TW202204662A - 用於沉積鉬層之方法及系統 - Google Patents

用於沉積鉬層之方法及系統 Download PDF

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TW202204662A
TW202204662A TW110125581A TW110125581A TW202204662A TW 202204662 A TW202204662 A TW 202204662A TW 110125581 A TW110125581 A TW 110125581A TW 110125581 A TW110125581 A TW 110125581A TW 202204662 A TW202204662 A TW 202204662A
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molybdenum
transition metal
reactant
precursor
reaction chamber
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保羅 瑪
羅格海葉 洛特菲
李在範
艾瑞克 克里斯多福 史帝芬斯
阿密特 米夏拉
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荷蘭商Ａｓｍ Ｉｐ私人控股有限公司
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Abstract

所揭示者係用於將鉬層形成至一基材的一表面上之方法及系統以及使用該等方法形成之結構及裝置。例示性方法包括在形成該鉬層之前形成一底層。該底層可用於操縱鉬層中之應力及/或降低形成鉬層之步驟的成核溫度及/或沉積溫度。

Description

用於沉積鉬層之方法及系統
本揭露大致上係關於適於在基材表面上形成層之方法及系統，並關於包括該等層之結構。更具體而言，本揭露係關於用於形成包括鉬之層的方法和系統，且關於使用該等方法及系統所形成的結構。
電子裝置（諸如半導體裝置）之縮放已導致積體電路的性能及密度之顯著改進。然而，習知的裝置縮放技術對未來技術節點而言面對重大的挑戰。
例如，一挑戰係找到適合的傳導材料，用於金屬間隙填充應用、襯墊應用及類似者，其展現所欲之特性，諸如所欲之有效電阻率、低沉積溫度及/或特性（例如，膜應力）之可調性。因此，所欲的是用於形成具有一或多種此類特性之金屬層的改良方法及系統。
本節提出之任何討論（包括問題及解決方案的討論）僅為了提供本揭露背景脈絡之目的而包括在本揭露中。此類討論不應視為承認資訊之任何或全部內容在完成本發明時已知或以其他方式構成先前技術。
本章節以簡化形式介紹選取的概念，其可於下文以進一步細節描述。本發明內容並非意欲必然地鑑別所主張主題之關鍵特徵或基本特徵，亦非意欲用以限制所主張主題的範疇。
本揭露之各種實施例係關於形成包括鉬層的結構之方法，關於使用此類方法所形成之結構，且關於用於執行該等方法及/或用於形成該等結構之系統。鉬層可用於各種應用中，包括間隙填充（例如，用於互補金屬氧化物半導體（CMOS））應用，其用作襯墊或障壁層（例如，用於3D-NAND或DRAM字線）應用，用於互連應用等。此外，如下文更詳細陳述，與用以沉積鉬層的傳統技術相比，本揭露的實例可用於在相對低溫度下沉積鉬層。
根據本揭露之例示性實施例，揭示一種形成一結構之方法。形成該結構之例示性方法包括提供一基材；形成一底層在該基材的一表面上，該底層包含一過渡金屬硫化物、一過渡金屬碳化物及一過渡金屬氮化物之一或多者；及形成覆蓋該底層之一鉬層。該過渡金屬可為第4族至第7族過渡金屬-例如，選自由以下組成之群組：鈦、鎢、鉬、釩、鈮、鉭、鈷、鉿及鋯。根據本揭露之實例，該底層之一厚度為大於0 nm且小於10 nm、約1至10 nm、約1至5 nm或大於5 nm且小於10 nm。根據額外實例，形成該底層之該步驟包含一循環沉積製程。循環沉積製程可包括提供一過渡金屬前驅物至一反應室；提供一碳反應物、一硫反應物及一氮反應物之一或多者至該反應室；及提供一還原反應物至該反應室。形成鉬層之步驟可包括循環沉積製程。在形成該底層及/或形成該鉬層之該步驟期間的一溫度可係小於650°C、小於600 °C、小於550°C、小於500 °C、在約300 °C與600 °C之間、在約300 °C與650 °C之間、在約300 °C與550 °C之間、在約300 °C與500 °C之間或在約300 °C與450 °C之間。在一些情況中，在形成底層之步驟期間之基材的溫度可係小於在形成鉬層之步驟期間之溫度。在形成鉬層之步驟期間，反應室內之壓力可係小於760托、約0.2至約300托、約0.5至約60托或約20至約80托。在形成底層之步驟期間，反應室內之壓力可係約1至約760托、約0.2至約300托、約0.5至約50托或約0.5至約20托。在形成底層之步驟期間，反應室內之壓力可係小於在形成鉬層之步驟期間之壓力（例如，在上文指定的範圍內）。
依據本揭露之尚有進一步例示性實施例，一種結構係使用如本文所述之方法形成。該結構可包括一基材、形成上覆於該基材的一底層及形成上覆於該底層的一鉬層。底層可用以操縱隨後形成之鉬層中之應力及/或增進鉬層之成核，且藉此降低在形成上覆於底層之鉬層之步驟期間所使用之沉積溫度（例如，基材之溫度）。鉬層可用於各種應用，包括間隙填充、作為襯墊或障壁、作為互連或類似者。
依據本揭露之尚有額外的實例，揭示一種用以執行如本文中所述之方法及/或用以形成一結構或其部份的系統。
所屬技術領域中具有通常知識者將從已參照隨附圖式之某些實施例的下列詳細描述輕易明白這些及其他實施例。本發明並未受限於任何所揭示具體實施例。
下文所提供之方法、結構、裝置及系統之例示性實施例的描述僅係例示性且僅係意欲用於說明之目的；下列描述並非意欲限制本揭露或申請專利範圍之範疇。此外，列舉具有所陳述特徵之多個實施例不意欲排除具有額外特徵之其他實施例或納入所陳述特徵之不同組合的其他實施例。舉例而言，各種實施例係提出作為例示性實施例，並可列舉於附屬項中。除非另有註明，例示性實施例或其等之組件可用各種組合來組合或可彼此分開應用。
如下文更詳細提出，本揭露之各種實施例提供用於形成適於各種應用之結構之方法。例示性方法可用以例如形成鉬層、合適的間隙填充應用、互連應用、障壁或襯墊應用或類似者。然而，除非另有註明，本發明不必然受限於此類實例。
在本揭露中，「氣體(gas)」可包括在常溫及常壓(NTP)下為氣體之材料、汽化固體及/或汽化液體，並可取決於上下文由單一氣體或氣體混合物構成。除了製程氣體以外的氣體（亦即，未通過氣體分配總成、其他氣體分配裝置或類似者而引入的氣體）可用於例如密封反應空間，且可包括諸如稀有氣體的密封氣體。在一些情況下，用語「前驅物(precursor)」可指參與生成另一化合物的化學反應之化合物，且具體係指構成膜基質或膜的主要骨架之化合物；用語「反應物(reactant)」可與用語前驅物互換地使用。用語「惰性氣體(inert gas)」可指不參與化學反應及/或不會在可察覺的程度上變為膜基質之一部分的氣體。例示性的惰性氣體包括氦、氬及其等之任何組合。在一些情況下，惰性氣體可包括氮及/或氫。
如本文所使用，用語「基材(substrate)」可指可用以形成或在其上可形成裝置、電路或膜之任何（多個）下伏材料。基材可包括塊材（諸如矽（例如單晶矽））、其他IV族材料（諸如鍺）或其他半導體材料（諸如II-VI族或III-V族半導體材料），並可包括上覆或下伏於塊材的一或多層。進一步地，基材可包括各種特徵，諸如形成在基材之一層的至少一部分之內或之上的凹部、突起部及類似者。舉實例而言，一基材可包括塊材半導體材料及上覆於該塊材半導體材料之至少一部分的一絕緣或介電材料層。
如本文所使用，用語「膜(film)」及/或「層(layer)」可指任何連續或不連續的結構及材料，諸如，藉由本文所揭示之方法沉積之材料。例如，膜及/或層可包括二維材料、三維材料、奈米粒子，或甚至是部分或完整分子層或部分或完整原子層或原子及/或分子團簇。膜或層可包含具有針孔的材料或層，其可係至少部分連續的。
如本文所使用，「結構(structure)」可係或可包括如本文所述之基材。結構可包括上覆於基材之一或多個層，諸如根據本文所述之方法形成的一或多個層。
用語「循環沉積製程(cyclic deposition process/cyclical deposition process)」可指將前驅物（及/或反應物）循序引入反應室中以在基材上方沉積層，並包括處理技術，諸如原子層沉積(ALD)、循環化學氣相沉積（循環CVD）及包括ALD成分及循環CVD成分之混合循環沉積製程。術語方法與製程可互換地使用。
用語「原子層沉積(atomic layer deposition)」可指氣相沉積製程，其中沉積循環（一般係複數個接續的沉積循環）係在製程室中實施。當使用（多個）前驅物/（多個）反應性氣體及（多個）沖洗（例如惰性載體）氣體的交替脈衝執行時，如本文中所使用之用語原子層沉積亦意指包括由相關用語指定的製程，諸如化學氣相原子層沉積、原子層磊晶(ALE)、分子束磊晶(MBE)、氣體源MBE或有機金屬MBE及化學束磊晶。
通常，對ALD製程而言，在各循環期間，前驅物係引入反應室且經化學吸附至沉積表面（例如，可包括來自先前ALD循環之先前經沉積材料或其他材料的基材表面），並形成不易與額外前驅物起反應（亦即，自限式反應）的材料單層或次單層。其後，在一些情況下，可隨後將反應物（例如，另一前驅物或反應氣體）引入至製程室中，以用於在沉積表面上將經化學吸附之前驅物轉化為所欲材料。反應物可能夠進一步與前驅物起反應。可在一或多個循環期間（例如在各循環之各步驟期間）利用沖洗步驟來從製程室移除任何過量前驅物，且/或從反應室移除任何過量反應物及/或反應副產物。
如本文中所使用，「鉬層」可為可由包括鉬（諸如金屬鉬）之化學式表示之材料層。
如本文中所使用，「鉬前驅物」包括氣體或材料，其可變為氣態且其可由包括鉬的化學式表示。
如本文中所使用，「鹵化鉬前驅物」包括氣體或材料，其可變為氣態且其可由包括鉬及鹵素（諸如氟(F)、氯(Cl)、溴(Br)及碘(I)之一或多者）的化學式表示。
用語「氮反應物(nitrogen reactant)」可指氣體或材料，其可變為氣態且其可由包括氮的化學式表示。在一些情況下，化學式包括氮及氫。在一些情況下，氮反應物不包括雙原子氮。
用語「硫反應物(nitrogen reactant)」可指氣體或材料，其可變為氣態且其可由包括硫的化學式表示。在一些情況下，化學式包括硫及氫。在一些情況下，硫反應物不包括原子硫。
用語「碳反應物(nitrogen reactant)」可指氣體或材料，其可變為氣態且其可由包括碳的化學式表示。在一些情況下，化學式包括碳及氫。
進一步地，在本揭露中，變數之任兩個數字可構成該變數之可工作範圍，且所指示之任何範圍可包括或排除端點。額外地，所指示的變數之任何數值（不管該等數值是否以「約」來指示）可指精確值或近似值並包括等效值，且可指平均值、中間值、代表值、多數值或類似者。進一步地，在本揭露中，於一些實施例中，用語「包括(including)」、「由……構成(constituted by)」及「具有(having)」係獨立地指「一般或廣泛地包含(typically or broadly comprising)」、「包含(comprising)」、「基本上由……組成(consisting essentially of)」或「由……組成(consisting of)」。在本揭露中，於一些實施例中，任何已定義之意義不必然排除尋常及慣例意義。
現轉向圖式，圖1繪示根據本揭露之例示性實施例之形成結構之方法100。方法100包括下列步驟：提供基材（步驟102）、形成底層（步驟104）及形成鉬層（步驟106）。
在步驟102期間，於反應室內提供基材。步驟102期間所用的反應室可係或可包括化學氣相沉積反應器系統的反應室，其經組態以執行循環沉積製程。反應室可係獨立反應室或叢集工具的部分。
步驟102可包括在反應室內將基材加熱至所欲的沉積溫度。在本揭露之一些實施例中，步驟102包括將基材加熱至低於800°C之溫度。例如，在本揭露之一些實施例中，將基材加熱至沉積溫度可包含將基材加熱至介於約20 °C與約800 °C之間、小於650 °C、小於600 °C、小於550 °C、小於500 °C、介於約300 °C與約600 °C之間、介於約300 °C與650 °C之間、介於約300 °C與550 °C、介於約300 °C與500 °C之間或介於約300 °C與450 °C之間之溫度。在一些情況中，步驟102及/或步驟104期間之基材之溫度係小於步驟106期間之基材之溫度。
除了控制基材溫度以外，亦可調節反應室內的壓力。例如，在本揭露之一些實施例中，步驟102及/或步驟104期間之反應室內的壓力可係小於760托、介於約0.2至約300托、介於約0.5至約50托或介於約0.5至約20托之間。在步驟102及/或步驟104期間之反應室內之壓力可係小於在形成鉬層之步驟期間之壓力。步驟102之溫度及壓力為步驟104之合適溫度及壓力。
在步驟104期間，在該基材之一表面上形成一底層，該底層包含一過渡金屬硫化物、一過渡金屬碳化物及一過渡金屬氮化物中之一或多者。底層可使用循環沉積製程形成，諸如循環CVD、ALD或混合式循環CVD/ALD製程。舉例而言，在一些實施例中，特定ALD製程之生長率與CVD製程相較可係低的。一個增加生長率的方法可係以高於ALD製程中典型採用的沉積溫度進行操作，導致一些部份的化學氣相沉積製程，但仍取得循序引入反應物的優勢。此一製程可稱為循環CVD。在一些實施例中，循環CVD製程可包含將二或更多個反應物引入反應室中，其中在反應室中之二或多個反應物之間可存在重疊的時間段，導致同時有沉積的ALD成分及沉積的CVD成分兩者。此係稱為混合式製程。根據進一步的實例，循環沉積製程可包含一個反應物/前驅物的連續流及第二反應物至反應室中之週期性脈衝。
根據本揭露之一些實例，循環沉積製程係熱沉積製程。在此等情況下，循環沉積製程不包括使用電漿以形成用於循環沉積製程中的活化物種。例如，循環沉積製程可不包含氮、硫或碳電漿之形成或使用、可不包含激發氮、硫或碳物種之形成或使用及/或可不包含氮、硫或碳自由基之形成或使用。
在其他情況中，步驟104可包括自一或多種前驅物、反應物及惰性氣體形成激發物種。可使用直接電漿及/或遠端電漿形成激發物種。
循環沉積製程可包括（例如，分開地及／或循序地）提供過渡金屬前驅物至反應室，以及提供反應物至反應室。
適用於步驟104之例示性循環沉積製程200繪示於圖2中。製程200包括以下步驟：提供一過渡金屬前驅物至一反應室（步驟202）；提供一碳反應物、一硫反應物及一氮反應物之一或多者至該反應室（步驟204）；及提供一還原反應物至該反應室（步驟206）。除非另外陳述，否則步驟202至206不需按所繪示之順序執行。例如，製程200可包括步驟202，隨後是步驟206，隨後是步驟204。或者，製程200可僅包括步驟202及204或步驟202及206。
過渡金屬前驅物中之過渡金屬可包括選自第4族至第7族過渡金屬之金屬。舉實例而言，該過渡金屬可選自由以下組成之群組：鈦、鎢、鉬、釩、鈮、鉭、鈷、鉿及鋯。
根據本揭露之進一步實例，該過渡金屬前驅物可包括一過渡金屬鹵化物、一過渡金屬硫族化物鹵化物、一過渡金屬羰基、一過渡金屬有機前驅物及一過渡金屬有機金屬前驅物之一或多者。
舉實例而言，過渡金屬可係或包括鉬。在此情況中，過渡金屬前驅物可包括鹵化鉬、氧鹵化鉬、有機金屬鉬化合物、金屬有機鉬化合物或類似者中之一或多者。
舉特定實例而言，鹵化鉬可選自氟化鉬、氯化鉬、溴化鉬及碘化鉬中之一或多者。鹵化鉬可僅包括鉬及一或多個鹵素。例示性適宜的鹵化鉬包括氯化鉬（MoCl3 ）、四氯化鉬（MoCl4 ）、五氯化鉬（MoCl5 ）、六氯化鉬（MoCl6 ）及六氟化鉬（MoF6 ）之或更多者。
氧鹵化鉬可選自氧鹵化鉬之一或多者，諸如氧氟化鉬、氧氯化鉬、氧溴化鉬及氧碘化鉬之一或多者。氧鹵化鉬可僅包括鉬、氧及一或多個鹵素。舉實例而言，氧鹵化鉬可選自包括溴、氯及碘之一或多者之化合物，且包括三氯化鉬(V)氧化物(MoOCl3 )、四氯化鉬(VI)氧化物(MoOCl4 )、 及二氯二氧化鉬(IV)(MoO2 Cl2 )之一或多者。
額外例示性鉬前驅物包括六羰基鉬(Mo(CO)6 )、四氯（環戊二烯基）鉬、Mo(tBuN)2 (NMe2 )2 、Mo(NBu)2 (StBu)2 、(Me2 N)4 Mo、(iPrCp)2 MoH2 、Mo(NMe2 )4 、Mo(NEt2 )4 、Mo2 (NMe2 )6 、Mo(tBuN)2 (NMe2 )2 、Mo(NtBu)2 (StBu)2 、Mo(NtBu)2 (iPr2 AMD)2 、Mo(thd)3 、MoO2 (acac)2 、MoO2 (thd)2 、MoO2 (iPr2 AMD)2 、Mo(Cp)2 H2 、Mo(iPrCp)2 H2 、Mo(η6 -乙苯)2 、MoCp(CO)2 (η3 -allyl烯丙基)及MoCp(CO)2 (NO)。
例示性過渡金屬（例如，鉬）前驅物可包括「異配位」或混合配位子前驅物，其中任何可得數目（一般來說，3至5配位子，但可存在例外）之例示性配位子類型之任何組合可附接至過渡金屬/鉬原子。在一些情況中，過渡金屬/鉬前驅物包含至少一鹵化物配位子。
相對於使用其他前驅物（諸如金屬有機前驅物）之方法，使用鹵化物及氧鹵化物前驅物或包括至少一鹵化物配位子之前驅物可係有利的，因為此類前驅物（且特別是鹵化物及氧鹵化物前驅物）可相對便宜，可得出具有較低雜質（諸如碳）濃度的鉬層，及/或相較於使用金屬有機或其他鉬或其他過渡金屬前驅物的製程，使用此類前驅物的製程可更加受控。進一步地，此類前驅物可在有或無電漿輔助下用以形成激發物種。此外，相較於使用有機金屬過渡金屬前驅物之方法，使用過渡金屬鹵化物前驅物的製程可更容易放大規模。
在步驟204期間，提供一碳反應物、一硫反應物及一氮反應物之一或多者至該反應室。
例示性氮反應物可選自氮(N2 )、氨(NH3 )、聯胺(N2 H4 )或一聯胺衍生物、氫與氮之一混合物、氮離子、氮自由基及激發氮物種以及其他含氮及氫的氣體之一或多者。氮反應物可包括氮及氫或者由氮及氫組成。在一些情況下，氮反應物不包括雙原子氮。
例示性硫反應物包括硫化氫(H2 S)、硫（例如S8 ）、硫醇（例如烷基及芳基硫醇）、包括二硫化物鍵的化合物、包括硫-烷基鍵的化合物及由式R-S-S-R’或S-R表示的化合物（其中R及R’係獨立地選自脂基（例如C1至C8）及芳香基）、鹵化硫（例如包括一個硫（諸如SCl2 或SBr2 ）或一個鹵化物（諸如二氯化二硫））。烷基硫醇可包括C1至C8烷基硫醇。
例示性碳反應物包括乙炔、乙烯、烷基鹵化物化合物、烯烴鹵化物化合物、金屬烷基化合物及類似者。例示性烷基鹵化物化合物包括CX4 、CHX3 、CH2 X2 、CH3 X，其中X＝F、Cl、Br或I。例示性烯烴鹵化物化合物包括C2 H3 X、C2 H2 X2 、C2 HX3 及C2 X4 ，其中X＝F、Cl、Br或I。例示性炔烴鹵化物化合物包括C2 X2 及HC2 X，其中X＝F、Cl、Br或I。例示性金屬烷基化合物包括AlMe3 、AlEt3 、Al(iPr)3 、Al(iBu)3 、Al(tBu)3 、GaMe3 、GaEt3 、Ga(iPr)3 、Ga(iBu)3 、Ga(tBu)3 、InMe3 、InEt3 、In(iPr)3 、In(iBu)3 、In(tBu)3 及ZnMe2 、ZnEt2 。
在步驟206期間，提供還原反應物至反應室。還原反應物可包括氫、氫自由基、氫離子、具有一式Sin H（ 2n + 2) 之矽烷、具有一式Gen H2n+2 之鍺烷、具有一式Bn Hn+4 或Bn Hn+6 之硼烷、其他硼氫化物、揮發性金屬氫化物及其加成物，諸如DIBAL及R3 N-AlH3 之一或多者，其中R係烷基或芳基，包括擁有能夠與金屬形成鉗合的雜原子的那些。
在一些情況下，二或更多個前驅物及/或二或更多個反應物可流至反應室，使得二或更多個前驅物及/或二或更多個反應物在反應室內重疊。例如，一或多個氮反應物及一或多個碳反應物可共流至反應室。
在熱循環沉積製程的情況下，提供反應物至反應室之步驟的持續時間可相對長，以允許反應物與前驅物或其衍生物起反應。例如，持續時間可係約0.1至約30秒、約1約5秒或約1.5至約10秒。
作為步驟104/製程200的部分，反應室可使用真空及/或惰性氣體沖洗，以例如緩解前驅物/反應物之間的氣相反應，並致能自飽和的表面反應（例如在ALD的情況下）。額外或替代地，可移動基材以分開地接觸第一氣相反應物及第二氣相反應物。在提供前驅物至反應室的步驟之後及/或在提供反應物至反應室的步驟之後及/或在提供還原反應物至反應室的步驟之後，可沖洗反應室及/或移動基材。
在本揭露之一些實施例中，製程200包括重複單位沉積循環，該單位沉積循環包括(1)過渡金屬前驅物至反應室，及(2)提供反應物至反應室，及(3)提供還原反應物至反應室，其中在步驟(1)及/或步驟(2)及/或步驟(3)之後進行可選的沖洗或移動步驟。可基於例如所需的底層厚度重複沉積循環一或多次，例如，大於0 nm且小於10 nm、約1至10 nm、約1至5 nm或大於5 nm且小於10 nm。
一旦該底層已沉積至一所需厚度，方法100繼續進行至步驟106。類似於步驟104，步驟106可包括循環製程。適用於步驟106之例示性循環製程繪示於圖3中，作為製程300。
製程300包括提供鉬前驅物至反應室（步驟302）及提供還原反應物至反應室（步驟304）。
在步驟302期間，將鉬前驅物提供至反應室，例如，與步驟104中所使用的相同反應室。鉬前驅物可係或可包括上述之鉬前驅物之任何者。
如上文所提及，如上所形成之底層之使用可允許在製程300期間相對低的沉積溫度。例如，步驟106/製程300期間之沉積溫度可係小於650 °C、小於600 °C、小於550 °C、小於500 °C、介於約300 °C與600 °C之間、介於約300 °C與650 °C之間、介於約300 °C與550 °C之間、介於約300 °C與500 °C之間或介於約300 °C與450 °C之間。步驟106/製程300期間之反應室內的壓力可係介於約0.2至約300托、約0.5至約60托或約20至約80托之間。如上文所提及，步驟106期間之基材溫度及/或反應室壓力可高於步驟102及/或步驟104期間之基材溫度及/或反應室壓力。
根據本揭露之各種實例，可在步驟104及/或106期間藉由操縱一或多個製程條件，一製程條件，諸如溫度、壓力、前驅物流量率、反應物流量率及是否形成激發物種，可用以操縱鉬層中之應力。例如，底層的使用允許在較低溫度下沉積鉬層。可在步驟104期間（形成底層）操縱製程條件，以操縱上覆鉬層中之應力。在諸如上文所提及之溫度之較低溫度下沉積的鉬層（例如，在介電材料（諸如氧化鋁）上方）相較於沒有底層下及/或較高溫度下沉積的鉬層，允許鉬層具有相對較高的壓縮應力。此外，藉由在步驟104及106期間控制製程條件，可具有鉬層之應力調節及在層中達成至多約450 MPa或大於200 MPa之壓縮應力，用於例如，20 nm鉬層。
具體實例
下文所提供之具體實例僅為例示性且出於說明的目的而呈現。除非另有所指，這些實例並非意欲限制申請專利範圍之範疇。
圖6至圖8繪示使用不同條件形成上覆於氧化鋁層之鉬層的膜應力，其繪示根據本揭露之底層的製程條件及/或特性可如何用於操縱上覆鉬層之應力之實例。圖6繪示沒有底層下所沉積之鉬層的應力值（602）；使用0.25 s鉬前驅物（例如，MoO2 Cl2 ）脈衝、20 s的氮脈衝（例如， NH3 ）、6 s還原劑（例如，H2 ）脈衝、於2托及450 °C下所形成之鉬層的應力值（604）（預處理1）；使用0.25 s鉬前驅物脈衝、60 s還原劑脈衝及0.1 s氮反應物脈衝、於8托及500 °C下所形成之鉬層的應力值（606）（預處理2）；以及1 s鉬前驅物、30 s氮反應物、5 s還原劑、於2托及450 °C下的應力值（608）（預處理3）。該底層厚度係約20埃。在鉬層沉積步驟期間之溫度為約550°C。
圖7繪示在具有不同底層厚度之基材上方沉積之鉬層中的應力。特定言之，應力值係針對形成在氧化鋁層上方的鉬膜而繪示，該氧化鋁層不具有底層（702）、具有約10埃的底層（704）、具有約20埃的底層（706）及約30埃的底層（708）。圖7中形成層之條件相似於預處理1之條件，除了循環數目有所改變之外。
圖8繪示在鉬層沉積期間之溫度效應。特定言之，應力值係針對形成在氧化鋁層上方的鉬膜而繪示，該氧化鋁層不具有底層（802）、鉬形成於約550°C下（804）、鉬形成於約525°C下（806）及鉬形成於約475°C下（808）。形成具有圖8中所繪示之應力值之層的條件與預處理1的條件類似。
在一些實施例中，在具有多於約2、多於約5、多於約10、多於約25、多於約50、多於約100、介於約10與100之間或約5及約25之間之深寬比（高度/寬度）的結構之中/之上，鉬層之步階覆蓋係等於或大於約50%、或大於約80%、或大於約90%、或約95%、或約98%、或約99%或更大。
圖4繪示依據本揭露之額外實例之裝置部分/結構400。裝置部分或結構400包括基材402、鉬層404及底層406，其介於（例如，與一或兩者接觸）基材402及鉬層404之間。
基材402可係或可包括本文所述之基材材料中的任何者。根據本揭露之實例，基材402包括介電層或絕緣層。
介電或絕緣層可包括一或多個介電或絕緣材料層。舉實例來說，介電或絕緣層可係高k材料，諸如例如具有大於約7之介電常數的金屬氧化物。在一些實施例中，高k材料具有的介電常數高於氧化矽的介電常數。例示性高k材料包括下列之一或多者：氧化鉿(HfO2 )、氧化鉭(Ta2 O5 )、氧化鋯(ZrO2 )、氧化鈦(TiO2 )、矽酸鉿(HfSiOx )、氧化鋁(Al2 O3 )、氧化鑭 (La2 O3 )、氮化鈦及包含一或多個此類層之混合物/層合物。
鉬層404及底層406可根據本文所述之方法形成。當底層406使用循環沉積製程形成時，底層406成分（例如，過渡金屬、C、S或N）之濃度可例如藉由控制在一或多個沉積循環期間之前驅物及/或反應物及/或各別的脈衝時間之量而自底層406之底部改變至底層406之頂部。在一些情況中，鉬層404可為鉬金屬。鉬層404之應力可藉由在形成底層406期間改變特性（例如，厚度及/或組成物）及/或製程條件來改變。
鉬層404可包括雜質（諸如鹵化物、氫或類似者），其單獨或組合的量係小於一原子百分比、小於0.2原子百分比、小於0.1原子百分比或小於0.05原子百分比。
額外或替代地，鉬層404可例如使用方法100形成連續膜，其厚度係＜ 5 nm、＜ 4 nm、＜ 3 nm、＜ 2 nm、＜ 1.5 nm、＜ 1.2 nm、＜ 1.0 nm或＜ 0.9 nm。
圖5繪示根據本揭露之尚有額外的例示性實施例之系統500。系統500可用以執行如本文所述之方法或製程及/或形成如本文所述之結構或裝置部分。
在所繪示之實例中，系統500包括一或多個反應室502、前驅物氣體源504、反應物氣體源506、還原反應物源507、沖洗氣體源508、排氣源510及控制器512。
反應室502可包括任何合適的反應室（諸如ALD或CVD反應室）。
前驅物氣體源504可包括容器及單獨或與一或多個載體（例如惰性）氣體混合之如本文所述之一或多個鉬前驅物。反應物氣體源506可包括容器及單獨或與一或多個載體氣體混合之如本文所述之一或多個反應物。還原反應物源507可包括單獨或與一或多個載體氣體混合之一或多個還原反應物。如本文所述，沖洗氣體源508可包括一或多個惰性氣體。雖然經繪示為具有四個氣體源504、506、507及508，系統500可包括任何合適數目的氣體源。例如，系統500可包括另一過渡金屬前驅物源。氣體源504、506、507及508可經由管線514、516、518及519耦接至反應室502，該等管線可各自包括流量控制器、閥、加熱器及類似者。
排氣源510可包括一或多個真空泵。
控制器512包括電子電路系統及軟體，以選擇性地操作閥、歧管、加熱器、泵及包括在系統500中的其他組件。此類電路系統及組件運作以從各別源504、506、507及508引入前驅物、反應物及沖洗氣體。控制器512可控制氣體脈衝序列的時序、基材及/或反應室的溫度及反應室內的壓力以及各種其他操作以提供系統500的合宜操作。控制器512可包括控制軟體以電氣或氣動地控制閥，以控制前驅物、反應物及沖洗氣體進出反應室502的流動。控制器512可包括執行某些任務之模組（諸如軟體或硬體組件，例如FPGA或ASIC）。模組可有利地經組態以常駐在控制系統之可定址儲存媒體上，並經組態以執行一或多個製程。
系統500可包括一或多個遠端激發源520及/或直接激發源522，諸如遠端及/或直接電漿生成設備。
系統500之其他組態係可行的，包括不同數目及種類的前驅物及反應物源以及沖洗氣體源。進一步地，將理解閥、導管、前驅物源及沖洗氣體源有許多配置，其等可用以實現將氣體選擇性饋入反應室502的目標。進一步地，作為一系統示意圖示，為了容易繪示已省略許多組件，且此類組件可包括例如各種閥、歧管、純化器、加熱器、容器、通氣孔及/或旁路。
在反應器系統500之操作期間，基材（諸如半導體晶圓（未繪示））係從例如基材搬運系統傳遞至反應室502。一旦將（多個）基材傳遞至反應室502，來自氣體源504、506、507及508之一或多個氣體（諸如前驅物、反應物、載體氣體及/或沖洗氣體）引入反應室502中。
上文所述之本揭露之實例實施例並不限制本發明之範疇，由於此等實施例僅為本發明之實施例之實例，本發明之範疇由隨附之申請專利範圍及其法定等效物界定。任何等效實施例皆意欲在本發明之範疇內。實際上，除本文中所示及所述者以外，所屬技術領域中具有通常知識者可由本說明書明白本揭露之各種修改（諸如所述元件之替代可用組合）。此類修改及實施例亦意欲落在隨附之申請專利範圍的範疇內。
100:方法 102,104,106:步驟 200:製程 202,204,206:步驟 300:製程 302,304:步驟 400:裝置部分或結構 402:基材 404:鉬層 406:底層 500:系統 502:反應室 504:前驅物氣體源 506:反應物氣體源 507:還原反應物源 508:沖洗氣體源 510:排氣源 512:控制器 514,516,518,519:管線 520:遠端激發源 522:直接激發源 602,604,606,608:應力值 702,704,706,708:應力值 802,804,806,808:應力值
當結合下列闡釋性圖式考慮時，可藉由參照實施方式及申請專利範圍而得到對本揭露之實施例的更完整理解。 ［圖1］繪示根據本揭露之例示性實施例之方法。 ［圖2］繪示根據本揭露之例示性實施例之製程。 ［圖3］繪示根據本揭露之例示性實施例之製程。 ［圖4］繪示根據本揭露之實例之結構。 ［圖5］繪示根據本揭露之額外的例示性實施例之反應器系統。 ［圖6至圖8］繪示根據本揭露之實例所形成之膜及結構中的鉬膜應力。 應瞭解，圖中之元件係為簡單且清晰起見而繪示且不必然按比例繪製。舉例而言，圖中之元件中之一些之尺寸可相對於其他元件而言放大以幫助改善對所繪示本揭露實施例的理解。
100:方法
102,104,106:步驟

Claims (21)

  1. 一種形成一結構之方法，該方法包含下列步驟： 提供一基材； 在該基材之一表面上形成一底層，該底層包含一過渡金屬硫化物、一過渡金屬碳化物及一過渡金屬氮化物中之一或多者；及 形成覆蓋該底層之一鉬層。
  2. 如請求項1之方法，其中該底層包含該過渡金屬氮化物。
  3. 如請求項1或2之方法，其中該底層包含選自一第4族至第7族過渡金屬之一過渡金屬。
  4. 如請求項1至3中任一項之方法，其中該底層之一厚度為大於0 nm且小於10 nm、約1至10 nm、約1至5 nm或大於5 nm且小於10 nm。
  5. 如請求項1至4中任一項之方法，其中形成該底層的該步驟包含一循環沉積製程。
  6. 如請求項5之方法，其中該循環沉積製程包含： 提供一過渡金屬前驅物至一反應室； 提供一碳反應物、一硫反應物及一氮反應物之一或多者至該反應室；及 可選地提供一還原反應物至該反應室。
  7. 如請求項6之方法，其中該過渡金屬前驅物包含一過渡金屬鹵化物、一過渡金屬硫族化物鹵化物、一過渡金屬羰基、一過渡金屬有機前驅物及一過渡金屬有機金屬前驅物之一或多者。
  8. 如請求項6或7之方法，其中該碳反應物包含乙炔、乙烯、烷基鹵化物化合物、烯鹵化物化合物及金屬烷基化合物之一或多者。
  9. 如請求項6至8中任一項之方法，其中該氮反應物包含氮(N2 )、氨(NH3 )、聯胺(N2 H4 )或一聯胺衍生物、氫與氮之一混合物、氮離子、氮自由基及激發氮物種之一或多者。
  10. 如請求項6至9中任一項之方法，其中該硫反應物包含硫化氫（H2 S）、硫、硫醇、包括二硫鍵之化合物、包括一硫烷基鍵之化合物及由式R-S-S-R’或S-R表示之化合物中之一或多者，其中R及R’獨立地選自脂族及芳族基及硫鹵化物。
  11. 如請求項6至10中任一項之方法，其中該還原反應物包含氫、氫自由基、氫離子、具有一式Sin H(2n + 2) 之矽烷、具有一式Gen H2n+2 之鍺烷及具有一式Bn Hn+4 或Bn Hn+6 之硼烷之一或多者。
  12. 如請求項1至11中任一項之方法，其中形成該鉬層的該步驟包含一循環沉積製程。
  13. 如請求項12之方法，其中該循環沉積製程包含： 提供一鉬前驅物至一反應室；及 提供一還原反應物至該反應室。
  14. 如請求項13之方法，其中該鉬前驅物包含一鹵化鉬、一硫族化鉬鹵化物、一羰基鉬、一金屬有機鉬前驅物及一有機金屬鉬前驅物中之一或多者。
  15. 如請求項13或14之方法，其中該鉬前驅物包含至少一鹵化物配位子。
  16. 如請求項13至15中任一項之方法， 其中該鉬前驅物包含三氯化鉬(MoCl3 )、四氯化鉬 (MoCl4 )、五氯化鉬(MoCl5 )、六氯化鉬(MoCl6 )、六氟化鉬(MoF6 )、六羰基鉬(Mo(CO)6 )、四氯（環戊二烯基）鉬、 三氯化鉬(V)氧化物(MoOCl3 )、四氯化鉬(VI)氧化物(MoOCl4 )、 及二氯二氧化鉬(IV)(MoO2 Cl2 )、Mo(tBuN)2 (NMe2 )2 、Mo(NBu)2 (StBu)2 、(Me2 N)4 Mo、(iPrCp)2 MoH2 、Mo(NMe2 )4 、Mo(NEt2 )4 、Mo2 (NMe2 )6 、Mo(tBuN)2 (NMe2 )2 、Mo(NtBu)2 (StBu)2 、Mo(NtBu)2 (iPr2 AMD)2 、Mo(thd)3 、MoO2 (acac)2 、MoO2 (thd)2 、MoO2 (iPr2 AMD)2 、Mo(Cp)2 H2 、Mo(iPrCp)2 H2 、Mo(η6 -乙苯)2 、MoCp(CO)2 (η3-烯丙基)及MoCp(CO)2 (NO)之一或多者。
  17. 如請求項13至16中任一項之方法，其中在形成該鉬層之該步驟期間的一沉積溫度係小於650°C、小於600 °C、小於550°C、小於500 °C、在約300 °C與650 °C之間、在約300 °C與600 °C之間、在約300 °C與550 °C之間、在約300 °C與500 °C之間或在約300 °C與450 °C之間。
  18. 如請求項1至17中任一項之方法，其中該底層係用以操縱該鉬層內之應力。
  19. 如請求項1至18中任一項之方法，其中該底層為一障蔽層。
  20. 一種結構，其係如請求項1至19中任一項之方法所形成。
  21. 一種反應器系統，用以執行如請求項1至19中任一項之方法。
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