TWI617538B - High purity 1H-heptafluorocyclopentene - Google Patents
High purity 1H-heptafluorocyclopentene Download PDFInfo
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- TWI617538B TWI617538B TW103105589A TW103105589A TWI617538B TW I617538 B TWI617538 B TW I617538B TW 103105589 A TW103105589 A TW 103105589A TW 103105589 A TW103105589 A TW 103105589A TW I617538 B TWI617538 B TW I617538B
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- Prior art keywords
- heptafluorocyclopentene
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- AWDCOETZVBNIIV-UHFFFAOYSA-N 1,3,3,4,4,5,5-heptafluorocyclopentene Chemical compound FC1=CC(F)(F)C(F)(F)C1(F)F AWDCOETZVBNIIV-UHFFFAOYSA-N 0.000 title claims abstract description 109
- 150000001875 compounds Chemical class 0.000 claims abstract description 26
- 239000012495 reaction gas Substances 0.000 claims abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 30
- 238000001312 dry etching Methods 0.000 claims description 25
- 239000007789 gas Substances 0.000 claims description 23
- 229910052757 nitrogen Inorganic materials 0.000 claims description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 15
- 239000001301 oxygen Substances 0.000 claims description 15
- 229910052760 oxygen Inorganic materials 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 229910001868 water Inorganic materials 0.000 claims description 15
- 238000005984 hydrogenation reaction Methods 0.000 claims description 6
- 238000000746 purification Methods 0.000 claims description 6
- MYVQKOLPIBOMHY-UHFFFAOYSA-N 1-chloro-1,2,2,3,3,4,4,5,5-nonafluorocyclopentane Chemical compound FC1(F)C(F)(F)C(F)(F)C(F)(Cl)C1(F)F MYVQKOLPIBOMHY-UHFFFAOYSA-N 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 5
- 238000005268 plasma chemical vapour deposition Methods 0.000 claims description 4
- MTXFJQPFMARORW-UHFFFAOYSA-N 3-chloro-1,2,3,4,4,5,5-heptafluorocyclopentene Chemical compound FC1=C(F)C(F)(Cl)C(F)(F)C1(F)F MTXFJQPFMARORW-UHFFFAOYSA-N 0.000 claims description 2
- 238000010574 gas phase reaction Methods 0.000 claims description 2
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 claims description 2
- JQAHBADBSNZKFG-UHFFFAOYSA-N 1,2,3,3,4,4,5-heptafluorocyclopentene Chemical compound FC1C(F)=C(F)C(F)(F)C1(F)F JQAHBADBSNZKFG-UHFFFAOYSA-N 0.000 claims 1
- 239000004065 semiconductor Substances 0.000 abstract description 4
- 238000005530 etching Methods 0.000 description 17
- 238000004821 distillation Methods 0.000 description 15
- 238000004519 manufacturing process Methods 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 13
- 239000012535 impurity Substances 0.000 description 13
- XUMFLKOMBYRBCK-UHFFFAOYSA-N 1-chloro-2,3,3,4,4,5,5-heptafluorocyclopentene Chemical compound FC1=C(Cl)C(F)(F)C(F)(F)C1(F)F XUMFLKOMBYRBCK-UHFFFAOYSA-N 0.000 description 11
- 238000004817 gas chromatography Methods 0.000 description 11
- 238000009835 boiling Methods 0.000 description 10
- 238000010992 reflux Methods 0.000 description 8
- 238000005229 chemical vapour deposition Methods 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 5
- 239000003463 adsorbent Substances 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 229910052801 chlorine Inorganic materials 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 239000002808 molecular sieve Substances 0.000 description 5
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 5
- YBMDPYAEZDJWNY-UHFFFAOYSA-N 1,2,3,3,4,4,5,5-octafluorocyclopentene Chemical compound FC1=C(F)C(F)(F)C(F)(F)C1(F)F YBMDPYAEZDJWNY-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000001577 simple distillation Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- QVEJLBREDQLBKB-UHFFFAOYSA-N 1,1,2,2,3,3,4,5-octafluorocyclopentane Chemical compound FC1C(F)C(F)(F)C(F)(F)C1(F)F QVEJLBREDQLBKB-UHFFFAOYSA-N 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 3
- 229910000617 Mangalloy Inorganic materials 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 238000012790 confirmation Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- OCNKVPIYWRQFQI-UHFFFAOYSA-N 2,2,3,3,4,4,5-heptafluorocyclopentan-1-one Chemical compound FC1C(=O)C(F)(F)C(F)(F)C1(F)F OCNKVPIYWRQFQI-UHFFFAOYSA-N 0.000 description 2
- ZYXLKQPTUOSLFA-UHFFFAOYSA-N 4-chloro-1,1,2,2,3,3-hexafluorocyclopentane Chemical compound ClC1C(C(C(C1)(F)F)(F)F)(F)F ZYXLKQPTUOSLFA-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 101000956368 Trittame loki CRISP/Allergen/PR-1 Proteins 0.000 description 2
- 238000004380 ashing Methods 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 125000001309 chloro group Chemical group Cl* 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- LPIQUOYDBNQMRZ-UHFFFAOYSA-N cyclopentene Chemical compound C1CC=CC1 LPIQUOYDBNQMRZ-UHFFFAOYSA-N 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000007327 hydrogenolysis reaction Methods 0.000 description 2
- 229910052756 noble gas Inorganic materials 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- MITPAYPSRYWXNR-UHFFFAOYSA-N 1,1,2,2,3,3-hexafluorocyclopentane Chemical compound FC1(F)CCC(F)(F)C1(F)F MITPAYPSRYWXNR-UHFFFAOYSA-N 0.000 description 1
- LGPPATCNSOSOQH-UHFFFAOYSA-N 1,1,2,3,4,4-hexafluorobuta-1,3-diene Chemical compound FC(F)=C(F)C(F)=C(F)F LGPPATCNSOSOQH-UHFFFAOYSA-N 0.000 description 1
- FHQKLIHFKVAEEP-UHFFFAOYSA-N 3,3,4,4,5,5-hexafluorocyclopentene Chemical compound FC1(F)C=CC(F)(F)C1(F)F FHQKLIHFKVAEEP-UHFFFAOYSA-N 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000007514 bases Chemical class 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000001687 destabilization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000000895 extractive distillation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 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 group [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000012450 pharmaceutical intermediate Substances 0.000 description 1
- 229920002120 photoresistant polymer Polymers 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 1
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K13/00—Etching, surface-brightening or pickling compositions
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/23—Preparation of halogenated hydrocarbons by dehalogenation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D25/00—Details of other kinds or types of rigid or semi-rigid containers
- B65D25/38—Devices for discharging contents
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C23/00—Compounds containing at least one halogen atom bound to a ring other than a six-membered aromatic ring
- C07C23/02—Monocyclic halogenated hydrocarbons
- C07C23/08—Monocyclic halogenated hydrocarbons with a five-membered ring
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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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
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- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/12—Gaseous compositions
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- H—ELECTRICITY
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- 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
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
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- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
- H01L21/02274—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition in the presence of a plasma [PECVD]
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- 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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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/06—Systems containing only non-condensed rings with a five-membered ring
- C07C2601/10—Systems containing only non-condensed rings with a five-membered ring the ring being unsaturated
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- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
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- H—ELECTRICITY
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- 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
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
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- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Plasma & Fusion (AREA)
- General Chemical & Material Sciences (AREA)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Drying Of Semiconductors (AREA)
Abstract
本發明為一種1H-七氟環戊烯,其特徵在於純度為99.9重量%以上,且有機氯系化合物的含量為350重量ppm以下。
根據本發明,其提供一種具有適當的高純度的1H-七氟環戊烯作為半導體用的電漿反應用氣體。
Description
本發明係關於一種高純度IH-七氟環戊烯,其係使用作為乾式蝕刻氣體或CVD成膜用氣體等電漿反應用氣體、含氟醫藥中間體、氫氟碳化合物系溶劑等。
近年來,半導體製造技術的微細化正在發展中,在最先進的製程中,逐漸採用線寬為20nm世代,進一步為10nm世代。伴隨著微細化,其加工時的技術難度亦提升,已藉由使用的材料、裝置、加工方法等從多方面的處理方法發展技術開發。
由此種狀況來看,就亦可對應於最先進的乾式蝕刻製程的乾式蝕刻用氣體而言,已開發出IH-七氟環戊烯(專利文獻1)。此化合物具有超越現今在工業上已廣泛用作矽氧化膜的蝕刻氣體之六氟-1,3-丁二烯的性能,其用處已逐漸受到認可。
就製造1H-七氟環戊烯的方法而言,已知有將八氟環戊烯氫化,變換成1H,2H-八氟環戊烷,使其與如碳酸鉀之鹼性化合物接觸而脫去HF之方法(專利文獻2);及在以鈀為基質之氫化觸媒的存在下,將1-氯七氟環戊烯氫化(氯原子的氫解)之方法(專利文獻3)等。
[專利文獻1]WO2009/041560號
[專利文獻2]日本特開平11-292807號公報
[專利文獻3]WO2010/007968號
如上所述,1H-七氟環戊烯係作為亦可對應於最先進的乾式蝕刻製程之乾式蝕刻用氣體而受到矚目。
然而,在將填充在容器中的1H-七氟環戊烯連續地供給至乾式蝕刻裝置而進行乾式蝕刻的情況下,蝕刻速度會逐漸降低,在某些情況下,蝕刻會停止而造成問題。
本發明人為了解決上述課題而深入研究,結果找到造成蝕刻速度降低的物質是1H-七氟環戊烯中所含有的不純物、特別是1H-七氟環戊烯中所含有的少量有機氯系化合物,以及此不純物的有機氯系化合物會隨著持續實施乾式蝕刻而在容器內濃縮,在容器內的殘留量變少的步驟中,會引起1H-七氟環戊烯的純度降低,並引起蝕刻速度降低。而且,在填充在容器內的高純度的1H-七氟環戊烯使用作為乾式蝕刻或CVD成膜用氣體時,從使用開始時直到幾乎是空的狀態為止,為了實現穩定的乾式蝕刻,發現必須要將1H-七氟環戊烯中所含有的有機氯系化合物的量限制在某一定量以下,從而完成本發明。
因此根據本發明,能夠提供下述(1)~(5)記載之1H-七氟環戊烯、(6)、(7)記載之使用方法、(8)記載之附有閥的容器。
(1)一種1H-七氟環戊烯,其特徵在於:純度為99.9重量%以上,而且有機氯系化合物的含量為350重量ppm以下。
(2)如(1)記載之1H-七氟環戊烯,其係經由步驟(I)及步驟(II)而得者,其中步驟(I):藉由氣相反應而在觸媒存在下將1-氯七氟環戊烯氫化,得到粗製的1H-七氟環戊烯;步驟(II):使用理論板數為50板以上的精餾塔精製步驟(1)所得到之粗製的1H-七氟環戊烯。
(3)如(1)記載之1H-七氟環戊烯,有機氯系化合物為氯九氟環戊烷及/或氯七氟環戊烯。
(4)如(1)記載之1H-七氟環戊烯,其中含氮量為100體積ppm以下,且含氧量為50體積ppm以下。
(5)如(3)記載之1H-七氟環戊烯,其中含水量為20重量ppm以下。
(6)一種使用1H-七氟環戊烯作為乾式蝕刻氣體的方法,其係使用如前述(1)至(5)中任一項記載之1H-七氟環戊烯作為乾式蝕刻氣體的方法。
(7)一種使用1H-七氟環戊烯作為電漿CVD的反應氣體的方法,其係使用如前述(1)至(5)中任一項記載之1H-七氟環戊烯作為電漿CVD的反應氣體的方法。
(8)一種附有閥的容器,其係填充如前述(1)至(5)中任一項記載之1H-七氟環戊烯而成。
本發明之經高純度化的1H-七氟環戊烯尤其是在使用電漿反應之半導體裝置的製造領域中,適合用作電漿蝕刻氣體、化學氣相沉積法(CVD)用反應氣體等。
本發明之1H-七氟環戊烯之特徵在於:純度為99.9重量%以上,而且有機氯系化合物的含量為350重量ppm以下。
又,氮與氧的含量相對於1H-七氟環戊烯的總量,分別較佳為100體積ppm以下、50體積ppm以下,再者,含水量特佳為20重量ppm以下。
在本發明中,1H-七氟環戊烯的純度以及有機氯系化合物的含量係使用以火焰游離偵檢器(FID)作為偵檢器的氣相層析法來測定的值。
有機氯系化合物係可使用氣相層析法質量分析來鑑定。
1H-七氟環戊烯中的氮與氧的含量係使用以熱電導偵檢器(TCD)作為偵檢器的氣相層析法來測定的值。
又,1H-七氟環戊烯中的含水量係使用FT-IR來測定的值。
若本發明之高純度1H-七氟環戊烯的純度為99.9重量%以上,而且有機氯系化合物的含量為350重量
ppm以下,則其製造方法並沒有特殊的限定。
其中,以經由使用理論板數為50板以上的精餾塔來精製粗製的1H-七氟環戊烯的步驟(II)所得到者為佳。
<粗製的1H-七氟環戊烯的製造>
粗製的1H-七氟環戊烯係可使用日本特開平11-292807號公報或WO2010/007968號所記載的方法來製造,前者係在氫化觸媒的存在下使用氫氣將八氟環戊烯轉換成1H,2H-八氟環戊烷,使所得到的1H,2H-八氟環戊烷在鹼的存在下進行脫HF反應而導向期望的粗製的1H-七氟環戊烯的方法。另一方面,後者係在氫化觸媒的存在下使用氫氣將1-氯七氟環戊烯氫化(氯原子的氫解反應),得到粗製的1H-七氟環戊烯的方法。從工業的觀點來說,在製造步驟數、操作的方便性、原料的供應成本等方面下,以使用後者的方法來進行製造為佳。
<粗製的1H-七氟環戊烯的精製>
在進行上述1-氯七氟環戊烯的氫化反應後,藉由蒸餾精製法等,從粗製的1H-七氟環戊烯去除有機系不純物。使用蒸餾精製法去除有機系不純物時,可使用精餾塔。尤其是為了有效地去除沸點與1H-七氟環戊烯(沸點46℃)接近的有機系不純物,適於使用高理論板數的精餾塔。使用的精餾塔的理論板數通常為30板以上,較佳為50板以上。從製造上的觀點來看,理論板數的上限較佳為100板以下。
精餾時的壓力以計示壓計,通常為常壓~5大氣壓,較佳為常壓~2大氣壓左右。為了去除1H-七氟
環戊烯中所含有的微量不純物、尤其是與1H-七氟環戊烯之間的沸點差距小的不純物,回流量與提取量的比(以下有時稱為「回流比」)係以將回流比設定成40:1以上為佳。回流比若太小,則無法有效地去除微量不純物,1H-七氟環戊烯的純度提升會變小,而且初餾物會變多,實質上作為製品而取得的1H-七氟環戊烯的量會變少。又,若回流比極度過大,則由於到每1次提取的回收為止需要大量的時間,因此精餾其本身需要大量的時間。
就精餾的方式而言,在製造量少的情況下,精餾可為批式,但在製造量多的情況下,亦可採用經由數個精餾塔的連續式。又,亦可組合添加萃取溶劑的萃取蒸餾操作來進行。
作為有機系不純物,存在有沸點比1H-七氟環戊烯低的化合物、與沸點比1H-七氟環戊烯高的化合物兩者。在蒸餾精製中,例如可進行:在第1次蒸餾時去除前者的化合物、在第2次蒸餾時去除後者的化合物等的逐步蒸餾。在此情況下,亦以回流比在40:1以上較佳。
又,使用精餾塔精製粗製的1H-七氟環戊烯時,可在0族的惰性氣體中進行精餾。0族的惰性氣體並沒有特殊的限定,可列舉屬於週期表第0族的氦、氖、氬、氪、氙等。從工業上容易入手的觀點來看,較佳為氦、氬。
在使用上述方法將純度提高至99.9重量%以上的1H-七氟環戊烯中,含有在1H-七氟環戊烯的製造過程中共存的微量反應原料與副產物作為有機系不純物。
具體而言,可列舉八氟環戊烯、七氟環戊酮、氯九氟環戊烷及1-氯七氟環戊烯。
在這些有機系不純物之中,一旦存在大量的沸點比1H-七氟環戊烯(沸點46℃)高的氯九氟環戊烷(沸點52℃)及1-氯七氟環戊烯(沸點56℃),則會隨著在填充於容器的狀態下連續供給至蝕刻裝置,而在容器內的1H-七氟環戊烯的殘留量減少的步驟中造成濃縮。
在將含有作為有機氯系化合物之氯九氟環戊烷與1-氯七氟環戊烯的濃縮物之1H-七氟環戊烯使用作為乾式蝕刻氣體的情況下,會引起蝕刻時的速度降低,或是蝕刻本身中途會停止。這樣的舉動意味著容器內所填充的1H-七氟環戊烯的預估可使用量會減少,而且會導致引起半導體裝置製造的良率降低之缺陷。
又,關於1H-七氟環戊烯中所含有的氮與氧,其含量亦會引起問題。關於氮,若含量多、或是在每個容器含量不均,則會引起乾式蝕刻時的蝕刻速度的極端變動,也就是說每個批次會引起蝕刻速度的不均一化,因此可能會引起製造程序的不穩定化。又,關於氧,其取決於乾式蝕刻時的被蝕刻材料或加工製程,但1H-七氟環戊烯的沉積性會變化,也就是說這可能會成為與被蝕刻材料的選擇性降低或不均的主要因素。因此,關於1H-七氟環戊烯中所含有的氮與氧,亦以盡可能降低的狀態為佳。
去除1H-七氟環戊烯中所含有的氮與氧的方法並沒有特別的限制,可列舉例如:以精餾進行前述有
機氯系化合物的去除時,在0族的惰性氣體中進行精製的方法;或將1H-七氟環戊烯簡單蒸餾,進行提取餾分的操作之方法等。後者的情況下,藉由透過簡單蒸餾將氮與氧與1H-七氟環戊烯一起提取,而降低殘留在釜中的1H-七氟環戊烯中所含有的氮與氧的含量。提取出的1H-七氟環戊烯中的氮與氧的含量相對於裝入至蒸餾釜中的1H-七氟環戊烯,以重量為基準,較佳為20~50%,更佳為30~40%。提取出的1H-七氟環戊烯先儲存,再加入到下一個批次,藉以能夠回收、再使用。
又,去除1H-七氟環戊烯所含有的水分的方法並沒有特別的限制,可採用與吸附劑接觸的方法等的一般方法。
作為吸附劑,可使用分子篩或氧化鋁等。分子篩或氧化鋁在市面上有許多種類被販售,因此能夠從此等之中適當選擇。其中,較佳為分子篩3A、4A及5A等,更佳為3A。又,氧化鋁較佳為藉由氧化鋁水合物的加熱脫水而生成之結晶性低的活性氧化鋁。分子篩或氧化鋁等的吸附劑較佳為在接觸1H-七氟環戊烯前,藉由燒製等操作而預先進行活性化。藉由預先使其活性化,能夠吸附更多的水分。像這樣,藉由使1H-七氟環戊烯與吸附劑接觸,而能夠使1H-七氟環戊烯中的含水量降低至20重量ppm以下。含水量若多,則在對基板進行蝕刻加工後,水分可能會在加工面上吸附殘留,而造成在銅等的配線形成步驟中使積層膜剝離、或是造成嵌入的配線腐蝕,因此以盡可能地降低含水量為佳。
如上述說明,將反應粗製產物中所含有的粗製的1H-七氟環戊烯精製至純度99.9重量%以上且將有機氯系化合物精製至350重量ppm以下之精餾步驟係能夠藉由進一步與吸附劑接觸而進行去除水分的步驟,接著藉由將1H-七氟環戊烯簡單蒸餾而取得1H-七氟環戊烯中的氮、氧濃度降低至100體積ppm以下,較佳為降低至50體積ppm以下之高純度的1H-七氟環戊烯。像這樣藉由控制不純物的量,而能夠提高乾式蝕刻時的加工穩定性與進行電漿CVD的成膜穩定性。
因此,本發明之高純度1H-七氟環戊烯係適於作為乾式蝕刻、CVD及灰化等的電漿反應用氣體來使用。作為本發明之高純度1H-七氟環戊烯之較佳的具體例,可列舉電漿反應乾式蝕刻用氣體、電漿反應CVD用氣體及電漿反應灰化用氣體。
本發明之高純度1H-七氟環戊烯係填充在附有閥的容器中,此填充容器若為金屬製的耐壓容器,則材質並沒有特殊的限定,但一般是使用錳鋼、鉻鉬鋼、不鏽鋼、鎳鋼及鋁合金鋼。又,關於閥(以下有時稱為「鋼瓶閥」),考慮到該化合物的腐蝕性等或安全性,以使用基於高壓氣體保安法及JIS-B8246規格的鋼瓶閥為佳。此鋼瓶閥係可列舉隔膜式、凹槽板式及直接隔膜密封鋼瓶閥等。從取得的容易性來看,以附有隔膜式閥的錳鋼容器為佳。
以下藉由實施例更詳細說明本發明,惟本發
明並不因以下的實施例而限定其範圍。
以下所採用的分析條件係如下所述。
‧氣相層析法分析(GC分析)
裝置:HP-6890(Agilent公司製)
管柱:Inert Cap-1、長度60m、內徑0.25mm、膜厚1.5μm(GL Sciences公司製)
管柱溫度:在40℃下保持10分鐘,接著以20℃/分鐘進行升溫,之後在240℃下保持10分鐘
注射溫度:250℃
載體氣體:氮
分流比(split ratio):100/1
偵檢器:FID
‧不純物的分析(氣相層析法質量分析)
GC部分:HP-6890(Agilent公司製)
管柱:Inert Cap-1、長度60m、內徑0.25mm、膜厚1.5μm(GL Sciences公司製)
管柱溫度:在40℃下保持10分鐘,接著以20℃/分鐘進行升溫,之後在240℃下保持10分鐘
MS部分:5973 NETWORK(Agilent公司製)
偵檢器:EI型(加速電壓:70eV)
‧氮及氧含量的測定(氣相層析法分析)
GC部分:HP-7890(Agilent公司製)
管柱:HP-5 長度30m、內徑0.32mm、膜厚0.25μm(Agilent公司製)
管柱溫度:在40℃下保持5分鐘,接著以5℃/分鐘進
行升溫,之後在65℃下保持1分鐘
氣體取樣器:100℃
載體氣體:氦
偵檢器:TCD+脈衝放電型
‧含水量測定(FT-IR)
IG-1000(大塚電子公司製)
槽長度:10m
[製造例]
(粗製的1H-七氟環戊烯的製造)
在直徑1吋、長度1m的SUS316製反應管中填充35g之載持2%Pd-0.2%Bi的活性碳(粒徑約3mm)觸媒,透過質流控制器以1500ml/分鐘的速度持續供給氫氣2小時。反應管循環接觸熱媒並加溫至150℃,維持此溫度。之後,將氫氣的流量調整至830ml/分鐘,使用泵並以5g/分鐘的速度將作為原料的1-氯七氟環戊烯供給至已加溫到100℃的汽化器,接著導入至反應管。從反應管出來的氣體對裝在玻璃燒瓶中的氫氧化鉀水溶液進行起泡,而且將從玻璃燒瓶內出來的氣體成分收集到經乾冰/乙醇冷卻的玻璃收集器中。繼續此反應約2個禮拜,得到約79kg的粗製的1H-七氟環戊烯。以氣相層析法分析所得到的粗製的1H-七氟環戊烯,結果為主要含有1H-七氟環戊烯59.77重量%、1-氯七氟環戊烯12.26重量%、1H,1H,2H-七氟環戊烷11.55重量%、1H,2H-六氟環戊烯1.33重量%及六氟環戊烷10.26重量%的混合物。
[試樣1的調製]
在附有理論板數50板(填充劑、商品名:Sulzer packing)的管柱之SUS316製精餾塔的容量50L釜中,裝入35.7kg的以製造例製造之粗製的1H-七氟環戊烯,將釜加溫至100℃。在回流用冷凝器中使約10℃的冷卻水循環,使其全回流約12小時而使其在系統內穩定化。當精餾塔的塔頂部的溫度變成46℃時,以回流比40:1開始餾分的提取。得到24.6g的經蒸餾精製的1H-七氟環戊烯(以加入的1H-七氟環戊烯為基準,產率70%)。
接著,在容量20L的SUS316製槽(內面:電解研磨處理)中裝入22kg的已蒸餾精製的1H-七氟環戊烯。在直徑1吋×長度60cm的SUS316製管中填充200cm3的分子篩3A(UNION SHOWA K.K.製),使用泵供給裝在SUS槽內的1H-七氟環戊烯,進行水分去除。從SUS製管的出口出來的1H-七氟環戊烯送回至SUS316製槽中,使其循環。經過8小時後,將SUS316製槽內的1H-七氟環戊烯(約100g)取樣至小型的鋼瓶。使用FT-IR之水分分析,結果為已取樣的1H-七氟環戊烯的含水量為9重量ppm。
再者,在容量20L的SUS316製釜的上部組裝短柱及冷凝器、及設製有接受器的簡單蒸餾裝置,冷凝器係以10℃的冷卻水進行循環。在釜中裝入已去除水分的1H-七氟環戊烯(15kg),將釜加溫至80℃。使用氣相層析法測定此時的1H-七氟環戊烯中的氮及氧濃度,結果分別為1418體積ppm及638體積ppm。相對於裝入的1H-七氟環戊烯而言,提取30重量%至接受器時,停止簡單蒸餾,將釜冷卻至室溫為止。將釜內的1H-七氟環戊烯填充10kg
至附有隔膜式閥之容量10L的錳鋼製鋼瓶(內面粗度:1S)中。將以氣相層析法分析此已填充1H-七氟環戊烯1(試樣(1))的內容物之結果、測定氮、氧及水分濃度的結果顯示於表1。
[試樣2~6的調製]
精餾條件中除了變更回流比及蒸餾次數以外,與(試樣1的調製)同樣地進行,得到填充於鋼瓶中的1H-七氟環戊烯的試樣2~6。將以氣相層析法分析填充有所得到的試樣2~6之內容物之結果、測定氮及氧濃度以及水分濃度之結果顯示於表1。
F7E:1H-七氟環戊烯
MCL:1-氯七氟環戊烯
C5ClF9:氯九氟環戊烷
F8E:八氟環戊烯
C5HF7O:七氟環戊酮
[評價方法]
(1)1H-七氟環戊烯的純度變化確認試驗
蒸餾精製後,進行確認從填充在鋼瓶內的狀態連續地供給進行水分去除且進行簡單蒸餾所得到的1H-七氟環戊烯時的純度變化之試驗。
透過質流控制器,以25sccm/分鐘的速度從容器餾出1H-七氟環戊烯,依據表2記載的各餾出時間,使用氣相層析法調查1H-七氟環戊烯的純度與有機氯系化合物的濃度。
(2)1H-七氟環戊烯的乾式蝕刻評價
使用CCP(電容耦合電漿)方式的乾式蝕刻裝置,進行實行確認從填充在鋼瓶內的狀態連續供應時的純度變化之試驗的1H-七氟環戊烯的蝕刻評價。
在膜厚2μm的矽氧化膜上塗布0.6μm的光阻劑作為遮罩,將已形成0.1μm的孔型樣的矽晶圓(直徑20cm)安裝在蝕刻裝置的腔室內,將系統內作成真空後,分別以300sccm、25sccm及30sccm的流量導入氬氣、1H-七氟環戊烯及氧氣,將壓力維持在10mTorr,實施乾式蝕刻2分鐘。
以使用餾出時間25小時後的1H-七氟環戊烯時的蝕
刻速度為基準,將在任意時間餾出時的1H-七氟環戊烯作為乾式蝕刻用氣體而進行評價。
[評價結果]
進行所得到之試樣(1)~(6)的純度變化確認試驗及乾式蝕刻評價,將其結果顯示於表2。
如同由表2可以看出,從純度變化確認試驗的結果得知,沸點比1H-七氟環戊烯還高的有機氯系化合物(1-氯七氟環戊烯及氯九氟環戊烷)會隨著從容器餾出的時間而濃縮。又,從乾式蝕刻評價的結果得知,在有機氯系化合物濃度為350重量ppm以下的情況下,蝕刻速度的降低在餾出750小時後亦為10%以下(試樣1~4)。
另一方面,在有機氯系化合物濃度為407重量ppm的情況下,蝕刻速度降低在餾出600小時後為11%以上(試樣5)。又,在有機氯系化合物濃度為558重量ppm的情況下,蝕刻速度降低在餾出400小時後為11%以上,在餾出650小時後蝕刻停止(試樣6)。
Claims (8)
- 一種1H-七氟環戊烯,其特徵在於:純度為99.9重量%以上,而且含有有機氯系化合物,該有機氯系化合物的含量為350重量ppm以下。
- 如請求項1之1H-七氟環戊烯,其係經由步驟(1)及步驟(2)而得者,其中步驟(1):藉由氣相反應而在觸媒存在下將1-氯七氟環戊烯氫化,得到粗製的1H-七氟環戊烯;步驟(2):使用理論板數為50板以上的精餾塔精製步驟(1)所得到之粗製的1H-七氟環戊烯。
- 如請求項1之1H-七氟環戊烯,其中有機氯系化合物為氯九氟環戊烷及/或氯七氟環戊烯。
- 如請求項1之1H-七氟環戊烯,其中含氮量為100體積ppm以下,且含氧量為50體積ppm以下。
- 如請求項3之1H-七氟環戊烯,其中含水量為20重量ppm以下。
- 一種使用1H-七氟環戊烯作為乾式蝕刻氣體的方法,其係使用如請求項1至5中任一項之1H-七氟環戊烯作為乾式蝕刻氣體的方法。
- 一種使用1H-七氟環戊烯作為電漿CVD的反應氣體的方法,其係使用如請求項1至5中任一項之1H-七氟環戊烯作為電漿CVD的反應氣體的方法。
- 一種附有閥的容器,其係填充如請求項1至5中任一項之1H-七氟環戊烯而成。
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