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TWI620751B - 用於ａｌｄ／ｃｖｄ含矽薄膜應用之有機矽烷前驅物 - Google Patents

用於ａｌｄ／ｃｖｄ含矽薄膜應用之有機矽烷前驅物 Download PDF

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TWI620751B
TWI620751B TW102126078A TW102126078A TWI620751B TW I620751 B TWI620751 B TW I620751B TW 102126078 A TW102126078 A TW 102126078A TW 102126078 A TW102126078 A TW 102126078A TW I620751 B TWI620751 B TW I620751B
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precursor
containing film
sih
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克里斯均 杜薩拉特
葛藍 庫亨拜瑟爾
凡卡特斯瓦拉Ｒ 帕雷姆
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液態空氣喬治斯克勞帝方法研究開發股份有限公司
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Abstract

本發明揭示形成含Si薄膜之前驅物、其合成方法及使用其以使用氣相沉積製程沉積含矽薄膜用於製造半導體、光伏打裝置、LCD-TFT、平板型裝置、耐火材料或航空材料之方法。

Description

用於ALD/CVD含矽薄膜應用之有機矽烷前驅物 【相關申請案的交互參照】
本申請案主張2012年7月20日申請之美國臨時申請案第61/674,103號之優先權，該申請案之全部內容以引用之方式併入本文中。
揭示形成含Si薄膜之前驅物、其合成方法及使用其以使用氣相沉積製程沉積含矽薄膜製造半導體、光伏打裝置、LCD-TFT、平板型裝置、耐火材料或航空材料之方法。
含Si薄膜廣泛用於半導體、光伏打裝置、LCD-TFT、平板型裝置、耐火材料或航空行業中。含Si薄膜可例如用作具有電學性質之可絕緣的介電材料(SiO2、SiN、SiCN、SiCOH、MSiOx，其中M為Hf、Zr、Ti、Nb、Ta或Ge且x大於零)，含Si薄膜可用作導電薄膜，諸如金屬矽化物或金屬矽氮化物。由於電學裝置架構朝向奈米級(尤其低於28nm節點)降低尺寸所施加的嚴格要求，需要愈來愈精細調節之分子前驅物，該等分子前驅物除具有高沉積速率、所產生薄膜之保形性及堅實度以外亦滿足揮發性(對於ALD製程)、較低製程溫度、與各種氧化劑之反應性及低薄膜污染之要求。
熟知矽烷(SiH4)可用於熱CVD。然而，此分子具自燃性，由此使得此室溫氣體在安全處理方面面臨挑戰。已使用採用鹵代矽烷(諸 如二氯矽烷SiH2Cl2)之CVD方法。然而，此等方法可能需要較長吹掃時間，造成薄膜之鹵素污染及粒子形成(由氯化銨鹽形成)，且甚至破壞某些基質，從而引起不希望的界面層形成。以烷基部分地替代鹵素可得到一些改良，但代價是薄膜內產生不利的碳污染。
有機胺基矽烷已用作含Si薄膜之CVD的前驅物。Dussarrat等人之US 7192626報導了使用三矽烷胺N(SiH3)3來沉積SiN薄膜。其他已報導之前驅物包括二異丙胺基矽烷[SiH3(NiPr2)]及類似SiH3(NR2)化合物(參見例如Thridandam等人之US 7875312)以及苯基甲基胺基矽烷[SiH3(NPhMe)]及相關經取代之矽烷苯胺(參見例如Xiao等人之EP 2392691)。
另一相關類別之用於含Si薄膜之CVD的Si前驅物由通式(R1R2N)xSiH4-x給出，其中x在1與4之間且R取代基獨立地為H、C1-C6直鏈、分支鏈或環狀碳鏈(參見例如Dussarrat等人之WO2006/097525)。
Hunks等人在US2010/0164057中揭示諸多含Si前驅物，包括具有式R4-xSiLx之矽化合物，其中x為具有1至3之值的整數；R可選自H、分支鏈及未分支鏈C1-C6烷基、C3-C8環烷基及C6-C13芳基；且L可選自異氰酸酯基、甲基乙基酮肟、三氟乙酸酯、三氟甲磺酸酯、醯氧基、β-二酮亞胺(β-diketiminate)、β-二-亞胺(β-di-iminate)、脒、胍、烷胺基、氫化物、烷氧化物或甲酸酯配位體。Pinnavaia等人主張了一種由乙醯基丙酮酸矽及1,3-二酮矽(silicon 1,3-diketonate)前驅物製備多孔合成半結晶有機-無機雜合氧化矽組成物的方法(US6465387)。
儘管有諸多選擇可用於含Si薄膜之沉積，但仍不斷尋找其他前驅物以為裝置工程師提供調節製造製程要求及達成具有所要電學及物理性質之薄膜的能力。
記法及命名法
貫穿以下說明書及申請專利範圍使用某些縮寫、符號及術 語，且包括：
如本文所用，不定冠詞「一(a/an)」意謂一或多個。
如本文所用，術語「獨立地」在用於描述R基團之情形中時應理解為表示所述R基團不僅相對於帶有相同或不同下標或上標之其他R基團獨立地選擇，亦相對於同一R基團之任何其他種類獨立地選擇。舉例而言，在式MR1 x(NR2R3)(4-x)(其中x為2或3)中，兩個或三個R1基團可但無需彼此或與R2或R3相同。另外，應瞭解，除非另外特定陳述，否則當用於不同式子中時R基團之值彼此獨立。
如本文所用，術語「烷基」指排他性地含有碳及氫原子之飽和官能基。另外，術語「烷基」指直鏈、分支鏈或環狀烷基。直鏈烷基之實例包括但不限於甲基、乙基、丙基、丁基等。分支鏈烷基之實例包括但不限於第三丁基。環狀烷基之實例包括但不限於環丙基、環戊基、環己基等。
如本文所用，術語「芳基」指已自環中移除一個氫原子的芳環化合物。如本文所用，術語「雜環」指環狀化合物，其具有至少兩種不同元素之原子作為其環之成員。
如本文所用，縮寫「Me」指甲基；縮寫「Et」指乙基；縮寫「Pr」指任何丙基(亦即正丙基或異丙基)；縮寫「iPr」指異丙基；縮寫「Bu」指任何丁基(正丁基、異丁基、第三丁基、第二丁基)；縮寫「tBu」指第三丁基；縮寫「sBu」指第二丁基；縮寫「iBu」指異丁基；縮寫「Ph」指苯基；縮寫「Am」指任何戊基(異戊基、第二戊基、第三戊基)；縮寫「Hex」指6員烷基，其可為直鏈、分支鏈或環狀；且縮寫「Cy」指環狀烷基(環丁基、環戊基、環己基等)。
如本文所用，首字母縮寫詞「SRO」表示氧化鍶釕薄膜；首字母縮寫詞「HCDS」表示六氯二矽烷；且首字母縮寫詞「PCDS」表示五氯二矽烷。
本文使用元素週期表之元素的標準縮寫。應瞭解，可用此等 縮寫來指代元素(例如Si指矽，N指氮，O指氧，C指碳等)。
揭示具有下式之有機矽烷分子：
其中L1及L2各為氮原子；L1及L2經由具有兩個至三個碳原子之碳橋連接在一起；L1、L2及碳橋形成鍵結於矽之單陰離子配位體。所揭示之分子可具有以下態樣中之一或多者：‧有機矽烷分子具有下式：
其中R1、R2、R3、R4及R5可各獨立地為H、C1至C6烷基或C3-C20芳基或雜環；‧R1與R2及/或R2與R3及/或R3與R4及/或R4與R5連接以形成環狀鏈；‧有機矽烷分子為H3Si(-(iPr)N-C3H3-N(iPr)-)；‧有機矽烷分子具有下式：
其中R1、R2、R3、R4、R5及R6可各獨立地為H、C1至C6烷基或C3-C20芳基或雜環；‧R1與R2及/或R2與R3及/或R3與R4及/或R4與R5及/或R5與R6連接以形成環狀鏈；‧有機矽烷分子為H3Si(-(iPr)N-C3H6-N(Me)2-)；‧有機矽烷分子具有下式：
其中R1、R2、R3、R4及R5可各獨立地為H、C1至C6烷基或C3-C20芳基或雜環；‧R1與R2及/或R2與R3及/或R3與R4連接以形成環狀鏈；‧有機矽烷分子為H3Si(-(iPr)N-CH2CH=N(iPr)-)；‧有機矽烷分子具有下式：
其中R1、R2、R3、R4及R5可各獨立地為H、C1至C6烷基或C3-C20芳基或雜環；‧R1與R2及/或R2與R3及/或R3與R4及/或R4與R5連接以形成環狀鏈；且‧有機矽烷分子為H3Si((iPr)NC2H4N(Me)2。
亦揭示具有下式之形成含Si薄膜之前驅物：
其中L1及L2各為氮原子；L1及L2經由具有兩個至三個碳原子之碳橋連接在一起；L1、L2及碳橋形成鍵結於矽之單陰離子配位體。所揭示之分子可具有以下態樣中之一或多者：‧形成含Si薄膜之前驅物具有下式：
其中R1、R2、R3、R4及R5可各獨立地為H、C1至C6烷基或C3-C20芳 基或雜環；‧R1與R2及/或R2與R3及/或R3與R4及/或R4與R5連接以形成環狀鏈；‧形成含Si薄膜之前驅物為H3Si(-(iPr)N-C3H3-N(iPr)-)；‧形成含Si薄膜之前驅物具有下式：
其中R1、R2、R3、R4、R5及R6可各獨立地為H、C1至C6烷基或C3-C20芳基或雜環；‧R1與R2及/或R2與R3及/或R3與R4及/或R4與R5及/或R5與R6連接以形成環狀鏈；‧形成含Si薄膜之前驅物為H3Si(-(iPr)N-C3H6-N(Me)2-)；‧形成含Si薄膜之前驅物具有下式：
其中R1、R2、R3、R4及R5可各獨立地為H、C1至C6烷基或C3-C20芳基或雜環；‧R1與R2及/或R2與R3及/或R3與R4連接以形成環狀鏈；‧形成含Si薄膜之前驅物為H3Si(-(iPr)N-CH2CH=N(iPr)-)；‧形成含Si薄膜之前驅物具有下式：
其中R1、R2、R3、R4及R5可各獨立地為H、C1至C6烷基或C3-C20芳基或雜環；‧R1與R2及/或R2與R3及/或R3與R4及/或R4與R5連接以形成環狀鏈； 且‧形成含Si薄膜之前驅物為H3Si((iPr)NC2H4N(Me)2。
亦揭示在基板上沉積含Si層之方法。
以上揭示之至少一種有機矽烷前驅物引入內部安置有至少一個基板之反應器中。使用氣相沉積法將至少一部分有機矽烷前驅物沉積至至少一個基板上以形成含Si層。所揭示之方法可具有以下態樣中之一或多者：‧向反應器中引入包含至少一種第二前驅物之蒸氣；‧至少一種第二前驅物之元素選自由以下組成之群：第2族、第13族、第14族、過渡金屬、鑭系元素及其組合；‧至少一種第二前驅物之元素選自Mg、Ca、Sr、Ba、Zr、Hf、Ti、Nb、Ta、Al、Si、Ge、Y或鑭系元素；‧向反應器中引入至少一種共反應物；‧共反應物選自由以下組成之群：O2、O3、H2O、H2O2、NO、NO2、羧酸、其自由基及其組合；‧共反應物為經電漿處理之氧氣；‧共反應物為臭氧；‧含Si層為氧化矽層；‧共反應物選自由以下組成之群：H2、NH3、(SiH3)3N、氫化矽烷(諸如SiH4、Si2H6、Si3H8、Si4H10、Si5H10、Si6H12)、氯矽烷及氯聚矽烷(諸如SiHCl3、SiH2Cl2、SiH3Cl、Si2Cl6、Si2HCl5、Si3Cl8)、烷基矽烷(諸如Me2SiH2、Et2SiH2、MeSiH3、EtSiH3)、肼(諸如N2H4、MeHNNH2、MeHNNHMe)、有機胺(諸如NMeH2、NEtH2、NMe2H、NEt2H、NMe3、NEt3、(SiMe3)2NH)、吡唑啉、吡啶、含B分子(諸如B2H6、9-硼雙環[3,3,1]壬烷、三甲基硼、三乙基硼、硼吖(borazine))、烷基金屬(諸如三甲基鋁、三乙基鋁、二甲基鋅、二乙 基鋅)、其自由基物質及其混合物。
‧共反應物選自由以下組成之群：H2、NH3、SiH4、Si2H6、Si3H8、SiH2Me2、SiH2Et2、N(SiH3)3、其氫自由基及其混合物；‧共反應物經電漿處理；‧共反應物經遠端電漿處理；‧共反應物不經電漿處理；‧共反應物為H2；‧共反應物為NH3；‧共反應物為HCDS；‧共反應物為PCDS；‧共反應物為四氯矽烷；‧共反應物為三氯矽烷；‧共反應物為六氯環六矽烷；‧氣相沉積製程為化學氣相沉積製程；‧氣相沉積製程為原子層沉積(ALD)製程；‧氣相沉積製程為空間ALD製程；‧含矽層為Si；‧含矽層為SiO2；‧含矽層為SiN；‧含矽層為SiON；‧含矽層為SiCN；且‧含矽層為SiCOH。
揭示形成含Si薄膜之前驅物、其合成方法及使用其以使用氣相沉積製程沉積含矽薄膜用於製造半導體、光伏打裝置、LCD-TFT、平板型裝置、耐火材料或航空材料之方法。
所揭示之形成含Si薄膜之前驅物具有下式：
其中L1及L2各為氮原子，L1及L2經由具有兩個或三個碳原子之碳橋連接在一起；L1、L2及碳橋形成鍵結於矽之單陰離子配位體。如該式中所說明，L1及L2氮原子鍵結於矽原子，從而產生五配位Si(IV)中心。碳橋中之碳原子可為sp2雜化，從而在單陰離子配位體上產生非定域電荷。或者，碳橋中之碳原子可為sp3雜化或sp2與sp3雜化的某種組合，從而在L1或L2中之一者上產生負電荷且在L1或L2中之另一者上產生中性電荷。氮及碳原子可各獨立地經H、C1-C6烷基、芳基或雜環基取代。
所揭示之有機矽烷前驅物由於矽原子處之超配位而可能比其他R4-xSiLx前驅物更具反應性。換言之，儘管矽原子為+IV，但三個氫鍵及單陰離子螯合配位體與矽原子形成總共5個鍵。
由於其在N-(C)n-N配位體(其中n為2或3)上之氮含量增加，此等分子可用於產生亦含有氮之含矽薄膜，諸如SiN、SiCN、SiON、MSiN或MSiON，其中M為諸如Hf、Zr、Ti、Nb、Ta或Ge之元素，或用於調節彼等薄膜中之氮的量。
當所揭示之有機矽烷前驅物的碳橋包括三(3)個碳原子(亦即-N-(C(R))3-N-)時，所得前驅物為β-二酮亞胺基矽烷(β-diketiminatosilane)化合物。例示性β-二酮亞胺基矽烷前驅物具有下式：
其中R1、R2、R3、R4及R5可各獨立地為H、C1至C6烷基或C3-C20芳基或雜環，R1與R2及/或R2與R3及/或R3與R4及/或R4與R5可連接以形成環狀鏈。三個碳原子為sp2雜化。若R1與R5相同且R2與R4相同(亦即均為Me或R1及R5=Me且R2及R4=H)，則由於配位體上電子之非定域作用，此等分子所產生之傅立葉變換紅外(FTIR)光譜將針對兩個N原子產生一個峰。
具有上式之例示性β-二酮亞胺基矽烷前驅物包括：
較佳地，β-二酮亞胺基矽烷前驅物為H3Si(-(iPr)N-C3H3-N(iPr)-)。
當所揭示之有機矽烷前驅物的碳橋包括三(3)個碳原子(亦即-N-(C(R))3-N-)時，所得前驅物為胺基矽烷胺化合物。例示性胺基矽烷胺有機矽烷前驅物具有下式：
其中R1、R2、R3、R4、R5及R6可各獨立地為H、C1至C6烷基或C3-C20芳基或雜環。一般技術者將想到以上結構中碳上所隱含之H，其由於空間限制已省去。R1與R2及/或R2與R3及/或R3與R4及/或R4與R5及/或R4與R6可連接以形成環狀鏈。三個碳原子可為sp2或sp3雜化。陰離子電荷可定域在「頂部」氮原子處。「底部」氮原子可與Si原子形成配位鍵。由於配位體之不對稱性，在核磁共振(NMR)光譜中三個碳原子將產生不同的峰。
具有上式之例示性胺基矽烷胺前驅物包括：
較佳地，胺基矽烷胺前驅物為H3Si(-(iPr)N-C3H6-N(Me)2-)。
H3Si[RN(CR)3NR]或H3Si[R2N(CR)3NR]前驅物可如下合成：藉由將SiXH3(其中X為Cl、Br、I或三氟甲磺酸根(SO3CF3 -))之烴溶液與純配位體化合物(諸如Li[RN(CR)3NR]或Li[R2N(CR)3NR])或其烴溶液在氮氣氛圍下組合，混合燒瓶之出口與油起泡器連接以抑制空氣及水分回流。
獲得所揭示之H3Si[RN(CR)3NR]或H3Si[R2N(CR)3NR]前驅物之第二合成途徑為藉由在惰性氛圍下使質子化配位體RN(CR)3NHR或RHN(CR)3NR2與純二烷基胺基矽烷[SiH3(NR2)]或其烴溶液反應。
或者，所揭示之H3Si[RN(CR)3NR]或H3Si[R2N(CR)3NR]前驅物 可如下合成：藉由使SiHnCl4-n與單一當量之配位體化合物(亦即Li[RN(CR)3NR]或Li[R2N(CR)3NR])反應隨後使用所選金屬氫化物(諸如LAH(氫化鋰鋁))還原。
在所有三個合成途徑中，可在室溫下攪拌所得溶液隔夜。適合於此等合成方法之例示性烴溶液包括乙醚、戊烷、己烷或甲苯。過濾所得懸浮液且蒸餾所得溶液以移除溶劑。分別藉由蒸餾或昇華來純化所得液體或固體。除了配位體化合物Li[RN(CR)3NR]或Li[R2N(CR)3NR]，所有起始材料均可在市面上購得。配位體化合物可藉由將有機金屬鹽(亦即烷基鋰)之烴溶液與適當二胺(亦即R1N=CR2-CR3-CR4-NHR5、R1N=CR2-CR3=CR4-NHR5、R1HN-CR2-CR3-CR4-NR5R6)之烴溶液組合來合成。一般技術者將認識到適當選擇配位體將產生不飽和β-二酮亞胺基矽烷前驅物或飽和胺基矽烷胺前驅物。
當所揭示之有機矽烷前驅物的碳橋包括兩(2)個碳原子(亦即-N-(C(R))2-N-)時，所得前驅物為亞胺基矽烷胺化合物。例示性亞胺基矽烷胺有機矽烷前驅物具有下式：
其中R1、R2、R3及R4可各獨立地為H、C1至C6烷基或C3-C20芳基或雜環。一般技術者將想到以上結構中碳上所隱含之H，其由於空間限制已省去。R1與R2及/或R2與R3及/或R3與R4可連接以形成環狀鏈。兩個碳原子可為sp2或sp3雜化。上式說明定域在「頂部」氮原子處之陰離子電荷。與C(R3)具有雙鍵之「底部」氮原子與矽原子形成配位鍵。然而，一般技術者應認識到當碳原子為sp2雜化時雙鍵亦可在環上非定域。若R1與R4相同且R2與R3相同(亦即均為Me或R1及R4=Me且R2及R3=H)，則由於配位體上 電子之非定域作用，此等分子所產生之傅立葉變換紅外(FTIR)光譜將針對兩個N原子產生一個峰。
具有上式之例示性亞胺基矽烷胺前驅物包括：
較佳地，亞胺基矽烷胺為H3Si(-(iPr)N-CH2CH=N(iPr)-)。
當所揭示之有機矽烷前驅物的碳橋包括兩(2)個碳原子(亦即-N-(C(R))2-N-)時，所得前驅物為胺基矽烷胺化合物。例示性胺基矽烷胺有機矽烷前驅物具有下式：
其中R1、R2、R3、R4及R5可各獨立地為H、C1至C6烷基或C3-C20芳基或雜環。一般技術者將想到以上結構中碳上所隱含之H，其由於空間限制已省去。R1與R2及/或R2與R3及/或R3與R4及/或R4與R5可連接以形成環狀鏈。兩個碳原子可為sp2或sp3雜化。陰離子電荷可定域在氮原子處。另一氮原子可與Si原子形成配位鍵。由於配位體之不對稱性，在核磁共振(NMR)光譜中兩個碳原子將產生不同的峰。
具有上式之例示性胺基矽烷胺前驅物包括：
較佳地，胺基矽烷胺前驅物為H3Si((iPr)NC2H4N(Me)2。
H3Si[RN(CR)2NR]或H3Si[R2N(CR)2NR]前驅物可如下合成：藉由將SiXH3(其中X為Cl、Br、I或三氟甲磺酸根(SO3CF3 -))之烴溶液與純配位體化合物(諸如Li[RN(CR)2NR]或Li[R2N(CR)2NR])或其烴溶液在氮氣氛圍下組合，混合燒瓶之出口與油起泡器連接以抑制空氣及水分之回流。
獲得所揭示之H3Si[RN(CR)2NR]或H3Si[R2N(CR)2NR]前驅物之第二合成途徑為藉由在惰性氛圍下使質子化配位體RN(CR)2NHR或RHN(CR)2NR2與純二烷基胺基矽烷[SiH3(NR2)]或其烴溶液反應。
或者，所揭示之H3Si[RN(CR)2NR]或H3Si[R2N(CR)2NR]前驅物可如下合成：藉由使SiHnCl4-n與單一當量之配位體化合物(亦即Li[RN(CR)2NR]或Li[R2N(CR)2NR])反應隨後使用所選金屬氫化物(諸如LAH(氫化鋰鋁))還原。
在所有三個合成途徑中，可在室溫下攪拌所得溶液隔夜。適合於此等合成方法之例示性烴溶液包括乙醚、戊烷、己烷或甲苯。過濾所得懸浮液且蒸餾所得溶液以移除溶劑。分別藉由蒸餾或昇華來純化所得液體或固體。除了配位體化合物Li[RN(CR)2NR]或Li[R2N(CR)2NR]，所有起始材料均可在市面上購得。配位體化合物可藉由將有機金屬鹽(亦即烷基鋰) 之烴溶液與適當二胺(亦即R1N=CR2-CR3-NHR4、R1HN-CR2-CR3-NR4R5)之烴溶液組合來合成。一般技術者將認識到適當選擇配位體將產生飽和胺基矽烷胺基或不飽和亞胺基矽烷胺基前驅物。
亦揭示使用所揭示之有機矽烷前驅物進行氣相沉積法之方法。所揭示之方法提供有機矽烷前驅物用於沉積含矽薄膜之用途。所揭示之方法可適用於製造半導體、光伏打裝置、LCD-TFT或平板型裝置。該方法包括：提供基板；提供包括所揭示之有機矽烷前驅物中之至少一者的蒸氣；及使蒸氣與基板接觸(且典型地將蒸氣導引至基板)以在基板之至少一個表面上形成含矽層。
所揭示之方法亦可使用氣相沉積製程在基板上形成含雙金屬層且更特定言之沉積SiMOx薄膜，其中x可為0-4且M為Ta、Hf、Nb、Mg、Al、Sr、Y、Ba、Ca、As、Sb、Bi、Sn、Pb、Co、鑭系元素(諸如Er)或其組合。所揭示之方法可適用於製造半導體、光伏打裝置、LCD-TFT或平板型裝置。該方法包括：提供基板；提供包括所揭示之有機矽烷前驅物中之至少一者的蒸氣且使蒸氣與基板接觸(且典型地將蒸氣導引至基板)以在基板之至少一個表面上形成含雙金屬之層。諸如O3、O2、H2O、NO、H2O2、乙酸、福爾馬林、三聚甲醛、其氧自由基及其組合但較佳O3或經電漿處理之O2的氧源亦可與蒸氣一起提供。
所揭示之有機矽烷前驅物可用於使用熟習此項技術者已知之任何沉積方法沉積含矽薄膜。適合沉積方法之實例包括但不限於習知化學氣相沉積(CVD)、低壓化學氣相沉積(LPCVD)、原子層沉積(ALD)、脈衝式化學氣相沉積(P-CVD)、熱ALD、熱CVD、電漿增強式原子層沉積(PE-ALD)、電漿增強式化學氣相沉積(PE-CVD)、空間ALD或其組合。較佳地，沉積方法為ALD、空間ALD或PE-ALD。
將有機矽烷前驅物蒸氣引入含有至少一個基板之反應室 中。反應室內之溫度及壓力以及基板之溫度保持在適合於將至少一部分有機矽烷前驅物氣相沉積至基板上之條件下。換言之，在將汽化前驅物引入腔室中之後，腔室內之條件使得至少一部分汽化前驅物沉積至基板上以形成含矽薄膜。共反應物亦可用於幫助形成含Si層。
反應室可為裝置中進行沉積方法之任何封閉區域或腔室，諸如但不限於平行板型反應器、冷壁型反應器、熱壁型反應器、單晶圓反應器、多晶圓反應器或其他此種類型之沉積系統。所有此等例示性反應室均能夠充當ALD反應室。反應室可維持在約0.5毫托至約20托範圍內之壓力下。此外，反應室內之溫度可在約20℃至約600℃範圍內。一般技術者應認識到可僅經由實驗來優化溫度以達成所要結果。
可藉由控制基板固持器之溫度或控制反應器壁之溫度來控制反應器溫度。用於加熱基板之裝置為本領域中已知。將反應器壁加熱至足以獲得處於充足生長速率下且具有所要物理狀態及組成之所要薄膜的溫度。可將反應器壁加熱至的非限制性例示性溫度範圍包括約20℃至約600℃。當使用電漿沉積製程時，沉積溫度可在約20℃至約550℃範圍內。或者，當執行熱製程時，沉積溫度可在約300℃至約600℃範圍內。
或者，可將基板加熱至足以獲得處於充足生長速率下且具有所要物理狀態及組成之所要含矽薄膜的溫度。可將基板加熱至的非限制性例示性溫度範圍包括150℃至600℃。較佳地，基板溫度保持低於或等於500℃。
上面將沉積含矽薄膜之基板的類型將視預期的最終用途而不同。在一些具體實例中，基板可為由氫化碳(例如CHx，其中x大於零)製成之圖案化光阻薄膜。在一些具體實例中，基板可選自在MIM、DRAM或FeRam技術中用作介電材料之氧化物(例如基於ZrO2之材料、基於HfO2之材料、基於TiO2之材料、基於稀土氧化物之材料、基於三元氧化物(ternary oxide)之材料等)或選自用作銅與低k層之間的氧障壁之基於氮化物之薄膜(例如TaN)。可使用其他基板來製造半導體、光伏打裝置、LCD-TTFT或平板裝置。此類基板之實例包括但不限於固體基板，諸如含有金屬氮化物之基板(例如TaN、TiN、WN、TaCN、TiCN、TaSiN及TiSiN)；絕緣體(例如SiO2、Si3N4、SiON、HfO2、Ta2O5、ZrO2、TiO2、Al2O3及鈦酸鋇鍶)；或包括此等材料之多種組合的其他基板。所使用之實際基板亦可視所使用之特定前驅物具體實例而定。但在許多情況下，所使用之較佳基板將選自氫化碳、TiN、SRO、Ru及Si型基板，諸如多晶矽或結晶矽基板。
所揭示之有機矽烷前驅物可以純形式或以與適合溶劑(諸如甲苯、乙苯、二甲苯、均三甲苯、癸烷、十二烷、辛烷、己烷、戊烷、三級胺、丙酮、四氫呋喃、乙醇、乙基甲基酮、1,4-二烷或其他溶劑)之摻合物形式供應。所揭示之前驅物可以不同濃度存在於溶劑中。舉例而言，所得濃度可在約0.05M至約2M範圍內。
純的或摻合的有機矽烷前驅物藉由習知構件(諸如管道及/或流量計)以蒸氣形式引入反應器中。可藉由經由習知汽化步驟(諸如直接汽化、蒸餾、藉由鼓泡或藉由使用昇華器(諸如Xu等人之PCT公開案WO2009/087609中所揭示之昇華器))使純的或摻合的前驅物溶液汽化來產生呈蒸氣形式之前驅物。純的或摻合的前驅物可以液態饋至汽化器中，在該汽化器中其經汽化隨後將其引入反應器中。或者，可藉由將載氣通入含有前驅物之容器中或藉由使載氣鼓泡至前驅物中來使純的或摻合的前驅物汽化。載氣可包括但不限於Ar、He或N2及其混合物。用載氣鼓泡亦可移除存在於純的或摻合的前驅物溶液中之任何溶解氧。接著，載氣及前驅物以蒸氣形式引入反應器中。
必要時，可將容器加熱至允許有機矽烷前驅物呈其液相且具有充足蒸氣壓之溫度。容器可維持在例如0-150℃範圍內之溫度下。熟習此 項技術者認識到可以已知方式調節容器之溫度以控制汽化之有機矽烷前驅物之量。
除所揭示之前驅物以外，反應氣體(亦即共反應物)亦可引入反應器中。反應氣體可為氧化劑，諸如以下中之一者：O2；O3；H2O；H2O2；含氧自由基，諸如O．或OH．；NO；NO2；羧酸，諸如甲酸、乙酸、丙酸；NO、NO2或羧酸之自由基物質；三聚甲醛；及其混合物。較佳地，氧化劑選自由以下組成之群：O2、O3、H2O、H2O2、其含氧自由基(諸如O．或OH．)及其混合物。較佳地，當執行ALD製程時，共反應物為經電漿處理之氧氣、臭氧或其組合。當使用氧化氣體時，所得含矽薄膜亦將含有氧。
或者，反應氣體可為還原劑，諸如以下中之一者：H2、NH3、(SiH3)3N、氫化矽烷(諸如SiH4、Si2H6、Si3H8、Si4H10、Si5H10、Si6H12)、氯矽烷及氯聚矽烷(諸如SiHCl3、SiH2Cl2、SiH3Cl、Si2Cl6、Si2HCl5、Si3Cl8)、烷基矽烷(諸如(CH3)2SiH2、(C2H5)2SiH2、(CH3)SiH3、(C2H5)SiH3)、肼(諸如N2H4、MeHNNH2、MeHNNHMe)、有機胺(諸如N(CH3)H2、N(C2H5)H2、N(CH3)2H、N(C2H5)2H、N(CH3)3、N(C2H5)3、(SiMe3)2NH)、吡唑啉、吡啶、含B分子(諸如B2H6、9-硼雙環[3,3,1]壬烷、三甲基硼、三乙基硼、硼吖)、烷基金屬(諸如三甲基鋁、三乙基鋁、二甲基鋅、二乙基鋅)、其自由基物質及其混合物。較佳地，還原劑為H2、NH3、SiH4、Si2H6、Si3H8、SiH2Me2、SiH2Et2、N(SiH3)3、其氫自由基或其混合物。當使用還原劑時，所得含矽薄膜可為純Si。
反應氣體可經電漿處理，以便使反應氣體分解成其自由基形式。當經電漿處理時N2亦可用作還原劑。舉例而言，可產生功率在約50W至約500W、較佳約100W至約200W範圍內之電漿。電漿可產生或存在於反應器自身內。或者，電漿可通常處於移離反應器之位置處，例如在遠端定位之電漿系統中。熟習此項技術者將想到適合於該電漿處理之方法及 裝置。
所揭示之有機矽烷前驅物亦可與鹵代矽烷或聚鹵代矽烷(諸如六氯二矽烷、五氯二矽烷或四氯二矽烷)及一或多種共反應物氣體一起使用，以形成SiN或SiCN薄膜，如PCT公開案第WO2011/123792號中所揭示，該公開案之全部內容以其全文併入本文中。
當所要含矽薄膜亦含有另一元素(諸如但不限於Ta、Hf、Nb、Mg、Al、Sr、Y、Ba、Ca、As、Sb、Bi、Sn、Pb、Co、鑭系元素(諸如Er)或其組合)時，共反應物可包括含金屬前驅物，其選自但不限於金屬烷基，諸如Ln(RCp)3或Co(RCp)2；金屬胺，諸如Nb(Cp)(NtBu)(NMe2)3；及其任何組合。
有機矽烷前驅物及一或多種共反應物可同時(化學氣相沉積)、相繼(原子層沉積)或以其他組合形式引入反應室中。舉例而言，有機矽烷前驅物可在一次脈衝中引入且兩種其他金屬來源可在獨立脈衝中一起引入[改良的原子層沉積]。或者，反應室在引入有機矽烷前驅物之前可能已含有共反應物。可使共反應物通過定位於反應室遠端之電漿系統，且分解成自由基。或者，有機矽烷前驅物可連續引入反應室中，而其他金屬來源藉由脈衝引入(脈衝式化學氣相沉積)。在各實施例中，可在脈衝之後進行吹掃或抽空步驟以移除所引入之過量組分。在各實施例中，脈衝可持續約0.01s至約10s，或者約0.3s至約3s，或者約0.5s至約2s範圍內之時間。在另一替代方案中，有機矽烷前驅物及一或多種共反應物可同時自淋浴噴頭噴灑，在該淋浴噴頭下固持若干晶圓之基座旋轉(空間ALD)。
在一個非限制性例示性原子層沉積型製程中，有機矽烷前驅物之氣相引入反應室中，在該反應室中其與適合基板接觸。接著，可藉由吹掃及/或抽空反應室來自反應室中移除過量有機矽烷前驅物。將氧源引入反應室中，在該反應室中其與所吸收之有機矽烷前驅物以自限制方式反 應。藉由吹掃及/或抽空反應室自反應室中移除任何過量氧源。若所要薄膜為氧化矽薄膜，則此兩步製程可提供所要膜厚度或可重複直至已獲得具有必需厚度之薄膜。
或者，若所要薄膜為矽金屬氧化物薄膜(亦即SiMOx，其中及x可為0-4且M為Ta、Hf、Nb、Mg、Al、Sr、Y、Ba、Ca、As、Sb、Bi、Sn、Pb、Co、鑭系元素(諸如Er)或其組合)，則可在以上兩步製程之後將含金屬前驅物之第二蒸氣引入反應室中。含金屬前驅物將基於所沉積之矽金屬氧化物薄膜之性質來選擇。在引入反應室中之後，含金屬前驅物與基板接觸。藉由吹掃及/或抽空反應室自反應室中移除任何過量含金屬前驅物。再次，可將氧源引入反應室中以與含金屬前驅物反應。藉由吹掃及/或抽空反應室自反應室中移除過量氧源。若已達成所要膜厚度，則製程可終止。然而，若需要較厚薄膜，則可重複整個四步驟製程。藉由交替提供有機矽烷前驅物、含金屬前驅物及氧源，可沉積具有所要組成及厚度之薄膜。
另外，藉由改變脈衝次數，可獲得具有所要化學計量M：Si比率之薄膜。舉例而言，藉由進行一次有機矽烷前驅物之脈衝及一次含金屬前驅物之脈衝，且在各脈衝之後進行氧源之脈衝可獲得SiMO2薄膜。然而，一般技術者應認識到為獲得所要薄膜所需之脈衝次數可能不等於所得薄膜之化學計量比率。
在另一替代方案中，可經由ALD或改良的ALD製程使用所揭示之化合物及具有式SiaH2a+2-bXb(其中X為F、Cl、Br或I；a=1至6；且b=1至(2a+2))之鹵代矽烷化合物；或具有式-SicH2c-dXd-(其中X為F、Cl、Br、或I；c=3-8；且d=1至2c)之環狀鹵代矽烷化合物沉積Si或緻密SiCN薄膜。較佳地，鹵代矽烷化合物為三氯矽烷、六氯二矽烷(HCDS)、五氯二矽烷(PCDS)、四氯二矽烷或六氯環六矽烷。一般技術者應認識到當必需為較低沉積溫度時此等化合物中之Cl可經Br或I取代，此歸因於Si-X鍵 之較低鍵能(亦即Si-Cl=456kJ/mol；Si-Br=343kJ/mol；Si-I=339kJ/mol)。必要時，沉積可進一步使用含N共反應物，諸如NH3。所揭示之前驅物及鹵代矽烷化合物之蒸氣可視所要之最終薄膜濃度而相繼或同時引入反應器。所選前驅物注入順序將基於所要目標薄膜組成來確定。可重複前驅物引入步驟直至沉積層達成適合厚度。一般技術者應認識到當使用空間ALD裝置時引導性脈衝(introductory pulse)可為同時的。如PCT公開案第WO2011/123792號中所描述，可改變前驅物引入順序且可在存在或不存在NH3共反應物下執行沉積，以便調節SiCN薄膜中碳及氮之量。
由上文所論述之製程產生之含矽薄膜可包括SiO2、SiN、SiON、SiCN、SiCOH或MSiOx，其中M為諸如Hf、Zr、Ti、Nb、Ta或Ge之元素，且x可為4，當然視M之氧化態而定。一般技術者應認識到藉由慎重選擇適當有機矽烷前驅物及共反應物，可獲得所要薄膜組成。
獲得所要膜厚度後，可對薄膜進行進一步處理，諸如熱退火、爐退火、快速熱退火、UV或電子束固化及/或電漿氣體暴露。熟習此項技術者可想到用於執行此等額外加工步驟之系統及方法。舉例而言，含矽薄膜可在惰性氛圍、含H氛圍、含N氛圍、含O氛圍或其組合下暴露於約200℃至約1000℃範圍內之溫度，持續約0.1秒至約7200秒範圍內之時間。最佳地，溫度為400℃，在含H氛圍下持續3600秒。所得薄膜可含有較少雜質，且因此可具有改良之效能特性。可在執行沉積製程之同一反應室中執行退火步驟。或者，可自反應室中移除基板，且在獨立裝置中執行退火/急驟退火製程。已發現以上後處理方法中之任一者、尤其熱退火可有效減少含矽薄膜之碳及氮污染。
應瞭解，在如所附申請專利範圍中所表述之本發明原理及範疇內，熟習此項技術者可對本文中已描述且說明以便解釋本發明之性質的細節、材料、步驟及部件配置作出許多其他改變。因此，本發明並不意欲 限於以上所提供之實施例及/或隨附圖式中的特定具體實例。

Claims (15)

  1. 一種形成含Si薄膜之前驅物，其具有下式： 其中L1及L2各為氮原子；L1及L2經由具有兩個至三個碳原子之碳橋連接在一起；L1、L2及該碳橋形成鍵結於矽之單陰離子配位體。
  2. 如申請專利範圍第1項之形成含Si薄膜之前驅物，其具有下式： 其中R1、R2、R3、R4及R5可各獨立地為H或C1至C6烷基。
  3. 如申請專利範圍第2項之形成含Si薄膜之前驅物，其中該形成含Si薄膜之前驅物為H3Si(-(iPr)N-C3H3-N(iPr)-)。
  4. 如申請專利範圍第1項之形成含Si薄膜之前驅物，其具有下式： 其中R1、R2、R3、R4、R5及R6可各獨立地為H或C1至C6烷基。
  5. 如申請專利範圍第4項之形成含Si薄膜之前驅物，其中該形成含Si薄膜之前驅物為H3Si(-(iPr)N-C3H6-N(Me)2-)。
  6. 如申請專利範圍第1項之形成含Si薄膜之前驅物，其具有下式： 其中R1、R2、R3及R4可各獨立地為H或C1至C6烷基。
  7. 如申請專利範圍第6項之形成含Si薄膜之前驅物，其中該形成含Si薄膜之前驅物為H3Si(-(iPr)N-CH2CH=N(iPr)-)。
  8. 如申請專利範圍第1項之形成含Si薄膜之前驅物，其具有下式： 其中R1、R2、R3、R4及R5可各獨立地為H或C1至C6烷基。
  9. 如申請專利範圍第8項之形成含Si薄膜之前驅物，其中該形成含Si薄膜之前驅物為H3Si((iPr)NC2H4N(Me)2。
  10. 一種在基板上沉積含Si層之方法，該方法包含：將至少一種如申請專利範圍第1項至第9項中任一項之形成含Si薄膜之前驅物引入內部安置有至少一個基板之反應器中；使用氣相沉積法將至少一部分該形成含Si薄膜之前驅物沉積至該至少一個基板上以形成含Si層。
  11. 如申請專利範圍第10項之方法，其進一步包含向該反應器中引入至少一種共反應物。
  12. 如申請專利範圍第11項之方法，其中該共反應物係選自由以下組成之群：O2、O3、H2O、H2O2、NO、NO2、羧酸、其自由基及其組合。
  13. 如申請專利範圍第11項之方法，其中該共反應物係選自由以下組成之群：H2、NH3、(SiH3)3N、氫化矽烷、氯矽烷及氯聚矽烷、烷基矽烷、肼、有機胺、吡唑啉、吡啶、含B分子、烷基金屬、其自由基物質及其混合物。
  14. 如申請專利範圍第13項之方法，其中該共反應物係選自由以下組成之群：H2、NH3、SiH4、Si2H6、Si3H8、SiH2Me2、SiH2Et2、N(SiH3)3、其氫自由基及其混合物。
  15. 如申請專利範圍第13項之方法，其中該共反應物係選自由以下組成之群：SiHCl3、Si2Cl6、Si2HCl5、Si2H2Cl4及環-Si6H6Cl6。
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