TW202124757A - 生長低電阻率含金屬膜之方法 - Google Patents

生長低電阻率含金屬膜之方法 Download PDF

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TW202124757A
TW202124757A TW109137389A TW109137389A TW202124757A TW 202124757 A TW202124757 A TW 202124757A TW 109137389 A TW109137389 A TW 109137389A TW 109137389 A TW109137389 A TW 109137389A TW 202124757 A TW202124757 A TW 202124757A
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metal
film
substrate
reducing agent
following
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蘭卡摩Ｃ 卡路塔瑞奇
立其 吳
普拉塔姆 偕恩
傑佛瑞Ｗ 安瑟斯
馬克 薩利
鎂 張
大衛 湯普森
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美商應用材料股份有限公司
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Abstract

茲描述使用環1,4-二烯還原劑與金屬前驅物及反應劑來形成含金屬膜。形成含金屬膜之方法包含以下步驟：同步地、部分同步地或分別並依序地，將基板表面暴露於金屬前驅物、還原劑及反應劑，以形成含金屬膜。

Description

生長低電阻率含金屬膜之方法
一般而言，本揭示內容之實施例與沉積金屬膜之方法有關。具體而言，本揭示內容與提供具低電阻率的金屬膜之方法有關。
因微電子裝置小型化之故，半導體製造正成為材料創新的關鍵因素。新材料及用於沉積新材料之製程需要持續創新。二維金屬氧化物半導體(MOS)電晶體裝置的維度正在縮減，並朝著鰭狀三維電晶體的方向發展。隨著電晶體的維度縮減，共形薄膜的沉積和裝置閾值電壓的調節變得更為困難。
類似地，記憶體裝置的維度減小並具有增加的深寬比而達到業界從未見過的範圍。因此，由於內在表面限制了生長製程，通常較佳的是類似原子層沉積(ALD)等沉積方法。此外，因為基於電漿之ALD製程會造成基板損壞和非共形的膜，通常較佳的是熱ALD。
氮化鈦(TiN)膜用於邏輯和記憶體應用。TiN有望成為鎢、釕及鈷之阻障材料。此外，TiN用作高K蓋體且用作閘極層疊中之p型金屬材料。通常，藉由使氯化鈦(TiCl4 )與氨(NH3 )在大於400 ºC之溫度下反應，來沉積熱ALD的TiN膜，以便獲得合適的電阻率之膜。
因此，需要在高深寬比結構上沉積具有低電阻率及/或良好保形性的含金屬膜之方法。需要在較低溫度下沉積含金屬膜之方法。
本揭示內容之一或多個實施例涉及了形成金屬膜之方法。將基板表面暴露於具有金屬之金屬前驅物，所述金屬具有第一氧化態。將基板表面暴露於還原劑，以將所述金屬之第一氧化態降低為第二氧化態。將基板表面暴露於反應劑，以形成含金屬膜，含金屬膜包含以下一或多者：金屬氮化物、金屬碳化物、金屬矽化物或金屬氧化物。
本揭示內容之額外實施例涉及了形成金屬膜之方法。將基板表面暴露於金屬鹵化物前驅物，以於基板表面上形成含金屬層，所述金屬鹵化物前驅物具有金屬，所述金屬具有第一氧化態。將基板表面上之含金屬層暴露於還原劑，以將金屬的第一氧化態降低為第二氧化態，並於基板表面上形成經還原含金屬層。將基板表面上的經還原含金屬層暴露於反應劑，以形成含金屬膜，所述含金屬膜包含以下一或多者：金屬氮化物、金屬碳化物、金屬矽化物或金屬氧化物。
本揭示內容之進一步實施例涉及了形成金屬膜之方法。將基板表面暴露於金屬前驅物、還原劑和反應劑，以形成含金屬膜，所述含金屬膜包含以下一或多者：金屬氮化物、金屬碳化物、金屬矽化物或金屬氧化物。還原劑包含了具有下式之化合物：
Figure 02_image001
。
在描述本揭示內容的數個示例性實施例之前，應瞭解到本揭示內容不受限於下面說明書中所闡述的建置或處理程序的細節。本揭示內容能夠具有其他實施例，並能夠被由各種方式實作或執行。
如在此說明書及隨附申請專利範圍中所使用，術語「基板(substrate)」指的是表面，或表面的部分，其中製程在所述表面或表面的部分上進行。本案所屬技術領域中具通常知識者亦將理解的是，除非上下文另有明確指示，否則參照基板可僅指基板的一部分。此外，對沉積在基板上之參照可指裸基板和具有在其上沉積或形成的一或多個膜或特徵之基板二者。
如本文所用，「基板」指的是任何基板或形成於基板上之材料表面，在製造製程期間，在所述基板或形成於基板上之材料表面上進行膜處理。舉例而言，取決於應用，於上面可進行處理之基板表面可包括：諸如矽、氧化矽、應變矽、絕緣體上矽(SOI)、經碳摻雜的氧化矽、非晶矽、經摻雜的矽、鍺、砷化鎵、玻璃、藍寶石等材料，及任何其他材料(如金屬、金屬氮化物、金屬合金及其它導電材料)。基板可包括，但不限於，半導體晶圓。可將基板暴露於預處理製程，以研磨、蝕刻、還原、氧化、羥基化、退火、UV硬化、電子束硬化及/或烘烤基板表面。除了在基板本身的表面上直接進行膜處理之外，在本揭示內容中，也可在形成於基板上的下方層(underlayer)上進行本文所揭示的任何膜處理程序(如下文更詳細地揭示)，且術語「基板表面」欲包括前後文所指的此類下方層。因此，舉例而言，當膜/層或部分膜/層已被沉積至基板表面上，新沉積之膜/層的暴露表面便成為基板表面。
本揭示內容之實施例涉及用於沉積金屬膜之方法。一些實施例有利地形成電阻率降低之金屬氮化物膜。本揭示內容之一些實施例有利地提供用於沉積含金屬膜之熱原子層沉積(ALD)製程。如以此方式所使用，「熱(thermal)」ALD製程為其中不採用電漿反應劑來沉積膜之原子層沉積製程。熱ALD製程可包括基於電漿之後沉積製程，以控制或修飾膜的某些性質(如，密度)。
本揭示內容的一些實施例有利地降低溫度以獲得目標電阻率及/或較低的總電阻率。本揭示內容之一或多個實施例提供了用於沉積膜之方法，所述方法首先將金屬中心還原成較低的氧化態，並接著與反應劑(如，氨)反應。在一些實施例中，金屬前驅物、還原劑及反應劑同步對基板暴露。在一些實施例中，還原劑對具有金屬前驅物或反應劑中之一者的基板暴露。
在一些實施例中，金屬前驅物、還原劑及反應劑分別且依序地對基板暴露。舉例而言，在一些實施例中，在暴露於下個反應性氣體之前，清除基板表面或製程腔室之反應性氣體。儘管在整個說明書中給出了與鈦膜的形成有關之實例，但本案所屬技術領域中具通常知識者將認知到，本揭示內容不限於鈦，且可使用本文所述之任何合適的金屬。
用於形成氮化鈦膜之範例製程包含：將基板暴露於鈦前驅物(如，TiCl4 )；清除製程腔室或基板表面之未反應的鈦前驅物；將基板暴露於還原劑；清除基板表面的製程腔室之未反應的還原劑；將基板表面暴露於反應劑(如，氨)；及清除基板表面的製程腔室之未反應的反應劑。不受任何特定操作理論的束縛，咸信TiCl4 中之鈦金屬中心一旦被還原(從4+至小於4+氧化態)，新形成的鈦表面變得比4+氧化態更具反應性，從而使氨能更快且更乾淨地與表面反應。(Ti4+ 氧化態為最穩定的形式，且小於4+則沒這麼穩定)。
在一些實施例中，一些實施例的還原劑從TiCl4 吸引Cl，降低了膜的氯化物含量。咸信降低氯化物含量可減小膜電阻率。在一些實施例中，金屬前驅物包含金屬氯化物，且將基板表面暴露於還原劑降低了膜之氯含量。
方案(I)描繪了在一個範例ALD循環期間之反應。
Figure 02_image003
(I)
在一些實施例中，還原劑包含有機矽烷還原劑，且咸信根據方案(II)進行TiCl4 與還原劑之間的反應。
Figure 02_image005
(II)
咸信TiClX 不穩定且對氨有反應性。與氨的可能反應示於以下方案(III)。
Figure 02_image007
(III)
因此，本揭示內容之一或多個實施例涉及形成金屬膜之方法。一些實施例的金屬膜包含金屬原子及以下一或多者：氮原子、碳原子、矽原子或氧原子。
在一些實施例中，將基板表面暴露於具有金屬之金屬前驅物，所述金屬具有第一氧化態。將基板表面暴露於還原劑，以將所述金屬之第一氧化態降低為第二氧化態。將基板表面暴露於反應劑，以形成含金屬膜，含金屬膜包含以下一或多者：金屬氮化物、金屬碳化物、金屬矽化物或金屬氧化物。在一些實施例中，金屬前驅物、還原劑及反應劑同時對基板暴露。例如，在化學氣相沉積(CVD)製程中。在一些實施例中，還原劑與金屬前驅物或反應劑中之一者同時對基板表面暴露。例如，在混合式化學氣相沉積(CVD) – 原子層沉積(ALD)製程中。在一些實施例中，金屬前驅物、還原劑及反應劑分別且依序地對基板表面暴露。例如，在原子層沉積(ALD)製程中。
用於形成金屬膜之方法的一些實施例包含：將基板表面暴露於具有金屬之金屬鹵化物前驅物，以於基板表面上形成含金屬層，所述金屬具有第一氧化態。將基板表面上之含金屬層暴露於還原劑，以將金屬的第一氧化態降低為第二氧化態，並於基板表面上形成經還原含金屬層。將基板表面上的經還原含金屬層暴露於反應劑，以形成含金屬膜，所述含金屬膜包含以下一或多者：金屬氮化物、金屬碳化物、金屬矽化物或金屬氧化物。
金屬前驅物可為任何合適的金屬前驅物。在一些實施例中，金屬前驅物包含金屬鹵化物，所述金屬鹵化物具有通式MXa Rb ，其中M為金屬原子，各個X為獨立地選自F、Cl、Br及I中之鹵素，各個R獨立地選自C1-C6烷基、N-供體配體(N-donor ligand)、CO及環戊二烯基團，a在0至6的範圍內，且b在0至6的範圍內。如以此方式所使用，術語「C1-C6」及使用「C」後接數字意指取代基團具有所指稱之碳原子數。舉例而言，C4烷基團具有四個碳原子。合適的C4烷基團包括正丁基團、異丁基團、三級丁基團。在一些實施例中，b為0。在一些實施例中，b為0，且各個X為相同元素。如以此方式所使用，術語「各個X為相同元素」意指大於或等於約95%、98%、99%或99.5%的鹵素原子包含所指稱之原子。
此方法可擴展到其他金屬，且可使用各種金屬前驅物來獲得低電阻率金屬氮化物。金屬前驅物的金屬原子包含任何合適的金屬物種。在一些實施例中，金屬原子選自週期表的III族至XIV族金屬。合適的金屬物種包括，但不限於：鈧、釔、鑭、鈦、鋯、鉿、釩、鈮、鉭、鉻、鉬、鎢、錳、鎝、錸、鐵、釕、鋨、鈷、銠、銥、鎳、鈀、鉑、銅、銀、金、鋅、鎘、硼、鋁、鎵、銦、鉈、碳、矽、鍺、錫或鉛。
在一些實施例中，金屬原子選自由鈦、鎵或鉭組成之群組。在一些實施例中，金屬前驅物包含以下一或多者：TiCl4 、TaCl4 或GaCl4 。在一些實施例中，金屬前驅物基本上由以下一或多者組成：TiCl4 、TaCl4 或GaCl4 。以此方式所使用，術語「基本上由…組成」意指以莫耳計，金屬前驅物的反應性物種之約95%、98%、99%或99.5%為所指稱物種。在此計算中不考慮載氣惰性。
在一些實施例中，還原劑包含以下一或多者：環1,4-二烯、矽烷、碳矽烷、硼烷、胺基硼烷、氫化錫、氫化鋁或錫(II)化合物。
在一些實施例中，還原劑具有通式：
Figure 02_image009
其中各個R及R’獨立地選自H、C1-C6烷基團、-NR’’ 2 基團及–SiR’’ 3 ，其中R’’選自H、C1-C4支鏈或非支鏈烷基團。
在一些實施例中，還原劑包含具有以下通式之化合物或基本上由具有以下通式之化合物組成：
Figure 02_image011
其中各個R及R’獨立地選自H、C1-C6烷基團、-NR’’ 2 基團及–SiR’’ 3 ，其中R’’選自H、C1-C4支鏈或非支鏈烷基團。
在一些實施例中，還原劑包含還原劑(A)或基本上由還原劑(A)組成：
Figure 02_image001
(A)。
在一些實施例中，金屬物種的第一氧化態為大於或等於2+。在一些實施例中，金屬物種的第一氧化態為大於或等於3+、4+、5+或6+。在一些實施例中，在暴露於還原劑之後的第二氧化態為小於或等於5+、4+、3+、2+、1+或0，且第二氧化態小於第一氧化態。
在一些實施例中，相同的概念用於沉積金屬氧化物、金屬矽化物及金屬碳化物。在一些實施例中，反應劑包含以下一或多者：氮化劑，用以形成金屬氮化物膜；氧化劑，用以形成金屬氧化物膜；矽化劑，用以形成金屬矽化物膜；或碳化劑，用以形成金屬碳化物膜。
在一些實施例中，反應劑包含氮化劑。一些實施例的氮化劑包含氨或基本上由氨組成。在一些實施例中，使用除了氨以外的氮化劑。合適的氮化劑包括，但不限於：聯胺、胺、氮化電漿可被使用。在一些實施例中，反應劑包含以下一或多者：氨、聯胺、胺或氮化電漿。
在一些實施例中，形成金屬氧化物膜。舉例而言，在藉由還原劑還原金屬物種之後，將金屬物種暴露於氧化劑。合適的氧化劑包括，但不限於：水、O2 、O3 、過氧化物、醇或氧化電漿。不受理論束縛，咸信由於與表面物種的高反應性，氧化劑可容易地與表面反應，與沒有還原劑的表面吸收/化學吸附的金屬前驅物反應相比可導致更乾淨的反應；因而產生更純的金屬氧化物膜。
在一些實施例中，形成金屬碳化物膜。為了獲得金屬碳化物，首先可以還原劑還原金屬前驅物並在晶圓表面上形成反應性物種。其後，碳分子暴露會將表面轉化為金屬碳化物。在此步驟期間也可使用電漿處理。
在一些實施例中，形成金屬矽化物膜。為了獲得金屬矽化物，可將矽烷或碳-矽烷對使金屬前驅物與還原劑反應後獲得之表面暴露。具體而言，可藉由使TiCl4與A反應來形成可用作接觸材料之TiSi。在高於400 C的溫度下，矽傾向擴散且可形成TiSi。藉由在TiCl4和A之後導入矽烷可沉積TiSi。這可以ALD脈衝方式，或藉由共同流入前驅物來完成。可使用H2來促進反應。以上TiSi的形成將在經清潔的Si上發生，但不會在SiO或SiN上發生，這是對接觸材料的要求。
在一些實施例中，由還原劑及/或反應劑控制含金屬膜的金屬含量。在一些實施例中，含金屬膜包含富含金屬的含金屬膜。如以此方式所使用，術語「富含金屬(metal-rich)」及類似者意指膜的金屬含量大於基於膜中原子的化學計量比所預期之含量。在一些實施例中，含金屬膜包含富含鈦的氮化鈦膜。在一些實施例中，含金屬膜包含富含鉭的氮化鉭膜。
在一些實施例中，將基板表面暴露於氫(H2 )，以降低含金屬膜的電阻率，及/或減少含金屬膜中之汙染物。在一些實施例中，氫暴露是在預定數量的沉積循環之後進行的後處理製程。各個沉積循環包含暴露於金屬前驅物、還原劑及反應劑。
在一些實施例中，形成經混合的含金屬膜。在一些實施例中，所述方法進一步包含以下步驟：將基板表面暴露於來自金屬前驅物、還原劑或反應劑中之一或多者的超過一種金屬物種，以形成以下一或多者：經混合金屬氮化物、經混合金屬氧化物、經混合金屬碳化物或經混合金屬矽化物膜。藉由使用經混合的金屬前驅物來提供一些實施例的經混合金屬(如，TiCl4 和TaCl4 的混合物提供經混合TiTa膜)。在一些實施例中，藉由還原劑或反應劑提供一或多種金屬。
在小於或等於約500 ºC、450 ºC、400 ºC、350 ºC、300 ºC、250 ºC、200 ºC、150 ºC或100 ºC之溫度下沉積一些實施例的含金屬膜。
根據一些實施例之用於形成含金屬膜的上位方法包含：將金屬前驅物蒸發到ALD腔室，隨後惰性清除過量的金屬前驅物及副產物。接著，將還原劑蒸發並流入腔室。當還原劑與表面結合的金屬前驅物物種交互作用時，金屬中心被還原成較低的氧化態並形成反應性表面。接著，施加惰性氣體清除以去除所有未反應的分子及副產物。其後，將諸如氨之氮化劑輸送至腔室。氨與表面反應而形成金屬氮化物膜。可重複此循環多次以得到期望的厚度。可將腔室壓力及溫度分別維持在從1托耳至10托耳及100 C至500 C。
實例：TiN膜之沉積
以ALD方式利用TiCl4 、還原劑A及氨，以沉積低電阻率TiN膜。在ALD腔室中將氧化矽基板加熱至400 ºC。接著執行以下ALD脈衝序列：0.3秒的TiCl4 脈衝接著10 s氮淨化、2 s的還原劑A脈衝、接著10 s氮淨化及6 s的氨脈衝接著30 s氮淨化。重複循環以沉積具有預定厚度之膜。在不同的溫度下執行此製程，並測量生長率和電阻率。將來自上述製程與基線製程(TiN而無還原劑A)之生長率還有電阻率數據進行比較，顯示生長率明顯增加而電阻率明顯降低。膜的成分分析顯示鈦對氮比例之增加。
在整個說明書中對「一個實施例」、「某些實施例」、「一或多個實施例」或「一實施例」之參照意味著結合該實施例描述之具體特徵、結構、材料或特性包括在本揭示內容之至少一個實施例中。因此，在整個說明書多處出現之片語，如「在一或多個實施例中」、「在某些實施例中」、「在一個實施例中」或「在實施例中」不必然指稱本揭示內容之相同實施例。此外，在一或多個實施例中，具體特徵、結構、材料或特性可以任何方式組合。
儘管已參照特定實施例描述本文之揭示內容，但本案所屬技術領域中具通常知識者將可瞭解這些實施例僅是對本揭示內容之原理和應用的解說。對本案所屬技術領域中具通常知識者而言顯然可對本揭示內容之方法及設備進行各種修飾和變化，而不悖離本揭示內容之精神及範疇。因此，本揭示內容欲包括隨附申請專利範圍及其均等者之範疇內的修飾和變化。
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Claims (20)

  1. 一種形成一金屬膜之方法，該方法包含以下步驟： 將一基板表面暴露於一金屬前驅物，該金屬前驅物具有一金屬，該金屬具有一第一氧化態； 將該基板表面暴露於一還原劑，以將該金屬之該第一氧化態降低為一第二氧化態；以及 將該基板表面暴露於一反應劑，以形成一含金屬膜，該含金屬膜包含以下一或多者：金屬氮化物、金屬碳化物、金屬矽化物或金屬氧化物。
  2. 如請求項1所述之方法，其中該金屬前驅物包含一金屬鹵化物，該金屬鹵化物具有通式MXa Rb ，其中M為一金屬原子，各個X為獨立地選自F、Cl、Br及I中之一鹵素，各個R獨立地選自C1-C6烷基、N-供體配體(N-donor ligand)、CO及環戊二烯基團，a在0至6的範圍內，且b在0至6的範圍內。
  3. 如請求項2所述之方法，其中該金屬原子選自週期表的III族至XIV族金屬。
  4. 如請求項3所述之方法，其中該金屬原子選自由鈦、鎵或鉭所組成之群組。
  5. 如請求項4所述之方法，其中該金屬前驅物包含以下一或多者：TiCl4 、TaCl4 或GaCl4 。
  6. 如請求項1所述之方法，其中該還原劑包含以下一或多者：環1,4-二烯、矽烷、碳矽烷、硼烷、胺基硼烷、氫化錫、氫化鋁或錫(II)化合物。
  7. 如請求項6所述之方法，其中該還原劑具有以下通式：
    Figure 03_image009
    其中各個R及R’獨立地選自H、C1-C6烷基團、-NR’’ 2 基團及–SiR’’ 3 ，其中R’’選自H、C1-C4支鏈或非支鏈烷基團。
  8. 如請求項6所述之方法，其中該還原劑具有以下通式：
    Figure 03_image011
    其中各個R及R’獨立地選自H、C1-C6烷基團、-NR’’ 2 基團及–SiR’’ 3 ，其中R’’選自H、C1-C4支鏈或非支鏈烷基團。
  9. 如請求項6所述之方法，其中該還原劑包含：
    Figure 03_image001
    。
  10. 如請求項9所述之方法，其中該金屬前驅物包含一金屬氯化物，且將該基板表面暴露於該還原劑降低了該膜之氯含量。
  11. 如請求項1所述之方法，其中該反應劑包含以下一或多者：一氮化劑，用以形成一金屬氮化物膜；一氧化劑，用以形成一金屬氧化物膜；矽化劑，用以形成一金屬矽化物膜；或一碳化劑，用以形成一金屬碳化物膜。
  12. 如請求項1所述之方法，其中該含金屬膜包含一富含金屬的金屬氮化物膜。
  13. 如請求項1所述之方法，其中該第一氧化態係大於或等於2+。
  14. 如請求項1所述之方法，其中該反應劑包含以下一或多者：氨、聯胺、胺或氮化電漿。
  15. 如請求項1所述之方法，進一步包含以下步驟：將該基板表面暴露於氫(H2 )，以降低該含金屬膜的電阻率，及/或減少該含金屬膜中之汙染物。
  16. 如請求項1所述之方法，其中將該基板表面依序且分別暴露於該金屬前驅物、該還原劑及該反應劑。
  17. 如請求項1所述之方法，其中將該基板表面暴露於以下二或更多者之共流(coflow)：該金屬前驅物、該還原劑或該反應劑。
  18. 如請求項1所述之方法，進一步包含以下步驟：將該基板表面暴露於來自該金屬前驅物、還原劑或反應劑中之一或多者的超過一種金屬物種，以形成以下一或多者：一經混合金屬氮化物、一經混合金屬氧化物、一經混合金屬碳化物或一經混合金屬矽化物膜。
  19. 一種形成一金屬膜之方法，該方法包含以下步驟： 將一基板表面暴露於一金屬鹵化物前驅物，以於該基板表面上形成一含金屬層，該金屬鹵化物前驅物具有一金屬，該金屬具有一第一氧化態； 將該基板表面上之該含金屬層暴露於一還原劑，以將該金屬之該第一氧化態降低為一第二氧化態，並於該基板表面上形成一經還原含金屬層；以及 將該基板表面上之該經還原含金屬層暴露於一反應劑，以形成一含金屬膜，該含金屬膜包含以下一或多者：金屬氮化物、金屬碳化物、金屬矽化物或金屬氧化物。
  20. 一種形成一金屬膜之方法，該方法包含以下步驟： 將一基板表面暴露於一金屬前驅物、一還原劑及一反應劑，以形成一含金屬膜，該含金屬膜包含以下一或多者：金屬氮化物、金屬碳化物、金屬矽化物或金屬氧化物，該還原劑包含：
    Figure 03_image001
    。
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