TWI822206B - 一種利用反應揮發性化學物質的氣相沉積裝置 - Google Patents

一種利用反應揮發性化學物質的氣相沉積裝置 Download PDF

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TWI822206B
TWI822206B TW111127939A TW111127939A TWI822206B TW I822206 B TWI822206 B TW I822206B TW 111127939 A TW111127939 A TW 111127939A TW 111127939 A TW111127939 A TW 111127939A TW I822206 B TWI822206 B TW I822206B
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transition metal
precursor
certain embodiments
metal halide
gas phase
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凱嘉 費瑞南
提摩 哈坦帕
米可 雷鐵娜
瑪庫 雷可拉
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荷蘭商Ａｓｍ Ｉｐ私人控股有限公司
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Abstract

本發明揭露一種藉由週期性沉積處理在基材上形成一含過渡金屬薄膜的方法。該方法可包括：使該基材接觸一第一氣相反應物，所述第一氣相反應物包括含雙牙氮加合物配位基之過渡金屬鹵化合物；及使該基材接觸一第二氣相反應物。本發明揭露一種用於將含雙牙氮加合物配位基之過渡金屬鹵化合物供應給一反應腔之方法及相關的氣相沉積裝置。

Description

一種利用反應揮發性化學物質的氣相沉積裝置
本發明大體上有關藉由週期性沉積處理在基材上形成含過渡金屬薄膜的方法及特別用於形成含鈷、銅和鎳薄膜之方法。本發明還大體上亦有關用於將過渡金屬鹵化合物供應給氣相沉積工具之方法及相關的氣相沉積裝置。 ［共同研究協議之各方］
本說明書所主張的發明是代表及/或關於赫爾辛基大學和ASM Microchemistry Oy之間的共同研究協議。該協定在所主張之本發明作成之日及之前生效，且所主張之本發明係由於在該協定範疇內所進行之活動而作成。
先進技術世代中的半導體器件製程通常需要用於形成含過渡金屬薄膜的最新技術沉積方法，諸如(例如)元素過渡金屬、過渡金屬氧化物、過渡金屬氮化物、過渡金屬矽化物、過渡金屬磷化物、過渡金屬硒化物或過渡金屬硼化物。
沉積含過渡金屬薄膜的共同要求在於沉積處理是非常保形性(conformal)。例如，時常需要保形性沉積，以在包括高縱橫比特徵的三維結構上均勻沉積含過渡金屬薄膜。沉積含過渡金屬薄膜的另一常見要求在於沉積處理能夠沉積在大基材面積上是連續的超薄膜。在含過渡金屬薄膜是導電的特定情況下，可能需要最佳化沉積處理以產生低電阻薄膜。
諸如(例如)原子層沉積(Atomic Layer Deposition，ALD)和週期性化學氣相沉積(Cyclical Chemical Vapor Deposition，CCVD)的週期性沉積處理將一或多個前驅體(反應物)順序引入一反應腔中，其中前驅體採用順序、自我限制的方式每次在基材表面上起反應。產生具優異保形性和原子級厚度控制的含金屬薄膜之週期性沉積處理已經過證明。
週期性沉積處理可用於沉積含過渡金屬薄膜，諸如(例如)含銅薄膜、含鎳薄膜、且特別是含鈷薄膜。然而，適用於週期性沉積含過渡金屬薄膜、而且特別是含鈷薄膜的化學前驅體是不常見且成本過高。例如，用於週期性沉積含鈷薄膜的現有化學前驅體可能需不想要的高溫沉積處理及/或使用電漿增強沉積處理。此外，由於基材材料的沉積處理敏感性，使得利用現有鈷化學前驅體的週期性沉積處理可能不需要。因此，週期性沉積方法，適用於週期性沉積處理的化學前驅體和相關的氣相沉積裝置對於形成含過渡金屬薄膜，而且特別是含鈷、銅和鎳薄膜是理想的。
本發明內容以簡化形式來介紹一系列概念。這些概念會在下文的本發明示例實施例中做進一步詳述。本發明內容非意圖確定所請求保護主題的關鍵特徵或必要特徵，也非意圖用來限制所請求保護主題的範圍。
在本發明的某些實施例中，提供藉由週期性沉積處理在基材上形成含金屬薄膜的方法。該方法可包括：使該基材接觸一第一氣相反應物，其包括含雙牙氮(bidentate nitrogen)加合物配位基之過渡金屬鹵化合物；及使該基材接觸一第二氣相反應物。
在本發明的某些實施例中，提供藉由週期性沉積處理在基材上形成含金屬薄膜的其他方法。該方法可包括：使該基材接觸一第一氣相反應物，所述第一氣相反應物含有加合物配位基之過渡金屬化合物；及使該基材接觸一第二氣相反應物，其中該過渡金屬是選自於由銅(Cu)、鎳(Ni)和鈷(Co)所組成的群組。
在本發明的某些實施例中，提供用於將一含雙牙氮加合物配位基的過渡金屬鹵化合物供應給反應腔的方法。該方法可包括：提供一構造成含過渡金屬鹵化合物的前驅體來源器皿，將該前驅體來源器皿流體連通到反應腔；將該前驅體來源器皿中所含的過渡金屬鹵化合物加熱至高於150°C的溫度；產生該至少0.001毫巴(mbar)的過渡金屬鹵化合物的蒸氣壓；及將該過渡金屬鹵化合物供給該反應腔。
在本發明的某些實施例中，提供利用反應揮發性化學物質的一氣相沉積裝置。該氣相沉積裝置可包括：一反應腔；一基材，其設置在該反應腔中；及一前驅體來源器皿，其係流體連通該反應腔；及一過渡金屬鹵化合物，其含有設置在該前驅體來源器皿中的一含雙牙氮加合物配位基。
為概述本發明之目的及相較於先前技術所達成之優點，本發明之某些目的及優點已於此描述於上文中。  當然，應明瞭無須所有該等目的或優點皆可根據本發明之任何特定具體例來達成。因此，舉例而言，熟悉本技藝者當認知本發明可依達成或最佳化本文所教示或提出之一個優點或一組優點而無須達成本文中可能教示或提出之其他目的或優點的方式來具體化或實施。
此等具體例全部意欲在本文所揭示之本發明範疇內。此等及其他具體例將自以下參考附圖的某些具體例之詳細描述而對熟悉本技藝者變得顯而易見，但本發明並不受限於所揭示之任何特定具體例。
儘管在下文中揭示特定實施例及實例，但彼等熟悉本技藝者應理解，本發明延伸超出本發明所具體揭示之實施例及/或用途及其明顯修改及等效物。因此，期望所揭示之本發明範疇不應受限於下文所描述之特定揭露的實施例。
本文介紹的圖示並非表示為任何特定材料、構造或裝置的實際視圖，而僅用於描述本發明實施例的理想表現。
如本文所使用，術語「循環沉積」可指將前驅體(反應物)連續引入至反應腔室中以在基板上方沉積一膜且包括諸如原子層沉積及循環化學氣相沉積之沉積技術。
如本文所使用，術語「循環化學氣相沉積」可指當中基板依序暴露於兩種或更多種揮發性前驅體之任何製程，該等前驅體在基板上反應及/或分解以產生所需沉積物。
如本文所使用，術語「基板」可指代可使用或在其上可形成裝置、電路或膜之任何底層材料。
如本文所使用，術語「原子層沉積(Atomic Layer Deposition，ALD)」可指在處理腔中實施沉積循環(較佳地複數個連續沉積循環)的氣相沉積製程。通常地，在各循環期間，前驅體化學吸附至沉積表面(例如基板表面或先前所沉積之底層表面，諸如來自先前ALD循環之材料)，從而形成不容易與其他前驅體反應(亦即自我限制反應)的單層或亞單層。之後，必要時可接著將反應物(例如另一前驅體或反應氣體)引入至處理腔室中以用於將經化學吸附之前驅體轉化為沉積表面上的所需材料。通常，此反應物能夠進一步與前驅體反應。此外，亦可在各循環期間利用沖洗步驟自處理腔室移除過量前驅體及/或在轉化經化學吸附之前驅體之後自處理腔室移除過量反應物及/或反應副產物。此外，當使用前驅體組合物、反應性氣體和沖洗(例如，惰性載體)氣體的交替脈衝進行時，如本文使用的術語「原子層沉積」還意指包括相關術語指定的處理，諸如「化學氣相原子層沉積」、「原子層磊晶」(Atomic Layer Epitaxy，ALE)、分子束磊晶(Molecular Beam Epitaxy，MBE)、氣體源MBE或有機金屬MBE和化學束磊晶。
如本說明書的使用，術語「膜」、「薄膜」、「層」和「薄層」可意指藉由本說明書揭露方法沉積的任何連續或非連續結構和材料。例如，「膜」、「薄膜」、「層」和「薄層」可包括2D材料、奈米棒、奈米管或奈米顆粒或甚至部分或整個分子層或部分或整個原子層或原子及/或或分子簇。「膜」、「薄膜」、「層」和「薄層」可包括一具有針孔的材料或層，但仍然是至少部分連續。
如本說明書的使用，術語「含過渡金屬的薄膜」可意指含過渡金屬物薄膜，包括但沒有限於元素過渡金屬、過渡金屬氧化物、過渡金屬氮化物、過渡金屬矽化物、過渡金屬硒化物、過渡金屬磷化物、過渡金屬硼化物及其混合物。此外，術語「含過渡金屬薄膜」可意指一含過渡金屬物以及含碳及/或氫薄膜。
在本發明的實施例中提供許多示例性材料，應注意，針對所示示例性材料的每一者提供的化學式不應構成限制，而且提供的非限制性示例材料應不受限於一特定實例化學計量。
本發明包括用於在基材上形成含過渡金屬薄膜的方法及特別用於在基材上週期性沉積含過渡金屬薄膜的方法。本發明的實施例可包括用於週期性沉積含過渡金屬薄膜的方法，諸如(例如)含銅薄膜、含鎳薄膜，及特別是含鈷薄膜。
在本發明的特別具體實施例，可使用週期性沉積處理來沉積含鈷薄膜，諸如(例如)元素鈷、氧化鈷、氮化鈷、矽化鈷、磷化鈷、硒化鈷或硼化鈷。在新興的半導體器件處理中，鈷金屬薄膜在諸如襯層和覆蓋層的應用方面可能是重要，以抑制銅互連材料電遷移至周圍介電材料。實際上，隨著先進技術世代的器件特徵尺寸減小，使得鈷金屬薄膜可當作互連材料使用，取代普遍使用的銅互連。鈷金屬薄膜在巨磁阻應用和磁記憶體應用方面亦是有意義。此外，鈷薄膜亦可沉積在積體電路的矽閘接觸，以在退火時形成矽化鈷。鈷的氧化物可應用於新興的能源相關技術，諸如(例如)鋰離電池和電化學水氧化以及用作催化材料。
通常利用濺射技術以及採用金屬有機前驅體的CVD方法來實現元素鈷和含鈷薄膜的沉積。然而，此用於沉積含鈷薄膜的已知方法由於其固有的非保形性而可能不適用於先進技術世代。諸如原子層沉積的週期性沉積方法是特徵保形性沉積方法，而且非常適宜在包括高縱橫比特徵的三維結構上沉積含保形過渡金屬薄膜。因此，非常需要用於沉積含過渡金屬薄膜，而且特別用於沉積含鈷薄膜的週期性沉積方法。
此外，由於缺乏適宜化學前驅體和成本有效的化學前驅體，已阻礙含鈷薄膜的週期性沉積方法的發展。例如，利用已知化學前驅體進行週期性沉積含鈷薄膜可能需要不想要的高溫沉積處理，例如高於300°C。電漿增強原子層沉積處理可用於在較低沉積溫度下沉積含鈷薄膜，但是由於來自高能量電漿反應物的基底半導體器件結構的可能損壞，使得在某些器件應用方面可能不想要使用電漿處理。因此，想要適宜沉積含過渡金屬薄膜的化學前驅體，而且是藉由週期性沉積處理沉積含鈷薄膜的特定化學前驅體。此外，需要方法和相關裝置將一化學前驅體供應給一適宜氣相沉積系統，諸如(例如)一原子層沉積裝置。
因此，本發明的實施例可包括藉由週期性沉積處理在基材上形成一含過渡金屬薄膜的方法。該方法可包括：使該基材接觸一第一氣相反應物，其包括含雙牙氮加合物配位基之過渡金屬鹵化合物；及使該基材接觸一第二氣相反應物。
在本發明的某些實施例中，可藉由將過渡金屬鹵化合物當作金屬前驅體使用的週期性沉積處理來沉積含過渡金屬層(或薄膜)。週期性沉積處理的一非限制性示例實施例可包括原子層沉積(ALD)，其中ALD是基於通常自限制反應，藉使反應物的順序和交替脈衝用於每個沉積週期性沉積約一原子(或分子)單層材料。通常選擇沉積條件和前驅體以提供自飽和反應，使得一反應物的吸附層留下沒有與相同反應物的氣相反應物起反應的表面鈍化(Surface termination)。隨後使基材接觸能與先前鈍化起反應的不同反應物，以允許繼續沉積。因此，交替脈衝之各循環通常留下不超過約一個單層的所需材料。然而，如前述，熟習該項技藝者將明白，在一或多個ALD循環中，可沉積一個以上的材料單層，例如，如果儘管處理的交替本質發生某些氣相反應。
在用於沉積一含過渡金屬薄膜的ALD型處理中，一沉積循環可包括使該基材接觸一第一反應物；從反應空間移除任何未反應的第一反應物和反應副產物；及使該基材接觸一第二反應物，並伴隨一第二移除步驟。所述第一反應物可包含一過渡金屬鹵化合物(金屬前驅體)，而且所述第二反應物可包含一氧前驅體、一氮前驅體、一矽前驅體、一硫前驅體、一硒前驅體、一磷前驅體、一硼前驅體或一還原劑之至少一者。
前驅體可藉由惰性氣體(諸如氬氣(Ar)或氮氣(N 2)分離以避免在反應物之間的氣相反應並可實現自飽和表面反應。然而，在某些實施例中，可移動基材以分別接觸一第一氣相反應物和一第二氣相反應物。因為反應是自飽和，使得可不需要對基材進行嚴格溫度控制和前驅體的精確劑量控制。然而，基材溫度最好使得入射氣體物不會凝結成單層且不會在表面上分解。在基材接觸下一反應化學物質之前，諸如藉由沖洗反應空間或藉由移動基材，從基材表面去除如存在的過剩化學品和反應副產物。藉助惰性沖洗氣體可有效從反應空間排出不想要的氣體分子。可使用真空泵來輔助沖洗。
能夠用於沉積含過渡金屬薄膜的反應器可用於沉積。此反應器包括ALD反應器以及具有適當提供前驅體的設備和器件的CVD反應器。根據某些實施例，可使用一噴灑頭式反應器。根據某些實施例，可使用交叉流、批式、小批式或空間式ALD反應器。
可使用的適宜反應器的實例包括市售單基板(或單晶圓)沉積設備，諸如可購自亞利桑那州菲尼克斯之ASM America,Inc.及ASM Europe B.V., Almere, Netherlands之Pulsar ®反應器(諸如Pulsar ®2000及Pulsar ®3000及Pulsar ®XP ALD)以及EmerALD ®XP及EmerALD ®反應器。其他市售反應器包括來自ASM Japan K.K(日本東京)商品名為Eagle ®XP 及XP8之彼等反應器。在某些實施例中，反應器是空間ALD反應器，其中基材在處理期間移動或旋轉。
在本發明的某些實施例中，可使用一批式反應器。適宜的批式反應器包括但不限於來自ASM Europe B.V(荷蘭阿爾梅勒)市售之商品名稱為A400及A412 PLUS的Advance ®400系列反應器。在某些實施例中，晶圓在處理期間旋轉。在其他實施例中，所述批式反應器包括構造成調適10個或更少晶圓、8個或更少晶圓、6個或更少晶圓、4個或更少晶圓或2個或更少晶圓的小批式反應器。在使用批式反應器的某些實施例中，晶圓對晶圓的不均勻性是小於3%(1σ)、小於2%、小於1%或甚至小於0.5%。
本說明書描述的沉積處理可選擇性實現在連接到模組化組合工具的一反應器或反應腔。在一模組化組合工具中，因為每個反應腔專屬於一類型處理，使得每個模組中的反應腔溫度可保持恆定，其相較於每次運行之前基材被加熱到處理溫度的反應器，此可提高產量。此外，在模組化組合工具中，可減少將反應腔泵吸到介於基材間的想要處理壓力位準的時間。在本發明的某些實施例中，沉積處理可在包括多個反應腔的模組化組合工具中進行，其中每個單獨的反應腔可用於將基材暴露於一單獨的前驅體氣體，而且所述基材可在不同反應腔之間轉移，用於暴露多種前驅體氣體，在受控環境下進行基材轉移以防止基材的氧化/污染。在本發明的某些實施例中，沉積處理可在包括多個反應腔的模組化組合工具中進行，其中每個單獨反應腔可構造成將基材加熱到不同沉積溫度。
一獨立式反應器可具有加載互鎖。在這情況下，沒有必要在每次運行之間冷卻反應空間。在某些實施例中，一用於沉積含過渡金屬薄膜的沉積處理可包括複數個沉積循環，例如ALD循環或週期性CVD循環。
在某些實施例中，週期性沉積處理用於在基材上形成含過渡金屬薄膜，而且週期性沉積處理可為一ALD型處理。在某些實施例中，週期性沉積可為一混合ALD/CVD或週期性CVD處理。例如，在某些實施例中，相較於一CVD處理，ALD處理的生長速率可能較低。一增加生長速率的方法可為在較高於通常在ALD處理中使用的基材溫度下操作的方法，導致化學氣相沉積處理，但仍然利用順序引入前驅體，此一處理可稱為週期性CVD。
根據本發明的某些實施例，ALD處理可用於在基材上沉積一含過渡金屬薄膜，諸如一部分製造的半導體器件結構。在本發明的某些實施例中，每個ALD循環包括兩不同沉積步驟或階段。在沉積循環的一第一階段(金屬相)中，需要沉積的基材表面係接觸一含經化學吸附到基材表面上的金屬前驅體之一第一氣相反應物，在所述基材表面上形成不超過約一單層反應物。在沉積的一第二階段中，需要沉積的基材表面係接觸含有一氧前驅體、一氮前驅體、一矽前驅體、一硫前驅體、一硒前驅體、一磷前驅體、一硼前驅體或一還原劑之至少一者的一第二氣相反應物，其中所述第二氣相反應物可在基材表面上與過渡金屬物起反應，以在基材上形成一含過渡金屬薄膜，諸如(例如)一元素過渡金屬、一過渡金屬氧化物、一過渡金屬氮化物、一過渡金屬矽化物、一過渡金屬硒化物、一過渡金屬磷化物、一過渡金屬硼化物及其混合物，以及進一步含有碳及/或氫的含過渡金屬薄膜。
在本發明的某些實施例中，所述第一氣相反應物可包括一含金屬前驅體，在本說明書亦稱為「金屬化合物」。在某些實施例中，所述第一氣相反應物可包含一具有加合物形成配位基的過渡金屬化合物。在某些實施例中，所述第一氣相反應物可包含一過渡金屬化合物。在某些實施例中，所述第一氣相反應物可包含一過渡金屬鹵化合物。在某些實施例中，所述第一氣相反應物可包含一具有加合物形成配位基的過渡金屬化合物，諸如單齒(monodentate)、雙齒(bidentate)或多齒(multidentate)加合物形成配位基。在某些實施例中，所述第一氣相反應物可包含一具有加合物形成配位基的過渡金屬鹵化合物，諸如單齒、雙齒或多齒加合物形成配位基。在某些實施例中，所述第一氣相反應物可包含一具有含氮的加合物形成配位基的過渡金屬化合物，諸如含氮的單齒、雙齒或多齒加合物形成配位基。在某些實施例中，所述第一氣相反應物可包含一具有含磷、氧或硫的加合物形成配位基的過渡金屬化合物，諸如含磷、氧或硫的單齒、雙齒或多齒加合物形成配位基。例如，在某些實施例中，該過渡金屬鹵化合物可包含一過渡金屬氯化物、一過渡金屬碘化物、一過渡金屬氟化物或一過渡金屬溴化物。在本發明的某些實施例中，該過渡金屬鹵化合物可包含一過渡金屬物，包括但沒有限於鈷、鎳或銅之至少一者。在本發明的某些實施例中，該過渡金屬鹵化合物可包含氯化鈷、氯化鎳或氯化銅之至少一者。在某些實施例中，該過渡金屬鹵化合物可包括含雙牙氮加合物形成配位基。在某些實施例中，該過渡金屬鹵化合物可包括含有兩個氮原子的加合物形成配位基，其中該等氮原子之每一者鍵結至少一個碳原子。在本發明的某些實施例中，該過渡金屬鹵化合物包含鍵結一中心過渡金屬原子的一或多個氮原子，藉此形成一金屬配合物(Metal complex)。
在本發明的某些實施例中，所述第一氣相反應物可包含一具有化學式(I)的過渡金屬化合物： [化學式1] (加合物) n-M-X a(I) 其中每個「加合物」是一加合物形成配位基，而且可獨立選擇成單齒、雙齒或多齒加合物形成配位基或其混合物；如果是單齒形成配位基，n是從1至4；如果是雙齒或多齒加合物形成配位基，n是從1至2；M是一過渡金屬，諸如(例如)鈷(Co)、銅(Cu)或鎳(Ni)；其中每個X a是另一配位基，而且可獨立選擇成一鹵化物或其他配位基；其中a是從1至4，而且在某些情況，a是2。
在本發明的某些實施例中，該過渡金屬化合物中的加合物形成配位基(諸如一過渡金屬鹵化合物)可包含一單齒、雙齒或多齒加合物形成配位基，其透過一氮原子、一磷原子、一氧原子或一硫原子之至少一者而配位所述過渡金屬化合物的過渡金屬原子。在本發明的某些實施例中，該過渡金屬化合物中的加合物形成配位基可包含一週期性加合物配位基。在本發明的某些實施例中，該過渡金屬化合物中的加合物形成配位基可包含單胺、雙胺或多胺。在本發明的某些實施例中，該過渡金屬化合物中的加合物形成配位基可包含單醚、雙醚或聚醚。在某些實施例中，該過渡金屬化合物中的加合物形成配位基可包含單膦、雙膦或多膦。在某些實施例中，該過渡金屬化合物中的加合物形成配位基可包含碳及/或除了在加合物形成配位基中的氮、氧、磷或硫之外。
在本發明的某些實施例中，該過渡金屬化合物中的加合物形成配位基可包含一單齒加合物形成配位基。在本發明的某些實施例中，該過渡金屬化合物中的加合物形成配位基可包含兩個單齒加合物形成配位基。在本發明的某些實施例中，該過渡金屬化合物中的加合物形成配位基可包含三個單齒加合物形成配位基。在本發明的某些實施例中，該過渡金屬化合物中的加合物形成配位基可包含四個單齒加合物形成配位基。在本發明的某些實施例中，該過渡金屬化合物中的加合物形成配位基可包含一個雙齒加合物配位基。在本發明的某些實施例中，該過渡金屬化合物中的加合物形成配位基可包含兩個雙齒加合物形成配位基。在本發明的某些實施例中，該過渡金屬化合物中的加合物形成配位基可包含一個多齒加合物形成配位基。在本發明的某些實施例中，該過渡金屬化合物中的加合物形成配位基可包含兩個多齒加合物形成配位基。
在本發明的某些實施例中，該加合物形成配位基包含氮，諸如胺、雙胺或多胺加合物形成配位基。在此實施例中，該過渡金屬化合物可包含三乙胺(TEA)、N,N,N',N'-四甲基-1,2-乙二胺(CAS：110-18-9)(TMEDA)、N,N,N',N'-四乙基乙二胺(CAS：150-77-6)(TEEDA)、N,N'-二乙基-1,2-乙二胺(CAS：111-74-0)(DEEDA)、N,N'-二異丙基乙二胺(CAS：4013-94-9)、N,N,N',N'-四甲基-1,3-丙二胺(CAS：110-95-2)(TMPDA)、N,N,N',N'-四甲基甲烷二胺(CAS：51-80-9)(TMMDA)、N,N,N',N'',N''-五甲基二乙烯三胺(CAS：3030-47-5)(PMDETA)、二伸乙三胺(diethylenetriamine)(CAS：111-40-0)(DIEN)、三乙烯四胺(triethylenetetramine)(CAS：112-24-3)(TRIEN)、三(2-氨基乙基)胺(CAS：4097-89-6)(TREN, TAEA)、1,1,4,7,10,10-六甲基三乙烯四胺(CAS：3083-10-1)(HMTETA)、1,4,8,11-四氮雜環十四烷(CAS：295-37-4)(Cyclam)、1,4,7-三甲基-1,4,7-三氮雜環壬烷(CAS：96556-05-7)或1,4,8,11-四甲基-1,4,8,11-四氮環十四烷(CAS：41203-22-9)之至少一者。
在本發明的某些實施例中，該加合物形成配位基包含磷，諸如膦、雙膦或多膦加合物形成配位基。例如，該過渡金屬化合物可包含三乙膦(triethylphosphine)(CAS：554-70-1)、亞磷酸三甲酯(CAS：121-45-)、1,2-雙(二乙基膦)乙烷(CAS：6411-21-8)(BDEPE)或1,3-二(聯苯基膦)丙烷(CAS：29149-93-7)之至少一者。
在本發明的某些實施例中，該加合物形成配位基包含氧、諸如醚、二醚或聚醚加合物形成配位基。例如，該過渡金屬化合物可包含1,4-二噁烷(CAS：123-91-1)、1,2-二甲氧乙烷(CAS：110-71-4)(DME，乙二醇二甲醚)、二乙二醇二甲醚(CAS：111-96-6)(二甘醇二甲醚)、三乙二醇二甲醚(CAS：112-49-2)(三甘醇二甲醚)或1,4,7,10-四氧雜環十二烷(CAS：294-93-9)(12-冠醚-4)之至少一者。
在本發明的某些實施例中，該加合物形成配位基可包含硫醚化合物或混合醚胺，諸如1,7-二氮-12-冠醚-4：1,7-二氧雜-4,10-二氮雜環十二烷(CAS：294-92-8)或1,2-雙(甲硫基)乙烷(CAS：6628-18-8)之至少一者。
在某些實施例中，該過渡金屬鹵化合物可包含氯化鈷N,N,N',N'-四甲基-1,2-乙二胺(CoCl 2(TMEDA))。在某些實施例中，該過渡金屬鹵化合物可包含溴化鈷四甲基乙二胺(CoBr 2(TMEDA))。在某些實施例中，該過渡金屬鹵化合物可包含碘化鈷四甲基乙二胺(CoI 2(TMEDA))。在某些實施例中，該過渡金屬鹵化合物可包含氯化鈷N,N,N',N'-四甲基-1,3-丙二胺(CoCl 2(TMPDA))。在本發明的某些實施例中，該過渡金屬鹵化合物可包含氯化鈷N,N,N',N'-四甲基-1,2-乙二胺(CoCl 2(TMEDA))、氯化鎳四甲基-1,3-丙二胺(NiCl 2(TMPDA))或碘化鎳四甲基-1,3-丙二胺(NiI 2(TMPDA))之至少一者。
在本發明的某些實施例中，使該基材接觸含過渡金屬鹵化合物的一第一氣相反應物，即是所述含有加合物形成配位基的過渡金屬鹵化物可包括將該基材暴露(即是，接觸)於該過渡金屬鹵化物介於約0.01秒和約60秒、介於約0.05秒和約10秒或介於約0.1秒和約5.0秒之間的時間。此外，在過渡金屬鹵化合物的脈衝期間，該過渡金屬鹵化合物的流動速率可小於2000sccm、小於500sccm或甚至小於100sccm。此外，在該過渡金屬鹵化合物在基材上的脈衝期間，該過渡金屬鹵化合物的流動速率範圍可從約1至2000sccm、從約5至1000sccm或從約10至約500sccm。
過量的過渡金屬鹵化合物和反應副產物(如存在)可例如藉由使用惰性氣體泵吸而從表面去除。例如，在本發明的某些實施例中，該等方法可包括一沖洗循環，其中沖洗基材表面時間小於約2.0秒。藉助於流體連通反應腔的一泵吸系統所產生的真空可去除過量的過渡金屬鹵化合物和任何反應副產物。
在沉積循環的一第二階段中，所述基材可接觸一第二氣相反應物，所述第二氣相反應物包含一氧前驅體、一氮前驅體、一矽前驅體、一硫前驅體、一硒前驅體、一磷前驅體、一硼前驅體或一還原劑之至少一者。在某些實施例中，所述第二氣相反應物可包含一氧前驅體，而且藉由本說明書揭露的週期性沉積方法所沉積的含過渡金屬薄膜可包含一過渡金屬氧化物。在某些實施例中，所述第二氣相反應物可包含一還原劑，下面將更詳細描述，而且藉由本說明書揭露的週期性沉積方法所沉積的含過渡金屬薄膜可包含一元素過渡金屬。在某些實施例中，所述第二氣相反應物可包含一氮前驅體，而且藉由本說明書揭露的週期性沉積方法所沉積的含過渡金屬薄膜可包含一過渡金屬氮化物。在某些實施例中，所述第二氣相反應物可包含一矽前驅體，而且藉由本說明書揭露的週期性沉積方法所沉積的含過渡金屬薄膜可包含一過渡金屬矽化物。在某些實施例中，所述第二氣相反應物可包含一硫前驅體，而且藉由本說明書揭露的週期性沉積方法所沉積的含過渡金屬薄膜可包含一過渡金屬硫化物。在某些實施例中，所述第二氣相反應物可包含一硒前驅體，而且藉由本說明書揭露的週期性沉積方法所沉積的含過渡金屬薄膜可包含一過渡金屬硒化物。在某些實施例中，所述第二氣相反應物可包含一磷前驅體，而且藉由本說明書揭露的週期性沉積方法所沉積的含過渡金屬薄膜可包含一過渡金屬磷化物。在某些實施例中，所述第二氣相反應物可包含一硼前驅體，而且藉由本說明書揭露的週期性沉積方法所沉積的含過渡金屬薄膜可包含一過渡金屬硼化物。
在本發明的實施例中，其中所述第二氣相反應物包含一氧前驅體，所述氧前驅體可包含臭氧(O 3)、氧分子(O 2)、氧原子(O)、氧電漿、氧自由基、氧受激態物、水(H 2O)或過氧化氫(hydrogen peroxide)(H 2O 2)之至少一者。
在本發明的實施例中，其中所述第二氣相反應物包含一氮前驅體，所述氮前驅體可包含氨(NH 3)、肼(hydrazine)(N 2H 4)、三氮烷(tertbutylhydrazine)(N 3H 5)、叔丁基肼(tertbutylhydrazine)(C 4H 9N 2H 3)、甲肼(methylhydrazine)(CH 3NHNH 2)、二甲肼(dimethylhydrazine)((CH 3) 2N 2H 2)或一氮電漿或含氫的氮電漿之至少一者。
在一些實施例中，所述第二氣相反應物可包含一烴取代肼前驅體。在沉積循環的一第二階段(取代肼相)中，使該基材接觸一含有烴取代肼前驅體的第二氣相反應物。在本發明的某些實施例中，方法可更包括選擇該取代肼以包含具有至少四(4)個碳原子的烷基(alkyl group)，其中「烷基」是指至少四(4)個碳原子長度的飽和或不飽和烴鏈，諸如，但沒有限於丁基、戊基、己基、庚基和辛基及其異構體，諸如這些的n-(正-)、iso-(異-)、sec-(第二-)和tert-(第三-)異構體。所述烷基可為直鏈或支鏈，而且可包括烷基的所有結構異構體形式。在某些實施例中，烷基鏈(alkyl chain)可被取代。在本發明的某些實施例中，烷基-肼可包含至少一氫鍵結氮。在本發明的某些實施例中，烷基-肼可包含至少二個氫鍵結氮。在本發明的某些實施例中，烷基-肼可包含至少一氫鍵結氮與至少一烷基鏈鍵結氮。在本發明的某些實施例中，所述第二反應物可包含一烷基-肼，而且可更包含叔丁基肼(tertbutylhydrazine)(C 4H 9N 2H 3)、二甲肼(dimethylhydrazine)或二乙基肼(diethylhydrazine)之一或多者。在本發明的某些實施例中，取代肼具有至少一烴基相連氮。在本發明的某些實施例中，取代肼具有至少二個烴基相連氮。在本發明的某些實施例中，取代肼具有至少三個烴基相連氮。在本發明的某些實施例中，取代肼具有至少一C1-C3烴基相連氮。在本發明的某些實施例中，取代肼具有至少一C4-C10烴基相連氮。在本發明的某些實施例中，取代肼具有直鏈、支鏈或環狀或芳香烴基相連氮。在本發明的某些實施例中，取代肼包含取代烴基相連氮。
在本發明的某些實施例中，所述取代肼具有下化學式II： [化學式2] R IR II-N-NR IIIR IV,                   (II) 其中R I可選自於由烴基，諸如直鏈、支鏈、環狀、芳族或取代烴基，而且R II、R III、 R IV基之每一者可獨立選擇為氫或烴基，諸如直鏈、支鏈、環狀、芳族或取代烴基。
在化學式(II)的某些實施例中，R I、R II、 R III、R IV之每一者可為C1-C10烴、C1-C3烴、C4-C10烴或氫，諸如直鏈、支鏈、環狀、芳族或取代烴基。在某些實施例中，R I、R II、R III、R IV基之至少一者包含芳基，諸如苯基。在某些實施例中，R I、R II、R III、 R IV基之至少一者包含甲基、乙基、正丙基、異丙基、正丁基、異丁基、仲丁基、叔丁基或苯基。在某些實施例中，每個R I、 R II、R III、R IV基之至少兩者可獨立選擇成包含甲基、乙基、正丙基、異丙基、正丁基、異丁基、仲丁基、叔丁基或苯基。在某些實施例中，R II、R III、 R IV基是氫。在某些實施例中，R II、R III、 R IV基之至少兩者是氫。在某些實施例中，R II、R III、R IV基之至少一者是氫。在某些實施例中，全部 R II、R III、R IV基都是烴。
在本發明的實施例中，其中所述第二氣相反應物包含一矽前驅體，所述矽前驅體可包含矽烷(silane)(SiH 4)、二矽烷(disilane)(Si 2H 6)、三矽烷(trisilane)(Si 3H 8)、四矽烷(tetrasilane)(Si 4H 10)、異戊矽烷(isopentasilane)(Si 5H 12)或新戊矽烷(neopentasilane)(Si 5H 12)之至少一者。在本發明的實施例中，其中所述第二氣相反應物包含一矽前驅體，所述矽前驅體可包含一C1-C4烷基矽烷。在所述第二氣相反應物包含一矽前驅體之本發明的實施例中，所述矽前驅體可包含來自矽烷族的一前驅體。
在本發明的實施例中，其中所述第二氣相反應物包含一硼前驅體，所述硼前驅體可包含硼烷(BH 3)、二硼烷(B 2H 6)或其他硼烷之至少一者，諸如十硼烷(B 10H 14)。
在本發明的實施例中，其中所述第二氣相反應物包含一氫前驅體，所述氫前驅體可包含H 2、H原子、H-離子、H-電漿或H-自由基之至少一者。
在本發明的某些實施例中，所述第二氣相反應物包含一磷前驅體、一硫前驅體或一硒化物前驅體。在某些實施例中，所述硫前驅體包含氫和硫。在某些實施例中，所述硫前驅體是一烷基硫化合物。在某些實施例中，所述第二反應物包含元素硫、H 2S、(CH 3) 2S、(NH 4) 2S、((CH 3) 2SO)和H 2S 2之一或多者。在某些實施例中，所述硒前驅體是一烷基硒化合物。在某些實施例中，所述第二反應物包含元素硒、H 2Se、(CH 3) 2Se和H 2Se 2之一或多者。在某些實施例中，所述硒前驅體包含氫和硒。在某些實施例中，所述第二反應物可包含Te、Sb、Se的烷矽基化合物，諸如(Me3Si)2Te、(Me3Si)2Se或(Me3Si)3Sb。在某些實施例中，所述磷前驅體是一烷基磷化合物。在某些實施例中，所述第二反應物包含元素磷、PH 3或烷基膦之一或多者，諸如甲膦。在某些實施例中，所述磷前驅體包含氫和磷。
在本發明的實施例中，其中所述第二氣相反應物包含一有機前驅體，諸如一還原劑，例如，可使用醇、醛或羧酸或其他有機化合物，例如不含金屬或半金屬的有機化合物，但是包含-OH基。醇可為伯醇(primary alcohol)、仲醇(secondary alcohol)、叔醇(tertiary alcohol)、多羥基醇(polyhydroxy alcohol)、環醇(cyclic alcohol)、芳醇和醇的其他衍生物。
伯醇具有一-OH基相連到鍵結另一碳原子的一碳原子，特別是根據通用化學式(III)的伯醇： [化學式3] R1-OH                      (III) 其中R1是一直鏈或支鏈C1-C20烷基或烯基，諸如甲基、乙基、丙基、丁基、戊基或己基。伯醇的實例包括甲醇、乙醇、丙醇、丁醇、2-甲基丙醇和2-甲基丁醇。
仲醇具有一-OH基相連到鍵結於兩個其他碳原子的一碳原子。特別是，仲醇具有通用化學式(IV)： [化學式4] OH ｜ R1-CH-R1                              (IV) 其中每個R1是獨立選自於直鏈或支鏈C1-C20烷基和烯基的群組，諸如甲基、乙基、丙基、丁基、戊基或己基。仲醇的實例包括2-丙醇和2-丁醇。
叔醇具有一-OH基相連到鍵結於三個其他碳原子的一碳原子。特別是，叔醇具有通用化學式(V)： [化學式5] OH ｜ R1-C-R1                                (V) ｜ R1 其中每個R1是獨立選自於直鏈或支鏈C1-C20烷基和烯基的群組，諸如甲基、乙基、丙基、丁基、戊基或己基。叔醇的一實例是叔丁醇。
諸如二元醇和三元醇的多羥基醇具有如前述的伯醇、仲醇及/或叔醇基。多羥基醇的實例是乙二醇和甘油。
環狀醇具有一-OH基相連到1至10(諸如5-6)個碳原子環之一部分的至少一碳原子。
芳醇具有相連一苯環或支鏈中的一碳原子的至少一-OH基。
有機前驅體可包含至少一醛基(-CHO)，其是選自於由具有通用化學式(VI)的化合物、具有通用化學式(VII)的烷基化合物、鹵代醛及醛的其他衍生物所組成的群組。
因此，在一實施例中，有機前驅體是具有通用化學式(VI)的醛： [化學式6] R3-CHO                                 (VI)  其中R3是選自於由氫和直鏈或支鏈C1-C20烷基和烯基所組成的群組，諸如甲基、乙基、丙基、丁基、戊基或己基。在某些實施例中，R3是選自於由甲基和乙基所組成的群組。根據化學式(VI)的示例性化合物但沒有限於甲醛、乙醛和丁醛。
在另一實施例中，有機前驅體是具有通用化學式(VII)的醛： [化學式7] OHC-R4-CHO                       (VII) 其中R4是一直鏈或支鏈C1-C20飽和或不飽和烴。或者，醛基可彼此直接鍵結(R4是無功能)。
含有至少一-COOH基的有機前驅體可選自於由通用化學式(VIII)、多羧酸、鹵代羧酸及羧酸的其他衍生物之化合物所組成的群組。
因此，在一實施例中，有機前驅體是具有通用化學式(VIII)的羧酸： [化學式8] R5-COOH                       (VIII) 其中R5是氫或直鏈或支鏈C1-C20烷基或烯基，諸如甲基、乙基、丙基、丁基、戊基或己基，例如甲基或乙基。在某些實施例中，R5是一直鏈或支鏈C1-C3烷基或烯基。根據化學式(VII)的化合物之實例是甲酸(formic acid)、丙酸(propanoic acid)和乙酸(acetic acid)，在某些實施例中是甲酸(HCOOH)。
在本發明的某些實施例中，將基材暴露(即是，接觸)於所述第二氣相反應物包括使所述第二氣相反應物在基材上脈衝介於0.1秒和2.0秒之間或從約0.01秒至約10秒，或小於約20秒、小於約10秒或小於約5秒的時間。在所述第二氣相反應物在基材上脈衝期間，所述第二氣相反應物的流動速率可小於50sccm、小於25 sccm、小於15 sccm或甚至小於10sccm。
過量的第二氣相反應物和反應副產物(如存在)可例如藉由沖洗氣體脈衝及/或由一泵吸系統產生的真空而從基材表面去除。沖洗氣體最好是任何惰性氣體，諸如但沒有限於氬(Ar)、氮(N 2)、氦(He)；或在某些情況下，可使用氫(H 2)。如果介入沖洗法(即是，沖洗氣體脈衝)或其他反應物去除步驟，通常認為一階段緊接另一階段。
在沉積含過渡金屬薄膜達到想要厚度之前，基材交替接觸所述第一氣相反應物(即是，金屬鹵化合物)和所述第二氣相反應物(例如，一氧前驅體)的沉積循環可重複一或多次。應明白，在本發明的某些實施例中，使該基材接觸所述第一氣相反應物和所述第二氣相反應物的順序可使得該基材先接觸所述第二氣相反應物，然後接觸所述第一氣相反應物。此外，在某些實施例中，週期性沉積處理可包括先使該基材接觸所述第一氣相反應物一或多次，然後使該基材接觸所述第二氣相反應物一或多次；而且同樣地，可替代性包括使該基材先接觸所述第二氣相反應物一或多次，然後使該基材接觸所述第一氣相反應物一或多次。
此外，本發明的某些實施例可包含非電漿反應物，例如，所述第一和第二氣相反應物基本上不含離子化反應物。在某些實施例中，所述第一和第二氣相反應物基本上不含離子化反應物、受激態物或自由基物。例如，所述第一氣相反應物和所述第二氣相反應物兩者可包含非電漿反應物，以防止基材的電離損壞及由此產生的相關缺陷。當基材包含製造或至少部分製造易碎性半導體器件結構時，使用非電漿反應物可能特別有用，因為高能電漿物可能損壞及/或使器件性能特性惡化。
在本發明的某些實施例中，本發明的示例週期性沉積方法可包括其他處理步驟，包括使該基材接觸一含有還原劑的第三氣相反應物。在某些實施例中，所述還原劑可包含氫(H 2)、氫(H 2)電漿、氨(NH 3)、氨(NH 3)電漿、肼(N 2H 4)、矽烷(SiH 4)、二矽烷(Si 2H 6)、三矽烷(Si 3H 8)、鍺烷(GeH 4)、二鍺烷(Ge 2H 6)、硼烷(BH 3)、二硼烷(B 2H 6)、叔丁基肼(C 4H 12N 2、一硒前驅體、一硼前驅體、一磷前驅體、一硫前驅體、一有機前驅體(例如，醇、醛或羧酸)或一氫前驅體之至少一者。在本發明的某些實施例中，本發明的示例週期性沉積方法可包括使該基材接觸一當作還原劑的第二氣相反應物(沒有任何其他前驅體/反應物接觸步驟)。
所述含有還原劑的第三氣相反應物可引入反應腔中，而且在一示例週期性沉積方法中的多個處理階段下接觸基材。在本發明的某些實施例中，所述還原劑可引入反應腔中，而且接觸從所述第一氣相反應物分開及從所述第二氣相反應物分開的基材。例如，所述還原劑可先引入反應腔而且在使該基材接觸所述第一氣相反應物接觸之前接觸基材，然後使該基材接觸所述第一氣相反應物而且在使該基材接觸所述第二氣相反應物之前及/或在使該基材接觸所述第二氣相反應物之後。在本發明的某些實施例中，所述還原劑可引入反應腔中而且使該基材同時接觸所述第一氣相反應物及/或同時接觸所述第二氣相反應物。例如，該還原劑和所述第一氣相反應物可共同流入反應腔中而且同時接觸基材，及/或該還原劑和所述第二氣相反應物可共同流入反應腔中而且同時接觸基材。
在本發明的某些實施例中，所述第一氣相反應物可包含一過渡金屬鹵化合物，而且所述第二氣相反應物可包含一氧前驅體。在此實施例中，週期性沉積處理可在基材上沉積一過渡金屬氧化物。如一非限制性實例所示，所述第一氣相反應物可包含CoCl 2(TMEDA)，所述第二氣相反應物可包含水(H 2O)，而且沉積在該基材上的薄膜可包含氧化鈷。在某些實施例中，可藉由將該過渡金屬氧化物暴露於一還原劑而進一步處理所述過渡金屬氧化物。在某些實施例中，所述過渡金屬氧化物可暴露於至少一還原劑，包括形成氣體(H 2+ N 2)、氨(NH 3)、肼(N 2H 4)、分子氫(H 2)、氫原子(H)、一氫電漿、氫自由基、氫受激態物、醇、醛、羧酸、硼烷或胺。
在某些實施例中，將所述過渡金屬氧化物暴露於一還原劑可將該過渡金屬氧化物還原成一元素過渡金屬。如一非限制性實例所示，本發明的週期性沉積處理可用於沉積厚度50奈米的氧化鈷薄膜，而且氧化鈷薄膜可在1000毫巴(mbar)的壓力和約250°C溫度下暴露於10%形成氣體，以將氧化鈷薄膜還原成元素鈷。在本發明的某些實施例中，所述過渡金屬氧化物具有的厚度可小於500奈米、小於100奈米、小於50奈米、小於25奈米、小於20奈米、小於10奈米或甚至小於5奈米。在某些實施例中，所述過渡金屬氧化物可暴露於還原劑少於5小時、少於1小時、少於30分鐘、少於15分鐘、少於10分鐘、少於5分鐘或甚至少於1分鐘。在某些實施例中，所述過渡金屬氧化物可在低於500°C、低於400°C、低於300°C、低於250°C、低於200°C或甚至低於150°C 的基材溫度下暴露於還原劑。在某些實施例中，所述過渡金屬氧化物可在減壓大氣中暴露於還原劑，其中壓力可為從約0.001毫巴至約10巴或從約1毫巴至約1000毫巴。
本說明書所述的週期性沉積處理(利用一第一氣相反應物包含一過渡金屬鹵化合物和一第二氣相反應物以沉積一含過渡金屬薄膜)可在具有加熱基材的ALD或CVD沉積系統中進行。例如，在某些實施例中，方法可包括將該基材加熱至介於約80°C和約150°C之間的溫度，或甚至將該基材加熱至介於約80°C和約120°C之間的溫度。當然，諸如針對ALD反應的任何特定週期性沉積處理的適當溫度窗口將取決於所涉及的表面鈍化和反應物。在本說明書，溫度隨著所使用的前驅體而變化，而且通常是在或低於約700°C。在某些實施例中，針對氣相沉積處理的沉積溫度通常是在或高於約100°C，在某些實施例中，沉積溫度是介於約100°C和約300°C之間，而且在某些實施例中，沉積溫度是介於約120°C和約200°C之間。在某些實施例中，沉積溫度是低於約500°C、低於約400°C、低於約350°C或低於約300°C。在某些情況下，沉積溫度可低於約300°C、低於約200°C或低於約100°C。在某些情況下，沉積溫度可高於約20°C、高於約50°C和高於約75°C。在本發明的某些實施例中，沉積溫度(即是，沉積期間的基材溫度)是約275°C。
在某些實施例中，所述含過渡金屬薄膜的生長速率是從約0.005 Å/循環至約5 Å/循環、從約0.01 Å/循環至約2.0Å/循環。在某些實施例中，所述含過渡金屬薄膜的生長速率大於約0.05 Å/循環、大於約0.1 Å/循環、大於約0.15 Å/循環、大於約0.20Å/循環、大於約0.25 Å/循環或大於約0.3 Å/循環。在某些實施例中，所述含過渡金屬薄膜的生長速率小於約2.0Å/循環、小於約1.0Å/循環、小於約0.75 Å/循環、小於約0.5 Å/循環或小於約0.2 Å/循環。在本發明的某些實施例中，所述含過渡金屬薄膜的生長速率可為約0.4 Å/循環。
本發明的實施例可包括如圖1的示例週期性沉積方法100更詳細示意說明的週期性沉積。該週期性沉積方法100可從處理步驟110開始，包括將至少一基材提供到一反應腔中而且將該基材加熱到沉積溫度。例如，該基材可包括一或多個部分製造的半導體器件結構，該反應腔可包括一原子層沉積反應腔，而且該基材可被加熱到約小於275°C的沉積溫度。此外，反應腔內的壓力可控制成在反應腔中提供減少的大氣。例如，在週期性沉積處理期間的反應腔內的壓力可小於1000毫巴、小於100毫巴、小於10毫巴、小於5毫巴或在某些情況下甚至小於1毫巴。
該週期性沉積方法100可繼續於處理步驟120，包括使該基材接觸一過渡金屬鹵化合物，例如，該基材接觸所述過渡金屬鹵化合物約1秒的時間。在本發明的某些實施例中，所述過渡金屬化合物可接觸基材介於約0.01秒和約60秒、介於約0.05秒和約10秒或介於約0.1秒和約5秒之間的時間。此外，在過渡金屬前驅體於基材上的脈衝期間，所述過渡金屬前驅體的流動速率可小於2000sccm、小於1000sccm、小於500sccm、小於200sccm或甚至小於100sccm。
在使該基材接觸所述過渡金屬鹵化合物時，可藉由沖洗/泵處理去除反應腔中的過量金屬前驅體和任何反應副產物。
該週期性沉積方法100可繼續於處理步驟130，包括使基材接觸一第二氣相反應物，諸如(例如)一氧前驅體、一氮前驅體、一矽前驅體、一磷前驅體、一硒前驅體、一硼前驅體或一還原劑。所述第二氣相反應物(例如，水)可接觸基材約4秒的時間。在本發明的某些實施例中，所述第二氣相反應物可接觸基材介於約0.01秒和約60秒、介於或約0.05秒和約10秒、介於或約0.1秒和約5.0秒之間的時間。此外，在所述第二氣相反應物在基材上的脈衝期間，所述第二氣相反應物的流動速率可小於2000sccm、小於1000sccm、小於500sccm、小於200sccm或甚至小於100sccm。
在使該基材接觸所述第二氣相反應物前驅體時，可藉由一沖洗/泵處理去除反應腔中的過量第二氣相反應物和任何反應副產物。
該基材交替及順序接觸所述過渡金屬鹵化合物(處理步驟120)及接觸所述第二氣相反應物(處理步驟130)的示例週期性沉積方法100可構成一沉積循環。在本發明的某些實施例中，沉積一含過渡金屬薄膜的方法可包括重複沉積循環一或多次。例如，該週期性沉積方法100可繼續於一判斷步驟140，判斷該週期性沉積方法100是否經由處理步驟150繼續或退出。判斷步驟140是基於所沉積過渡金屬薄膜的厚度進行判斷，例如，如果含過渡金屬薄膜的厚度不足用於想要的器件結構，則該週期性沉積方法100可返回處理步驟120，而且使基材接觸所述過渡金屬鹵化合物及使基材接觸所述第二氣相反應物的處理可重複一或多次。一旦含過渡金屬薄膜已沉積到想要厚度，該方法可經由處理步驟150退出，而且含過渡金屬薄膜和基底半導體結構可經歷其他處理以形成一或多個器件結構。
包含根據本說明書描述的某些實施例沉積的過渡金屬之薄膜或層可為連續薄膜。在某些實施例中，包含根據本說明書所述某些實施例沉積的過渡金屬之薄膜在低於約100奈米、低於約60奈米、低於約50奈米、低於約40奈米、低於約30奈米、低於約25奈米、低於約20奈米、低於約15奈米、低於約10奈米、低於約5奈米或更低的厚度下可為連續。本說明書意指的連續性可為實質連續性或電連續性。在某些實施例中，一薄膜可實質連續的厚度可不同於一薄膜是電連續的厚度，而且一薄膜可電連續的厚度可不同於一薄膜實質連續的厚度。
在某些實施例中，根據本說明書描述的某些實施例沉積的一含過渡金屬薄膜可具有從約20奈米至約100奈米的厚度。在某些實施例中，根據本說明書描述的某些實施例沉積的一含過渡金屬薄膜可具有從約20奈米至約60奈米的厚度。在某些實施例中，根據本說明書描述的某些實施例沉積的一含過渡金屬薄膜可具有大於約20奈米、大於約30奈米、大於約40奈米、大於約50奈米、大於約60奈米、大於約100奈米、大於約250奈米、大於約500奈米或更大的厚度。在某些實施例中，根據本說明書描述的某些實施例沉積的一含過渡金屬薄膜可具有小於約50奈米、小於約30奈米、小於約20奈米、小於約15奈米、小於約10奈米、小於約5奈米、小於約3奈米、小於約2奈米或甚至小於約1奈米的厚度。
在本發明的某些實施例中，所述含過渡金屬薄膜可沉積在三維結構上，例如，一包含高縱橫比特徵的非平面基材。在某些實施例中，所述含過渡金屬薄膜的步階式覆蓋率在具有大於約2、大於約5、大於約10、大於約25、大於約50或甚至大於約100的縱橫比(高度/寬度)結構中可等於或大於約50%、大於約80%、大於約90%、大於約95%、大於約98、大於約99%或更大。
在本發明的某些實施例中，根據本發明的實施例沉積的含過渡金屬薄膜可包含小於約50%原子氧、小於約25%原子氧、小於約10%原子氧、小於約5%原子氧、小於約2%原子氧或甚至小於約1%原子氧。在進一步實施例中，所述含過渡金屬薄膜可包含小於約5%原子氫、小於約2%原子氫、小於約1%原子氫或甚至小於約0.5%原子氫。在仍進一步實施例中，所述含過渡金屬薄膜可包含小於約5%原子碳、小於約2%原子碳、小於約1%原子碳或甚至小於約0.5%原子碳。在仍進一步的實施例，所述含過渡金屬薄膜可包含少於約5%原子滷化物、少於約2%原子滷化物、少於約1%原子滷化物或甚至少於約0.5%原子滷化物。在某些實施例中，所述含過渡金屬材料的原子%可利用飛行時彈反衝探測分析(Time of Flight Elastic Recoil Detection Analysis，ToF-ERDA)來決定。
在本發明的某些實施例中，本發明的週期性沉積處理可用於沉積一過渡金屬氧化物，諸如(例如)氧化鈷。用於諸如原子層沉積的週期性沉積處理之先前鈷前驅體已證明對水(H 2O)不起反應，因此臭氧(O 3)通常已用為氧前驅體。然而，臭氧用於週期性沉積氧化鈷通常導致形成氧化鈷(II,III)(Co 3O 4)而不是氧化鈷(II)(CoO)。在某些實施例中，沉積CoO而不是沉積Co 3O 4可能是有益的，例如，CoO形式的鈷之較低氧化態可更容易還原成鈷金屬。因此，在本發明的某些實施例中，本發明的週期性沉積處理可用於基本上沉積鈷(II)氧化物(CoO)薄膜，即是，其中鈷與氧的比率基本上等於1：1。在本發明的某些實施例中，週期性沉積處理期間的沉積溫度可能影響沉積薄膜的化學計量。例如，當利用本說明書揭露的週期性沉積處理沉積氧化鈷薄膜時，基材溫度可能影響在沉積薄膜中的鈷和氧的比率(Co：O)。因此，如本發明的一非限制性示例實施例所示，可將CoCl 2(TMEDA)當作鈷前驅體使用及將水(H 2O)當作氧前驅體使用來沉積氧化鈷薄膜。在此一週期性沉積處理期間，基材溫度可受控制在約275°C，此可能導致沉積具有約1：1的鈷和氧比率(Co：O)的氧化鈷(II)(CoO)。
藉由本說明書揭露的週期性沉積處理沉積的含過渡金屬薄膜可用於各種環境中，諸如(例如)襯層、覆蓋層、間隙填充層、溝槽填充層、晶種層、接觸層/接觸填充層、電遷移改善層、後段處理(back-end-of-line，BEOL)應用的導電互連及用於半導體器件接點的矽化物形式。在某些實施例中，本發明的含過渡金屬薄膜可用為一電極或一電極的至少一部分，其構造成用於提供電流給一或多個器件結構。在本發明的某些實施例中，本發明的含過渡金屬薄膜在CMOS器件應用中可當作一或多個CMOS器件的至少一部分電極使用。
如一非限制性示例實施例所示，一諸如(例如)鈷的含過渡金屬薄膜在後段處理(BEOL)金屬化應用中可當作一阻隔材料及/或一覆蓋層使用，如圖2所示。更詳細地，圖2示意說明一部分製造的半導體器件結構200，其包含基材202，該基材可包含部分製造及/或製造的半導體器件結構，諸如電晶體和記憶體元件(未示出)。該部分製造的半導體器件結構200可包括在含有低介電常數材料(即是，一低k介電質)的基材202上形成的一介電材料204，諸如一含矽介電質或一金屬氧化物。一溝槽可形成在介電質材料204，而且一阻隔材料206可配置在防止或基本上防止金屬互連材料208擴散到周圍介電質材料204的溝槽表面上。在本發明的某些實施例中，阻隔材料206可包括藉由本說明書描述的週期性沉積處理沉積的鈷。在本發明的某些實施例中，該鈷薄膜可具有小於35埃、25埃或甚至15埃的厚度。該部分製造的半導體器件結構200可亦包括一金屬互連材料208，用於電互連配置在基材202中的數個器件結構。在某些實施例中，該金屬互連材料208可包括銅或鈷之一或多者。除了使用鈷做為一阻隔材料，鈷也可用來作為一覆蓋層。因此，請即參考圖2，該部分製造的半導體器件結構200可亦包括直接配置在該金屬互連材料208的上表面上的一覆蓋層210。該覆蓋層210可用於防止該金屬互連材料208的氧化，而且重要的是，在後續的處理中，防止該金屬互連材料208擴散到在該部分製造的半導體器件結構200上形成的附加介電質材料，即是，針對多層互相連構。在本發明的某些實施例中，該覆蓋層210可亦包括鈷，其厚度小於20埃、小於15埃或甚至小於10埃。在某些實施例中，金屬互連材料208、阻隔材料206和覆蓋層210可整個形成一電極，用於電互連在該基材202中配置的複數個半導體器件。
本發明的實施例可亦用於合成對氣相沉積處理很有用的化學前驅體，諸如(例如)原子層沉積、化學氣相沉積和週期性化學氣相沉積。因此，本發明的實施例可包括用於合成一含有加合物形成配位基的過渡金屬鹵化合物之方法，如先前本說明書的描述，諸如(例如)一包括含雙牙氮加合物配位基之過渡金屬鹵化合物。在某些實施例中，本發明的方法可用於合成氯化鈷(II)(TMEDA)、氯化鎳(II)(TMEDA)或氯化銅(II)(TMEDA)之一或多者。在某些實施例中，本發明的方法可用於合成碘化鈷(II)(TMEDA)、碘化鎳(II)(TMEDA)或碘化銅(II)(TMEDA)之一或多者。在某些實施例中，本發明的方法可用於合成溴化鈷(II)(TMEDA)、溴化鎳(II)(TMEDA)或溴化銅(II)(TMEDA)之一或多者。此外，在某些實施例中，本發明的方法可用於合成氯化鈷(II)(TMPDA)、氯化鎳(II)(TMPDA)和氯化銅(II)(TMPDA)。
下面描述揭露一種用於合成CoCl 2(TMEDA)的方法，應瞭解，所揭露用於合成CoCl 2(TMEDA)的方法同樣適用於本說明書揭露的另外過渡金屬鹵化合物的合成方法，而且不應該被解釋為限制。
該化學前驅體合成方法可利用標準希莱克(Schlenk)技術和一惰性氣體(例如，N 2或Ar)手套箱而使用在嚴格排除空氣和水分的情況下實現所有處理和操作下進行。無水CoCl 2(99%)和N,N,N`,N`-四甲基乙二胺(TMEDA)(99%)是當作反應物使用。此外，二氯甲烷(CH 2Cl 2)是當作一適宜溶劑使用，該處理包括在4Å分子篩上使CH 2Cl 2脫氧和乾燥。
在本發明的某些實施例中，一定量CoCl 2可經由計量及添加到適宜器皿中，諸如Schlenk瓶。一定量CH 2Cl 2可添加到CoCl 2。隨後，一化學計量TMEDA可滴式添加到溶液中。在某些實施例中，例如TMEDA的加合物形成配位基可加入過量的滷化物，諸如(例如)，大於鹵化物量的2倍、5倍或甚至10倍量。可將所得懸浮液在室溫下攪拌約1小時。如一非限制性實例所示，6.00g(46.211 mmol)CoCl 2可經由計量及連同100ml的CH 2Cl 2添加到Schlenk瓶。可將5.37g(46.211 mmol)TMEDA添加到溶液中，而且在室溫下攪拌1小時。可將所得藍色溶液蒸發至乾，產生一藍色粗製產物。可將所得粗製產物轉移至一昇華器，其中產物在介於約150-200°C的溫度下可昇華，藉此產生CoCl 2(TMEDA)。在本發明的某些實施例中，所得揮發性過渡金屬鹵化合物，例如CoCl 2(TMEDA)，可具有小於5%、小於2%、小於1%、小於0.1%或甚至小於0.01%的百分比雜質濃度。在本發明的某些實施例中，相較於有機過渡金屬前驅體，該揮發性過渡金屬鹵化合物可具有一較高的分解溫度。例如，本發明的過渡金屬鹵化合物可具有大於150°C或甚至大於200°C的分解溫度。
因此，在本發明的某些實施例中，一過渡金屬鹵化合物可合成用於含過渡金屬薄膜的氣相沉積。在某些實施例中，含有加合物形成配位基的金屬鹵化合物可利用一單步合成方法合成，所述方法包括在低於約50°C、低於約30°C或甚至低於約15°C的溫度下組合一過渡金屬鹵化合物和一加合物形成配位基，其中整個合成處理可在小於5小時、小於2小時、小於1小時或甚至小於30分鐘的時間內完成。
本發明的實施例可亦包括氣相沉積裝置，其包括構造成包含過渡金屬鹵化合物及將一過渡金屬鹵化合物供應給反應腔之一或多個前驅體來源器皿。因此，在本發明的某些實施例中，提供利用反應揮發性化學物質的氣相沉積裝置。該裝置可包括：一反應腔；一基材，其配置在該反應腔內；一前驅體來源器皿，其係流體連通該反應腔；及一過渡金屬鹵化合物，其包含配置在該前驅體來源器皿中的一含配位基的雙牙氮。
更詳細地，圖4示意說明一包含反應腔402的氣相沉積裝置400。應注意，圖4是該氣相沉積裝置400的簡化示意圖，而且不包含每個及每一元素，即是，諸如每個但沒有限於閥、電連接、質量流量控制器、密封件和氣體導管，其都可使用在本發明的該氣相沉積裝置400中。在本發明的某些實施例中，該反應腔402可包括一構造成用於支撐在反應腔內的基材406之基座404。一噴灑頭氣體分配器408亦配置在反應腔中，用於選擇性將基材暴露於各種氣體。
在本發明的某些實施例中，一前驅體來源器皿410A可經由導管或其他適當氣體導管412A流體連通至該反應腔402，而且可進一步耦接至一歧管、閥控制系統、質量流量控制系統或機構，以控制源自該前驅體來源器皿410A的一氣態前驅體。該前驅體來源器皿410A可構造成儲存一包括含有配位基的雙牙氮之過渡金屬鹵化合物。在某些實施例中，該前驅體來源器皿410A可包括一石英材料，其對於儲存在該前驅體來源器皿410A內的過渡金屬鹵化合物基本上是化學惰性。在本發明的替代性實施例中，該前驅體來源器皿410A可利用一防腐蝕金屬或金屬合金製成，諸如(例如)赫史特合金(Hastelloy)、蒙乃爾合金(Monel)或其組合。
在本發明的某些實施例中，該前驅體來源器皿410A可更包括構造成加熱儲存在該前驅體來源器皿410A中的過渡金屬鹵化合物的一或多個加熱單元414。在某些實施例中，該一或多個加熱單元400可用於將所述過渡金屬鹵化合物加熱至約大於0°C、約大於20°C、約大於100°C、約大於150°C、約大於200°C、約大於200°C、約大於300°C或甚至約大於400°C的溫度。在某些實施例中，該一或多個加熱單元414可構造成將儲存在該前驅體來源器皿410A中的過渡金屬鹵化合物加熱至約170°C的溫度。
在某些實施例中，有關該前驅體來源器皿410A的一或多個加熱單元414構造成將所述過渡金屬鹵化合物從固態轉化成液態或氣態。在某些實施例中，有關該前驅體來源器皿410A的一或多個加熱單元414可用於控制儲存在該前驅體來源器皿410A中的過渡金屬鹵化合物的黏度。在某些實施例中，有關該前驅體來源器皿410A的一或多個加熱單元414可構造成控制由儲存在該前驅體來源器皿內的過渡金屬鹵化合物產生的蒸氣壓。在本發明的某些實施例中，該過渡金屬鹵化合物在大於25°C、大於50°C或甚至大於100°C的溫度下可具有大於0.01毫巴的蒸氣壓。在本發明的某些實施例中，該過渡金屬鹵化合物在小於350°C、小於250°C、小於200°C或甚至小於150°C的溫度下可具有大於0.01毫巴的蒸氣壓。在本發明的某些實施例中，該過渡金屬鹵化合物在大於25 °C或甚至大於100°C的溫度下可具有大於0.1毫巴的蒸氣壓。在本發明的某些實施例中，該過渡金屬鹵化合物可在低於400°C、低於200°C或甚至低於100°C的溫度下具有大於0.1毫巴的蒸氣壓。在本發明的某些實施例中，該過渡金屬鹵化合物在大於25 °C或甚至大於100°C的溫度下可具有大於1毫巴的蒸氣壓。例如，可將過渡金屬鹵化合物加熱至高於150°C的溫度，藉此產生大於0.001毫巴的蒸氣壓。
在某些實施例中，儲存在該前驅體來源器皿410A內的過渡金屬鹵化物416可包含氯化鈷(TMEDA)或氯化鎳(TMEDA)之至少一者。在某些實施例中，儲存在該前驅體來源器皿410A內的過渡金屬鹵化物416可包括碘化鈷(TMEDA)。在某些實施例中，儲存在該前驅體來源器皿410A內的過渡金屬鹵化物416可包含。此外，在某些實施例中，儲存在該前驅體來源器皿410A內的過渡金屬鹵化物416可包含氯化鈷(TMPDA)和氯化鎳(TMPDA)。
在本發明的某些實施例中，一氣流通道418可連接於前驅體來源器皿410A，以將一或多種載氣從一或多個載氣儲存器皿(未示出)經由氣流通道418輸送到該前驅體來源器皿。在某些實施例中，一質量流量控制器(未示出)可置放在該氣流通道418上而且配置接近該前驅體來源器皿410A。例如，一質量流量控制器可經校準，以控制進入該前驅體來源器皿410A的載氣質量通量，藉此允許較大程度控制從該前驅體來源器皿410A流出到該反應腔402的過渡金屬鹵化合物蒸汽的隨後流動。
在某些實施例中，所述載氣(例如，氫氣、氮氣、氦氣、氬氣及其混合物)可在所述過渡金屬鹵化合物416的暴露表面上流動，藉此從所述過渡金屬鹵化合物吸收一部分蒸氣，而且將所述過渡金屬鹵化合物、連同載氣一起輸送到該反應腔402。在本發明的替代實施例中，所述載氣可例如藉由選擇性蒸氣通道418`，透過所述過渡金屬鹵化物416形成「鼓泡」，藉此攪拌及拾取一部分過渡金屬鹵化合物416，而且經由氣體導管412A將所述過渡金屬鹵化合物蒸氣輸送到該反應腔402。
在本發明的某些實施例中，該氣相沉積裝置400可包括其他前驅體來源器皿及用於惰性沖洗氣體的一或多個來源器皿。例如，前驅體來源器皿410B可構造成含有一第二氣相反應物，諸如(例如)一氧前驅體、一氮前驅體、一硫前驅體、一硒前驅體、一磷前驅體、一硼前驅體、一矽前驅體或一還原劑之一或多者。該前驅體來源器皿410B中包含的所述第二氣相反應物可經由氣體導管412B輸送到該反應腔402。在某些實施例中，該前驅體來源器皿410B可亦具有用於控制儲存在該前驅體來源器皿410B內的前驅體溫度的相關聯加熱器414。此外，來源器皿410C可用於含有一惰性沖洗氣體，諸如(例如)但沒有限於氬氣(Ar)、氮(N 2)或氦(He)。儘管該氣相沉積系統400包括三個來源器皿，但應明白，可構造成連同該反應腔402使用的含有另外化學前驅體的其他來源器皿。
在本發明的某些實施例中，該氣相沉積裝置400可更包括一提供電子電路和機械組件以選擇性操作閥、歧管、泵的系統操作和控制機構420、與有關該氣相沉積裝置400的其他設備。此電路和化合物用於從各自的前驅體來源器皿410A、410B和沖洗氣體器皿410C引入前驅體、沖洗氣體。該系統操作和控制機構420可亦控制氣體脈衝時序、基材和反應腔的溫度及反應腔的壓力與提供該氣相沉積裝置400適當操作的所需各種其他操作。該系統操作和控制機構420可包括控制軟體和電氣或氣動控制閥，以控制前驅體、反應物和沖洗氣體流入和流出該反應腔402。所述控制系統可包括諸如軟體及/或硬體組件的模組，例如，執行某些工作的FPGA或ASIC。一模組可特別構造成存在控制系統的可定址儲存媒體，而且可構造成執行一或多個處理。
熟習該項技藝者應明白，目前氣相沉積裝置的其他配置是可能，包括不同數量和種類的前驅體反應物來源和沖洗氣體來源。此外，熟習該項技藝者將亦明白，存有許多閥、導管、前驅體來源、沖洗氣體來源的配置，其可用於實現將氣體選擇性供應給反應腔402的目標。此外，如一氣相沉積裝置的示意圖，為了簡化說明，已省略許多組件，而且這類組件可包括例如各種閥、歧管、淨化器、加熱器、容器、通風口及/或旁路管。
圖4所示的氣相沉積裝置400可用於將包括含雙牙氮加合物配位基之過渡金屬鹵化合物供應給一氣相沉積工具。該方法可包括：提供一構造成含有該過渡金屬鹵化合物的前驅體來源器皿；流體連通該前驅體來源器皿與一反應腔；將該前驅體來源器皿中所含的過渡金屬鹵化合物加熱至高於150°C的溫度；產生該至少0.001毫巴的過渡金屬鹵化合物的蒸氣壓；及將該過渡金屬鹵化合物供應給該反應腔。在本發明的某些實施例中，該過渡金屬鹵化合物在大於25°C、大於50°C或甚至大於100°C的溫度下可具有大於0.01毫巴的蒸氣壓。在本發明的某些實施例中，該過渡金屬鹵化合物在小於350°C、小於250°C、小於200°C或甚至小於150°C的溫度下可具有大於0.01毫巴的蒸氣壓。在本發明的某些實施例中，該過渡金屬鹵化合物在大於25°C或甚至大於100°C的溫度下可具有大於0.1毫巴的蒸氣壓。在本發明的某些實施例中，該過渡金屬鹵化合物在低於400°C、低於200°C或甚至低於100°C的溫度下可具有大於0.1毫巴的蒸氣壓。在本發明的某些實施例中，該過渡金屬鹵化合物在大於25°C或甚至大於100°C的溫度下可具有大於1毫巴的蒸氣壓。
在某些實施例中，該過渡金屬鹵化合物可包含氯化鈷(TMEDA)或氯化鎳(TMPDA)之至少一者。
上述本發明的示例實施例沒有限制本發明的範疇，因為這些實施例僅是本發明之實施例的示例，而且是由文後申請專利範圍及其適法性的類似請求項限制。任何等同實施例都在本發明的範疇內。實際上，除了本說明書所示和所述之類以外，本發明的各種修改，諸如所述元素的替代有用組合，熟習該項技藝者可從描述中能更明白。這些修改和實施例亦在文後申請專利範圍的範疇內。
100:週期性沉積方法 110:處理步驟 120:處理步驟 130:處理步驟 140:判斷步驟 150:處理步驟 200:半導體器件結構 202:基材 204:介電材料 206:阻隔材料 208:金屬互連材料 210:覆蓋層 400:氣相沉積裝置 402:反應腔 404:基座 406:基材 408:噴灑頭氣體分配器 410A:前驅體來源器皿 410B:前驅體來源器皿 410C:來源器皿/沖洗氣體器皿 412A:氣體導管 412B:氣體導管 412C:氣體導管 414:加熱單元 416:過渡金屬鹵化物 418:氣流通道 418`:蒸氣通道 420:系統操作和控制機構
儘管本說明書以具體指出且明確主張視為本發明之實施例的申請專利範圍作結，但在結合隨附圖式理解時可更容易自本揭示之實施例之某些實例的描述來確定本揭示之實施例的優勢，在隨附圖式中： [圖1]示意說明根據本發明的實施例之示例週期性沉積處理的處理流程； [圖2]示意說明一示例性器件結構包含根據本發明所沉積含過渡金屬薄膜的示意圖； [圖3]示意說明在本發明的週期性沉積處理中使用的過渡金屬鹵化合物之實例； [圖4]示意說明根據本發明的實施例之示例性氣相沉積裝置的示意圖。
100:週期性沉積方法
110:處理步驟
120:處理步驟
130:處理步驟
140:判斷步驟
150:處理步驟

Claims (20)

  1. 一種利用反應揮發性化學物質的氣相沉積裝置，該裝置包含：反應腔；基材，其設置在該反應腔中；前驅體來源器皿，其與該反應腔流體連通；及過渡金屬鹵化合物，其含有設置在該前驅體來源器皿中的含雙牙氮加合物配位基。
  2. 如請求項1所述之裝置，其中該加合物配位基包含兩個氮原子，其中每個氮原子鍵結至少一個碳原子。
  3. 如請求項1所述之裝置，其中該過渡金屬鹵化合物包含過渡金屬氯化物化合物。
  4. 如請求項3所述之裝置，其中該過渡金屬氯化物化合物包含氯化鈷、氯化鎳或氯化銅之至少一者。
  5. 如請求項4所述之裝置，其中該過渡金屬氯化物化合物包含氯化鈷(TMEDA)或氯化鎳(TMPDA)之至少一者。
  6. 如請求項1所述之裝置，其中在過渡金屬鹵化合物高於150℃的溫度下，該過渡金屬鹵化合物表現出大於0.001毫巴的蒸氣壓。
  7. 如請求項1所述之裝置，其中該含雙牙氮加合物配位基經配置以配位該過渡金屬鹵化合物的過渡金屬原子，且其中鹵原子鍵結該金屬原子。
  8. 如請求項1所述之裝置，其進一步包含載氣儲存器皿，該載氣儲存器皿包含與該前驅體來源器皿流體連通的載氣。
  9. 如請求項8所述之裝置，其中該載氣包含氫氣、氮氣、氦氣及氬氣之至少一者。
  10. 如請求項8所述之裝置，其進一步包含使該載氣流體耦接到該 前驅體來源器皿的氣流通道。
  11. 如請求項10所述之裝置，其中該氣流通道設置在該前驅體來源器皿內的包含該過渡金屬鹵化合物的液態過渡金屬鹵化物中，使得該載氣可流過該氣流通道並進入該液態過渡金屬鹵化物，其中該載氣經配置以響應該液態過渡金屬鹵化物的鼓泡而拾取一部分該過渡金屬鹵化合物並使該過渡金屬鹵化合物輸送到該反應腔。
  12. 如請求項1所述之裝置，其進一步包含與該反應腔流體連通的第二前驅體來源器皿。
  13. 如請求項12所述之裝置，其進一步包含設置在該第二前驅體來源器皿中的第二氣相反應物。
  14. 如請求項13所述之裝置，其中該第二氣相反應物包含氧前驅體、氮前驅體、矽前驅體、硫前驅體、硒前驅體、磷前驅體、硼前驅體或還原劑之至少一者。
  15. 如請求項14所述之裝置，其中該第二氣相反應物包含該氧前驅體，該氧前驅體包含臭氧(O3)、氧分子(O2)、氧原子(O)、氧電漿、氧自由基、氧受激態物、水(H2O)和過氧化氫(H2O2)之至少一者。
  16. 如請求項14所述之裝置，其中該第二氣相反應物包含該還原劑，該還原劑包含形成氣體(H2+N2)、氨(NH3)、肼(N2H4)、分子氫(H2)、氫原子(H)、氫電漿、氫自由基、氫受激態物、醇、醛、羧酸、硼烷或胺之至少一者。
  17. 請求項13所述之裝置，其進一步包含與該反應腔流體連通的惰性氣體器皿。
  18. 如請求項17所述之裝置，其進一步包含設置在該惰性氣體器皿中的惰性氣體，其中該惰性氣體包含氮氣、氦氣及氬氣之至少一者。
  19. 如請求項4所述之裝置，其進一步包含系統操作和控制機構， 該系統操作和控制機構經配置以控制該過渡金屬鹵化合物及第二氣相反應物進出該反應腔的流量。
  20. 如請求項19所述之裝置，其進一步包含複數個閥及泵，其中該系統操作和控制機構與該複數個閥及泵之至少一者電子連通，以控制該過渡金屬鹵化合物及該第二氣相反應物進出該反應腔的流量。
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