JP2001523768A - 有機薄膜の低圧蒸着 - Google Patents
有機薄膜の低圧蒸着Info
- Publication number
- JP2001523768A JP2001523768A JP2000521253A JP2000521253A JP2001523768A JP 2001523768 A JP2001523768 A JP 2001523768A JP 2000521253 A JP2000521253 A JP 2000521253A JP 2000521253 A JP2000521253 A JP 2000521253A JP 2001523768 A JP2001523768 A JP 2001523768A
- Authority
- JP
- Japan
- Prior art keywords
- organic
- reaction chamber
- substrate
- tube
- pipe
- Prior art date
- 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.)
- Withdrawn
Links
- 239000010409 thin film Substances 0.000 title claims abstract description 36
- 230000008021 deposition Effects 0.000 title claims description 26
- 239000002243 precursor Substances 0.000 claims abstract description 67
- 239000000758 substrate Substances 0.000 claims abstract description 57
- 238000000034 method Methods 0.000 claims abstract description 55
- 238000006243 chemical reaction Methods 0.000 claims description 57
- 239000000463 material Substances 0.000 claims description 45
- 239000010408 film Substances 0.000 claims description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 21
- 239000007789 gas Substances 0.000 claims description 21
- 239000012044 organic layer Substances 0.000 claims description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 239000000376 reactant Substances 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- 238000007740 vapor deposition Methods 0.000 claims description 4
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052743 krypton Inorganic materials 0.000 claims description 2
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 claims description 2
- IBHBKWKFFTZAHE-UHFFFAOYSA-N n-[4-[4-(n-naphthalen-1-ylanilino)phenyl]phenyl]-n-phenylnaphthalen-1-amine Chemical compound C1=CC=CC=C1N(C=1C2=CC=CC=C2C=CC=1)C1=CC=C(C=2C=CC(=CC=2)N(C=2C=CC=CC=2)C=2C3=CC=CC=C3C=CC=2)C=C1 IBHBKWKFFTZAHE-UHFFFAOYSA-N 0.000 claims description 2
- 229910052754 neon Inorganic materials 0.000 claims description 2
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 2
- AYEKOFBPNLCAJY-UHFFFAOYSA-O thiamine pyrophosphate Chemical compound CC1=C(CCOP(O)(=O)OP(O)(O)=O)SC=[N+]1CC1=CN=C(C)N=C1N AYEKOFBPNLCAJY-UHFFFAOYSA-O 0.000 claims description 2
- 229910052724 xenon Inorganic materials 0.000 claims description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 2
- 230000008016 vaporization Effects 0.000 claims 4
- 238000005516 engineering process Methods 0.000 abstract 1
- 238000000151 deposition Methods 0.000 description 34
- 239000010410 layer Substances 0.000 description 30
- 239000012159 carrier gas Substances 0.000 description 23
- 239000011521 glass Substances 0.000 description 8
- 230000003287 optical effect Effects 0.000 description 8
- 230000008901 benefit Effects 0.000 description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 239000002019 doping agent Substances 0.000 description 4
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 4
- 239000011368 organic material Substances 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- -1 bis- (8-hydroxyquinoline) aluminum Chemical compound 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000012937 correction Methods 0.000 description 3
- CSJLBAMHHLJAAS-UHFFFAOYSA-N diethylaminosulfur trifluoride Substances CCN(CC)S(F)(F)F CSJLBAMHHLJAAS-UHFFFAOYSA-N 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- YLYPIBBGWLKELC-RMKNXTFCSA-N 2-[2-[(e)-2-[4-(dimethylamino)phenyl]ethenyl]-6-methylpyran-4-ylidene]propanedinitrile Chemical compound C1=CC(N(C)C)=CC=C1\C=C\C1=CC(=C(C#N)C#N)C=C(C)O1 YLYPIBBGWLKELC-RMKNXTFCSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 239000004305 biphenyl Substances 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- ZYGHJZDHTFUPRJ-UHFFFAOYSA-N coumarin Chemical compound C1=CC=C2OC(=O)C=CC2=C1 ZYGHJZDHTFUPRJ-UHFFFAOYSA-N 0.000 description 2
- 239000003599 detergent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 230000005525 hole transport Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- VUQUOGPMUUJORT-UHFFFAOYSA-N methyl 4-methylbenzenesulfonate Chemical compound COS(=O)(=O)C1=CC=C(C)C=C1 VUQUOGPMUUJORT-UHFFFAOYSA-N 0.000 description 2
- BQJCRHHNABKAKU-KBQPJGBKSA-N morphine Chemical compound O([C@H]1[C@H](C=C[C@H]23)O)C4=C5[C@@]12CCN(C)[C@@H]3CC5=CC=C4O BQJCRHHNABKAKU-KBQPJGBKSA-N 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 229920000128 polypyrrole Polymers 0.000 description 2
- 238000002390 rotary evaporation Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002207 thermal evaporation Methods 0.000 description 2
- 238000001947 vapour-phase growth Methods 0.000 description 2
- 125000001637 1-naphthyl group Chemical group [H]C1=C([H])C([H])=C2C(*)=C([H])C([H])=C([H])C2=C1[H] 0.000 description 1
- IEJPPSMHUUQABK-UHFFFAOYSA-N 2,4-diphenyl-4h-1,3-oxazol-5-one Chemical compound O=C1OC(C=2C=CC=CC=2)=NC1C1=CC=CC=C1 IEJPPSMHUUQABK-UHFFFAOYSA-N 0.000 description 1
- ZNJRONVKWRHYBF-VOTSOKGWSA-N 4-(dicyanomethylene)-2-methyl-6-julolidyl-9-enyl-4h-pyran Chemical compound O1C(C)=CC(=C(C#N)C#N)C=C1\C=C\C1=CC(CCCN2CCC3)=C2C3=C1 ZNJRONVKWRHYBF-VOTSOKGWSA-N 0.000 description 1
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 241000283986 Lepus Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 229960000956 coumarin Drugs 0.000 description 1
- 235000001671 coumarin Nutrition 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000003113 dilution method Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000005401 electroluminescence Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002052 molecular layer Substances 0.000 description 1
- 229960005181 morphine Drugs 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- ZUQDDQFXSNXEOD-UHFFFAOYSA-N quinoxalin-5-ol Chemical compound C1=CN=C2C(O)=CC=CC2=N1 ZUQDDQFXSNXEOD-UHFFFAOYSA-N 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- YYMBJDOZVAITBP-UHFFFAOYSA-N rubrene Chemical compound C1=CC=CC=C1C(C1=C(C=2C=CC=CC=2)C2=CC=CC=C2C(C=2C=CC=CC=2)=C11)=C(C=CC=C2)C2=C1C1=CC=CC=C1 YYMBJDOZVAITBP-UHFFFAOYSA-N 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 1
- 230000007723 transport mechanism Effects 0.000 description 1
- TVIVIEFSHFOWTE-UHFFFAOYSA-K tri(quinolin-8-yloxy)alumane Chemical compound [Al+3].C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1 TVIVIEFSHFOWTE-UHFFFAOYSA-K 0.000 description 1
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 1
- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
Classifications
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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
- C23C16/448—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 characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4481—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 characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation using carrier gas in contact with the source material
- C23C16/4482—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 characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation using carrier gas in contact with the source material by bubbling of carrier gas through liquid source material
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/50—Substrate holders
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/12—Organic material
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/26—Vacuum evaporation by resistance or inductive heating of the source
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
- C23C14/568—Transferring the substrates through a series of coating stations
-
- 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
-
- 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
- C23C16/455—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 characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45561—Gas plumbing upstream of the reaction chamber
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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Abstract
Description
及び有機発光デバイスで利用されるそのような薄膜の低圧製造に関する。
る。ディスプレイへの潜在的な用途に刺激されて、有機発光デバイス(OLED
)は、3%を越える外部量子効率を達成し、ビデオ輝度で10,000時間の程
度の作動寿命を達成することができる。低分子とポリマーの両方をベースとする
OLEDが知られているが、ポリマーベースのデバイスは回転蒸着法により簡単
で安価に製造できる一般的利点を有する。これに対し、低分子によるデバイスは
、通常真空中での熱的蒸発により製造されており、それは通常回転蒸着よりも高
価な方法である。OLED構造及び処理方法の例は、公開されたPCT出願WO
96/19792(言及することによって本明細書に組み入れる)に与えられ
ている。
り、ディスプレイ等の多くの潜在的光学的デバイス用途を持つ低分子量の有機層
の低コストで大規模な蒸着が進歩してきた。OVPD法はホレスト(Forrest)等 の米国特許第5,554,220号明細書、S.R.ホレスト等の「有機蒸着に
より成長させた有機塩薄膜の強力な二次調波発生及び長距離構造配列」(Intense
Second Harmonic Generation and Long-Range Structural Ordering in Thin F
ilms of an Organic Salt Grown by Organic Vapor Phase Deposition)、68 App
l. Phys. Lett., 1326 (1996)、及びP.E.バローズ(Burrows)等の「有機蒸 着:大きな光学的非線形性を持つ有機薄膜の新規な成長方法」(Organic Vapor P
hase Deposition: a New Method for the Growth of Organic Thin Films with
Large Optical Non-linearities)、156 J. of Crystal Growth 91 (1995)(それ
らは言及することによって本明細書に組み入れる)に記載されている。
が凝縮して希望の薄膜を形成する。例えば、OVPD法を用いて、揮発性前駆物
質、沃化4′−ジメチルアミノ−N−メチル−4−スチルバゾリウム(DASI
)及びメチルp−トルエンスルホネート(メチルトシレート、MT)をキャリヤ
ーガスにより加熱された基体へ運ぶことにより、光学的に非線形の有機(NLO
)塩、4′−ジメチルアミノ−N−メチル−4−スチルバゾリウムトシレート(
DASI)の膜を蒸着してきた。この方法ではDASIが熱分解して4−ジメチ
ルアミノ−4−スチルバゾール(DAS)を形成し、それが次にMTと反応して
基体上にDASTを形成する。
OVPDは多成分薄膜の正確な化学量論的成長を行うための唯一の方法であると
考えられている。しかし、OVPD法は大気圧で行われ、大気圧又はその近くで
成長する膜は屡々粗く、気相核生成及び拡散律速成長過程により不均一な表面形
態を有する。
いる。一つの態様として、本発明は、基体上に有機薄膜を形成する方法において
、複数の有機前駆物質を与え、然も前記有機前駆物質は気相になっており、前記
基体を存在させて減圧で前記複数の有機前駆物質を反応させて前記基体上に薄膜
を形成する諸工程からなる方法にある。別の態様として、本発明は、そのような
方法により製造された有機膜を包含する。更に別の態様として、本発明は、大気
の常態値以下の圧力で有機前駆物質の反応を促進して基体上に有機膜を形成する
ように設計された装置を含む。
ができる多成分有機薄膜を与えることである。
る。
成長させる低圧有機蒸着法及び装置を与えることである。
成させる低圧有機分子ビーム蒸着法及び装置を与えることである。
る方法及び装置を与えることである。
法及び装置を与える。本発明の方法は、ここでは低圧有機蒸着(LPOVPD)
として規定する。本発明のLPOVPD法は、多成分有機薄膜の蒸着を正確精密
に制御することができる。更に、本発明の薄膜は、表面粗さが小さいと言った優
れた表面性を特徴とする。
0は、反応管12のような反応室及び反応室中へ伸びる配管を有する。反応管1
2は、実験装置では、例えば、10cmの直径及び約45cmの長さのような適
当な大きさを有する円筒である。反応管12は、ガラス又は石英のような適当な
材料から作られている。坩堝14のような開口容器には第一有機前駆物質材料が
入っており、反応管12の一方の端20に近い管36内に配置されている。別法
として、坩堝14は直接反応管12上に置かれているか、又はその中の棚又は管
に配置されている。坩堝14は、実質的に反応管12を取り巻く多領域加熱器/
冷却器18により加熱又は冷却される。坩堝14の温度制御により、坩堝14内
の第一有機前駆物質材料の熱分解又は蒸発を与えることになる。不活性キャリヤ
ガスの調節した流れ30を、管36を通って反応室中へ送り、それにより第一有
機前駆物質の蒸気を反応管12に沿ってその排出端22の方へ流す。不活性キャ
リヤガスは、窒素、ヘリウム、アルゴン、クリプトン、キセノン、ネオン等の不
活性ガスである。水素、アンモニア、メタン等の還元性を持つガスも多くの有機
材料に対しては不活性である。これらの還元性ガスを使用することにより、望ま
しくない過剰の反応物の燃焼を助ける付加的利点が屡々得られる。
なくとも二つの流路30及び38を通って反応管12中へ送られる。一つの流路
30は、直列に接続された圧力調節器32、流量計34、及び高速切り替えバル
ブ35を有し、そこからキャリヤガスが反応管12の端20中へ送られる。第二
流路38は、直列に接続された圧力調節器40、流量計42に、及び高速切り替
えバルブ39を有し、そこからキャリヤガスがバブラー(bubbler)46中へ流れ 、そのバブラーには第二有機前駆物質材料48が入っている。第二有機前駆物質
材料48の温度制御をし易くするため、バブラー46は容器52内の浴50内に
部分的に浸漬されている。タンク24からの不活性ガスは、第二有機前駆物質4
8を気泡として通り、配管54を通って第二有機前駆物質48の蒸気を反応管1
2中へ運ぶ。この工程中、管54は、気化した第二有機前駆物質48がバブラー
から反応室へ移動する間に再び凝縮しないように充分高い温度に維持されなけれ
ばならない。
物の温度のような処理パラメータにより制御される。LPOVPD法は、前駆物
質又は反応物の蒸気圧又は化学的性質とは無関係に、圧力質量流量制御器を用い
てそれらの正確な計量を与える。本発明の方法は、このようにして希望の膜の製
造に必要な比率で非常に異なった特性を持つ材料の組合せを可能にする。
ど瞬間的にオン・オフの切り替えを行うことができる。これらのバルブは前駆物
質流を反応器12又はバイパス管(図示せず)中へ送り、どの時間においても異
なった前駆物質流が反応器12中へ入り、異なった組成及び特性の膜を蒸着する
ことができる。バルブ39は、バブラー46へ入るキャリヤガスの調節も行う。
バルブ35及び39は、このようにして反応器12中へ入る反応物の流れを迅速
に変化し、成長する膜の性質及び組成を変化させ得る。従って、例えば、各文字
が異なった分子層又は組成を表すものとして、ABAB、ABCABC、ABA
BCAB、及びABCDABCD−型の膜を成長させることができる。
所に取付ける。基体58上に蒸着しなかった有機蒸気の殆どは、ポンプ66より
上流に配置されたトラップ64中で凝縮する。トラップ64には、例えば液体窒
素又は中性フルオロカーボンオイルが入っている。スロットルバルブ68は反応
器10中の圧力を調節する。適当な圧力ゲージを反応器に取付け(図示せず)、
反応器中に希望の圧力を維持するように制御スロットルバルブ68に電気的フィ
ードバックを行う。
る。受容体層、供与体層、及び単一成分層のいかなる組合せに対しても、実際の
圧力は、前駆物質材料を蒸発するために必要な温度、前駆物質材料の凝縮を防ぐ
壁温度、及び反応領域温度勾配に関連して実験的に決定する。圧力の最適選択は
、各蒸着される有機層の要件に特有のものである。例えば、トリス−(8−ヒド
ロキシキノリン)アルミニウム(Alq3)又はN,N′−ジフェニル−N,N−
ビス(3−メチルフェニル) 1,1′−ビフェニル−4,4′ジアミン(TP
D)等の単一成分層の蒸着のための最適圧力は約0.1〜10トールである。
般に使用される材料から選択されるのが典型的である。例えば、そのような材料
には、ガラス、石英、珪素、砒化ガリウム及び他のIII−V半導体、アルミニウ ム、金及び他の貴金属及び卑金属、ポリマー膜、二酸化珪素及び窒化珪素、イン
ジウム錫酸化物等が含まれる。高品質の光学的薄膜のためには、蒸着した有機膜
と結晶性相互作用を与えてエピタキシャル成長を起こす基体を用いるのが好まし
い。そのようなエピタキシャル成長を達成するためには、蒸着すべき膜と同様な
結晶構造を有する非極性有機物で基体を被覆することが屡々必要である。
々好ましい。基体温度の独立した制御は、例えば、水、ガス、フレオングリセリ
ン、液体窒素等の物質を循環させるためのチャンネルを有する温度制御ブロック
60を基体58と接触させることにより達成する。基体は、ブロック60上又は
その近くに配置した抵抗又は輻射線加熱器を使用することにより加熱することも
できる。
ブラー46Nを含ませるように拡大し得る。同様に、多重キャリヤガス流路30
Nを用いて坩堝14Nからの更に付加的前駆物質を送る。別法として、坩堝14
、14Nは、付加的前駆物質を処理するため反応管12中の棚上又は管中に垂直
方向に重ねることもできる。蒸着すべき有機膜により、一つ以上の流路30及び
38を単独又は組合せて用い、必要な前駆物質材料を与えることができる。
着することができる。ここで用いる「反応」とは、前駆物質反応物が明確な反応
生成物を形成する化学反応を意味するか、又は別法としてそれは前駆物質材料の
組合せ又は混合物を単に意味するか、又は前駆物質材料が供与体・受容体、又は
ゲスト・ホストの関係を形成する場合を意味する。例えば、本発明に従い、列挙
した前駆物質の反応により薄膜として次のNLO物質が形成される:
物質は、例えば、テトラチスファルバレン(tetrathisferlvalene)(TFF)及び
7,7,8,8−テトラシアノキノジメタン(TCNQ)からなる。混合工程は
、基体上に蒸着する電荷移動錯体TTF−TCNQを与える結果になる。OLE
Dに関する別の例では、4−(ジシアノメチレン)−2−メチル−6−(p−ジ
メチルアミノスチリル)−4H−ピラン(DCM)を大きな流量のキャリヤーガ
ス流中に添加し、一方、Alq3を低流量のキャリヤガス中に添加する。次にこ れらの流れを中心反応管中で混合し、それによりホストマトリックス膜中のゲス
ト分子を希望通りに希釈し、単一の発光層を形成する。Alq3ホスト中の他の ゲスト分子の例は、5,10,15,20−テトラフェニル−21H,23H−
ホルフィン(TPP)、ルブレン(Rubrene)、DCM2、クマリン等である。別 法として、効率的な広範な色の変化を達成するため、単一ホスト中に多種ドーパ
ントを添加してもよい。
TPD、α−4,4′−ビス[N−(1−ナフチル)−N−フェニル−アミノ]
ビフェニル(α−NPD)、又はMTDATA等のホール輸送層(HTL)、又
はこれらの層のドープした組合せからなる二相発光デバイスは、連続的にHTL
及びELを希望の厚さに成長させることにより形成する。次にそれら有機層の上
に付加的層を成長させるか、又はトリメチル・インジウム、トリメチル・ガリウ
ム等のような有機金属原料を用いて金属接点(コンタクト,contact)層を成長さ せる。
応器70及び方法を包含する。反応器70は、改良した超高真空室71及びバル
ブ72に接続されたターボ分子ポンプ等の真空ポンプ(図示せず)を有する。室
71中の典型的な室基底圧力は10-3〜10-11トールである。反応器70を用 いた有機層蒸着法は、有機分子ビーム蒸着(OMVD)と呼ばれている。LPO
VPD及びOMVDの両方共有機層を蒸着するのに減圧を用いているが、これら
の方法の原理的差は、後者では分子平均自由行程が室70の大きさに匹敵するか
、又はそれより大きいことである。比較として、LPOVPDの平均自由行程は
、ガス反応器の大きさよりもかなり短い。従って、OMVDはインジェクタから
基体へ高度に配向した「分子ビーム」の形成を可能にし、成長膜厚さ、純度及び
形態の正確な速度論的制御を可能にする。
ラー74は容器76中に入れられ、温度制御浴80中に浸漬されている。高純度
不活性キャリヤガス78が第一前駆物質75を気泡として通り、各蒸気を加熱さ
れた配管79を通ってインジェクタ82により真空室71中へ運ぶ。室71中に
入ると、前駆物質蒸気は分子ビーム83を形成し、それが基体85に衝突する。
基体85には、例えば、冷却剤入口81のような温度を制御するための手段が配
備されている。
配備されており、その中には第二前駆物質材料88が入っている。K−セル86
は、真空中で蒸発物を流出させるための均一に加熱され、制御された炉である。
例えば、K−セル86はDASI又は他の前駆物質を分解するまで加熱され、得
られたDASを昇華し、それを分子ビーム89として反応器70中へ注入する。
別法として、K−セル86は、単にAlq3等の単一成分物質を昇華するだけで ある。別法として、K−セル86には、加熱によりガス流中に昇華又は蒸発され
る分子物質の濃度を希釈するのに用いられるキャリヤガス入口が取付けてある。
この希釈方法は、浴80及びクヌーセン・セル86の温度の外、バブラー74へ
のキャリヤガス78の流れを制御することにより、DCM−Alq3等のゲスト ・ホスト系の正確なドーピング量を達成するのに特に有用である。
膜の厚さを石英結晶93により監視する。試料ホールダ90は回転して前駆物質
材料の均一な蒸着及び反応を確実に与える。前駆物質材料の蒸着は、更に分子ビ
ーム83及び89を遮断するのに用いられるシャッタ87により制御する。
再蒸発された前駆物質材料のための最小値に維持するのに役立つ。前駆物質材料
が移動して互いに汚染することがないように隔壁92を配備するのも好ましい。
、高速切り替えバルブ、バイパス導管等の多くのものが配備されている。反応器
70には、多重クヌーセンセル及びバブラーを、基体85の上に複数の前駆物質
材料を蒸着するために取付けることができる。反応器70は、試料導入のための
「ロード・ロック(load-lock)」を有するのが好ましい。ロード・ロック94は ドア95及び真空ポンプ96を有し、室71の圧力を低下することなく、試料の
交換を与えることができる。
体上に有機層を連続的に蒸着できるように修正する。図3の装置は、導入室14
6、有機層蒸着室150及び152、接点蒸着室154、及び取出し室156の
ような複数の真空室を有する。例として、各蒸着室は図1のLPOVPD反応器
10である。基体137はコンベヤベルト148に乗せて室150、152、1
54及び156の各々を通って運ぶ。図3に示した態様では、室150、152
及び154は、夫々輻射熱源158、160及び162を有し、有機蒸気の凝縮
を防ぐ。図3には唯二つの有機層蒸着室150及び152しか示されていないが
、希望に応じて付加的室を配備する。導入室146から有機層蒸着室150及び
152へ、また接点蒸着室154から取出し室156へ送られる間に、基体13
7は空気遮断部(図示せず)を通過し、室150、152及び154の中の真空
を低下しないようにしてある。OLEDに関する例として、室150及び152
を夫々TPD及びAlq3の蒸着のために用い、室154をMg:Ag接点層を 蒸着するために用いる。
に示すように、有機前駆物質材料の蒸着のための反応物ガス分配器(RGD)1
08が含まれている。RGD108は、図1及び2の有機前駆物質導入機構の代
替物として用いられ、ガスカーテン、120、120′、120″及び120″
′を与えるのに用いられる。RGD108は、多種有機前駆物質を蒸着する場合
に、それら前駆物質が基体上に蒸着されるまで分離されているのを確実にし、そ
れにより前駆物質の反応を行わせることができる。RGD108には、加熱器1
22、第二キャリヤガス入口112及びガスマニホルド132が含まれる。加熱
器122は、有機前駆物質材料の凝縮が速過ぎるのを防ぐ。RGD108の上に
は第一キャリヤガス入口114及び分配器板110が存在する。第一キャリヤガ
ス入口114は、例えば、MT等の一般に低揮発性第一有機前駆物質を通常運ぶ
ガスを供給する。第一キャリヤガスは、例えば、ワイヤ網、ガラスフィルタ材料
、又は多孔質ステンレス鋼板である分配器板110を通って反応室へ入る。分配
器板110を通って流れるキャリヤガスのカラムは、RGD108により陰にな
っている。RGD108は、例えばDAS等の一般に低い蒸気圧の第二有機前駆
物質の平面状ガスカーテン120を与える。第二有機前駆物質を含む第二キャリ
ヤガスは、入口112から入り、ガスマニホルド132の中へ送られる。マニホ
ルド132は、環状空洞126中へ第二キャリヤガスを供給するための並んだ孔
134を有する中空管であり、その環状空洞はマニホルド132を取り巻いてい
る。第二キャリヤガスはスリット136を通ってRGD108を出、それによっ
て平面状カーテンの形態をそれに与える。
role)、金属有機化合物等の蒸気からなる。もし望むならば、OLEDにより発 する光の色の制御又は調節を、Alq3層の適当なドーピングにより行うことが でき、室152中の付加的RGDデバイス108によりドーパント蒸気のカーテ
ン120″′を与える。
」基体搬送装置を用いることにより修正する。図5に示す搬送装置は、大面積可
撓性基体上に有機薄膜を蒸着するのに適している。例えば、基体180はポリマ
ーシート又は金属箔からなり、ロール181からロール182へ送る。基体18
0への有機前駆物質の蒸着は、基体180がロール181から解かれた時に行わ
れ、従って図1の反応室へ露出されるか、又は図2及び3の分子ビーム又はカー
テンに夫々露出された時に行われる。ロール181及び182は、速度可変モー
タ等の適当な手段により駆動する。基体180がロール181からロール182
へ送られる速度は、基体180上に形成される有機膜の厚さを決定する。
されるものではない。
ラス及び可撓性ポリエステル基体を用いて、有機発光材料の層を成長させた。I
TOは装置のアノードを形成し、ガラス及びポリエステル基体に対し、夫々17
00Å及び1200Åの厚さを持ち、夫々10Ω及び60Ωのアノード抵抗を与
えた。ガラス基体は超音波浴中の洗剤溶液及び脱イオン水で濯ぎ、次に1,1,
1−トリクロロエタン中で沸騰させ、アセトンで濯ぎ、最後に2−プロパノール
で濯くことにより清浄にした。可撓性基体は、有機溶媒に曝すことによる損傷を
避けるため、洗剤及び2−プロパノール溶液だけで濯ぐことにより清浄にした。
表面上に蒸着した第一層はTPD、ホール輸送材料であった。特に、TPD蒸気
を窒素キャリヤガスにより坩堝14から基体28へ運んだ。TPD成長条件には
、200±5℃の原料温度、100sccmの窒素キャリヤガス流量、0.50
トールの反応器圧力、及び20分の成長時間が含まれる。100sccmの窒素
流量で、装置のレイノルズ数は〜500であり、層流領域内に充分入る操作であ
ることを示していた。TPD層は100〜300Åの厚さに成長させた。
lq3の電子輸送層を、別の窒素導管を開けて坩堝14NからAlq3蒸気を室1
2中へ運ぶことにより成長させた。Alq3成長条件には、247±8℃の原料 温度、50sccmの窒素流量、0.65トールの圧力、及び10分の成長時間
が含まれる。TPD及びAlq3の両方の蒸着中、水冷されたステンレス鋼基体 ホールダを用いて基体を15℃に維持した。TPD層は700〜1100Åの厚
さに成長させた。
加熱蒸着により適用した。接点(コンタクト)は、1000Åの厚さの保護Ag
層を蒸着させて完成した。
を与える結果になった。例えば、TPD及びAlq3 層を原子力顕微鏡で測定し
て、夫々6〜8Å及び9〜11ÅのRMS粗さを持っていた。得られたOLED
装置は、低電圧でI∝V、高電圧でI∝V9である電流・電圧特性を示した。I 対Vのパワー法則依存性(power law dependence of I on V)が変化するターン・
オン(turn-on)電圧、VTは約6Vであった。
80〜100℃に温度を維持した30cm3バブラー46中にMT48を入れた 。窒素ガスを用いてMT48に気泡として通し、それによりMT蒸気をガラス管
54を通って反応管12中へ、坩堝14を約5cm越えた位置の所から導入した
。その坩堝は反応管12の床上に置かれており、DASIが入っていた。反応管
12中の圧力を約10-2トールに維持した。DAS蒸気はMT蒸気と反応し、基
体ブロック60上に支持された基体58上にDASTの固体膜を形成した。過剰
の未反応MT蒸気及び揮発性副反応生成物を排出管62から排出した。かくして
形成したDAST膜は、例えば、光学的スイッチとして有用である。
機薄膜を製造する。本発明の種々の態様をここに示し記述してきたが、それらは
限定的意味を持たない。例えば、当業者はこれらの態様に或る修正を認めること
ができるであろうが、それら修正は特許請求の範囲の本質及び範囲に含まれる。
「高信頼性、高効率、集積可能な有機発光デバイス及びその製法」(High Reliab
ility, High Efficiency, Integratable Organic Light Emitting Devices and
Methods of Producing Same)、シリアル番号08/774,119(1996年
12月23日出願);「多色LEDのための新規な材料」(Novel Materials for
Multicolor LED's)、シリアル番号08/850,264(1997年5月2日
出願);「有機遊離ラジカルに基づく電子輸送及び発光層」(Electron Transpor
ting and Light Emitting Layers Based on Organic Free Radicals)、シリアル
番号08/774,120(1996年12月23日出願);「多色表示デバイ
ス」(Multicolor Display Devices)、シリアル番号08/772,333(19
96年12月23日出願);「赤色光有機発光デバイス(LED)」(Red-Emitt
ing Organic Light Emitting Devices (LED's))、シリアル番号08/774,
087(1996年12月23日出願);「積層有機発光デバイスのための駆動
回路」(Driving Circuit For Stacked Organic Light Emitting Devices)、シリ
アル番号08/792,050(1997年2月3日出願);「高効率有機発光
デバイス構造体」(High Efficiency Organic Light Emitting Device Sturcture
s)、シリアル番号08/772,332(1996年12月23日出願);「真
空蒸着した非ポリマー可撓性有機発光デバイス」(Vacuum Deposited, Non-Polym
eric Flexible Organic Light Emitting Devices)、シリアル番号08/789 ,319(1997年1月23日出願);「メサピクセル構造を有するディスプ
レイ」(Displays Having Mesa Pixel Configuration)、シリアル番号08/79
4,595(1997年2月3日出願);「積層有機発光デバイス」(Stacked O
rganic Light Emitting Devices)、シリアル番号08/792,048(199
7年2月3日出願);「高コントラスト透明有機発光デバイス表示器」(High Co
ntrast Transparent Organic Light Emitting Device Display)シリアル番号0 8/821,380(1997年3月20日出願);「ホスト物質として5−ヒ
ドロキシ−キノキサリンの金属錯体を含む有機発光デバイス」(Organic Light E
mitting Devices Containing A Metal Complex of 5-Hydroxy-Quinoxaline as A
Host Materials)、シリアル番号08/838,099(1997年4月15日
出願);「大きな輝度を有する発光デバイス」(Light Emitting Devices Having
High Brightness)、シリアル番号08/844,353(1997年4月18 日出願);「有機半導体レーザ」(Organic Semiconductor Laser)、シリアル番 号60/046,061(1997年5月9日出願);「有機半導体レーザ」(O
rganic Semiconductor Laser)、シリアル番号08/859,468(1997 年5月19日出願);「飽和天然色積層有機発光デバイス」(Saturated Full Co
lor Stacked Organic Light Emitting Devices)、シリアル番号08/858, 994(1997年5月20日出願);「ホール注入促進層を有する有機発光デ
バイス」(An Organic Light Emitting Device Containing a Hole Injection En
hancement Layer)、シリアル番号08/865,491(1997年5月29日
出願);「伝導性層のプラズマ処理」(Plasma Treatment of Conductive Layers
)、シリアル番号PCT/US97/10252(1997年6月12日出願) ;「有機多色ディスプレイを製造するための薄膜パターン化」(Patterning of T
hin Films for the Fabrication of Organic Multi-color Displays)、シリアル
番号PCT/US97/10289/(1997年6月12日出願);「二重ヘ
テロ構造赤外線及び垂直空洞表面発光有機レーザ」(Double Heterostructure In
frared and Vertical Cavity Surface Emitting Organic Lasers)、シリアル番 号60/053,176(1997年7月18日出願);「オレッド含有熱安定
性不斉電荷キャリヤ材料」(Oleds Containing Thermally Stable Asymmetric Ch
arge Carrier Materials)、シリアル番号08/929,029(1997年9 月8日出願);「オレッド積層体を有する発光デバイス及び燐光体周波数逓降変
換器」(Light Emitting Device with Stack of Oleds and Phosphor Downconver
ter)、シリアル番号08/925,403(1997年9月9日出願);「有機
発光デバイス中のインジウム錫酸化物層を蒸着するための改良方法」(An Improv
ed Method for Depositing Indium Tin Oxide Layers in Organic Light Emitti
ng Devices)、シリアル番号08/928,800(1997年9月12日出願 );「オレッドの発光層中のアズラクトン関連ドーパント」(Azlactone-Related
Dopants in the Emissive Layer of an Oled)、シリアル番号08/948,1
30(1997年10月9日出願);「非金属カソードを用いた高透明性有機発
光デバイス」(A Highly Transparent Organic Light Emitting Device Employin
g A Non-Metallic Cathode)、(1997年11月3日出願)、代理人書類番号 10020/40(暫定出願)、及び「非金属カソードを用いた高透明性有機発
光デバイス」(A Highly Transparent Organic Light Emitting Device Employin
g A Non-Metallic Cathode)、(1997年11月5日出願)、代理人書類番号 10020/44、各係属中の出願は、言及することによって本明細書に組み入
れる。本発明は、係属中の米国特許出願シリアル番号08/354,674、0
8/613,207、08/632,322、及び08/693,359、及び
暫定特許出願シリアル番号60/010,013、06/024,001、及び
60/025,501(これらの各々は言及することによってその全体を本明細
書に組み入れる)の各々の主題に関連して用いることもできる。
図である。
Claims (43)
- 【請求項1】 基体上に有機薄膜を形成する方法において、 複数の有機前駆物質を気相で与え、 基体を存在させて、大気の常態値以下の圧力で前記複数の有機前駆物質を反応
させ、該基体上に薄膜を形成する、 諸工程を有する、上記方法。 - 【請求項2】 基体を反応室中に配置する、請求項1記載の方法。
- 【請求項3】 複数の有機前駆物質の一つを、反応工程前に反応室中へ輸送
する工程を更に有する、請求項2記載の方法。 - 【請求項4】 輸送工程が、不活性ガスを用いて、輸送された有機前駆物質
を反応室へ運ぶ工程を含む、請求項3記載の方法。 - 【請求項5】 不活性ガスを、窒素、アルゴン、ヘリウム、ネオン、クリプ
トン及びキセノンからなる群から選択する、請求項4記載の方法。 - 【請求項6】 複数の有機前駆物質の少なくとも一つを、MT、DASI、
MM、MfM、DASTh、MeOSI、DAS(Et)I、DAS(Et)O H、トルエンスルホン酸アセチル、MAf、TTF、TCNQ、DCM、Alq3 、TPP、TPD、α−NPD、MTDATA、及び(Alq2)′−OPhか らなる群から選択する、請求項1記載の方法。 - 【請求項7】 輸送工程前に、輸送される有機前駆物質を気化する工程を更
に有する、請求項3記載の方法。 - 【請求項8】 気化工程が、輸送される有機前駆物質をバブラーへ導入する
工程を含み;輸送工程が、前記バブラーに不活性ガスを通して前記輸送される有
機前駆物質を反応室中に運ぶ工程を含む;請求項7記載の方法。 - 【請求項9】 気化工程が、輸送される有機前駆物質を開口容器中へ入れて
、該開口容器を加熱する工程を含み;しかも、輸送工程が、前記開口容器上に不
活性ガスを送り、前記輸送される有機前駆物質を反応室中に運ぶ工程を含む;請
求項7記載の方法。 - 【請求項10】 気化工程が、 反応室中へ伸びているクヌーセン・セルの中へ、輸送される有機前駆物質を導
入し、次いで 該クヌーセン・セルを加熱する、 諸工程を含む、請求項7記載の方法。 - 【請求項11】 基体を、回転試料ホールダに取付ける、請求項1記載の方
法。 - 【請求項12】 大気圧の常態値以下の圧力が約10-11〜102トールの範
囲内にある、請求項1記載の方法。 - 【請求項13】 請求項1に記載の方法により製造された有機膜。
- 【請求項14】 膜が発光材料を含む、請求項13記載の有機膜。
- 【請求項15】 膜が光学的非線形の材料を含む請求項13記載の有機膜。
- 【請求項16】 基体上に有機薄膜を形成する装置において、 反応室、 前記反応室を実質的に取り巻く加熱器、 前記反応室中へ伸びる配管、及び 前記反応室へ取付けられた真空ポンプ、 を具えた上記装置。
- 【請求項17】 反応室が反応管を有する、請求項16記載の装置。
- 【請求項18】 加熱器が多領域加熱器/冷却器である、請求項16記載の
装置。 - 【請求項19】 配管が、 第一端部及び、反応室中へ伸びる第二端部を有する管、及び 前記管の第一端部に接続されたガス源、 を有する、請求項16記載の装置。
- 【請求項20】 管の内部に配置された開口容器であって、有機前駆物質材
料を保持するための該開口容器を更に具えた、請求項19記載の装置。 - 【請求項21】 管が圧力調節器及びバルブを有する、請求項20記載の装
置。 - 【請求項22】 配管が、 第一端部及び第二端部を有する第一管であって、第一管の第二端部が反応室中
へ伸びている第一管、 第一管の第一端部に接続された、有機前駆物質材料を入れるためのバブラー、 第一端部及び第二端部を有する第二管であって、第二管の第二端部が前記バブ
ラーに接続されている第二管、並びに 第二管の第一端部に接続されたガス源、 を有する、請求項16に記載の装置。 - 【請求項23】 第二管が圧力調節器及びバルブを有する、請求項22に記
載の装置。 - 【請求項24】 基体と接触し、中にチャンネルを有する温度制御ブロック
を更に具えた、請求項16記載の装置。 - 【請求項25】 反応室に取付けられたトラップを更に具えた、請求項16
記載の装置。 - 【請求項26】 第一ロールと第二ロールとの間に基体を通すため、反応室
内に第一ロール及び第二ロールを更に具えた、請求項16記載の装置。 - 【請求項27】 基体上に有機薄膜を形成するための装置において、 反応室、 前記反応室中へ伸びるクヌーセン・セル、 基体に接続され、回転可能な試料ホールダ、及び 前記反応室に取付けられた真空ポンプ、 を具えた上記装置。
- 【請求項28】 反応室中へ伸びる配管を更に具え、然も、該配管が、 第一端部及び第二端部を有する第一管であって、第一管の第二端部が前記反応
室中へ伸びている第一管、 第一管の第一端部に接続された、有機前駆物質材料を入れるためのバブラー、 第一端部及び第二端部を有する第二管であって、第二管の第二端部が前記バブ
ラーに接続されている第二管、並びに 第二管の第一端部に接続されたガス源、 を有する、請求項27記載の装置。 - 【請求項29】 第一管が加熱されている、請求項27記載の装置。
- 【請求項30】 反応室中に冷却された囲いを更に具えた、請求項27記載
の装置。 - 【請求項31】 薄膜の厚さを検出するセンサを更に具えた、請求項27記
載の装置。 - 【請求項32】 センサが石英結晶である、請求項31記載の装置。
- 【請求項33】 反応室へ接続されたロード・ロックを更に具えた、請求項
27記載の装置。 - 【請求項34】 真空ポンプがターボ分子ポンプである、請求項27記載の
装置。 - 【請求項35】 第一ロールと第二ロールとの間に基体を通すため、反応室
中に第一ロール及び第二ロールを更に具えた、請求項27記載の装置。 - 【請求項36】 基体上に有機薄膜を形成するための装置において、 複数の真空室で、導入室及び有機層蒸着室を含めた複数の真空室、並びに 前記複数の真空室を通過するコンベアベルトで、その上に基体を有するコンベ
アベルト、 を具えた上記装置。 - 【請求項37】 有機層蒸着室が反応物ガス分配器を有する、請求項36記
載の装置。 - 【請求項38】 有機層蒸着室が加熱器を有する、請求項36記載の装置。
- 【請求項39】 接触蒸着室を更に具えた、請求項36記載の装置。
- 【請求項40】 基体上に有機薄膜を形成するための装置において、 反応器、 前記反応器を加熱するための手段、 前記反応室へ有機前駆物質材料の蒸気を導入するための手段、及び 前記反応室中の圧力を大気圧より低く低下するための手段、 を具えた上記装置。
- 【請求項41】 OLEDを製造するための方法において、 複数の有機前駆物質を気相で与え、次いで 前記複数の有機層を大気の常態値以下の圧力で反応させる、 諸工程を有する、上記方法。
- 【請求項42】 有機前駆物質が発光材料である、請求項41記載の方法。
- 【請求項43】 反応工程が発光物質を形成する結果を与える、請求項41
記載の方法。
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US08/972,156 US6337102B1 (en) | 1997-11-17 | 1997-11-17 | Low pressure vapor phase deposition of organic thin films |
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PCT/US1998/024424 WO1999025894A1 (en) | 1997-11-17 | 1998-11-16 | Low pressure vapor phase deposition of organic thin films |
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1997
- 1997-11-17 US US08/972,156 patent/US6337102B1/en not_active Expired - Lifetime
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1998
- 1998-11-16 KR KR1020007005399A patent/KR100585286B1/ko not_active IP Right Cessation
- 1998-11-16 JP JP2000521253A patent/JP2001523768A/ja not_active Withdrawn
- 1998-11-16 WO PCT/US1998/024424 patent/WO1999025894A1/en active IP Right Grant
- 1998-11-16 DE DE1998627293 patent/DE69827293T2/de not_active Expired - Lifetime
- 1998-11-16 AU AU14124/99A patent/AU1412499A/en not_active Abandoned
- 1998-11-16 KR KR1020067004695A patent/KR100606325B1/ko not_active IP Right Cessation
- 1998-11-16 EP EP19980957997 patent/EP1032722B1/en not_active Expired - Lifetime
- 1998-11-17 TW TW87118943A patent/TW575699B/zh not_active IP Right Cessation
-
2000
- 2000-12-13 US US09/736,090 patent/US20010002279A1/en not_active Abandoned
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2002
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2003
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2007
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2009
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2010
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2013
- 2013-04-05 US US13/857,218 patent/US20150114296A1/en not_active Abandoned
- 2013-05-17 JP JP2013104840A patent/JP2013177692A/ja not_active Withdrawn
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2016
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Also Published As
Publication number | Publication date |
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AU1412499A (en) | 1999-06-07 |
JP4890592B2 (ja) | 2012-03-07 |
US6558736B2 (en) | 2003-05-06 |
DE69827293T2 (de) | 2006-02-02 |
KR20010024652A (ko) | 2001-03-26 |
US20100104753A1 (en) | 2010-04-29 |
EP1032722A4 (en) | 2001-09-12 |
WO1999025894A1 (en) | 1999-05-27 |
JP2013177692A (ja) | 2013-09-09 |
US20070131172A1 (en) | 2007-06-14 |
JP2009238756A (ja) | 2009-10-15 |
EP1032722B1 (en) | 2004-10-27 |
US20040007178A1 (en) | 2004-01-15 |
US20010002279A1 (en) | 2001-05-31 |
DE69827293D1 (de) | 2004-12-02 |
US6337102B1 (en) | 2002-01-08 |
JP5371837B2 (ja) | 2013-12-18 |
US20020155230A1 (en) | 2002-10-24 |
KR100585286B1 (ko) | 2006-05-30 |
US20150114296A1 (en) | 2015-04-30 |
JP2016104913A (ja) | 2016-06-09 |
EP1032722A1 (en) | 2000-09-06 |
TW575699B (en) | 2004-02-11 |
KR20060034312A (ko) | 2006-04-21 |
KR100606325B1 (ko) | 2006-07-31 |
JP2010159497A (ja) | 2010-07-22 |
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