TWI374887B - Precursors for depositing silicon-containing films and methods for making and using same - Google Patents

Precursors for depositing silicon-containing films and methods for making and using same Download PDF

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TWI374887B
TWI374887B TW098126843A TW98126843A TWI374887B TW I374887 B TWI374887 B TW I374887B TW 098126843 A TW098126843 A TW 098126843A TW 98126843 A TW98126843 A TW 98126843A TW I374887 B TWI374887 B TW I374887B
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precursor
group
carbon atoms
aminodecane
amine
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TW201006842A (en
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Hansong Cheng
Manchao Xiao
Gauri Sankar Lal
Thomas Richard Gaffney
Chenggang Zhou
Jinping Wu
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Air Prod & Chem
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
    • C07F7/02—Silicon compounds
    • C07F7/08—Compounds having one or more C—Si linkages
    • C07F7/10—Compounds having one or more C—Si linkages containing nitrogen having a Si-N linkage
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—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 inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34—Nitrides
    • C23C16/345—Silicon nitride
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
    • C07F7/02—Silicon compounds
    • C07F7/025—Silicon compounds without C-silicon linkages
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—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 inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/42—Silicides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/20—Deposition of semiconductor materials on a substrate, e.g. epitaxial growth solid phase epitaxy

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  • Engineering & Computer Science (AREA)
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  • Manufacturing & Machinery (AREA)
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  • Power Engineering (AREA)
  • Chemical Vapour Deposition (AREA)
  • Formation Of Insulating Films (AREA)

Description

1374887 六、發明說明： 發明所屬之技術領域 在本文中描述了，可用於沉積含矽薄膜的前驅物，尤其 是胺基石夕院前驅物，所述薄膜包括但不限於氮化砂、氧化 石夕、氮碳化石夕（silicon carbo-nitride)和氮氧化石夕（siiicon oxynitride)薄膜》—方面’本發明描述了胺基矽烷前驅物的 製備方法。另一方面，本發明描述了胺基矽烷前驅物在積 體電路器件的製備中用於沉積含石夕介電薄膜的用途。在這 些方面或其他方面中，胺基矽烷前驅物可以用於各種沉積 方法’包括但不限於，原子層沉積（"ALD")，化學氣相沉積 (CVD")、電漿增強的化學氣相沉積（"pEcvd")、低壓化學 氣相沉積（"LPCVD”）和大氣壓化學氣相沉積。 先前技術 含石夕介電薄膜在半導體器件或積體電路的製備中起著 重要作用。在半導體器件的製備中，化學惰性介電材料（如 氮化矽）的薄鈍化層（passive layer)可能是必需的。在所述器 件内部，一個和多個氮化矽薄層可以用作，例如，擴散掩 膜或阻擋層、氧化阻擋層、用於溝槽隔離的閘極絕緣層 inSulator)、電容器電介質、具有高介電崩潰電壓的金屬間 材料（uitermetallic material)，和/或鈍化層。氮化矽薄膜還 D 、早獨用作金屬氧化物半導體的側壁隔片，或者與氧化 夕和/或氮氧化矽電介質結合用於如Iv和ιι ν族電晶體器 件含矽電介質如氮化矽薄膜的其他應用，可以參考文獻 1374887 例如由 Gary E. McGuire 編寫的 Semic〇nductor and Process
Technology_Han_dbo〇k, Noyes Publication, New Jersey, (1988)，第 289-301 頁。 多種含矽化合物可以用作用於含矽薄膜（如氮化矽薄膜） 的前驅物》適合用作前驅物的含矽化合物的實施例包括， 矽烷、氯矽烷、聚矽氮烷、胺基矽烷和疊氮矽烷 (azidosilane)。還可以使用惰性載體氣體或稀釋劑，如但不 限於，氦氣、氫氣、氮氣等。 低壓化學氣相沉積（LPCVD)方法是半導體工業用於沉 積含矽薄膜的被廣泛接受的方法之一。使用氨的低壓化學 氣相沉積（LPCVD)可能需要高於75〇t的沉積溫度來獲得 適當的生長速率和均勻性。一般使用更高的沉積溫度來提 供改進的薄膜性能。生成氮化矽或其他含矽薄膜的更通常 的工業方法之一，是通過在熱壁反應器（h〇t waU react〇r) 中，在>750 c的溫度的低壓化學氣相沉積，使用前驅物矽 烷 '二氯矽烷和/或氨來進行。然而，使用該方法存在很多 缺陷。例如，某些前驅物如矽烷和二氯矽烷是引火的。這 會在處理和使用中產生問題。另外，由石夕院和二氣石夕院沉 積的薄膜可能包含某些雜質。例如使用二氯矽烷沉積的薄 膜可能包含某些雜質，如氯和氯化銨，它們會在沉積方法 中以副產物的形式形成。使用矽烷沉積的薄膜可能包含氫。 曰本專利6-132284描述了使用具有通式（RiR2N)nSiH4n 的有機矽烷，通過在氨或氮的存在下的電漿增強化學氣相 况積或熱化學氣相沉積形成氮化矽薄膜的方法。這些有機 5 1374887 石夕烧前驅物是第三胺，且不含nh鍵。沉積實驗在單片反 應器（single wafer reactor)中在 40CTC 和 80-100 Torr 的壓力 下進行。 參考文獻 Sorita 等 ’ Maw 幻/ieiic
Study of Low-Pressure Chemical Vapor Deposition of Si3N4
Thin Films From SiH2Cl2 and NH3) J. Electro. Chem. Soc., 第 141 卷 ’ No.l2,（1994)，第 3 505-351 1 頁，描述了 使用二 氯矽烷和氨在LPCVD製程中沉積氮化矽的方法。該方法的 主產物是胺基氯矽烷、氮化矽和氯化銨。如上所述，氯化 敍的形成可能是使用含Si-Cl前驅物的主要缺陷。氯化銨的 形成會導致’尤其是顆粒的形成和氣化敍在管的尾端以及 管道和系系統内的沉積。其中在前驅物中含有氯的方法還 可能導致NH4C1的形成。這些方法可能需要經常清潔從而 導致長的反應器停工期》 參考 Xtk 它 專，Preparation of Silicon Nitride with Good Interface Properties by Homogeneous Chemical Vapour Deposition, Chemtronics, 1989,第 4 卷，Dec.,第 230-34頁，描述了使用石夕烧和氨通過均勻CVD方法，在 500-800C的氣體溫度同時保持200-500 的基材溫度沉積 氮化妙的方法。如上所述，使用石夕貌作為前驅物，可能會 在薄膜中引入氫雜質。 參考文獻 J. M. Grow 等，GVowi/ι Characterization of Low Pressure Chemically Vapor Deposited Si3N4 Films from (C4H9)2SiH2 and NH3, Materials 1374887
Letters，23,（1995)，第 187-193 頁，描述 了通過 LPCVD 方 法，使用600-700°C的溫度，使用二第三丁基矽烷和氨沉積 氮化矽的方法。沉積的氮化矽薄膜被約10原子重量％的碳 雜質污染。 參考文獻 W-C. Yeh，R. Ishihara，S. Moishita，和 M. Matsumura，Japan. J. Appl. Phys.，35,（1996)，第 1509-1512 頁’描述了使用六氣二矽烷和肼在接近350°C的低溫沉積 矽-氮薄膜。該薄膜在空氣中不穩定並緩慢轉換成矽-氧薄 參考文獻 A. K. Hochberg 和 D. L. O’Meara, Diethylsilane as a Silicon Source for the Deposition of Silicon Nitride and Silicon Oxynitride Film By LPCVD, Mat.
Res. Soc_ Symp. Proc，.第 204 卷，（1991)，第 509-514 頁，公 開了使用二乙基石夕烧和氨以及氮氧化物通過LPCVD形成 氮化矽和氮氧化矽薄膜。所述沉積在650-700°C的溫度範圍
中進行。所述沉積通常被限制在650 °C的溫度，因為在更 低的溫度下沉積速率會下降到低於4埃/分鐘。在LPCVD 方法中，含有直接Si-C鍵的前驅物導致薄膜中的碳污染。 無碳沉積需要高於5:1的ΝΗγ前驅物比率。在較低的氨濃 度下會發現薄膜中含有碳。二乙基石夕烧和氨方法的處理一 般需要覆蓋舟孤或溫度梯度（temperature ramping)，以改進 整個晶片上的均勻性。 美國專利No. 5, 234, 869("‘869專利"）公開了使用 Si(N(CH3)2)4和氨作為反應氣體，在700°C和〇.5 Torr的壓 7 1374887 力下，通過LPCVD形成氮化矽薄膜。其他選自於由 SiH(N(CH3)2)3、SiH2(N(CH3)2)2 和 SiH3(N(CH3)2)組成的組 的反應物與氨或氮的組合也被建議作為反應物。869專利 還公開了通過使用由氣體產生的電漿來或通過用紫外線輻 射來激發氣體使沉積溫度降低到300°C。 參考文獻 R. G. Gordon 和 D. M. Hoffman, Dimethylamido Complexes and Ammonia as Precursors for the Atmospheric Pressure Chemical Vapor Deposition of Silicon Nitride Thin Films, Chem, Mater., 2 4-(1990) > 480-482頁，公開了減少包括胺基矽烷，如四（二甲基胺基） 矽烷的氮化矽薄膜中的含碳量的其他嘗試。該參考檔公開 了使用前驅物四（二曱基醯胺基）矽烷Si(NMe2)4和氨在 600-75 0°C的沉積溫度下通過APCVD沉積氮化矽薄膜。該 參考檔還教導了使用Si(NMen)4_n而不使用氨在750。(：的沉 積溫度的薄膜沉積，將導致以較低的生長速率獲得該薄 膜’同時還含有大量的碳（22-30%)和氧（15-17%)污染。 US專利No.5,874,368("‘3 68專利"）描述了使用雙（第三 丁基胺基）矽烷（t-C4H9NH)2SiH2和氨在50(TC-800°C的溫度 範圍，通過LPCVD方法來沉積氮化矽薄膜。 用於沉積氮化矽薄膜的前驅物如BTBAS和氯矽烷通常 在高於550°C的溫度沉積薄膜。半導體器件的微型化和低 熱量衡算（thermal budget)的趨勢需要較低的加工溫度和較 向的沉積速率。應該降低氮化石夕薄膜沉積的溫度，以防止 離子在晶格中擴散，特別是對於那些包含金屬化層的並在 1374887 °C或更低）沉積的胺基矽烷前驅物，可以打算通過在si-N 鍵附近引入吸電子基團以從Si-N鍵移動電子密度來減弱所 述Si-N鍵。
使用量子力學在'度泛函理論（quantum mechanical density funcitonal theory)，使用電腦模型軟體進行大量計 算’以系統評估一系列被各種具有至少一個吸電子取代基 序列取代的各種S iN前驅物的反應能《通過使用與雙數原 子基设疋增強的極化函數（d〇uble numerical atomic basis set augmented with polarization functions)結合的由
Perdew-Wang (PW91)提出的交換-關聯泛函數 (exchange-correlation functional)，根據廣義梯度近似（GGA) 進行所述計算。所有的分子結構都被完全優化，以獲得能 量最有利的幾何結構。隨後，使用下述方程式（2)評估反應 能： ΔΕ = [E((R1R2N)n.1Si(NH2)R34.n) + ECR^^^-ECNHa) -E((R,R2N)nSiR34.n)] (2) 在方程式（2)中，期望的是，△]5的值越低，則以卞鍵越弱， 從而可以獲得越低的沉積溫度。 圖1提供了對於下述的胺基矽烷前驅物16或分別地三 (1，1-二甲基肼基）第三了基石夕炫、雙（U•二甲基骄）_乙基石夕 烧、雙（1山二甲基肼基）_曱基石夕⑦、雙（二乙基胺基）石夕烧、 三（異丙基胺基）矽烷和三（第三丁基胺基）矽烷，實驗上測定 的沉積溫度和使用電腦模型軟體所計算的活化能水準之間 的關係不意圖。圖i表明，活化能隨沉積溫度而增大。圖 15 1374887 2提供了對於胺基矽烷前驅物16，實驗上測定的沉積溫度 和使用電腦模型軟體計算的反應熱的示意圖。圖2表明， 沉積溫度隨反應熱的搢大而升高。圖3提供了對於胺基矽 烷前驅物1-6 ’實驗上測定的活化能與使用電腦模型軟體計 算的反應熱的關係示意圖。該實施例表明，活化能隨反應 熱的增大而增大。通過回顧圖丨_3的結果，在某些實施方
案中’前驅物的沉積溫度可以通過使用上述方程式的反 應熱進行計算推測。在某些實施方案中，優選地，所述胺 基矽烷前驅物的活化能為約45kcal/m〇1或更低、或者約 kcal/mol或更低、 kcal/mol或更低、 他實施方案中，優 kcal/mol或更低、 或者約35 kcal/mol或更低 '或者約3〇 或者約25 kcal/mol或更低。在這個或其 選地胺基矽烷前驅物的反應能為約5.5 約 4.0 kcal/mol 或更低、約 3.5 kcal/m〇1 或更低、或者約3.0 keal/mGl或更低、或者約2 5 ^秦〇1 或更低。
圖中使用的前驅物i-6，或三（1，κ二甲基肼基） 三丁基矽烷、雙（1，丨·二曱基肼）·乙基矽烷雙（1，1二甲^ 肼基基發燒、雙（二乙基胺基）㈣、三（異丙基胺❹ 烷和三（第三丁基胺基）矽烷的結構如下所示： 16 J374887 N-N-Si—N—N ’ Η I H 、 NH 、
H
N一N—Si—N—N
N—N-Si—N—N ，H、 3
在一個實施方案中’如式（I)或（II)所述的具有至少一個 吸電子取代基的胺基矽烷前驅物可以通過氯矽烷與相應胺 的胺基化反應製得。很適合用於所述反應的代表性胺是烷 基、其為環狀或雜環的。優選的胺是低級烷基胺如乙基、 異丙基、第三丁基和環己基。進一步地，根據所需要產物， 所述胺可以是第一或第二胺。所述氨化反應典型地在室溫 或更低的溫度下進行。烴溶劑如己烷和戊烷通常用作反應 介質。在一個特定實施方案中，具有式⑴或（11)的胺基矽烷 前驅物可以如由下面示例性的反應（A)、（B)和（C)進行製備： WNH + ClSiH3 ----- R'R^-SiHs + R^^H-HCl (A) 4 RWNH + H2SiCl2 ----- R1R2N-SiH2-NR1R2 + 2R1R2NH-HC1 (B) 6 rVNH + HSiCl3…—（RYNhSiH + SRWNH-HCl (〇 在另一個實施方案中，式（I)的胺基矽烷前驅物使用本文 戶斤述的實施例4、5和6描述的方法製得。在這些或其他實 施方案中’本文所述的胺基石夕炫•前驅物由更通常可獲得的 17 1374887 胺基石夕烧通過胺基交換反應（transarninati〇n reaction)得到。 如上所述’本文描述的式⑴或（π)的胺基矽烷前驅物可 以用作用於在基材上沉積含矽薄膜的前驅物，所述含矽薄 膜例如但不限於氮化矽薄膜、氧化矽薄膜、碳氮化矽薄膜 和氮氧化矽薄膜。合適的基材的實例包括但不限於，半導 體材料如砷化鎵（"GaAs")、氮化硼（"BN")矽，和包含矽（如 結日日矽、多晶矽、非晶矽、磊晶矽（epiUxial siHc〇n)、二氧 化矽（"si〇2")、碳化矽（"Sic")、碳氧化矽（"si〇c")、氮化矽 (SiN )、碳氮化矽（"SiCN")、有機矽酸鹽玻璃（"〇sg")、有 機氟矽酸鹽玻璃（"〇FSG")、氟矽酸鹽玻璃（"MG"))的組合 物，以及其他合適的基材或它們的混合物。基材還可以進 一步包括各種的將薄膜施用於其上的層，例如抗反射塗 層、光阻劑、有機聚合物、多孔有機和無機材料、金屬如 銅和鋁、或擴散阻擋層。式⑴的胺基矽烷前驅物可以使用 任何的本發明描述的或本領域已知的技術進行沉積。沉積 技術的典型實例包括但不限於，化學氣相沉積（cvd)、原子 層儿積（ALD ) ’脈衝CVD (pulsed CVD) '電漿辅助的化 學氣相沉積（"PACVD")和電漿增強的化學氣相沉積 ("PECVD”）。 在某些實施方案令，胺基矽烷前驅物通過使用CVD或 ALD技術被沉積到基材上。在某些實施方案中，式或（η) 的胺基矽烷前驅物的沉積可以在55〇r或更低、或者5〇〇 °c或更低、或者40(rc或更低、3〇(rc或更低、或者2〇〇它 或更低、或者100°C或更低、或者是上述端點之間的任意 1374887 範圍，如3〇〇。〇 -5 50°C的溫度下進行。取決於使用的沉積技 術 5〇 mtorr-1 00 torr的壓力是示例性的。在典型的cvd 沉積方法中，胺基矽烷前驅物被引入加工室中，例如真空 至在某些實施方案中，除式（I)的胺基石夕院前驅物之外的 其他化學試劑，可以在胺基矽烷前驅物被引入之前、期間 和/或之後被引入。能量源，例如熱、電漿或其他源，激發 胺基矽烷前驅物和任選的化學試劑，從而在至少部分基材 上形成薄膜。 原子層沉積（ALD)包括連續引入第一前驅物脈衝和，在 某些實施方案中，第二前驅物脈衝。在其中在ALD方法中 使用多於一種前驅物的實施方案中，連續地引入第一前驅 物脈衝，接奢是吹掃氣體脈衝和/或泵抽真空，接著是第二 前驅物脈衝，隨後是吹掃氣體脈衝和/或泵抽真空。單個脈 衝的連續引入導致每種前驅物在基材表面的單層的交替自 限（self-limiting)化學吸附，並在每個週期形成沉積材料的 % 單層。如需要地重複所述週期以產生所需厚度的薄膜。在 ALD處理期間，基材被保持在易於化學吸附的溫度範圍， 即，所述溫度足夠低以保持被吸附物種和底層基材之間的 鍵完整，同時又足夠高，以避免前驅物的縮合和提供足夠 的活化能用於在每個方法週期中的表面反應。加工室的溫
度可以為 0°C -400°C、或 0°C -300°C，或 〇°C -275°C » 在 ALD 處理期間，加工室内的壓力可以為〇U000 T〇rr、或〇 l T0rr或〇_ 1-10 Ton·。然而，理解的是，用於任何特定的ald 方法的溫度和壓力可以根據包含的一個或多個前驅物而變 工374887 化。 方法相傳統的CVD方法，ALD的生長速率較低。則 2的典型生長速率為W埃/週期。—個提高生長速率的 二=高的基材溫度下進行沉積。本發明描述的胺基 :?別：物可以在相對較低的溫度下沉積切薄膜，從而 知尚了薄膜的生長速率。 根據所需要的薄膜’在切薄膜的沉積方法中可以使用 傳統的氧化劑。代表性的氧化劑包括過氧化氫、—氧化二 氮、臭氧和分子氧。典型地，氧㈣與胺基錢前驅物的 比率為大m，優選為CM_6摩爾氧化劑/摩爾有機胺基石夕 烷前驅物。 式⑴或（II)的胺基矽烷前驅物的沉積可以在沒有、或存 在活性氮源時進行，所述氮源例如氨、肼、烷基肼、二烷 基肼以及它們的混合物。氮源與胺基矽烷的摩爾比通常在 〇到>1〇:1的一個很寬範圍内。所述上限受限於對前驅物的 稀釋效果，這種稀釋效果會顯著降低沉積速率❶優選的範 圍為0.1至4:1»經由沉積的薄膜形成還可以在有或沒有其 他氣體時進行，所述其他氣體包括惰性氣體，如氮和氦氣。 製造者使用氣體以獲得相應的前驅物的稀釋，可以改進沉 積的均勻性或改進化學氣相滲透的滲透作用。 如上所述，在某些實施方案中，另外的化學試劑或前驅 物可以在式（I)或（II)的胺基>6夕烧前驅物被引入加工室之 前、期間和/或之後被引入。化學試劑的選擇可取決於希望 獲得的薄膜的組成。示例性化學試劑包括但不限於氧化劑 20 ^74887 (即，
◦2、NO、N02、〇3、CO、C02 等）；水；鹵化物；含 南素<5夕燒；烷基氣石夕烧、烧基溴發烧或烧基破石夕烧；石夕鹵 物錯合物（silicon halide complexes)如四氣化發、四漠化 石夕或四峨化矽；或它們的組合。還設想的是，還可以使用 上述錯合物的衍生物。所述化學試劑可以直接作為氣體被 輸送到加工室’作為蒸發的液體、昇華的固體進行輸送和/ 或通過惰性載體氣被傳送到反應室中。惰性載體氣的實施 例包括氮氣、氫氣、氮氣、氙氣等。 在進行/冗積方法中，本發明描述的胺基石夕烧可以與其他 甲矽烷基前驅物摻合以改變薄膜的性能。其他前驅物的實 例包括一-第三丁基胺基矽烷、三-異丙基胺基矽烷、雙-二 乙基胺基矽烷、二_二甲基胺基矽烷和二異丙基胺基矽烷。 本發月描述的任何上述成膜方法以及本領域已知的其 他成膜方法，可以單獨或結合進行使用。 下歹J實施例舉例說明在本文中描述的胺基石夕烧前驅 物匕們而不旨在以任何方式限制本發明。 實施例1.在A c + BAS中-CH3被_CF3置換的效果 如下列結構7所示，罅 一 ητ T雙（第二丁基胺基）矽烷bTBas的 第二丁基中的—個甲某：田Pc «· 1图T基用-CF3基團連續地置換。 21 1374887 ch3 --ch3 ch3 cf3 η
I H3C--N-Si-Ν' ch3 h 使用上述方知式（2)通過名為DMol3, Materials Studio v. 4.2.0.2的化學模型軟體程式計算上述分子以及具有2或3 個被置換甲基的類似分子的反應能，所述軟體程式由
Accelyrs，Inc. of San Diego，California 提供，結果如圖 4 所示。圖4表明’用-CF3基團完全置換甲基會導致反應能 降低。特別地’所述分子中的全部甲基全部被_CF3基團完 全置換使所述反應由吸熱反應改變為放熱反應。因此，si_N 鍵的斷裂被期望在比在BTBAS中低很多的溫度下發生，從 而允許更低的沉積溫度。 實施例2.在BTBAS中-CH3被-CN置換的效果 BTB AS的第三丁基中的曱基用-CN基團進行連續置 換。通過使用名為 DMol3, Materials Studio v. 4.2.0.2 的化 學模型軟體程式和上述方程式（2)計算BTBAS和具有1、2 或3個甲基被-CN基團置換的式（I)的胺基石夕烧前驅物的反 應月’所述軟體程式由Accelyrs, Inc. of San Diego， California提供。結果如圖5所示。由於分子内氫鍵的形成， 置換初始時引起反應能增大◊然而，一旦完全置換，所述 反應能比BTBAS低約1.6kcal/mol。因此，Si-N鍵的斷裂 期望在比在BTBAS中更低的溫度下發生。 22 1374887 實施例3. ~F取代的效果 將一系列具有烷基和芳基的包含至少一個吸電子取代 基或I的胺基妙焼前驅物與不包含氟而包含氫的類似胺基 石夕燒前驅物進行比較。對表丨中所列的分子進行計算以檢 測Η被F的置換’通過使用本文所述的方程式（2)以及由 ACCelyrS’ Inc· of San Diego, California 提供，名為 DMol3, Materials Studi〇 v 4 2 〇 2的化學模型軟體程式計算的反應 熱也同樣列於表中。對照的結果如下表工所示。
表I
23 1374887 實施例3 b FH( N-SiH, J -—«—j 0.93 實施例3 c f2c N--SiH3 」 ------- 0.42 對照例3 < N-SiH3 w 0.27 實施例3 d ( N—SiH3 FHC-' 0.07 實施例3 e ~~~r\ FHC N SiH3 0.11 實施例3f { H-SiH, V_/ N-CHF -1.20 結果表明’在所有情況下’所有通過F置換η能夠降 低反應能。特別地，在α位元的溫度降低效果最明顯，接 著疋在沒位然後7位。較高的置換率產生更有利的反應能。 實細例4a .從3,3_二氟呱啶前驅物製備雙（3,3_二氟呱 啶）矽烷 在裝有磁力擔垃技 現评棒、n2放氣閥和橡膠隔片的240ml特 24

Claims (1)

1374 (2012年8月修正） is ⑯巧 七、申請專利範圍：一一一」 1、一種用於沉積含矽薄膜的胺基矽烷前驅物，其包含 下式（I): (R'R2N)nSiR14.n (I) 其中取代基R1和R2各自獨立地選自包含1_2〇個碳原子 的烧基和包含6_30個碳原子的芳基，其中式⑴的Rl及尺2 選自連接形成一環狀結構的Ri和R2及不連接形成一環狀結 構的R1和R2， 其中取代基R1和R2中的至少一個包含至少一個吸電子 取代基’該吸電子取代基選自：？、（：卜81'、1、€1^、1^02、 P〇(OR)2、OR、RCOO、COOH、及 S02R，其中所述至少一 個吸電子取代基中的R選自烷基或芳基，R1選自Η、包含 1-20個碳原子的烷基或包含6-12個碳原子的芳基； 其中R、R、R及R1的任一個或者全部及該吸電子取代 基是被取代的或未被取代的； 以及η為1-4的整數。 2、 如申請專利範圍第1項的胺基矽烷前驅物，其包含 雙（3,3-二氟呱啶基）矽烷。 28 1 一種在基材上通過化學氣相沉積來沉積含矽薄膜的 方法，該方法包括： 在加工室中提供所述基材； 在足以使含矽薄膜反應並沉積在所述基材上的溫度和 1374887 (2012年8月修正) . 壓力下，將胺基矽烷前驅物引入所述加工室中，其中所述 胺基矽烷前驅物包含具有下式（I)的化合物： (R'R2N)nSiR34_n ⑴ 其中取代基R和R各自獨立地選自包含1_2〇個碳原 子的烷基和包含6-30個碳原子的芳基，其中式⑴的Rl及 R2選自連接形成一環狀結構的R1和R2及不連接形成一環 狀結構的R1和R2， 其中取代基R1和R2中的至少一個包含至少一個吸電孑 _取代基，該吸電子取代基選自：F、Cl、Br、I、CN、Ν〇2、 PCK〇R)2 ' 〇R、RC〇〇、SO、S〇2、s〇2r，其中在所述至少 一個吸電子取代基中的R選自烷基或芳基；R3選自H、包 含1-20個碳原子的烷基或包含6_12個碳原子的芳基；其 中R1、R2、R及R3的任一個或者全部及該吸電子取代基是 被取代的或未被取代的；以及η為丨_4的整數。 φ 4、如申請專利範圍第3項的方法，其中引入步驟進〆 步包括選自氨、氮和肼的氮源。 5、 如申請專利範圍第4項的方法，其中所述氮源是象 或氮，且該氮源以氮源：前驅物為〇.丨_4:1的量存在。 6、 如申請專利範圍第3項的方法，其中所述溫度為約 400〇C -約 700。。。 29 7、如由咬击伙 （2〇丨2年8月修正） 如申凊專利範圍第^ 9Λ ^ 弟j項的方法，其中所述壓力為約 U mT〇rr-約 20 Torr。 下式（II) 種用於沉積含石夕薄膜的胺基石夕院前驅物其包含 A"SiR44-n (II) 、田A疋至夕―個選自下列胺基（a)至⑷及（f)至（h) 的基團時，R4撰自_ , 匕3 1-20個碳原子的烧基或包含 6·12/碳原子的芳基；以及的整數：及 田A是⑴時’ R4選自氫，包含1-20個碳原子的烧基或 包含：12,破原子的芳基；以及…-4的整數，及 田A疋⑴時，R4選自A，包含1-20個碳原子的烷基或 包含6_12個碳原子的芳基；以及η為2-4的整數， F
F
F b
F F
〇Me OMe VI f cf3 cf^Cj c NI g NC、n/CN nc、n,ch3 9、如申請專利範圍第8項的胺基矽烷前驅物，其中A 是下列的胺基（a): 30 1374887 (2012年8月修正)
10、如申請專利範圍第8項的胺基矽烷前驅物，其中A 是下列的胺基（b):
(b) 〇 11、如申請專利範圍第8項的胺基矽烷前驅物，其中A 是下列的胺基（c):
(c)。 12、如申請專利範圍第8項的胺基矽烷前驅物，其中A 是下列的胺基（d):
⑹。 31 J374887 (2012年8月修正) 13、如申請專利範圍第8項的胺基矽烷前驅物，其中a 是下列的胺基（f): OMe OMe V I (f)。
14、如申請專利範圍第8項的胺基矽烷前驅物，其中A 是下列的胺基（g):
(g) 0 15、如申睛專利範圍第8項的胺基矽烧前驅物，其中A 是下列的胺基（h): cf3 cf3
F2C、n^CF2 I ⑻。 16、如申凊專利範圍第8項的胺基矽烷前驅物，其中A 是下列的胺基（i): nc、n;n
32 J374BB7 (2012年8月修正) ; 丨7、如申請專利範圍第8項的胺基矽烷前驅物，其中A . 0下列的胺基（j): Ά I ⑴。 18、 如申請專利範圍第8項的胺基矽烷前驅物，其中的 • R1及R2為不連接形成一環狀結構的Rl和R2。 19、 一種胺基矽烷前驅物，其包含雙[雙（2-甲氧基乙基） 胺基]*夕燒。 〇 一種胺基矽烷前驅物，其包含雙（2-曱氧基乙基）胺 基矽烷。 33
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