TWI715787B - 薄膜形成用原料及薄膜之製造方法 - Google Patents
薄膜形成用原料及薄膜之製造方法 Download PDFInfo
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- TWI715787B TWI715787B TW106121625A TW106121625A TWI715787B TW I715787 B TWI715787 B TW I715787B TW 106121625 A TW106121625 A TW 106121625A TW 106121625 A TW106121625 A TW 106121625A TW I715787 B TWI715787 B TW I715787B
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- thin film
- raw material
- film
- general formula
- metal
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- 239000002994 raw material Substances 0.000 title claims abstract description 71
- 239000010409 thin film Substances 0.000 title claims description 71
- 238000000034 method Methods 0.000 title claims description 57
- 238000004519 manufacturing process Methods 0.000 title claims description 34
- 150000001875 compounds Chemical class 0.000 claims abstract description 58
- 229910052751 metal Inorganic materials 0.000 claims abstract description 46
- 239000002184 metal Substances 0.000 claims abstract description 45
- 239000010936 titanium Substances 0.000 claims abstract description 16
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 15
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 15
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- 229910052719 titanium Inorganic materials 0.000 claims abstract description 14
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052735 hafnium Inorganic materials 0.000 claims abstract description 13
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 13
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 9
- 239000010408 film Substances 0.000 claims description 77
- 239000000758 substrate Substances 0.000 claims description 20
- 239000000126 substance Substances 0.000 claims description 18
- 230000008016 vaporization Effects 0.000 claims description 12
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- 230000006837 decompression Effects 0.000 description 4
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- 238000010586 diagram Methods 0.000 description 4
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- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 description 4
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- 150000001298 alcohols Chemical class 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 238000007664 blowing Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
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- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 2
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- XGGCYHBYGFNQIP-UHFFFAOYSA-N 2,2,6-trimethyloctane-3,5-dione Chemical group CCC(C)C(=O)CC(=O)C(C)(C)C XGGCYHBYGFNQIP-UHFFFAOYSA-N 0.000 description 2
- OISVCGZHLKNMSJ-UHFFFAOYSA-N 2,6-dimethylpyridine Chemical group CC1=CC=CC(C)=N1 OISVCGZHLKNMSJ-UHFFFAOYSA-N 0.000 description 2
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 description 2
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 description 2
- HCFAJYNVAYBARA-UHFFFAOYSA-N 4-heptanone Chemical compound CCCC(=O)CCC HCFAJYNVAYBARA-UHFFFAOYSA-N 0.000 description 2
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- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 2
- 229910052772 Samarium Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- DHXVGJBLRPWPCS-UHFFFAOYSA-N Tetrahydropyran Chemical compound C1CCOCC1 DHXVGJBLRPWPCS-UHFFFAOYSA-N 0.000 description 2
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 229910052769 Ytterbium Inorganic materials 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
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- 238000002716 delivery method Methods 0.000 description 2
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 2
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- 238000011156 evaluation Methods 0.000 description 2
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- 229910017053 inorganic salt Inorganic materials 0.000 description 2
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Abstract
Description
本發明係關於一種含有特定之化合物而成之薄膜形成用原料及使用該薄膜形成用原料薄膜之製造方法。
氧化鋯或氧化鈦等之金屬氧化物被應用作為半導體記憶體材料中閘極絕緣膜。又,含有碳化鋯、碳化鉿、碳化鈦等的金屬碳化物之薄膜可使用於切削工具、電子材料用之配線或電極,例如亦被檢討對半導體記憶體材料或鋰空氣電池用的電極等之應用。
作為上述薄膜之製造法,舉例為濺鍍法、離子鍍敷法、塗佈熱分解法或溶凝膠法等之MOD法、化學氣相成長法等,但包含ALD(Atomic Layer Deposition,原子層成長)法之化學氣相成長(以下有時僅記載為「CVD」)法,由於具有組成控制性、階差被覆性優異,適於量產 化,且可混成積體等之多種優點,故為最適之製造製程。
在專利文獻1及專利文獻2中,作為ALD法之含有鈦的薄膜形成用原料被揭示為Ti(C5Me5)(Me)3。然而,Ti(C5Me5)(Me)3係熱安定性不佳,故在薄膜中混入作為有機物之殘留碳成分,有無法形成高品質的薄膜之問題。
[專利文獻1]日本特開2006-310865號公報
[專利文獻2]日本特表2009-545135號公報
使用化學氣相成長法之含有金屬的薄膜之製造方法中所要求的事係在所使用之薄膜形成用原料中無自燃性,可安全地形成薄膜,且該薄膜形成用原料之熱分解性及/或反應性氣體之反應性佳、生產性優良。又,在所得之含有金屬的薄膜中混入碳成分為少,亦要求高品質者。以往,藉由該等之點,並無可充分地滿足之薄膜形成用原料及薄膜之製造方法。
本發明人等重複檢討之結果,發現含有特定 之化合物之薄膜形成用原料及使用該薄膜形成用原料之含有金屬的薄膜之製造方法可解決上述課題,因而完成本發明。
(式中,R1~R4係表示可相同或相異之碳原子數1~5之烷基,R5~R7係表示可相同或相異之碳原子數1~5之烷基,M係表示鈦、鋯或鉿)。
本發明係提供一種薄膜之製造方法,其係將含有使上述之薄膜形成用原料氣化而得之以通式(1)表示之化合物的蒸氣,導入設置有基體的成膜腔室內,使該化合物分解及/或使其進行化學反應而於該基體之表面形成含有選自鈦、鋯及鉿中至少1種之金屬的薄膜。
依據本發明,可提供一種薄膜形成用原料,其適合於用以形成含有金屬之薄膜所使用的化學氣相成長 用之薄膜形成用原料,故再進一步安全地製造生產性優良、品質佳之含有金屬的薄膜。
[圖1]圖1係顯示本發明之含有金屬的薄膜之製造方法中可使用之化學氣相成長用裝置之一例之概要圖。
[圖2]圖2係顯示本發明之含有金屬的薄膜之製造方法中可使用之化學氣相成長用裝置之另一例之概要圖。
[圖3]圖3係顯示本發明之含有金屬的薄膜之製造方法中可使用之化學氣相成長用裝置之另一例之概要圖。
[圖4]圖4係顯示本發明之含有金屬的薄膜之製造方法中可使用之化學氣相成長用裝置之另一例之概要圖。
本發明之薄膜形成用原料係含有以上述通式(1)表示之化合物的薄膜形成用原料,可較佳地作為具有CVD法等之氣化步驟之薄膜製造方法之前驅物者,亦可使用ALD法形成薄膜。
上述通式(1)中,R1~R4係表示可相同或相異之碳原子數1~5之烷基,R5~R7係表示可相同或相異之碳原子數1~5之烷基,M係表示鈦、鋯或鉿。
作為以上述R1~R4及以R5~R7表示之碳原子數1~5之烷基係可舉例甲基、乙基、丙基、異丙基、丁基、 異丁基、第二丁基、第三丁基、戊基、異戊基等。
上述通式(1)中,R1~R4之至少1種為1級烷基之時或R5~R7之至少1種為1級烷基之時,以通式(1)表示之化合物的蒸氣壓為高,故可製造生產性佳之含有金屬的薄膜,故為佳。其中,R1~R4之全部為1級烷基之時或、R5~R7之全部為1級烷基之時,以通式(1)表示之化合物之蒸氣壓特別高,故可製造生產性佳之含有金屬的薄膜,故為佳。再者,R1~R4及R5~R7之全部為甲基之時,可適用於稱為ALD視窗之ALD法的溫度範圍寬廣,可製造高品質的薄膜,故為佳。
以上述通式(1)表示之化合物係依據其製造方法並不特別限制,應用周知之反應而製造。作為製造方法係例如M為鈦之時,在四烷基環戊二烯基三氯鈦中,於-20℃~50℃下,較佳於0℃~30℃下,藉由使其反應得到烷基鋰。M為鋯或鉿之時亦可用相同之方法製造。
作為以通式(1)表示之化合物之較佳具體例以例如舉例為以下述化合物No.1~No.12表示之化合物。尚,下述化合物No.1~No.12中,「Me」表示甲基,「Et」表示乙基。
所謂本發明之薄膜形成用原料係將以通式(1)表示之化合物,作為用以形成含有金屬之薄膜的化學氣相成長法用前驅物者,且該形態可依據該薄膜形成用原料所適用之製造製程而相異。例如,製造含有選自鈦、鋯及鉿中至少1種之金屬的薄膜時,本發明之薄膜形成用原料不含以上述通式(1)表示之化合物以外之金屬化合物及半金屬化合物。另一方面,製造含有鈦、鋯及鉿以外之金屬及/或半金屬與選自鈦、鋯及鉿中至少1種的金屬之薄膜時,除了上述以通式(1)表示之化合物以外,本發明之薄膜形成用原料含有包含鈦、鋯及鉿以外之金屬的化合物及/或包含半金屬之化合物(以下亦稱為「其他前驅物」)。本發明之薄膜形成用原料如後述,亦可進一步含有有機溶劑及/或親核性試藥。本發明之薄膜形成用原料如上述說明, 由於適用於以前驅物之通式(1)表示之化合物的物性為CVD法、ALD法,故特別作為化學氣相成長用原料(以下亦稱為「CVD用原料」)有用。
本發明之薄膜形成用原料之形態可依據所使用的CVD法之輸送供給方法等方法而適當選擇。
作為上述之輸送供給方法,有將CVD用原料於儲存該原料之容器(以下有時亦簡單記載為「原料容器」)中加熱及/或減壓而氣化為蒸氣,將該蒸氣與根據需要使用之氬、氮、氦等之載氣一起導入設置基體之成膜腔室內(以下有時亦記載為「堆積反應部」)之氣體輸送法,將CVD用原料以液體或溶液狀態輸送至氣化室,於氣化室藉由加熱及/或減壓而氣化為蒸氣,將該蒸氣導入成膜腔室內之液體輸送法。氣體輸送法時,以上述通式(1)表示之化合物本身可使用作為CVD用原料。液體輸送法之情況,可將以上述通式(1)表示之化合物本身或該化合物溶於有機溶劑中之溶液作為CVD用原料。該等之CVD用原料亦可進一部包含其他前驅物或親核性試藥。
又,於多成分系之CVD法中,有使CVD用原料各成分獨立氣化並供給之方法(以下有時亦記載為「單一源法」)與使多成分原料預先以期望組成混合之混合原料氣化並供給之方法(以下有時亦記載為「混合源法」)。混合源法之情況,可將以上述通式(1)表示之化合物與其他前驅物之混合物或者將該混合物溶於有機溶劑之混合溶液作為CVD用原料。該混合物或混合溶液亦可進一步包含 親核性試藥等。
作為上述有機溶劑並未特別限制,可使用周知之一般有機溶劑。作為該有機溶劑可舉例為例如甲醇、乙醇、異丙醇、正丁醇等之醇類;乙酸乙酯、乙酸丁酯、乙酸甲氧基乙酯等之乙酸酯類;四氫呋喃、四氫吡喃、乙二醇二甲醚、二乙二醇二甲醚、三乙二醇二甲醚、二丁醚、二噁烷等之醚類;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、甲基環己酮等之酮類;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、二甲苯等之烴類;1-氰基丙烷、1-氰基丁烷、1-氰基己烷、氰基環己烷、氰基苯、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、1,4-二氰基苯等之具有氰基之烴類;吡啶、二甲基吡啶(lutidine)等。該等之有機溶劑可根據溶質之溶解性、使用溫度與沸點、起火點之關係等而單獨或混合兩種類以上之使用。使用該等之有機溶劑時,將前驅物溶於有機溶劑之溶液的CVD用原料中之前驅物全體量0.01~2.0莫耳/升為佳,特佳為0.05~1.0莫耳/升。所謂前驅物全體量,於本發明之薄膜形成用原料不含以上述通式(1)表示之化合物以外之金屬化合物及半金屬化合物時,為以上述通式(1)表示之化合物的量,於本發明之薄膜形成用原料含有除了包含以上述通式(1)表示之化合物以外之金屬的化合物及/或包含半金屬的化合物(其他前驅物)時,為以上述通式(1)表示之化合物及其他前驅物之 合計量。
且,於多成分系之CVD法時,作為與以上述通式(1)表示之化合物一起使用之其他前驅物並未特別限制,可使用於CVD用原料中所用之周知一般前驅物。該前驅物所使用之配位基係於構造中不含氧原子,但可減少所得之含有金屬的薄膜中之氧的混入量,故特別佳。
作為上述之其他的前驅物係可舉例選擇自醇化合物、二醇化合物、β-二酮化合物、環戊二烯化合物、作為有機胺化合物等之有機配位基可使用之化合物所成之群中一種類或二種類以上與矽或金屬(但是,除了鈦、鋯及鉿之外)之化合物。又,作為前驅物之金屬種,可舉例為鎂、鈣、鍶、鋇、釩、鈮、鉭、鋁、錳、鐵、釕、鈷、銠、銥、鎳、鈀、鉑、銅、銀、金、鋅、鎵、銦、鍺、錫、鉛、銻、鉍、鈧、釔、鑭、鈰、鐠、釹、鉅、釤、銪、釓、鋱、鏑、鈥、鉺、銩、鐿、鎦等。
作為上述之有機配位基可使用之醇化合物係可舉例甲醇、乙醇、丙醇、異丙醇、丁醇、第2丁醇、異丁醇、第3丁醇、戊醇、異戊醇、第3戊醇等之烷醇類;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-s-丁氧基-1,1-二乙基乙醇、3-甲氧基-1,1-二甲基丙醇等之醚醇類 等。
作為上述之其他前驅物之有機配位基可使用之二醇化合物係可舉例1,2-乙二醇、1,2-丙二醇、1,3-丙二醇、2,4-己二醇、2,2-二甲基-1,3-丙二醇、2,2-二乙基-1,3-丙二醇、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-丙二醇、2,4-戊二醇、2-甲基-1,3-丙二醇、2-甲基-2,4-戊二醇、2,4-己二醇、2,4-二甲基-2,4-戊二醇等。
又,作為β-二酮化合物係可舉例乙醯丙酮、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-3,5-二酮等之烷基取代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-1,3-二酮等之氟取代烷基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-3,5-二酮等之醚取代β-二酮類等。
又,作為環戊二烯化合物係可舉例環戊二烯、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、第2丁基環戊二烯、異丁基環戊二烯、第3丁基環戊二烯、二甲基環戊二烯、四甲基環戊二烯等;作為上述之有機配位基可使用之有機胺化合物係可舉例甲基胺、乙基胺、丙基胺、異丙基胺、丁基胺、第2丁基胺、第3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。
作為上述之有機配位基可使用之有機胺化合物係可舉例酮亞胺化合物、脒基化合物(amidinate compound)、甲基胺、乙基胺、丙基胺、異丙基胺、丁基胺、第2丁基胺、第3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、雙(三甲基矽烷基)胺等。
上述之其他前驅物為本技術領域中習知者,其製造方法亦為習知。若舉製造方法之一例,在例如使用醇化合物作為有機配位基時,藉由使如前述之金屬無機鹽或其水合物與該醇化合物之鹼金屬烷氧化物反應,可製造前驅物。於此,金屬之無機鹽或其水合物可舉例為金屬之鹵化物、硝酸鹽等,作為鹼金屬烷氧化物可舉例為烷氧化鈉、烷氧化鋰、烷氧化鉀等。
上述之其他前驅物,於單一源法時,以上述通式(1)表示之化合物與熱及/或氧化分解行為類似之化合物為佳,於混合源法時,除了熱及/或氧化分解行為類似以外,混合時不引起化學反應等變質者為較佳。
又,本發明之薄膜形成用材料,根據需要,為了賦予該原料之安定性,亦可含有親核性試藥。作為該親核性試藥舉例為甘醇二甲醚、二甘醇二甲醚、三甘醇二甲醚、四甘醇二甲醚等之乙二醇醚類,18-冠狀醚-6、二環己基-18-冠狀醚-6、24-冠狀醚-8、二環己基-24-冠狀醚-8、二苯并-24-冠狀醚-8等之冠狀醚類,乙二胺、N,N’-四甲基乙二胺、二伸乙三胺、三伸乙四胺、四伸乙五胺、五伸乙六胺、1,1,4,7,7-五甲基二伸乙三胺、1,1,4,7,10,10-六甲基三伸乙四胺、三乙氧基三伸乙胺等之聚胺類,四氮雜環十四烷(cyclam)、四氮雜環十二烷(cyclen)等之環狀聚胺類,吡啶、吡咯啶、哌啶、嗎啉、N-甲基吡咯啶、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、氧雜硫雜環戊烷(oxathiolane)等之雜環化合物類,乙醯乙酸甲酯、乙醯乙酸乙酯、乙醯乙酸-2-甲氧基乙酯等之β-酮酯類或乙醯丙酮、2,4-己二酮、2,4-庚二酮、3,5-庚二酮、二特戊醯基甲烷等之β-二酮類,該等親核性試藥之使用量,對於上述通式(1)表示之化合物1莫耳,0.1莫耳~10莫耳之範圍為佳,1~4莫耳為更佳。又,使用該等之親核性試藥時,於該親核性試藥之構造中不包含氧原子為佳,進一步於構造中包含氮原子為特別佳。
在本發明之薄膜形成用原料中極力不包含構成其之成分以外之雜質金屬元素分、雜質氯等之雜質鹵素分及雜質有機分。雜質金屬元素分之每原素100ppb以下為佳,10ppb以下為更佳,總量計係1ppm以下為佳,100ppb 以下為更佳。尤其,使用作為LSI之閘極絕緣膜、閘極膜、障壁層時,必須減少對所得薄膜之電特性有影響之鹼金屬元素、鹼土類金屬元素及同族元素之含量。雜質鹵素分100ppm以下為佳,10ppm以下為更佳,1ppm以下為最佳。雜質有機分總量計係500ppm以下為佳,50ppm以下為更佳,10ppm以下為最佳。又,由於水分係化學氣相成長用原料中之顆粒發生或薄膜形成中之顆粒發生之原因,故前驅物、有機溶劑及親核性試藥中,為了減低各自之水分,使用時較佳預先儘可能去除水分。前驅物、有機溶劑及親核性試藥各水分量10ppm以下為佳,1ppm以下為更佳。
又,本發明之薄膜形成用原料,為了減低或防止所形成之薄膜的顆粒污染,較好極力不包含顆粒。具體而言,於液相之藉由光散射式液中粒子檢測器之顆粒測定中,大於0.3μm之粒子數於液相1ml中100個以下為佳,大於0.2μm之粒子數於液相1ml中1000個以下為更佳,大於0.2μm之粒子數於液相1ml中100個以下為最佳。
作為本發明之薄膜之製造方法,係將以上述通式(1)表示之化合物氣化之蒸氣及根據需要使用之反應性氣體導入設置有基體之成膜腔室內,接者,使前驅物於基體上及/或成膜腔室內及/或氣體導入口附近分解及/或化學反應,於基體表面成長並堆積含金屬之薄膜的CVD法者。原料之輸送供給方法、堆積方法、製造條件、製造裝置等並未特別受到限制,可使用周知之一般條件及方法。
作為上述根據需要使用之反應性氣體,例如作為氧化性者舉例為氧、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,作為還原性者舉例為氫,且作為製造氮化物者,舉例為單烷胺、二烷胺、三烷胺、伸烷二胺等之有機胺化合物、聯胺、氨等,該等可使用一種或兩種以上。又,使上述反應性氣體與前驅物反應之前,亦可預先進行電漿處理。
且,作為上述輸送供給方法,舉例為前述之氣體輸送法、液體輸送法、單一源法、混合源法等。
又,作為上述之堆積方法,舉例為使原料氣體或使原料氣體與反應性氣體僅藉由熱而反應並堆積薄膜之熱CVD,使用熱與電漿之電漿CVD,使用熱與光之光CVD,使用熱、光及電漿之光電漿CVD,將CVD之堆積反應分為基本過程,以分子等級進行階段性堆積之ALD。
上述基體之材質舉例為例如矽;砷化銦、砷化銦鎵、二氧化矽、氮化矽、碳化矽、氮化鈦、氧化鉭、氮化鉭、氧化鈦、氮化鈦、氧化釕、氧化鋯、氧化鉿、氧化鑭、氮化鎵等之陶瓷;玻璃;鉑-釕、鋁、銅、鎳、鈷、鎢、鉬等之金屬。基體之形狀舉例為板狀、球狀、纖維狀、鱗片狀,基體表面可為平面,亦可成為溝槽構造等之三次元構造。
且,作為上述製造條件,舉例為反應溫度(基體溫度)、反應壓力、堆積速度等。關於反應溫度,使之以上述通式(1)表示之化合物充分地反應之溫度的100℃以 上為佳,150℃~400℃為更佳。又,反應壓力於熱CVD、光CVD時,大氣壓~10Pa為佳,使用電漿時,2000Pa~10Pa為佳。又,堆積速度可藉由原料之供給條件(氣化溫度、氣化壓力)、反應溫度、反應壓力而控制。堆積速度若太大則有所得薄膜特性惡化之情況,太小則有生產性產生問題之情況,因此0.01~100nm/分鐘為佳,1~50nm/分鐘為更佳。且,ALD法時,以循環次數進行控制以獲得所期望膜厚。
作為上述製造條件進一步舉例為使薄膜形成用原料氣化成為蒸氣時之溫度或壓力。使薄膜形成用原料氣化成為蒸氣之步驟可在原料容器內進行,亦可在氣化室內進行。任一情況下,本發明薄膜之製造方法中使用之薄膜形成用原料在0~150℃蒸發為佳。又,於原料容器內或氣化室內使薄膜形成用原料氣化成為蒸氣時,原料容器內之壓力及氣化室內之壓力均佳為1~10000Pa。
本發明之薄膜之製造方法除了採用ALD法,藉由上述輸送供給方法使薄膜形成用原料氣化成為蒸氣,將該蒸氣導入成膜腔室內之原料導入步驟以外,亦可具有藉由該蒸氣中之以上述通式(1)表示之化合物於上述基體表面形成前驅物薄膜之前驅物薄膜成膜步驟,將未反應之以上述通式(1)表示之化合物氣體排氣之排氣步驟,及使該前驅物薄膜與反應性氣體化學反應,於該基體表面形成含有選自鈦、鋯及鉿中至少1種之金屬之薄膜之含金屬的薄膜形成步驟。
以下,針對上述各步驟,以形成將含金屬的薄膜藉由ALD法之情況為例詳細說明。藉由ALD法形成含金屬的薄膜時,首先進行前述說明之原料導入步驟。使薄膜形成用原料成為蒸氣時之較佳溫度或壓力與上述說明者相同。接者,藉由導入成膜腔室部之以上述通式(1)表示之化合物,於基體表面成膜前驅物薄膜(前驅物薄膜成膜步驟)。此時,亦可加熱基體、或加熱成膜腔室部而施加熱。
以該步驟成膜之前驅物薄膜為以上述通式(1)表示之化合物吸著於基體表面者或該化合物或是該化合物之一部分分解及/或反應而生成之薄膜,具有與目的之含金屬的薄膜不同之組成。進行本步驟時之基體溫度以室溫~600℃為佳,150~400℃為更佳。進行本步驟時之系(成膜腔室內)之壓力1~10000Pa為佳,10~1000Pa為更佳。
接者,自成膜腔室部排出未反應之以上述通式(1)表示之化合物氣體或副生之氣體(排氣步驟)。未反應之以上述通式(1)表示之化合物氣體或副生之氣體理想上係自成膜腔室部完全排氣,但並無必要必定完全排氣。排氣方法有藉由氮氣、氦氣、氬氣等之惰性氣體吹拂系內之方法,藉由使系內減壓而排氣之方法,組合該等之方法等。減壓時之減壓度0.01~300Pa為佳,0.01~100Pa為更佳。
接者,於成膜腔室部導入反應性氣體,藉由該反應性氣體或反應性氣體及熱之作用,自以先前之前驅 物薄膜成膜步驟所得之前驅物薄膜形成含有金屬之薄膜(含有金屬之薄膜形成步驟)。本步驟中,使熱作用時之溫度的室溫~600℃為佳,150~400℃為更佳。進行本步驟時之系(成膜腔室內)之壓力1~10000Pa為佳,10~1000Pa為更佳。
本發明的薄膜之製造方法,採用如上述之ALD法時,將由上述之原料導入步驟、前驅物薄膜成膜步驟、排氣步驟及含有金屬之薄膜形成步驟所成之一連串操作之薄膜堆積設為1循環,可重複複數次該循環直至獲得必要膜厚之薄膜。該情況下,進行1循環後,與上述排氣步驟同樣地,自成膜腔室部排出未反應之以上述通式(1)表示之化合物氣體及反應性氣體進一部排出副生之氣體後,進行下一循環為佳。
又,本發明之薄膜之製造方法中,採用上述之ALD法之情況,亦可施加電漿、光、電壓等之能量,亦可使用觸媒。施加該等之能量之時期並未特別限定,宜為例如於原料導入步驟中之化合物氣體導入時,前驅物薄膜成膜步驟或含有金屬之薄膜形成步驟中之加溫時,排氣步驟之系內排氣時,含有金屬之薄膜形成步驟中之反應性氣體導入時,亦可為上述各步驟之間。又,於反應性氣體導入前,亦可對於反應性氣體施加該等之能量。
又,在本發明的薄膜之製造方法中,採用如上述之電漿ALD法時,反應性氣體可於製造方法中全部步驟之間對成膜腔室內持續流入,並僅於含有金屬之薄膜形 成步驟時,將對於反應性氣體進行電漿處理者導入成膜腔室即可。高頻(以下,有時亦稱為RF)輸出係過低,則不易成為含有良好的金屬之膜,過高則對基板之破損為大,故0~1500W為佳,50~600W為更佳。在本發明之製造方法中,採用電漿ALD法時,可含有非常高品質的金屬之薄膜,故為佳。
又,本發明之薄膜之製造方法中,薄膜堆積後,為了獲得更良好之電特性,亦可在惰性環境下進行退火處理,於必須埋入階差時,亦可設回焊步驟。該情況之溫度為200~1000℃,250~500℃為佳。
使用本發明之薄膜形成用原料製造含有金屬的薄膜之裝置可使用周知的化學氣相成長法用裝置。作為具體的裝置之一例舉例為例如圖1所示之可藉冒泡供給前驅物而進行之裝置,或如圖2所示之具有氣化室之裝置。且,舉例為如圖3及圖4之可對反應性氣體進行電漿處理之裝置。不限於如圖1、圖2、圖3及圖4之單片式裝置,亦可使用利用批式爐可同時處理多數片之裝置。
使用本發明之薄膜形成用原料而製造的含有金屬之薄膜可使用於切削工具、電子材料用之配線或電極,例如可使用於半導體記憶體材料或鋰空氣電池用之電極等。
以下列舉實施例及評估例更詳細說明本發 明。然而,本發明不受以下實施例等之任何限制。
藉由將上述化合物No.1放置於大氣中,來確認自燃性之有無。將結果表示於表1。
依據表1之結果,化合物No.1係無法顯示自燃性,可了解即使於大氣中可安全地使用作為化學氣相成長用原料。
將化合物No.1作為化學氣相成長用原料,使用圖3所示之裝置,藉由以下之條件的ALD法,於矽晶圓上製造氧化鈦薄膜。對於所得到之薄膜,利用X射線反射率法測定膜厚、利用X射線繞射法及X射線光電子光譜法(X-ray Photoelectron Spectroscopy)進行薄膜構造及薄膜組成之確認時,膜厚係4.0nm,膜組成係氧化鈦,含碳量之檢測下限少於0.1atom%。每1循環所得之膜厚為0.08nm。
反應溫度(基體溫度):200℃,反應性氣體:臭氧
將由下述(1)~(4)所成之一連串步驟設為1循環,重複50次循環:(1)於原料容器溫度:70℃、原料容器壓力:0.6Torr(80Pa)之條件下,將氣化之化學氣相成長用原料之蒸氣導入於成膜腔室內,於系壓力0.5Torr(67Pa)下,於矽晶圓表面堆積10秒;(2)藉由15秒之氬吹拂,去除未反應原料;(3)導入反應性氣體,以系壓力0.5Torr(67Pa)反應10秒; (4)藉由15秒之氬吹拂,去除未反應原料。
除了使用作為化學氣相成長法用原料(五甲基環戊二烯基)(三甲基)鈦以外,於與實施例1相同條件下進行氧化鈦薄膜之製造。
對於所得到之薄膜,利用X射線反射率法測定膜厚、利用X射線繞射法及X射線光電子光譜法進行薄膜構造及薄膜組成之確認時,膜厚係3.0nm,膜組成係氧化鈦,含碳量為10atom%。每1循環所得之膜厚為0.06nm。
以實施例1所得之薄膜係作為有機物之殘留碳成分的含量非常少,為高品質之氧化鈦薄膜。另一方面, 以比較例1所得之薄膜係作為有機物之殘留碳成分之含量為多,為低品質之氧化鈦薄膜。且,可了解實施例1係每一循環獲得之膜厚較比較例1為多。
尚,本國際申請係基於2016年7月5日申請之日本國專利申請第2016-133140號主張優先權,且將該日本國際申請之全內容納入本國際申請。
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