JP7157299B2 - 酸フッ化金属の処理方法及びクリーニング方法 - Google Patents
酸フッ化金属の処理方法及びクリーニング方法 Download PDFInfo
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- JP7157299B2 JP7157299B2 JP2017137765A JP2017137765A JP7157299B2 JP 7157299 B2 JP7157299 B2 JP 7157299B2 JP 2017137765 A JP2017137765 A JP 2017137765A JP 2017137765 A JP2017137765 A JP 2017137765A JP 7157299 B2 JP7157299 B2 JP 7157299B2
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- 229910052751 metal Inorganic materials 0.000 title claims description 124
- 239000002184 metal Substances 0.000 title claims description 124
- 238000000034 method Methods 0.000 title claims description 58
- 238000004140 cleaning Methods 0.000 title description 15
- 239000007789 gas Substances 0.000 claims description 117
- 238000006243 chemical reaction Methods 0.000 claims description 72
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 70
- 229910052731 fluorine Inorganic materials 0.000 claims description 70
- 239000011737 fluorine Substances 0.000 claims description 70
- 229910052721 tungsten Inorganic materials 0.000 claims description 24
- 229910052750 molybdenum Inorganic materials 0.000 claims description 23
- 239000011261 inert gas Substances 0.000 claims description 17
- 229910001512 metal fluoride Inorganic materials 0.000 claims description 11
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- WSWMGHRLUYADNA-UHFFFAOYSA-N 7-nitro-1,2,3,4-tetrahydroquinoline Chemical compound C1CCNC2=CC([N+](=O)[O-])=CC=C21 WSWMGHRLUYADNA-UHFFFAOYSA-N 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 11
- NXHILIPIEUBEPD-UHFFFAOYSA-H tungsten hexafluoride Chemical compound F[W](F)(F)(F)(F)F NXHILIPIEUBEPD-UHFFFAOYSA-H 0.000 description 11
- QKCGXXHCELUCKW-UHFFFAOYSA-N n-[4-[4-(dinaphthalen-2-ylamino)phenyl]phenyl]-n-naphthalen-2-ylnaphthalen-2-amine Chemical compound C1=CC=CC2=CC(N(C=3C=CC(=CC=3)C=3C=CC(=CC=3)N(C=3C=C4C=CC=CC4=CC=3)C=3C=C4C=CC=CC4=CC=3)C3=CC4=CC=CC=C4C=C3)=CC=C21 QKCGXXHCELUCKW-UHFFFAOYSA-N 0.000 description 10
- 238000009835 boiling Methods 0.000 description 9
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 9
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical group [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 9
- 239000010937 tungsten Substances 0.000 description 9
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 8
- 229910001873 dinitrogen Inorganic materials 0.000 description 8
- 230000008018 melting Effects 0.000 description 8
- 238000002844 melting Methods 0.000 description 8
- 239000011733 molybdenum Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 229910015648 MoOF Inorganic materials 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- XRURPHMPXJDCOO-UHFFFAOYSA-N iodine heptafluoride Chemical compound FI(F)(F)(F)(F)(F)F XRURPHMPXJDCOO-UHFFFAOYSA-N 0.000 description 5
- JOHWNGGYGAVMGU-UHFFFAOYSA-N trifluorochlorine Chemical compound FCl(F)F JOHWNGGYGAVMGU-UHFFFAOYSA-N 0.000 description 5
- 229910015275 MoF 6 Inorganic materials 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000005078 molybdenum compound Substances 0.000 description 2
- 150000002752 molybdenum compounds Chemical class 0.000 description 2
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- GVGCUCJTUSOZKP-UHFFFAOYSA-N nitrogen trifluoride Chemical compound FN(F)F GVGCUCJTUSOZKP-UHFFFAOYSA-N 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 150000003658 tungsten compounds Chemical class 0.000 description 2
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 2
- 229910020323 ClF3 Inorganic materials 0.000 description 1
- 101100441092 Danio rerio crlf3 gene Proteins 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- VKGXXSUCNHXKKH-UHFFFAOYSA-H F[W](F)(F)(F)(F)F.F.F.F.F.F.F Chemical compound F[W](F)(F)(F)(F)F.F.F.F.F.F.F VKGXXSUCNHXKKH-UHFFFAOYSA-H 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- YGTSMYMNDOTCEI-UHFFFAOYSA-N [W].FOF Chemical compound [W].FOF YGTSMYMNDOTCEI-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000011437 continuous method Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000005108 dry cleaning Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- HXHQDHKWCRUPKS-UHFFFAOYSA-N fluoro hypofluorite molybdenum Chemical compound [Mo].FOF HXHQDHKWCRUPKS-UHFFFAOYSA-N 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- -1 metal oxide fluorides Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 1
- 238000009849 vacuum degassing Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
- C01G1/06—Halides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/04—Halides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B5/00—Cleaning by methods involving the use of air flow or gas flow
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
- B08B7/0064—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes
- B08B7/0071—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes by heating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
- B08B7/04—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by a combination of operations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/08—Cleaning containers, e.g. tanks
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/04—Halides
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
- C23C16/08—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material from metal halides
- C23C16/14—Deposition of only one other metal element
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4405—Cleaning of reactor or parts inside the reactor by using reactive gases
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
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- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
- H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
- H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
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- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/3065—Plasma etching; Reactive-ion etching
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
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- Drying Of Semiconductors (AREA)
- Treating Waste Gases (AREA)
- Electrodes Of Semiconductors (AREA)
Description
W(s)+3F2(g)→WF6(g) …反応式(1-1)
W(s)+2NF3(g)→WF6(g)+N2(g) …反応式(1-2)
Mo(s)+3F2(g)→MoF6(g) …反応式(2-1)
Mo(s)+2NF3(g)→MoF6(g)+N2(g) …反応式(2-2)
WO3(s)+2F2(g)→WOF4+O2(g) ・・・反応式(3-1)
WO3(s)+4/3NF3(g)→WOF4+O2(g)+2/3N2(g) ・・・反応式(3-2)
MoO3(s)+2F2(g)→MoOF4+O2(g) ・・・反応式(4-1)
MoO3(s)+4/3NF3(g)→MoOF4+O2(g)+2/3N2(g) ・・・反応式(4-2)
WO3(s)+2WF6(g)→3WOF4 ・・・反応式(3-3)
WO3(s)+2WF6(g)→3WOF4 ・・・反応式(4-3)
H2O+WF6(g)→WOF4+2HF ・・・反応式(3-4)
H2O+MoF6(g)→MoOF4+2HF ・・・反応式(4-4)
2WF6+3Si→2W+3SiF4 ・・・反応式(5-1)
WF6+3H2→W+6HF ・・・反応式(5-2)
2WF6+SiO2→2WOF4+3SiF4 ・・・反応式(5-3)
2MoF6+3Si→2Mo+3SiF4 ・・・反応式(6-1)
MoF6+3H2→Mo+6HF ・・・反応式(6-2)
2MoF6+SiO2→2MoOF4+3SiF4 ・・・反応式(6-3)
WOF4+H2O→WO2F2+2HF ・・・反応式(7-1)
WO2F2+H2O→WO3+2HF ・・・反応式(7-2)
MoOF4+H2O→MoO2F2+2HF ・・・反応式(8-1)
MoO2F2+H2O→MoO3+2HF ・・・反応式(8-2)
MOF4+2F2(g)→MF6(g)+1/2O2(g)…反応式(9-1)
MOF4+2/3NF3(g)→MF6(g)+1/2O2(g)+1/3N2(g)…反応式(9-2)
MOF4+ClF3(g)→MF6(g)+1/2O2(g)+ClF(g)…反応式(9-3)
MOF4+IF7(g)→MF6(g)+1/2O2(g)+IF5(g)…反応式(9-4)
但し、Mはタングステン又はモリブデンである。
本発明の酸フッ化金属の処理方法を用いた、フッ化金属製造装置のクリーニング方法を、図1を用いて説明する。図1に示すフッ化金属製造装置11は、反応器13を有する。フッ化金属を製造する際には、反応器13内に粉末状、粒状又は塊状の金属タングステン又は金属モリブデンを充填し、フッ素ガスや三フッ化窒素ガスなどを反応器13内に供給して、六フッ化金属などのガス状のフッ化金属を得る。その際に、前述の反応式(3-1)などにより酸フッ化金属が生成するため、反応器13や配管の内面に付着物17として付着する。以下、反応器13の内面の付着物17を有するフッ化金属製造装置11のクリーニング方法を説明する。
本発明の酸フッ化金属の処理方法を用いた、成膜装置のクリーニング方法を、図2を用いて説明する。図2に示す成膜装置51は、チャンバー53を有する。成膜装置を使用する際には、チャンバー53の内部にあるステージ57に、シリコンウェハなどの被処理物を載置し、そこに六フッ化タングステンガス又は六フッ化モリブデンガスを供給し、必要に応じてH2なども供給し、被処理物にタングステン、モリブデン又はこれらの化合物を成膜する。その際に、水や酸化物の影響により酸フッ化金属が生成するため、チャンバー53や配管の内面、ステージ57の表面に付着物59として付着する。以下、チャンバー53の内面とステージ57の表面に付着物59を有する成膜装置51のクリーニング方法を説明する。
容積100cm3の容器103に、酸フッ化金属105としてタングステン酸フッ化物を33g充填した。不活性ガス供給部102から窒素ガスを供給し、ガス排出装置104で真空脱気により置換した。フッ素含有ガス供給部101から、図示しない圧力計で絶対圧100kPaとなるまで、フッ素ガスを導入し、酸フッ化金属105と接触させた。フッ素含有ガスに対する酸フッ化金属のモル比を30とした。ヒータ106で容器103を20℃にして、2時間静置させた後、反応器103中のガスの一部を抜出して、赤外分光光度計で六フッ化タングステンの濃度を測定して、フッ素含有ガスの転化率を算出した。転化率は、容器内に導入したフッ素ガスのうち、2時間の反応時間で六フッ化タングステンの転化に消費されたフッ素ガスの割合を示す。その結果、フッ素の転化率は1%だった。ただし、反応時間をより長くすれば、転化率はより高くなる。
フッ素含有ガスを三フッ化窒素とする以外は、実施例1と同様に、フッ素含有ガスと酸フッ化金属を接触させた。その結果、三フッ化窒素の転化率は、1%だった。
フッ素含有ガスを三フッ化塩素とする以外は、実施例1と同様に、フッ素含有ガスと酸フッ化金属を接触させた。その結果、三フッ化塩素の転化率は、53%だった。
フッ素含有ガスを七フッ化ヨウ素とする以外は、実施例1と同様に、フッ素含有ガスと酸フッ化金属を接触させた。その結果、七フッ化ヨウ素の転化率は、43%だった。
酸フッ化金属をモリブデン酸フッ化物とする以外は、実施例1と同様に、フッ素含有ガスと酸フッ化金属を接触させた。その結果、フッ素の転化率は、1%だった。
酸フッ化金属をモリブデン酸フッ化物とする以外は、実施例2と同様に、フッ素含有ガスと酸フッ化金属を接触させた。その結果、三フッ化窒素の転化率は、1%だった。
酸フッ化金属をモリブデン酸フッ化物とする以外は、実施例3と同様に、フッ素含有ガスと酸フッ化金属を接触させた。その結果、三フッ化塩素の転化率は、65%だった。
酸フッ化金属をモリブデン酸フッ化物とする以外は、実施例4と同様に、フッ素含有ガスと酸フッ化金属を接触させた。その結果、七フッ化ヨウ素の転化率は、57%だった。
ヒータ106で容器103を150℃にする以外は、実施例1と同様に、フッ素含有ガスと酸フッ化金属を接触させた。その結果、フッ素の転化率は、19%だった。
ヒータ106で容器103を150℃にする以外は、実施例2と同様に、フッ素含有ガスと酸フッ化金属を接触させた。その結果、三フッ化窒素の転化率は、14%だった。
ヒータ106で容器103を150℃にする以外は、実施例3と同様に、フッ素含有ガスと酸フッ化金属を接触させた。その結果、三フッ化窒素の転化率は、86%だった。
ヒータ106で容器103を150℃にする以外は、実施例9と同様に、フッ素含有ガスと酸フッ化金属を接触させた。その結果、七フッ化ヨウ素の転化率は、78%だった。
酸フッ化金属をモリブデン酸フッ化物とする以外は、実施例10と同様に、フッ素含有ガスと酸フッ化金属を接触させた。その結果、フッ素の転化率は、25%だった。
酸フッ化金属をモリブデン酸フッ化物とする以外は、実施例11と同様に、フッ素含有ガスと酸フッ化金属を接触させた。その結果、三フッ化窒素の転化率は、16%だった。
酸フッ化金属をモリブデン酸フッ化物とする以外は、実施例12と同様に、フッ素含有ガスと酸フッ化金属を接触させた。その結果、三フッ化塩素の転化率は、89%だった。
酸フッ化金属をモリブデン酸フッ化物とする以外は、実施例13と同様に、フッ素含有ガスと酸フッ化金属を接触させた。その結果、七フッ化ヨウ素の転化率は、80%だった。
フッ素含有ガスの代わりに不活性ガス供給部から窒素を供給する以外は、実施例1と同様に、窒素ガスと酸フッ化金属を接触させた。その結果、六フッ化タングステンの生成は認められず、転化率を算出することはできなかった。
フッ素含有ガスの代わりに不活性ガス供給部から窒素を供給する以外は、実施例5と同様に、窒素ガスと酸フッ化金属を接触させた。その結果、六フッ化モリブデンの生成は認められず、転化率を算出することはできなかった。
ヒータ106で容器103を150℃にする以外は、比較例1と同様に、窒素ガスと酸フッ化金属を接触させた。その結果、六フッ化タングステンの生成は認められず、転化率を算出することはできなかった。
ヒータ106で容器103を150℃にする以外は、比較例2同様に、窒素ガスと酸フッ化金属を接触させた。その結果、六フッ化モリブデンの生成は認められず、転化率を算出することはできなかった。
13 反応器
15 ヒータ
17 付着物
21 フッ素含有ガス供給部
23 バルブ
31 不活性ガス供給部
33 バルブ
41 ガス排出ライン
43 バルブ
45 ガス排出装置
51 成膜装置
53 チャンバー
55 ヒータ
57 ステージ
59 付着物
61 フッ素含有ガス供給部
63 バルブ
71 不活性ガス供給部
73 バルブ
81 ガス排出ライン
83 バルブ
85 ガス排出装置
100 実験装置
101 フッ素含有ガス供給部
102 不活性ガス供給部
103 容器
104 ガス排出装置
105 酸フッ化金属
106 ヒータ
111、112、113 バルブ
Claims (6)
- 一般式MO(6-x)/2Fx(0<x<6、M=W又はMo)で表される酸フッ化金属を、フッ素含有ガスとしてF 2 ガス、NF 3 ガス、ClF 3 ガス、及びIF 7 ガスからなる群より選ばれる少なくとも一種のガスと温度10℃以上200℃以下で接触させて、化学反応によって一般式MF6(M=W又はMo)で表される六フッ化金属へ変換することを特徴とする酸フッ化金属の処理方法。
- 前記酸フッ化金属と前記フッ素含有ガスを接触させる際の圧力が、絶対圧で0.01kPa以上300kPa以下であることを特徴とする請求項1に記載の酸フッ化金属の処理方法。
- 前記酸フッ化金属を、不活性ガスで希釈された前記フッ素含有ガスと接触させることを特徴とする請求項1又は2に記載の酸フッ化金属の処理方法。
- 前記酸フッ化金属を、前記フッ素含有ガスと接触させる際に、プラズマを発生させないことを特徴とする請求項1~3の何れか1項に記載の酸フッ化金属の処理方法。
- 一般式MF6(M=W又はMo)で表される六フッ化金属を製造するフッ化金属製造装置の内面に堆積した一般式MO(6-x)/2Fx(0<x<6、M=W又はMo)で表される酸フッ化金属を、請求項1に記載の処理方法で六フッ化金属へ変換して除去することを特徴とするフッ化金属製造装置のクリーニング方法。
- 一般式MF6(M=W又はMo)で表される六フッ化金属を使用する成膜装置の内面に堆積した一般式MO(6-x)/2Fx(0<x<6、M=W又はMo)で表される酸フッ化金属を、請求項1に記載の処理方法で六フッ化金属へ変換して除去することを特徴とする成膜装置のクリーニング方法。
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