TW200813245A - Method of forming dielectric films, new precursors and their use in the semi-conductor manufacturing - Google Patents

Method of forming dielectric films, new precursors and their use in the semi-conductor manufacturing Download PDF

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TW200813245A
TW200813245A TW096119873A TW96119873A TW200813245A TW 200813245 A TW200813245 A TW 200813245A TW 096119873 A TW096119873 A TW 096119873A TW 96119873 A TW96119873 A TW 96119873A TW 200813245 A TW200813245 A TW 200813245A
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mecp
nme2
etcp
formula
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TW096119873A
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TWI525210B (zh
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Christian Dussarrat
Nicolas Blasco
Audrey Pinchart
Christophe Lachaud
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Air Liquide
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    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
    • H01L21/02205—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition
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    • C23C16/18—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material from metallo-organic compounds
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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Description

200813245
V
九、發明說明： 【發明所屬之技術領域】 物的係關於—種形成諸如給㈣之氧化物或氮氧化 物的局k介電膜之方法及其用於製造半導體之用途。 【先前技術】 ' 需要引 CMOS Si〇2， 隨著未來產生之半導體裝置的臨界尺寸減小， 入新材料，尤其是具有高介電常數之新穎材料。在 架構中’需要高k介電體以替換達到其物理極限之 該等介電體通常具有約lnm之Si〇2等效厚度。 一、々也在RAM應用之金屬-絕緣體_金屬架構中亦需 =k介電體1種金屬組合物已被認為滿足材料需求（二 電常數、_電流、結晶溫度、電荷收集)及整合需求（界 面處之熱穩定性、乾式蝕刻可行性…）。 最有希望之材料為基於第Iv族之材料，諸如幵⑺^、 HfSi〇4、Zr〇2、ZrSl〇4、肌a、HfLn〇x ( Ln 係選自由銳、 釔及稀土元素所組成之群組）及更通常HfMOx及ZrMOX， M為選自第π族、第nia族及第IIIb族之元素或過渡金屬。 此外第1 V族金屬組合物亦可考慮用於電極及/或cu擴 政I1早壁應用，諸如用於中間能隙金屬閘極之TiN及用於mim 電極之 HfN、ZrN、HfSi、ZrSi、HfSiN、ZrSiN、TiSiN。 使得能狗沈積具有合理產量及可接受純度之該等薄膜 之主要工業選擇為氣相沈積技術，諸如MOCVD (金屬-有 機化學氣相沈積）或ALD (原子層沈積）。該等沈積方法 需要必須滿足適當工業用途之極端需求之金屬前驅物。該 7 200813245 等方法需要金屬-有機物或金屬-画化物前驅物。多種銓及 锆之金屬-有機化合物已被視為能夠實現此類沈積之前驅 物。 諸如HfCl4、ZrCl4之鹵化物為最常見Hf/Zr前驅物且 已得到廣泛描述。Kim等人揭示了 HfCl4在以ALD使Hf02 沈積上之用途（Kim 等人，Electrochem Soc Proceedings 2005-05， 3 97，2005 )。然而，沈積過程中所產生諸如HC1 或Cl2之一些副產物可引起會對最終特性有害之表面/界面 粗糙度。視所用氧源而定，其他可能的副產物亦可能有害。 舉例而言，已偵測出根據QMS經由OC1片段產生之0C12 為HfCl4與03之間反應之副產物。此外，在高k氧化物之 情形下，C1或F雜質對最終電學特性極其有害。
Triyoso等人及Chang等人分別研究了 Hf (OtBu)4用 於 Hf02 MOCVD 及 ALD 之用途[Triyoso 等人；J. Electrochem. Soc.，152 (3)，G203-G209 (2005) ; Chang 等 人；Electrochem. Solid. State Let·，7 (6)，F42-F44 (2004)] 〇 Williams等人已評估了用於Hf02 MOCVD之Hf (mmp)4及 Hf (OtBu)2 (mmp)2。在 W02003035926 中，Jones 等人揭示 了經供體官能化烷氧基配位基（1-甲氧基-2-甲基-丙醇酸鹽 [OCMe2CH2OMe，mmp])改良之固體 Ti、Hf、Zr 及 La 前 驅物，該烷氧基配位基有助於抑制Zr及Hf醇鹽化合物之 寡聚化且增加其對抗濕氣之穩定性。然而，如Potter等人 所建議，所有彼等醇鹽前驅物均具有無法在ALD方法中實 現自我限制型沈積之缺點（R· J· Potter，P. R· Chalker，T. D_ 8 200813245 v
Manning，H. C· Aspinall，Υ· F. Loo, A. C. Jones，L. M. Smith， G. W. Critchlow, M. Schumacher, Chem. Vap. Deposition, 2005, 11， N0 3， 159-167) °
文獻中已廣泛揭示諸如Hf (NEtMe)4、Hf (NMe2)4、Hf (NEt2)4之烧基酸胺前驅物[Senzaki等人，J· Vac. Sci· Technol· A 22 (4)，2004 年 7 月 /8 月；Haussmann 等人，Chem. Mater. 2002，14，4350-4353 ; Kawahara 等人，J. Appl· Phys·， 第 43 卷，N°7A，2004，第 4129-4134 頁；Hideaki 等人，JP • 2002-093804; Metzner 等人，US 6,858,547; Dip 等人，US 2005/0056219 Al]。第 IV 族烷基醯胺對 ALD 及 MOCVD 方法均適合。此外，一些烷基醯胺在室溫下為液體（Hf (NEt2)4及Hf (NEtMe)4 )且具有足夠揮發性，且其允許在 低溫下發生自我限制型ALD以用於受限熱預算之程序。然 而，第IV族烷基醯胺（尤其Zr化合物之烷基醯胺）亦具 有多種缺陷，其中：其可能會在分布期間分解至導致進料 管線或蒸發器可能堵塞之程度，其可能會在沈積期間產生 ® 顆粒，其可能會在深溝槽沈積過程期間產生非均一組合 物，及其僅允許狹窄的自我限制型ALD溫度窗口，因此縮 減程序窗口。詳言之，Zr (NEtMe)4可在分布管線中分解且 在常用分布溫度170°C以上產生顆粒。Hf (NEtMe)4更具熱 穩定性，然而因熱分解而無法在300°C以上提供自我限制 型原子層沈積。 在WO 2007/055088中，Thenappan等人揭示脈基給及 鍅錯合物及其氣相沈積應用。Hf (NEt2)2 [(NiPr-CNEt2)2作 9 200813245 為貫例給出。然而，胍基銓及錘通常為具有極其有限揮發 性之固體。如熱解重量分析所例示，在無熱分解及後續顆 粒產生之風險下，無法獲得氣相Hf (NEt2)2 [(NiPr-CNEt2)2。
Lehn 等人（chem· Vap. Deposition，2006, 12, 280-284) 揭不肆（三甲基肼基）锆[Z]： (NMeN]v[e2)4]及銓以及其用於 低Λ CVD之用途。該等例示化合物具有可接受之揮發性 (據報導，在〇·06托（T〇rr) 、9{rc下昇華），但其在室 溫下為固體。
Carta等人揭示雙（環戊二烯基）雙二甲基铪[HfCp2Me2] (Carta 等人揭示於 Electrochem Soc Proceedings，260, 2005_09, 2005 中）’且多名作者（codato 等人，chem Vapor
Deposition，159, 5, 1995; Putkcmen 等人，J Mater Chem，3 141， 11，2001 ; Niinisto 等人，Langmuir，7321，21，2005 )提議 將一類新穎Zr及Hf化合物用作銓及锆烷基醯胺之替代 物：雙（環戊二烯基）雙二甲基铪、雙（環戊二烯基）雙 二甲基鍅，其允許ALD窗口高達400°C之有效ALD沈積 程序且在以H2〇作為共反應物之最適化條件下獲得具有小 於0.2% C之薄膜。然而，HfCp2Me2及ZrCp2Me2均具有在 室溫下為固體產物之缺點（HfChM^熔點為57.51)。此 使得1C製造者無法以工業方式使用彼等前驅物（即，使 用非定域谷為填充）’且會帶來簡便性與製程方面的問題。 在 US 6,743,473 中，Parkhe 等人揭示將（Cp(R)JxMHy. ,用於製造金屬及/或金屬氮化物層之用途，其中M係選自 钽、釩、鈮及铪，CP為環戊二烯基，R為有機基團。僅揭 200813245 示環戊二烯基钽及鈮化合物之實例。然而，並未揭示液體 前驅物或熔點低於5〇。(：之前驅物。
Heys等人近來已在w〇 2006/131751 A1中提議液體雙 (%：戊一細基）衍生物。然而，其亦呈現有限揮發性之缺 點且亦可能存在可能會使所達成生長速率受到限制之大的 位阻。 現今’需要提供液體或低熔點（< 50°C)第IV族前驅 物化合物’且詳言之及Zr化合物，其將同時允許適當 _ 分布（在分布溫度下之物理狀態、熱穩定性）、寬的自我 限制型ALD窗口及藉由ALD或MOCVD來沈積純薄膜。 【發明内容】 根據本發明，已發現某些基於環戊二烯基或戊二烯基 之第IV族金屬-有機前驅物適於藉由ALD或MOCVD方法 來沈積含第IV族金屬之薄膜，且具有下列優勢： -其在室溫下為液體或具有低於50°C之熔點； -其為熱穩定的，而能夠在無顆粒產生下適當的分布 ® (氣相或直接液體注射）； -其為熱穩定的以允許寬的自我限制型ALD窗口； 4) 允許藉由使用共反應物（選自由H2、NH3、02、H20、〇3、 SiH4、Si2H6、Si3H8、TriDMAS、BDMAS、BDEAS、TDEAS、 TDMAS、TEMAS、（SiH3)3 N、（SiH3)2 Ο、TMA 或含鋁前 驅物、TBTDET、TAT-DMAE、PET、TBTDEN、PEN、含 鑭系前驅物，諸如Ln (tmhd)3···所組成之群組）之一或其 組合來沈積多種含第IV族金屬之薄膜，包括三級材料或 11 200813245
V 四級材料。 根據第一具體實例，本發明係關於一種將含至少一種 金屬之介電膜沈積於基板上之方法，該介電膜包含式（J) 化合物： (MS.a M2a) ObNc5 ⑴ 其中： 〇 < a < 1 ； 〇 < b $ 3，較佳 1·5 £ b $ 2.5 ; ® 〇 < c < 1 ； M1表示選自铪（Hf)、锆（Zr)及鈦（Ti)之金屬； 且 Μ2表示選自下列各物之金屬原子：鎂（Mg )、鈣（Ca )、 辞（zn)、硼（B)、鋁（A)、銦（In)、矽（si)、鍺 (G〇、錫（Sn)、給（Η〇、鍅（Zr)、鈦（Ti)、釩 (V)、鈮（仙）、钽（Ta);及鑭系原子，更特定言之， _ 銳（Sc)、釔（Y)及鑭（La)及稀土金屬原子； 該方法包含下列步驟： 步驟a):提供基板於反應腔室中； 步驟b):蒸發含有至少一種1^1金屬之式（11)前驅 物以形成第一氣相金屬源； (VyOpUR'CiOzM1 R，〜 (π) 其中： M1係如上文所定義； 〇 S X $ 3，較佳 X = 〇 或 1 ; 12 200813245 〇Sz$3，較佳 z=l 或 2; 1 < (x + z) < 4 ； 〇 S y S 7，較佳 y = 2 ; 0 $ t $ 5，較佳 t =工·， (RiyOp )表示未經取代或經一或多個R1基團取代之 戊一烯基（Op)配位基’ y表示該戊二稀基配位基上取代 性R1基團的數目； (R2tCp )表示未經取代或經一或多個R2基團取代之 壞戊二烯基（Cp )配位基’ ί表示該環戊二烯基配位基上 _ 之取代性R1基團的數目； R1及R2相同或不同，且係獨立地選自由下列各物組 成之群：氯；具有1至4個碳原子之直鏈或支鏈烷基；Ν_ 烧基fe基，其中該烧基為直鏈或支鏈且具有丨至4個碳原 子，N，N-二烷基胺基，其中各烷基彼此相同或不同，為直 鏈或支鏈且具有1至4個碳原子；具有丨至4個碳原子之 直鏈或支鏈烧氧基；烧基石夕烧基酸胺基；脒基；及魏基，· R表示獨立地選自由下列各物組成之群之配位基：氫、 _ 氟、氯、溴或碘原子；具有1至4個碳原子之直鏈或支鏈 炫基；N-烷基胺基，其中該烷基為直鏈或支鏈且具有1至 4個碳原子；N，N_二烷基胺基，其中各烷基彼此相同或不 同’為直鏈或支鏈且具有1至4個碳原子；具有1至4個 石炭原子之直鏈或支鏈烷氧基；烷基矽烷基胺基，其中該烷 基為直鏈或支鏈且具有1至4個碳原子；二烷基矽烷基胺 基’其中各烷基彼此相同或不同，為直鏈或支鏈且具有1 至4個碳原子；三烷基矽烷基胺基，其中各烷基彼此相同 13 200813245 或不同，為直鏈或支鏈且具有1至4個碳原子；脉基；及 羰基；應瞭解，若該式（II)包含一個以上R，基團，則各 R1可彼此相同或不同， 視情況，步驟b’）：蒸發含至少一種μ2金屬之前驅 物，M2係如上文所定義；以形成視情況需要之第二氣相金 屬源； 步驟c):將該第一氣相金屬源及該視情況需要之第 二氣相金屬源引入反應腔室中，以促使其與該基板接觸， _ 從而在該基板上產生包含如上文所定義之式（〗）化合物的 含金屬介電膜之沈積； 其限制條件在於，若欲形成之含至少一種金屬之介電 膜包含式（Γ)化合物·· M1 丨 〇2 (Γ)， 其對應於如上文所定義之式（1)，其中a = 0，b = 2 且C = 〇;且若步驟b)中所涉及之含_金屬之前驅物為 式（ΙΓ)化合物： ^ (R2tCp)2 M1 r，2 (ιγ) 其對應於如上文所定義之式（II)，其中\ ==0且2 = 2, 則在該式（II’）中，在兩個（R2tCp )配位基中之至少一者 中 t > 0 〇 ^在如上文所定義之方法中，含至少一種金屬之式（II) il驅物及必要日寸含至少一種M2金屬之前驅物具有通常低 於50°c、較佳低於饥线點，且其在室溫下較佳為液體。 根據如上文所定義之方法之一特定具體實例，蒸發步 14 200813245 驟b)及必要時蒸發步冑b，）係、藉由將栽氣引入經加熱之 容器中而實現’該容器含有該含至少—種1^1金屬之式（11) 前驅物： (R^Op), (R2tCp)z Μ1 (π) 及必要時也含至少一種Μ2金屬之前驅物。該容器較 佳在允許獲得該等液相金屬源之溫度下及在足夠蒸氣壓力 下經加熱。必要時，可將一種或該兩種金屬前驅物混合至 溶劑或溶劑混合物及/或穩定劑中。舉例而言，該溶劑係選 自辛烷、己烷、戊烷或四甲基矽烷。溶劑或溶劑混合物中 金屬说驅物之濃度通常在〇·〇1 Μ與〇·5 Μ之間，且更特定 言之為約0.05 Μ。載氣係選自（但不限於）Ar、取、Η2、 &或其混合物。必要時，可在介於8〇_U(rc範圍内之溫度 下加熱合為。熟習此項技術者應考慮，可調節容器溫度以 控制所欲蒸發之前驅物之量。 載氣/瓜里通系h於1〇 sccm(標準立方公分）與5⑽sccln 之間。較佳地，載氣流量介於50sccm與2〇〇sccm之間。 根據如上文所定義之方法之另一特定具體實例，蒸發 步驟b)及必要時蒸發步驟b,)係藉由將液體形式的含 金屬之式（II)前驅物： (Rly°P)x (R2tCp)z M1 Rf4.x.z ( II) 及必要時含M2金屬之前驅物引入使其蒸發之蒸發器 中而貫現。必要時，可將一種或該兩種金屬前驅物混合至 溶劑或溶劑混合物及/或穩定劑中。舉例而言，該溶劑係選 自辛k己少兀、戊烷或四甲基矽烷。溶劑或溶劑混合物中 15 200813245 金屬前驅物之濃度通常在〇·01 Μ與0.5 Μ之間，且更特定 言之為約0·05 Μ。 根據一更特定具體實例，將蒸發步驟b )及蒸發步驟b，） 組合於兩種金屬源之一個蒸發步驟b ”）中。 在如上文所定義之方法之步驟c)中，將經蒸發之含 金屬前驅物引入使其與基板接觸之反應腔室中。 在本發明之上下文中，基板意謂半導體製造中所用之 任何基板，其因技術功能而需要經含金屬之薄膜塗覆。舉 _ 例而言，該等基板不僅選自矽基板（Si)、矽石基板（Si02 )、 氮化石夕基板（SiN)或氮氧化矽基板（si〇N)，且亦選自 鎢基板（W)或貴金屬基板，諸如鉑基板（pt)、鈀基板 (Pd)、鍺基板（Rh)或金基板（Au)。 將基板加熱至所需溫度以獲得具有足夠生長速率及所 要物理狀態與組成之所要薄膜。 步驟c)期間之溫度通常在15〇。〇至60(rc之範圍内。 該溫度較佳低於或等於4 5 〇 °C。 _ 控制反應腔室中之壓力以獲得具有足夠生長速率的所 要含金屬薄膜。步驟c)期間之壓力通常在約i毫托（mT〇rr) ( 0.1333224 Pa)至約 100 托（ 13332.24 pa)範圍内。 在本發明之上下文中，含M2金屬之前驅物係選自由 下列各物組成之群： 其鍺同系物，諸如： 一矽氧烷、三矽烷基胺、二矽烷、三矽烷、式（HI) 之烧氧基秒烧： 16 200813245 (III】） 至6個碳原子之直鍵
SiHx(OR3)4_x， 其中：〇Sx$3且R3表示具有 或支鏈烴基； 式（III2)之矽烷醇衍生物：
Si，)x(〇RVx (1„2) 其令：15x^3且Μ表示具有4 6個碳原子之直鍵 或支鏈烷基，較佳為Si (0H) (OR4)3且更佳為si (〇h) (0tBu)3 ；
式（III3)之胺基碎烧衍生物：
SiHx(NR5R6)“ (III3) 其中：〇 S X $ 3,且R5及R6相同或不同且獨立地表 示氫原子或具有1至6個碳原子之直鏈或支鏈烷基，較佳 為 SiH (NMe2)3 (THDMAS)、SiH2 (NHtBu)2 ( BTBAS )、SiH2 (NEt2)2 (BDEAS)及其混合物； 2 物，.諸如三甲基鋁[A1 (CH3)3]、氫化二甲基紹 [A1H (CH3)2]、式（ιν!)之烷氧基鋁烷： A1R8X (〇R7)3-x (IVi) 其中·0$Χ$3，且R7表示具有1至6個碳原子之直 鏈或支鏈烷基，且R8與R7相同或不同且表示氫原子或較 佳A1R9R10(OR7)，其中R9及Rl〇相同或不同且獨立地表示 具有1至6個碳原子之直鏈或支鏈烷基，最佳為aim^ (OiPr) ； 2 式（IV2)之酸胺基1呂烧（arnid〇alane): AlRnx (NR12R13)3 x 17 200813245 其中：〇Sx$3,且反^及以3相同或不同且表示氫原 子或具有1至6個碳原子之直鏈或支鏈烷基，且^^與汉7 相同或不同且表示氫原子或具有i至6個碳原子之直鏈或 支鏈烷基； 丝_衍生物，諸如 Ta (0Me)5、Ta (〇Et)5、Ta (NMe2)5、 Ta(NEt2)5、1^(湘认、式（Vi)之钽衍生物：
Ta (OR14)4 [0-C (R15) (R16)-CH2-OR17]
八中R R 、尺6及R17相同或不同且獨立地表示氡 原子或具有1至6個碳原子之直鏈或支鏈烷基，較佳為U (OEt)4 (〇CMe2CH2-〇Me) (TAT-DMAE);式（V2)之鈕衍 生物：
Ta (OR18)4 [O-C (R19) (R20)-CH2-N (R21) (R22)] 其中R18、R19、R2〇、汉2!及R22相同或不同且獨立地表 示氫原子或具有1至6個碳原子之直鏈或支鏈烷基；式 (V3 )之鈕衍生物··
Ta 卜 NR24) (NR25R26)3 ( v } 其中R24、R25及R26相同或不同且獨立地表示氫原子 或具有1至6個碳原子之直鏈或支鏈烷基； 起Jt±.物，諸如則（〇Me)5、Nb (OEt)5、Nb (NMe2)5 ' Nb (NEq)4、Nb (NEtJ5、式（VI〗）之銳衍生物：
Nb (OR27)4 (O-C (R28) (R29).CH2-OR30) ( V、） 其中r27、r28、r29& R3〇相同或不同且獨立地表^氫 原子或具有1至6個碳原子之直鏈或支鏈烷基，較佳為Nb (OEt)4 (〇CMe2CH2-OMe) (NBT-DMAE);式（vi2)之鈮衍 200813245 生物： (VI2)
Nb (0R31)4[0-C (R32) (R33)-CH2-N (R34) (R35)] 其中R31、R32、R33、R34及R35相同或不同且獨立地表 示氫原子或具有1至6個碳原子之直鏈或支鏈烷基；式 (VI3)之鈮衍生物： (VI3)
Nb (= NR36) (NR37R38)3 其中R36、R3?及r38相同或不同且獨立地表示氫原子 或具有1至6個碳原子之直鏈或支鏈烧基；
麵__系衍生物.二諸如銃衍生物、釔衍生物、鈽衍生物、 镨（praseodinum)衍生物、釓衍生物、鏑衍生物、铒衍生 物、鑭衍生物、具有至少一個β_二酮酸酯基（diket〇nate) 配位基或至少-個經—或多個具有！ i 6個碳原子的直鍵 或支鏈烷基取代之環戊二烯基配位基之衍生物： 二仏*屬衍生物’諸如具有至少一個β _二酮酸酯基配 位基或至少一個視情況經一或多個具有i至6個碳原子的 直鏈或支鏈烷基取代之環戊二烯基配位基之鋰（Sr)、鋇 (Ba)、鎮（Mg)、鈣（Ca)或辞（Zn)衍生物； 甚生物丄諸如鎢(W)、鉬（Mo)、姶（Hf) 或鍅（Zr)衍生物，例如烷氧基衍生物、胺基衍生物或含 該等物質之加成物，應瞭解該等衍生物並非如上文所定義 之式（II )化合物。 根據另一特定具體實例，如上文所定義之方法包含： -步驟d)，其中在步驟c)之前將至少一種含M1金 屬之式（II)前驅物及必要時至少—種含m2金屬之前驅物 19 200813245 與至少一種反應物物質混合。 在本發明之上下文中’關於基於目標金屬之薄膜來選 擇該至少一種反應物物質。 根據另一具體實例’該反應物物質為氧源且更特定言 之為氧氣（〇2)、含氧自由基0·或〇Η·(例如，由遠端; 聚產生）、臭氧（〇3)、濕氣（h2〇)&H2〇2及其混合物。 根據另一具體實例，該反應物物質為氮源且更特定言 之為氮氣（N2)、含氮自由基（例如N·、nh,、NH , > 、 ♦氨（簡3)、肼（則2丽2)及其燒基或芳基衍生物丄其混 合物。 根據另一具體實例，該反應物物質為氮源及氧源兩者， 且更特定言之為助、助2、咐、乂〇5、〜〇4及其混合物。 視所需N/O比率而定，必要時用於如上文所定義之方 中之反應物物質可為氧源、氧源混合物及氮源混合物、 氧及氮源或其混合物。 # 入根據本發明之另一具體實例，若基於目標金屬之薄膜 有炭例如（但不限於）金屬碳化物或金屬碳氮化物時， 、 種反應物物質為碳源，更特定言之為甲烷、乙烷、 丙烷丁力元、乙烯、丙烯、第三丁烯。 入梦根據本發明之另一具體實例，若基於目標金屬之薄膜 山」如（但不限於）金屬矽化物、石夕氮化物、石夕酸鹽 ，二氮化物枯，則至少一種反應物物質為矽源，諸如·· 夕氧烷、二矽烷基胺、二矽烷（Si2H6 )、三矽烷 ^ )、如上玄％ 上文所疋義之式（ΙΠι) 、（IIl2)或（IIl3) 20 200813245 之烷氧基矽烷（例如 SiH (NMe2)3 (TriDMAS)、SiH2 (NHtBu)2 (BTBAS)、SiH2(NEt2)2(BDEAS))及其混合物。 根據另一特定具體實例，如上文所定義之方法包含： 步驟df )，其中在反應腔室中將至少一種含M1金屬 之式（II )前驅物及必要時至少一種含M2金屬之前驅物與 至少一種反應物種混合。
將至少一種含M1金屬之式（Π )前驅物及必要時至少 一種含M2金屬之前驅物與至少一種反應物種引入反應腔 室中之模式通常視將薄膜沈積於基板上之模式而定。通 常’同時將含金屬之前驅物及反應物種引入化學氣相沈積 方法中，或相繼將其引入原子層沈積方法中，或根據若干 組合將其引入（例如）脈衝改良原子層沈積方法中，其中 將至少一種含M1金屬之式（π )前驅物及必要時至少一種 含M2金屬之前驅物一起引入一脈衝中，且將至少一種反 應物種引人另-脈衝中；或將其弓丨人脈衝化學氣相沈積方 法中’其中藉由脈衝引入至少一種含^金屬之式（π)前 驅物及必要時至少一種+ Μ2金屬之前驅物，且持續引入 至少一種反應物種。 具體實例，使至少一種反應物種經 電漿系統且分解為自由基。 根據本發明之另一 過位於反應腔室遠端之 根據另一具體實例，如卜-V α 一 Μ 貝』如上文所定義之方法之步驟（b) 係由下列步驟組成：步驟f ，將至少一種第一含金屬 之式（II )前驅物與下列前 卜到别驅物中之至少一種第二前驅物 混 a 在一起：m1 (NMe 彳、αλί 2)4 M (聰2)4、M1 (NMeEt)4、M1 21 200813245 (mmp)4 μ (〇tBu)4、M1 (〇tBu)2 (mmp)2 及其混合物；及 步驟（匕），蒸發該混合物。 更特定具體實例，本發 沈積 —^ 卜丁、肿J 斯上人广疋我 匕έ式（I )化合物的含金屬介電膜之方法，其中含以1 金屬之别驅物為式（II i )前驅物： (R2tCp) Ml [N (R39) (R4〇)]3 (11〇, 其對應於式（II)，其中乂=〇,2=1且以，表示基團N (R39) (R )其中R及R40相同或不同且獨立地表示氫原子；
具有1至4個碳原子之直鏈或支鏈烷基；烷基矽烷基，其 中該烧基為直鏈或支鏈且具有1至4個碳原子；二烷基矽 烧基’其中各烧基彼此相同或不同，為直鏈或支鏈且具有 1至4個碳原子；或三烷基矽烷基，其中各烷基彼此相同 或不同，為直鏈或支鏈且具有1至4個碳原子。 根據一更特定具體實例，本發明係關於如上文所定義 沈積包含式（I!)化合物的含金屬介電膜之方法： M1〇2 ( 1\ ) 其對應於式（I)，其中a = 0，b = 2且c = 0，其中含 金屬之式（II )前驅物係選自由下列各物組成之群： HfCp2Cl2、Hf (MeCp)2 Me2、HfCp (MeCp) Cl2、Hf (MeCp)2
Cl2、HfCp (MeCp) Me2、Hf (EtCp) (MeCp) Me2、Hf (EtCp)2 Me2、Hf (MeCp)2 (CO)2、ZrCp2Cl2、Zr (MeCp)2 Me2、ZrCp (MeCp) Cl2、Zr (MeCp)2 Cl2、ZrCp (MeCp) Me2、Zr (EtCp) (MeCp) Me2、Zr (EtCp)2 Me2、Zr (MeCp)2 (CO)2、Zr (MeCp) (NMe2)3、Zr (EtCp) (NMe2)3、ZrCp (NMe2)3、Zr (MeCp) 22 200813245 (NEtMe)3、Zr (EtCp) (NEtMe)3、ZrCp (NEtMe)3、Zr (MeCp) (NEt2)3、Zr (EtCp) (NEt2)3、ZrCp (NEt2)3、Zr (iPr2Cp) (NMe2)3、Zr (tBu2Cp) (NMe2)3、Hf (MeCp) (NMe2)3、Hf (EtCp) (NMe2)3、HfCp (NMe2)3、Hf (MeCp) (NEtMe)3、Hf (EtCp) (NEtMe)3、HfCp (NEtMe)3、Hf (MeCp) (NEt2)3、Hf (EtCp) (NEt2)3、HfCp (NEt2)3、Hf (iPr2Cp) (NMe2)3、Hf (tBu2Cp) (NMe2)3及其混合物。 根據一更特定具體實例，本發明係關於如上文所定義 沈積包含式（12)化合物的含金屬介電膜之方法： M1。，Nc5 ( 12) 其對應於式（I)，其中 a = 0，1.5$b£2_5 且 0<c£0.5, 其中含金屬之式（II )前驅物係選自由下列各物組成之群： HfCp2Cl2、Hf(MeCp)2Me2、HfCp (MeCp) Cl2、Hf(MeCp)2 Cl2、HfCp (MeCp) Me2、Hf(EtCp') (MeCp) Me2、Hf(EtCp)2 Me2、Hf (MeCp)2 (CO)2、ZrCp2Cl2、Zr (MeCp)2 Me2、Zr (MeCp)2 Cl2、ZrCp (MeCp) Me2、Zr (EtCp) (MeCp) Me2、 Zr (EtCp)2 Me2、Zr (MeCp)2 (CO)2、Zr (MeCp) (NMe2)3、Zr (EtCp) (NMe2)3、ZrCp (NMe2)3、Zr (MeCp) (NEtMe)3、Zr (EtCp) (NEtMe)3、ZrCp (NEtMe)3、Zr (MeCp) (NEt2)3、Zr (EtCp) (NEt2)3、ZrCp (NEt2)3、Zr (iPr2Cp) (NMe2)3、Zr (tBu2Cp) (NMe2)3、Hf (MeCp) (NMe2)3、Hf (EtCp) (NMe2)3、 HfCp (NMe2)3、Hf (MeCp) (NEtMe)3、Hf (EtCp) (NEtMe)3、 HfCp (NEtMe)3、Hf (MeCp) (NEt2)3、Hf (EtCp) (NEt2)3、HfCp (NEt2)3、Hf (iPr2Cp) (NMe2)3、Hf (tBu2Cp) (NMe2)3 及其混 23 200813245 - 合物。 根據一更特定具體實例，本發明係關於如上文所定義 沈積包含式（i3)化合物的含金屬介電膜之方法： (MS., M2a) 0b (I3) 其對應於式（I)，其中〇$a<l且c = 〇，其中含金 屬之式（II)前驅物係選自由下列各物組成之群·· HfCp2Cl2、
Hf (MeCp)2 Me2、HfCp (MeCp) Cl2、Hf (MeCp)2 Cl2、HfCp (MeCp) Me2、Hf (EtCp) (MeCp) Me2、Hf (EtCp)2 Me2、Hf _ (MeCp)2 (CO)2、ZrCp2Cl2、Zr (MeCp)2 Me2、ZrCp (MeCp) Cl2、Zr (MeCp)2 ci2、ZrCp (MeCp) Me2、Zr (EtCp) (MeCp) Me2、Zr (EtCp)2 Me2、Zr (MeCp)2 (CO)2、Zr (MeCp) (NMe2)3、 Zr (EtCp) (NMe2)3、ZrCp (NMe2)3、Zr (MeCp) (NEtMe)3、 Zr (EtCp) (NEtMe)3、ZrCp (NEtMe)3、Zr (MeCp) (NEt2)3、 Zr (EtCp) (NEt2)3、ZrCp (NEt2)3、Zr (iPr2Cp) (NMe2)3、Zr (tBu2Cp) (NMe2)3、Hf (MeCp) (NMe2)3、Hf (EtCp) (NMe2)3、 HfCp (NMe2)3、Hf (MeCp) (NEtMe)3、Hf (EtCp) (NEtMe)3、 • HfCp (NEtMe)3、Hf (MeCp) (NEt2)3、Hf (EtCp) (NEt2)3、HfCp (NEt2)3、Hf (iPr2Cp) (NMe2)3、Hf (tBu2Cp) (NMe2)3，且含 M2金屬之前驅物較佳係選自如上文所定義之石夕衍生物或其 鍺同系物、钽衍生物、鑭系衍生物及鎂衍生物。 根據一更特定具體實例，本發明係關於如上文所定義 沈積包含式（I4 )化合物的含金屬介電膜之方法： (MS.a M2a) Ob Nc ( I4) 其對應於式（I)，其中〇Sa<l且0<cS0.5，其中 24 200813245 含金屬之式（ιι)前驅物係選自由下列各物組成之群： HfCp2Cl2、Hf (MeCp)2Me2、HfCp (MeCp) Cl2、Hf (MeCp)2 Cl2、HfCp (MeCp) Me2、Hf (EtCp) (MeCp) Me2、Hf (EtCp)2 Me2、Hf (MeCp)2 (CO)2、ZrCp2Cl2、Zr (MeCp)2 Me2、ZrCp (MeCp) Cl2、Zr (MeCp)2 Cl2、ZrCp (MeCp) Me2、Zr (EtCp) (MeCp) Me2、Zr (EtCp)2 Me2、Zr (MeCp)2 (CO)2、Zr (MeCp) (NMe2)3、Zr (EtCp) (NMe2)3、ZrCp (NMe2)3、Zr (MeCp) (NEtMe)3、Zr (EtCp) (NEtMe)3、ZrCp (NEtMe)3、Zr (MeCp) (NEt2)3、Zr (EtCp) (NEt2)3、ZrCp (NEt2)3、Zr (iPr2Cp) (NMe2)3、Zr (tBu2Cp) (NMe2)3、Hf (MeCp) (NMe2)3、Hf (EtCp) (NMe2)3、HfCp (NMe2)3、Hf (MeCp) (NEtMe)3、Hf (EtCp) (NEtMe)3、HfCp (NEtMe)3、Hf (MeCp) (NEt2)3、Hf (EtCp) (NEt2)3、HfCp (NEt2)3、Hf (iPr2CP) (NMe2)3、Hf (tBu2CP) (NMe2)3 ’含m2金屬之前驅物較佳係選自如上文所定義之 秒竹生物或其錯同糸物、组衍生物、鋼系衍生物及鎂衍生 物，且將至少一種含氧前驅物及至少一種含氮前驅物引入 反應器中。 根據另一具體實例，本發明係關於如上文所定義之式 (II )化合物之用途，其係用以製造更特定言之用於積體 電路之介電膜，或用以製備用於隨機存取記憶體（Rand〇m
Access Memories)之金屬絕緣體金屬（Mim)架構。 根據另一具體實例，本發明係關於式（Πι)化合物： (R2tCp) μ1 [N (R39) (R40)]3 (Πι) 其對應於式（II )，其中x = 0, z = i且R，表示基團N (R39) 25 200813245 (R )，其中R39及相同或不同且獨立地表示氫原子； 具有1至4個碳原子之直鏈或支鏈烷基；烷基矽烷基，其 中該烷基為直鏈或支鏈且具有！至4個碳原子；二烷基矽 烷基，其中各烷基彼此相同或不同，為直鏈或支鏈且具有 1至4個碳原子；或三烷基矽烷基，其中各烷基彼此相同 或不同，為直鏈或支鏈且具有1至4個碳原子。 根據一特定具體實例，本發明係關於如上文所定義之 式（II!)化合物，其中R2、R39及R4〇相同或不同且獨立 _ 地表示選自曱基、乙基、丙基、異丙基、丁基、異丁基、 第一丁基及第三丁基之基團，且更特定言之係關於下列化 合物：
Zr (MeCp) (NMe2)3、Zr (EtCp) (NMe2)3、ZrCp (NMe2)3、 Zr (MeCp) (NEtMe)3、Zr (EtCp) (NEtMe)3、ZrCp (NEtMe)3、 Zr (MeCp) (NEt2)3、Zr (EtCp)(NEt2)3、ZrCp (NEt2)3、Zr (iPr2Cp) (NMe2)3、Zr (tBu2Cp) (NMe2)3、Hf (MeCp) (NMe2)3、Hf (EtCp) (NMe2)3、HfCp (NMe2)3、Hf (MeCp) 鲁 （NEtMe)3、Hf (EtCp) (NEtMe)3、HfCp (NEtMe)3、Hf (MeCp) (NEt2)3、Hf (EtCp) (NEt2)3、HfCp (NEt2)3、Hf (iPr2Cp) (NMe2)3、Hf (tBu2Cp) (NMe2)3。 根據一更特定具體實例，本發明係關於下列化合物：
Zr (EtCp) (NMe2)3、Zr (MeCp) (NMe2)3、ZrCp (NMe2)3、 Hf (EtCp) (NMe2)3、Hf (MeCp) (NMe2)3 及 HfCp (NMe2)3。 熟習此項技術者應瞭解，上述金屬-有機化合物可用於 除氣相沈積方法以外之任何其他應用，諸如催化劑或需要 26 200813245 使用金屬-有機化合物之任何其他工業方法或應用。 根據另一具體實例’本發明係關於一種用於製備如上 文所定義之式（)化合物之方法，其包含： 免其係由藉由使MWU與（R2tCp) Na反應來製備 式（VIIO化合物組成， (R2tCp) Μπΐ3 ( νΠι) 其中Μ1、R2及t係如上文關於式（η )所定義；
免丄其係由使步驟1中所製備之式（VIIJ化合 物與nh(r39)(r，反應以產生式（ΪΙι)化合物組成。Q 根據一最終具體實例，本發明係關於如上文所定義之 下列式（II)化合物：
Hf (EtCp)2 Me2、Zr (MeCp)2 Me2 或 Zr (EtCp)2 Me2。 【實施方式】 下列實例說明本發明之各種具體實例，而非對其進行 限制。 丁 置例I :沈積金屬氣化物膜τν^ΓΚ，其中μ1妨4 . ^ 所欲沈積之膜包含式（1)化合物，其中a = 〇, b = 2 c = 〇 〇 為使該膜沈積於晶圓表面或沈積於深溝槽中以製造用 於DRAM之MIM結構，需要蒸發如步驟（b )所定義之⑷ 至屬源且將其引入反應器中（較佳為铪或鍅），將氧源（較 =為濕氣、氧氣或臭氧）注入該反應器中，使產物在適當 溫度（較佳在150。〇與35(rc之間）及壓力（較佳在25匕 27 200813245 2 1GGG Pa W )下反應’歷經在基板上達成薄膜沈積或 藉由ALD或脈衝CVD方法（需要連續脈衝注入金屬源以 使氧化物規則沈積於溝槽中，從而逐漸填滿此溝槽且使介 電膜不含空隙，且因此使電容器介電膜無缺陷）來填滿深 溝槽所需之持續時間。 該介電膜應具有所要最終組成（本文中，b值基本上 在2左右變化，從而改變前驅物與氧源之比率）。 • 根據下列三個選項a、b或c來選擇式（„)化合物類 型之三個實例： Ο 式（π)化合物係選自 Zr(MeCp)2Me2、Zr(EtCp)2
Me2、Hf (MeCp)2 Me2 及 Hf (MeCp)2 Me2。 呈液體形式之分子之傳遞通常係藉由將惰性氣體 (N2、He、Ar··.)鼓泡至該液體中且將惰性氣體加液態氣 體混合物提供至反應器中來進行。 b )式（II )化合物係選自Zr (2,心Me2〇p)2仏2及Hf _ (2,4-Me2〇p)2 Me2。 c )式（II )化合物係選自 Zr (MeCp) (2,‘Me2〇p) Μ。 及 Hf (MeCp) (2,4-Me2〇p) Me2。 氧源較佳應為（但不限於）氧氣（〇2 )、氧自由基（例 如Ο或OH，諸如由遠端電漿系統產生之自由基）、臭氧、 NO、N20、N02、濕氣（H20 )及 H，〇。 關於其自身之沈積過程，可將反應物同時（化學氣相 沈和）相^ (原子層沈積）或以不同組合（一例子係將 金屬源及另一金屬源一起引入一脈衝中，且將氧氣引入另 28 200813245 積];另—選項係持續引入氧氣及/ (脈衝化學氣相沈積））引入反應 :沈豬合μ Λ叙h 所欲沈積之膜包含式⑴化合物， 及C不等於0。 、τ 實施例I所給出之戶斤古次
有1訊均可應用於此實施例π 中，除了需要將氮引入反應器中之外。 氮應選自氮源，該氮湄备 Α你係選自包含氮氣（ν2 )、氨、 肼及烧基衍生物、含氮自由基（例如Ν·、ΝΗ·、ΝΗ2·)、 NO、N20、NO〗或其類似物之群。 氧化物膜，:Μ!妨接 為_财或Zr且Μ2鲮隹A1 所欲沈積之膜包含式（〇化合物，其中a # 0, b # 〇 且 c = 0 〇
一脈衝中[改良原子層沈 或藉由脈衝引入金屬源 器中。 且b 貫施例i所給出之所有資訊均可應用於此實施例ΠΙ 中，除了額外需要Μ2金屬源之外。 亦將含Μ之前驅物引入反應器中以產生金屬之μ2 源。此含Μ之别驅物源較佳應為·· a) 矽（或鍺）源，例如 Si (〇H)(〇tBu)3、SiH (NMe2)3 (TriDMAS)、SiH2 (NHtBu)2 (BTBAS)及 SiH2 (NEt2)2 (BDEAS)； b) 鋁源，例如A1Me2 (〇iPr);或 29 200813245 c )组（或銳）源，例如 Ta (OMe)5、Ta (OEt)5 及 Ta (〇Et) (OCMe2CH2-OMe) (TATDMAE) o
本發明係、關於使用ALD、CVD、MOCVD、脈衝cVD 方法在反應中將式I之介電膜沈積於諸如晶圓之載體 上。 寛瘅例IV :沈積M1M2金屬氮氣化物膜，糞中Ml輕 隹為Hf或Zr且M2趣钱為Si或Ai 所欲沈積之膜包含式（I)化合物，其中a # 〇，b # 〇 •且c关0。 實施例III所給出之所有資訊均可應用於此情形中， 除了需要將氮氣引入反應器中之外。 氮源應選自包含氮氣（n2 )、氨、肼及烷基衍生物、 含氮自由基（例如Ν·、ΝΗ·、NH2· ) 、NO、Ν,Ο、NO之 群。 JL施例v :合成（乙基環戊二媾基）春（二甲基路 鐘，Zr (EtCpWNMq」 % 以3個步驟製備Zr (EtCp) (NMe2)3。 第一步驟係藉由使（EtCp) Na於ZrCl4上反應來製備 Zr(EtCp)Cl3 〇 第二步驟係使LiNMe2與Zr (EtCp) Cl3反應以產生Zr (EtCp) (NMeD3。所得化合物藉由蒸餾來純化。總產率為 35%。 已發現（乙基環戊二烯基）參（二曱基胺基）锆為穩 定液態淡黃色化合物。 30 200813245
Zx(EtCp) (NMe2h _之 TGA 分析 將熱解重量分析設備儲存於濕氣及氧氣含量均經維持 低於i PPmv之氬氣手套箱中。藉由將35叫樣品置於銘 坩鍋中來執行熱解重量分析。隨後加熱樣品，以i〇ec/min 將溫度自35T：逐漸上升至赋。監測隨坩鍋溫度變化之 質量損失。在26(TC之完全蒸發溫度下，殘餘含量為26%。 所得圖式在圖1中。 fJl 例 VI:使用 Zr 支進行 Zr〇二嫌 m 子層沈葙 — 將Zr (EtCp) (NMe2)3儲存於容器中。在9〇。〇下加熱容 為且將N2用作載氣，流量為50 scem。將容器中之壓力控 制在50托。將A用作氧源。在35〇t下加熱基板。在^ 一步驟期間，在2 s内將Zr (EtCp) (NMe2)3引入反應腔室 中之後’作為弟一步驟來執行5 s之Ν2淨化。作為第三 步驟，隨後在2 s内將〇3脈衝引入反應腔室中，繼而作為 φ 第四步驟來執行2 s之A淨化。將所有四個步驟重複1〇〇 次以獲得Zr〇2膜。獲得自我限制型原于層沈積。 可以Hf類似物來執行類似實驗。亦可以h2〇作為氧 源來執行類似實驗。 复為例VII :使用Zr (EtCp) 來進行ZrO,之 —-_ 一 機化學氩相沈赡 — 將Zr (EtCp) (NMeA儲存於容器中。在9(rc下加熱容 =且將N〗用作載氣，流量為5 0 seem。將容器中之壓力控 制在50托。在反應腔室中將Zr (EtCp) (NMe2)3與〇2/N2氣 31 200813245 體混合物混合。在500°C下加熱基板。將反應腔室内之壓 力設定為10托。獲得鍅氧化物膜。 可以Hf類似物來執行類似實驗。 實施例 VIII :比較 Zr (EtCp) (NMeJ:及 Zr iNEtM% 熱行為 在類似條件下，對 Zr (EtCp) (NMe2)3 及 Zr (NEtMe)4 執行熱解重量分析。將熱解重量分析設備儲存於濕氣及氧 _ 氣含量均經維持低於1 ppmv之氬氣手套箱中。藉由將35 mg 樣品置於紹堆鍋中來執行熱解重量分析。隨後加熱樣品， 以l〇°C/min將溫度自35它逐漸上升至40(rC。監測隨坩鍋 溫度變化之質量損失。以閉杯式組態將穿孔盤（〇 8 ) 置於含有金屬-有機化合物之坩鍋中以減緩蒸發。其表明在 較鬲溫度下具有熱穩定性。結果表明Zr (EtCp) (νμ~)3比 心（NEtMe)4更具熱穩定性，從而使其更適用作氣相前驅 物。結果顯示於圖2中。 • 之合成及熬杆1 藉由使1莫耳HfCl4於EtCpNa上反應易於獲得Hf (EtCp)2 Cl2。 隨後，藉由在-20°c下將2莫耳LiMe緩慢添加於i莫 2 Hf (EtCp)2 Cl2上且增加溫度直至而獲得(价 Μ=。藉由蒸餾使所獲得之透明液態Hf (EtCp)2 與uci 及岭劑分離。在真空條件下進行Hf (EtCp)2 之Τ(}α分 析起始質量為約3〇mg，留下1〇%殘餘物。（見圖3) *^L^LgjL(EtC為也心i行HfO,之原子 32 200813245 層沈精 此實施例係關於給氧化物膜之製造。將石夕晶圓安置於 周緣具有加熱器之沈積腔室巾，且使所要膜形成於石夕晶圓 表面上：以泵排空腔室。將此情形所涉及之金屬前驅物二 曱基二茂铪(dimethylhafnocene)刪、（EtCp)2儲存於經加 由使氮氣流經该液化材料來傳送液體容器中之 。經質量流量控制器將氮氣傳送至蒸發器中。Hf (Etcp^ Me2蒸氣由氮氣載運且一起被供給至腔室中或當將前驅物 引入反應裔中之閥門閉合時，轉向旁路管線。亦經由質量 熱之液體容器中。將氮氣用#Hf (EtCp)2心之載氣。藉
流量控制器將氧氣/臭氧氣體混合物（氧化劑）供給至腔室 中，或供給至旁路管線。從不將一側之氧氣/臭氧與另一侧 之Hf (EtCp)2 Me2 —起引入以避免高可能性CVD反應發 生。其通常依次引入，各反應物脈衝均間隔著僅將乂引入 腔室中之脈衝時間。 使用所述工具’在下列條件下以約〇·7 A/週期產生給 氧化物膜： 壓力=3托，溫度=350°C，Hf (EtCp)2 Me2流動速率=〇·5 seem，〇2流動速率=loo sccm，流動速率^ 8 sccm，>^2流 動速率=100 seem。 以實施例形式給出所得膜之歐傑（Auger )分佈況（見 圖4)。 【圖式簡單說明】 圖1為Zr(EtCp)(NMe2)3之熱解重量分析； 33 200813245 圖2為顯示Zr(EtCp)(NMe2)3比Zi* (NEtMe)4更加熱安 定的圖式， 圖 3 為 Hf(EtCp)2Me2i TGA 分析；及 圖4為根據本發明所得膜之歐傑（Auger)分佈。 【主要元件符號說明】 無
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Claims (1)

  1. 200813245 十、申請專利範固： 1 · 一種將含至少一 方法，該介電膜包含式 (MlI-a M2J 〇b Ν〇5 其中： 種金屬之介電膜沈積於一基板上之 (1 )化合物： (I)， 〇 < a < 1 ; 0 < b S 3，較佳 〇 < c < 1 ;
    M1表示選自給（Hf)、錯（ζ〇及鈦（Ti)之金屬; M2表示選自下列各物 屬原子·鎖（Mg)、鈣（Ca)、 鋅（Zn)、硼（B )、鉋 f Δ 〗、h , 、（Α1)、錮（Ιη)、矽（Si)、鍺 (Ge)、錫（Sn)、銓（Hf)、錯（zr)、欽⑺）、叙
    1,5 ^ b < 2.5 ； 、（V)、rt(Nb)、纽（Ta);及鑭系原子，更特定言之 為銳（Sc )、紀（Y)及鑭（La)，及稀土金屬原子· 該方法包含下列步驟： 步驟a ):提供一基板於一反應腔室中； 步驟b) ··蒸發至少一種含M1金屬之★ Γ ττ、， 喝 < 式（Π)前驅物 以形成第一氣相金屬源： (R!y〇p)x (R2tCp)z M1 R\.x.z (II) 其中： M1係如上文所定義； 0 $ x S 3，較佳 X = 0 或 1 ; 0 S z S 3，較佳 z = 1 或 2 ; 35 200813245 1 <(x + z) < 4 ； 〇 S y S 7，較佳 y = 2; 〇 s t $ 5，較佳 t = 1 ; (R^Op )表不未經取代或經一或多個Rl基團取代之 戊二烯基（Op)配位基，y表示該戊二烯基配位基上取代 性R1基團的數目； (R2tCp )表示未經取代或經一或多個R2基團取代之 裱戊二烯基（Cp)配位基，t表示該環戊二烯基配位基上 取代性R1基團的數目； ® R1及R2相同或不同，且係獨立地選自由下列各物組 成之群：氯；具有1至4個碳原子之直鏈或支鏈烷基；… 烷基胺基，其中該烷基為直鏈或支鏈且具有1至4個碳原 子，N，N-二烷基胺基，其中各烷基彼此相同或不同，為直 鍵或支鏈且具有1至4個碳原子；具有1至4個碳原子之 直鏈或支鏈烷氧基；烷基矽烷基醯胺基；脒基；及幾基； R’表示獨立地選自由下列各物組成之群之配位基：氫、 _ 氣氣、>臭或職原子，具有1至4個碳原子之直鏈或支鏈 烷基；N-烷基胺基，其中該烷基為直鏈或支鏈且具有}至 4個碳原子；N，N-二烷基胺基，其中各烷基彼此相同或不 同’為直鏈或支鏈且具有1至4個碳原子；具有1至4個 石厌原子之直鏈或支鏈烧氧基；烧基石夕燒基胺基，其中該炫 基為直鏈或支鏈且具有1至4個碳原子；二烷基矽烷基胺 基’其中各烧基彼此相同或不同，為直鏈或支鏈且具有1 至4個碳原子；三烷基矽烷基胺基，其中各烷基彼此相同 或不同，為直鏈或支鏈且具有1至4個碳原子；脎基；及 36 200813245 羰基；應瞭解，若該式（II)包含一個以上R，基團，則各 可彼此相同或不同； 視情況，步驟b’）：蒸發至少一種含M2金屬之前驅 物以形成視情況需要之第二氣相金屬源，m2係如上文所定 義； 步驟C )·將該第一氣相金屬源及該視情況需要之第 二氣相金屬源引入該反應腔室中’以促使其與該基板接 觸，從而在該基板上產生包含如上文所定義之式（1)化合 物的含金屬介電膜沈積； 其限制條件在於，若欲形成之含至少一種金屬之介電 膜包含式（Γ)化合物： u\ 〇2 2 (Γ)， 其對應於如上文所定義之式（1)，其中a = 0，b = 2 且C = 0 ;且若步驟b)中所涉及之含Ml金屬之前驅物為 式（)化合物： (R'Cp)2 M1 R、 （ir)， 其對應於如上文所定義之式（11)，其中乂 = 〇且2 = 2, 則在該式（ir)中，在兩個（R2tCp)配位基中之至少一者 中 t > 〇 〇 2.如:請專利範圍第1項之方法，其中將該蒸發步驟 b )及该瘵發步，驟b’）組合於該兩個氣相金屬源之一個蒸 發步驟b’’）中。 3:如申請專利範圍第i或2項之方法，其中該含…金 屬之前驅物係選自由下列各物組成之群： 37 200813245 ♦衍生物或其鍺同系物，諸如： 二矽氧烷、三矽烷基胺、二矽烷、三矽烷、式（Πΐι) 之烧氧基碎烧： SiHx (OR3)4.x, (ΠΙι), 其中：〇$χ$3且R3表示具有1至6個碳原子之直鍵 或支鏈烴基； 式（m2)之矽烷醇衍生物：
    Si(〇H)x(OR，4_x (III2), 其中：1 S X S 3且R4表示具有i至6個碳原子之直鍵 或支鏈烷基，較佳為Si (OH) (〇R4)3且更佳為Si (〇H) (OtBu)3 ; 式（III3)之胺基石夕烧衍生物： siH“NR5R6)“ （III3)， 其中·· 0 S x S 3，且R5及R6相同或不同且獨立地表 示氫原子或具有1至6個碳原子之直鏈或支鏈烷基，較佳 為 SiH (NMe2)3 (TriDMAS)、SiH2 (NHtBn)2 (BTBAS)、SiH2 (NEt2)2(BDEAS)及其混合物； 鱼JL生物’諸如三甲基銘[A1 (CH3)3]、氫化二甲基鋁 [A1H (CH3)2]、式（IVl)之烷氧基鋁烷·· A1R8x (OR7)3 x 3·χ (IV】）， 其中：0<χ<3，主一 θ 丄 1 -- 丑R表不具有1至ό個碳原子之直 鏈或支鏈烧基’且R7相同或不同且表示氯原子，或 較佳為AIR9R，R7)，其+ R9& R1。相同或不同且獨立地 表示具有1至6個碳原子之直鏈或支鏈烷基，最佳為紙 38 200813245 (OiPr)； 式（IV2)之龜胺基鋁烷： A1R11X (NR12R13)3.x (IV2)， 其中·〇£χ$3，且R12及R13相同或不同且表示氫原 子或具有1至6個蚊原子之直鏈或支鏈烧基，且汉u與尺7 相同或不同且表示氫原子或具有1至6個碳原子之直鍵或 支鏈烷基； #旦衍生.物’諸如 Ta (〇Me)5、Ta (OEt)5、Ta (NMe2)5、 _ Ta (NEt2)5、Ta (NEt2)5 ;式（Vi)之鈕衍生物： Ta (OR14)4 [O-C (R15) (R16)-CH2-〇R17] ^ 其中R14、R15、R16及相同或不同且獨立地表示氫 原子或具有1至6個碳原子之直鏈或支鏈烧基，較佳為^ (OEt)4 (OCMe2CH2-OMe) (TAT-DMAE);式（γ2)之釦衍 生物： Ta (OR18)4 [O-C (R19) (R20)-CH2-N (R21) (R22)j ( γ
    其中R18、R19、R2〇、R2i及R22相同或不同且獨立地表 示氫原子或具有1至6個碳原子之直鏈或支鏈烷基；式 (V3)之鈕衍生物： Ta (= NR24) (NR25R^)3 ( V )， 其中R24、R25及R26相同或不同且獨立地表示氫原子 或具有1至6個碳原子之直鏈或支鏈烷基； 星致生物’_諸如勘（〇Me)5、Nb (OEt)5、Nb (NMe2)5、 Nb (膽2)4、Nb (NEq)5，·式（VIl )之鈮衍生物： Nb (OR27)4 (O-C (R28) (R29)-CH2-OR30) (VI!)， 39 200813245 其中R R、R及反3〇相同或不同且獨立地表示氯 原子或具有1至6個碳原子之直鏈或支鏈烷基，較佳為= (OEt)4 (〇CMe2CH2-〇Me) (NBT-DMAE);式（VI、夕力， 衍 生物： Nb (OR31)4 [O-C (R32) (R33).CH2-N (R34) (R35)] ( VI )， 其中R31、R32、R33、反34及R35相同或不同且獨立地表 示氫原子或具有1至6個碳原子之直鏈或支鏈烷基；式 (VI3)之鈮衍生物： I
    Nb (= NR36) (NR37R38)3 ( VI ) 其中R36、R37及R38相同或不同且獨立地表示氫原子 或具有1至6個瑗原子之直鏈或支鏈烧基； 系衍-生物’諸如銳衍生物、釔衍生物、鈽衍生物、 镨（praesidium)衍生物、釓衍生物或Nd衍生物、具有至 少一個β _二酮酸酯基（diketonate)配位基或至少一個視 情況經一或多個具有1至6個碳原子之直鏈或支鏈烷基取 代的環戊二烯基配位基之衍生物： 三i賈金屬_衍生物’諸如具有至少一個β -二酮酸酯基配 位基或至少一個視情況經一或多個具有〗至6個碳原子之 直鏈或支鏈烷基取代的環戊二烯基配位基之鳃（Sr )、鋇 (Ba)、鎂（Mg)、鈣（Ca)或鋅（Zn)衍生物； 甚A金屬衍生物，諸如鎢（W )、錮（Mo )、铪（Hf) 或鍅（Zr )衍生物，例如烷氧基衍生物、胺基衍生物或含 該等物質之加合物，應瞭解該等衍生物並非如上文所定義 之式（II )化合物。 200813245 4. 如申請專利範圍第丨至3項中任一項之方法，其進 一步包含： ” 八 V驟d)，其中在步驟c)之前將該至少一種含μ1 金屬之式（II)前驅物及必要時該至少一種含M2金屬之前 驅物與至少一種反應物種混合。 5. 如申請專利範圍第丨至4項中任一項之方法，其進 一步包含： 乂驟d’），其中在該反應腔室中將該至少一種含m1 孟屬之式（11)前驅物及必要時該至少一種含Μ2金屬之前 驅物與至少一種反應物種混合。 6. 如申請專利範圍第i至5項中任一項之方法，其中 ”亥步驟（b)係由下列步驟組成：步驟（，將至少 第 '一含今M i b ， 、 一 w 之式（II )鈾驅物與下列前驅物中之至少一種 第二前驅物混合在一起：M1 (NMe2)4、M1 (NEt丄、M1 (N^eEt)4、M1 (mmp)4、M1 (〇飯）4、M1 (〇tBu)2 (mmp)2 及 其此*合物；及步驟（t>2 )，蒸發該混合物。 7. 如申請專利範圍第丨至6項中任一項之方法，直 該含W金屬之前驅物具有式（II1): '、 ^R2tcP) Μ1 [N (R39) (R40)]3 ( II )， 4〇其對應於式（Π)，其中x = 〇, z = 1且R，表示基團N (R39) ()八中R39及R40相同或不同且獨立地表示氫原子； 具有1至4個碳原子之直鏈或支鏈烷基；烷基矽烷基，其 中該烧基為直鏈或支鏈且具有1纟4個碳原子；二院基石夕 烷基，其中各烷基彼此相同或不同，為直鏈或支鏈且具有 200813245 ， 1至4個碳原子；或三烷基矽烷基，其中各烷基彼此相同 或不同，為直鏈或支鏈且具有1至4個碳原子。 8 ·如申請專利範圍第1至7項中任一項之方法，其係 沈積含金屬介電膜，該介電膜包含式（L)化合物： m1〇2 (I!)， 其對應於式（I)，其中a = 0，b = 2且c = 〇，其中該 含金屬之式（II )前驅物係選自由下列各物組成之群： HfCp2Cl2、Hf (MeCp)2 Me2、HfCp (MeCp) Cl2、Hf (MeCp)2 _ C12、HfCp (MeCp) Me2、Hf (EtCp) (MeCp) Me2、Hf (EtCp)2 Me2、Hf (MeCp)2 (CO)2、ZrCp2Cl2、Zr (MeCp)2 Me2、ZrCp (MeCp) Cl2、Zr (MeCp)2 Cl2、ZrCp (MeCp) Me2、Zr (EtCp) (MeCp) Me2、Zr (EtCp)2 Me2、Zr (MeCp)2 (CO)2、Zr (MeCp) (NMe2)3、Zr (EtCp) (NMe2)3、ZrCp (NMe2)3、Zr (MeCp) (NEtMe)3、Zr (EtCp) (NEtMe)3、ZrCp (NEtMe)3、Zr (MeCp) (NEt2)3、Zr (EtCp) (NEt2)3、ZrCP (NEt2)3、Zr (iPr2Cp) (NMe2)3、Zr _2Cp) (NMe2)3、Hf (MeCp) (NMe2)3、Hf (EtCp) 修 （NMe2)3、HfCp (NMe2)3、Hf (MeCp) (NEtMe)3、Hf (EtCp) (NEtMe)3、HfCp (NEtMe)3、Hf (MeCp) (NEt2)3、Hf (EtCp) (NEt2)3、HfCp (NEt2)3、Hf (iPr2Cp) (NMe2)3、Hf (tBu2Cp) (NMe2)3及其混合物。 9 ·如申請專利範圍第1至7項中任一項之方法，其係 沈積含金屬介電膜，該介電膜包含式（12)化合物： M]〇b Nc? (l2)， 其對應於式（I)，其中 a = 0，1.5$b$2.5 且 0<c$0.5， 42 200813245 其中該含金屬之式（Π)前驅物係選自由下列各物組成之 群：HfCp2Cl2、Hf (MeCp)2 Me2、HfCp (MeCp) Cl2、Hf (MeCp)2 Cl2、HfCp (MeCp) Me2、Hf (EtCp) (MeCp) Me2、Hf (EtCp)2 Me2、Hf (MeCp)2 (CO)2、ZrCp2Cl2、Zr (MeCp)2 Me2、Zr (MeCp)2 Cl2、ZrCp (MeCp) Me2、Zr (EtCp) (MeCp) Me2、 Zr (EtCp)2 Me2、Zr (MeCp)2 (CO)2、Zr (MeCp) (NMe2)3、Zr (EtCp) (NMe2)3、ZrCp (NMe2)3、Zr (MeCp) (NEtMe)3、Zr (EtCp) (NEtMe)3、ZrCp (NEtMe)3、Zr (MeCp) (NEt2)3、Zr (EtCp) (NEt2)3、ZrCp (NEt2)3、Zr (iPr2Cp) (NMe2)3、Zr (tBu2Cp) (NMe2)3、Hf (MeCp) (NMe2)3、Hf (EtCp) (NMe2)3、 HfCp (NMe2)3、Hf (MeCp) (NEtMe)3、Hf (EtCp) (NEtMe)3、 HfCp (NEtMe)3、Hf (MeCp) (NEt2)3、Hf (EtCp) (NEt2)3、HfCp (NEt2)3、Hf (iPr2Cp) (NMe2)3、Hf (tBu2Cp) (NMe2)3 及其混 合物。 10.如申請專利範圍第1至7項中任一項之方法，其係 沈積含金屬介電膜，該介電膜包含式（13)化合物： (MS., M2a) 〇b (I3)， 其對應於式（I)，其中〇$a<l且c = 0，其中該含 金屬之式（II )前驅物係選自由下列各物組成之群·· HfCp2Cl2、Hf (MeCp)2 Me2、HfCp (MeCp) Cl2、Hf(MeCp)2 Cl2、HfCp (MeCp) Me2、Hf (EtCp) (MeCp) Me2、Hf (EtCp)2 Me2、Hf (MeCp)2 (CO)2、ZrCp2Cl2、Zr (MeCp)2 Me2、ZrCp (MeCp) Cl2、Zr (MeCp)2 Cl2、ZrCp (MeCp)Me2、Zr (EtCp) (MeCp) Me2、Zr (EtCp)2 Me2、Zr (MeCp)2 (CO)2、Zr (MeCp) 43 200813245 (NMe2)3、Zr (EtCp) (NMe2)3、ZrCp (NMe2)3、Zr (MeCp) (NEtMe)3、Zr (EtCp) (NEtMe)3、ZrCp (NEtMe)3、Zr (MeCp) (NEt2)3、Zr (EtCp) (NEt2)3、ZrCp (NEt2)3、Zr (iPr2Cp) (NMe2)3、Zr (tBu2Cp) (NMe2)3、Hf (MeCp) (NMe2)3、Hf (EtCp) (NMe2)3、HfCp (NMe2)3、Hf (MeCp) (NEtMe)3、Hf (EtCp) (NEtMe)3、HfCp (NEtMe)3、Hf (MeCp) (NEt2)3、Hf (EtCp) (NEt2)3、HfCp (NEt2)3、Hf (iPr2Cp) (NMe2)3、Hf (tBu2Cp) (NMe2)3，且該含M2金屬之前驅物較佳係選自如上文所定 義之矽衍生物或其鍺同系物、鈕衍生物、鑭系衍生物及鎂 衍生物。 11 ·如申請專利範圍第1至7項中任一項之方法，其係 沈積含金屬介電膜，該介電膜包含式（14)化合物·· (MS.a M2a) Ob Nc (I4)， 其對應於式（I)，其中〇Sa<l且0<c$0.5，其中 該含金屬之式（II )前驅物係選自由下列各物組成之群·· HfCp2Cl2、Hf (MeCp)2 Me2、HfCp (MeCp) Cl2、Hf (MeCp)2 Cl2、HfCp (MeCp) Me2、Hf (EtCp) (MeCp) Me2、Hf (EtCp)2 Me2、Hf (MeCp)2 (CO)2、ZrCp2Cl2、Zr (MeCp)2 Me2、ZrCp (MeCp) Cl2、Zr (MeCp)2 Cl2、ZrCp (MeCp) Me2、Zr (EtCp) (MeCp) Me2、Zr (EtCp)2 Me2、Zr (MeCp)2 (CO)2、Zr (MeCp) (NMe2)3、Zr (EtCp) (NMe2)3、ZrCp (NMe2)3、Zr (MeCp) (NEtMe)3、Zr (EtCp) (NEtMe)3、ZfCp (NEtMe)3、Zr (MeCp) (NEt2)3、Zr (EtCp) (NEt2)3、ZrCp (NEt2)3、Zr (iPr2Cp) (NMe2)3、Zr (tBu2Cp) (NMe2)3、Hf (MeCp) (NMe2)3、Hf (EtCp) 44 200813245 (NMe2)3、HfCp (NMe2)3、Hf (MeCp) (NEtMe)3、Hf (EtCp) (NEtMe)3、HfCp (NEtMe)3、Hf (MeCp) (NEt2)3、Hf (EtCp) (NEt2)3、HfCp (NEt2)3、Hf (iPr2Cp) (NMe2)3、Hf (tBn2Cp) (NMe2)3 ’该含。M2金屬之前驅物較佳係選自如上文所定義 之矽衍生物或其鍺同系物、钽衍生物、鑭系衍生物及鎂衍 生物’且將至少一種含氧前驅物及至少一種含氮前驅物引 入該反應器中。 12·一種如申請專利範圍第1項之式（II)化合物之用 ® 途’其係用以製造更特定言之用於積體電路之介電膜，或 用以製備用於隨機存取記憶體（Randorn Access Memories ) 之金屬絕緣體金屬（MIM )架構。 13·—種式（nj化合物， (R2tCp) Μ1 [N (R39) (R40)]3 (uj , 其對應於如申請專利範圍第丨項之式（n)，其中x = ， z = 1且R，表示基團N (R39) (R40)，其中r39及R40相同或 _ 不同且獨立地表示氫原子；具有1至4個碳原子之直鏈或 支鏈烷基；烷基矽烷基，其中該烷基為直鏈或支鏈且具有 1至4個碳原子；二烷基矽烷基，其中各烷基彼此相同或 不同，為直鏈或支鏈且具有丨至4個碳原子；或三烷基矽 烷基，其中各烷基彼此相同或不同，為直鏈或支鏈且具有 1至4個碳原子。 14.如申請專利範圍第13項之式（Πι)化合物，其中 R2、R39及R4〇相同或不同且獨立地表示選自甲基、乙基、 丙基、異丙基、丁基、異丁基、第二丁基及第三丁基之基 45 200813245 團。 1 5·如申請專利範圍第14項之式（Π!)化合物，其為： Zr (MeCp) (NMe2)3、Zr (EtCp) (NMe2)3、ZrCp (NMe2)3、 Zr (MeCp) (NEtMe)3、Zr (EtCp) (NEtMe)3、ZrCp (NEtMe)3、 Zr (MeCp) (NEt2)3、Zr (EtCp) (NEt2)3、ZrCp (NEt2)3、Zr (iPr2Cp) (NMe2)3、Zr (tBu2Cp) (NMe2)3、Hf (MeCp) (NMe2)3、Hf (EtCp) (NMe2)3、HfCp (NMe2)3、Hf (MeCp) (NEtMe)3、Hf (EtCp) (NEtMe)3、HfCp (NEtMe)3、Hf (MeCp) • (NEt2)3、Hf (EtCp) (NEt2)3、HfCp (NEt2)3、Hf (iPr2Cp) (NMe2)3、Hf (tBu2Cp) (NMe2)3。 16·如申請專利範圍第15項之式（I' )化合物，其為： Zr (EtCp) (NMe2)3、Zr (MeCp) (NMe2)3、ZrCp (NMe2)3、 Hf (EtCp) (NMe2)3、Hf (MeCp) (NMe2)3 及 HfCp (NMe2)3。 17·—種用於製備如申請專利範圍第i3至i6項中任一 項之式（Ili )化合物之方法，其包含： Φ 步# 1 ’其係由藉由使MWl4與（R'Cp) Na反應來製備 式（VIL )化合物所組成， (R2tCp) M^C13 (VII,), 其中Μ1、R2及t係如上文關於式（π )所定義； 其係由使步驟1中所製備之式（VIIi)化合 物與NH(R”）⑻❶）反應以產生式（II1)化合物所組成。 1δ.如申請專利範圍第1項之式（Π)化合物，其為： Hf (EtCp)2 Me2 . Zr (MeCp)2 Me2 Zr (EtCp)2 Me2 〇 46
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