TWI713608B - 沉積包含SiO及SiN之可流動薄膜的方法 - Google Patents

沉積包含SiO及SiN之可流動薄膜的方法 Download PDF

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TWI713608B
TWI713608B TW105133831A TW105133831A TWI713608B TW I713608 B TWI713608 B TW I713608B TW 105133831 A TW105133831 A TW 105133831A TW 105133831 A TW105133831 A TW 105133831A TW I713608 B TWI713608 B TW I713608B
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film
intermediate film
substrate
sio
flowable
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TW201728777A (zh
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蘭卡摩 卡路塔瑞奇
馬克 薩利
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

本案提供了沉積包含SiO或SiN的可流動薄膜的方法。某些方法包含：將基板表面曝露於矽氧烷或矽氮烷前驅物中；將基板表面曝露於電漿活化的共反應物中以提供SiON中間薄膜；紫外線固化SiON中間薄膜以提供固化的中間薄膜；以及退火固化的中間薄膜以提供包含SiO或SiN之薄膜。

Description

沉積包含SiO及SiN之可流動薄膜的方法
本發明大體上係關於沉積薄膜的方法。詳言之，本發明係關於含有矽的薄膜之可流動化學氣相沉積。
在包括半導體處理、擴散阻障塗層及磁讀取/寫入頭之介電質之各種行業中，在基板表面上沉積薄膜是重要的製程。詳言之，在半導體行業中，小型化受益於薄膜沉積之高階控制以在高深寬比結構上產生保形的塗層。用相對控制及保形沉積來沉積薄膜之一個方法是化學氣相沉積(chemical vapor deposition; CVD)。化學氣相沉積涉及將基板（例如晶圓）曝露於一或更多個前驅物中，該等前驅物反應以在基板上沉積薄膜。可流動化學氣相沉積(flowable chemical vapor deposition; FCVD)是一種化學氣相沉積類型，其允許沉積可流動薄膜，尤其是用於縫隙填充應用。
SiO及SiN可流動薄膜用於縫隙填充應用。目前，藉由三矽基胺(trisilylamine; TSA)以自由基形式NH3/O2作為共反應物生成該等薄膜。SiO薄膜的濕式蝕刻速率比(wet etch rate ratio; WER)為3。然而，小於2之濕式蝕刻速率比大體上目標是縫隙填充應用。自三矽基胺製程獲得之初沉積的薄膜包含作為主要組分之矽及氮，其中氧作為微量組分。
需要商業上可行並且展現可流動性質以及低濕式蝕刻速率比兩者之新的沉積化學品。本發明之態樣藉由提供新穎的化學品解決了該問題，該化學品是經特別設計並且經最佳化以利用沉積製程。尤其需要用於沉積包含SiO及SiN之可流動薄膜之新的化學品。
本發明之一個態樣係關於沉積包含SiO或SiN之薄膜之方法，該方法包含：將基板表面曝露於矽氧烷或矽氮烷前驅物中；將基板表面曝露於電漿活化的共反應物中以提供SiON中間薄膜；紫外線固化SiON中間薄膜以提供固化的中間薄膜；以及退火固化的中間薄膜以提供包含SiO或SiN之薄膜。
本發明之另一態樣係關於一種沉積包含SiO之薄膜之方法，該方法包含：將基板表面曝露於包含二矽氧烷之矽氧烷前驅物中；將基板表面曝露於遠端電漿活化的氨氣中以提供SiON中間薄膜；在臭氧存在下，紫外線固化SiON中間薄膜以提供固化的中間薄膜；以及蒸汽退火固化的中間薄膜以提供包含SiO之薄膜。
本發明之另一態樣係關於一種沉積包含SiN之薄膜之方法，該方法包含：將基板表面曝露於包含N,N'二矽基三矽氮烷之矽氮烷前驅物中；將基板表面曝露於遠端電漿活化的氨氣及/或氧氣中以提供SiON中間薄膜；紫外線固化SiON中間薄膜以提供固化的中間薄膜；以及氨氣退火固化的中間薄膜以提供包含SiN之薄膜。
在描述本發明之數個示範性實施例之前，應理解，本發明並不限制於以下描述中所列出的構造或製程步驟細節。本發明能夠具有其他實施例並且能夠以各種方式被實施或被執行。圖示的結構意欲包含具有標明化學式之所有該等錯合物及配位體。
已經驚人地發現，能夠在可流動化學氣相沉積(flowable chemical vapor; FCVD)製程中使用矽氧烷或矽氮烷前驅物獲得高品質可流動薄膜。此等前驅物與自電漿生成的自由基形式之共反應物一起使用。薄膜具有低濕式蝕刻速率比及低收縮率的有利效應。給定二矽氧烷的極高反應性情況下，使用二矽氧烷之實施例的結果尤其令人驚訝。由於該等薄膜之優越的特徴，薄膜尤其適合於縫隙填充應用。詳言之，薄膜的可流動性允許填充間隙。
在一或更多個實施例中，將矽氧烷或矽氮烷前驅物汽化至化學氣相沉積腔室，以及經由遠端電漿源將共反應物（例如，僅僅為氨氣或為具有或沒有氬氣的氨氣/氧氣）輸送至腔室，遠端電漿源將生成作為共反應物的電漿活性物質。電漿活化共反應物分子（自由基）具有高能量並且在氣相中與含矽前驅物分子反應以形成可流動SiON聚合物。該等聚合物沉積在晶圓上並且由於其流動性，該等聚合物將流過溝槽以及產生縫隙填充。隨後對該等薄膜進行固化（例如臭氧及/或紫外線）以及退火（例如蒸汽或氨氣）。
在一些實施例中，由直接電漿來生成可流動聚合物。隨後在開啟電漿時，可將矽氧烷或矽氮烷前驅物汽化至化學氣相沉積腔室，及將共反應物（例如氮氣、氬氣、氨氣、氧氣之任何組合或單一的共反應物）輸送至腔室。在一些實施例，自直接電漿沉積可流動薄膜，使得汽化的矽前驅物流入處理腔室中並且有或沒有共反應物都開啟電漿。
因此，本發明之一態樣係關於沉積包含SiO或SiN之薄膜之方法。在一或更多個實施例中，該方法包含：將基板表面曝露於矽氧烷或矽氮烷前驅物中；將基板表面曝露於電漿活化的共反應物中以提供SiON中間薄膜；紫外線固化SiON中間薄膜以提供固化的中間薄膜；以及退火固化的中間薄膜以提供包含SiO或SiN之薄膜。在一或更多個實施例中，該方法是可流動化學氣相沉積製程。
矽氧烷及矽氮烷都是含矽前驅物，該前驅物用作矽源及氧源或者氮源。在化學氣相沉積(chemical vapor deposition; CVD)腔室中汽化矽氧烷或矽氮烷前驅物以便曝露於基板表面。
在一些實施例中，前驅物是矽氧烷前驅物。在使用矽氧烷前驅物的實施例中，所得的薄膜包含SiO。如本文所使用的，「矽氧烷」係指具有至少一個Si-O-Si官能基之化合物。在一或更多個實施例中，矽氧烷可為支鏈的、環狀的或直鏈的。在一些實施例中，矽氧烷可具有多個Si-O-Si官能基。在一或更多個實施例中，矽氧烷沒有其他元素。例如，在一或更多個實施例中，矽氧烷前驅物選自式(I)至式(IX)：
Figure 02_image001
Figure 02_image003
在進一步實施例中，矽氧烷前驅物包含具有式(I)結構之二矽氧烷。
在一或更多個實施例中，前驅物是矽氮烷前驅物。在使用矽氮烷前驅物的實施例中，所得的薄膜包含SiN。如本文所使用的，「矽氮烷」係指具有至少一個Si-N-Si官能基之化合物。在一或更多個實施例中，矽氧烷可為支鏈的、環狀的或直鏈的。在一些實施例中，矽氮烷可具有多個Si-N-Si官能基。在一或更多個實施例中，矽氮烷沒有其他元素。例如，在一些實施例中，矽氮烷前驅物選自由以下各項組成的群組：
Figure 02_image005
在一或更多個實施例中，矽氮烷前驅物包含具有式(X)之結構之N,N'二矽基三矽氮烷。
如上所論述的，將基板表面曝露於電漿活化的共反應物。在一些實施例中，共反應物選自由氨氣、氧氣及其組合組成的群組。共反應物還可包含氬氣、氦氣及/或氮氣之一或更多者。視所使用的共反應物而定，電漿活化的共反應物亦將氮及/或氧輸送至薄膜。在涉及矽氧烷前驅物之一些實施例中，共反應物包含氨氣。在涉及矽氮烷前驅物之一些實施例中，共反應物包含氨氣和氧氣的混合物或僅僅包含氨氣。
在一些製程中，使用電漿提供足夠的能量以促進物質進入表面反應變得有利及可能的激發態。將電漿引入製程可為連續的或脈衝的。在一些實施例中，前驅物（或反應性氣體）及電漿之順序脈衝用以處理層。在一些實施例中，可直接地（即在處理區域內）或者遠端地（即在處理區域外）使試劑電離。在一些實施例中，遠端電離可發生於沉積腔室之上游，使得離子或其他高能或發光物質不與沉積薄膜直接接觸。在一些電漿增強製程中，諸如藉由遠端電漿產生器系統自處理腔室外部生成電漿。可經由熟習此項技術者已知的任何合適的電漿生成製程或技術生成電漿。例如，藉由微波(microwave; MW)頻率產生器或射頻(radio frequency; RF)產生器之一或更多者生成電漿。電漿之頻率可視所使用的特定反應性物質而調節。合適的頻率包括但不限於2MHz、13.56MHz、40MHz、60MHz及100MHz。
在一或更多個實施例中，經由遠端電漿源將共反應物輸送至含有汽化矽氧烷或矽氮烷前驅物之化學氣相沉積腔室，該遠端電漿源將生成電漿活性物質作為共反應物。在替代的實施例中，由直接電漿來生成可流動聚合物。
在一些實施例中，可按需要將基板連續地同時地或大體上同時地曝露於前驅物及電漿活化的共反應物中。如本文所使用的，術語「大體上同時地」意謂著一種組分流之大多數與另一種組分流重疊，儘管其中他們有時可能並非共同流動的。在替代的實施例中，順序地或大體上順序地將基板表面與兩個或兩個以上前驅物接觸。如本文所使用的，「大體上順序地」意謂著一個組分流之大多數並非與另一組分流重合，儘管可能存在一些重疊。
本說明書通篇所使用的「基板」係指在製造製程期間在其上執行薄膜處理之任何基板或形成於基板上之材料表面。例如，視應用而定，能夠在其上執行處理之基板表面包括諸如矽、氧化矽、應變矽、絕緣體上矽(silicon on insulator; SOI)、碳摻雜氧化矽、氮化矽、摻雜矽、鍺、砷化鎵、玻璃、藍寶石之材料以及諸如金屬、金屬氮化物、金屬合金及其他導電材料之任何其他材料。基板包括但不限於半導體晶圓。可將基板曝露於預處理製程以研磨、蝕刻、還原、氧化、羥基化、退火及/或烘焙基板表面。基板可包含節點裝置結構（例如32nm、22nm或低於20nm），以及可包括電晶體隔離、各種整合及犧牲間隔物，以及側壁間隔物雙圖案化(sidewall spacer double patterning; SSDP)微影術。在一或更多個實施例中，基板包含至少一個縫隙。基板可具有用於形成於基板上之裝置部件（例如電晶體）的間距及結構的複數個縫隙。縫隙可具有限定高度與寬度（即H/W）之深寬比(aspect ratio; AR)之高度及寬度，該深寬比顯著地大於1:1（例如5:1或5:1以上、6:1或6:1以上、7:1或7:1以上、8:1或8:1以上、8:1或8:1以上、10:1或10:1以上、11:1或11:1以上、12:1或12:1以上等等）。在許多情況下，高的深寬比是由於小的縫隙寬度，該縫隙寬度之範圍為自約90nm至約22nm或更少（例如約90nm、65nm、45nm、32nm、22nm、16nm等等）。
除了在基板自身的表面上直接地處理薄膜外，在本發明中還可在形成於基板上之下層上執行所揭示的薄膜處理步驟的任何步驟，如下面更詳細地揭示，並且術語「基板表面」意欲包括如上下文指示的此類下層。
在上述反應之任何反應之一或更多個實施例中，基於薄膜前驅物及基板表面之性質將選擇沉積反應的反應條件。可在大氣壓力下進行沉積，但還可在低壓下進行沉積。試劑的蒸氣壓應足夠的低以在該等應用中實用。基板的溫度應足夠的低以保持基板表面的鍵完整並且以防止氣體反應物熱分解。然而，基板的溫度還應足夠的高以保持薄膜前驅物處於氣態並且以提供充足的表面反應能量。特定的溫度視特定的基板、薄膜前驅物及壓力而定。可使用本領域已知的方法評估特定的基板、薄膜前驅物等之性質，允許選擇用於反應之適當的溫度和壓力。在一些實施例中，壓力小於約6.0托、5.0托、4.0托、3.0托、2.6托、2.0托或1.6托。在一或更多個實施例中，在溫度小於約200℃、175℃、150℃、125℃、100℃、75℃及/或大於約-1℃、0℃、23℃、50℃或75℃下進行沉積。
在將基板曝露於矽氧烷或矽氮烷前驅物及電漿活化的共反應物中之後沉積的薄膜包含SiON（被稱作「SiON中間薄膜」）。大體上，初沉積的薄膜是具有較少網狀結構及更多諸如Si-H、Si-OH及N-H之懸鍵之相對低緻密薄膜。因此，薄膜的濕式蝕刻速率比通常非常地高。為達得到低濕式蝕刻速率比/緻密薄膜的目的，進一步處理薄膜以獲得高密度薄膜。在該等處理期間，剩餘的反應鍵（例如SiH鍵、NH鍵）彼此相互反應或者與引入的分子（例如臭氧、水、氨氣）反應以形成具有更多網狀結構的薄膜。因此，為達移除氧或者氮以得到目標薄膜的目的，則對薄膜進行額外的固化及退火製程。在SiO薄膜情況下，在固化/退火期間移除氮以及增加氧給薄膜以生成SiO薄膜。然而，矽氧烷前驅物之一個優點是，由於矽氧烷前驅物包含Si-O，所以初沉積的薄膜在薄膜中已經具有更多的氧。因此，與自標準製程（例如彼等使用三矽基胺的製程）獲得的薄膜相比，自矽氧烷前驅物獲得的初沉積的薄膜更容易轉化成SiO。因此，對於矽氧烷薄膜來說將需要較少數量的固化/退火，這將有利地節約了晶圓處理時間。同樣，藉由矽氮烷獲得的SiN薄膜比自三矽基胺獲得的薄膜具有更多的存在於初沉積的薄膜中的氮。
在一或更多個實施例中，固化包含將中間SiON薄膜曝露於臭氧及/或紫外線(ultraviolet; UV)輻射中。在進一步實施例中，將中間SiON薄膜曝露於臭氧及紫外線固化以獲得包含SiO的薄膜。在另一實施例中，將中間SiON薄膜僅曝露於紫外線固化以獲得包含SiON的薄膜。
一或更多個實施例亦涉及退火製程。在一些實施例中，退火包含蒸汽退火。在另一實施例中，退火包含氨氣退火。
因此，例如在涉及矽氧烷前驅物（例如二矽氧烷）的一或更多個實施例中，使用臭氧及紫外線固化以及隨後藉由蒸汽退火SiON中間薄膜以生成SiO薄膜。在涉及矽氮烷前驅物（例如N,N'二矽基三矽氮烷）的一些實施例中，藉由紫外線固化，隨後藉由氨氣退火以生成SiN薄膜。
在一個示範性實施例中，方法包含：將基板表面曝露於包含二矽氧烷的矽氧烷前驅物中；將基板表面曝露於遠端電漿活化的氨氣中以提供SiON中間薄膜；在臭氧存在下紫外線固化SiON中間薄膜以提供固化的中間薄膜；以及蒸汽退火固化的中間薄膜以提供包含SiO之薄膜。
在進一步實施例中，方法是可流動化學氣相沉積製程。在另一示範性實施例中，方法包含：將基板表面曝露於包含N,N'二矽基三矽氮烷之矽氮烷前驅物中；將基板表面曝露於遠端電漿活化的氨氣及/或氧氣中以提供氮SiON中間薄膜；紫外線固化SiON中間薄膜以提供固化的中間薄膜；以及氨氣退火固化的中間薄膜以提供包含SiN之薄膜。
在進一步實施例中，方法是可流動化學氣相沉積製程。本發明之另一態樣係關於藉由本文描述的方法沉積的薄膜。薄膜與以前已知的可流動薄膜不同，由存在於下面實例部分的資料證明。在一或更多個實施例中，沉積的薄膜的濕式蝕刻速率比小於約2。
該等製程的優點是生成具有低濕式蝕刻速率及低收縮率的高密度可流動薄膜。矽氧烷已經在分子中具有Si-O鍵，此導致Si-O鍵存在於初沉積的薄膜中（與一些氮）。與目前已知技術相比，初沉積的薄膜轉化至SiO薄膜可使用較少的固化/退火時間及能量。又，初沉積的薄膜中存在SiO導致低收縮率以及低濕式蝕刻速率比。同樣，自矽氮烷獲得的初沉積的薄膜具有更多氮，這將需要較少的固化/退火時間和能量，以及薄膜具有低收縮率以及低濕式蝕刻速率比。該等薄膜特別適用於縫隙填充應用。因此，在一些實施例中，基板具有至少一個縫隙，並且製程至少部分地填充縫隙。
根據一或更多個實施例，在形成層之前或之後對基板進行處理。可在相同的腔室或在一或更多個分離處理腔室中執行該處理。在一些實施例中，將基板自第一腔室中移動至分離的第二腔室中以進一步處理。可將基板直接地自第一腔室移動至分離的處理腔室，或者可將基板自第一腔室移動至一或更多個移送腔室，以及隨後移動至所要的分離的處理腔室。因此，處理設備可包含與移送站連通的多個腔室。該類別的設備可被稱為「叢集工具」或「叢集系統」等等。
大體上，叢集工具是包含多個腔室之模組化系統，該腔室執行包括基板中心尋找及定向、除氣、退火、沉積及/或蝕刻之各種功能。根據一或更多個實施例，叢集工具包括至少第一腔室及中心移送腔室。中心移送腔室可容納機器人，機器人可介於處理腔室與載入鎖腔室之間及在處理腔室和載入鎖腔室之中往復移動基板。移送腔室通常保持在真空狀態並提供用於將基板自一個腔室往復移動至另一腔室及/或至定位在叢集工具之前端之載入閘室。可適用於本發明的兩種眾所周知的叢集工具是Centura®及Endura®，兩者都可購自加利福尼亞的聖克拉拉的應用材料公司(Applied Materials, Inc., of Santa Clara, Calif)。然而，為了執行如本文所描述的製程之特定步驟之目的，可改變腔室之準確的佈置及組合。可使用的其他處理腔室包括但不限於循環層沉積(cyclical layer deposition; CLD)，原子層沉積(atomic layer deposition; ALD)、化學氣相沉積(chemical vapor deposition; CVD)、物理氣相沉積(physical vapor deposition; PVD)、蝕刻、預清洗、化學清洗、諸如快速熱處理(rapid thermal treatment; RTP)的熱處理、電漿氮化、除氣、定向、羥基化及其他基板製程。藉由在叢集工具上之腔室內執行製程，在沉積後續薄膜之前無需氧化就能夠避免大氣雜質對基板表面的污染。
根據一或更多個實施例，基板連續地處於真空或「載入鎖」狀態下，並且當自一個腔室移動至下一個腔室時不曝露於周圍空氣中。因此，移送腔室處於真空狀態且在真空壓下「泵送」。惰性氣體可存在於處理腔室或移送腔室中。在一些實施例中，惰性氣體用作淨化氣體以在在基板表面形成層之後移除一些或所有的反應物。根據一或更多個實施例，將淨化氣體注入沉積腔室之出口以防止反應物自沉積腔室移動至移送腔室及/或額外的處理腔室。因此，惰性氣體流在腔室出口形成簾幕。
可在單個基板沉積腔室中處理基板，其中載入、處理及在處理另一個基板之前卸載單個基板。還可以以連續的方式處理基板，如輸送系統，其中將多個基板各自地載入腔室第一部分、移動穿過腔室並且自腔室的第二部分卸載。腔室之形狀及關聯的輸送系統可形成直線路徑或曲線路徑。另外，處理腔室可為旋轉料架，多個基板可在其中圍繞中心軸移動並且曝露於貫穿旋轉料架路徑的沉積、蝕刻、退火、清洗等製程中。
在處理期間，可加熱或冷卻基板。可藉由任何合適的手段來完成該加熱或冷卻，此任何合適的手段包括但不限於改變基板支撐的溫度以及流動加熱或冷卻氣體至基板表面。在一些實施例中，基板支撐包括可經控制以傳導性改變基板溫度之加熱器/冷卻器。在一或更多個實施例中，可加熱或冷卻所使用的氣體（反應性氣體或者惰性氣體）以局部地改變基板的溫度。在一些實施例中，加熱器/冷卻器經定位在鄰近基板表面之腔室內部以對流改變基板溫度。
在處理期間，基板還可為固定的或旋轉的。可連續地或以不連續的步驟將旋轉基板作旋轉。例如，可在整個製程中旋轉基板，或在曝露於不同反應性或淨化氣體之間可少量地旋轉基板。由於最小化例如在氣流幾何形態中的局部可變性的效應，在處理(連續地或者逐步地)期間旋轉基板可幫助產生更多均勻沉積或蝕刻。
在停止流動前驅物、共試劑等之後，可將基板及腔室曝露於淨化步驟。在本文所描述的任何態樣之一或更多個實施例中，可在將任何前驅物流動至/曝露於基板表面之後流動淨化氣體。可用流動速率來控制淨化氣體進入處理腔室，流動速率處於自約10sccm至約2,000sccm範圍內，例如，自約50sccm至約1,000sccm範圍內，並且在特定實例中，自約100sccm至約500sccm範圍內，例如約200sccm。淨化步驟移除處理腔室內的任何過量前驅物、副產物及其他污染物。可在一定時間段內實施淨化步驟，該時間段為自約0.1秒至約8秒範圍內，例如，自約1秒至約5秒的範圍內，以及在特定實例中，為約4秒。載氣、淨化氣體、沉積氣體或其他處理氣體可包含氮氣、氫氣、氬氣、氖氣、氦氣或其組合。在一個實例中，載氣包含氮氣。
該說明書通篇引用的「一個實施例」、「某些實施例」、「一或更多個實施例」或「實施例」意指與實施例有關所描述的特定特徴、結構、材料或特性被包括在本發明之至少一個實施例中。因此，在該說明書通篇各處的諸如「在一或更多個實施例中」、「在一些實施例中」、「在一個實施例中」或「在實施例中」的短語之出現無需參閱本發明相同的實施例。此外，特定特徵、結構、材料或特性可以任何合適的方式結合在一或更多個實施例中。
儘管已參考特定實施例描述了本文之本發明，應理解，該等實施例僅僅為說明瞭本發明的原理及應用。熟習此項技術者顯而易見的是，在不脫離本發明之精神及範疇的情況下可對本發明之方法及設備進行各種修改及變化。因此，本發明意欲包括在附加申請專利範圍及其等同物的範疇內之修改及變化。 實例 實例1——SiO沉積
根據本發明之一或更多個實施例使用二矽氧烷及遠端電漿活化的氨氣沉積薄膜。二矽氧烷、氨氣、氬氣及氦氣的流動速率分別地自400sccm至500sccm、10sccm至50sccm、400sccm至600sccm、50sccm至150sccm變化。初沉積的薄膜的折射率(refractive index; RI)為1.48。第1圖展示了示範性沉積薄膜之傅立葉變換紅外(fourier transform infrared; FTIR)光譜。自圖中可以看出，SiO、SiN、SiH及NH的峰是顯著的。存在兩種類型的SiH鍵伸展，一種在2175cm-1 處並且肩峰在2238cm-1 處。後一種峰源自在較多類網狀結構環境中的SiH鍵，同時在2175cm-1 處的峰源自在較少類網狀結構環境中的SiH鍵。在3374cm-1 處的NH伸展源自連接於SiON網狀結構中的NH鍵。 實例2——SiO薄膜的老化
根據本發明之一或更多個實施例使用二矽氧烷及遠端電漿活化的氨氣沉積薄膜。藉由保持在周圍條件（室溫、大氣壓力、在空氣中）將該薄膜老化四天。第2圖展示了初沉積的薄膜以及老化四天之後的沉積薄膜的傅立葉變換紅外光譜。自圖中可以看出，在老化四天之後，SiH及NH峰減少。反之，在老化四天之後，SiO及SiN峰增加。SiH峰自右向左偏移、NH峰的減少、SiO及SiN峰的增加展示了當老化時薄膜形成更多的網狀結構。因此，正如所料，因為SiH的存在，薄膜隨著時間而老化，導致薄膜收縮及折射率降低。
量測薄膜的折射率(refractive index; RI)及收縮率，並且在表1中展示。在表中可以看出，初沉積的薄膜的收縮率及折射率在四天內改變。在四天期間，折射率自1.48下降至1.45，同時收縮率自2增加至6.8。表 1 ：
Figure 105133831-A0304-0001
 實例3——比較SiO薄膜
使用三矽基胺(trimethylsilyl amine; TSA)及遠端電漿活化的氨氣/氧氣沉積比較薄膜（被稱作「三矽基胺薄膜」）。第3圖展示了該薄膜的傅立葉變換紅外光譜與實例1之薄膜的傅立葉變換紅外光譜的比較。自圖中可以看出，初沉積的三矽基胺薄膜並不具有顯著的SiO及SiN峰，而本發明的薄膜具有顯著的SiO及SiN峰。又，三矽基胺薄膜具有非常顯著的SiH峰，這意謂著本發明的薄膜的SiO+SiN/SiH之比率高於三矽基胺薄膜。該比率表示本發明薄膜比三矽基胺薄膜更穩定，因為二矽氧烷具有較少的SiH鍵，該SiH鍵反應性強。
初沉積的三矽基胺薄膜的折射率為1.6。如上文所論述，本發明的薄膜的折射率為1.48，該折射率接近純SiO薄膜。該結果指示，本發明的薄膜的特性比使用三矽基胺沉積的彼等薄膜更類似於純SiO薄膜。 實例4——蒸汽退火之效果
根據本發明之一或更多個實施例使用二矽氧烷及遠端電漿活化的氨氣沉積薄膜。第4圖展示了該薄膜的傅立葉變換紅外光譜。隨後藉由保持在環境條件（室溫、大氣壓力、在空氣中）將該薄膜老化十天。第5圖展示老化之後的薄膜的傅立葉變換紅外光譜。在老化十天之後亦將薄膜在500℃下蒸汽退火。第6圖展示了退火之後的薄膜的傅立葉變換紅外光譜。自圖中可以看出，在蒸汽退火之後，僅僅可以看出對應於純SiO薄膜的峰。
進行根據上文的數個薄膜的蒸汽退火試驗以確定退火薄膜的濕式蝕刻速率比及收縮率隨沉積溫度而變化。第7圖概述了結果。如圖中所展示，當沉積溫度較高時，濕式蝕刻速率比及收縮率較低。該等薄膜的濕式蝕刻速率比為自3.5至5的範圍內及收縮率為自22至28%的範圍內。
第8A圖至第8D圖展示了演示蒸汽退火效果及稀氫氟酸(dilute hydrofluoric acid; DHF)的裝飾之掃描式電子顯微鏡(scanning electron microscope; SEM)影像。第8A圖是使用二矽氧烷及遠端電漿活化的氨氣在53℃下沉積的不退火或不稀氫氟酸浸沒的初沉積的薄膜的掃描式電子顯微鏡影像。第8B圖至第8D圖展示了使用二矽氧烷及遠端氨氣電漿分別在-1℃、24℃及53℃下沉積的且在蒸汽退火及一分鐘稀氫氟酸浸沒之後的薄膜。自圖中可以看出，對於在53℃沉積的薄膜，溝槽內的薄膜在稀氫氟酸中已經部分地保存下來而其他在較低溫度下沉積的薄膜在稀氫氟酸中被蝕刻。該等結果表示較高沉積溫度得到更好的薄膜品質。 實例5——SiN沉積
使用N,N'二矽基三矽氮烷作為含矽前驅物以及遠端電漿活化的氨氣或者遠端電漿活化的氨氣/氧氣作為反應性氣體來沉積包含SiN薄膜。介於40℃至60℃之間在自0.9托至1.2托範圍內的壓力下沉積可流動薄膜。N,N'二矽基三矽氮烷、氨氣、氧氣、氬氣及氦氣的流動速率分別地自0.2至0.4g/min、55sccm至85sccm、7sccm至10sccm、560sccm至725sccm、700sccm至800sccm變化。初沉積的薄膜之折射率為1.58。
第9圖展示了來自遠端電漿活化的氨氣及遠端電漿活化的氨氣/氧氣的初沉積的薄膜的典型的傅立葉變換紅外光譜。在僅氨氣的薄膜的傅立葉變換紅外光譜中，SiN、SiH及NH的峰顯著，而对於SiO在1000cm-1 處的SiH峰中存在肩部。在氨氣/氧氣的薄膜中，SiN峰顯著降低並且SiO的肩部比僅氨氣的薄膜的SiO的肩部高一點。因此，當使用氨氣時，薄膜的SiN多於SiO。 實例6——比較SiN薄膜
使用三矽基胺及氨氣沉積比較薄膜。氨氣為遠端電漿活化的。第10圖展示該薄膜的傅立葉變換紅外光譜以及實例5之N,N'二矽基三矽氮烷/氨氣薄膜之傅立葉變換紅外光譜資料。自圖中可以看出，與三矽基胺薄膜相比，N,N'二矽基三矽氮烷薄膜的SiN尖峰強度更高及SiH強度更低。當轉化成SiN薄膜時，在薄膜中存在較高數量的SiN是有利的。較低數量的SiH表示自N,N'二矽基三矽氮烷獲得的薄膜反應性較小，這將導致較小的收縮率。
同樣，第11圖展示了使用三矽基胺及氨氣/氧氣以及N,N'二矽基三矽氮烷/氨氣/氧氣沉積的薄膜的傅立葉變換紅外光譜的比較。該等光譜展示了自N,N'二矽基三矽氮烷獲得的薄膜的較低的SiH及較高的SiN尖峰強度，此再次表明對於SiN可流動薄膜來說，N,N'二矽基三矽氮烷是比三矽基胺更優越的前驅物。
實例7--SiN薄膜及比較薄膜之老化
隨後藉由保持在環境條件(室溫、大氣壓力、在空氣中)將使用三矽基胺及遠端電漿活化的氨氣/氧氣混合物沉積的薄膜老化四天。第12圖展示了初沉積的三矽基胺薄膜及其老化之後的傅立葉變換紅外光譜。第13圖展示使用N,N'二矽基三矽氮烷及電漿活化的氨氣/氧氣混合物沉積的薄膜的初沉積時及其老化四天之後的傅立葉變換紅外光譜資料。
自圖中可以看出，當與N,N'二矽基三矽氮烷薄膜相比時，三矽基胺薄膜顯示出在老化期間增加的SiO尖峰強度。該等結果表示自空氣中吸收水分及氧氣，三矽基胺薄膜比N,N'二矽基三矽氮烷薄膜更快速。又，因為N,N'二矽基三矽氮烷薄膜反應性較小，N,N'二矽基三矽氮烷薄膜中的SiH尖峰強度的下降更小。
實例8--SiN薄膜之掃描式電子顯微鏡影像
第14圖展示了初沉積的可流動薄膜之掃描式電子顯微鏡影像。使用N,N'二矽基三矽氮烷及遠端電漿活化的氨氣/氧氣混合物沉積薄膜。
實例9--SiO及SiN薄膜之組成分析
進行三矽基胺、二矽氧烷及N,N'二矽基三矽氮烷薄膜之溝槽內的成分分析。執行透射式電子顯微鏡(transmission electron microscopy；TEM)/電子能耗譜儀(electron energy loss spectroscopy; EELS)以分析薄膜的溝槽內組成物。第15A圖至第15C圖展示了如上所述製備的二矽氧烷及三矽基胺薄膜的矽、氧和氮的元素組成。第16A圖至第16C圖展示了如上所述製備的N,N'二矽基三矽氮烷及三矽基胺薄膜之成分。如上所述沉積該等薄膜，隨後藉由臭氧及紫外線固化。在三矽基胺薄膜與二矽氧烷薄膜比較中，二矽氧烷薄膜的矽及氧含量比三矽基胺薄膜的矽及氧含量高。最重要地，氮含量幾乎為零。因此，對於沉積可流動SiO，二矽氧烷可為比三矽基胺前驅物更好的矽前驅物。與自三矽基胺獲得的薄膜相比，自N,N'二矽基三矽氮烷獲得的薄膜具有較高的矽及氮含量。又，N,N'二矽基三矽氮烷薄膜中的氧含量較低，此表示N,N'二矽基三矽氮烷是沉積SiN可流動薄膜的更好的候選。在二矽氧烷及N,N'二矽基三矽氮烷兩種情況下，電子能耗譜儀結果與初沉積的薄膜的傅立葉變換紅外光譜相當。
無
因此，以可詳細理解本發明上述特徵的方式，參考實施例可獲得上文簡要地概述本發明之更特定描述，在附圖中圖示一些實施例。然而，應注意，附圖僅圖示本發明之典型實施例，並且因此不應認為是本發明之範疇之限制，因為本發明可承認其他同等有效之實施例。
第1圖是根據本發明之一或更多個實施例沉積的薄膜之傅立葉變換紅外(fourier transform infrared; FTIR)光譜；
第2圖是根據本發明之一或更多個實施例沉積的薄膜以及在老化四天之後的薄膜之傅立葉變換紅外光譜；
第3圖是根據本發明之一或更多個實施例沉積的薄膜及比較薄膜之傅立葉變換紅外光譜之比較；
第4圖是根據本發明之一或更多個實施例沉積的薄膜之傅立葉變換紅外光譜；
第5圖是根據本發明之一或更多個實施例沉積的老化十天之後的薄膜之傅立葉變換紅外光譜；
第6圖是根據本發明之一或更多個實施例沉積的蒸汽退火之後的薄膜之傅立葉變換紅外光譜；
第7圖是根據本發明之一或更多個實施例沉積的薄膜之濕式蝕刻比及收縮率之曲線圖；
第8A圖至第8D圖是根據本發明之一或更多個實施例在各種條件下沉積的薄膜之掃描式電子顯微鏡影像；
第9圖是根據本發明之一或更多個實施例沉積的兩個薄膜之傅立葉變換紅外光譜；
第10圖是根據本發明之一或更多個實施例沉積的薄膜及比較薄膜之傅立葉變換紅外光譜之比較；
第11圖是根據本發明之一或更多個實施例沉積的薄膜及比較薄膜之傅立葉變換紅外光譜之比較；
第12圖是初沉積的比較薄膜及老化四天之後的比較薄膜之傅立葉變換紅外光譜之比較；
第13圖是根據本發明之一或更多個實施例沉積的薄膜在初沉積時及老化四天之後之傅立葉變換紅外光譜之比較；
第14圖是根據本發明之一或更多個實施例沉積的薄膜之掃描式電子顯微鏡影像；
第15A圖至第15C圖是展示根據本發明之一或更多個實施例沉積的薄膜及比較薄膜之溝槽內組成物之散點圖；以及
第16A圖至第16C圖是展示根據本發明之一或更多個實施例沉積的薄膜及比較薄膜之溝槽內組成物之散點圖。
國內寄存資訊(請依寄存機構、日期、號碼順序註記) 無
國外寄存資訊 (請依寄存國家、機構、日期、號碼順序註記) 無
(請換頁單獨記載) 無

Claims (9)

  1. 一種沉積包含SiO之一薄膜的方法，該方法包含以下步驟：將一基板表面曝露於一矽氧烷前驅物中，該矽氧烷前驅物選自由以下各項組成的群組：
    Figure 105133831-A0305-02-0028-1
     將該基板表面曝露於一遠端電漿活化的共反應物中以藉由化學氣相沉積提供一可流動SiON中間薄膜；紫外線固化該可流動SiON中間薄膜以提供一固化的中間薄膜；以及退火該固化的中間薄膜以提供包含SiO之一薄膜。
  2. 如請求項1所述之方法，其中該共反應物包含氨氣及/或氧氣。
  3. 如請求項1所述之方法，其中退火包含蒸汽退火。
  4. 如請求項1所述之方法，其中該矽氧烷前驅物進一步包含二矽氧烷。
  5. 一種沉積包含SiO之一薄膜之方法，該方法包含以下步驟：將一基板表面曝露於包含二矽氧烷之一矽氧烷前驅物中；將該基板表面曝露於一遠端電漿活化的氨氣中以藉由化學氣相沉積提供一可流動SiON中間薄膜；在臭氧存在下，紫外線固化該SiON中間薄膜以提供一固化的中間薄膜；以及蒸汽退火該固化的中間薄膜以提供包含SiO之一薄膜。
  6. 一種使用氧化矽填充一基板中的一縫隙的方法，該方法包含以下步驟：將一基板表面曝露於一矽氧烷前驅物中，該矽氧烷前驅物選自由以下各項組成的群組：
    Figure 105133831-A0305-02-0029-2
    Figure 105133831-A0305-02-0030-3
     將該基板表面曝露於一遠端電漿活化的共反應物中以藉由化學氣相沉積提供一可流動SiON中間薄膜，該可流動SiON中間薄膜流入該縫隙中以填充該縫隙；將填充該縫隙之該可流動SiON中間薄膜紫外線固化以提供填充該縫隙之一固化的中間薄膜；以及退火該固化的中間薄膜以提供一使用包含SiO之一薄膜填充之縫隙。
  7. 如請求項6所述之方法，其中該共反應物包含氨氣及/或氧氣。
  8. 如請求項6所述之方法，其中退火包含蒸汽退火。
  9. 如請求項6所述之方法，其中該矽氧烷前驅物進一步包含二矽氧烷。
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