TWI839104B - 含鑭系元素先質之製備及含鑭系元素膜之沈積 - Google Patents

含鑭系元素先質之製備及含鑭系元素膜之沈積 Download PDF

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TWI839104B
TWI839104B TW112104009A TW112104009A TWI839104B TW I839104 B TWI839104 B TW I839104B TW 112104009 A TW112104009 A TW 112104009A TW 112104009 A TW112104009 A TW 112104009A TW I839104 B TWI839104 B TW I839104B
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lanthanide
deposition
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金大玹
宋浚賢
盧沅泰
凡卡特斯瓦拉Ｒ 帕雷姆
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法商液態空氣喬治斯克勞帝方法研究開發股份有限公司
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Abstract

所揭露的鑭系元素先質化合物包含具有至少一個脂族基團作為取代基的環戊二烯基配位基和至少一個二齒配位基。該等先質適用於沈積含鑭系元素的膜。

Description

含鑭系元素先質之製備及含鑭系元素膜之沈積
本揭露之領域關於用於氣相沈積用於半導體製造的材料的化學品。
本發明至少在工業上適用於沈積用於半導體製造的鑭系元素材料。
半導體工業面臨的嚴重挑戰之一為開發用於動態隨機存取記憶體（DRAM）和電容器的新穎閘極介電材料。數十年來，二氧化矽（SiO 2）為可靠電介質，但作為電晶體已持續縮小且技術由「全Si」電晶體變為「金屬閘極/高k」電晶體，基於SiO 2的閘極電介質的可靠性達到其物理極限。隨著用於目前技術的尺寸正在縮小，對新穎高介電常數材料和製程的需求正在增加，並且變得越來越關鍵。新一代的氧化物，尤其是基於含鑭系元素的材料（具有原子序數為57-17的鑭系元素原子，但主要是鑭），被認為與常規介電材料相比在電容方面具有顯著的優勢。
然而，沈積含鑭系元素層係困難的，並且越來越需要新穎的材料和製程。例如，原子層沈積（ALD）已被視為用於微電子器件製造的重要薄膜生長技術，其依賴於藉由惰性氣體吹掃而分開的、交替施用的先質的順序及飽和的表面反應。ALD的表面受控性質使得薄膜的生長能夠在精確厚度控制下具有高的保形性及均一性。對開發用於鑭系元素材料的新穎ALD製程的需求係顯而易見的。
不幸的是，已證明將化合物成功併入沈積製程中是困難的。典型地提出三類分子：β-二酮、雙(三甲基矽基)醯胺和環戊二烯基化合物。前兩類化合物係穩定的，但熔點可以超過90°C，使其不實用。例如，2,2-6,6-四甲基庚二酮酸鑭[La(thd)3]的熔點高達230°C，並且三(雙(三甲基矽基)胺基)鑭[La(tmsa)3]的熔點係150°C。此外，那些先質的輸送效率非常難以控制。未經取代的環戊二烯基化合物也表現出低的揮發性及髙熔點。分子設計可以既有助於改進揮發性又降低熔點。然而，在製程條件中，該等種類的材料已被證明具有有限的用途。例如，La(iPrCp)3並不允許高於225°C的ALD方案。
如以上所討論的，目前可得到的許多含鑭系元素的先質在用於沈積方法中時表現許多缺點。因此，仍然需要用於沈積含鑭系元素膜的替代性的先質。
所揭露的先質化合物包含具有至少一個脂族基團作為取代基的環戊二烯基配位基和二齒配位基。先質具有以下三個通式之一： 1.  Ln(R 1Cp)m(O-CR 2=CH-CR 2=O)n 2.  Ln(R 1Cp)m(R 3N-CR 2=CH-CR 2=O)n 3.  Ln(R 1Cp)m(R 3N-CR 2=CH-CR 2=NR 3)n
在上述式1-3中，Ln = 鑭系元素，La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu。R 1、R 2和R 3各自獨立地是H或C 1-C 5烷基（直鏈或支鏈）鏈。m = 1或2並且n = 1或2。
當與它們相應的均配型化合物（包括三取代的環戊二烯基鑭系元素化合物Ln(RCp)3和三取代的β-二酮酸鹽化合物Ln(O-CR=CH-CR=O)3（或Ln(R’N-CR=CH-CR=O)3、Ln(R’N-CR=CH-CR=NR’)3））相比時，上述式1-3所揭露的先質化合物提供了獨特的物理和化學特性。此類特性包括更好地控制金屬中心周圍的空間擁擠，這進而控制基材上的表面反應以及與第二種反應物（如氧源）的反應。獨立地微調配位基上的取代基增加了揮發性和熱穩定性，並降低了熔點，以產生液體或低熔點固體（具有低於大約105°C、較佳的是低於約80°C的熔點）。 [表1]中總結了某些示例性分子和對比分子的特性： - thd ： -O-C(tBu)=CH-C(tBu)=O - N EtO-DK ： -(Et)N-C(Me)=CH-C(Me)=O - N nPrO-DK ： -(nPr)N-C(Me)=CH-C(Me)=O
工作實例 實例 1 -異丙基環戊二烯基四甲基庚二酮酸鑭 = La(iPrCp) 2(thd)的合成
在-78°C下，將2,2,6,6-四甲基-3,5-庚二酮（2 g，10.8 mmol）在30 mL的甲苯中的溶液逐滴添加到La(iPrCp) 3（5 g，10.8 mmol）在15 mL的甲苯中的溶液中。將反應混合物緩慢升溫至室溫，攪拌過夜。過濾後，將溶劑在減壓下除去，以獲得棕色固體。將棕色固體在約180°C下在35毫托下昇華，以產生約44%（2.54 g）產率的黃色固體。
在開口杯TGA分析期間，在10°C/min的溫度升高速率下，在200 mL/min流動氮氣的氣氛中測量的，純化的產物留下5.4%的剩餘質量。該等結果在圖1中示出，圖1係展示溫度升高時重量百分比的TGA圖。藉由差示掃描量熱法（DSC）測量產物的熔化的開始溫度（77°C）和分解的開始溫度（410°C），如圖2所示。 標記和命名
雖然已經結合本發明之具體實施方式描述了本發明，但顯然，鑒於前述說明，許多替代方案、修改、和變化對於熟悉該項技術者將是清楚的。因此，旨在包含落入所附請求項的精神和廣泛範圍內的所有此類替代方案、修改和變化。本發明可以適合地包括所揭露的要素、由所揭露的要素組成或基本上由所揭露的要素組成，並且可以在不存在未揭露的要素下實施。此外，如果存在關於順序的語言，如第一和第二，應在示例性意義上、而不是在限制性意義上進行理解。例如，熟悉該項技術者可以認識到，可以將某些步驟組合成單一步驟。
單數形式「一個/種（a/an）」和「該」包括複數個指示物，除非上下文另外清楚地指出。
請求項中的「包括」係開放式過渡術語，其係指隨後確定的請求項要素係無排他性的清單（即，其他任何事物可以另外地被包括並且保持在「包括」的範圍內）。除非在此另有說明，否則如在此使用的「包括」可以由更受限制的過渡術語「基本上由……組成」和「由……組成」代替。
請求項中的「提供」被定義為係指供給、供應、使可獲得或製備某物。該步驟可以相反地由任何行動者在請求項中沒有明確的語言的情況下執行。
視需要的或視需要意指隨後描述的事件或情況可能發生或可能不發生。本說明書包括其中事件或情況發生的實例以及其中事件或情況不發生的實例。
在本文中範圍可以表述為從約一個具體值和/或到約另一個具體值。當表述此種範圍時，應理解的是另一個實施方式係從一個具體值和/或到另一個具體值、連同在所述範圍內的所有組合。
在此確定的所有參考文檔各自特此藉由引用以其整體結合到本申請中，並且是為了具體的資訊，引用各個參考文檔以獲得具體的資訊。
應當理解，由熟悉該項技術者可在如所附請求項中所表述的本發明之原則和範圍內做出本文已經描述以解釋本發明之本質的細節、材料、步驟和零件佈置上的許多附加的改變。因此，本發明不旨在限於以上給出的示例中的具體實施方式。
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為了進一步理解本發明之本質和目的，應結合附圖來參考以下詳細說明，在附圖中類似的元件被賦予相同或類似的附圖標記，並且在附圖中： [圖1]   係展示溫度升高時重量百分比之TGA圖；以及 [圖2]   係藉由差示掃描量熱法（DSC）測量產物的熔化之開始溫度（77°C）和分解之開始溫度（410°C）。
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Claims (6)

  1. 一種化學品，其具有選自La(異丙基-Cp)2(thd)、Er(甲基-Cp)2(NEtO-DK)、或Er(甲基-Cp)2(NnPrO-DK)之式中的任一項。
  2. 一種組成物，其適用於半導體製造的化學氣相沈積和/或原子層沈積，該組成物包含請求項1所述之化學品。
  3. 如請求項2所述之組成物，其中該化學品按重量計係該組成物的99%或更多。
  4. 一種沈積含鑭系元素膜之方法，該方法包括向化學氣相沈積或原子層沈積製程提供請求項1所述之化學品的氣相的步驟。
  5. 如請求項4所述之方法，其中該化學氣相沈積或原子層沈積製程在基材上產生含鑭系元素的膜。
  6. 如請求項5所述之方法，其中該基材係半導體基材。
TW112104009A 2022-02-08 2023-02-04 含鑭系元素先質之製備及含鑭系元素膜之沈積 TWI839104B (zh)

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