CN105386008A - 金属膜形成方法 - Google Patents
金属膜形成方法 Download PDFInfo
- Publication number
- CN105386008A CN105386008A CN201510540239.2A CN201510540239A CN105386008A CN 105386008 A CN105386008 A CN 105386008A CN 201510540239 A CN201510540239 A CN 201510540239A CN 105386008 A CN105386008 A CN 105386008A
- Authority
- CN
- China
- Prior art keywords
- metal film
- organic solvent
- film formation
- mist
- metal
- 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.)
- Granted
Links
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 87
- 239000002184 metal Substances 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 title claims abstract description 63
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 61
- 239000003960 organic solvent Substances 0.000 claims abstract description 59
- 239000012159 carrier gas Substances 0.000 claims abstract description 54
- 239000003595 mist Substances 0.000 claims abstract description 53
- 239000002253 acid Substances 0.000 claims abstract description 48
- 238000000889 atomisation Methods 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 49
- -1 amine compound Chemical class 0.000 claims description 48
- 239000012528 membrane Substances 0.000 claims description 46
- 239000004065 semiconductor Substances 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 239000000463 material Substances 0.000 claims description 27
- 239000007789 gas Substances 0.000 claims description 14
- 239000010949 copper Substances 0.000 claims description 13
- 239000011159 matrix material Substances 0.000 claims description 13
- 239000010948 rhodium Substances 0.000 claims description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 10
- 229910052802 copper Inorganic materials 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 9
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 9
- 229910052703 rhodium Inorganic materials 0.000 claims description 8
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 7
- 239000010931 gold Substances 0.000 claims description 7
- 239000004411 aluminium Substances 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 239000011651 chromium Substances 0.000 claims description 6
- 239000011572 manganese Substances 0.000 claims description 6
- 150000004985 diamines Chemical class 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052763 palladium Inorganic materials 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 229910052707 ruthenium Inorganic materials 0.000 claims description 3
- 239000012266 salt solution Substances 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 239000010937 tungsten Substances 0.000 claims description 3
- 230000026030 halogenation Effects 0.000 claims description 2
- 238000005658 halogenation reaction Methods 0.000 claims description 2
- 125000003158 alcohol group Chemical group 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000002738 chelating agent Substances 0.000 abstract description 2
- 239000007800 oxidant agent Substances 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 239000000758 substrate Substances 0.000 description 43
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 25
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 21
- 230000006978 adaptation Effects 0.000 description 16
- 229910052757 nitrogen Inorganic materials 0.000 description 13
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 150000001875 compounds Chemical class 0.000 description 10
- 238000010790 dilution Methods 0.000 description 10
- 239000012895 dilution Substances 0.000 description 10
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 9
- 239000012046 mixed solvent Substances 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 6
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 6
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- DKPFZGUDAPQIHT-UHFFFAOYSA-N butyl acetate Chemical compound CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 6
- 238000000151 deposition Methods 0.000 description 6
- 150000002576 ketones Chemical class 0.000 description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 6
- 229940043265 methyl isobutyl ketone Drugs 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 229920000768 polyamine Polymers 0.000 description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 6
- 239000000872 buffer Substances 0.000 description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 description 5
- 239000011707 mineral Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 description 4
- 235000011054 acetic acid Nutrition 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- QYJPSWYYEKYVEJ-FDGPNNRMSA-L copper;(z)-4-oxopent-2-en-2-olate Chemical compound [Cu+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O QYJPSWYYEKYVEJ-FDGPNNRMSA-L 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- 239000010431 corundum Substances 0.000 description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 4
- 230000004907 flux Effects 0.000 description 4
- 150000004767 nitrides Chemical class 0.000 description 4
- 238000013022 venting Methods 0.000 description 4
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 3
- ZFFMLCVRJBZUDZ-UHFFFAOYSA-N 2,3-dimethylbutane Chemical group CC(C)C(C)C ZFFMLCVRJBZUDZ-UHFFFAOYSA-N 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 3
- 239000000443 aerosol Substances 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 229960004132 diethyl ether Drugs 0.000 description 3
- 238000006073 displacement reaction Methods 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- WBJINCZRORDGAQ-UHFFFAOYSA-N ethyl formate Chemical group CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 230000005669 field effect Effects 0.000 description 3
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- 239000012212 insulator Substances 0.000 description 3
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 description 3
- 229910052594 sapphire Inorganic materials 0.000 description 3
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- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical compound [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 238000004804 winding Methods 0.000 description 3
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- 239000004215 Carbon black (E152) Substances 0.000 description 2
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
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- 150000001412 amines Chemical class 0.000 description 2
- 125000004202 aminomethyl group Chemical group [H]N([H])C([H])([H])* 0.000 description 2
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- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
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- HIDKSOTTZRMUML-UHFFFAOYSA-M potassium;dodecanoate Chemical compound [K+].CCCCCCCCCCCC([O-])=O HIDKSOTTZRMUML-UHFFFAOYSA-M 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
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- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 2
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- 239000002912 waste gas Substances 0.000 description 2
- HMTSWYPNXFHGEP-UHFFFAOYSA-N (4-methylphenyl)methanamine Chemical compound CC1=CC=C(CN)C=C1 HMTSWYPNXFHGEP-UHFFFAOYSA-N 0.000 description 1
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- MBVAQOHBPXKYMF-LNTINUHCSA-N (z)-4-hydroxypent-3-en-2-one;rhodium Chemical compound [Rh].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O MBVAQOHBPXKYMF-LNTINUHCSA-N 0.000 description 1
- VCOZQJVNADDWET-UHFFFAOYSA-N 1,1'-biphenyl;ethanol Chemical compound CCO.C1=CC=CC=C1C1=CC=CC=C1 VCOZQJVNADDWET-UHFFFAOYSA-N 0.000 description 1
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 description 1
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Classifications
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Abstract
提供一种能够有利于工业上形成密合性优良的金属膜的金属膜形成方法以及通过其方法形成的金属膜。一种在基体上形成金属膜的金属膜形成方法,包括在氧化剂、胺化合物或者质子酸的有机溶剂中,使金属溶解或分散形成原料溶液,将原料溶液雾化产生雾的雾化工序,将载气提供给所述雾的载气供给工序,通过所述载气将所述雾提供给所述基体的供给工序和使所述雾热反应,在所述基体表面的一部分或者全部层积金属膜的金属膜形成工序。
Description
【技术领域】
本发明涉及对半导体装置的电极形成等有用的金属膜形成方法。
【背景技术】
在现有技术中,蒸镀或者溅射法被用于金属膜形成方法。应用电子束或者高频的真空蒸镀法等被广泛用于蒸镀,并且,用直流电源或者交流电源产生等离子体,随后,用等离子体溅射阳极金属,在阴极沉积金属的手法等被广泛用于溅射法中。但是,蒸镀或者溅射法需要真空工序,为此,在成本花费、大型化、量产化上还存在课题。
并且,熟知涂敷方法等被广泛用于金属膜形成方法。涂敷金属膏,干燥之后煅烧的手法被用于涂敷方法。但是,这样的涂敷方法中,煅烧需要650℃以上的高温,金属膜形成方法未必令人满意。另外,已知有有机金属气相沉积法等,和涂敷方法一样需要高温工序,并且未必能充分获得密合性。
对此,近年来尝试使用膏体来分散超微粒子,在基板上形成图案化金属膜。例如专利文献1中,已知一种手法,使由金属芯部和有机物涂敷层构成的复合金属超微粒子分散在溶剂中调制成金属膏,使该金属膏附着在半导体元件的电极上低温煅烧形成超微粒子电极。但是,Ag或者Au等贵金属超微粒子形成的金属薄膜难与平滑的无机酸化物基板发生反应,不能得到充分的密合性,尤其在为了增加导电性在薄金属排线上形成金属镀覆被膜时,由于电镀前处理或者电镀液导致的化学反应,存在金属排线从无机酸化物基板剥离的问题。
并且,在近年,正在研究通过气溶胶沉积法形成金属膜。专利文献2中记载一种方法,将金属离子气雾化,通过将所述气雾化金属粒子吹到基板上,在所述基板上形成由金属薄膜构成的电极或者排线图案,专利文献3中记载了一种方法,在透明电极表面通过气溶胶沉积法形成有金属薄膜构成的辅助电极。但是,根据气溶胶沉积法,电极和基板的密合性非常差,尤其不适用于在电极上形成需要的厚膜,并且,因为成膜时需要真空工序,成膜之后需要高温热处理,并不令人满意。
【背景技术文献】
【专利文献】
【专利文献1】日本专利特开2001-168141号公报
【专利文献2】日本专利特开2011-153329号公报
【专利文献3】日本专利特开2013-129887号公报
【发明内容】
【发明要解决的课题】
本发明的目的是提供一种能够有利于工业成膜的密合性优良的金属膜形成方法以及通过其方法形成的金属膜。
【为了解决课题的技术手段】
本发明人等为了达到上述目的进行了认真的研究,结果发现,使用含有氧化剂、胺化合物或者质子酸的有机溶剂作为溶剂,雾化CVD法形成金属膜的话,与金属酸化物膜成膜时不同,容易形成密合性优良的金属膜。
并且,本发明人等得到了上述见解后,加以研究,完成了本发明。
即,本发明涉及到以下发明。
[1]一种在基体上形成金属膜的金属膜形成方法,特征是包括在含有氧化剂、胺化合物或者质子酸的有机溶剂中,使金属溶解或分散形成原料溶液,将原料溶液雾化产生雾的雾化工序,将载气提供给所述雾的载气供给工序,通过所述载气将所述雾提供给所述基体的供给工序和使所述雾热反应,在所述基体表面的一部分或者全部层积金属膜的金属膜形成工序。
[2]如所述[1]中所述的金属膜形成方法,所述有机溶剂包括氧化剂。
[3]如所述[2]中所述的金属膜形成方法,所述氧化剂与所述有机溶剂的体积比在1:99~50:50范围内。
[4]如所述[2]或[3]中所述的金属膜形成方法,所述氧化剂为水或过氧化氢。
[5]如所述[1]中所述的金属膜形成方法,所述有机溶剂包括胺化合物。
[6]如所述[5]中所述的金属膜形成方法,所述胺化合物为二胺。
[7]如所述[1]中所述的金属膜形成方法,所述有机溶剂包括质子酸。
[8]如所述[7]中所述的金属膜形成方法,所述质子酸为卤化氢酸。
[9]如所述[1]~[8]中任意一项所述的金属膜形成方法,所述热反应在200℃~650℃的温度进行。
[10]如所述[1]~[9]中任意一项所述的金属膜形成方法,所述热反应惰性气体或在还原气体的环境下进行。
[11]如所述[1]~[10]中任意一项所述的金属膜形成方法,所述金属从金(Au),银(Ag),白金(Pt)、铜(Cu)、铁(Fe)、锰(Mn)、镍(Ni)、钯(Pd)、钴(Co)、铑(Rh)、钌(Ru)、铬(Cr)、钼(Mo),钨(W)以及铝(Al)中选出的1种或两种以上金属的。
[12]如所述[1]~[11]中任意一项所述的金属膜形成方法,所述有机溶剂为乙醇。
[13]如所述[1]~[12]中任意一项所述的金属膜形成方法,所述原料溶液为为如下溶液a)和b)的混合物,a)含有氧化剂,胺化合物或包括质子酸的有机溶剂,b)含有所述金属的金属络化物溶液或金属盐溶液。
[14]一种利用所述[1]~[13]中任意一项记载的金属膜形成方法形成的金属膜。
[15]如所述[14]中所述的金属膜作为电极。
[16]如所述[15]中所述的金属膜作为电极时,还至少具备半导体层的半导体装置。
[17]一种用于形成金属膜的雾之前体溶液,特征为含有氧化剂,胺化合物或质子酸的有机溶剂中,使金属溶解或分散形成溶液。
[18]如所述[17]中所述的用于形成金属膜的雾之前体溶液,所述有机溶剂包括氧化剂。
[19]如所述[18]中所述的用于形成金属膜的雾之前体溶液,所述氧化剂和所述有机溶剂的体积比在1:99~50:50范围内。
[20]如所述[17]中所述的用于形成金属膜的雾之前体溶液,所述有机溶剂包括胺化合物或质子酸。
【发明效果】
根据本发明的金属膜形成方法,能够形成密合性优良的有利于工业成膜的金属膜。并且,本发明的金属膜密合性优良。
【附图说明】
【图1】实施例1使用的雾化发生装置的构成图。
【图2】表示实施例1中横截面SEM像的图。
【图3】表示实施例1中金属膜表面的SEM像的图。
【图4】实施例4使用的雾化发生装置的概略构成图。
【图5】表示实施例4中XRD测量结果的图。
【图6】表示实施例5中XRD测量结果的图。
【图7】表示实施例6中XRD测量结果的图。
【图8】表示实施例5中金属膜表面照片的图。
【具体实施方式】
本发明的金属膜形成方法是一种在基体上形成金属膜的金属膜形成方法,特征是包括:在含有氧化剂、胺化合物或者质子酸的有机溶剂中,使金属溶解或分散形成原料溶液,将原料溶液雾化产生雾的雾化工序;将载气提供给所述雾的载气供给工序;通过所述载气将所述雾提供给所述基体的供给工序和使所述雾热反应,在所述基体表面的一部分或者全部层积金属膜的金属膜形成工序。
所述雾化工序是在含有氧化剂、胺化合物或者质子酸的有机溶剂中使金属溶解或分散调制成原料溶液,使原料溶液雾化产生雾。
本工序中使用的含有氧化剂的有机溶剂(以下,也说成「含有氧化剂的有机溶剂」),有机溶剂中没有特别限定含有氧化剂,例如,可以通过公知的有机溶剂和氧化剂混合得到。所述氧化剂和所述有机溶剂的体积比,优选1:99~50:50范围内,更优选1:99~40:60范围内,更优选1:99~10:90范围内,最优选1:99~5:95范围内。通过这样的优选范围,雾更适于成膜,并且膜质更加良好。
作为所述氧化剂可以是例如水,水溶性或非水溶性的公知的氧化剂等,不过,在本发明中,所述氧化剂优选水或水溶性的氧化剂,更优选水或过氧化氢更可喜,最优选水。并且,使用水溶性氧化剂作为所述氧化剂时,优选和水混合的水溶液形态(例如过氧化氢水等)。
作为所述氧化剂,更具体的可以是例如水,过氧化氢(H2O2),过氧化钠(Na2O2),过氧化钡(BaO2),过氧化苯甲酰(C6H5CO)2O2等过氧化物,次亚氯酸(HClO),过氯酸,硝酸,过醋酸或者硝基苯等的有机过氧化物等。
作为所述水,更具体的可以是例如纯水,超纯水,自来水,井水,矿泉水,矿物水,温泉水,泉水,淡水,海水等,也包括对这些水进行例如精制,加热,杀菌,过滤,离子交换,电解,渗透压调整,缓冲化等处理之后的水(例如,臭氧水,纯净水,热水,离子交换水,生理盐水,磷酸缓冲液,磷酸缓冲生理食盐水等)。
所述有机溶剂只要不妨碍本发明的目的,没有特别的限定,作为这样的溶剂,可以是例如醇(例如甲醇,乙醇,丙醇,异丙醇,丁醇,叔丁醇等),醚(例如二噁烷,四氢呋喃,二乙基醚(Diethylether),叔丁基甲基醚(t-butylmethylether),二异丙醇醚,乙二醇-二甲基醚等),酯(例如甲酸乙基,醋酸乙基,醋酸正丁酯等),羧酸(例如甲酸,醋酸,丙酸等),卤化烃(例如二氯甲烷,氯仿,四氯化碳,三氯乙烯,1,2-二氯甲烷,氯苯等),烃(例如正己烷,苯,甲苯等),酰胺(例如甲酰氨基,N,N-二甲基甲酰氨基,N,N-二甲基乙酰胺等),酮(例如丙酮,甲乙酮,甲基异丁基酮等),腈类(例如乙腈,丙腈等),环丁砜,六甲基磷酰胺等的单独使用或它们的混合溶剂。本发明中,所述有机溶剂优选醇,酮或者它们的混合溶剂,更优选醇,最优选低级醇(优选C1~3)。
本工序中用使用的含有胺化合物的有机溶剂(以下又叫做含有胺化合物的有机溶剂),在有机溶剂中含有胺化合物的话就没有特别限定,例如,可以通过将公知的有机溶剂和胺化合物混合而得到。所述胺化合物和所述有机溶剂的混合物的配合比例,在所述有机溶剂中,所述胺化合物优选0.001摩尔/L~10摩尔/L范围内,更优选0.005摩尔/L~1摩尔/L范围内,最优选0.01摩尔/L~0.1摩尔/L范围内。在这样的优选范围,雾更适于成膜,并且膜质能更加良好。
所述胺化合物只要不妨碍本发明的目的没有特别的限定,可以是含有氧原子、硫原子、氮原子等的化合物。作为所述胺化合物,可以是例如,甲胺,乙胺,丙基胺,异丙基胺,正丁胺,异丁胺,仲丁基胺,叔丁胺,己基胺,2-甲氧基乙胺,2-乙氧乙基胺,3-甲氧基丙基胺,3-甲基硫代丙胺,乙二胺,丙二胺,丁二胺,己二胺,二亚乙基三胺,三亚乙基四胺,四乙烯五胺,亚氨基二丙胺,甲基亚氨基二丙胺,十二烷基亚氨基二丙胺,N,N’-二氨基丙基-1,3-丙二胺,N,N’-二氨基丙基-1,3-丁二胺,1,2-二氨基丙烷,二-(3-氨基丙基)醚,1,2-双(3-氨基丙氧基)乙烷,1,3二-(3-氨基丙氧基)-2,2-二甲基丙烷,N-月桂基丙二胺,N,N’-N,N′-二叔丁基乙二胺,N-甲基乙二胺,N-乙基乙二胺,N,N-二甲基乙撑二胺,烯丙基胺等具有C1~C16碳数的脂肪族化合物;环戊胺,环己胺,环庚胺,环辛基胺,氨基甲基环己烷,4-甲基环己胺,1-环己基乙胺,3,3,5-三甲基环己胺,异佛尔酮二胺,己二氨基甲基环等具有C1~C16碳数的脂环化合物;苄胺,苯乙胺,4-甲基苄基胺,N-氨基丙基苯胺,2-氨基-1,2-二苯基乙醇,9-氨基芴,二苯甲基胺,苯二甲胺,苯二胺,二氨基二苯甲烷,N-二苄基乙二胺,2-氨基吡啶,3-氨基吡啶,4-氨基吡啶,2,3-二氨基吡啶,2,5-二氨基吡啶,2,3,6-鸟氨基吡啶,N-氨基丙基苯胺,2-氨基-3-甲基吡啶,2-氨基-4-甲基吡啶,2-氨基-6-甲基吡啶,2-氨基-3-乙基吡啶,2-氨基-3-丙基吡啶,2-氨基-4,6-二甲基吡啶,2,6-二氨基-4-甲基吡啶,3-氨基-6-异丙基吡啶,2,6-二氨基吡啶等具有C1~C16碳数的芳香族化合物;哌嗪,N-氨基丙基哌嗪,2-甲基哌嗪,2,6-二甲基哌嗪,2,5-二甲基哌嗪,3-甲基氨基哌啶,2-氨基甲基哌嗪,3-氨基吡咯烷,同型哌嗪,N-氨基丙基哌嗪,1,4-(双-氨基丙基)哌嗪,N-氨基乙基哌啶,N-氨基丙基哌啶,2-氨基甲基哌啶,4-氨基甲基哌啶,糠胺,四氢糠胺,3-(甲基氨基基)吡咯烷,5-甲基糠胺,2-(硫代乙酸糠)乙胺,2-吡啶甲基胺,3-吡啶甲基胺,4-吡啶甲基胺等具有C1~C16碳数的杂环化合物;2-羟基乙基胺,甲基(2-羟乙基)胺,1-氨基-2-丙醇,3-氨基-1-丙醇,2-氨基-1-丙醇,1-氨基-2-丙醇,二乙醇胺,3-氨基-1,2--丙二醇,2-(2-氨基乙氧基)乙醇,N-(2-羟乙基)乙二胺,2-氨基-1,3-丙二醇等含有一个以上羟基的化合物。本发明中,所述胺化合物优选多胺,更优选二胺。另外,所述多胺可以是例如乙二胺,二亚乙基,三亚乙基四胺,四亚乙基五胺,聚氧丙烯二胺,聚氧化丙烯三胺等脂肪族多胺;异佛尔酮二胺,烯二胺,双(4-氨基-3-甲基二环己基)甲烷,二氨基二环己基甲烷,双(氨基甲基)环己烷,N-氨基乙基哌嗪,3,9-双(3-氨基丙基)-2,4,8,10-四恶螺(5.5)十一烷脂环式多胺等;间-苯二胺,对苯二胺,甲苯-2,4-二胺,甲苯-2,6-二胺,均三甲苯-2,4-二胺,均三甲苯-2,6-二胺,3-,5-二乙基甲苯-2,4-二胺,3,5-单核多胺如二乙基甲苯-2,6-二胺;亚联苯基二胺,4,4-二氨基二苯甲烷,2,5-萘二胺,2,6-萘二胺等芳香族多胺;2-咪唑氨丙基等的咪唑等。
用在含有胺化合物的有机溶剂中的有机溶剂只要不妨碍本发明的目的,就没有特别的限定,作为这样的溶剂,可以是例如醇(例如甲醇,乙醇,丙醇,异丙醇,丁醇,叔丁醇等),醚(例如二噁烷,四氢呋喃,二乙基醚(Diethylether),叔丁基甲基醚(t-butylmethylether),二异丙醇醚,乙二醇-二甲基醚等),酯(例如甲酸乙基,醋酸乙基,醋酸正丁酯等),羧酸(例如甲酸,醋酸,丙酸等),卤化烃类(例如二氯甲烷,氯仿,四氯化碳,三氯乙烯,1,2-二氯甲烷,氯苯等),烃(例如正己烷,苯,甲苯等),酮(例如丙酮,甲乙酮,甲基异丁基酮等)等的单独使用或它们的混合溶剂。本发明中,所述有机溶剂优选醇,酮或者它们的混合溶剂,更优选醇,最优选低级醇(优选C1~3)。
本工序中使用的含有质子酸的有机溶剂(以下,也说成「含有质子酸的有机溶剂」),有机溶剂中含有质子酸的话就没有特别限定,例如,可以通过公知的有机溶剂和质子酸混合得到。所述质子酸和所述有机溶剂的混合物的配合比例,在所述有机溶剂中,所述质子酸优选0.001摩尔/L~10摩尔/L范围内,更优选0.005摩尔/L~1摩尔/L范围内,最优选0.01摩尔/L~0.1摩尔/L范围内。在这样的优选范围,雾更适于成膜,并且膜质更加良好。
所述质子酸只要不妨碍本发明的目的没有特别的限定,公知的质子酸就可以。所述质子酸可以是例如盐酸、硫酸、硝酸、磷酸、氟硼酸、氢氟酸、高氯酸等无机酸或有机羧酸、酚类、有机磺酸等。而且,有机羧酸可以是例如甲酸、乙酸、草酸(Oxalicacid)、苯甲酸、邻苯二甲酸、马来酸、富马酸、丙二酸、酒石酸、柠檬酸、乳酸、琥珀酸、一氯乙酸、二氯乙酸、三氯乙酸、三氟乙酸、乙酸硝基、三苯基酯等。有机磺酸可以是例如烷基苯磺酸,烷基萘磺酸,烷基萘二磺酸,萘磺酸福尔马林缩聚物,三聚氰胺磺酸盐福尔马林缩聚物,萘二磺酸,萘三磺酸,二萘甲烷二磺酸,蒽醌磺酸,蒽醌二磺酸,蒽磺酸,芘磺酸等。并且,可以使用它们的金属盐。在本发明中,所述质子酸优选无机酸,更优选氢卤酸。氢卤酸可以是例如盐酸,氢溴酸,氢碘酸,氢氟酸等。
用在含有质子酸的有机溶剂中的有机溶剂只要不妨碍本发明的目的,就没有特别的限定,作为这样的溶剂,可以是例如醇(例如甲醇,乙醇,丙醇,异丙醇,丁醇,叔丁醇等),醚(例如二噁烷,四氢呋喃,二乙基醚(Diethylether),叔丁基甲基醚(t-butylmethylether),二异丙醇醚,乙二醇-二甲基醚等),酯(例如甲酸乙基,醋酸乙基,醋酸正丁酯等),酮(例如丙酮,甲乙酮,甲基异丁基酮等)等的单独使用或它们的混合溶剂。本发明中,所述有机溶剂优选醇,酮或者它们的混合溶剂,更优选醇,最优选低级醇(优选C1~3)。
本工序中使用的金属只要不妨碍本发明的目的没有特别限定,优选从金(Au),银(Ag),白金(Pt)、铜(Cu)、铁(Fe)、锰(Mn)、镍(Ni)、钯(Pd)、钴(Co)、铑(Rh)、钌(Ru)、铬(Cr)、钼(Mo),钨(W)以及铝(Al)中选出的1种或两种以上金属。
本工序中,所述含有氧化剂的有机溶剂中,含有胺化合物的有机溶剂中或者含有质子酸的有机溶剂中,使金属溶解或分散调制成原料溶液。
所述原料溶液中,所述金属只要能在含有氧化剂的有机溶剂中,含有胺化合物的有机溶剂中或者含有质子酸的有机溶剂中溶解或分散的话没有特别限定,本发明中优选:含有氧化剂,胺化合物或质子酸的有机溶剂与含有所述金属的金属络化物溶液或金属盐溶液之混合溶液。所述金属的配合比例没有特别限定,对原料溶液整体来说,优选0.01~70质量%,更优选0.12~50质量%。
在含有氧化剂,胺化合物或质子酸的有机溶剂中,使金属溶解或分散形成溶液作为用于形成金属膜的雾之前体(Precursor)溶液特别有用。
本工序中,所述原料溶液雾化产生雾。雾化方法,只要能使所述原料雾化的话没有特别限定,可以是公知的雾化方法,本发明中,优选使用超声波的雾化方法。
所述载气供给工序,将载气供给所述雾。载气种类只要不妨碍本发明的目的没有特别限定,合适的实例是例如氧,氮或氩气等惰性气体,再者氢气或成膜气体(Forminggas)等还原性气体。并且,载气的种类可以是一种,也可以是两种以上,改变载气浓度后的稀释气体(例如10倍稀释气体等)等可以作为第二载气使用。并且,载气的供给部位不只限于一处,可以是是两处以上。
供给工序通过所述载气将所述雾提供给所述基体。载气的流量没有特别限定,优选0.01~20L/分钟,更优选1~10L/分钟。
所述基体只要能够支持金属膜的话没有特别限定。所述质子酸只要不妨碍本发明的目的没有特别的限定,公知的质子酸就可以,有机化合物也可以,无机化合物也可以。所述基体的形状可以是例如平板或圆板、纤维状、棒状、圆柱状,棱柱状、筒状、螺旋状、球状、环状等,本发明中优选基板。
所述基板为板状,只要能作为膜的支持体没有特别限定。可以是绝缘体基板、半导体基板、导电性基板,所述基板优选绝缘体基板,优选表面有金属膜的基板。本发明中,所述基板优选具有刚玉结构的结晶物为主要成分的基板,或者具有β-高卢结构的结晶物为主要成分的基板。具有刚玉结构的结晶物为主要成分的基板,基板组成比中,具有刚玉结构的结晶物只要含量在50%以上,没有特别限定,本发明中,优选含量70%以上,更优选含量90%以上。具有刚玉结构的结晶物为主要成分的基板可以是例如蓝宝石基板(例:c面蓝宝石基板)或者α型氧化镓基板等。具有β-高卢结构的结晶物为主要成分的基板,基板组成比中,具有β-高卢结构的结晶物只要含量在50%以上,没有特别限定,本发明中,优选含量70%以上,更优选含量90%以上。具有β-高卢结构的结晶物为主要成分的基板,可以是例如β-Ga2O3基板或者含有Ga2O3和Al2O3,Al2O3比0wt%多且在60wt%以下的混晶体基板等。其他的底层基板可以是含有六方晶体结构的基板(例:SiC基板、ZnO基板、GaN基板)等。含有六方晶体结构的基板上,优选直接或者通过其他的层(例:缓冲层)形成膜。基板的厚度在本发明中没有特别的限定,优选50~2000μm,更优选200~800μm。
金属膜形成工序中,使所述雾热反应,在所述基体表面的一部分或者全部层积金属膜。所述热反应中,通过热使所述雾反应即可,反应条件等只要不妨碍本发明的目的没有特别限制。本工序中,所述热反应优选在200℃~650℃的温度,更优选在300℃~600℃的温度,最优选在400℃~550℃的温度下进行。并且,所述热反应优选在无氧环境下进行,更优选氮气或氩气等惰性气体,或是成膜气体(Forminggas)或氢气等还原性气体环境下进行,最优选惰性气体下进行。并且,可在加压下、减压下、常压下以及大气压下的任何条件下反应,本发明中,优选常压下或者大气压下反应。另外,膜厚可以通过调整成膜时间来设定,本发明中因为膜越厚密合性越优良,成膜时间优选设定长一些。成膜时间优选10分钟以上,更优选30分钟以上,最优选1小时以上。
根据本发明,能否断续地结晶生长还是未知的,但无论如何,能形成密合性优良的金属膜。并且,根据本发明,保持密合性优良的状态下,能够容易形成膜厚200nm以上的金属膜(优选膜厚300nm以上,更优选500nm以上,更优选1μm以上,最优选10μm以上的金属膜)。为此,根据本发明的金属膜形成方法制得的金属膜适用于电极或接触层,这样的金属膜也包括在本发明内,本发明的金属膜可作为电极或接触层使用。并且,本发明的金属膜构成的电极适用于半导体装置,至少能和半导体层一起用于半导体装置。
所述半导体层可以是例如氧化物半导体层,氮化物半导体层,含有硅的半导体层。所述氧化物半导体层优选主要成分为含有铟、铝和镓中一种或两种以上元素的氧化物的半导体层。所述氮化物半导体层优选为含有氮化物半导体作为主要成分之半导体层,该氮化物半导体含有铟、铝和镓中的一种或两种以上的元素。所述含有硅的半导体层优选为:含有硅或碳化硅作为主要成分之半导体层。
本发明的金属膜可用于传统金属膜的各种用途,例如作为电极或接触层,适用于各种半导体层,尤其适用于功率器件。并且,所述半导体装置可以分为电极在半导体层的一侧形成的横型元件(横型设备)和电极在半导体层的表里两面侧形成的纵型元件(纵型设备),本发明的金属膜在横型设备和纵型设备中都适用。
本发明中,所述金属膜作为电极优选用于纵型设备。
所述半导体装置可以是例如肖特基势垒二极管(SBD)、金属半导体场效应晶体管(MESFET)、高电子迁移率晶体管(HEMT)、金属氧化物半导体场效应晶体管(MOSFET)、静电感应晶体管(SIT)、结型场效应晶体管(JFET)、绝缘栅型双极晶体管(IGBT)或者发光二极管等。本发明中,所述半导体装置优选SBD、MOSFET、SIT、JFET或者IGBT,更优选SBD、MOSFET或者SIT。
另外,所述半导体装置还可以含有其他层等(例如绝缘体层、半导体层、导体层、半导体层、缓冲层、或者其他中间层等)。
【实施例1】
用图1说明实施例中使用的雾化发生装置。图1的雾化发生装置19具有载置基板20的基座21、提供载气的载气供给装置22a、调节载气供给装置22中送出载气流量的流量调节阀23a、提供载气(稀释)的载气供给装置22b、调节载气(稀释)供给装置22中送出载气流量的流量调节阀23b、容纳原料溶液的雾发生源24,水25a的容器25、安装在容器25底面的超声波振子26、内径为40mm的石英管构成的供给管27、设置在供给管27周围的加热器28和排出热反应后的雾、液滴以及废气的排气口29。基座21由石英构成,载置基板20的面相对水平面倾斜。成膜室的供给管27和基座21都是由石英制作成的,因此抑制:于基板20上形成的膜内混入来自装置的杂质。
使用将乙酰丙酮酸铑(Rhodiumacetylacetonate,0.01mol/L)加入到甲醇和水的混合溶剂(甲醇:水=9.5:0.5)而被分散的溶液作为原料溶液。用c面蓝宝石作为基板。用氮气作为载气。载气流量为5L/分钟,载气(稀释)的流量设定为0.5L/分钟。成膜在氮气环境下以500℃进行。对于得到的金属膜,用x射线衍射装置确认铑金属膜的形成。并且对于得到的铑金属膜,在断面SEM处测定膜厚。结果约11.7μm。另外这个断面的SEM像如图2所示。并且,用SEM观察金属膜表面。结果具有凹凸少,光滑的表面。另外这个金属膜表的SEM像如图3所示。并且,对于密合性,施加应力,通过目视来观察剥离状况,完全没有发生剥离等,密合性也优良。
【实施例2】
除了将水合甲醇的配合比例(体积比)设定为如表1所示比例之外,和实施例1一样形成金属膜,观察其成膜状态,进一步评价密合性。
【表1】
【实施例3】
除了使用乙酰丙酮铝代替乙酰丙酮酸铑以外,和实施例1一样形成金属膜。发现使用铝能和使用铑时一样能成膜。
【实施例4】。
1.成膜装置
实施例4中,使用图4所示雾化发生装置1代替实施例1中使用的雾化发生装置。用图4说明实施例中使用的CVD装置。雾CVD装置1具有提供载气的载气源2a、提供载气的载气供给源2a、调节载气供给源2a中送出载气流量的流量调节阀3a、提供载气(稀释)的载气(稀释)源2b、调节载气(稀释)源2b中送出载气(稀释)流量的流量调节阀3b、容纳原料溶液的雾发生源4,装水5a的容器5、安装在容器5底面的超声波振子6、成膜室7、雾发生源4连接成膜室7的供给管9、成膜室7内设置的热板8、热反应后的雾、排出液滴和废气的排气口11。另外,热板8上设置有基板10。
2.原料溶液的制备
使乙酰丙酮酸铜0.05摩尔/L、在甲醇中混合乙酰丙酮酸铜,进一步,作为螯合剂(Chelatingagent),添加混合溶液0.5%体积的乙二胺(Ethylenediamine),调制成原料溶液4a。
3.成膜准备
将上述2.中得到的原料溶液4a容纳在雾发生源4内。其次,用玻璃基板作为基板10,玻璃基板设置在热板8上,使热板8工作将成膜室7内的温度升到500℃。其次,打开流量阀3a、3b,将载气从作为载气源的载气供给装置2a、2b供给到成膜室7中,用载气充分置换成膜室7的气体环境后,分别调节载气的流量为5.0L/分钟,载气(稀释)的流量为0.5L/分钟。另外,使用氮气作为载气。
4.金属膜的形成。
其次,使超声波振子6以2.4MHz振动,其振动通过水5a传播到原料溶液4a,因此使原料溶液4a雾化产生雾4b。这个雾4b由载气通过供给管9内导入到成膜室7内,大气压下400℃在成膜室7内雾发生热反应,在基板10上形成铜膜。成膜时间在30分钟内。对于铜膜,用X射线测定装置进行确认。XRD测定结果如图5所示。并且和实施例1一样对密合性进行评价,结果良好。
【实施例5】
除了成膜温度用500℃代替400℃以外,和实施例4一样得到了铜膜。对于铜膜,用X射线测定装置进行确认。XRD测定结果如图6所示。并且,膜厚为925nm。并且和实施例1一样对密合性进行评价,结果良好。
【实施例6】
使乙酰丙酮酸铜为0.05摩尔/L、在甲醇中混合乙酰丙酮酸铜,进一步,作为质子酸,添加混合溶液0.25%体积的盐酸,调制成原料溶液。除了用这个原料溶液代替实施例4中的原料溶液4a以外,和实施例4一样而制得铜膜。对于铜膜,用X射线测定装置进行确认。XRD测定结果如图7所示。并且,膜厚为799nm。并且和实施例1一样对密合性进行评价,结果良好。
实施例4以及5中使用螯合剂时,金属膜的光泽更加良好。作为参考,实施例5中得到的铜膜的表面图片如图8所示。并且,如实施例6,用质子酸时成膜速率更加良好。
【产业上的利用可能性】
本发明的金属膜形成方法可以使用在半导体(例如化合物半导体电子设备等)电子部件、电机器部件、光学·电子照相相关装置、工业部件等所有领域,能够形成优良的电极,因此尤其适用于半导体装置的制造。
【符号说明】
1雾化发生装置
2a载气源
2b载气(稀释)源
3a流量调节阀
3b流量调节阀
4雾发生源
4a原料溶液
4b雾
5容器
5a水
6超声波振子
7成膜室
8热板
9供给管
10基板
11排气口
19雾化发生装置
20基板
21基座
22a载气供给装置
22b载气供给(稀释)装置
23a流量调节阀
23b流量调节阀
24雾发生起源
24a原料溶液
25容器
25a水
26超声波振子
27供给管
28加热器
29排气口
Claims (20)
1.一种在基体上形成金属膜的金属膜形成方法,其特征为,含有如下工序:
在含有氧化剂、胺化合物或者质子酸的有机溶剂中,使金属溶解或分散而形成原料溶液,将该原料溶液雾化产生雾的雾化工序;
将载气提供给所述雾的载气供给工序;
通过所述载气将所述雾提供给所述基体的供给工序;以及
使所述雾发生热反应,在所述基体表面的一部分或者全部层积金属膜的金属膜形成工序。
2.如权利要求1中所述的金属膜形成方法,所述有机溶剂含有氧化剂。
3.如权利要求2中所述的金属膜形成方法,所述氧化剂与所述有机溶剂的体积比在1:99~50:50范围内。
4.如权利要求2所述的金属膜形成方法,所述氧化剂为水或过氧化氢。
5.如权利要求1中所述的金属膜形成方法,所述有机溶剂含有胺化合物。
6.如权利要求5中所述的金属膜形成方法,所述胺化合物为二胺。
7.如权利要求1中所述的金属膜形成方法,所述有机溶剂含有质子酸。
8.如权利要求7中所述的金属膜形成方法,所述质子酸为卤化氢酸。
9.如权利要求1中所述的金属膜形成方法,所述热反应在200℃~650℃的温度下进行。
10.如权利要求1中所述的金属膜形成方法,所述热反应在惰性气体或还原气体的环境下进行。
11.如权利要求1中所述的金属膜形成方法,所述金属为从金(Au),银(Ag),白金(Pt)、铜(Cu)、铁(Fe)、锰(Mn)、镍(Ni)、钯(Pd)、钴(Co)、铑(Rh)、钌(Ru)、铬(Cr)、钼(Mo),钨(W)以及铝(Al)中选出的一种或两种以上。
12.如权利要求1中所述的金属膜形成方法,所述有机溶剂为醇。
13.如权利要求1中所述的金属膜形成方法,所述原料溶液为下述a)和b)的混合溶液,
a)含有氧化剂,胺化合物或质子酸的有机溶剂;
b)含有所述金属的金属络化物溶液或金属盐溶液。
14.一种利用权利要求1~13中任意一项所述的金属膜形成方法而形成的金属膜。
15.如权利要求14中所述的金属膜作为电极。
16.一种半导体装置,具备如权利要求15中所述的金属膜作为电极,并且还至少具备半导体层。
17.一种用于形成金属膜的雾之前体溶液,特征在为含有氧化剂,胺化合物或质子酸的有机溶剂中,使金属溶解或分散形成溶液。
18.如权利要求17中所述的用于形成金属膜的雾之前体溶液,所述有机溶剂含有氧化剂。
19.如权利要求18中所述的用于形成金属膜的雾之前体溶液,所述氧化剂和所述有机溶剂的体积比在1:99~50:50范围内。
20.如权利要求17中所述的用于形成金属膜的雾之前体溶液,所述有机溶剂含有胺化合物或质子酸。
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CN108690969A (zh) * | 2017-03-31 | 2018-10-23 | 流慧株式会社 | 成膜方法、导电性层压结构体及电子装置 |
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US12037683B2 (en) | 2018-08-27 | 2024-07-16 | Shin-Etsu Chemical Co., Ltd. | Film forming method |
CN111188025A (zh) * | 2018-11-14 | 2020-05-22 | 丰田自动车株式会社 | 燃料电池用隔板的制造方法 |
CN111188025B (zh) * | 2018-11-14 | 2022-09-16 | 丰田自动车株式会社 | 燃料电池用隔板的制造方法 |
CN111254489A (zh) * | 2018-12-03 | 2020-06-09 | 丰田自动车株式会社 | 成膜装置 |
CN110318021A (zh) * | 2019-07-26 | 2019-10-11 | 中国科学技术大学 | 一种晶圆级二氧化钒薄膜的制备方法 |
CN112813406A (zh) * | 2020-12-30 | 2021-05-18 | 武汉工程大学 | 基于cvd技术在异形件表面制备三维金属单质薄膜的设备及方法 |
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JP2016050357A (ja) | 2016-04-11 |
EP2990503B1 (en) | 2022-01-12 |
TW201608048A (zh) | 2016-03-01 |
TWI597381B (zh) | 2017-09-01 |
CN110952077A (zh) | 2020-04-03 |
EP2990503A1 (en) | 2016-03-02 |
KR20160026761A (ko) | 2016-03-09 |
CN110952077B (zh) | 2022-09-13 |
US9828694B2 (en) | 2017-11-28 |
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US20160060788A1 (en) | 2016-03-03 |
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