TWI849250B - 新穎化合物、含有該化合物的薄膜形成用原料及薄膜的製造方法 - Google Patents
新穎化合物、含有該化合物的薄膜形成用原料及薄膜的製造方法 Download PDFInfo
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- TWI849250B TWI849250B TW109137199A TW109137199A TWI849250B TW I849250 B TWI849250 B TW I849250B TW 109137199 A TW109137199 A TW 109137199A TW 109137199 A TW109137199 A TW 109137199A TW I849250 B TWI849250 B TW I849250B
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- 239000010409 thin film Substances 0.000 title claims abstract description 108
- 150000001875 compounds Chemical class 0.000 title claims abstract description 98
- 239000002994 raw material Substances 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims description 51
- 238000004519 manufacturing process Methods 0.000 title claims description 31
- 229910052751 metal Inorganic materials 0.000 claims abstract description 53
- 239000002184 metal Substances 0.000 claims abstract description 52
- 125000001153 fluoro group Chemical group F* 0.000 claims abstract description 17
- 125000004429 atom Chemical group 0.000 claims abstract description 15
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 14
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 13
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 13
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 7
- 239000010408 film Substances 0.000 claims description 59
- 239000007789 gas Substances 0.000 claims description 51
- 239000002243 precursor Substances 0.000 claims description 50
- 230000015572 biosynthetic process Effects 0.000 claims description 23
- 239000000758 substrate Substances 0.000 claims description 23
- 239000010949 copper Substances 0.000 claims description 14
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- 229910052802 copper Inorganic materials 0.000 claims description 13
- 230000008016 vaporization Effects 0.000 claims description 13
- 229910017052 cobalt Inorganic materials 0.000 claims description 12
- 239000010941 cobalt Substances 0.000 claims description 12
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- 229910052725 zinc Inorganic materials 0.000 claims description 6
- 239000011701 zinc Substances 0.000 claims description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 5
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- 238000012545 processing Methods 0.000 claims description 5
- 239000011135 tin Substances 0.000 claims description 5
- 229910052718 tin Inorganic materials 0.000 claims description 5
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- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 239000011572 manganese Substances 0.000 claims description 3
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- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 1
- LIWAQLJGPBVORC-UHFFFAOYSA-N ethylmethylamine Chemical compound CCNC LIWAQLJGPBVORC-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 125000003709 fluoroalkyl group Chemical group 0.000 description 1
- 125000003784 fluoroethyl group Chemical group [H]C([H])(F)C([H])([H])* 0.000 description 1
- 125000004216 fluoromethyl group Chemical group [H]C([H])(F)* 0.000 description 1
- 125000005816 fluoropropyl group Chemical group [H]C([H])(F)C([H])([H])C([H])([H])* 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- ZTOMUSMDRMJOTH-UHFFFAOYSA-N glutaronitrile Chemical compound N#CCCCC#N ZTOMUSMDRMJOTH-UHFFFAOYSA-N 0.000 description 1
- CATSNJVOTSVZJV-UHFFFAOYSA-N heptan-2-one Chemical compound CCCCCC(C)=O CATSNJVOTSVZJV-UHFFFAOYSA-N 0.000 description 1
- NGAZZOYFWWSOGK-UHFFFAOYSA-N heptan-3-one Chemical compound CCCCC(=O)CC NGAZZOYFWWSOGK-UHFFFAOYSA-N 0.000 description 1
- DGCTVLNZTFDPDJ-UHFFFAOYSA-N heptane-3,5-dione Chemical compound CCC(=O)CC(=O)CC DGCTVLNZTFDPDJ-UHFFFAOYSA-N 0.000 description 1
- SDAXRHHPNYTELL-UHFFFAOYSA-N heptanenitrile Chemical compound CCCCCCC#N SDAXRHHPNYTELL-UHFFFAOYSA-N 0.000 description 1
- 150000002391 heterocyclic compounds Chemical class 0.000 description 1
- QAMFBRUWYYMMGJ-UHFFFAOYSA-N hexafluoroacetylacetone Chemical compound FC(F)(F)C(=O)CC(=O)C(F)(F)F QAMFBRUWYYMMGJ-UHFFFAOYSA-N 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 229940035429 isobutyl alcohol Drugs 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 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
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 description 1
- NFWSQSCIDYBUOU-UHFFFAOYSA-N methylcyclopentadiene Chemical compound CC1=CC=CC1 NFWSQSCIDYBUOU-UHFFFAOYSA-N 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- DNIAPMSPPWPWGF-UHFFFAOYSA-N monopropylene glycol Natural products CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 1
- DWFKOMDBEKIATP-UHFFFAOYSA-N n'-[2-[2-(dimethylamino)ethyl-methylamino]ethyl]-n,n,n'-trimethylethane-1,2-diamine Chemical compound CN(C)CCN(C)CCN(C)CCN(C)C DWFKOMDBEKIATP-UHFFFAOYSA-N 0.000 description 1
- GVWISOJSERXQBM-UHFFFAOYSA-N n-methylpropan-1-amine Chemical compound CCCNC GVWISOJSERXQBM-UHFFFAOYSA-N 0.000 description 1
- XHFGWHUWQXTGAT-UHFFFAOYSA-N n-methylpropan-2-amine Chemical compound CNC(C)C XHFGWHUWQXTGAT-UHFFFAOYSA-N 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- GJYXGIIWJFZCLN-UHFFFAOYSA-N octane-2,4-dione Chemical compound CCCCC(=O)CC(C)=O GJYXGIIWJFZCLN-UHFFFAOYSA-N 0.000 description 1
- BTNXBLUGMAMSSH-UHFFFAOYSA-N octanedinitrile Chemical compound N#CCCCCCCC#N BTNXBLUGMAMSSH-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- OOFGXDQWDNJDIS-UHFFFAOYSA-N oxathiolane Chemical compound C1COSC1 OOFGXDQWDNJDIS-UHFFFAOYSA-N 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- UKODFQOELJFMII-UHFFFAOYSA-N pentamethyldiethylenetriamine Chemical compound CN(C)CCN(C)CCN(C)C UKODFQOELJFMII-UHFFFAOYSA-N 0.000 description 1
- GTCCGKPBSJZVRZ-UHFFFAOYSA-N pentane-2,4-diol Chemical compound CC(O)CC(C)O GTCCGKPBSJZVRZ-UHFFFAOYSA-N 0.000 description 1
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 1
- XRVCFZPJAHWYTB-UHFFFAOYSA-N prenderol Chemical compound CCC(CC)(CO)CO XRVCFZPJAHWYTB-UHFFFAOYSA-N 0.000 description 1
- 229950006800 prenderol Drugs 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 235000013772 propylene glycol Nutrition 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 1
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 description 1
- 125000001973 tert-pentyl group Chemical group [H]C([H])([H])C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- 238000003852 thin film production method Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 150000003613 toluenes Chemical class 0.000 description 1
- 125000005270 trialkylamine group Chemical group 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- 125000004205 trifluoroethyl group Chemical group [H]C([H])(*)C(F)(F)F 0.000 description 1
- 125000000725 trifluoropropyl group Chemical group [H]C([H])(*)C([H])([H])C(F)(F)F 0.000 description 1
- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Abstract
一種含有下述式(1)所示化合物之薄膜形成用原料。
(式(1)中,R1
~R5
各自獨立表示氫原子、碳原子數1~5的烷基或含有氟原子的基,M表示金屬原子,n表示M所示金屬原子之價數。但,R2
、R3
及R4
中至少一個含有氟原子之基)。
Description
本發明係關於新穎化合物、含有該化合物的薄膜形成用原料、將該化合物作為先驅物而使用的方法、使用該方法所製造的薄膜及薄膜之製造方法。
對於半導體、光電池、顯示材料等電子裝置領域,已知有具有β-二亞胺配位基(β-diketiminate)之化合物可作為具有導電性之薄膜的原料。作為薄膜的製造方法,可舉出濺鍍法、離子電鍍法、塗布熱分解法或溶膠-凝膠法等金屬有機化合物分解(MOD:Metal Organic Decomposition)法、化學氣相成長(CVD:Chemical Vapor Deposition)法等。此等中亦以化學氣相成長法之一種的原子層堆積(ALD:Atomic Layer Deposition)法由組成控制性、逐步被覆性優異且適用於量產化,且具有可進行混合整合(Hybrid integration)等多數長所來看,其為薄膜之最佳製造製程。
例如在專利文獻1~3中,使用具有β-二亞胺配位基(β-diketiminate)之化合物,藉由ALD法之含金屬薄膜形成的方法被提案。
[先前技術文獻]
[專利文獻]
[專利文獻1]日本專利第5181292號
[專利文獻2]日本專利第5003978號
[專利文獻3]日本特表2009-503247號公報
[發明所解決的問題]
藉由CVD法將含金屬薄膜形成於基體表面時,可形成蒸氣壓高,熔點低且高品質之含金屬薄膜的薄膜形成用原料為必要,特別欲提高薄膜之生產性,蒸氣壓高的薄膜形成用原料被期待著。過去的β-二亞胺(diketiminate)金屬錯體因蒸氣壓尚未充分,故期待進一步的改善。且,專利文獻3中雖記載包含具有1個以上含氟有機基之β-二亞胺配位基(β-diketiminate)的化合物,但對於該具體結構則無記載。
[解決課題的手段]
本發明者等經重複詳細檢討結果,發現含有具有在特定位置上含有氟原子之基的β-二亞胺配位基(β-diketiminate)之化合物可解決上述課題而完成本發明。
本發明為下述式(1)所示化合物。
式(1)中,R1
~R5
各自獨立表示氫原子、碳原子數1~5的烷基,或含有氟原子的基,M表示金屬原子,n表示M所示金屬原子之價數。但,R2
、R3
及R4
的至少一個表示含有氟原子之基。
式(1)中的R1
~R5
所示含有氟原子的基係以由氟原子所取代的碳原子數1~5的烷基者為佳。
式(1)中之R1
及R5
為碳原子數1~5的烷基,R2
及R4
的至少一個由氟原子所取代之碳原子數1~5的烷基,R3
係以氫原子為佳。
式(1)中之M係以選自銅、鎳、鈷、錫、錳及鋅的金屬原子者為佳。
本發明為含有上述化合物之薄膜形成用原料。
本發明係為使用於藉由化學氣相成長法而製造含金屬薄膜時的使用上述化合物作為先驅物之方法。
本發明為使用上述方法而製造的薄膜。
本發明為將使上述薄膜形成用原料經氣化而得之原料氣體,導入於設置有基體的處理環境內,將該原料氣體中之上述化合物進行分解及/或化學反應而於該基體的表面上形成含金屬薄膜之薄膜的製造方法。
[發明之效果]
依據本發明,可提供蒸氣壓高且熔點低的化合物(β-二亞胺(diketiminate)金屬錯體)。含有該化合物之薄膜形成用原料為藉由CVD法,特別為藉由ALD法,可形成高品質含金屬薄膜。
[實施發明的型態]
本發明之化合物如下述式(1)所示。本發明之化合物適合作為先驅物而使用於具有CVD法之一種的ALD法等氣化步驟的薄膜之製造方法。
(式(1)中,R1
~R5
各自獨立表示氫原子、碳原子數1~5的烷基,或含有氟原子的基,M表示金屬原子,n表示M所示金屬原子的價數。但R2
、R3
及R4
的至少一個表示含有氟原子的基)。
對於上述式(1),作為R1
~R5
所示碳原子數1~5的烷基,可舉出甲基、乙基、丙基、異丙基、丁基、sec-丁基、tert-丁基、異丁基、戊基、異戊基、tert-戊基等。由可得到蒸氣壓高的化合物之觀點來看,以碳原子數1~4的烷基者為佳,以甲基、乙基、異丙基或sec-丁基者為較佳,以甲基或乙基者為更佳。
對於上述式(1),含有R1
~R5
所示氟原子的基若為含有氟原子者即可,亦可為氟原子。此等中亦由可顯著本發明之效果的觀點來看,以由氟原子所取代的碳原子數1~5的烷基為佳,以氟甲基、二氟甲基、三氟甲基、氟乙基、二氟乙基、三氟乙基、氟丙基、二氟丙基、三氟丙基等氟烷基為較佳,以三氟甲基為更佳。
對於上述式(1),M所示金屬原子可舉出鋇、鈦、鋯、鉿、釩、鈮、鉭、鉻、鉬、鎢、錳、鐵、鋨、釕、鈷、錫、銠、銥、鎳、鈀、鉑、銅、銀、金、鋅、鋁、鎵、銦、鍺、鉛、銻、鉍、鐳、鈧、釕、釔、鑭、鈰、鐠、釹、鉤、釤、銪、釓、鋱、鏑、鈥、鉺、銩、鐿、鎦等。此等中亦由可顯著本發明之效果的觀點來看,M以選自銅、鎳、鈷、錫、錳及鋅的金屬原子者為佳。
對於上述式(1),R1
及R5
為碳原子數1~5的烷基,R2
及R4
的至少一個為由氟原子所取代的碳原子數1~5的烷基,且R3
為氫原子之化合物因熔點低,揮發性高,與反應性氣體在低溫下反應,可生產性優良下形成含金屬薄膜故較佳,特別為R1
及R5
為甲基或乙基,R2
為三氟甲基,R3
為氫原子,且R4
為甲基的化合物因可使此等效果顯著故更佳。此等化合物之中,亦以M為鈷之化合物因在常溫下為液體故特佳。
作為本發明之較佳化合物的具體例子,可舉出下述化合物No.1~No.48,但本發明並未限定於此等化合物。且,對於下述化合物No.1~No.48,「Me」表示甲基,「Et」表示乙基,「iPr」表示異丙基,「tBu」表示tert-丁基,「sBu」表示sec-丁基,「CF3
」表示三氟甲基。
上述式(1)所示化合物之製造方法並無特別限制,該化合物可應用周知方法而製造。例如,M為銅之化合物係,將銅甲氧化物溶解於乙醇,加入二亞胺(diketimine)使其反應,除去溶劑,使期蒸餾純化後可得到。又,M為鈷之化合物係,將鈷雙三甲基矽基醯胺溶解於甲苯,加入二亞胺(diketimine)使其反應,除去溶劑,藉由蒸餾純化而可得到。
對於使用本發明之化合物而製造薄膜之成膜裝置,欲確保成膜裝置之配管內的輸送性,本發明之化合物的熔點以未達100℃者為佳,在常溫為液體者為更佳。
其次,對於本發明之薄膜形成用原料進行說明。
本發明之薄膜形成用原料若為含有上述式(1)所示化合物,而可成為薄膜之先驅物者即可,該組成可依據目的的薄膜之種類而相異。例如製造含有作為金屬之僅單一金屬的薄膜時,本發明之薄膜形成用原料中未含有該金屬以外的金屬化合物及半金屬化合物。另一方面,製造含有複數金屬及/或半金屬之薄膜時,本發明之薄膜形成用原料除上述式(1)所示化合物以外,亦可包含具有所望金屬之化合物及/或具有半金屬之化合物(以下稱為「其他先驅物」)。
又,對於使用複數之先驅物的多成分系之CVD法的情況,作為可一起使用上述式(1)所示化合物之其他先驅物,並無特別限制,可使用用於CVD法之薄膜形成用原料中所使用的周知一般先驅物。
作為上述的其他先驅物,例如可舉出選自由醇化合物、甘醇化合物、β-二酮化合物、環戊二烯化合物、有機胺化合物等作為有機配位子使用的化合物所成群的一種類或二種類以上,與矽或金屬之化合物。又,作為先驅物之金屬種,可舉出鋰、鈉、鉀、鎂、鈣、鍶、鋇、鈦、鋯、鉿、釩、鈮、鉭、鉻、鉬、鎢、錳、鐵、鋨、釕、鈷、銠、銥、鎳、鈀、鉑、銅、銀、金、鋅、鋁、鎵、銦、鍺、鉛、銻、鉍、鐳、鈧、釕、釔、鑭、鈰、鐠、釹、鉤、釤、銪、釓、鋱、鏑、鈥、鉺、銩、鐿或鎦。
作為使用作為上述其他先驅物之有機配位子的醇化合物,例如可舉出甲醇、乙醇、丙醇、異丙醇、丁醇、sec-丁基醇、異丁基醇、tert-丁基醇、戊基醇、異戊基醇、tert-戊基醇等的烷基醇類;2-甲氧基乙醇、2-乙氧基乙醇、2-丁氧基乙醇、2-(2-甲氧基乙氧基)乙醇、2-甲氧基-1-甲基乙醇、2-甲氧基-1,1-二甲基乙醇、2-乙氧基-1,1-二甲基乙醇、2-異丙氧基-1,1-二甲基乙醇、2-丁氧基-1,1-二甲基乙醇、2-(2-甲氧基乙氧基)-1,1-二甲基乙醇、2-丙氧基-1,1-二乙基乙醇、2-sec-丁氧基-1,1-二乙基乙醇、3-甲氧基-1,1-二甲基丙醇等醚醇類;二甲基胺基乙醇、乙基甲基胺基乙醇、二乙基胺基乙醇、二甲基胺基-2-戊醇、乙基甲基胺基-2-戊醇、二甲基胺基-2-甲基-2-戊醇、乙基甲基胺基-2-甲基-2-戊醇、二乙基胺基-2-甲基-2-戊醇等二烷基胺基醇類等。
作為使用作為上述其他先驅物之有機配位子的甘醇化合物,例如可舉出1,2-乙烷二醇、1,2-丙烷二醇、1,3-丙烷二醇、2,4-己二醇、2,2-二甲基-1,3-丙烷二醇、2,2-二乙基-1,3-丙烷二醇、1,3-丁二醇、2,4-丁二醇、2,2-二乙基-1,3-丁二醇、2-乙基-2-丁基-1,3-丙烷二醇、2,4-戊烷二醇、2-甲基-1,3-丙烷二醇、2-甲基-2,4-戊烷二醇、2,4-己二醇、2,4-二甲基-2,4-戊烷二醇等。
作為使用作為上述其他先驅物的有機配位子之β-二酮化合物,例如可舉出乙醯丙酮、己烷-2,4-二酮、5-甲基己烷-2,4-二酮、庚烷-2,4-二酮、2-甲基庚烷-3,5-二酮、5-甲基庚烷-2,4-二酮、6-甲基庚烷-2,4-二酮、2,2-二甲基庚烷-3,5-二酮、2,6-二甲基庚烷-3,5-二酮、2,2,6-三甲基庚烷-3,5-二酮、2,2,6,6-四甲基庚烷-3,5-二酮、辛烷-2,4-二酮、2,2,6-三甲基辛烷-3,5-二酮、2,6-二甲基辛烷-3,5-二酮、2,9-二甲基壬烷-4,6-二酮、2-甲基-6-乙基癸烷-3,5-二酮、2,2-二甲基-6-乙基癸烷-3,5-二酮等的烷基取代β-二酮類;1,1,1-三氟戊烷-2,4-二酮、1,1,1-三氟-5,5-二甲基己烷-2,4-二酮、1,1,1,5,5,5-六氟戊烷-2,4-二酮、1,3-二全氟己基丙烷-1,3-二酮等氟取代烷基β-二酮類;1,1,5,5-四甲基-1-甲氧基己烷-2,4-二酮、2,2,6,6-四甲基-1-甲氧基庚烷-3,5-二酮、2,2,6,6-四甲基-1-(2-甲氧基乙氧基)庚烷-3,5-二酮等醚取代β-二酮類等。
作為使用作為上述其他先驅物之有機配位子的環戊二烯化合物,例如可舉出環戊二烯、甲基環戊二烯、乙基環戊二烯、丙基環戊二烯、異丙基環戊二烯、丁基環戊二烯、sec-丁基環戊二烯、異丁基環戊二烯、tert-丁基環戊二烯、二甲基環戊二烯、四甲基環戊二烯等。
作為使用作為上述其他先驅物的有機配位子之有機胺化合物,可舉出甲基胺、乙基胺、丙基胺、異丙基胺、丁基胺、sec-丁基胺、tert-丁基胺、異丁基胺、二甲基胺、二乙基胺、二丙基胺、二異丙基胺、乙基甲基胺、丙基甲基胺、異丙基甲基胺等。
上述其他先驅物在該技術領域中為公知者,該製造方法亦為公知。若要舉出製造方法之一例子,例如作為有機配位子使用醇化合物時,藉由使先前敘述的金屬之無機鹽或該水合物,與該醇化合物之鹼金屬烷氧化物進行反應,可製造出先驅物。其中,作為金屬之無機鹽或該水合物,例如可舉出金屬之鹵化物、硝酸鹽等。作為鹼金屬烷氧化物,例如可舉出鈉烷氧化物、鋰烷氧化物、鉀烷氧化物等。
對於如上述之多成分系的CVD法,有將薄膜形成用原料在各成分獨立下進行氣化、供給的方法(以下稱為「單源方法」),與將預先將多成分原料以所望組成進行混合的混合原料進行氣化、供給之方法(以下稱為「雞尾酒源方法」)。單源方法之情況中,作為上述其他先驅物,以熱及/或氧化分解之作用與上述式(1)所示化合物類似的化合物為佳。雞尾酒源方法之情況中,作為上述其他先驅物,除熱及/或氧化分解之作用與上述式(1)所示化合物類似以外,與上述式(1)所示化合物進行混合時不會因藉由化學反應等而產生變質者為佳。
又,於多成分系之CVD法中的雞尾酒源方法之情況時,將上述式(1)所示化合物與其他先驅物之混合物或該混合物溶解於有機溶劑的混合溶液可作為薄膜形成用原料。
作為上述有機溶劑,可無特別限制下使用公知的一般有機溶劑。作為該有機溶劑,例如可舉出乙酸乙酯、乙酸丁酯、乙酸甲氧基乙酯等乙酸酯類;四氫呋喃、四氫吡喃、乙二醇二甲基醚、二乙二醇二甲基醚、三乙二醇二甲基醚、二丁基醚、二噁烷等醚類;甲基丁基酮、甲基異丁基酮、乙基丁基酮、二丙基酮、二異丁基酮、甲基戊基酮、環己酮、甲基環己酮等酮類;己烷、環己烷、甲基環己烷、二甲基環己烷、乙基環己烷、庚烷、辛烷、甲苯、二甲苯等烴類;1-氰基丙烷、1-氰基丁烷、1-氰基己烷、氰基環己烷、氰苯、1,3-二氰基丙烷、1,4-二氰基丁烷、1,6-二氰基己烷、1,4-二氰基環己烷、1,4-二氰苯等具有氰基的烴類;吡啶、盧剔啶等。此等有機溶劑可藉由溶質之溶解性、使用溫度與沸點、引火點的關係等,可單獨使用,或亦可混合二種類以上使用。
本發明之薄膜形成用原料若為與上述有機溶劑的混合溶液之情況時,於薄膜形成用原料中之先驅物全體的量以0.01莫耳/公升~2.0莫耳/公升者為佳,以0.05莫耳/公升~1.0莫耳/公升者為較佳。
其中,所謂先驅物全體之量表示,本發明之薄膜形成用原料若為未含有上述式(1)所示化合物以外之金屬化合物及半金屬化合物之情況時,其為上述式(1)所示化合物之量,本發明之薄膜形成用原料若為除上述式(1)所示化合物以外,亦含有具有其他金屬的化合物及/或具有半金屬的化合物(其他先驅物)之情況時,其為上述式(1)所示化合物及其他先驅物之合計量。
又,本發明之薄膜形成用原料在視必要時,欲提高上述式(1)所示化合物及其他先驅物之穩定性,可含有求核性試藥。作為該求核性試藥,例如可舉出乙二醇二甲醚(Glyme)、二甘醇二甲醚、三甘醇、四甘醇二甲醚等乙二醇醚類、18-冠-6、二環己基-18-冠-6、24-冠-8、二環己基-24-冠-8、二苯並-24-冠-8等冠醚類、乙二胺、N,N’-四甲基乙二胺、二伸乙基三胺、三亞乙基四胺、四伸乙基五胺、五亞乙基六胺、1,1,4,7,7-五甲基二伸乙基三胺、1,1,4,7,10,10-六甲基三亞乙基四胺、三乙氧基三伸乙基胺等聚胺類、環楞胺(cyclen)、環楞胺(cyclen)等環狀聚胺類、吡啶、吡咯烷、哌啶、嗎啉、N-甲基吡咯烷、N-甲基哌啶、N-甲基嗎啉、四氫呋喃、四氫吡喃、1,4-二噁烷、噁唑、噻唑、氧雜硫戊環等雜環化合物類、乙醯乙酸甲酯、乙醯乙酸乙酯、乙醯乙酸-2-甲氧基乙酯等β-酮酯類或乙醯丙酮、2,4-己烷二酮、2,4-庚烷二酮、3,5-庚烷二酮、二新戊醯基甲烷等β-二酮類。此等求核性試藥之使用量相對於先驅物全體之量1莫耳而言以0.1莫耳~10莫耳之範圍為佳,以1莫耳~4莫耳之範圍為較佳。
本發明之薄膜形成用原料中,使其極力地不要含有構成此的成分以外之雜質金屬元素成分、雜質氯等雜質鹵素成分,及雜質有機成分者為佳。雜質金屬元素成分以每元素中100ppb以下者為佳,以10ppb以下為較佳,在總量中,以1ppm以下為佳,以100ppb以下為較佳。特別為作為LSI之閘絕緣膜、閘膜、阻隔層使用時,必須減少會影響到所得之薄膜的電特性之鹼金屬元素及鹼土類金屬元素的含有量。雜質鹵素成分以100ppm以下為佳,以10ppm以下為較佳,以1ppm以下為更佳。雜質有機成分其總量以500ppm以下為佳,以50ppm以下為較佳,以10ppm以下為更佳。又,水分會成為在薄膜形成用原料中的顆粒產生,或在薄膜形成中之顆粒產生的原因,故對於先驅物、有機溶劑及求核性試藥,欲減低各成分中之水分時,在使用前盡量去除水分較佳。先驅物、有機溶劑及求核性試藥之各水分量以10ppm以下為佳,以1ppm以下為較佳。
又,於本發明之薄膜形成用原料中,欲減低或防止所形成的薄膜之顆粒污染,極力地使其不含顆粒者為佳。具體為,對於在液相藉由光散射式液中粒子檢測器之顆粒測定,比0.3μm大之粒子數在液相1ml中100個以下者為佳,比0.2μm大之粒子數在液相1ml中100個以下者為較佳。
其次,對於使用上述薄膜形成用原料的本發明之薄膜的製造方法做說明。
於本發明之薄膜的製造方法中,可使用公知ALD裝置。作為具體的ALD裝置之例子,可舉出如圖1及圖3所示可使先驅物供給於起泡之裝置,或如圖2及圖4所示具有氣化室之裝置。又,可舉出如圖3及圖4所示對於反應性氣體可進行電漿處理之裝置。且,未限定於如圖1~圖4具備成膜室(以下稱為「堆積反應部」)之葉片式裝置,對於使用分批爐的多數片可同時處理之裝置亦可使用。且,此等亦可作為CVD裝置使用。
本發明之薄膜的製造方法為含有以下步驟者;將使上述薄膜形成用原料進行氣化的原料氣體導入於堆積反應部(處理環境)的步驟(原料氣體導入步驟)、於基體的表面上堆積該原料氣體中之金屬化合物而形成前驅物薄膜之步驟(前驅物薄膜形成步驟)、將反應性氣體導入於堆積反應部(處理環境),使前驅物薄膜與反應性氣體進行反應,於基體之表面上形成含金屬薄膜之步驟(含金屬薄膜形成步驟)。又,本發明之薄膜的製造方法以下述者為佳,其為於前驅物薄膜形成步驟與含金屬薄膜形成步驟之間及/或含金屬薄膜形成步驟之後,具有排出堆積反應部(處理環境)之氣體的步驟(排氣步驟)者為佳。
作為本發明之薄膜的製造方法之一實施形態,依序以前驅物薄膜形成步驟、排氣步驟、含金屬薄膜形成步驟及排氣步驟進行,將藉由一連串的操作之堆積作為1循環,藉由重複該循環,可調整本發明之薄膜的厚度。以下對於本發明之薄膜的製造方法之各步驟進行說明。
(原料氣體導入步驟)
原料氣體導入步驟表示,將上述薄膜形成用原料進行氣化使其成為蒸氣(以下稱為「原料氣體」),將該原料氣體導入於設置有基體之成膜室的步驟。
作為薄膜形成用原料之輸送供給方法,如圖1及圖3所示,在貯藏有本發明之薄膜形成用原料的容器(以下稱為「原料容器」)中藉由加熱及/或減壓進行氣化而成為蒸氣,視必要與氬、氮、氦等載體氣體同時,將該蒸氣導入於設置有基體之堆積反應部內的氣體輸送法,以及如圖2及圖4所示,將薄膜形成用原料在液體或溶液之狀態下輸送至氣化室,在氣化室藉由加熱及/或減壓使其氣化而成為蒸氣,將該蒸氣作為原料氣體導入於堆積反應部之液體輸送法。氣體輸送法之情況中,可將上述式(1)所示化合物本身作為薄膜形成用原料。液體輸送法之情況中,可將上述式(1)所示化合物,或將該化合物溶解於有機溶劑之溶液作為薄膜形成用原料。該混合物或混合溶液可進一步含有求核性試藥等。
又,除上述氣體輸送法及液體輸送法以外,作為使用於原料氣體導入步驟之方法,其中作為含有複數先驅物之多成分系的ALD法,雖有如薄膜形成用原料之欄所記載的單源方法與雞尾酒源方法,對於使用其中任一導入方法,亦以本發明之薄膜形成用原料在0℃~200℃進行氣化者為佳。又,在原料容器內或氣化室內使薄膜形成用原料進行氣化而成為蒸氣時的原料容器內之壓力及氣化室內的壓力係以1Pa~10,000Pa之範圍內者為佳。
其中,作為設置於堆積反應部之上述基體的材質,例如可舉出矽;氮化矽、氮化鈦、氮化鉭、氧化鈦、氧化釕、氧化鋯、氧化鉿、氧化鑭等陶瓷;玻璃;金屬鈷、金屬釕等金屬。作為基體之形狀,可舉出板狀、球狀、纖維狀、鱗片狀。基體表面可為平面亦可成為溝槽結構等三次元結構。
(前驅物薄膜形成步驟)
在前驅物薄膜形成步驟中,導入於設置有基體之堆積反應部的原料氣體中,將上述式(1)所示化合物堆積於基體表面上,於基體表面形成前驅物薄膜。此時,可加熱基體,或加熱堆積反應部而加熱。形成前驅物薄膜時的製造條件並無特別限定,例如可將反應溫度(基體溫度)、反應壓力、堆積速度等對應薄膜形成用原料之種類而適宜地決定。對於反應溫度,本發明之薄膜形成用原料可充分反應之溫度的100℃以上為佳,以100℃~400℃為較佳。反應壓力以1Pa~10,000Pa為佳,以10Pa~1,000Pa為較佳。
又,上述堆積速度可藉由薄膜形成用原料之供給條件(氣化溫度、氣化壓力)、反應溫度、反應壓力來控制。堆積速度過大時所得之薄膜的特性有惡化的情況產生,若過小時在生產性上有問題之情況產生,以0.01nm/分~100nm/分為佳,以0.1nm/分~50nm/分為較佳。
(排氣步驟)
形成前驅物薄膜後,將未在基體的表面上堆積之原料氣體由堆積反應部排出。此時,雖原料氣體由堆積反應部完全排氣者為理想,但非必要完全排氣。作為排氣方法,例如可舉出藉由氦、氮、氬等惰性氣體清除堆積反應部之系統內的方法、減壓系統內而排氣之方法、組合此等的方法等。減壓時的減壓度以0.01Pa~300Pa之範圍為佳,以0.01Pa~100Pa之範圍為較佳。
(含金屬薄膜形成步驟)
在含金屬薄膜形成步驟中,於排氣步驟後,於堆積反應部導入反應性氣體,藉由反應性氣體之作用或反應性氣體之作用與熱的作用,使反應性氣體堆積於前驅物薄膜,即堆積於基體的表面,而與上述式(1)所示化合物進行反應形成含金屬薄膜。
作為上述反應性氣體,例如可舉出氧、臭氧、二氧化氮、一氧化氮、水蒸氣、過氧化氫、甲酸、乙酸、乙酸酐等氧化性氣體、氫等還原性氣體、單烷基胺、二烷基胺、三烷基胺、烷二胺等有機胺化合物、肼、氨等氮化性氣體等。此等反應性氣體可單獨使用,或亦可混合二種類以上使用。
對於前驅物薄膜與反應性氣體之反應,使用熱時,以50℃~200℃為佳,以100℃~200℃為較佳。又,進行本步驟時的堆積反應部中之壓力以1Pa~10,000Pa為佳,以10Pa~1,000Pa為較佳。
(排氣步驟)
上述含金屬薄膜形成後,將未反應的反應性氣體及副產物氣體自堆積反應部排氣。此時,雖反應性氣體及副產物氣體自堆積反應部完全排氣者為理想,但非必要完全排氣。排氣方法及減壓時的減壓度與上述前驅物薄膜形成步驟後之排氣步驟相同。
以上如說明,依序進行原料氣體導入步驟、前驅物薄膜形成步驟、排氣行程、含金屬薄膜形成步驟及排氣步驟,將藉由一連串的操作之堆積作為1循環,重複進行複數次該循環至得到必要膜厚之薄膜,進而製造出含有所望膜厚之含金屬薄膜。在使用ALD法的薄膜之製造方法中,可將所形成之含金屬薄膜的膜厚以上述循環的次數進行控制。
又,對於本發明之薄膜的製造方法,如圖3及圖4所示,對堆積反應部可輸入電漿、光、電壓等能量,亦可使用觸媒。輸入該能量之時期及使用觸媒之時期並無特別限定,例如原料氣體導入步驟中之薄膜形成用原料的原料氣體導入時、形成前驅物薄膜時的加熱步驟,或含金屬薄膜形成步驟中之反應氣體導入時,或亦可為使反應性氣體與前驅物薄膜進行反應時、排氣步驟中之系統內的排氣時,亦可在上述各步驟之間。
又,對於本發明之薄膜的製造方法,於薄膜之形成後,欲得更良好的電氣特性,可在惰性環境下、氧化性環境下或還原性環境下進行退火處理,逐步嵌入為必要時,可設有回流步驟。此時的溫度以200℃~1,000℃為佳,以250℃~500℃為較佳。
使用本發明之薄膜形成用原料而製造之薄膜可藉由適宜地選擇其他先驅物、反應性氣體及製造條件,包覆金屬、氧化物陶瓷、氮化物陶瓷、玻璃等基體,成為所望種類的薄膜。本發明之薄膜因電氣特性及光學特性優異,故例如可廣泛地使用於DRAM元件作為代表的記憶元件之電極材料、電阻膜、使用於硬碟記錄層之反磁性膜及固體高分子形燃料電池用之觸媒材料等製造上。
[實施例]
以下使用實施例等更詳細說明本發明。但本發明並非受到以下實施例等限制者。
[實施例1] 化合物No.1之合成
於100ml之四口燒瓶中,在室溫下加入銅(II)甲氧化物錯體0.60g(4.7mmol)與脫水乙醇20ml,將對應的二亞胺(diketimine)配位子1.69g(9.4mmol)在冰冷下滴入,在室溫下進行20小時攪拌。在油浴75℃且微減壓下餾去乙醇。此後將殘留於燒瓶內之紫色固體在減壓下(50Pa)蒸餾,作為流出成分得到紫色固體0.92g(2.2mmol,產率46%)。該固體的藉由單結晶X線解析之分析結果,確認為目的化合物之化合物No.1。所得之紫色固體的藉由單結晶X線解析之分子結構如圖5所示。
化合物No.1之單結晶X線解析結果
結晶格子尺寸:0.11mm×0.11mm×0.10mm
結晶系:三斜晶系
(於非對稱單位中分子2個,R1=0.0820,wR2=0.1807)
格子參數:
a=8.859Å
b=9.349Å
c=12.58Å
α=74.69°
β=71.28°
γ=63.91°
V=877Å3
[實施例2] 化合物No.19之合成
於100ml之四口燒瓶中,在室溫下加入鈷雙三甲基矽基醯胺錯體8.4g(22.2mmol)與脫水甲苯50ml,將對應的二亞胺(diketimine)配位子6.8g(44.4mmol)在室溫下滴入,進行2小時反應。在油浴100℃且微減壓下餾去甲苯溶劑。此後將殘留於燒瓶內之濃褐色黏性液體在減壓下(20~30Pa)蒸餾,得到作為餾出成分之濃紅褐色液體7.5g (20.5mmol,產率92.4%)。所得之濃紅褐色液體在室溫下慢慢地固化而成為熔點38℃之濃紅褐色固體。該固體之藉由單結晶X線解析的分析結果,確認其為目的化合物之化合物No.19。所得之濃紅褐色固體的藉由單結晶X線解析之分子結構如圖6所示。
化合物No.19之單結晶X線解析結果
結晶格子尺寸:0.26mm×0.24mm×0.07mm
結晶系:單斜晶系
(於非對稱單位中分子8個,R1=0.0598,wR2=0.1310)
格子參數:
a=28.047Å
b=9.9896Å
c=18.954Å
β=125.704°
V=4312Å3
[實施例3] 化合物No.27之合成
於100ml之四口燒瓶中,在室溫下加入錫雙三甲基矽基醯胺錯體1.65g(3.8mmol)與脫水己烷25ml,將對應的二亞胺(diketimine)配位子1.58g(7.6mmol)在冰冷下滴入,進行16小時反應。在油浴60℃且微減壓下將己烷溶劑餾去。此後將殘留於燒瓶內之橙色液體在減壓下(20~30Pa)蒸餾,得到作為餾出成分之黃色固體0.05g(0.1mmol,產率2.5%)。該黃色固體之藉由1
H-NMR及ICP-AES的分析結果,確認其為目的化合物之化合物No.27。所得之黃色固體的藉由1
H-NMR及ICP-AES之分析結果如以下所示。
(藉由1
H-NMR(重苯)之分析結果)
0.868-0.904ppm (3H, triplet)、1.147-1.183ppm (3H, triplet)、1.563ppm (3H, singlet)、3.049-3.067ppm (2H, doublet)、3.585ppm (2H, singlet)、5.166ppm (1H, singlet)
(藉由ICP-AES之分析結果)
錫含有量:22.1質量%(理論值:22.27質量%)
[實施例4] 化合物No.43之合成
於100ml的四口燒瓶中,在室溫下加入氯化鋅錯體0.57g(4.2mmol)與醚40ml,將經Li化的對應之二亞胺(diketimine)配位子1.93g(8.4mmol)在冰冷下滴入,進行16小時反應。在油浴50℃且常壓下使醚溶液餾去。於所得之黃色固體中加入己烷並進行過濾。將濾液在油浴60℃且微減壓下進行脫溶劑。此後將殘留於燒瓶內之橙色液體在減壓下(20~30Pa)蒸餾,得到作為餾出成分的淡黃色液體1.18g(2.5mmol,產率59%)。該淡黃色液體的藉由1
H-NMR及ICP-AES之分析結果,確認其為目的化合物之化合物No.43。所得之淡黃色液體的藉由1
H-NMR及ICP-AES之分析結果如以下所示。
(藉由1
H-NMR(重苯)之分析結果)
0.889-0.925ppm (3H, triplet)、1.079-1.115ppm (3H, triplet)、1.547ppm (3H, singlet)、2.977-3.043ppm (2H, multiplet)、3.502-3.557ppm (2H, multiplet)、5.008ppm (1H, singlet)
(藉由ICP-AES之分析結果)
鋅含有量:13.8質量%(理論值:13.63質量%)
[比較例1] 比較化合物1之合成
嘗試進行於式(1)中,R1
及R5
為CH2
CF3
,R2
及R4
為Me,R3
為H,且M為Cu之下述比較化合物1的合成。
在100ml之四口燒瓶中,於室溫下加入銅(II)甲氧化物錯體1.07g(8.5mmol)與脫水乙醇50ml,將下述比較化合物1與對應的二亞胺(diketimine)配位子4.46g(17mmol)在冰冷下滴入,在室溫進行18小時攪拌。在油浴75℃且微減壓下將乙醇餾去。此後將殘留於燒瓶內之黑色固體在減壓下(50Pa)蒸餾,但無法分離出目的物。
[評估例]
使用在上述實施例1~4所合成而得之化合物No.1、化合物No.19、化合物No.27、化合物No.43及下述表1~4所記載的比較化合物2~5進行下述評估。
(1)熔點評估
藉由目視,觀察在常壓25℃中之化合物的狀態,對於固體化合物使用微小熔點測定裝置來測定熔點。此等結果如表1~4所示。
(2)減壓TG-DTA50質量%減少時之溫度(℃)
使用TG-DTA,在10Torr、Ar流量:50mL/分、昇溫速度10℃/分且將掃描溫度範圍設定在30℃~600℃而測定,將試驗化合物之重量減少50質量%時的溫度(℃)作為「減壓TG-DTA50質量%減少時之溫度(℃)」而評估。減壓TG-DTA50質量%減少時之溫度(℃)越低,在低溫下更能得到蒸氣。對於此等結果如表1~4所示。
[實施例5]
將上述化合物No.1作為薄膜形成用原料使用,使用圖1之ALD裝置,在下述條件下,於基體的釕晶圓之表面上製造薄膜。使用X線電子分光法來分析薄膜之組成時,確認薄膜為含有銅之薄膜,殘留碳含有量比檢測限界之0.1atom%更少。又,使用掃描型電子顯微鏡法來測定薄膜之膜厚時,形成於釕晶圓表面上之薄膜為2nm之平滑膜,每1循環所得之膜厚約0.02nm。
(製造條件)
製造方法:ALD法
反應溫度(基體溫度):200℃
反應性氣體:氫
(步驟)
將由下述(1)~(4)所成的一連串步驟作為1循環,重複進行100循環。
(1)在原料容器溫度120℃,原料容器內壓力100Pa之條件下,將經氣化的薄膜形成用原料之蒸氣(原料氣體)導入於堆積反應部,在系統壓力100Pa下20秒間,於基體表面堆積原料氣體而形成前驅物薄膜。
(2)藉由15秒間之氬清除,將未堆積的原料氣體自系統內排氣出。
(3)將反應性氣體導入於堆積反應部,在系統壓力100Pa下20秒間,使前驅物薄膜與反應性氣體進行反應。
(4)藉由15秒間之氬清除,將未反應的反應性氣體及副產物氣體自系統內排氣出。
[實施例6]
將上述化合物No.19作為薄膜形成用原料使用,將反應溫度變更為300℃,將步驟變更為300循環以外,藉由與實施例5同樣之方法,於釕晶圓的表面上製造出薄膜。使用X線電子分光法分析薄膜之組成時,薄膜為含有鈷之薄膜,確認殘留碳含有量比檢測限界的0.1atom%少。又,使用掃描型電子顯微鏡法來測定薄膜的膜厚時,形成於釕晶圓表面上之薄膜為6nm的平滑膜,每1循環所得之膜厚約0.02nm。
[實施例7]
將釕晶圓變更為銅晶圓以外,藉由與實施例6之同樣方法,於銅晶圓的表面上製造出薄膜。使用X線電子分光法分析薄膜的組成後,確認薄膜為含有鈷之薄膜,殘留碳含有量比檢測限界之0.1atom%少。使用掃描型電子顯微鏡法來測定薄膜的膜厚時,於銅晶圓表面上所形成的薄膜為3nm之平滑膜,每1循環所得之膜厚約0.01nm。
[比較例6]
將化合物No.1變更為比較化合物2,將原料容器溫度120℃變更為140℃以外,以與實施例5同樣方法,於釕晶圓的表面上製造出含有銅之薄膜,但無法形成平滑膜。又,於所得之膜上檢測出殘留碳。
[比較例7]
將化合物No.19變更為比較化合物3,將原料容器溫度120℃變更為140℃以外,以與實施例6同樣方法,於釕晶圓之表面上製造出含有鈷的薄膜,但無法形成平滑膜。又,於所得之膜檢測出殘留碳。
[比較例8]
將釕晶圓變更為銅晶圓以外,以與比較例7同樣方法,於銅晶圓的表面上製造出含有鈷之薄膜,但無法形成平滑膜。又,於所得之膜檢測出殘留碳。
由比較例1之結果可得知,於式(1)中之R2
、R3
及R4
以外的R為含有氟原子的基之化合物的製造為困難。
作為對於比較例6、7及8無法製造出良好薄膜的原因,考慮為因比較化合物2及3之蒸氣壓低,而必須提高原料容器溫度,但在原料容器溫度在140℃之條件下,對比較化合物2及3會產生熱分解之故。
由以上可確認,對於將式(1)所示化合物中,R2
、R3
及R4
的至少一個由含有氟原子之基所取代的化合物作為薄膜形成用原料使用時,可製造出揮發性高且品質佳的薄膜。
[圖1]表示使用於有關本發明的薄膜之製造方法的ALD裝置之一例概略圖。
[圖2]表示使用於有關本發明的薄膜之製造方法的ALD裝置之其他例子概略圖。
[圖3]表示使用於有關本發明的薄膜之製造方法的ALD裝置之另其他例子概略圖。
[圖4]表示使用於有關本發明的薄膜之製造方法的ALD裝置之進一步另其他例子概略圖。
[圖5]表示化合物No.1藉由單結晶X線解析之分子結構圖。
[圖6]表示化合物No.19藉由單結晶X線解析之分子結構圖。
Claims (6)
- 如請求項1之化合物,其中式(1)中之M為選自銅、鎳、鈷、錫、錳及鋅之金屬原子。
- 一種薄膜形成用原料,其中含有如請求項1或2之化合物。
- 一種使用於製造含金屬薄膜的藉由將如請求項1或2之化合物作為先驅物之化學氣相成長法的用途。
- 一種薄膜,其為使用如請求項4之方法而製造者。
- 一種薄膜的製造方法,其為將使如請求項3之薄膜形成用原料進行氣化而得之原料氣體,導入於設置有基體之處理環境內,將前述原料氣體中之前述化合物進行分解及/或化學反應之於該基體的表面形成含金屬薄膜之薄膜的製造方法。
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