TW202120730A - 銦前體化合物、利用該銦前體化合物的薄膜的製備方法及由此製備的基板 - Google Patents
銦前體化合物、利用該銦前體化合物的薄膜的製備方法及由此製備的基板 Download PDFInfo
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- TW202120730A TW202120730A TW109137942A TW109137942A TW202120730A TW 202120730 A TW202120730 A TW 202120730A TW 109137942 A TW109137942 A TW 109137942A TW 109137942 A TW109137942 A TW 109137942A TW 202120730 A TW202120730 A TW 202120730A
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- thin film
- precursor compound
- indium
- indium precursor
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- 239000002243 precursor Substances 0.000 title claims abstract description 100
- 229910052738 indium Inorganic materials 0.000 title claims abstract description 88
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 150000001875 compounds Chemical class 0.000 title claims abstract description 82
- 239000010409 thin film Substances 0.000 title claims abstract description 67
- 239000000758 substrate Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 40
- 239000000126 substance Substances 0.000 claims abstract description 26
- 230000008021 deposition Effects 0.000 claims abstract description 25
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 23
- 125000005842 heteroatom Chemical group 0.000 claims abstract description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 10
- 239000001257 hydrogen Substances 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- 239000010408 film Substances 0.000 claims description 51
- 238000000151 deposition Methods 0.000 claims description 33
- 125000004432 carbon atom Chemical group C* 0.000 claims description 18
- 238000005229 chemical vapour deposition Methods 0.000 claims description 14
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 13
- 229910052733 gallium Inorganic materials 0.000 claims description 13
- 239000011701 zinc Substances 0.000 claims description 12
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 11
- 238000000231 atomic layer deposition Methods 0.000 claims description 11
- 229910052725 zinc Inorganic materials 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- NWAIGJYBQQYSPW-UHFFFAOYSA-N azanylidyneindigane Chemical compound [In]#N NWAIGJYBQQYSPW-UHFFFAOYSA-N 0.000 claims description 2
- 229910003437 indium oxide Inorganic materials 0.000 claims description 2
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 238000003860 storage Methods 0.000 abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 4
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- 239000000203 mixture Substances 0.000 description 18
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 15
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- 230000015572 biosynthetic process Effects 0.000 description 10
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- UHOVQNZJYSORNB-MZWXYZOWSA-N benzene-d6 Chemical compound [2H]C1=C([2H])C([2H])=C([2H])C([2H])=C1[2H] UHOVQNZJYSORNB-MZWXYZOWSA-N 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000012495 reaction gas Substances 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
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- 238000010926 purge Methods 0.000 description 5
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
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- 238000005481 NMR spectroscopy Methods 0.000 description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
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- 239000011261 inert gas Substances 0.000 description 4
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- 238000000691 measurement method Methods 0.000 description 4
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- FOJZPLNOZUNMJO-UHFFFAOYSA-M chloro(dimethyl)indigane Chemical compound [Cl-].C[In+]C FOJZPLNOZUNMJO-UHFFFAOYSA-M 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
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- 238000003756 stirring Methods 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 description 3
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 2
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 2
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- AYYIQBPXJSIPFB-UHFFFAOYSA-N N-tert-butyl-N',N'-bis(methylamino)ethane-1,2-diamine Chemical compound CC(C)(C)NCCN(NC)NC AYYIQBPXJSIPFB-UHFFFAOYSA-N 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- 239000004696 Poly ether ether ketone Substances 0.000 description 2
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- 239000004642 Polyimide Substances 0.000 description 2
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- 239000006227 byproduct Substances 0.000 description 2
- 150000001721 carbon Chemical group 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- HQWPLXHWEZZGKY-UHFFFAOYSA-N diethylzinc Chemical compound CC[Zn]CC HQWPLXHWEZZGKY-UHFFFAOYSA-N 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 2
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- 230000000704 physical effect Effects 0.000 description 2
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 229920002530 polyetherether ketone Polymers 0.000 description 2
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- 229920001721 polyimide Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
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- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- LQLJZSJKRYTKTP-UHFFFAOYSA-N 2-dimethylaminoethyl chloride hydrochloride Chemical compound Cl.CN(C)CCCl LQLJZSJKRYTKTP-UHFFFAOYSA-N 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- 229920012266 Poly(ether sulfone) PES Polymers 0.000 description 1
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
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- QYHNIMDZIYANJH-UHFFFAOYSA-N diindium Chemical compound [In]#[In] QYHNIMDZIYANJH-UHFFFAOYSA-N 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- QNDQILQPPKQROV-UHFFFAOYSA-N dizinc Chemical compound [Zn]=[Zn] QNDQILQPPKQROV-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
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- 229910052736 halogen Inorganic materials 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
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- 125000004491 isohexyl group Chemical group C(CCC(C)C)* 0.000 description 1
- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000004518 low pressure chemical vapour deposition Methods 0.000 description 1
- AUHZEENZYGFFBQ-UHFFFAOYSA-N mesitylene Substances CC1=CC(C)=CC(C)=C1 AUHZEENZYGFFBQ-UHFFFAOYSA-N 0.000 description 1
- 125000001827 mesitylenyl group Chemical group [H]C1=C(C(*)=C(C([H])=C1C([H])([H])[H])C([H])([H])[H])C([H])([H])[H] 0.000 description 1
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- 150000004767 nitrides Chemical class 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
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- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
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- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 description 1
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- 238000002411 thermogravimetry Methods 0.000 description 1
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- 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
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
- C23C16/18—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material from metallo-organic compounds
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C16/34—Nitrides
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45553—Atomic layer deposition [ALD] characterized by the use of precursors specially adapted for ALD
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- Mechanical Engineering (AREA)
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Abstract
Description
本發明關於一種銦前體化合物、利用該銦前體化合物的薄膜的製備方法及由此製備的基板。更具體地,關於由於在沉積製程中表現出恆定的蒸氣壓而保持恆定的組成,從而能夠形成均勻的薄膜,並由於改善沉積速度而提高生產率的銦前體化合物,利用該銦前體化合物的薄膜的製備方法及由此製備的基板。
下一代顯示器以低功耗、高解析度及高可靠性為目標進行發展。為了實現這些目標,需要具有高電荷遷移率的薄膜電晶體(thin film transistor;TFT)物質。
以往在薄膜電晶體中使用了非晶矽,但是近來使用著電荷遷移率高於矽且低溫製程比多晶矽更加容易的金屬氧化物。作為這種金屬氧化物,使用添加了銦(Indium)、鋅(Zinc)等各種金屬原子的材料,金屬氧化物薄膜藉由濺射(Sputtering)、原子層沉積(Atomic Layer Deposition;ALD)、脈衝雷射沉積(Pulsed Laser Deposition;PLD)、化學氣相沉積(Chemical Vapor Deposition;CVD)等製程製備。
銦由於透明性和導電性優秀而被廣泛應用於透明電極,如韓國公開專利公報第2011-0020901號,當利用濺射靶藉由濺射形成包含銦(In)的金屬薄膜時,所沉積的薄膜的組成由濺射靶決定,因此在均勻調節薄膜的組成方面存在局限性。另外,當進行大面積沉積時,很難均勻地保持薄膜的組成及厚度,從而在獲取均勻的膜特性方面也有困難。
另外,當以化學氣相沉積(Chemical Vapor Deposition;CVD)方式替代濺射(Sputtering)進行製備時,以往使用的銦前體(例如三甲基銦(CAS NO. 3385-78-2))大部分為固體,因此在調節蒸氣壓及膜質重現性方面存在問題。特別是在高溫條件(250℃以上)下,大部分的銦(In)前體具有被熱分解的特性,因而很難獲取高品質的薄膜,並且,當進行大面積沉積時,在獲得厚度和多組分組成均勻的薄膜方面也存在限制。
因此,急需開發高溫熱穩定性優秀且均勻沉積的高品質銦前體。
[先前技術文獻]
[專利文獻]
專利文獻1:韓國公開專利第2011-0020901號。
[技術問題]
為了解決上述先前技術的問題,本發明的目的在於,提供在具有高沉積速度及高揮發性的同時,熱穩定性和保存穩定性優秀,且易於處理的銦前體化合物。
另外,本發明的目的在於,提供包含前述銦前體化合物,並由於在沉積製程中表現出恆定的蒸氣壓而保持恆定的組成,從而能夠形成均勻的薄膜,且膜厚度的均勻性優秀的薄膜的製備方法,及包含由前述方法製備的薄膜的基板。
本發明的前述目的及其他目的能夠藉由以下說明的本發明全部實現。
[技術方案]
為了實現前述目的,本發明提供一種銦前體化合物,該銦前體化合物由化學式1表示,
[化學式1]
在前述化學式1中,R1
、R3
及R4
各自獨立地為被取代或未被取代的碳原子數1至6的烷基,R2
為碳原子數1至6的直鏈或者支鏈烷基,R5
及R6
各自獨立地為氫或碳原子數1至3的烷基,X為碳原子或雜原子,n為1至3的整數。
另外,本發明提供一種薄膜的製備方法,包括以下步驟:將前述銦前體化合物沉積於基材上而形成薄膜。
另外,本發明提供借一種基板,該基板由前述薄膜的製備方法製成。
[發明效果]
根據本發明,能夠提供在具有高揮發性的同時,熱穩定性及保存穩定性優秀,且易於處理的銦前體化合物;在製備包含該銦前體化合物的薄膜時,由於在沉積製程中表現出恆定的蒸氣壓而保持恆定的組成,從而能夠製備均勻的薄膜,並由於改善沉積速度而提高生產率的薄膜的製備方法;及包含由此製備的均勻的薄膜的基板。
以下,對本發明的銦前體化合物,利用該銦前體化合物的薄膜的製備方法及由此製備的基板進行詳細說明。
在本發明說明書及發明申請專利範圍中使用的術語或單詞不應被解釋為限於通常含義或詞典含義,而應當基於“發明人可以為了以最佳方式描述其自身的發明而適當地定義術語的概念”這一原則,解釋為符合本發明的技術思想的含義和概念。
在本說明書中,當提及某一部件位於其他部件“上”時,這不僅包括與其他部件直接接觸的情況,還包括在兩個部件之間存在其他部件的情況。
在本說明書中,當提及某一部分“包括”某一構成要素時,除非有相反的記載,否則並非排除其他構成要素,而是指可以進一步包括其他構成要素。
本發明人確認了使銦前體的配體包含雙鍵並簡化配體,從而使其熱穩定性優秀的同時大幅改善沉積速度,在此基礎上,經過更為深入的研究,完成了本發明。
本發明的銦前體化合物由化學式1表示。
[化學式1]
在前述化學式1中,R1
、R3
及R4
各自獨立地為被取代或未被取代的碳原子數1至6的烷基,R2
為碳原子數1至6的直鏈或者支鏈烷基,R5
及R6
各自獨立地為氫或碳原子數1至3的烷基,X為碳原子或雜原子,n是滿足X化合價的值,為1至3的整數。
在前述化學式1中,作為一例,X可以是包含非共價電子對的雜原子。作為一例,包含前述非共價電子對的雜原子可以是N、O或者S,較佳為N。此時,如化學式1-1所示,由於包含在前述雜原子的非共價電子對,銦和雜原子之間形成配位鍵,從而使前述銦前體化合物變得非常穩定,並且改善熱穩定性及保存穩定性。
[化學式1-1]
作為一例,當X為氮(N)時,n可以是2,當X為氧(O)或者硫(S)時,n可以是1,當X為碳(C)時,n可以是3。
在前述化學式1中,R2
為碳原子數1至6的直鏈或者支鏈烷基,較佳為支鏈烷基。作為一例,可以是仲烷基或者叔烷基,具體地,可以是異丙基、仲丁基、異丁基、叔丁基、仲戊基、異戊基、叔戊基、新戊基、異己基、仲己基、叔己基或新己基。最佳地,可以是異丁基、叔丁基、叔戊基或新戊基。此時,防止前述銦前體化合物的分子間形成二聚體(dimer),從而使沉積製程更加穩定,並且增強前述X元素和銦之間的配位鍵,從而進一步提高前述前體化合物的熱穩定性及保存穩定性。
在前述化學式1中,R1
、R3
及R4
各自獨立地為被取代或未被取代的碳原子數1至6的烷基,較佳為碳原子數1至3的未被取代的烷基。此時,改善前述銦前體化合物的穩定性,從而改善沉積製程中的熱穩定性及保存穩定性,且由於分子的簡化,提高沉積速度,從而提高薄膜製備速度,並提高生產率。此時,被取代的碳原子數1至6的前述烷基是指被諸如鹵素、氧或者氮等取代基取代的烷基。
作為較佳一例,前述R1
、R3
及R4
可以各自獨立地為甲基或者乙基。
在前述化學式1中,R5
及R6
可以各自獨立地為氫或碳原子數1至3的烷基,較佳為氫或碳原子數1或2的烷基,更佳為氫或甲基。此時,由於分子的簡化,提高前述銦前體化合物的沉積速度,從而提高薄膜製備速度,並提高生產率。
在前述化學式2中,R2
至R6
與在前述化學式1中定義的相同,R1a
及R1b
各自為碳原子數1至6的烷基,較佳為碳原子數1至3的烷基,更佳為甲基,此時,由於分子的簡化,進一步改善前述銦前體化合物的穩定性,從而改善在沉積製程中的熱穩定性及保存穩定性,並且進一步提高沉積速度,從而提高薄膜製備速度,並提高生產率。
作為一例,前述銦前體化合物在25℃下測量的蒸氣壓可以是0.01至400 mmHg,較佳為0.01至100 mmHg,更佳為0.01至10 mmHg。當在前述範圍內製備薄膜時,能夠具有足以沉積的蒸氣壓,並提高沉積速度。
在本發明中,沒有特別限制蒸氣壓的測量方法,只要其是本發明所屬領域中通常實施的公知測量方法即可,作為一例,可以藉由熱重分析法測量。
本發明的銦前體化合物如前所述具有優秀的揮發性且在薄膜的成膜製程中具有充分的蒸氣壓,因此,在應用於CVD、ALD等沉積製程時,改善製程效率及所製備的包含該銦前體化合物的薄膜的膜質。
本發明的銦前體化合物由於在與銦鍵合的配體中包含含有雙鍵的碳,而使化合物穩定,從而能夠大幅改善熱穩定性,還改善保存穩定性,並且,在製備成薄膜時,由於保持蒸氣壓恆定而保持恆定的組成,從而能夠形成均勻的薄膜。另外,當前述銦前體化合物的X為包含非共價電子對的雜原子時,銦和X元素之間形成配位鍵,從而能夠使化合物更加穩定,並根據前述R2
的種類,增強銦和X元素之間的相互作用,從而使化合物穩定。並且,與以往的薄膜形成用銦前體相比,簡化配體,從而大幅提高沉積速度,並且,當製備包含其的薄膜時,能夠大幅提高薄膜的生產率。另外,由於前述X元素和銦的配位鍵比化合物中的其他鍵相對容易斷裂,在形成薄膜製程中,能夠與反應氣體更加穩定地進行反應,因此容易進行薄膜形成製程。並且,由於前述化合物自身的化學穩定性,在200℃以下的溫度下不能熱分解,因而不僅熱穩定性優秀,而且在常溫下的反應性低,無需擔心自燃,且易於處理。
本發明提供一種薄膜的製備方法,其包括以下步驟:將前述銦前體化合物沉積於基材(substrate,例如晶圓)上而形成薄膜。
本發明的薄膜的製備方法由於利用前述銦前體化合物而熱穩定性優秀,從而防止熱分解,並且,保持蒸氣壓恆定,從而能夠穩定且均勻地形成薄膜,提高沉積速度,從而能夠提高生產率。
作為一例,前述薄膜的製備方法可以包括以下步驟:將選自鎵前體及鋅前體中的至少一種和前述銦前體化合物沉積於基材上而形成薄膜。在這種情況下,有利於製備多組分的組成均勻且熱穩定性優秀的透明電子元件。
作為一例,前述薄膜的形成步驟能夠將前述銦前體化合物、鎵前體及鋅前體依次沉積於基材上而形成多層結構的薄膜。作為另一例,能夠將前述銦前體化合物、鎵前體及鋅前體同時沉積於基材上,或者將由前述銦前體化合物、鎵前體化合物及鋅前體化合物混合而成的混合前體化合物沉積於基材,從而形成單層結構的薄膜。
作為一例,前述薄膜的製備方法可以在200至1000 ℃的沉積溫度下進行。前述沉積溫度可以具體為250至500 ℃,較佳為270至400 ℃,更佳為300至350 ℃,此時,能夠在相對低溫下進行銦前體化合物的沉積,從而提高製程效率,並且,減少用於沉積製程的化合物的熱分解,從而大幅改善沉積製程的穩定性及生產率。
作為一例,前述薄膜的製備方法能夠根據需要將前述銦前體化合物與溶劑或者前述銦前體化合物、鎵前體及鋅前體與溶劑混合並進行沉積。作為一例,前述溶劑可以是有機溶劑,具體為選自四氫呋喃(THF)、乙醚(diethyl ether)、二甲氧基乙烷(DME)、二氯甲烷(DCM)、二氯乙烷(DCE)、苯(Benzene)、甲苯(Toluene)、己烷(hexane)、戊烷(pentane)、庚烷(heptan)及均三甲苯(Mesitylene)中的一種,此時,當沉積薄膜時,更加容易調節前體化合物的黏度或蒸氣壓。
作為一例,前述薄膜的製備方法可以進一步包括利用電漿在形成於前述基材上的薄膜上進行沉積的步驟,在這種情況下,即使在溫度相對低的沉積條件下也能獲得高品質的薄膜。作為一例,前述電漿可以是氧電漿,但不限於此。
本發明的薄膜的製備方法可以包括如下步驟中的至少一個並實施:
- 在基材(substrate)上以吸附方式沉積本發明的銦前體化合物的步驟;
- 利用惰性氣體來吹掃未被吸附的銦前體化合物的步驟;
- 注入反應氣體,以與被吸附的銦前體化合物發生反應的步驟;
- 使用惰性氣體來吹掃前述反應的副產物及未反應物質的步驟。
作為一例,前述薄膜的製備方法可以將多個前述步驟作為一循環,重複數十次前述循環,直至形成所需厚度的薄膜。具體地,前述循環的重複次數為50至1000次,較佳為100至300次,在這種情況下,能夠適當地實現薄膜的厚度,並且提高製程效率。
作為具體一例,前述薄膜的製備方法可以包括如下步驟並實施:
a)將基材運輸到反應腔室內部並保持燒結溫度的步驟;
b)將惰性氣體注入到前述反應腔室內部的第一次吹掃步驟;
c)將本發明的銦前體化合物注入到前述反應腔室內部並吸附在前述基材上的步驟;
d)將惰性氣體注入到前述反應腔室內部,從而使化學吸附於基材上的銦前體殘留,並去除物理吸附於基材上的銦前體化合物的第二次吹掃步驟;
e)將反應氣體注入到前述反應腔室內部,以與被化學吸附的前述銦前體化合物發生反應的步驟;及
f)將前述反應的副產物及未反應物質釋放到前述反應腔室外部的第三次吹掃步驟。
作為一例,前述薄膜的製備方法可以將前述步驟a)至f)作為一循環,重複進行前述循環。具體地,前述循環重複次數為50至1000次,較佳為100至300次,在這種情況下,能夠適當地實現薄膜的厚度,並且提高製程效率。
作為一例,前述薄膜的製備方法可以藉由化學氣相沉積法(CVD)、有機金屬化學氣相沉積法(MOCVD)、低壓氣相沉積法(LPCVD)、電漿增強氣相沉積法(PECVD)、原子層沉積法(ALD)或者電漿增強原子層沉積法(PEALD)實施,較佳地,可以藉由化學氣相沉積法或原子層沉積法實施,但不限於此。作為一例,前述化學氣相沉積法或原子層沉積法將薄膜沉積原料以氣體狀態供給到基板,從而能夠在縱橫比大的結構的表面形成均勻厚度的膜,而且將本發明的銦前體化合物以均勻濃度供給到大面積或者卷(roll)狀的基板上,從而能夠形成均勻的膜。
作為一例,前述沉積溫度可以是200至1000 ℃,具體為250至500 ℃,較佳為270至400 ℃,更佳為300至350 ℃,此時,在相對低溫下也能進行銦前體化合物的沉積,從而提高製程效率,並且減少用於沉積製程的化合物的熱分解,從而大幅改善沉積製程的穩定性及生產率。另外,減少所製備的薄膜中諸如碳(carbon)等雜質(impurity)的含量,從而能夠提高薄膜的物性。
作為一例,前述沉積可以使用將原料依次供給並沉積的時分沉積設備。
作為另一例,可以使用基板旋轉並往返於填充有一種原料氣體的空間和填充有另一種原料氣體的空間之間的方式的空間分割沉積裝置。
作為另一例,當前述基板為卷狀的高分子基材時,可以使用以卷狀捲繞的卷對卷(roll-to-roll)沉積設備。
作為一例,前述反應氣體可以選自水蒸氣(H2
O)、過氧化氫(H2
O2
)、氧氣(O2
)、臭氧(O3
)、氫氣(H2
)、氮氣(N2
)、肼(N2
H4
)、氨氣(NH3
)及矽烷(silane)中的至少一種,但不限於此。
作為具體的一例,當在諸如水蒸氣、氧氣、臭氧等氧化性反應氣體環境下進行前述銦前體化合物的沉積時,能夠形成含銦的金屬氧化物薄膜。
作為具體的另一例,當在諸如氫氣、矽烷等反應氣體環境下進行前述銦前體化合物的沉積時,能夠形成含銦的金屬薄膜。
作為具體的另一例,在諸如氨氣、肼等氮類反應氣體環境下進行前述銦前體化合物的沉積時,能夠形成含銦的金屬氮化物薄膜。
在前述薄膜的製備方法中,作為一例,前述銦前體化合物的注入時間可以是1至30秒,較佳為1至20秒,更佳為2至10秒,在該範圍內,能夠改善薄膜的厚度均勻性,從而在複雜形態的基板上也能易於製備均勻的薄膜。
在前述薄膜的製備方法中,作為一例,反應氣體的注入時間可以是1至40秒,較佳為1至30秒,更佳為2至10秒,在該範圍內,由於優秀的覆蓋性及均勻的塗布性而改善薄膜的物性。
作為一例,前述基材(例如晶圓)可以包含選自玻璃、矽、金屬聚酯(Polyester;PE)、聚對苯二甲酸乙二醇酯(Polyethyleneterephthalate;PET)、聚萘二甲酸乙二醇酯(Polyethylenenapthalate;PEN)、聚碳酸酯(Polycarbonate;PC)、聚醚醯亞胺(Polyetherimide;PEI)、聚醚碸(Polyethersulfone;PES)、聚醚醚酮(Polyetheretherketone;PEEK)及聚醯亞胺(Polyimide;PI)中的至少一種基材,但不限於此。
在本發明中,將在薄膜製備製程中供給到腔室的基板稱為基材(substrate)。
本發明提供一種基板,該基板包含藉由前述薄膜的製備方法製備的薄膜。其中,基板包括基材及形成在基材上的薄膜,且前述薄膜包含前述銦前體化合物。
作為一例,藉由前述薄膜的製備方法製備的薄膜可以是銦氧化物薄膜、銦薄膜或者銦氮化物薄膜。在這種情況下,薄膜的膜形成速度快,且膜厚度的均勻性及熱穩定性優秀。
作為一例,藉由前述薄膜的製備方法製備的薄膜可以是單層結構或者多層結構。
作為一例,前述單層結構的薄膜可以是將前述銦前體化合物沉積而形成,或者是將由前述銦前體化合物與選自鎵前體及鋅前體中的至少一種混合而成的混合物沉積而形成,較佳地,可以是將銦前體化合物和鎵前體的混合物、銦前體化合物和鋅前體的混合物、或者銦前體化合物、鎵前體及鋅前體的混合物沉積而形成。作為具體的一例,前述鎵前體及前述鋅前體可以分別是三甲基鎵(trimethylgallium;TMG)及二乙基鋅( diethylzinc;DEZ)。
作為一例,前述多層結構的薄膜可以是將前述銦前體化合物和其他前體沉積的層疊結構,作為具體一例,可以是將選自鎵前體及鋅前體中的至少一種和前述銦前體化合物在基材上沉積的層疊結構。
作為具體一例,藉由前述薄膜的製備方法製備的薄膜可以是銦鎵鋅氧化物(IGZO)薄膜,作為一例,以莫耳比為基準,前述IGZO薄膜的In:Ga:Zn組成比可以是1~10 : 1~10 : 1~10,較佳為1~5 : 1~5 : 1~5,更佳為1 : 1 : 1。
作為一例,藉由前述薄膜的製備方法製備的薄膜在25℃下的電阻值可以是1×10-5
至1×102
Ωcm,較佳為1×10-4
至1×102
Ωcm,更佳為1×10-3
至10 Ωcm。
在本發明中,沒有特別限制電阻率的測量方法,只要其為本發明所屬領域中通常實施的測量方法即可,作為具體一例,可以藉由4-探針法(4-probe測量法)測量。
以下,為了方便理解本發明而提出較佳實施例,但本領域技術人員應清楚以下實施例僅例示了本發明,能夠在本發明的範圍及技術思想範圍內進行各種變更及修改,並且這些變形及修改也屬於所附的發明申請專利範圍。
[實施例]
[合成例1]
[銦前體化合物的製備]
步驟1)向250mL舒倫克燒瓶(Schlenk Flask)中添加10g(62.5mmol)的無水三甲基銦和200mL的甲苯(toluene)並冷卻至-20 ℃而製備溶液,向該溶液中,慢慢滴加6.91 g(31.3mmol)的三氯銦並攪拌30分鐘後,逐漸升高溫度,並在室溫下攪拌。反應結束後,在常溫下施加真空以去除溶劑,從而獲得16.91g(93.8mmol)的具有如反應式2-1中的1-1所示結構的二甲基氯化銦,為白色固體。1
H NMR (C6D6, 400 MHz): δ 0.19 (s, 6H)
[反應式2-1]
步驟2)向500mL舒倫克燒瓶中添加50g(347.12mmol)的2-氯-N,N-二甲基乙胺鹽酸鹽和50mL的蒸餾水並冷卻至-20℃而製備溶液,向該溶液中,慢慢滴加253.88g(3.47mol)的叔丁胺並攪拌30分鐘後,逐漸升高溫度,在室溫下攪拌1小時。其後,升溫至80℃後,攪拌1小時,然後逐漸降溫至室溫。反應結束後,將燒瓶冷卻至-20 ℃後,慢慢滴加將20.83 g(520.68 mmol)的NaOH稀釋於50 mL的蒸餾水而成的溶液後,逐漸提升溫度,在室溫下攪拌1小時。將由此獲得的溶液用150 mL的己烷萃取3次後,在常溫下,向己烷層施加100 torr的真空,以去除己烷後,利用減壓蒸餾法,獲得35 g(242.61 mmol)的無色液態的具有如反應式2-2中的2-1所示結構的N,N-二甲基氨基-N'-叔丁基乙二胺。1
H NMR (C6D6, 400 MHz): δ 1.06 (s, 9H), 1.21 (br, 1H), 2.06 (s, 6H), 2.33 (t, 2H), 2.56 (q, 2H)
[反應式2-2]
步驟3)向250mL舒倫克燒瓶中添加50 mL的甲苯並添加13.86 mL的正丁基鋰(2.5M在己烷中)溶液後,在冷卻至-20 ℃的同時,慢慢滴加前述步驟2)中所製備的5 g(34.66 mmol)的N,N-二甲基氨基-N'-叔丁基乙二胺後,逐漸升溫至室溫,並攪拌1小時。其後,將所獲得的溶液冷卻至-20 ℃後,逐漸添加前述步驟1)中所製備的6.25 g(34.66 mmol)的二甲基氯化銦。添加完成後,逐漸提升燒瓶的溫度並在室溫下攪拌1小時後,升溫至110 ℃並攪拌1小時,並重新逐漸降溫至室溫。其後,在室溫條件下,逐漸添加前述步驟1)中所製備的6.25 g(34.66 mmol)的二甲基氯化銦,在將燒瓶的溫度提升至110 ℃的狀態下,攪拌2小時後,重新逐漸降溫至室溫。反應結束後,從得到的溶液中濾除固體後,施加真空以去除溶劑,從而獲得橙色液體,對前述液體進行真空蒸餾,以去除雜質後,獲得透明且無色的由反應式2-13中的3-1表示的化合物(薄膜形成用前體),如前所述,該結構藉由1
H NMR譜分析進行確認,並將其結果示於圖1中。1
H NMR (C6D6, 400 MHz): δ -0.01 (s, 6H), 1.17 (s, 9H), 2.02 (s, 6H), 4.08 (d, 1H), 6.48 (d, 1H)
[反應式2-3]
能夠確認所製備的前述銦前體化合物為穩定的化合物,因為其即使暴露在大氣中也不會被點燃或產生煙霧(fume)。
無。
圖1是示出對本發明的合成例中製備的前體化合物的核磁共振氫譜(1
H NMR)的圖。
Claims (11)
- 如請求項1所述之銦前體化合物,其中,在前述化學式1中,X是具有非共價電子對的雜原子。
- 如請求項1所述之銦前體化合物,其中,在前述化學式1中,R2 是支鏈烷基。
- 如請求項1所述之銦前體化合物,其中,前述銦前體化合物在25℃下測量的蒸氣壓為0.01至400 mmHg。
- 一種薄膜的製備方法,包括以下步驟: 將請求項1至4中任一項所述之銦前體化合物沉積於基材上而形成薄膜。
- 如請求項5所述之薄膜的製備方法,其中,包括以下步驟: 將選自鎵前體及鋅前體中的至少一種和前述銦前體化合物沉積於基材上而形成薄膜。
- 如請求項5所述之薄膜的製備方法,其中,前述薄膜的製備方法在200至1000℃的沉積溫度下實施。
- 如請求項5所述之薄膜的製備方法,其中,前述沉積藉由化學氣相沉積法(CVD)或者原子層沉積法(ALD)實施。
- 一種基板,包括: 基材;及 薄膜,形成在前述基材上, 前述薄膜由請求項5至8中任一項所述之方法製成。
- 如請求項9所述之基板,其中,前述薄膜是銦氧化物薄膜、銦薄膜或銦氮化物薄膜。
- 如請求項9所述之基板,其中,前述薄膜是銦鎵鋅氧化物(IGZO)薄膜。
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