TW202225172A - 原子層沉積法用薄膜形成原料及薄膜之製造方法 - Google Patents
原子層沉積法用薄膜形成原料及薄膜之製造方法 Download PDFInfo
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- TW202225172A TW202225172A TW110134195A TW110134195A TW202225172A TW 202225172 A TW202225172 A TW 202225172A TW 110134195 A TW110134195 A TW 110134195A TW 110134195 A TW110134195 A TW 110134195A TW 202225172 A TW202225172 A TW 202225172A
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- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 1
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- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 125000003548 sec-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
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- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- 238000000427 thin-film deposition Methods 0.000 description 1
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- 239000010936 titanium Substances 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
- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Abstract
Description
本發明有關含有具有特定構造之釔化合物之原子層沉積法用薄膜形成原料及使用其之薄膜的製造方法。
釔係使用作為用以構成化合物半導體之成分。作為用以製造含釔原子之薄膜的薄膜形成原料,已報導有各種原料。
作為薄膜之製造方法,舉例為例如濺鍍法、離子鍍敷法、塗佈熱分解法或溶凝膠法等之金屬有機化合物分解(MOD:Metal Organic Decomposition)法、化學氣相沉積(CVD:Chemical Vapor Deposition)法、原子層沉積(ALD:Atomic Layer Deposition)法等。該等中ALD法由於組成控制性及階差被覆性優異,適於量產化,可混合集成等之多種優點,故而為薄膜之最適宜製造製程。
於如CVD法及ALD法之氣相薄膜形成法中可使用之材料雖已有多種報告。可適用於ALD法之薄膜形成原料,必須具有稱為ALD範圍(ALD window)之溫度區域,該溫度區域必須充分廣。因此,即使於CVD法中可使用之薄膜形成原料大多情況亦無法適用於ALD法為本技術領域中之技術常識。
非專利文獻1中揭示以三(2,2,7-三甲基-3,5-辛二酸)釔為主成分之CVD法用原料。且專利文獻1中,作為ALD法可使用之釔化合物,揭示有三(2,2,6,6-四甲基-3,5-庚二酸)釔。
[先前技術文獻]
[專利文獻]
專利文獻1:日本特開2001-355070號公報
[非專利文獻]
非專利文獻1:Materials Research Society Symposium Proceedings, Volume:363, Pages:195-206, 1995
[發明欲解決之課題]
然而,非專利文獻1並無有關ALD法之記載,關於三(2,2,7-三甲基-3,5-辛二酸)釔是否適用於ALD法無任何記載。且,ALD法用薄膜形成原料被要求可生產性良好地製造熔點低、熱穩定性優異、殘留碳量少的高品質薄膜。然而,專利文獻1中記載之三(2,2,6,6-四甲基-3,5-庚二酸)釔並非可滿足該等要求者。且專利文獻1完全未記載三(2,2,6,6-四甲基-3,5-庚二酸)釔化合物以外的釔化合物適用於ALD法之具體例。
因此,本發明之目的係提供可生產性良好地製造熔點低、熱穩定性優異、殘留碳量少的高品質薄膜之原子層沉積法用薄膜形成原料及使用其之薄膜之製造方法。
[用以解決課題之手段]
本發明人等重複積極檢討之結果,發現含有具有特定構造之釔化合物之原子層沉積法用薄膜形成原料可解決上述課題,因而完成本發明。
亦即本發明係提供一種原子層沉積法用薄膜形成原料,其含有以下述通式(1)表示之釔化合物,
(式中,R
1表示碳原子數3~8之二級烷基,R
2表示碳原子數4~8之三級烷基,R
3表示氫原子或碳原子數1~5之一級、二級或三級烷基)。
且本發明提供一種藉由原子層沉積法,於基體之表面製造含有釔原子的薄膜之方法,且包含使上述原子層沉積法用薄膜形成原料氣化使所得之原料氣體中之前述釔化合物吸附於前述基體之表面而形成前驅體薄膜之步驟,及使前驅體薄膜與反應性氣體反應而於基體之表面形成含有釔原子的薄膜之步驟。
[發明效果]
依據本發明,可提供可生產性良好地製造熔點低、熱穩定性優異、殘留碳量少的高品質薄膜之原子層沉積法用薄膜形成原料。且依據本發明,可提供可生產性良好地以原子層沉積法所製造的殘留碳量少的高品質薄膜之方法。
本發明之原子層沉積法用薄膜形成原料係含有以上述通式(1)表示之釔化合物者。
上述通式(1)中,R
1表示碳原子數3~8之二級烷基,R
2表示碳原子數4~8之三級烷基,R
3表示氫原子或碳原子數1~5之一級、二級或三級烷基。
作為碳原子數3~8之二級烷基,舉例為例如異丙基、第二丁基、1-乙基丙基、1,2-二甲基丙基、第二戊基、己-3-基、己-2-基、庚-3-基、庚-2-基、辛-4-基、辛-3-基、辛-2-基等。
作為碳原子數4~8之三級烷基,舉例為例如第三丁基、第三戊基、2-甲基戊-2-基、3-甲基戊-3-基、2-甲基己-2-基、2-甲基庚-2-基等。
作為碳原子數1~5之一級、二級或三級烷基,舉例為例如甲基、乙基、丙基、異丙基、丁基、異丁基、第二丁基、第三丁基、戊基、1-乙基丙基、1,2-二甲基丙基、第二戊基、第三戊基等。
上述通式(1)中,R
1為碳原子數5~8之二級烷基者,由於可生產性良好地形成熔點低、熱穩定性高、含釔之薄膜的效果特別高而較佳。其中,R
1為碳原子數7之二級烷基者,該等效果特別高故而特佳。
上述通式(1)中,R
2為碳原子數4~5之三級烷基者,因熱穩定性高故而較佳。其中,R
2為第三丁基者,因熱穩定性特別高故而特佳。
上述通式(1)中,R
3為氫原子或碳原子數1~3之烷基者,由於可生產性良好地形成含釔之薄膜的效果高故而較佳。其中,R
3為氫原子者,可生產性良好地形成含釔之薄膜的效果特別高故而特佳。
上述通式(1)中,R
1及R
2之碳原子數的和為10~13者,由於可生產性良好地形成熔點低、熱穩定性高、含釔之薄膜的效果高故而較佳。
作為以上述通式(1)表示之釔化合物之具體例,舉例為下述No.1~No.20之釔化合物。又,下述No.1~No.20中,「Me」表示甲基,「iPr」表示異丙基,「sBu」表示第二丁基,「tBu」表示第三丁基,「tAm」表示第三戊基(以下述式(2)表示之基),「Hep」表示庚-3-基(以下述式(3)表示之基),「Hex」表示己-3-基(以下述式(4)表示之基),「Oct」表示辛-4-基(以下述式(5)表示之基)。
(式中,✽表示鍵結鍵)。
(式中,✽表示鍵結鍵)。
(式中,✽表示鍵結鍵)。
(式中,✽表示鍵結鍵)。
以上述通式(1)表示之釔化合物其製造方法未特別限制,可藉由眾所周知之合成方法製造。例如,可於甲醇溶劑下使硝酸釔六水合物及對應構造的二酮化合物與氫氧化鈉反應而製造。具體而言,於甲醇溶劑下使硝酸釔六水合物與2,2-二甲基-6-乙基-3,5-癸二酮及氫氧化鈉反應,可製造化合物No.3。
本發明之原子層沉積法用薄膜形成原料只要含有以上述通式(1)表示之釔合物者即可,其組成隨目的薄膜之種類而異。例如製造僅含釔作為金屬的薄膜時,本發明之原子層沉積法用薄膜形成原料不含有上述通式(1)表示之釔化合物以外的金屬化合物及半金屬化合物。另一方面,製造包含釔與釔以外之金屬及/或半金屬之薄膜時,本發明之原子層沉積法用薄膜形成原料,除了含以上述通式(1)表示之釔化合物以外,還可包含有含有釔以外之金屬之化合物及/或含有半金屬之化合物(以下亦稱為其他前驅物)。本發明之原子層沉積法用薄膜形成原料,如後述,可進而含有有機溶劑及/或親核性試劑。
本發明之原子層沉積法用薄膜形成原料之形態是根據原子層沉積法之輸送供給方法等之手法適當選擇。
作為上述輸送供給方法,有如下方法:藉由於儲存本發明之原子層沉積法用薄膜形成原料之容器(以下有時亦記為「原料容器」)中加熱及/或減壓進行氣化而作成原料氣體,與根據需要使用之氬、氮、氦等之載氣一起將該原料氣體導入至設置有基體之成膜腔室內(以下有時亦記為「沉積反應部」)之氣體輸送法;將本發明之原子層沉積法用薄膜形成原料以液體或溶液狀態輸送至氣化室,藉由於氣化室加熱及/或減壓而氣化作成原料氣體,將該原料氣體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)表示之釔化合物本身可作為原子層沉積法用薄膜形成原料。液體輸送法時,以上述通式(1)表示之釔化合物本身或將該釔化合物溶解於有機溶劑之溶液可作為原子層沉積法用薄膜形成原料。該等原子層沉積法用薄膜形成原料亦可進而含有其他前驅物、親核性試劑等。
且,多成分系ALD法中,有將原子層沉積法用薄膜形成原料以各成分獨立氣化、供給之方法(以下亦記載為「單源法」),使多成分原料預先以期望組成混合之混合原料氣化、供給之方法(以下亦記載為「混合源法」)。混合源法之情況,可將以上述通式(1)表示之釔化合物與其他前驅物之混合物或將該混合物溶解於有機溶劑之混合溶液作為原子層沉積法用薄膜形成原料。該混合物或混合溶液可進而包含親核性試劑等。
作為上述有機溶劑,可謂受特別限制地使用眾所周知之一般有機溶劑。作為該有機溶劑舉例為例如乙酸乙酯、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、二甲基吡啶等。該等有機溶劑可根據溶質之溶解性、使用溫度與沸點、燃火點之關係等,而單獨使用,或混合兩種以上使用。
且,於多成分系ALD法時,作為與上述通式(1)表示之釔合物一起使用之其他前驅物,未特別限制,可使用原子層沉積法用薄膜形成原料所用之習知前驅物。
作為上述其他前驅物,舉例為例如選自醇化合物、二醇化合物、β-二酮化合物、環戊二烯化合物、有機胺化合物等之作為有機配位子使用之化合物所成之群中之一種或兩種以上與矽或金屬之化合物。又,作為前驅物之金屬種,舉例為鋰、鈉、鉀、鈣、鍶、鋇、鈦、鋯、鉿、釩、鈮、鉭、鉻、鉬、鎢、錳、鐵、釕、鈷、銠、銥、鎳、鈀、鉑、銅、銀、金、鋅、鋁、鎵、銦、鍺、錫、鉛、銻、鉍、鈧、釕、釔、鑭、鈰、鐠、釹、鉕、釤、銪、釓、鋱、鏑、鈥、鉺、銩、鐿或鎦。
作為上述其他前驅物之有機配位子使用之醇化合物舉例為例如甲醇、乙醇、丙醇、異丙醇、丁醇、第二丁醇、異丁醇、第三丁醇、戊醇、異戊醇、第三戊醇等之烷醇類;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-第二丁氧基-1,1-二乙基乙醇、3-甲氧基-1,1-二甲基丙醇等之醚醇類;二甲胺基乙醇、乙基甲基胺基乙醇、二乙胺基乙醇、二甲胺基-2-戊醇、乙基甲基胺基-2-戊醇、二甲胺基-2-甲基-2-戊醇、甲基乙基胺基-2-甲基-2-戊醇、二乙胺基-2-甲基-2-戊醇等之二烷胺基醇類等。
作為上述其他前驅物之有機配位子使用之二醇化合物舉例為例如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。
作為上述其他前驅物之有機配位子使用之β-二酮化合物舉例為例如乙醯丙酮、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之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。
作為上述其他前驅物之有機配位子使用之環戊二烯化合物舉例為例如環戊二烯、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、第二丁基環戊二烯、異丁基環戊二烯、第三丁基環戊二烯、二甲基環戊二烯、四甲基環戊二烯等。
作為上述其他前驅物之有機配位子使用之有機胺化合物舉例為甲胺、乙胺、丙胺、異丙胺、丁胺、第二丁胺、第三丁胺、異丁胺、二甲胺、二乙胺、二丙胺、二異丙胺、乙基甲基胺、丙基甲基胺、異丙基甲基胺等。
上述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,於例如使用醇化合物作為有機配位子時,藉由使前述之金屬之無機鹽或其水合物與其醇化合物之鹼金屬烷醇鹽反應,可製造前驅物。此處,作為金屬之無機鹽或其水合物可舉例例如金屬之鹵化物、硝酸鹽等,作為鹼金屬烷醇鹽可舉例例如烷醇鈉、烷醇鋰、烷醇鉀等。
單源法時,作為上述其他前驅物,較佳為熱及/或氧化分解行為與上述通式(1)表示之釔化合物類似的化合物。混合源法時,作為上述其他前驅物,除了熱及/或氧化分解行為與上述通式(1)表示之釔化合物類似以外,較佳係混合時不因化學反應等引起變質之化合物。
又,本發明之原子層沉積法用薄膜形成原料根據需要,為了提高上述通式(1)表示之釔化合物及其他前驅物之安定性,亦可含有親核性試劑。作為親核性試劑,舉例為例如乙二醇二甲醚(glyme)、二乙二醇二甲醚、三乙二醇二甲醚、四乙二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、二伸乙基三胺、三伸乙基四胺、四伸乙基五胺、五伸乙基六胺、1,1,4,7,7-五甲基二伸乙基三胺、1,1,4,7,10,10-六甲基三伸乙基四胺、三乙氧基三伸乙基胺等之多胺類,四氮雜環十四烷(Cyclam)、四氮雜環十二烷(cyclen)等之環狀多胺類,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、氧硫雜環戊烷等之雜環化合物類,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-酮酯類或乙醯基丙酮,2,4-己烷二酮、2,4-庚烷二酮、3,5-庚烷二酮、二特戊醯基甲烷等之β-二酮類。該等親核性試藥之使用量,相對於前驅物全體之量1莫耳,較佳為0.1莫耳~10莫耳之範圍,更佳為1莫耳~4莫耳之範圍。
本發明之原子層沉積法用薄膜形成原料期望極力不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。雜質金屬元素分較佳每元素100ppb以下,更佳為10ppb以下,總量計,較佳為1ppm以下,更佳為100ppb以下。尤其,使用作為LSI之閘極絕緣膜、閘極膜、障壁膜時,必須減少對所得薄膜之電特性有影響之鹼金屬元素及鹼土類金屬元素之含量。雜質鹵素分較佳為100ppm以下,更佳為10ppm以下,最佳為1ppm以下。雜質有機分總量計較佳為500ppm以下,更佳為50ppm以下,最佳為10ppm以下。又,由於水分係原子層沉積法用薄膜形成原料中之顆粒發生及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較佳為10ppm以下,更佳為1ppm以下。
本發明之原子層沉積法用薄膜形成原料,為了減低或防止所形成之薄膜之顆粒污染,較佳極力不含顆粒。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中較佳為100個以下,更佳大於0.2μm之粒子數於液相1mL中為1000個以下,最佳大於0.2μm之粒子數於液相1mL中為100個以下。
本發明之薄膜之製造方法係藉由原子層沉積法,於基體之表面製造含有釔原子的薄膜之方法,且包含使上述原子層沉積法用薄膜形成原料氣化使所得之原料氣體中之釔化合物吸附(沉積)於基體之表面而形成前驅體薄膜之步驟,及使前驅體薄膜與反應性氣體反應而於基體之表面形成含有釔原子的薄膜之步驟。
作為上述基體之材質舉例為例如矽;氮化矽、氮化鈦、氮化鉭、氧化鈦、氧化釕、氧化鋯、氧化鉿、氧化鑭等之陶瓷;玻璃;金屬鈷、金屬鐵、金屬錳、金屬鎳、金屬銅等之金屬;不鏽鋼、黃銅、白銅、青銅、杜拉鋁(duralumin)、鎳鉻合金、鈷鉻合金(Stellite)、焊料、汞合金(amalgam)、碳鋼等之合金。作為基材之形狀舉例為板狀、球狀、纖維狀、鱗片狀。基體表面可為平面,亦可為溝槽構造等之三次元構造。
且,作為將上述原子層沉積法用薄膜形成原料氣化並將所得之原料氣體導入設置基體之成膜腔室內之方法,舉例為上述氣體輸送法、液體輸送法、單源法、混合源法等。
作為上述反應性氣體舉例為例如氧、臭氧、二氧化氮、一氧化氮、水蒸氣、過氧化氫、甲酸、乙酸、乙酸酐等之氧化性氣體、氫等之還原性氣體、單烷胺、二烷胺、三烷胺、伸烷二胺等之有機胺化合物、聯胺、氨等之氮化性氣體等。該等反應性氣體可單獨使用,或可混合兩種以上使用。該等中,本發明之原子層沉積法用薄膜形成原料具有於特異低的溫度與氧化性氣體反應之性質,尤其與臭氧及水蒸氣可於低的溫度反應。就每1循環所得之膜厚較厚,可生產性良好地製造薄膜之方面,作為反應性氣體,較佳使用含有臭氧、氧或水蒸氣之氧化性氣體,更佳使用含有臭氧之氧化性氣體。
作為上述製造條件,進而舉例為使原子層沉積法用薄膜形成原料氣化作成原料氣體時之溫度及壓力。使原子層沉積法用薄膜形成原料氣化作為原料氣體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,本發明之原子層沉積法用薄膜形成原料均較佳於0℃~300℃下氣化。且,於原料容器內或氣化室內使原子層沉積法用薄膜形成原料氣化作成原料氣體時,原料容器內之壓力及氣化室內之壓力均較佳為1Pa~10,000Pa。
又,作為本發明之薄膜之製造方法中的製造條件未特別限制,例如反應溫度(基體溫度)、反應壓力、沉積速度等可根據所需薄膜厚度及種類適當決定。關於反應溫度,較佳為使本發明之原子層沉積法用薄膜形成原料充分反應之溫度的100℃以上,更佳為150℃~400℃,於與反應性氣體匹配之ALD範圍內使用。膜厚係以獲得期望膜厚之方式以循環次數加以控制。
以下針對上述ALD法之各步驟,以形成氧化釔薄膜之情況為例詳細說明。首先,將原子層沉積法用薄膜形成原料氣化將所得之原料氣體導入成膜腔室(原料導入步驟)。使原子層沉積法用薄膜形成原料氣化時之較佳溫度及壓力於0℃~300℃及1Pa~10,000Pa之範圍內。其次,藉由使將導入至成膜腔室之原料氣體吸附(沉積)於基體表面,而於基體表面形成前驅物薄膜(前驅物薄膜形成步驟)。此時,可加熱基體或加熱成膜腔室,亦可施加熱。執行本步驟時之基體溫度較佳為室溫~500℃,更佳為150℃~400℃。組合使用本發明之原子層沉積法用薄膜形成原料與氧化性氣體時之ALD範圍大約為200℃~400℃之範圍。執行本步驟時之系統(成膜腔室內)之壓力較佳為1Pa~ 10,000Pa,更佳為10Pa~1,000Pa。
其次,自成膜腔室排出未反應之原料氣體或副生之氣體(排氣步驟)。未反應之原料氣體或副生之氣體理想上自成膜腔室完全排氣,但未必需要完全排氣。作為排氣方法,舉例為藉由氮、氦、氬等惰性氣體吹拂系統內之方法、藉由使系內減壓而排氣之方法、組合該等之方法。減壓時之減壓度較佳為0.01Pa~300Pa,更佳為0.01Pa~ 100Pa。
其次,將作為反應性氣體之氧化性氣體導入成膜腔室,藉由該氧化性氣體之作用或該氧化性氣體及熱之作用,自前驅物薄膜形成步驟中形成之前驅物薄膜形成氧化釔薄膜(氧化釔薄膜形成步驟)。此步驟中使熱作用時之溫度較佳為室溫~500℃,更佳為150℃~400℃。由於組合使用本發明之原子層沉積法用薄膜形成原料與氧化性氣體時之ALD範圍大概在200℃~400℃之範圍,故最佳於200℃~400℃範圍使前驅物薄膜與氧化性氣體反應。執行本步驟時之系統(成膜腔室內)之壓力較佳為1Pa~10,000Pa,更佳為10Pa~1,000Pa。本發明之原子層沉積法用薄膜形成原料與氧化性氣體之反應性良好,可以生產性良好地製造殘留碳含量少的高品質氧化釔薄膜。
本發明之薄膜製造方法中,將由上述原料導入步驟、前驅物薄膜形成步驟、排氣步驟及氧化釔薄膜形成步驟所成之一連串操作所至之薄膜沉積設為1循環,重複複數次該循環,直到獲得所需膜厚之薄膜。該情況下,較佳於進行1循環後,與上述排氣步驟同樣,自成膜腔室排出未反應之反應性氣體(形成氧化釔薄膜時為氧化性氣體)及副生之氣體後,進行下1循環。
又,本發明之薄膜之製造方法亦可施加電漿、光、電壓等之能量,亦可使用觸媒。施加該能量之時期及使用觸媒之時期並未特別限定,例如於原料導入步驟中原料氣體之導入時、前驅物薄膜形成步驟或氧化釔薄膜形成步驟之加熱時、排氣步驟之系內排氣時、氧化釔薄膜形成步驟之氧化性氣體導入時,亦可為上述各步驟之間。
又,本發明之薄膜之製造方法中,於薄膜形成後,為了獲得更良好的電氣特性,亦可於惰性環境下、氧化性環境下或還原性環境下進行退火處理,於需要階差嵌埋時,亦可設回焊步驟。該情況之溫度為200℃~1,500℃,較佳為500℃~1,000℃。
使用本發明之原子層沉積法用薄膜形成原料製造薄膜之裝置,可使用周知之原子層沉積法用裝置。作為具體裝置之例舉例為如圖1般之可通氣供給前驅物之裝置或圖2般之具有氣化室之裝置。又,舉例為如圖3及圖4般可對反應性氣體進行電漿處理之裝置。不限於如圖1~圖4般之單片式裝置,亦可使用利用批式爐之可多數片同時處理之裝置。
使用本發明之原子層沉積法用薄膜形成原料製造之薄膜,藉由適當選擇其他前驅物、反應性氣體及製造條件,可成為金屬、氧化物陶瓷、氮化物陶瓷、玻璃等之期望種類之薄膜。該薄膜已知顯示電性特性及光學特性等,而應用於各種用途。例如該等薄膜可廣泛使用於例如以DRAM元件為代表之記憶體元件之電極材料、電阻膜、硬碟之記錄層所用之反磁性膜及固體高分子形燃料電池用之觸媒材料等之製造。
[實施例]
以下,使用實施例、評價例及比較例更詳細說明本發明。然而,本發明不受以下實施例之任何限制。
[實施例1] 化合物No.3之合成
於1L之4頸燒瓶中饋入硝酸釔六水合物50g(0.131mol)與甲醇200mL,於室溫下攪拌。於其中,於室溫下滴加由2,2-二甲基-6-乙基-3,5-癸烷二酮89.6g(0.392mol)、氫氧化鈉15.67g(0.392mol)、甲醇300mL所調製之溶液。於室溫攪拌19小時後,自所得懸浮液去除溶劑,添加500mL脫水甲苯,於125℃使用迪恩斯塔克裝置進行脫水。自所得溶液去除溶劑,添加500mL脫水己烷,於60℃加熱攪拌1小時後過濾。自所得濾液去除溶劑,以浴溫210℃、壓力44Pa蒸餾生成之釔錯合物,獲得黃色透明黏性液體之化合物No.3(產量82.03g,產率82.1%)。
(分析值)
(1)常壓TG-DTA
質量減少50%溫度:305℃(760Torr,Ar流量:100mL/分鐘,升溫速度:10℃/分鐘,樣品量:9.860mg)
(2)減壓TG-DTA
質量減少50%溫度:215℃(10Torr,Ar流量:50 mL/分鐘,升溫速度:10℃/分鐘,樣品量:9.716mg)
(3)
1H-NMR(氘化苯)
0.91~0.97ppm(6H,多峰), 1.18ppm(9H,單峰), 1.26~1.48 ppm(6H,多峰), 1.71~1.78ppm(2H,多峰), 2.07-2.14ppm(1H,多峰), 5.76ppm(1H,單峰)
(4)元素分析(金屬分析:ICP-AES)
釔含量:11.6質量%(理論值:11.6質量%)
[評價例]
針對實施例1所得之化合物No.3及下述比較化合物1,進行以下評價。又,下述比較化合物1中,「tBu」表示第三丁基。
(1) 熔點評價
目視觀測20℃下之化合物狀態。針對於20℃下為固體者,使用微小熔點測定裝置測定熔點。結果示於表1。
(2)熱穩定性評價
使用DSC測定裝置測定熱分解起始溫度。熱分解起始溫度高者,不易發生熱分解,可判斷為可較佳作為原子層沉積法用薄膜形成原料。結果示於表1。
由表1之結果,可知化合物No.3係熔點比比較化合物1低150℃以上之化合物。且可知化合物No.3具有比比較化合物1高的熱穩定性。化合物No.3與具有類似構造之比較化合物1相比,可知極為適合作為原子層沉積法用薄膜形成原料。
[實施例2] 氧化釔薄膜之製造
將化合物No.3作為原子層沉積法用薄膜形成原料,使用圖1所示之裝置,藉以下條件之ALD法,於矽晶圓上製造氧化釔薄膜。藉由X射線光電子分光法確認所得薄膜之組成後,所得薄膜為氧化釔,殘留碳量少於1.0atom%。且藉由X射線反射率法進行膜厚測定,算出其平均值,平均膜厚為15.0nm,每1循環所得之平均膜厚為0.05nm。
(條件)
基板:矽晶圓,反應溫度(矽晶圓溫度):300℃,反應性氣體:臭氧
由下述(1)~(4)所成之一連串步驟設為1循環,重複300次循環。
(1)原料容器溫度:200℃,原料容器內壓力:於100Pa條件下將氣化之原料氣體導入成膜腔室,系統壓力:於100Pa下沉積10秒。
(2)藉由15秒之氬吹拂,去除未沉積之原料氣體。
(3)將反應性氣體導入成膜腔室,系統壓力:於100Pa反應10秒。
(4)藉由15秒之氬吹拂,去除未反應之反應性氣體及副生氣體。
[比較例1]氧化釔薄膜之製造
除了使用比較化合物1作為原子層沉積法用薄膜形成原料以外,在與實施例2相同之條件製造氧化釔薄膜。藉由X射線光電子分光法確認所得薄膜組成後,所得薄膜為氧化釔,殘留碳量為3.0atom%。且,藉由X射線反射率法測定膜厚,算出其平均值後,平均膜厚為9.0nm,每1循環所得之平均膜厚為0.03nm。
由實施例2及比較例1之結果可知,實施例2中每1循環所得之膜厚為比較例1之1.6倍以上,且可生產性良好地獲得殘留碳量較少之高品質氧化釔薄膜。
由以上,可說根據本發明可生產性良好地製造高品質之氧化釔薄膜。
[圖1]係顯示本發明之薄膜之製造方法所用之原子層沉積法用裝置之一例的概略圖。
[圖2]係顯示本發明之薄膜之製造方法所用之原子層沉積法用裝置之另一例的概略圖。
[圖3]係顯示本發明之薄膜之製造方法所用之原子層沉積法用裝置之又另一例的概略圖。
[圖4]係顯示本發明之薄膜之製造方法所用之原子層沉積法用裝置之又一例的概略圖。
Claims (6)
- 如請求項1之原子層沉積法用薄膜形成原料,其中R 1及R 2之碳原子數的和為10~13。
- 一種薄膜之製造方法,其係藉由原子層沉積法,於基體之表面製造含有釔原子的薄膜之方法,且包含 使如請求項1或2之原子層沉積法用薄膜形成原料氣化使所得之原料氣體中之前述釔化合物吸附於前述基體之表面而形成前驅體薄膜之步驟,及 使前述前驅體薄膜與反應性氣體反應而於前述基體之表面形成含有釔原子的薄膜之步驟。
- 如請求項3之薄膜之製造方法,其中前述反應性氣體為氧化性氣體。
- 如請求項4之薄膜之製造方法,其中前述氧化性氣體係含有臭氧、氧或水蒸氣之氣體。
- 如請求項3至5中任一項之薄膜之製造方法,其中於200℃~400℃之溫度範圍使前述前驅體薄膜與前述反應性氣體反應。
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