JP6914918B2 - 材料、この材料を用いた保存容器、この保存容器に取り付けられるバルブ、並びに、ClFの保存方法、ClFの保存容器の使用方法 - Google Patents
材料、この材料を用いた保存容器、この保存容器に取り付けられるバルブ、並びに、ClFの保存方法、ClFの保存容器の使用方法 Download PDFInfo
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- JP6914918B2 JP6914918B2 JP2018510288A JP2018510288A JP6914918B2 JP 6914918 B2 JP6914918 B2 JP 6914918B2 JP 2018510288 A JP2018510288 A JP 2018510288A JP 2018510288 A JP2018510288 A JP 2018510288A JP 6914918 B2 JP6914918 B2 JP 6914918B2
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- Prior art keywords
- storage container
- clf
- valve
- gold
- gas
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000003860 storage Methods 0.000 title claims description 47
- 239000000463 material Substances 0.000 title claims description 24
- 238000000034 method Methods 0.000 title claims description 15
- 239000007789 gas Substances 0.000 claims description 122
- 238000002161 passivation Methods 0.000 claims description 46
- 238000007789 sealing Methods 0.000 claims description 23
- 230000003647 oxidation Effects 0.000 claims description 13
- 238000007254 oxidation reaction Methods 0.000 claims description 13
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 9
- 239000010931 gold Substances 0.000 claims description 9
- 229910052737 gold Inorganic materials 0.000 claims description 9
- 238000007747 plating Methods 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 4
- 229910000990 Ni alloy Inorganic materials 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 229910000838 Al alloy Inorganic materials 0.000 claims description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 3
- 229910000531 Co alloy Inorganic materials 0.000 claims description 3
- 229910000617 Mangalloy Inorganic materials 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- OMRRUNXAWXNVFW-UHFFFAOYSA-N fluoridochlorine Chemical compound ClF OMRRUNXAWXNVFW-UHFFFAOYSA-N 0.000 description 86
- 238000012360 testing method Methods 0.000 description 47
- 239000010408 film Substances 0.000 description 45
- 238000010926 purge Methods 0.000 description 29
- 230000007797 corrosion Effects 0.000 description 27
- 238000005260 corrosion Methods 0.000 description 27
- 238000002474 experimental method Methods 0.000 description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 239000011261 inert gas Substances 0.000 description 10
- 238000012856 packing Methods 0.000 description 10
- 230000008859 change Effects 0.000 description 9
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 7
- 239000011737 fluorine Substances 0.000 description 7
- 229910052731 fluorine Inorganic materials 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
- 230000006837 decompression Effects 0.000 description 5
- 238000011049 filling Methods 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000003682 fluorination reaction Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 239000004973 liquid crystal related substance Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 101100441092 Danio rerio crlf3 gene Proteins 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 210000004907 gland Anatomy 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 229920002493 poly(chlorotrifluoroethylene) Polymers 0.000 description 2
- -1 polychlorotrifluoroethylene Polymers 0.000 description 2
- 239000005023 polychlorotrifluoroethylene (PCTFE) polymer Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 230000002250 progressing effect Effects 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- KNSWNNXPAWSACI-UHFFFAOYSA-N chlorine pentafluoride Chemical compound FCl(F)(F)(F)F KNSWNNXPAWSACI-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005429 filling process Methods 0.000 description 1
- 229910052743 krypton Inorganic materials 0.000 description 1
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 description 1
- 229910000734 martensite Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- JOHWNGGYGAVMGU-UHFFFAOYSA-N trifluorochlorine Chemical compound FCl(F)F JOHWNGGYGAVMGU-UHFFFAOYSA-N 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C1/00—Pressure vessels, e.g. gas cylinder, gas tank, replaceable cartridge
- F17C1/10—Pressure vessels, e.g. gas cylinder, gas tank, replaceable cartridge with provision for protection against corrosion, e.g. due to gaseous acid
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
- C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
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- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
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- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/10—Oxidising
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F16K1/02—Lift valves or globe valves, i.e. cut-off apparatus with closure members having at least a component of their opening and closing motion perpendicular to the closing faces with screw-spindle
- F16K1/04—Lift valves or globe valves, i.e. cut-off apparatus with closure members having at least a component of their opening and closing motion perpendicular to the closing faces with screw-spindle with a cut-off member rigid with the spindle, e.g. main valves
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16K—VALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
- F16K1/00—Lift valves or globe valves, i.e. cut-off apparatus with closure members having at least a component of their opening and closing motion perpendicular to the closing faces
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- F16K1/301—Lift valves or globe valves, i.e. cut-off apparatus with closure members having at least a component of their opening and closing motion perpendicular to the closing faces specially adapted for pressure containers only shut-off valves, i.e. valves without additional means
- F16K1/303—Lift valves or globe valves, i.e. cut-off apparatus with closure members having at least a component of their opening and closing motion perpendicular to the closing faces specially adapted for pressure containers only shut-off valves, i.e. valves without additional means with a valve member, e.g. stem or shaft, passing through the seat
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F16K1/32—Details
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- F16K1/36—Valve members
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F16K—VALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
- F16K31/00—Actuating devices; Operating means; Releasing devices
- F16K31/44—Mechanical actuating means
- F16K31/50—Mechanical actuating means with screw-spindle or internally threaded actuating means
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F16K—VALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
- F16K31/00—Actuating devices; Operating means; Releasing devices
- F16K31/44—Mechanical actuating means
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F16K—VALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F17C13/00—Details of vessels or of the filling or discharging of vessels
- F17C13/04—Arrangement or mounting of valves
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
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- F17C2203/06—Materials for walls or layers thereof; Properties or structures of walls or their materials
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
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Description
そして、特許文献1には、フッ素系ガスとして、ClF3(三フッ化塩素)を半導体製造装置のクリーニングに使用する技術が開示されている。
好ましくは、前記金メッキ層は酸化処理が施されてなる。
好ましくは、前記不動態被膜は前記金メッキ層に形成されてなる。
好ましくは、前記弁体は、ディスク型である。
好ましくは、前記弁体は、ダイヤフラムである。
好ましくは、前記不動態被膜は、ClF 3 及びF 2 からなる群より選択される1つ以上のガスとさらに接触してなる。
好ましくは、前記材料は、マンガン鋼、ステンレス鋼、クロムモリブデン鋼、ニッケル合金、アルミニウム合金、コバルト合金、金、及び樹脂の少なくとも1つに前記不動態被膜を形成してなる。
図1は、本発明の一実施形態に係る材料を用いたガスボンベ2の一部断面図である。ガスボンベ2は、ClFを保存するための耐圧性を有する保存容器であって、上部に開口4を有する器壁6、開口4に装着された円筒状の口金8、口金8に装着されたバルブ10などを備えている。
・使用ガス:ClFのみ、或いは、ClFに、ClF3及びF2からなる群より選択される1つ以上をさらに含むガス(ベースガスとして、N2(窒素)、その他の不活性ガスを混合しても良い)
・使用ガスのClF濃度:1重量%〜100重量%程度
・処理時間(使用ガスの接触時間):6時間以上
・処理温度:10℃〜100℃程度
・処理圧力:0MPaG〜0.1MPaG程度
ClFの濃度は、高い方が不動態被膜28を迅速に形成可能であるとともに、不動態被膜28の膜質が強固となる。また、処理時間は、長い方が不動態被膜28の膜質が強固となる。なお、接ガス時間とは、使用ガスが接ガスした瞬間からカウントされる時間である。
<充填工程:S1>
先ず、ステップS1では、不動態被膜28が形成された使用可能状態のガスボンベ2の内部にClFを含むガス(以下、単にClF、或いは保存ガスと称する)を充填して保存する。具体的には、バルブ10の開状態で、バルブ10の横接続部12bに図示しない保存ガス供給源を接続し、保存ガスをガスボンベ2に導入する。保存ガスの充填後には、バルブ10を閉として保存ガスをガスボンベ2内に密封保存する。
次に、ステップS2では、保存ガスが充填されたガスボンベ2を保存ガスの使用先まで搬送して使用する。具体的には、バルブ10の横接続部12bに図示しない保存ガス供給先を接続してバルブ10を開とし、保存ガスをガスボンベ2から流出させて保存ガス供給先に供給する。保存ガスの使用後には、バルブ10を閉としてガスボンベ2を使用先から回収する。
次に、ステップS3では、回収したガスボンベ2のバルブ10の横接続部12bに図示しないパージ装置を接続する。そして、パージ装置によりガスボンベ2を真空引きにより減圧しながらガスボンベ2内に微量に残留した保存ガスを排出した後、ガスボンベ2に不活性ガスを充填する。
<実験1>
バルブ10の弁体18を想定したテストピースに金メッキ層を形成し、表1に示すように、金メッキ層の層厚、金メッキ層に対する封孔処理、酸化処理の有無を変えることにより、これら変化がClFの耐久性に影響する度合いをテストピースの重量変化、表面腐食度、金メッキ層剥離の有無を指標として確認した。なお、表面腐食度は、テストピースの重量変化、表面積、実験時間から算出している。このため、金メッキ層の腐食によりテストピースの重量が減少した場合には負の値となる。また、ここでいう腐食とは、金メッキ層にフッ化物、或いは塩化物が形成されたり、或いは浸透したりし、その結果、金メッキ層が変色したり、或いは、金メッキ層が剥離する現象を含めて定義している。
・金メッキ層の層厚:7.3〜8.4μm
・金メッキ層に対する封孔処理:無し
・金メッキ層に対する酸化処理:無し
となるテストピースに対してClFの圧張り試験を実施した結果、
・テストピースの重量変化:0.009%増加
・テストピースの表面腐食度:0.0014 mg/cm2・h
との結果を得て、最終的に
・テストピースからの金メッキ層の剥離:無し
となり、合格であった。
・金メッキ層の層厚:2.5〜2.6μm
・金メッキ層に対する封孔処理:有り
・金メッキ層に対する酸化処理:無し
となるテストピースに対してClFの圧張り試験を実施した結果、
・テストピースの重量変化:0.002%増加
・テストピースの表面腐食度:0.0003 mg/cm2・h
との結果を得た。金メッキ層に封孔処理を施すことにより、実施例1の場合に比して、金メッキ層の層厚は約1/3に薄いものの、テストピースの重量変化、表面腐食度の双方とも約1/4に低減することができ、ClFによる金メッキ層の腐食を大幅に抑制することができた。従って、最終的に、
・テストピースからの金メッキ層の剥離:無し
となり、合格であった。
・金メッキ層の層厚:2.5〜2.6μm
・金メッキ層に対する封孔処理:無し
・金メッキ層に対する酸化処理:有り
となるテストピースに対してClFの圧張り試験を実施した結果、
・テストピースの重量変化:0.014%増加
・テストピースの表面腐食度:0.0021 mg/cm2・h
との結果を得た。金メッキ層に酸化処理を施すことにより、実施例1の場合に比して、金メッキ層の層厚は約1/3に薄いものの、テストピースの重量変化、表面腐食度の双方とも約1.5倍に増加した。これは、金メッキ層の表面に酸化被膜が形成されたためであるが、この酸化被膜によりClFによる金メッキ層の腐食は抑制される。従って、最終的に、
・テストピースからの金メッキ層の剥離:無しとなり、
合格であった。
・金メッキ層の層厚:2.5〜2.6μm
・金メッキ層に対する封孔処理:無し
・金メッキ層に対する酸化処理:無し
となるテストピースに対してClFの圧張り試験を実施した結果、
・テストピースの重量変化: 0.005%減少
・テストピースの表面腐食度:-0.0008 mg/cm2・h
との結果を得た。この場合、テストピースの重量は減少し、テストピースの表面腐食度は負の値となっているため、金メッキ層の腐食が進行している。そして、最終的に、
・テストピースからの金メッキ層の剥離:有り
となった。しかし、本例での金メッキ層の剥離は微量であり、後述する実験2でのリーク試験の結果、リークは発生しないことが判明したため、合格の判定を行った。
・金メッキ層の層厚:0.3μm
・金メッキ層に対する封孔処理:無し
・金メッキ層に対する酸化処理:無し
となるテストピースに対してClFの圧張り試験を実施した結果、
・テストピースの重量変化: 0.009%減少
・テストピースの表面腐食度:-0.0014 mg/cm2・h
との結果を得た。この場合、テストピースの重量は減少し、テストピースの表面腐食度は負の値となっているため、金メッキ層の腐食が進行している。そして、最終的に、
・テストピースからの金メッキ層の剥離:有り
となり、不合格であった。
ガスボンベ2にClFを充填し、図示しない実験用バルブを閉とした状態で、表2に示すように、バルブ10又はニードル弁を2000回開閉する実験を3回行った。その後、ガスボンベ2から実験用バルブを取り外し、ガスボンベ2からClFを排出した後、ガスボンベ2のサイクルパージを行った。その後、ガスボンベ2にHe(ヘリウム)を充填し、ガスボンベ2にHeリークディテクターを接続し、リークレートを測定した。
・弁体:ディスク型
・1回目リークレート:3.3×10-9Pa・m3/sec
・2回目リークレート:2.7×10-9Pa・m3/sec
・3回目リークレート:3.1×10-9Pa・m3/sec
との結果を得て、何れの測定も
・リーク:無し
となり、合格であった。
・弁体:ニードル型
・1回目リークレート:1.3×10-8Pa・m3/sec
・2回目リークレート:1.2×10-4Pa・m3/sec
・3回目リークレート:1.0×10-3Pa・m3/sec以上
との結果を得て、1回目の測定は
・リーク:無し
であり、2回目及び3回目の測定は、
・リーク:有り
となったため、最終的に不合格であった。
表3に示すように、テストピースにClFによる不動態化処理と、F2による不動態化処理とを以下の条件で実施したとき、不動態被膜の膜厚に差が見られるかどうかを測定した。
・使用ガスのClF濃度:1重量%〜100重量%程度
・処理時間(使用ガスの接触時間):6時間以上
・処理温度:10℃〜100℃程度
・処理圧力:0MPaG〜0.1MPaG程度
テストピースに形成されたF2による不動態被膜の膜厚は8nmであり、同一条件での不動態化処理で、2倍の膜厚の不動態被膜が形成された。
このように実験3では、ClFによる不動態化処理により、より薄膜の不動態被膜を形成することができるため、例えば、バルブ10の弁体18、弁座16、ディスクパッキン24などに、摩擦の影響を受けにくく、バルブ10の閉止性能に極力影響を与えない薄膜の不動態被膜28を形成可能である。従って、ClFによる不動態化処理がClFの保存、取り扱いにおいて有効であることを確認することができた。
ガスボンベ2にClFを充填し、その後にガスボンベ2からClFを流出させてガスボンベ2の使用後の状態を形成する。バルブ10が閉の状態で、バルブ10の本体12の横接続部12bに図示しない実験用バルブ、図示しないパージ装置を順次接続する。そして、実験用バルブを開とし、パージ装置によりガスボンベ2を−0.1MPaGまで真空引きにより減圧保持(60秒)し、ガスボンベ2内に微量に残留したClFを排出した後、ガスボンベ2に窒素を充填する。
・サイクルパージ回数:100
・減圧保持時間:60秒
のときは、
・ClF検知:無し
であり、合格であった。
・サイクルパージ回数:50
・減圧保持時間:60秒
のときは、
・ClF検知:有り(2ppm以上)
であり、不合格であった。
・サイクルパージ回数:70
・減圧保持時間:60秒
のときは、
・ClF検知:有り(2ppm以上)
であり、不合格であった。
例えば、ガスボンベ2に限らず、種々の部材や装置の材料の少なくとも一部に不動態被膜28を形成すれば、当該材料に接触したClFのフッ化反応を少なくとも抑制可能である。
6a 内面
10 バルブ
14 流路
16 弁座
18 弁体
18a シール面
26 金メッキ層
28 不動態被膜
Claims (10)
- 少なくとも一部に、ClFを含むガスと接触してなるフッ化物の不動態被膜を有する材料からなり、前記不動態被膜が形成された内面を有する保存容器であって、
前記保存容器に取り付けられるバルブを備え、
前記バルブは、
前記ガスの流路と、
前記流路が開口された弁座と、
前記弁座に対し離接することで前記流路を開閉する弁体と
を有し、
前記流路と、前記弁座及び弁体の接ガス部とに前記不動態被膜が形成されていることを特徴とする保存容器。 - 前記弁体は、前記流路を閉じるときに前記弁座に押圧されるシール面を有し、
前記シール面は2μm〜10μmの金メッキ層を有することを特徴とする請求項1に記載の保存容器。 - 前記金メッキ層は封孔処理が施されてなることを特徴とする請求項2に記載の保存容器。
- 前記金メッキ層は酸化処理が施されてなることを特徴とする請求項2又は3に記載の保存容器。
- 前記不動態被膜は前記金メッキ層に形成されてなることを特徴とする請求項2から4の何れか一項に記載の保存容器。
- 前記弁体は、ディスク型であることを特徴とする請求項1から5の何れか一項に記載の保存容器。
- 前記弁体は、ダイヤフラムであることを特徴とする請求項1から5の何れか一項に記載の保存容器。
- 前記不動態被膜は、5nm〜50nmの膜厚を有することを特徴とする請求項1から7の何れか一項に記載の保存容器。
- 前記不動態被膜は、ClF 3 及びF 2 からなる群より選択される1つ以上のガスとさらに接触してなることを特徴とする請求項1から8の何れか一項に記載の保存容器。
- 前記材料は、マンガン鋼、ステンレス鋼、クロムモリブデン鋼、ニッケル合金、アルミニウム合金、コバルト合金、金、及び樹脂の少なくとも1つに前記不動態被膜を形成してなることを特徴とする請求項1から9の何れか一項に記載の保存容器。
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CN112944204B (zh) * | 2021-02-02 | 2021-11-09 | 福建德尔科技有限公司 | 电子级三氟化氯的收集装置 |
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