CN105555790B - 用于制备含氧化铟的层的制剂、其制备方法及其用途 - Google Patents
用于制备含氧化铟的层的制剂、其制备方法及其用途 Download PDFInfo
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- CN105555790B CN105555790B CN201480035813.2A CN201480035813A CN105555790B CN 105555790 B CN105555790 B CN 105555790B CN 201480035813 A CN201480035813 A CN 201480035813A CN 105555790 B CN105555790 B CN 105555790B
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- indium
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- 238000002360 preparation method Methods 0.000 title claims abstract description 61
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910003437 indium oxide Inorganic materials 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 33
- 239000002904 solvent Substances 0.000 claims abstract description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 150000002472 indium compounds Chemical class 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 8
- 239000004020 conductor Substances 0.000 claims abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 39
- 235000019441 ethanol Nutrition 0.000 claims description 24
- 150000001875 compounds Chemical class 0.000 claims description 19
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims description 16
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims description 15
- 239000000758 substrate Substances 0.000 claims description 14
- 239000004065 semiconductor Substances 0.000 claims description 13
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims description 12
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical class COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 claims description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 11
- LZCLXQDLBQLTDK-UHFFFAOYSA-N ethyl 2-hydroxypropanoate Chemical compound CCOC(=O)C(C)O LZCLXQDLBQLTDK-UHFFFAOYSA-N 0.000 claims description 10
- 230000005855 radiation Effects 0.000 claims description 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- -1 2-methyl cellosolve Chemical compound 0.000 claims description 8
- MTZQAGJQAFMTAQ-UHFFFAOYSA-N ethyl benzoate Chemical compound CCOC(=O)C1=CC=CC=C1 MTZQAGJQAFMTAQ-UHFFFAOYSA-N 0.000 claims description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 7
- 239000001089 [(2R)-oxolan-2-yl]methanol Substances 0.000 claims description 7
- BSYVTEYKTMYBMK-UHFFFAOYSA-N tetrahydrofurfuryl alcohol Chemical compound OCC1CCCO1 BSYVTEYKTMYBMK-UHFFFAOYSA-N 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 6
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 claims description 6
- JTXMVXSTHSMVQF-UHFFFAOYSA-N 2-acetyloxyethyl acetate Chemical compound CC(=O)OCCOC(C)=O JTXMVXSTHSMVQF-UHFFFAOYSA-N 0.000 claims description 5
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 5
- 229940116333 ethyl lactate Drugs 0.000 claims description 5
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 4
- 230000005670 electromagnetic radiation Effects 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 4
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 4
- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- MRABAEUHTLLEML-UHFFFAOYSA-N Butyl lactate Chemical compound CCCCOC(=O)C(C)O MRABAEUHTLLEML-UHFFFAOYSA-N 0.000 claims description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000001191 butyl (2R)-2-hydroxypropanoate Substances 0.000 claims description 3
- 108700031620 S-acetylthiorphan Proteins 0.000 claims description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 2
- 239000011469 building brick Substances 0.000 claims description 2
- 150000002825 nitriles Chemical class 0.000 claims description 2
- 150000003333 secondary alcohols Chemical class 0.000 claims description 2
- 150000003509 tertiary alcohols Chemical class 0.000 claims description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 3
- COTNUBDHGSIOTA-UHFFFAOYSA-N meoh methanol Chemical compound OC.OC COTNUBDHGSIOTA-UHFFFAOYSA-N 0.000 claims 2
- 239000010409 thin film Substances 0.000 claims 1
- 229910052738 indium Inorganic materials 0.000 abstract description 28
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 abstract description 24
- 125000000217 alkyl group Chemical group 0.000 abstract description 9
- 229910052794 bromium Inorganic materials 0.000 abstract description 4
- 229910052801 chlorine Inorganic materials 0.000 abstract description 4
- 229910052731 fluorine Inorganic materials 0.000 abstract description 4
- 229910052740 iodine Inorganic materials 0.000 abstract description 4
- 125000000467 secondary amino group Chemical class [H]N([*:1])[*:2] 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 description 18
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 17
- 239000000203 mixture Substances 0.000 description 14
- 239000011248 coating agent Substances 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 10
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- 229910044991 metal oxide Inorganic materials 0.000 description 7
- 150000004706 metal oxides Chemical class 0.000 description 7
- 230000037230 mobility Effects 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 239000011541 reaction mixture Substances 0.000 description 7
- 150000003335 secondary amines Chemical class 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 125000004043 oxo group Chemical group O=* 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 229910021617 Indium monochloride Inorganic materials 0.000 description 4
- 150000001768 cations Chemical class 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- APHGZSBLRQFRCA-UHFFFAOYSA-M indium(1+);chloride Chemical compound [In]Cl APHGZSBLRQFRCA-UHFFFAOYSA-M 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000004528 spin coating Methods 0.000 description 4
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 3
- 239000008199 coating composition Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000005669 field effect Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 229910001449 indium ion Inorganic materials 0.000 description 2
- RJMMFJHMVBOLGY-UHFFFAOYSA-N indium(3+) Chemical compound [In+3] RJMMFJHMVBOLGY-UHFFFAOYSA-N 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 239000005711 Benzoic acid Substances 0.000 description 1
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical class CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 1
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N Lactic Acid Natural products CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 1
- 229910016287 MxOy Inorganic materials 0.000 description 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical class CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 1
- RSULWUXFWLWBAG-UHFFFAOYSA-N N=NC=NN.N=NC=NN.[Cl] Chemical compound N=NC=NN.N=NC=NN.[Cl] RSULWUXFWLWBAG-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
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- 125000001931 aliphatic group Chemical group 0.000 description 1
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- 239000002518 antifoaming agent Substances 0.000 description 1
- RRTCFFFUTAGOSG-UHFFFAOYSA-N benzene;phenol Chemical compound C1=CC=CC=C1.OC1=CC=CC=C1 RRTCFFFUTAGOSG-UHFFFAOYSA-N 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 230000002520 cambial effect Effects 0.000 description 1
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- 150000007942 carboxylates Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
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- 150000004292 cyclic ethers Chemical class 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- UZBQIPPOMKBLAS-UHFFFAOYSA-N diethylazanide Chemical compound CC[N-]CC UZBQIPPOMKBLAS-UHFFFAOYSA-N 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- WEHWNAOGRSTTBQ-UHFFFAOYSA-N dipropylamine Chemical compound CCCNCCC WEHWNAOGRSTTBQ-UHFFFAOYSA-N 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
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- 235000011194 food seasoning agent Nutrition 0.000 description 1
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- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
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- 239000012702 metal oxide precursor Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical class C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 description 1
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- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical class CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 150000003233 pyrroles Chemical class 0.000 description 1
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- 150000003512 tertiary amines Chemical class 0.000 description 1
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 description 1
- 230000010512 thermal transition Effects 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
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Classifications
-
- 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
- H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
- H01L21/288—Deposition of conductive or insulating materials for electrodes conducting electric current from a liquid, e.g. electrolytic deposition
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
-
- 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
- C23C16/40—Oxides
- C23C16/407—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
-
- 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
- C23C16/46—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 heating the substrate
-
- 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
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Abstract
本发明涉及能够通过将至少一种醇化铟化合物溶解在至少一种溶剂中而制备的液体制剂,其中该醇化铟化合物可以通过使如下物质反应而制备:三卤化铟InX3,其中X=F、Cl、Br、I,和式R'2NH的仲胺,其中R'=烷基,与所述三卤化铟的摩尔比为8:1至20:1,在通式ROH的醇的存在下,其中R=烷基;本发明还涉及其制备方法、其用于制备含氧化铟的层或者(半)导体层的用途以及使用本发明的制剂制备含氧化铟的层的方法。
Description
本发明涉及用于制备含氧化铟的层的制剂、其制备方法及其用途。
与许多的其它方法例如化学气相沉积(CVD)相比,依靠印刷和其它液体沉积方法来制备半导体电子组件层能够产生显著更低的制造成本,因为半导体能够在此以连续的工艺来沉积。此外,在较低的加工温度情况下,还开辟了下面的可能性:在柔性基材上工作,并且可能(特别是在非常薄的层的情况中,和特别是在氧化物半导体的情况中)实现印刷层的光学透明度。半导体层在这里和下面被理解为表示这样的层,其在50V栅源电压和50 V漏源电压时,在通道长度为20 µm的组件的情况中,具有1-50 cm2/Vs的载流子迁移率。
因为打算依靠印刷方法制造的组件层的材料对于具体层的性质具有决定性作用,因此它的选择对于含有这种组件层的各组件具有重要影响。用于印刷半导体层的重要参数是它们具体的载流子迁移率和它们的制造中所用的可印刷前体的加工性和加工温度。该材料应当具有良好的载流子迁移率,并且能够在明显低于500℃的温度从溶液中来制备,目的是适于多种应用和基材。同样对于许多新应用来说令人期望的是所获得的半导体层的光学透明度。
由于3.6到3.75 eV的大的带隙(在蒸镀的层上测量,H.S. Kim,P.D. Byrne,A.Facchetti,T.J. Marks;J. Am. Chem. Soc. 2008,130,12580-12581),氧化铟(氧化铟(III),In2O3)是一种有前景的和因此乐意使用的半导体。此外,几百纳米厚度的薄膜可以在可见光范围的550nm具有大于90%的高透明度。在极高有序的氧化铟单晶中,另外还可以测量到至多160 cm2/Vs的载流子迁移率。但是,这样的值通过从溶液中的加工迄今为止仍然无法实现(H. Nakazawa,Y. Ito,E. Matsumoto,K. Adachi,N. Aoki,Y. Ochiai;J. Appl. Phys. 2006,100,093706和A. Gupta,H. Cao,Parekh,K.K.V. Rao,A.R. Raju,U.V.Waghmare;J. Appl. Phys.,2007,101,09N513)。
氧化铟经常尤其与氧化锡(IV)(SnO2)一起作为半导体混合氧化物ITO来使用。由于ITO层相对高的电导率以及同时具有的在可见光范围中的透明度,它尤其用于液晶显示器(LCD)中,特别是用作“透明电极”。这些通常掺杂的金属氧化物层在工业上尤其是通过昂贵的蒸镀方法在高真空来制造。由于ITO涂覆的基材大的经济利益,这里现在存在着一些针对含氧化铟的层的涂覆方法,特别是基于溶胶-凝胶技术的涂覆方法。
原则上,存在着两种经由印刷方法来制造氧化铟半导体的可能方式:1)颗粒概念,在其中(纳米)颗粒存在于可印刷的分散体中,并且在印刷过程之后,通过烧结过程转化成期望的半导体层,和2)前体概念,在其中在印刷适当的组合物之后,将至少一种可溶的或者可分散的前体转化成含氧化铟的层。颗粒概念与使用前体相比具有两个重要缺点:首先,该颗粒分散体具有胶体不稳定性,其必须使用分散添加剂(这在随后的层性质方面是不利的);其次,许多能够使用的颗粒通过烧结仅仅不完全地形成了层(例如归因于钝化层),从而在层中出现了部分仍然粒状的结构。这导致在其颗粒边界处相当大的颗粒-颗粒阻抗,这降低了载流子的迁移率和提高了普遍的层阻抗。
存在着用于制造氧化铟层的不同的含前体的制剂。例如,除了铟盐之外,还可以使用醇化铟(均配(homoleptisch)的化合物,即,仅仅具有铟和醇根部分的化合物)作为在溶液中用于制造含氧化铟的层的前体。
例如,Marks等人描述这样的组件,它的制造使用了含前体的组合物,该组合物包含溶解在甲氧基乙醇中的盐InCl3和碱单乙醇胺(MEA)。在旋涂该组合物之后,相应的氧化铟层是通过在400℃热处理来获得的(H.S. Kim,P.D. Byrne,A. Facchetti,T.J. Marks;J. Am. Chem. Soc. 2008,130,12580-12581和补充信息)。
WO 2011/072887 A1描述了制备卤化-二醇化铟(III)的方法及其用于制造含氧化铟的层的用途。WO 2011/073005 A2公开了由这些卤化-二醇化铟(III)制造含氧化铟的层的方法。
然而,迄今为止,在溶液中的卤化-二醇化铟(III)无法产生具有足够好的电学性质的含氧化铟的层。氧代醇化铟,例如在WO 2012/010427 A1、WO 2012/010464 A1和尚未公开的德国申请DE 10 2012 209918中公开的通式In6O2X6(OR)6(R'CH(O)COOR'')2(HOR)x(HNR'''2)y、In7O2(OH)(OR)12X4(ROH)x和MxOy(OR)z[O(R'O)eH]aXbYc[R''OH]d 的化合物,会产生更好的层性质。
尽管已知的改进,持续地需要在形成层的性质和所获得的层的性质方面的改进。特别地,含有前体的合适溶液应当
- 能够很好地特别是在空气中加工,
- 能够均匀地转化成所述氧化物,
- 能够在尽可能低的温度下转化成所述氧化物,且
- 产生具有极好电学性质的层。
本发明的液体制剂可以满足这些复杂的要求条件,该液体制剂可以通过将至少一种醇化铟化合物溶解在至少一种溶剂中而制备,该醇化铟化合物可以通过使如下物质反应而制备:
- 三卤化铟InX3,其中X = F、Cl、Br、I,
- 式R'2NH的仲胺,其中R' = 烷基,
◦ 与所述三卤化铟的摩尔比为8:1至20:1
- 在通式ROH的醇的存在下,其中R = 烷基。
特别好的层可以使用含有醇化铟化合物的制剂制备,在其制备中在反应时使用仲胺与三卤化铟的摩尔比为8:1至15:1,更好为8:1至12:1。
在本发明中,在此情况下的醇化铟化合物是指具有至少一个铟原子和至少一个醇根基团的化合物,其可以在醇的存在下通过三卤化物与仲胺的上述反应而制备。通过本发明的方法可以获得的这些溶解的化合物的结构很难确定。然而,可以推测所产生的化合物是含有卤素的氧代醇化铟(Indiumoxoalkoxid)化合物。相应的固体结构能够借助X射线结构分析而确定。可以推测,这些化合物的类似结构也存在于溶液中。氧代醇化铟是指任选以离子形式存在的且通过氧代基团桥接的铟簇(Indiumcluster),其中未与氧代基团配位的价态至少部分地被醇根基团配位。对于可以通过本发明的方法获得的醇化铟化合物,可以推测他们在合成之后通常以盐的形式存在,特别是以与阳离子配位的含卤素的氧代醇化铟阴离子的形式。
特别优选的方法产物是通式[In6(O)(OR)12X6]2-Am z (ROH)x的醇化铟化合物,其中R= 烷基,X = F、Cl、Br、I,A = 阳离子,z = 阳离子的价态,m∙z = 2和x = 0至10,其尤其可以通过以9:1至10:1的比例使用仲胺而制备。所述化合物可以与醇分子ROH和任选地与在反应中存在的其它溶剂配位。
典型的阳离子是铵离子[NHyR4-y]+,优选式[NH2R2]+的铵离子。
非常特别优选的化合物是[In6(O)(OMe)12Cl6]2-[NH2R2]+ 2 (MeOH)2,其可以通过使用InCl3、Me2NH (后者的比例为9:1至10:1)和MeOH (甲醇)而制备。该化合物通过X射线结构分析而确定的结构显示在图1中。
本发明的制剂含有醇化铟化合物以实现特别好的半导体层,优选基于制剂的总质量计的重量百分比含量为0.1至10重量%,特别优选0.5至5重量%,非常特别优选1至2重量%。
本发明的制剂此外具有至少一种溶剂。为了得到特别好的制剂,优选的所述至少一种溶剂选自伯醇、仲醇、叔醇和芳族醇 (特别优选的醇为甲醇、乙醇、丁醇、四氢糠醇和苯酚),醚 (特别优选的是式ROCH2CH(R')OR"的乙二醇醚,其中R = -H或-C1-C10-烷基、R' = -H或–CH3和R" = -H或–C1-C10-烷基,和环状醚,特别是2-甲氧基乙醇、1-甲氧基-2-丙醇和四氢呋喃以及苯甲醚),酯 (特别优选的是羧酸酯和乳酸烷基酯,特别是乙酸丁酯、1-甲氧基-2-丙基乙酸酯(PGMEA)、苯甲酸乙酯、乙二醇二乙酸酯、乳酸乙酯和乳酸丁酯),芳族的烃(特别优选的是甲苯和二甲苯)和腈(特别优选的是乙腈)。
所述至少一种溶剂优选选自甲醇、乙醇、丁醇、四氢糠醇、苯酚、2-甲氧基乙醇、1-甲氧基-2-丙醇、四氢呋喃、苯甲醚、乙酸丁酯、1-甲氧基-2-丙基乙酸酯(PGMEA)、苯甲酸乙酯、乙二醇二乙酸酯、乳酸乙酯、乳酸丁酯、甲苯、二甲苯和乙腈。
本发明的制剂还优选具有至少两种,更还优选至少三种选自上述溶剂类型的溶剂。
本发明的制剂优选具有至少三种溶剂,其中之一选自乳酸乙酯、苯甲醚、四氢糠醇、乙酸丁酯、乙二醇二乙酸酯和苯甲酸乙酯,且另外两种在SATP条件下具有至少30℃的沸点差值。借助相应的制剂可以得到特别好的结果。
使用包含如下三种溶剂的制剂可以达到最好的结果:乙醇、1-甲氧基-2-丙醇和四氢糠醇。
本发明优选含有90至99.9重量%,优选 95至99.5重量%,特别优选98至99重量%的重量百分比含量的一种或多种溶剂,基于涂料组合物的总质量计。
为了实现有利的性质,本发明的组合物还可以具有添加剂,特别是润湿添加剂(特别是表面活性剂)、消泡剂、交联添加剂、表面张力添加剂和流平添加剂。如果存在添加剂,则其重量百分比含量基于涂料组合物的总质量计小于5重量%,优选小于2重量%。然而,本发明的组合物优选不具有额外添加剂,即其仅仅使用一种或多种溶剂以及一种或多种醇化铟化合物而制备。
为了实现特别好的性质,所述制剂基本上不含水,即其具有少于200 ppm的H2O。所述制剂还更优选使用基本上不含水的溶剂和化合物而制备。
本发明还提供了制备本发明的制剂的方法,其中将至少一种所述醇化铟化合物与至少一种溶剂混合。
为了制备本发明制剂而使用的醇化铟化合物通过如下方法制备,其中
- 三卤化铟InX3,其中X = F、Cl、Br、I
- 与式R'2NH的仲胺,其中R' = 烷基,
◦ 与所述三卤化铟的摩尔比为8:1至20:1
- 在通式ROH的醇的存在下反应,其中R = 烷基。
式InX3 的三卤化铟是本领域技术人员已知的且可以购得。
式R'2NH(其中R' = 烷基)的仲胺也属于现有技术。烷基R'优选是指直链、支化或环状的式CnH2n+1的C1-至C10-烷基,其中n = 1至10。一个或两个不同的仲胺的两个基团R'也可以共同形成亚烷基CnH2n。相应可以使用的化合物例如是二甲基胺、二乙基胺、二丙基胺、吡咯烷、哌啶和吡咯。优选的基团R'是如下基团:甲基、乙基、正丙基和异丙基。非常优选的基团R'是甲基,因为这会产生特别好的产率和特别稳定的化合物。
使用的醇ROH优选为具有直链、支化或环状的式CnH2n+1的C1至C10-烷基(其中n = 1至10)的那些醇。优选的基团R也为甲基、乙基、正丙基和异丙基。特别优选的基团R为甲基。
在所述方法中,三卤化铟的含量优选为0.1至50重量%,特别优选1至25重量%,非常特别优选2至10重量%,基于所有组分的总质量计。
所述三卤化铟可以溶解,即离解或以分子水平与溶剂分子/醇分子配位地,或者分散在液相中。
在所述方法中,醇ROH的含量优选为50至99.9重量%,特别优选75至99重量%,非常特别优选80至96重量%,基于所有组分的总质量计。
所述方法的反应混合物还可以具有至少一种对于所述反应呈惰性的液体溶剂或分散介质,即溶剂/分散介质或各种溶剂/分散介质的混合物,其在反应条件下不与所述三卤化铟反应。
优选可以使用的是质子惰性的溶剂,特别是选自如下的溶剂:质子惰性的非极性溶剂,即烷烃、取代的烷烃、烯烃、炔烃、具有或不具有脂族或芳族的取代基的芳烃、卤代烃和四甲基甲硅烷,以及选自质子惰性的极性溶剂,即醚、芳族的醚、取代的醚、酯或酸酐、酮、叔胺、硝基甲烷、DMF (二甲基甲酰胺)、DMSO (二甲基亚砜)或碳酸亚丙酯。
如果在所述反应混合物中存在至少一种对于所述反应呈惰性的液体溶剂或分散介质,则其含量优选为1至50重量%,特别优选1至25重量%,非常特别优选1至10重量%,基于所有组分的总质量计。
优选地,在反应中的仲胺的摩尔比为8:1至15:1,更优选8:1至12:1,相对于所述三卤化铟,因为由此可以以尤其高的产率制备对于层制造特别合适的醇化铟化合物。
优选地,如下实施本发明的方法:将三卤化铟预先置于醇ROH中。所述仲胺以气态、液态或溶解在溶剂中的形式 (特别包括ROH作为溶剂) 添加。
特别优选地,在SATP-条件 (25℃和1.013 bar)下进行添加。
因为所述反应可以特别好地控制和产生特别好的醇化铟化合物,所以所述二烷基胺优选以0.5至5 mol每小时和每摩尔卤化铟的速率,优选1.15至2.60 mol每小时和每摩尔卤化铟的速率进行添加。
更优选地,将所述方法的反应混合物在添加所有组分之后进行加热。优选地,将所述反应混合物经1-10 h的时间加热到40-70℃的温度。更优选地,将所述反应混合物经1-5h的时间加热到45-60℃的温度。之后冷却所述反应混合物。
在完成所述反应之后,将通常沉淀的产物或产物混合物优选与所述反应组合物的余下成分分离。优选地,这通过过滤进行。优选地,所述分离的产物混合物进一步使用合适的溶剂干燥和洗涤。
当所得到的产物或所得到的产物混合物在分离之后和任选在随后的干燥和/或洗涤之后进行重结晶,则会得到可以特别好地用于制备所述本发明的制剂的醇化铟化合物。优选地,所述重结晶在合成所述化合物时也使用的醇ROH中进行。优选地,如下进行所述重结晶:将分离的产物或产物混合物溶解在沸腾的醇中且然后在-30至0℃的温度下重结晶。将上清液的溶剂丢弃且将结晶的产物用于接下来的应用。
本发明的制剂特别有利地适合于制备具有改进的电学性质的含氧化铟的涂层,尤其经过湿化学方法。该改进目前是令人惊奇的,因为对于金属氧化物前体通常寻找具有尽可能低的结晶倾向的物质。然而,本发明的化合物却经常呈现为簇化合物,其由此已经具有微晶结构。所希望的金属氧化物层应该具有非晶而不是结晶的特性,以便提供特别好的电学性质。与所期望的相反,使用本发明的化合物可以制备特别均匀的层。
在这些情况下,含醇化铟的涂层是指氧化铟层或基本上包含氧化铟和其它金属和/或金属氧化物的层。在本发明中,氧化铟层是指由所述醇化铟可以制备的含金属的层,其基本上具有铟原子或铟离子,其中所述铟原子或铟离子基本上以氧化的形式存在。任选地,所述氧化铟层也可以具有未完全转化的卤素或醇根成分和/或氮、氢和/或碳。相应地,也适用于基本上包含氧化铟和其它金属和/或金属氧化物的层,前提条件是其还具有其它的金属和/或金属氧化物。
本发明的制剂还具有如下令人惊奇的优点:这些可以特别好地用于制造导体的或半导体的含氧化铟的用于电子组件的层,特别是当制造(薄膜)晶体管、二极管或太阳能电池时。
本发明还提供了制备含氧化铟的层的方法,其中将本发明的制剂施加于(任选预涂覆或预处理的)基材上,任选干燥和借助热和/或电磁辐射转化。
在本发明的这些方法中使用的基材优选是选自如下的基材:玻璃、硅、二氧化硅、金属氧化物或过渡金属氧化物或聚合物材料,特别是PE、PEN、PI或PET。
在涂覆之后和在转化之前,将所涂覆的基材进一步干燥。为此的相应措施和条件是本领域技术人员已知的。然而,所涂覆的基材并不必在转化之前一定干燥。
特别好地,本发明的组合物适合用于如下的涂覆方法:印刷法(特别是柔版/凹版印刷、喷墨印刷、(反向)胶版印刷、数字胶版印刷和丝网印刷)、喷涂法(“喷涂”)、旋转涂覆方法(“旋涂”)、浸渍法(“浸涂”)和其它液相涂覆法如槽-模涂覆方法、狭缝涂覆方法、幕涂方法和刮涂方法。
将所产生的结构或层转化成氧化铟或含氧化铟的层或结构可以通过热和/或UV-、IR-或VIS-辐射进行。
然而,当使用的转化温度为20至550℃,优选100至400℃,特别优选150至350℃时,可以实现特别好的结果。
此外,可以将施加的制剂替代地或补充地也借助电磁辐射,特别是借助UV辐射而进行转化。在此情况下,优选借助160至300 nm的波长的电磁辐射进行转化。优选地,可以借助具有250至258和180至190 nm的重要辐射部分的UVO辐射进行转化,这例如可以使用特定的汞蒸汽灯产生。也可以使用准分子灯或准分子激光器的辐射,尤其是160-190 nm波长的辐射进行转化。
当将所施加的制剂用热(尤其100至400℃,特别优选150至350℃的温度)和用电磁辐射(尤其160至300 nm的波长的电磁辐射)进行转化时,得到特别好的层。
在此情况下,通常使用的转化时间为几秒至几个小时。转化时间通常为1 s至24h,优选10 s至2 h,更优选1 min至40 min,特别优选1 min至20 min。
还可以如下辅助所述转化:将在涂覆步骤之后获得的层在热处理之前与水和/或过氧化氢接触,以便在热转化之前将其首先在一个中间步骤中转化为金属氢氧化物。
此外,所施加的涂料组合物的转化可以在通常大气的水含量下进行。
根据本发明的方法产生的层的品质可以进一步通过在转化步骤之后的组合的温度和气体处理(使用H2或O2)、等离子体处理(Ar、N2、O2或H2等离子体)、微波处理、激光处理(波长在UV、VIS或IR的范围中)、UV光、红外辐射或臭氧处理而进一步提高。
下面的实施例进一步解释本发明的主题,然而本发明并不限于此。
本发明的实施例
合成
在不含残余湿气的30 l反应器中,将1.30 kg的氯化铟 (III) (InCl3,5.9 mol)在保护气体气氛下通过搅拌悬浮在17.38 kg的干燥甲醇中。将二甲基胺 (2.57 kg,57mol) 通过质量流量控制器(0.86 kg/h,约4 h) 在室温下计量加入,其中观察到稍微放热的反应。之后,将所述反应混合物在两个小时内调温在50℃,然后冷却到室温且过滤。将过滤残余物用4 x 500 ml的干燥甲醇洗涤且在真空(0.1 mbar)下干燥8 h。将该材料溶解在沸腾的甲醇中且在-20℃下结晶。
制剂的制备
将所获得的物质以50 mg/ml的浓度溶解在1-甲氧基-2-丙醇中。将所获得的浓缩物如下制剂:1份浓缩物对应2份1-甲氧基-2-丙醇对应1份乙醇。向该制剂中再加入3重量%的四氢糠醇 (THFA)。所有使用的溶剂都是不含水的(< 200 ppm H2O)且混合是在惰性的条件下进行(同样不含水)。将所获得的制剂最终通过200 nm PTFE过滤器过滤。
涂覆
使用100 μl的上述制剂润湿如下掺杂的硅基材:其边长约15 mm且具有约200 nm厚的氧化硅涂层和ITO/金的指纹结构。然后在2000 rpm(30秒)下旋涂。将所涂覆的基材直接在该涂覆过程之后用来源于汞蒸气灯的UV辐射(波长范围150至300 nm)辐射10分钟。然后,将所述基材在加热板上在350℃的温度下加热一个小时。在转化之后可以在手套式操作箱中测定场效应迁移率的值为µFET = 14 cm2/Vs(在2 VDS的条件下,在直线范围内)。
对比例
合成
在不含残余湿气的500 ml玻璃圆底烧瓶中,将5.0 g的氯化铟 (III) (InCl3,22.5 mmol) 在保护气体气氛下通过搅拌溶解在250 ml的干燥甲醇中,其中剩余<10重量%(基于初始称重)的InCl3残余物。将碱性的二甲基胺 (5.0 g,111 mmol) 通过质量流量控制器计量加入且以基于InCl3化学计量的量在室温下经5小时的时间添加,其中开始时观察到稍微放热的反应。之后,将所述溶液完全蒸发,将剩余的固体用250 ml的干燥甲醇接收,在保护气体(N2)下过滤,用干燥的甲醇多次洗涤(十次)且在真空(<10 mbar)下在室温干燥12 h。氯二甲醇化铟(III)的产物产率为>80 mol%。
制剂的制备
将所获得的物质以50 mg/ml的浓度溶解在1-甲氧基-2-丙醇中。将所获得的浓缩物如下制剂:1份浓缩物对应2份1-甲氧基-2-丙醇对应1份乙醇。向该制剂中再加入3重量%的四氢糠醇 (THFA)。所有使用的溶剂都是不含水的(< 200 ppm H2O)且混合是在惰性的条件下进行(同样不含水)。将所获得的制剂最终通过200 nm PTFE过滤器过滤。
涂覆
使用100 μl的上述制剂润湿如下掺杂的硅基材:其边长约15 mm且具有约200 nm厚的氧化硅涂层和ITO/金的指纹结构。然后在2000 rpm(30秒)下旋涂。将所涂覆的基材直接在该涂覆过程之后用来源于汞蒸气灯的UV辐射(波长范围150至300 nm)辐射10分钟。然后,将所述基材在加热板上在350℃的温度下加热一个小时。在转化之后可以在手套式操作箱中测定场效应迁移率的值为µFET = 8 cm2/Vs(在2 VDS的条件下,在直线范围内)。
Claims (14)
1.能够通过将至少一种醇化铟化合物溶解在至少一种溶剂中而制备的液体制剂,其中该醇化铟化合物可以通过使如下物质反应而制备:
- 三氯化铟InCl3,
- 二甲基胺Me2NH,
与所述三氯化铟的摩尔比为8:1至20:1
- 在甲醇MeOH的存在下,
其特征在于,所述化合物具有通式[In6(O)(OMe)12Cl6]2-[NH2Me2]+ 2 (MeOH)2。
2.权利要求1的制剂,其特征在于,其包含0.1-10重量%的所述醇化铟化合物,基于所述制剂的总质量。
3.权利要求1或2的制剂,其特征在于,所述至少一种溶剂选自伯醇、仲醇、叔醇和芳族醇,醚,酯,芳族烃和腈。
4.权利要求1或2的制剂,其特征在于,所述至少一种溶剂选自甲醇、乙醇、丁醇、四氢糠醇、苯酚、2-甲氧基乙醇、1-甲氧基-2-丙醇、四氢呋喃、苯甲醚、乙酸丁酯、1-甲氧基-2-丙基乙酸酯、苯甲酸乙酯、乙二醇二乙酸酯、乳酸乙酯、乳酸丁酯、甲苯、二甲苯和乙腈。
5.权利要求4的制剂,其特征在于,其包含至少三种溶剂,其中之一选自乳酸乙酯、苯甲醚、四氢糠醇、乙酸丁酯、乙二醇二乙酸酯和苯甲酸乙酯,且另外两种在SATP条件下具有至少30℃的沸点差值。
6.权利要求1或2的制剂,其特征在于,其包含三种溶剂乙醇、1-甲氧基-2-丙醇和四氢糠醇。
7.权利要求1或2的制剂,其特征在于,其具有少于200 ppm的水。
8.制备权利要求1至7任一项的制剂的方法,其中将至少一种醇化铟化合物与至少一种溶剂混合,该醇化铟化合物可以通过使如下物质反应而制备:
- 三氯化铟InCl3,
- 二甲基胺Me2NH,
与所述三氯化铟的摩尔比为8:1至20:1
- 在甲醇MeOH的存在下。
9.权利要求1至7任一项的制剂的用途,用于制备含氧化铟的层。
10.权利要求1至7任一项的制剂的用途,用于制备电子组件用的半导体层或导体层。
11.权利要求10的用途,用于制备晶体管、二极管或太阳能电池。
12.权利要求11的用途,用于制备薄膜晶体管。
13.制备含氧化铟的层的方法,其中将权利要求1至7任一项的制剂施加到基材上且借助热和/或电磁辐射转化。
14.权利要求13的方法,其特征在于,将所施加的制剂借助热和电磁辐射转化。
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DE102009028801B3 (de) | 2009-08-21 | 2011-04-14 | Evonik Degussa Gmbh | Verfahren zur Herstellung Indiumoxid-haltiger Schichten, nach dem Verfahren herstellbare Indiumoxid-haltige Schicht und deren Verwendung |
DE102009054997B3 (de) | 2009-12-18 | 2011-06-01 | Evonik Degussa Gmbh | Verfahren zur Herstellung von Indiumoxid-haltigen Schichten, nach dem Verfahren hergestellte Indiumoxid-haltige Schichten und ihre Verwendung |
DE102010031895A1 (de) | 2010-07-21 | 2012-01-26 | Evonik Degussa Gmbh | Indiumoxoalkoxide für die Herstellung Indiumoxid-haltiger Schichten |
DE102010043668B4 (de) | 2010-11-10 | 2012-06-21 | Evonik Degussa Gmbh | Verfahren zur Herstellung von Indiumoxid-haltigen Schichten, nach dem Verfahren hergestellte Indiumoxid-haltige Schichten und ihre Verwendung |
DE102012209918A1 (de) | 2012-06-13 | 2013-12-19 | Evonik Industries Ag | Verfahren zur Herstellung Indiumoxid-haltiger Schichten |
DE102013212017A1 (de) | 2013-06-25 | 2015-01-08 | Evonik Industries Ag | Verfahren zur Herstellung von Indiumalkoxid-Verbindungen, die nach dem Verfahren herstellbaren Indiumalkoxid-Verbindungen und ihre Verwendung |
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2013
- 2013-06-25 DE DE102013212019.2A patent/DE102013212019A1/de not_active Withdrawn
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2014
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Patent Citations (2)
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CN102652137A (zh) * | 2009-12-18 | 2012-08-29 | 赢创德固赛有限公司 | 制备铟氯二醇盐的方法 |
CN103003286A (zh) * | 2010-07-21 | 2013-03-27 | 赢创德固赛有限公司 | 用于制备含氧化铟层的铟氧桥醇盐 |
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EP3013837A1 (de) | 2016-05-04 |
US9812330B2 (en) | 2017-11-07 |
RU2016101886A (ru) | 2017-07-28 |
JP6366702B2 (ja) | 2018-08-01 |
RU2659030C2 (ru) | 2018-06-27 |
JP2016534993A (ja) | 2016-11-10 |
TWI631100B (zh) | 2018-08-01 |
DE102013212019A1 (de) | 2015-01-08 |
TW201516022A (zh) | 2015-05-01 |
EP3013837B1 (de) | 2017-05-31 |
US20160141177A1 (en) | 2016-05-19 |
WO2014206599A1 (de) | 2014-12-31 |
KR102123262B1 (ko) | 2020-06-17 |
CN105555790A (zh) | 2016-05-04 |
KR20160022887A (ko) | 2016-03-02 |
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