TWI812757B - 形成熱穩定有機矽聚合物膜之方法 - Google Patents

形成熱穩定有機矽聚合物膜之方法 Download PDF

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TWI812757B
TWI812757B TW108124875A TW108124875A TWI812757B TW I812757 B TWI812757 B TW I812757B TW 108124875 A TW108124875 A TW 108124875A TW 108124875 A TW108124875 A TW 108124875A TW I812757 B TWI812757 B TW I812757B
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organosilicon polymer
gas
plasma
film
polymer
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TW202016338A (zh
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提摩希 朱利安 文森特 白卡特
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荷蘭商Ａｓｍ 智慧財產控股公司
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    • H01L21/02216—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si the compound comprising silicon and oxygen the compound being a molecule comprising at least one silicon-oxygen bond and the compound having hydrogen or an organic group attached to the silicon or oxygen, e.g. a siloxane
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Abstract

一種形成熱穩定有機矽聚合物之方法，包含：(i)在一反應空間中使用一含矽前驅物，將其主鏈由矽原子組成之有機矽聚合物沉積於一基材上；以及(ii)在該反應空間中於不存在前驅物下，以增加該有機矽聚合物中之Si-H鍵及減少其C-H鍵而不沉積有機矽聚合物的方式，將步驟(i)中沉積的有機矽聚合物暴露於氫電漿。

Description

形成熱穩定有機矽聚合物膜之方法
本發明大體上係有關一種用於形成熱穩定有機矽聚合物膜之方法，且其作為(例如)填充溝槽之空隙填充層。
在製造諸如用於淺溝槽隔離、金屬層間介電質層、鈍化層等之類的積體電路製程中，時常需要使用絕緣材料填充溝槽（通常具有深寬比為1或更高之任何凹部）。然而，隨著大型積體電路(LSI)元件的佈線間距微型化，由於現有沉積製程限制而使得高深寬比空間（例如，深寬比(AR) ≥ 3）的無孔洞填充變得越加困難。再者，即使可以實現無孔洞填充，當在經受隨後的熱或電漿暴露（諸如包含電漿灰化之後沉積處理）時，填充的材料會經歷收縮而藉此產生孔洞。而且，無孔洞填充容易表現出化學耐受性不足，諸如相對高的濕蝕刻速率。
有鑒於此，本發明之一實施例提供了一種後沉積處理，以使有機矽聚合物熱穩定。此技術不僅可應用於孔洞填充製程（諸如美國臨時專利申請案第62/619,569號中所揭露者），也可應用於保形成膜製程。該實施例可解決一或多個前面討論的問題。
相關技術中有關問題和解決方案的任何討論僅是為提供對本發明的背景而包括在本說明書中，且不應認為任何或所有討論在本發明完成時為已知。
在發明目的中，本發明之一目的為提供一種改善有機矽烷聚合物的之熱穩定性的方法，該聚合物由於其流動性而經常作為空隙填充材料，但其通常是熱不穩定的，使得藉由該聚合物所構成的薄膜在暴露於熱時（例如，400°C或更高溫度的環境，諸如在半導體製造中用於退火或灰化製程的環境），會表現出顯著收縮。薄膜的顯著收縮干擾了半導體製造製程。要改善熱穩定性的目標聚合物為有機矽烷聚合物（也稱為「含矽聚合物」），其主鏈由矽原子（聚矽烷）、Si-C-Si主鏈（聚碳矽烷）、Si-N-Si骨架（聚矽氮烷）、Si-O-Si骨架（聚矽氧烷）、前述任一者之改性骨架、或任何任一者之混合物所組成。有機矽烷聚合物在化學上係明顯不同於碳化矽（SiC），碳化矽已經有高度熱穩定性，且也未被歸類為由許多形成支鏈的重複次單元所構成的聚合物。在一些實施例中，第一步將這類有機矽烷聚合物膜沉積在基材上，厚度(例如)小於10 nm，接著，第二步將該有機矽烷聚合物膜暴露於氫電漿中增加該有機矽聚合物中之Si-H鍵及減少C-H鍵，藉以使有機矽烷聚合物的聚合物鏈彼此交聯，藉此使該聚合物密化並使該聚合物熱穩定。氫電漿處理可以在本發明中指定的條件下誘導聚合物支鏈的交聯。
為簡述本發明的態樣和相對於現有技術實現的優點之目的，在本發明中描述本發明的某些目的和優點。當然，應瞭解，根據本發明的任何特定實施例不必然可實現所有這些目的或優點。因此，例如，熟習該項技藝者將明白，本發明可採取實現或最佳化如本說明書所教示的一優點或一組優點的方式具體實施或實現，而不然實現如本說明書可教示或建議的其他目的或優點。
從下面實施方式將變得更明白本發明之其他態樣、特徵和優點。
在本發明中，「氣體」可包括蒸發的固態及/或液態，且可由單一氣體或某些氣體的混合物構成，此取決於實施環境。同樣地，根據實施環境，數量詞「一」意指包括多個物種之物種或屬物。在本發明中，透過氣體噴頭(Showerhead)導入反應腔室的製程氣體可由含矽前驅物和添加氣體組成、實質由其組成、或由其組成。添加氣體可包括一反應氣體，用於氮化及/或碳化前驅物，以及一惰性氣體（例如惰氣(noble gas)），用於當施加RF電力至該添加氣體時激發該前驅物。該惰性氣體可當作載氣及/或稀釋氣體而饋送到反應腔室。在本發明中，未使用用於氧化該前驅物的反應氣體。再者，於一些實施例中，未使用反應氣體，且只使用惰性氣體（作為載氣及/或稀釋氣體）。前驅物和添加氣體可當作一混合氣體或分開氣體導入反應空間。可使用諸如稀有氣體的載氣導入前驅物。除了製程氣體之外的氣體（即，沒有通過氣體噴頭所導入的氣體）可用於例如密封反應空間，其包括諸如稀有氣體的密封氣體。於一些實施例中，術語「前驅物」通常意指參與化學反應而生成另一化合物之化合物，特別是意指構成薄膜基質或薄膜的主骨架之化合物，然而術語「反應物」意指除了前驅物之外的化合物，其激活前驅物，改性前驅物，或催化前驅物的反應，其中反應物可對薄膜基質提供一元素(諸如N、C)且當施加RF電力時變成薄膜基質之一部分。術語「惰性氣體」意指當施加RF電力時其可激發前驅物的氣體，但不像不會變成薄膜基質之一部分的反應物。
於一些實施例中，「薄膜」意指實質在垂直於厚度方向的方向中連續延伸之一層，沒有針孔覆蓋整個目標或相關表面；或僅覆蓋目標或相關表面之一層。於一些實施例中，「層」意指在薄膜或非薄膜結構的表面或類似物上形成具有特定厚度的結構。一薄膜或層可由具有某些特徵的不連續單薄膜或單層、或多個薄膜或多層構成，且相鄰薄膜或層之間的邊界可以或可不透明，而且可基於物理、化學、及/或任何其他特徵、形成製程或順序、及/或相鄰薄膜或層的功能或目的建立。再者，在本發明中，任何兩個變量數目可構成變量的可行範圍，因為可行範圍可基於傳統工作決定，而且所指定的任何範圍可包括或排除端點值。另外，所指定變量的任何數值(不管其是否使用「約」表示)，都可視為精確值或近似值且包括等效值，而且於一些實施例中可指平均值、中值、代表性、多數等。再者，在本發明中，於一些實施例中，術語「由…構成」及「具有」獨立地指「通常或廣泛地包含」、「包含」、「基本上由…組成」或「由…組成」。在本發明中，於一些實施例中，任何定義的意義不必然排除普遍和慣用的意義。
在本發明中，「連續」意指沒有破壞真空；沒有時間線中斷；沒有任何材料介入步驟；沒有改變處理條件、緊隨其後未改變處理條件作為下一步驟；或除了於一些實施例中的兩結構之外的兩結構之間沒有介入離散性物理或化學結構。
於一些實施例中，術語「前驅物」一般係指參與產生另一化合物之化學反應的化合物，特別是構成薄膜基質或薄膜主骨架的化合物，而術語「反應物」係指活化前驅物、修飾前驅物、或催化前驅物的反應之化合物。
在本發明中，相鄰突出結構和任何其他凹部圖案之間的凹部稱為「溝槽」。也就是說，溝槽是含有孔/通孔的任何凹部圖案，而且於一些實施例中，孔/通孔的寬度約20 nm至約100 nm (通常約30 nm至約50 nm)(其中當溝槽的長度本質與寬度相同時，其稱為孔/通孔，且其直徑約20 nm至約100 nm)，深度約30 nm至約100 nm (通常約40 nm至約60 nm)，且深寬比約2至約10 nm (通常約2至約5)。溝槽的適當尺寸可根據製程條件、薄膜組成、預期應用等而變化。
於一些實施例中，形成熱穩定有機矽聚合物之方法包括：(i)在一反應空間中使用一含矽前驅物，將其主鏈由矽原子組成之有機矽聚合物沉積於一基材上；以及(ii)在該反應空間中於不存在前驅物下，以增加該有機矽聚合物中之Si-H鍵及減少其C-H鍵而不沉積有機矽聚合物的方式，將步驟(i)中沉積的有機矽聚合物暴露於氫電漿。
於一些實施例中，步驟(i)中的目標有機矽烷聚合物是熱不穩定的，其中術語「熱不穩定的」係指當在惰性氣體（例如，諸如氬氣之惰性氣體）環境中於450°C溫度下放置5分鐘時測量時，或在與其等效的條件下（諸如用於退火或灰化的條件），薄膜表現出收縮10%或更高的屬性。術語「熱穩定的」係指不是「熱不穩定的」（於與上述相同方法測量時，表現出收縮低於10%）之薄膜屬性，一般為表現出收縮5%或更低，較佳地實質上未表現出收縮（例如，低於10%、5%、1%或實質上0%）。
於一些實施例中，目標有機矽烷聚合物係由聚矽烷、聚碳矽烷、聚矽氮烷或聚矽氧烷所構成。於一些實施例中，該目標有機矽烷聚合物為可流動的含矽聚合物，且其作為(例如)填充溝槽之空隙填充層。例如，於美國臨時專利申請案第62/619,569號（其揭示內容係以全文引用方式併入本文中）中所揭露之可流動的含矽聚合物係可作為目標有機矽烷聚合物，且其中揭露了類PEALD製程（所述「類PEALD製程」包括PEALD條件，例如進料/吹驅/電漿衝擊/吹驅，其中進料後的吹驅被自動嚴格縮短以在電漿衝擊期間留下高分壓的前驅物，其類PEALD製程明顯不同於ALD化學或機構）。於一些實施例中，目標有機矽烷聚合物係由一保形薄膜（保形性為80%或更高）所構成。例如，H2 電漿可改善均勻沉積在上表面、溝槽側壁及溝槽底部上的薄膜品質（例如熱穩定性），其中，與沉積在溝槽側壁上之薄膜品質相比，H2 /Ar電漿或H2 /He電漿可因為Ar或He離子對重離子轟擊的貢獻，而更有效地改善沉積在溝槽上表面及底部上之薄膜品質（例如熱穩定性）。所述電漿較佳地為直接電漿（在反應腔室中用電容耦合的平行電極所產生）。對於遠距電漿，可在佈局上均勻改善，但處理效率比直接電漿低。
不僅可藉由電漿增強型原子層沉積(PEALD)沉積該目標有機矽烷聚合物，也可藉由使用連續電漿或脈衝電漿的電漿增強型化學氣相沉積法(PECVD)沉積。再者，這類聚合物亦可藉由熱CVD（包含脈衝CVD）及熱ALD使用合適的化學物質/催化劑熱形成。
步驟(ii)並不是沉積步驟(i)的一部分，即電漿係用以改造既存的聚合物，而非沉積或形成新的聚合物層。於步驟(ii)中，沒有前驅物（也沒有反應物）饋送到反應空間，或是沒有未反應的前驅物吸附在基板的表面上，使得基本上沒有新的薄膜形成在基板表面上。再者，於步驟(ii)中，除了前驅物之外，至少有一種使用於步驟(i)中的氣體並未使用到，且/或使用至少一種於步驟(i)中未使用的氣體，以進行氫電漿處理。在ALD製程中，其包括重複多次的沉積週期以沉積單層或至少等量的可流動材料，步驟(i)係由一或多個沉積週期所構成，而步驟(ii)中係於每次的步驟(i)之後進行。在進行步驟(ii)之前之於步驟(i)中沉積的薄膜厚度係小於10 nm，一般小於5 nm，使得薄膜藉由步驟(ii)而在厚度方向上完全改造。於一些實施例中，步驟(i)包括當每進行一次步驟(ii)就進行一或多個週期（例如2至10個週期）的電漿增強型原子層沉積(PEALD)，且重複步驟(i)及(ii)作為步驟(iii)，直至得到所要有機矽聚合物厚度（例如，約20 nm至約100 nm）。
於一些實施例中，步驟(i)及步驟(ii)係於相同的反應腔室中連續地進行。在本發明中，「連續地」係指在不破壞真空，不中斷時間線，沒有任何材料介入步驟，不改變處理條件，緊隨其後或作為下一步驟，這取決於實施例。
於一些實施例中，步驟(ii)包括施加0.07 W/cm2 至1.4 W/cm2 範圍（例如0.14至0.7 W/cm2 ）的RF電力至該反應空間以產生氫電漿。於一些實施例中，步驟(ii)係進行5秒至60秒（例如10秒至30秒）。於一些實施例中，步驟(ii)包括供應氫氣及惰性氣體至該反應空間，氫氣流對包含有氫氣與惰性氣體之氣體總流量的比率為0.1至0.9（例如0.5至0.8）。於一些實施例中，步驟(ii)包括只供應氫氣至該反應空間以產生氫電漿。
於一些實施例中，在步驟(ii)中，該氫電漿為通過脈衝將RF電力施加至該反應空間所產生的脈衝電漿，其間隔為約10毫秒至約500毫秒（例如，約50毫秒至約200毫秒）。
以下使用實例更詳細地解釋本發明，但本發明並非意欲受限於這些實例。
如上所述，待改造的物質為有機矽烷聚合物，其不被認為是由通常為熱穩定且不可流動的碳化矽(SiC)所構成。於一些實施例中，該有機矽烷聚合物具有聚矽烷基結構，其可或不可為可流動的，但具有低的熱穩定性。儘管碳化矽及含矽聚合物皆含有矽原子及碳原子，但含矽聚合物的密度低於碳化矽，且耐熱性比碳化矽低，因此，含矽聚合物的熱穩定性低於碳化矽，因此易受(例如)收縮及乾蝕刻的影響。含矽聚合物性質很大程度上取決於聚合物交聯狀態，這對聚合物的熱穩定性至關重要。氫電漿處理可引起交聯，對諸如熱穩定性及乾蝕刻耐性之薄膜性質有正面影響。
圖3為根據本發明一實施例藉由H2電漿處理所誘導之不同聚合物鏈之交聯示意圖。儘管電漿聚合有高度的隨機性，但如圖3所示，不同的聚合物支鏈（其可為相同的支鏈）係藉由氫電漿處理而交聯，藉以促進密化（增加RI），改善熱穩定性及對乾蝕刻或其他化學處理的耐性。
於一些實施例中，由於含矽聚合物沉積不需要是可流動的或自下而上沉積，因此可選擇用於沉積含矽聚合物的製程參數，且比用於自下而上沉積的製程參數（諸如美國臨時專利申請案第62/619,569號中所揭露者）設置得更為寬鬆。由於用於沉積SiC的參數及設定點可以是下表1中所示的那些，因此含矽聚合物可以在具有與表1中所示者有一或多個設定點不同之條件下形成，其中「SUS temp」（感受器溫度）及「吹驅」（饋送前驅物後的吹驅）可能是最有影響的參數。在表1中，「總He」係指包含He載氣、He密封氣體、He稀釋氣體等之He氣體的總流速，「空隙」係指電容耦合的平行電極之間的空隙，「壓力」係指反應空間的壓力，而「饋送」係指饋送前驅物。鑑於本發明之全部內容及美國臨時專利申請案第62/619,569號（其揭示內容係以全文引用方式併入本文中）之揭示內容，本領域中熟習該項技藝者係可容易地給出將製程條件最佳化的這類條件，作為常規實驗的事項。
表1 (數值為近似值)
有機矽烷聚合物係接著經受氫電漿處理以改善熱穩定性。圖4係繪示根據一實施例藉由PEALD沉積週期及H電漿處理所構成的製程順序，其中各欄之寬度不一定代表實際的時間長度，且各列中線條高度上升表示ON狀態，而各列中之線條底部高度表示OFF狀態的。在此順序中，「氣體穩定1 (Gas Stab 1)」係指在各沉積步驟之前進行的第一氣體穩定步驟，其中在不饋送前驅物且不施加RF電力的情況下，開始饋送電漿產生氣體（例如He）。「沉積(Depo)」係指一個包括有一或多個沉積週期之沉積步驟，各沉積週期係沉積單層或至少等量的可流動材料，其中各週期係由饋送前驅物、吹驅、施加RF電力及吹驅所構成（在此順序中，週期係重複一次，即執行兩個週期，但週期數量並不受限於此且可執行任何適宜數量的週期）。
此後，開始氫電漿處理步驟。在此順序中，「氣體穩定2 (Gas Stab 2)」係指在氫電漿處理步驟之前進行的第二氣體穩定步驟，其中係將電漿產生氣體（例如He）的饋送停止，同時供給氫氣及另外的電漿產生氣體（例如Ar），而不饋送前驅物且不施加RF電力。「H處理(H treat)」係指氫電漿處理步驟，其中係於不存在任何前驅物的情況下施加RF電力。儘管H2 /Ar電漿比H2 /He電漿更有效於改善熱穩定性（誘導聚合物交聯），但是可使用H2 /He電漿。此外，可單獨使用H2 電漿。於一些實施例中，只要沒有電弧且電漿是穩定的，He與總電漿產生氣體（包含He及/或Ar）的可行流量比例並不受到限制，且該可行流量比例係高度仰賴硬體。於一些實施例中，氫電漿處理係於下表2中所示條件下，以與圖4所繪示方法相似的方法進行。
表2 (數值為近似值)
於上表中，「RF功率（針對300-mm晶圓）」係可針對不同尺寸的晶圓，在類PEALD製程及使用連續或脈衝電漿的PECVD製程二者中，轉換成單位W/cm2 。在上表中，「暴露於H2電漿之經沉積有機矽烷聚合物的厚度」係指在基材上表面上之聚合物厚度。
於一些實施例中，沉積步驟及氫電漿處理係於相同反應腔室中連續進行。例如，圖1A為可用於本發明實施例中之用於沉積介電質薄膜之PEALD（電漿增強型原子層沉積）裝置之示意代表圖，其係經編程控制進行下述序列。在此圖中，透過在反應腔室3的內部11 (反應區)中以彼此平行及面對方式提供一成對的導電平板電極4、2，將HRF電力(50 Hz或2 GHz) 25施加於一側，而且在另一側12電接地，在電極間激發電漿。一溫度調節器設置在較低層2 (下電極)中，並且置放在其上的基材1的溫度在特定溫度下保持恆定。上電極4亦作為一噴淋板，電漿產生氣體（及稀釋氣體，若有的話）和前驅物氣體（及載氣，若有的話）分別透過一氣體管線21和一氣體管線22導入反應腔室3，並且通過噴淋板4。另外，在反應腔室3中，設置具有一排氣管7的圓形管道13，反應腔室3的內部11中的氣體可透過其排出。另外，設置在反應腔室3下方的傳送腔室5具有一密封氣體管線24，以經由傳送腔室5的內部16 (傳送區域)將密封氣體導入反應腔室3的內部11，其中提供一用於分離反應區和傳送區的分離板14 (此圖省略一閘閥，晶圓可通過其傳送入傳送腔室5，或從其傳送出)。傳送腔室亦具有一排氣管6。在某些實施例中，沉積多元件薄膜和表面處理在相同的反應空間中進行，使得所有步驟可連續進行而不會將基材暴露於空氣或其他含氧大氣。
載氣的連續流動可使用流通系統(Flow-pass System，FPS)實現，其中一載氣管線具有一含前驅物儲槽(儲瓶)的岐路管線，且主管線和岐路管線被切換，其中當只有一載氣饋送入反應腔室時，岐路管線則被關閉，然而當該載氣和一前驅物氣體兩者饋送入反應腔室時，主管線關閉而且載氣流過岐路管線且連同前驅物氣體從儲瓶流出。這樣，載氣可連續流入反應腔室，而且可透過切換主管線及岐路管線而以脈衝方式攜帶前驅物氣體。圖1B示意說明根據本發明之一實施例之使用流通系統(FPS)的前驅物供應系統(黑色閥表示閥關閉)。如圖1B中的(a)所示，當將前驅物饋送到反應腔室(未示出)時，首先，一諸如Ar (或He)的載氣流過具有閥b和c的氣體管線，然後進入一儲瓶(儲槽) 20。載氣從儲瓶20流出，同時攜帶符合儲瓶20內部蒸汽壓力相對量的前驅物氣體，並且流通過一具有閥f和e的氣體管線，然後連同前驅物饋送入反應腔室。於上文中，閥a和d是關閉。當僅將載氣(惰性氣體)饋送到反應腔室時，如圖1B中的(b)所示，載氣透過閥a流通過氣體管線，同時繞過儲瓶20。於上文中，閥b、c、d、e、和f是關閉。
在沉積步驟（例如，其可由2至6個週期的PEALD所構成）完成之後，除了不饋送前驅物氣體之外，該氫氣電漿處理步驟係以與沉積步驟相似的方法開始，且調整用於該氫氣電漿處理之製程參數。
熟習該項技藝者將明白，該裝置包括一或多個控制器(未示出)，其經編程或構造成進行本文中別處所述的沉積和反應器清潔處理。熟習該項技藝將明白，控制器係與各種電源、加熱系統、泵、自控機器、和氣體流量控制器或反應器的閥進行溝通。
在某些實施例中，可使用雙腔室反應器(用於處理彼此靠近設置晶圓的兩個部分或隔室)，其中一反應氣體和一惰性氣體可透過一共用管線供應，然而一前驅物氣體透過非共用管線供應。
具有填充能力的薄膜可應用於各種半導體元件，包括但沒有限於3D交叉點記憶體元件的單元隔離、自對準孔洞、假性閘極(替代目前的多晶矽)、反向色調圖案化、PC RAM隔離、裁切硬質罩幕層、和DRAM儲存節點觸點(SNC)隔離。
實例
在未指定條件及/或結構的下列實施例中，根據傳統實驗，熟習該項技藝者可從本說明書的觀點輕易提供這類條件及/或結構。熟習該項技藝者將明白，實施例中所使用的裝置包括一或多個控制器(未示出)，其經編程或構造成進行本說明書中所述的沉積和反應器清潔處理。熟習該項技藝者將明白，所述控制器係與各種電源、加熱系統、泵、自控機器、和氣體流量控制器或反應器的閥進行溝通。
實例1
以使用圖1A所示的裝置和圖1B所示的氣體供應系統(FPS)，在下表3所示的條件下，將有機矽聚合物藉由類PEALD製程（該「類PEALD製程」包括PEALD條件，例如進料/吹驅/電漿衝擊/吹驅，其中進料後的吹驅被自動嚴格縮短以在電漿衝擊期間留下高分壓的前驅物，其類PEALD製程明顯不同於ALD化學或機構）沉積在Si基材(具有直徑300 mm及厚度0.7 mm)上，其具有寬度約30 nm的窄溝槽及寬度約75 nm的寬溝槽，且其深度約70 nm。使用載氣(其流速0.1 slpm)將前驅物（二甲基二乙炔基矽烷作為揮發性烷基矽烷前驅物）饋送給反應腔室。然而，由於前驅物的高蒸氣壓力，使得不需要載氣。在此實例中，使用小質量流量的載體作為防止前驅物在管線中凝結的預防措施。如果管線充分加熱，則不需使用載氣。此外，雖然使用乾燥He流能使電漿點火較容易及更穩定，但是只要電漿點火，即可消除乾燥He流。
於表3中所定義的沉積週期係重複四次以作為沈積步驟，接著於下表4中所繪示的條件下（「實例1-1 (Ex. 1-1)」、「實例1-2 (Ex. 1-2)」及「實例1-3 (Ex. 1-3)」），以與圖4所繪示相似的方法進行H電漿處理以作為後沉積處理，其中此經修改的沉積週期（即，由沉積週期與後沉積處理所構成者）係被重複直至將薄膜沉積到完全填充溝槽並進一步堆積於上，形成一平坦上表面。上述沉積製程中係進行週期性H電漿處理以於退火後的收縮（於N2 環境中在450°C下30分鐘）、RI（用波長633 nm測得的折射率）及乾蝕刻速率(“DER”)特性（在20°C下使用8 Pa的CF4 /O2 /Ar作為蝕刻氣體混合物蝕刻該薄膜15秒時所測得）等方面帶來一些好處，其亦顯示於表4中。
表3 (數值為近似值)
表4 (數值為近似值)
於表4中，「D/T比例」係指沉積週期與後沉積處理的比例，「氣體穩定1」及「氣體穩定2」係分別對應圖4中的「氣體穩定1」及「氣體穩定2」。
並且，在比較例（表4中的「比較例1」）中係於表4所示條件下沉積薄膜而沒有後沉積處理，直至將薄膜沉積到完全填充溝槽並進一步堆積於上，形成一平坦上表面。
如表4中所示，藉由進行H電漿處理作為後沉積處理，可改善薄膜的RI，減少乾蝕刻速率（對乾蝕刻的耐受性更高），並顯著降低因退火收縮率或完全抑制收縮。於一些實施例中，可使用50至500 W (0.07至0.71 W/cm2 )的RF功率有效地進行H電漿處理10至180秒。
圖9係顯示利用該類PEALD製程之空隙填充層之傅立葉變換紅外線(FTIR)光譜。如圖9所示，經沉積的材料（「未處理的」）係含有Si-C鍵及C-H鍵，證實該材料為SiC基材料（有機矽聚合物），且通過H電漿處理（「經H2處理的」），C-H鍵明顯減少，同時Si-H鍵在該有機矽聚合物中顯著增加，增加了交聯聚合物支鏈並使該有機矽聚合物熱穩定。圖10及11為熱脫附氣相層析與質譜檢測圖，其顯示在所指溫度下之來自於「未處理的」聚合物及「經H2處理的」聚合物之揮發性有機化合物排出量。如圖10及11所示，未處理的聚合物顯示出顯著的CxHy成分脫氣，特別是C3 H5 從約400°C開始，在600°C附近急劇增加脫氣，並在約700°C達到高峰，導致薄膜顯著的密化（收縮），並且，未處理的聚合物顯示出顯著的Si成分脫氣，從約400°C開始，在500°C附近急劇增加，並在約600°C達到高峰，導致從薄膜中蒸發而損失Si。相反的，在「經H2處理的」聚合物中，即使在諸如500°C或更高的高溫下，基本上也完全抑制住Si蒸發，並且，即使在諸如600°C或更高的高溫下，基本上也完全抑制住C3 H5 的脫氣，防止薄膜收縮。
圖17係顯示於經受(a)中的週期性氫電漿處理之空隙填充寬溝槽，以及於經受(b)中的週期性氫電漿處理之空隙填充窄溝槽之橫截面圖的STEM照片。如圖17所示，藉由進行週期性氫電漿處理，觀察到在退火時經沉積薄膜（實例1-1）基本上沒有收縮。
實例2
在比較例2中，係以與比較例1相似的方法藉由類PEALD製程沉積一可流動薄膜。於實例2中，可流動薄膜係以與實例1-1（即，結合週期性H電漿處理的沉積）相似的方法藉由類PEALD製程沉積一可流動薄膜，以於RI及乾蝕刻速率特性，以及O含量等方面帶來一些好處，其係顯示於下表5中。
表5 (數值為近似值)
如表5所示，藉由進行H電漿處理係可進行聚合物支鏈的交聯，且不同的支鏈可以更緊密地彼此結合，藉以促進聚合物的密化。由於RI最常與材料密度相關，如表5所示，皆藉由H電漿處理增加了密度及RI。而且，H電漿處理改善了對乾蝕刻的化學抗性。
實例3
於比較例3中，係以與比較例1相似的方法藉由類PEALD製程沉積一可流動薄膜。於實例3中，以與實例1-1相似的方法藉由類PEALD製程沉積一可流動薄膜（即結合週期性H電漿處理的沉積），為經沈積的薄膜帶來高度熱穩定性。該等薄膜係經受在450°C的溫度於1,000 Pa的壓力下在Ar環境中所進行的退火0分鐘（即不退火），5分鐘及30分鐘。
圖14係顯示一指示出實例3之沉積薄膜通過退火的厚度改變，以及比較例3之沉積薄膜通過退火的厚度改變之圖式，其中進行了退火。如圖14所示，未處理的薄膜（「比較例3」）係顯著收縮，其中薄膜的厚度在退火5分鐘時降低約50%，在30分鐘時降低約75%，而令人驚訝的是，經處理的薄膜（「實例3」）即使在退火30分鐘時也沒有收縮，也就是說，即使在退火30分鐘時也沒有觀察到薄膜收縮，表明有極高度的熱穩定性。
一般而言，在低於400°C的溫度下，未處理的薄膜的收縮是飽和的，其中薄膜的厚度將收縮約30%，且額外的退火不會導致進一步的收縮。然而，未處理的薄膜的收縮通常在400°C或更高的溫度下變得不飽和。也就是說，若薄膜經受足夠長的退火，則未處理的薄膜最終將完全蒸發，除了一薄層殘留物之外。
圖2係顯示有機矽烷聚合物之溫度脫附分析數據，其中樣本係經加熱並藉由質譜儀分析放射出的種類。X軸表示檢測到的質量，接著可以將其歸因於放射出的種類（例如，質量2表示H2 ，質量15表示CH3 ）。左側的Y軸表示樣本的溫度，顯示在特定溫度下放射出的特定種類。右側的Z軸以灰階顯示發射信號強度（即，表示放射出多少）與對比密度（梯度）之間的關係，其顯示來自檢測極限的強度梯度（白色/亮 - 無放射出）至大量排放（暗色）。應注意到，原始數據是彩色的，且強度梯度顯示沒有發射出黃色/綠色，一開始放射出藍色，接著大量放射出紅色。然而，紅色似乎比灰階中的藍色更亮，且在圖2中，在每個檢測到放射的不同垂直暗區中，在由深灰色區域圍繞的中心中之略淺灰色的區域最初為紅色，表明中心的排放量高於周圍區域。此信息有相當定性，但清楚顯示出在約400°C或更高的溫度下，聚合物的大多成份開始顯著地去除，即該聚合物的收縮在約400°C或更高的溫度下開始並且不可逆地持續。在沒有週期性H電漿處理的情況下所沉積的聚合物是高度熱不穩定的。
相對的，如圖14中所示，結合週期性H電漿處理所沉積的聚合物（實例3）係顯示出高度的熱穩定性，顯示出在450°C下基本上沒有成分因退火分解或脫氣，表明聚合物交聯在一起，密化並形成具有抗熱降解性之穩定基質。
下表6係顯示未處理的薄膜及經H2處理的薄膜之質量損失(%)及收縮率(%)。如表中所示，H2 電漿處理可有效地誘導交聯作用並改善聚矽烷基薄膜的熱穩定性。
表6 (數值為近似值)
實例4
於比較例4（「未處理的」）中，以與比較例1相似的方法藉由類PEALD製程沉積一可流動薄膜。於實例4（「經H2處理的」）中，以與實例1-1相似的方法藉由類PEALD製程沉積一可流動薄膜（即結合週期性H電漿處理的沉積）。該等薄膜係經受後沉積退火/灰化，該後沉積退火/灰化係以200°C的溫度於400 Pa的壓力下2分鐘作為一般條件並在下表7中所示的特定條件下進行，以評估對於未處理的聚合物及經H2處理的聚合物之退火/灰化影響。
表7 (數值為近似值)
圖12係顯示一指示出各薄膜的厚度減少情形之圖式，而圖13係顯示一指示出各薄膜的濕蝕刻電阻率之圖式。如圖12及13所示，未處理的薄膜係受到所有退火/灰化的強烈影響，尤其是受N2 /H2 灰化的影響，其效果在降低對濕蝕刻的抗性方面有協同作用（圖13）。這可因為是聚矽烷基主鏈被N2 電漿部分破壞且因N2 電漿而終止N端，形成品質不佳的類氮化物薄膜，且H2 電漿促進了反應。相反的，經H2處理的薄膜對於退火/灰化有明顯更強的耐受性。
實例5至7
於實例5中，以與實例1-1相似的方法藉由類PEALD製程沉積一可流動薄膜（即結合週期性H電漿處理的沉積），除了用於H電漿處理的RF功率改變，如圖5所示。於實例6中，以與實例1-1相似的方法藉由類PEALD製程沉積一可流動薄膜（即結合週期性H電漿處理的沉積），除了每個H電漿處理的沉積週期數量改變，如圖6所示。於實例7中，以與實例1-1相似的方法藉由類PEALD製程沉積一可流動薄膜（即結合週期性H電漿處理的沉積），除了用於H電漿處理的RF功率施加期間改變，如圖7所示。各種所產生的薄膜之品質係根據在633 nm的RI來評估。RI值係用於評估聚合物的固化程度，其中RI越高，預期固化程度越高（密度變得越高）。結果係顯示於圖5至圖7中。
圖5為顯示用於H電漿處理的RI和RF功率之間的關係圖，且其顯示出RF功率愈高，RI變得愈高。圖6為顯示RI與每個H電漿處理沉積週期數之間的關係圖，且其顯示出每個H電漿處理的沉積週期數量愈大，RI變得愈低。圖7為顯出RI與用於H電漿處理的RF功率施加持續時間之間的關係圖，且其顯示出RF功率施加期間愈長，RI變得愈高。因此，通過使用製程參數操縱H電漿處理條件而可調整材料的品質。熟習該項技藝者可基於本申請案的揭示內容，經由常規實驗而可為所要的應用或所得薄膜的用途找到適宜條件。
進一步研究所得的薄膜以判定乾蝕刻速率比率(DERR)與RI之間的關係。圖8為顯示乾蝕刻速率比率(DEER)與RI之間的關係圖（通過將薄膜的絕對乾蝕刻速率(DER)除以PECVD碳化矽的絕對DER來計算DERR，其中DER係使用CF4 /O2 /Ar作為蝕刻氣體混合物在20°C於8 Pa下測量15秒）。如第8圖所示，DERR和RI高度相關，且通常RI愈高，DER變得愈低。
熟習該項技藝者將瞭解，在不悖離本發明的精神情況下，可進行許多和各種修改。因此，應清楚瞭解，本發明的形式僅是說明而沒有限制本發明的範疇。
1:基材 2:導電平板電極 3:反應腔室 4:導電平板電極 5:傳送腔室 6:排氣管 7:排氣管 11:反應區 12:電接地 13:圓形管道 14:分離板 16:傳送區域 20:儲瓶(儲槽) 21:氣體管線 22:氣體管線 24:密封氣體管線 25:HRF電力
現將參考旨在示意說明而不是限制本發明之較佳實施例的圖式來描述本發明的這些及其他特徵。為說明目的，圖式已明顯簡化，且不必然按比例圖示。
圖1A為用於沉積可用於本發明實施例的介電質薄膜的電漿增強型原子層沉積(Plasma-enhanced Atomic Layer Deposition，PEALD)裝置之示意圖。
圖1B係繪示使用可用於本發明之實施例之流通系統(Flow-pass System，FPS)的前驅物供應系統之示意圖。
圖2係顯示有機矽烷聚合物之溫度脫附分析數據，其中樣本係經加熱並藉由質譜儀分析放射出的種類。
圖3為根據本發明一實施例藉由H2電漿處理所誘導之不同聚合物鏈之交聯示意圖。
圖4係繪示根據一實施例藉由PEALD沉積週期及H電漿處理所構成的製程順序，其中各欄之寬度不一定代表實際的時間長度，且各列中線條高度上升表示ON狀態，而各列中之線條底部高度表示OFF狀態的。
圖5為顯示根據本發明實施例之用於H電漿處理的RI和RF功率之間的關係圖。
圖6為顯示根據本發明實施例之RI與每個H電漿處理沉積週期數之間的關係圖。
圖7為顯出根據本發明實施例之RI與用於H電漿處理的RF功率施加持續時間之間的關係圖。
圖8為顯示根據本發明實施例之乾蝕刻比率(DER)與RI之間的關係圖。
圖9係顯示根據本發明實施例之空隙填充層之傅立葉變換紅外線(FTIR)光譜。
圖10及11為熱脫附氣相層析與質譜檢測圖，其顯示來自於根據一比較例之「未處理的」聚合物以及從根據本發明一實施例之「經H2處理的」聚合物的揮發性有機化合物排出量。
圖12係顯示一指示出根據一比較例之未處理薄膜的厚度減少情形，以及根據本發明實施例之經H2處理薄膜的厚度減少情形之圖式。
圖13係顯示一指示出根據一比較例之未處理薄膜的濕蝕刻電阻率，以及根據本發明實施例之經H2處理薄膜的厚度減少情形之圖式。
圖14係顯示一指示出根據本發明實施例之沉積薄膜通過退火的厚度改變，以及根據一比較例之沉積薄膜通過退火的厚度改變之圖式。
圖15係顯示指示出根據本發明之實施例之使用統計數據分析軟體JMP®獲得製程參數與RI的改善之間的示意關係之圖式。
圖16係顯示指示出根據本發明之實施例之使用統計數據分析軟體JMP®獲得製程參數與RI之間的示意關係之圖式。
圖17係顯示根據本發明實施例於經受(a)中的週期性氫電漿處理之空隙填充寬溝槽，以及於經受(b)中的週期性氫電漿處理之空隙填充窄溝槽之橫截面圖的STEM照片。
1:基材
2:導電平板電極
3:反應腔室
4:導電平板電極
5:傳送腔室
6:排氣管
7:排氣管
11:反應區
12:電接地
13:圓形管道
14:分離板
16:傳送區域
21:氣體管線
22:氣體管線
24:密封氣體管線
25:HRF電力

Claims (13)

  1. 一種形成熱穩定有機矽聚合物膜之方法，包括：(i)在一反應空間中使用一含矽前驅物，將其主鏈由矽原子組成之有機矽聚合物沉積於一基材上，其中該主鏈包含Si-C-Si、Si-N-Si或Si-O-Si中之至少一者；以及(ii)在該反應空間中於不存在前驅物下，以增加該有機矽聚合物中之Si-H鍵及減少其C-H鍵而不沉積有機矽聚合物的方式，將步驟(i)中沉積的有機矽聚合物暴露於氫電漿，其中該氫電漿係使用0.07W/cm2至1.4W/cm2範圍的RF電力所產生，其中氫氣流對包含有氫氣與惰性氣體之氣體總流量的比率為0.1至0.9之間，並且其中步驟(ii)係進行5秒至60秒。
  2. 如請求項1之方法，其中步驟(i)包括進行一或多個週期的原子層沉積(ALD)，且重複步驟(i)及(ii)作為步驟(iii)，直至得到所要有機矽聚合物厚度。
  3. 如請求項1之方法，其中步驟(i)包括進行化學氣相沉積(CVD)，且重複步驟(i)及(ii)作為步驟(iii)，直至得到所要有機矽聚合物厚度。
  4. 如請求項2之方法，其中該ALD為電漿增強型ALD(PEALD)，在步驟(ii)之前進行2至10次。
  5. 如請求項3之方法，其中該CVD為熱增強型或電漿增強型CVD，且每次於步驟(i)中沉積1至50nm厚度的有機矽聚合物之後進行步驟(ii)。
  6. 如請求項1之方法，其中步驟(ii)包括施加0.07W/cm2至0.71W/cm2範圍的RF電力至該反應空間以產生該氫電漿。
  7. 如請求項1之方法，其中步驟(ii)係進行10秒至60秒。
  8. 如請求項1之方法，其中氫氣流對包含有氫氣與惰性氣體之氣體總流量的比率為0.1至0.8之間。
  9. 如請求項2之方法，更包括在步驟(iii)之後將該有機矽聚合物退 火，其中該有機矽聚合物未表現出收縮。
  10. 如請求項1之方法，其中該有機矽聚合物係由聚矽烷、聚碳矽烷、聚矽氮烷或聚矽氧烷所構成。
  11. 如請求項1之方法，其中在步驟(ii)中，該氫電漿為通過脈衝將RF電力施加至該反應空間所產生的脈衝電漿，其間隔為約10毫秒至約500毫秒。
  12. 如請求項1之方法，其中步驟(i)及步驟(ii)係連續在相同反應腔室內進行。
  13. 如請求項1之方法，其中在步驟(ii)中，除了前驅物之外，至少有一種使用於步驟(i)中的氣體並未使用到，且/或使用至少一種於步驟(i)中未使用的氣體。
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