in storage container 3Evolution path to nitric acid.
2NF 3+Fe 2O 3+H 2O+O 2→2HNO 3+2FeF 3
2NF 3+2FeO+H 2O+3/2O 2→2HNO 3+2FeF 3
Present NF 3The common acceptable NF of gas generation merchant and user 3Standard in, only determined the acidity of HF, and determined the acidity that nitric acid produces that nitric acid is very difficult controlled like this.
And, because the NF from be stored in the manganese steel container 3In can detect nitric acid, can think that this used container is unsuitable for storing NF 3
Therefore, NF 3User and manufacturer press for a kind of improved storage NF 3Method so that through storing for a long time NF 3Also undergo no deterioration.
Summary of the invention
The present invention is to NF 3Draw on the storage procedures research basis extensively and profoundly, find: be stored in by the NF in the chrome-molybdenum steel container of DDI explained hereafter 3Even through also undergoing no deterioration for a long time, has NF in the conventional manganese steel container of the roughness (Ra) that is less than or equal to 10 μ m and be stored in by the polishing inner surface of container 3Can and go bad with impurity reaction, though this impurity comprises through such process treating the still iron filings and the water of the trace that exists owing to the coarse inner vein of conventional vessel.
Therefore, the purpose of this invention is to provide a kind of storage NF 3Method, even through long time stored, NF 3Also undergo no deterioration.
The invention provides a kind of chrome-molybdenum steel container and store NF with the DDI explained hereafter 3The method of gas.
The gas that is used for semiconductor technology need have very high purity, and purity increases along with the increase of semiconductor level of integration.Therefore, need strict control to store such gas containers.Usually, the container that is used to store high-pure gas needs polishing treatment, making its roughness (Ra) be less than or equal to 10 μ m pollutes with water and the impurity particle that prevents to be stored in gas in the container and be adhered to inner surface of container, and then, remove the impurity of internal tank through in a vacuum cleaning and drying process.Yet although storage container is handled through above-mentioned strictness, effect is still undesirable, and this is because storage NF wherein 3Can acidifying gradually.The inventor has realized that the NF that is stored in the conventional manganese steel container 3Gas can develop into and comprise NO xImpurity, and its acidity (pH) can increase, and replaces NF in the container that manganese steel produces and be stored in by DDI technology with chrome-molybdenum steel 3Can keep high pure state, its acidity can not increase yet.That is to say, even its internal surface of conventional manganese steel container is through retrofit and thorough cleaning-drying, long time stored NF wherein 3Gas also can go bad, and forms acidic materials.Finally, gas can be detected and show acid pH.Yet, work as NF 3Gas storage detects less than pollutant in by in the chrome-molybdenum steel container of DDI explained hereafter the time, and stores for a long time that gas also undergoes no deterioration.Therefore, find that such chrome-molybdenum steel container is suitable as NF 3The storage container of gas.This is because employed chrome-molybdenum steel is the form of sheet material, and becomes chrome-molybdenum steel container rather than common manganese steel container employed tubing form by the DDI processes.Especially, the chrome-molybdenum steel container has uniform surface, and under the situation that does not have extra inter-process, its roughness (Ra) is less than or equal to 5 μ m, and this container material and processing technology with the manganese steel container is different.And if the internal surface of chrome-molybdenum steel container process is handled, this chrome-molybdenum steel container can preferably have the roughness (Ra) less than 1 μ m.Although use the internal surface of the manganese steel container of manganese steel tubing production to handle through abundant, the impurity as water or granule is difficult to remove fully from the micro-gap of container.In addition, the NF in the said vesse 3Can undesirable reaction take place with the iron filings in the gap that is exposed to inner surface of container, generate ferric flouride, this ferric flouride is then by catalysis, to quicken NF 3Decomposition, N like this 2The amount of O or acid ingredient will increase.In addition, in the container of producing with the chromium-molybdenum steel plate by DDI technology, through compacting and moulding, it is very fine and close that the inner vein of steel plate becomes, and like this, the composition of steel almost all is in same state, as through oversintering.And the internal surface of chrome-molybdenum steel container is even without through inner treatment process also being equal even cleanings.Can believe that this is because the micro-gap in the chrome-molybdenum steel such as the gap of internal surface are littler than manganese steel, remove inner impurity easily like this.And, along with the minimizing of iron filings and trace impurity quantity, avoided NF 3The decomposition of gas.
Embodiment
The present invention may be better understood by the following examples, this embodiment only for illustrative purposes, should not be construed as this is limitation of the present invention.
Ammonia and fluorine gas are added in the melt of hydrofluorination ammonium, prepare impure NF 3Gas.The gas purification of preparation is like this become the highly purified liquid phase NF of low temperature 3, in storage container, collect the NF of gas phase then 3In manganese steel container and the chrome-molybdenum steel container made by DDI technology, load the NF that 20Kg collects respectively 3Gas.Each container is placed under the room temperature, and detect NF in time 3The pH value of gas changes.Employed manganese steel container contains the manganese of 1.5wt%, and employed chrome-molybdenum steel container contains 1.5wt% chromium and 0.5wt% molybdenum.Analyze N with gas chromatograph (Valco, PDD detector) 2The content of O.In addition, analyze HNO in the following way 3: determine total acidity by the NaOH acid-base titration, from total acidity, deduct the amount of HF, convert end value to HNO again 3Amount.With the amount of F ion analyser detection HF, with sulfuric acid and FeSO 4By the negative ion qualitative analysis to confirm HNO 3Existence.Provide in result's table 1 and 2 below, wherein Ra is the measured value of inner surface of container.
Table 1
The acidity of gas in the storage container
Storage container Storage capacity (Kg) PH (color test)
Manganese steel (47L, Ra:25 μ m) 20 PH7 → pH3 (after 2 days)
Manganese steel (47L, Ra:10 μ m) 20 PH7 → pH5 (after 6 months)
Chrome-molybdenum steel (DDI) 20 PH7 → pH7 (after 2 years)
* the manganese of manganese steel: 1.5wt%
The chromium of chrome-molybdenum steel: 1.5wt% and the molybdenum of 0.5wt%
Table 2
Gas component after 6 months
Storage container HF (ppm) HNO 3 (ppm) N 2O (ppm) PH (color test)
Manganese steel (Ra:25 μ m) 0.418 3.339 1 3
Manganese steel (Ra:10 μ m) 0.022 1.816 Trace 5
Chrome-molybdenum steel (DDI) 0.004 0.932 Do not detect 7
* the manganese of manganese steel: 1.5wt%
The chromium of chrome-molybdenum steel: 1.5wt% and the molybdenum of 0.5wt%
Although in the manganese steel container, can detect acid in time, in 2 years or longer time, detect less than variation in the chrome-molybdenum steel container.And roughness is less than or equal to the gas that the manganese steel container of 10 μ m causes and decomposes well below the manganese steel container of roughness more than or equal to 25 μ m, but it decomposes the chrome-molybdenum steel container that still is higher than by the DDI explained hereafter.
Shown in gas component analysis result in the table 2, be stored in the gas of manganese steel container, nitric acid and fluoric acid content can slightly increase, and therefore show that the color of pH changes.Should be noted that the N in the gas that is stored in the manganese steel container in time 2O content can increase, even and for a long time, be stored in by the gas in the chrome-molybdenum steel container of DDI explained hereafter and also undergo no deterioration, can keep high pure state.Therefore, in the present invention, can confirm to contain the container that the chrome-molybdenum steel of 1.5～2.0wt% chromium and 0.2～0.5wt% molybdenum makes and be suitable for storing NF 3
By foregoing description as can be known, the invention provides a kind of storage NF 3Method.Therefore, according to the NF of method caching of the present invention 3Gas is even also undergo no deterioration through 2 years or longer time.
Though, for illustrative purposes, the preferred embodiment of the invention is disclosed, but, those skilled in the art should fully understand, under the prerequisite of scope that does not deviate from claims disclosure of the present invention and essence, have various improvement, replenish and substitute.

Claims (1)

1. the method for a storing nitrogen trifluoride comprises Nitrogen trifluoride is stored in the chrome-molybdenum steel container that adopts deep-draw pressing explained hereafter that wherein the chrome-molybdenum steel container is to be made by the chrome-molybdenum steel that contains 1.5～2.0wt% chromium and 0.2～0.5wt% molybdenum.
CNB2005100482999A 2005-06-14 2005-11-25 Method of storing nitrogen trifluoride Expired - Fee Related CN100460745C (en)

Applications Claiming Priority (2)

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KR1020050050668 2005-06-14
KR1020050050668A KR100660444B1 (en) 2005-06-14 2005-06-14 Storage method of Nitrogen trifluoride

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CN100460745C true CN100460745C (en) 2009-02-11

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US (1) US20060280642A1 (en)
JP (1) JP2006349171A (en)
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CN (1) CN100460745C (en)
DE (1) DE102005060954B4 (en)
IT (1) ITBO20060030A1 (en)

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4578113A (en) * 1983-05-19 1986-03-25 Union Carbide Corporation High strength steel
JPH04114910A (en) * 1990-08-31 1992-04-15 Mitsui Toatsu Chem Inc Production of nitrogen trifluoride gas
US5133928A (en) * 1989-10-28 1992-07-28 Chesterfield Cylinders Limited Cylinder body of a steel composition
JP2003232495A (en) * 2002-02-07 2003-08-22 Mitsui Chemicals Inc Charged high-purity high-pressure gas
JP2004025025A (en) * 2002-06-25 2004-01-29 Japan Pionics Co Ltd Agent and method for purifying gas containing nitrogen fluoride
CN1558869A (en) * 2001-09-28 2004-12-29 秘密股份公司(阿斯托电子) Method for producing nitrogen trifluoride
US20050006011A1 (en) * 2002-02-15 2005-01-13 Benteler Automobiltechnik Gmbh Use of a steel alloy for making tubes to produce compressed gas containers or for making formed structures in light weight steel construction
JP4114910B2 (en) * 2000-11-30 2008-07-09 現代自動車株式会社 Shift control method for automatic transmission for vehicle

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE737556C (en) * 1935-01-06 1943-07-19 Hoesch Ag Chromium-molybdenum-iron alloy for corrosion-resistant objects, the production of which requires a high level of deep-drawing ability
JP3068216B2 (en) * 1990-12-28 2000-07-24 東北特殊鋼株式会社 High cold forging electromagnetic stainless steel
JP2933826B2 (en) * 1994-07-05 1999-08-16 川崎製鉄株式会社 Chromium steel sheet excellent in deep drawing formability and secondary work brittleness and method for producing the same
TW336257B (en) * 1996-01-30 1998-07-11 Daido Hoxan Inc A method of carburizing austenitic stainless steel and austenitic stainless steel products obtained thereby
JP3116038B2 (en) * 1999-03-10 2000-12-11 三井化学株式会社 Inner surface treatment method for high pressure gas container
KR100428906B1 (en) * 2001-11-05 2004-04-29 주식회사 소디프신소재 Method for preparing of filling cylinder of highly pure nitrogen trifluoride(nf3) by treating the inner side of filling cylinder and filling cylinder prepared by the method
JP3107715U (en) * 2004-09-13 2005-02-03 中国工業株式会社 High pressure gas container

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4578113A (en) * 1983-05-19 1986-03-25 Union Carbide Corporation High strength steel
US5133928A (en) * 1989-10-28 1992-07-28 Chesterfield Cylinders Limited Cylinder body of a steel composition
JPH04114910A (en) * 1990-08-31 1992-04-15 Mitsui Toatsu Chem Inc Production of nitrogen trifluoride gas
JP4114910B2 (en) * 2000-11-30 2008-07-09 現代自動車株式会社 Shift control method for automatic transmission for vehicle
CN1558869A (en) * 2001-09-28 2004-12-29 秘密股份公司(阿斯托电子) Method for producing nitrogen trifluoride
JP2003232495A (en) * 2002-02-07 2003-08-22 Mitsui Chemicals Inc Charged high-purity high-pressure gas
US20050006011A1 (en) * 2002-02-15 2005-01-13 Benteler Automobiltechnik Gmbh Use of a steel alloy for making tubes to produce compressed gas containers or for making formed structures in light weight steel construction
JP2004025025A (en) * 2002-06-25 2004-01-29 Japan Pionics Co Ltd Agent and method for purifying gas containing nitrogen fluoride

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CN1880830A (en) 2006-12-20
DE102005060954A1 (en) 2006-12-28
DE102005060954B4 (en) 2008-07-31
KR20060130281A (en) 2006-12-19
KR100660444B1 (en) 2006-12-22
JP2006349171A (en) 2006-12-28
ITBO20060030A1 (en) 2006-12-15
US20060280642A1 (en) 2006-12-14

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