TWI756350B - 藉由熱ald及peald沉積氧化物膜之方法 - Google Patents

藉由熱ald及peald沉積氧化物膜之方法 Download PDF

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TWI756350B
TWI756350B TW107103230A TW107103230A TWI756350B TW I756350 B TWI756350 B TW I756350B TW 107103230 A TW107103230 A TW 107103230A TW 107103230 A TW107103230 A TW 107103230A TW I756350 B TWI756350 B TW I756350B
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reaction chamber
oxide film
gas
thermal ald
peald
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TW201835381A (zh
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深澤篤毅
福田秀明
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美商Ａｓｍ Ｉｐ控股公司
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Abstract

一種藉由熱ALD及PEALD於基板上沉積氧化物膜之方法，其包括：於反應室中提供基板；於反應室中藉由熱ALD於基板上沉積第一氧化物膜；及未中斷真空，於反應室中藉由PEALD於第一氧化物膜上連續沉積第二氧化物膜。

Description

藉由熱ALD及PEALD沉積氧化物膜之方法 發明背景
本發明大致係關於一種藉由熱原子層沉積(熱ALD)及電漿增強型原子層沉積(PEALD)沉積氧化物膜之方法。
隨著半導體裝置小型化的進展，在半導體製造製程期間所引起對凹部圖案或下方層的損傷更成問題。此係由於當裝置小型化時，由對凹部圖案或下方層的損傷所引起之尺寸變化更大程度地影響圖案化精密度，從而導致功能降級。習知使用SiO膜來進行圖案化或用作藉由PEALD沉積之功能膜；然而，使用直接電漿(即電容耦合電漿(CCP))之PEALD對凹部圖案或下方層導致損傷，且損傷程度傾向於與電漿功率相關，因此，已使用低RF功率來製造小型化半導體裝置。特定而言，對於具有低抗氧化性之碳基下方層，常使用施加低RF功率來最小化對下方層之損傷。當藉由膜收縮率來表示損傷時，習知下方膜通常顯示約2至5%之收縮率。然而，愈來愈需要小型化裝置中之較低膜收縮率。
對於相關技術之問題及解決方法的任何論述已包括在本揭示中，而僅用於提供本發明之背景脈絡之目的，且不應被視為同意該論述的任何或全部在本發明完成之際為已知。
在一些具體例中，使用包括熱ALD作為第一步驟及PEALD作為第二步驟之連續二步製程來形成氧化物膜，以避免使基板之下方層暴露至電漿，藉此抑制下方層的尺寸降級及/或氧化。在一些具體例中，第一步驟及第二步驟係於相同反應室中連續進行。在一些具體例中，由於即使當處於非激發狀態時，用於熱ALD之反應物及前驅體的反應性亦較用於PEALD者高，因此在熱ALD中以不同於PEALD的流動路徑將反應物供應至反應室。用於熱ALD之前驅體可與用於PEALD之前驅體相同或不同。
出於概述本發明之態樣及相對於相關技術所達成之優點的目的，在本揭示中描述本發明之某些目標及優點。當然，應明瞭無須所有該等目的或優點皆可根據本發明之任何特定具體例來達成。因此，舉例而言，熟習此項技術者將認知到，可以如本文中所教示般地達成或最佳化一個優點或一組優點而無須達成本文中可能教示或建議之其他目標或優點的方式來體現或實施本發明。
本發明之其他態樣、特徵及優點將自隨後之詳細描述顯而易見。
1‧‧‧基板
2‧‧‧導電平板電極；基座
3‧‧‧反應室
4‧‧‧導電平板電極；噴灑頭
5‧‧‧轉移室
6‧‧‧排氣管線
7‧‧‧排氣管線
11‧‧‧反應室3之內部
12‧‧‧電接地之一側
13‧‧‧圓管
14‧‧‧分隔板
16‧‧‧轉移室5之內部(轉移區)
17‧‧‧氣體埠
18‧‧‧氣體埠
20‧‧‧瓶(儲槽)
21‧‧‧氣體管線
22‧‧‧氣體管線
23‧‧‧歧管管道
24‧‧‧密封氣體管線
25‧‧‧RF源
26‧‧‧氣體管線
27‧‧‧氣體管線
31‧‧‧氣體管線
32‧‧‧氣體管線
33‧‧‧氣體管線
34‧‧‧氣體管線
35‧‧‧氣體管線
36‧‧‧氣體埠
37‧‧‧孔洞
41‧‧‧歧管管道
42‧‧‧閘閥
43‧‧‧基座
44‧‧‧噴灑頭
45‧‧‧排氣管線
51‧‧‧RF源
52‧‧‧反應室
a‧‧‧閥
b‧‧‧閥
c‧‧‧閥
d‧‧‧閥
e‧‧‧閥
f‧‧‧閥
現在將參看意欲說明而非限制本發明之較佳具體例的圖式來描述本發明之此等及其他特徵。該等圖式經大大簡化以用於說明性目的且未必按比例繪製。
圖1A為可用於本發明之一具體例中的用於熱ALD及電漿增強型ALD(PEALD)沉積氧化物膜之ALD(原子層沉積)設備之示意性表示圖。
圖1B說明可用於本發明之一具體例中之使用流通系統 (FPS)之前驅體供應系統的示意性表示圖，其中(a)呈現載氣流動通過瓶以自其載送前驅體之狀態，及(b)呈現載氣繞過瓶之狀態。
圖2顯示在根據本發明之一具體例之一個循環中之熱ALD的示意性製程序列，其中灰色格子表示「開」狀態，而白色格子表示「關」狀態，且各欄之寬度不代表各製程的持續時間。
圖3顯示根據本發明之一具體例於一個循環中之熱ALD之示意性製程序列與一個循環中之PEALD之示意性製程序列之組合，其中灰色格子表示「開」狀態，而白色格子表示「關」狀態，且各欄之寬度不代表各製程之持續時間。
圖4顯示在根據本發明之一具體例之一個循環中之PEALD的示意性製程序列，其中灰色格子表示「開」狀態，而白色格子表示「關」狀態，且各欄之寬度不代表各製程的持續時間。
圖5顯示在根據本發明之另一具體例之一個循環中之熱ALD的示意性製程序列，其中灰色格子表示「開」狀態，而白色格子表示「關」狀態，且各欄之寬度不代表各製程的持續時間。
圖6顯示根據本發明之另一具體例於一個循環中之熱ALD之示意性製程序列與一個循環中之PEALD之示意性製程序列之組合，其中灰色格子表示「開」狀態，而白色格子表示「關」狀態，且每一欄之寬度不表示各製程之持續時間。
圖7為可用於本發明之另一具體例中的用於熱ALD及電漿增強型ALD(PEALD)沉積氧化物膜之ALD(原子層沉積)設備之示意性表示圖。
在本揭示內容中，視上下文而定，「氣體」可包括汽化之固體及/或液體且可由單一氣體或氣體混合物構成。同樣地，視上下文而定， 冠詞「一(a)」或「一(an)」係指物種或包括多個物種之屬。在本揭示內容中，經由噴灑頭或另一埠引入至反應室之製程氣體可包含含矽或金屬之前驅體及添加劑氣體、基本上由含矽或金屬之前驅體及添加劑氣體組成或由含矽或金屬之前驅體及添加劑氣體組成。添加劑氣體可包括用於氧化前驅體之反應物氣體，及當向添加劑氣體施加RF功率時用來激發前驅體的惰性氣體(例如，稀有氣體)。惰性氣體可作為載氣及/或稀釋氣體饋送至反應室。前驅體及添加劑氣體可作為混合氣體或個別地引入至反應空間。前驅體可利用載氣(諸如稀有氣體)引入。可使用除製程氣體外之氣體(即，非通過噴灑頭引入之氣體)來(例如)密封反應空間，該氣體包括諸如稀有氣體之密封氣體。在一些具體例中，術語「前驅體」一般係指參與化學反應產生另一化合物之化合物，及特定言之係指一種構成膜基質或膜之主要骨架的化合物，而術語「反應物」係指除前驅體外之化合物，其活化前驅體、改質前驅體、或催化前驅體之反應，其中當施加RF功率時，該反應物可向膜基質提供元素(諸如O)並成為膜基質之一部分。術語「惰性氣體」係指當施加RF功率時激發前驅體的氣體，但不同於反應物，其未成為膜基質之一部分。
在一些具體例中，「膜」係指在垂直於厚度方向之方向中連續延伸且實質上無針孔以覆蓋整個目標或關注表面的層，或僅係覆蓋目標或關注表面之層。在一些具體例中，「層」指形成於表面上的具有特定厚度之結構，或膜之同義詞或非膜結構。膜或層可由具有特定特性之離散單一膜或層或多個膜或層構成，且相鄰膜或層之間的邊界可以或可不清晰且可基於相鄰膜或層之物理、化學及/或任何其他特性、形成製程或序列及/或功能或用途而確定。此外，在本揭示中，變數之任何兩個數目可構成變數之可工作範圍，此係因為可工作範圍可基於例行工作而判定，且所指示之任何範圍可包括或不包括端點。另外，所指示的變數之任何值(不管該等值是否用「約」指示)可指精確值或近似值且包括等效值，且在一些具體例中可指平均值、中值、代表值、多數值等。此外，在本揭示中，在一些具 體例中，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......構成」或「由......構成」。在本揭示中，在一些具體例中，任何已定義之意義未必不包括一般及慣用意義。
在本揭示中未規定條件及/或結構之處，熟悉本技藝者可鑒於本揭示根據常規實驗容易地提供此等條件及/或結構。
在所有所揭示具體例中，一具體例中所使用之任何元件可由與之等效的任何元件替換，包括用於預期用途而在本文中明確地、必須地或固有地揭示之彼等元件。此外，本發明同樣可適用於設備及方法。
將針對較佳具體例來說明該等具體例。然而，本發明不限於該等較佳具體例。
在一具體例中，一種藉由熱ALD及PEALD於基板上沉積氧化物膜之方法包括：於反應室中提供基板；於反應室中藉由熱ALD於基板上沉積第一氧化物膜；及未中斷真空，於反應室中藉由PEALD於第一氧化物膜上連續沉積第二氧化物膜。
以上，「連續」一詞係指下列中之至少一者：空間無中斷(例如，未移動基板)，流動無中斷(例如，至少一個未中斷的流入)，未暴露至環境氛圍，及無任何材料介入步驟(除諸如排空之輔助步驟或其他可忽略步驟外)，視具體例而定。在本揭示中，「連續」流動具有恆定流動速率(替代地，即使流動係「連續」，但其流動速率可隨時間改變)。
在一些具體例中，由於可將含H2O或OH基之氣體作為反應物用於熱ALD，因此可能會有殘餘水分留在反應室內部，因此，為藉由使用諸如H2之還原氣體來降低反應室內部的水分分壓，可在維持熱ALD及PEALD之連續性的同時於熱ALD與PEALD之間自反應室移除殘留水分。
由於第一氧化物膜係藉由熱ALD在未暴露至電漿之情況下沉積於基板之下方層上，因此可有效抑制對下方層的損傷，例如，在於(例 如)約100℃之溫度下進行之熱ALD期間可有效地抑制作為用於圖案化之下方層之含碳膜(例如，藉由旋塗或CVD製程製得之非晶形碳)的尺寸降級(例如，下方層的收縮率減小)，或在於(例如)約300℃之溫度下進行之熱ALD期間可有效地抑制作為下方層之矽基板的氧化(例如，下方層之經氧化部分的厚度減小)。於藉由熱ALD沉積第一氧化物膜後，藉由PEALD於第一氧化物膜上連續沉積第二氧化物膜。由於下方層受到第一氧化物膜保護免於PEALD中所使用之電漿，因此下方層不會受到PEALD的損傷。
在一些具體例中，氧化物膜係有效地沉積於具有圖案化凹部(例如，溝槽)的基板上。在本揭示內容中，將相鄰垂直間隔件間之凹部及任何其他凹部圖案稱作「溝槽」。換言之，溝槽係包括由垂直間隔件所形成之圖案的任何凹部圖案，且其在一些具體例中具有約20nm至約100nm(通常約30nm至約50nm)之寬度(其中當溝槽具有與寬度實質上相同的長度時，將其稱作孔洞/通孔，且其直徑為約20nm至約100nm)，約30nm至約100nm(通常約40nm至約60nm)之深度，及約1至約10(通常約2至約5)之縱橫比。溝槽的適合尺寸可視製程條件、膜組成、預期應用等而改變。
藉由熱ALD之第一氧化物膜的膜品質不如藉由PEALD之第二氧化物膜的膜品質般良好，因此，藉由於相同反應室中連續地進行熱ALD及PEALD，避免第一氧化物膜暴露至環境氛圍(例如，空氣)，從而保護第一氧化物膜之表面。通常，第一氧化物膜具有較第二氧化物膜高的濕蝕刻速率及低的密度。由於第一及第二氧化物膜係連續地沉積，因此將由第一及第二氧化物膜所構成的膜視為藉由ALD的單一氧化物膜，其中第一氧化物膜充作保護層，而第二氧化物膜充作決定或控制組合氧化物膜之整體性質的本體層。在一些具體例中，第一氧化物膜具有約1nm至約7nm(例如，約2nm至5nm)之厚度，及第二膜具有約5nm至約30nm(例如，約8nm至20nm)之厚度，其中第二膜較厚於第一膜。
雖然藉由熱ALD之第一氧化物膜及藉由PEALD之第二氧化物膜係連續地沉積，但其間的邊界或界面可藉由利用SIMS(第二離子質譜術)的組成分析來呈現或識別，例如，其顯示於邊界或界面處之Si、O、H、C等的濃度變化。例如，當藉由熱ALD之第一氧化物膜及藉由PEALD之第二氧化物膜皆係在相同溫度(例如，100℃)下沉積時，由於在熱ALD中之反應性較在PEALD中者弱，因此即使當使用相同的前驅體時，第一氧化物膜亦具有較第二氧化物膜高之碳及水分濃度。藉由STEM(掃描穿透電子顯微術)的結構觀察可能無法呈現邊界或界面。
在一些具體例中，熱ALD之循環包括將前驅體饋送至反應室，該前驅體係選自由胺基矽烷、矽烷胺、異氰酸酯矽烷、羥乙磺酸酯矽烷、無機矽烷、含矽烷氫氧化物、及含矽烷烷氧化物所組成之群之至少一種化合物的氣體。在一些具體例中，前驅體包含金屬(諸如Ti、Zr、及Hf)替代矽，從而形成(例如)由TiO、ZrO、及HfO所構成之膜。
在一些具體例中，熱ALD之循環包括將反應物饋送至反應室，該反應物係選自由H2O、醚、醇(例如，甲醇、乙醇等)、H2及O2之混合物、及H2O2所組成之群之至少一種氣體。此反應物可不利用電漿激發而與吸附於基板表面上之前驅體反應。因此，雖然通常存在三種將反應物饋送至反應室之方式(即藉由將反應物引入至設置於反應室內部之噴灑頭上游之歧管管道，藉由於噴灑頭處引入反應物，及/或藉由於噴灑頭與其上放置基板之基座之間引入反應物而將反應物饋送至反應室)，但應視反應物之反應性而選擇合適的饋送方法。
在一些具體例中，PEALD之循環包括使用連續流至反應室之載氣來於一脈衝中饋送前驅體，且將反應物連續饋送至反應室。在一些具體例中，反應物係選自由O2、CO2、及N2O組成之群的至少一種氣體。
在一些具體例中，熱ALD之循環包括在整個循環連續地將反應物饋送至反應室，該反應物係選自由乙醇、H2O、及O3組成之群的至少一種氣體。當反應物之反應性不高時，可使反應物連續流動通過反應室。 然而，由於反應性低，因此要耗費長時間來完成期望厚度之膜的沉積。因此，在一些具體例中，熱ALD之循環包括於一脈衝中將催化氣體饋送至反應室，其係除前驅體及反應物外之氣體並且能夠促進氧化物膜於循環中之沉積。藉由饋送催化氣體，可針對熱ALD顯著改良膜的沉積速率，且其使反應性可能低的反應物氣體能夠連續地流動。當反應物不僅於PEALD中並且於熱ALD中連續地流動時，儘管熱ALD及PEALD可能需要不同的反應物，但反應室內部之壓力可於整個熱ALD之循環及PEALD之循環中實質上地恆定。
在一些具體例中，催化氣體係選自由吡啶、烷基金屬、吡啶基矽烷、矽烷胺、及矽氮烷組成之群之至少一種化合物的氣體。
在一些具體例中，沉積方法進一步包括於藉由熱ALD及PEALD進行沉積後，清潔反應室。可於熱ALD及PEALD之後進行相同的清潔製程。在一些具體例中，清潔係使用清潔氣體藉由在於氣體混合室中混合前驅體及反應物之位置的上游饋送清潔氣體來實施，以致可清潔氣體混合室、噴灑頭之通道、反應室、排氣通道等。在一些具體例中，清潔氣體係藉由在反應室上游之遠端電漿單元來激發或使用含氟氣體(例如，ClF3)原位激發。在一些具體例中，清潔係於每n次重複由熱ALD之循環及PEALD之循環所構成之沉積循環後進行，其中重複次數n係小於沉積於反應室之內壁等等上之不期望的膜開始自內壁剝離，藉此產生污染物顆粒的重複次數。
該等具體例將參看圖式作說明。然而，本發明不限於該等圖式。
圖2顯示在根據本發明之一具體例之一個循環中之熱ALD的示意性製程序列，其中灰色格子表示「開」狀態，而白色格子表示「關」狀態，且各欄之寬度不代表各製程的持續時間。在圖2中所說明之序列中，在一脈衝(「饋送」)中，使用連續供應之載氣及稀釋氣體(共同稱為「惰性氣體」)來供應前驅體。此操作可使用流通系統(FPS)完成，在該系統中，載氣管線具備具有前驅體儲槽(瓶)之迂迴管線，且主管線及迂迴管線經切換，其中當僅意欲將載氣饋送至反應室時，迂迴管線關閉，而當意欲將載氣及前驅體氣體兩者饋送至反應室時，主管線關閉且載氣流過迂迴管線且與前驅體氣體一起自瓶流出。以此方式，載氣可連續地流至反應室中，且可藉由切換主管線及迂迴管線而於脈衝中載運前驅體氣體。圖1B說明根據本發明之一具體例的使用流通系統(FPS)的前驅體供應系統(黑色閥指示該等閥關閉)。如圖1B中之(a)所示，當將前驅體饋送至反應室(未圖示)時，首先，諸如Ar(或He)之載氣流過具有閥b及c之氣體管線，接著進入瓶(儲槽)20。載氣自瓶20流出，同時載運對應於瓶20內之蒸氣壓力之量的前驅體氣體，且流過具有閥f及e之氣體管線，接著與前驅體一起被饋送至反應室。在上述製程中，閥a及d關閉。當僅將載氣(稀有氣體)饋送至反應室時，如圖1B中之(b)所示，載氣流過具有閥a之氣體管線，同時繞過瓶20。在上述製程中，閥b、c、d、e及f關閉。
在圖2中，前驅體係藉助於載氣(「惰性氣體」)來提供。由於ALD係自限制吸附反應製程，因此所沉積的前驅體分子之數目係藉由反應性表面位點之數目確定，且與飽和後的前驅體暴露無關，且前驅體之供應係使得反應性表面位點在每個循環飽和。在一脈衝(「反應」)中將用於沉積反應之反應物供應至反應室，其中反應物經熱活化(例如，H2O蒸氣)以與暴露於吸附在基板上之前驅體表面上的位點(例如，-CH3)反應，同時未饋送前驅體而將惰性氣體連續地饋送至反應室，藉此形成一單層。
如上文所提及，每一沉積循環之每一脈衝或階段較佳為自限制的。在每一階段供應過量的前驅體以使敏感的結構表面飽和。表面飽和確保前驅體佔據所有可用反應性位點(受到例如實體大小或「位阻(steric hindrance)」限制)，且因此確保極佳之階梯覆蓋率。在一些具體例中，可減小一或多種前驅體的脈衝時間，使得未達到完全飽和且低於一單層吸附於 基板表面上。在「饋送」之後，排空反應室(「排空1」)，其中無前驅體被饋送至反應室，同時不供應反應物，而將惰性氣體連續地饋送至反應室，藉此自基板之表面移除非化學吸附的前驅體及多餘氣體。在「反應」之後，排空反應空間(「排空2」)，其中將惰性氣體連續地饋送至反應室，但不將前驅體及反應物饋送至反應室，藉此自基板之表面移除副產物及多餘氣體。歸因於惰性氣體之連續流動進入反應室中作為前驅體經間歇地或於脈衝中注入其中之恆定流，可有效率地進行排空以快速地自層之表面移除多餘氣體及副產物，藉此有效率地繼續多個熱ALD循環，直至獲得期望厚度的層為止。
圖4顯示在根據本發明之一具體例之一個循環中之PEALD的示意性製程序列，其中灰色格子表示「開」狀態，而白色格子表示「關」狀態，且各欄之寬度不代表各製程的持續時間。在圖4中所說明之序列中，在一脈衝(「饋送」)中，使用連續供應之載氣及稀釋氣體(共同稱為「惰性氣體」)來供應前驅體。此可使用如以上關於圖2之製程序列所述的流通系統(FPS)來完成。
在圖4中，前驅體係藉助於載氣(「惰性氣體」)來提供。由於ALD係自限制吸附反應製程，因此所沉積的前驅體分子之數目係藉由反應性表面位點之數目確定，且與飽和後的前驅體暴露無關，且前驅體之供應係使得反應性表面位點在每個循環飽和。用於沉積之電漿係藉由在整個沉積循環連續地流動之反應物氣體(「反應物」)(例如，O2)中在一脈衝(「RF」)中原位施加RF功率而產生，同時亦將惰性氣體及反應物連續地饋送至反應室，但不饋送前驅體，藉此形成一單層。
如以上關於圖2之序列所提及，供應過量的前驅體以使敏感的結構表面飽和。在一些具體例中，可減小一或多種前驅體的脈衝時間，使得未達到完全飽和且低於一單層吸附於基板表面上。在「饋送」之後，排空反應空間(「排空1」)，其中無前驅體被饋送至反應空間，同時將惰性 氣體及反應物氣體連續地饋送至反應空間，但不施加RF功率，藉此自基板之表面移除非化學吸附的前驅體及多餘氣體。在「RF」之後，排空反應空間(「排空2」)，其中將惰性氣體及反應物氣體連續地饋送至反應空間，但不饋送前驅體且不施加RF功率至反應空間，藉此自基板之表面移除副產物及多餘氣體。歸因於反應物氣體之連續流動，且亦歸因於惰性氣體之連續流動進入反應空間中作為前驅體經間歇地或於脈衝中注入其中之恆定流，可有效率地進行排空以快速地自層之表面移除多餘氣體及副產物，藉此有效率地繼續多個PEALD循環，直至獲得期望厚度的層為止。
圖3顯示根據本發明之一具體例之一個循環中之熱ALD之示意性製程序列與一個循環中之PEALD之示意性製程序列的組合，其中灰色格子表示「開」狀態，而白色格子表示「關」狀態，且每一欄之寬度不表示各製程之持續時間。在此於一個循環中之熱ALD及PEALD之連續組合製程序列中，熱ALD包括「饋送1」、「排空1」、「反應」、及「排空2」，其分別實質上對應於圖2中說明的「饋送」、「排空1」、「反應」、及「排空2」。在將上述循環重複m次之後(m為1至3000，較佳1至500之整數)，起始PEALD，其包含分別實質上對應於圖4中說明之「饋送」、「排空1」、「RF」及「排空2」的「饋送2」、「排空3」、「RF」及「排空4」。上述循環可重複n次(n為1至1000，較佳1至150之整數)。n/m之比可在0.1至3，較佳0.2至1之範圍內。
在熱ALD中，反應物的反應性通常低，因此，除非使用具高反應性之反應物(諸如烷氧化物矽烷)，否則與PEALD相比，沉積速率通常低。當使用具低反應性之反應物時，藉由添加諸如吡啶之觸媒，可顯著地改良反應性，其中(例如)暴露於單層表面上之SiO-H鍵藉由觸媒減弱，藉此提高反應物種及經吸附前驅體之經暴露位點的反應性。圖5顯示在根據本發明之另一具體例之一個循環中之熱ALD的示意性製程序列，其中灰色格子表示「開」狀態，而白色格子表示「關」狀態，且各欄之寬度不代表 各製程的持續時間。在圖5中所說明之序列中，在一脈衝(「饋送1」)中，使用連續地供應之載氣及稀釋氣體(共同稱為「惰性氣體」)來供應前驅體。此可使用如以上關於圖2之製程序列所述的流通系統(FPS)來完成。
在圖5中，前驅體係藉助於載氣(「惰性氣體」)來提供。由於ALD係自限制吸附反應製程，因此所沉積的前驅體分子之數目係藉由反應性表面位點之數目確定，且與飽和後的前驅體暴露無關，且前驅體之供應係使得反應性表面位點在每個循環飽和。在一脈衝(「饋送2」)中將用於提高反應物及前驅體之反應性的觸媒供應至反應室，其在整個沉積循環中連續地流動，同時反應物及惰性氣體係連續地饋送至反應室，但未饋送前驅體，藉此形成一單層。由於反應物之反應性低，因此反應物可於整個循環中連續地流動，及藉由於一脈衝中供應觸媒，可活化沉積反應。尚不知曉針對熱ALD的連續反應物流動，且可最小化或實質上地抑制壓力波動，並提高可控制性。
如以上關於圖2之序列所提及，於各階段中供應過量的前驅體以使敏感的結構表面飽和。在一些具體例中，可減小一或多種前驅體的脈衝時間，使得未達到完全飽和且低於一單層吸附於基板表面上。在「饋送1」之後，排空反應室(「排空1」)，其中無前驅體被饋送至反應室，同時將惰性氣體及反應物氣體連續地饋送至反應空間，但不供應觸媒，藉此自基板之表面移除非化學吸附的前驅體及多餘氣體。在「饋送2」之後，排空反應室(「排空2」)，其中將惰性氣體及反應物氣體連續地饋送至反應空間，但不饋送前驅體且不供應觸媒至反應室，藉此自基板之表面移除副產物及多餘氣體。歸因於反應物氣體之連續流動，且亦歸因於惰性氣體之連續流動進入反應空間中作為前驅體及觸媒經各別間歇地或於脈衝中注入其中之恆定流，可有效率地進行排空以快速地自層之表面移除多餘氣體及副產物，藉此有效率地繼續多個熱ALD循環，直至獲得期望厚度的層為止。
圖6顯示根據本發明之另一具體例之一個循環中之熱ALD 的示意性製程序列與一個循環中之PEALD之示意性製程序列的組合，其中灰色格子表示「開」狀態，而白色格子表示「關」狀態，且每一欄之寬度不表示各製程之持續時間。在此於一個循環中之熱ALD及PEALD之連續組合製程序列中，熱ALD包括「饋送1」、「排空1」、「饋送2」、及「排空2」，其分別實質上對應於圖5中說明的彼等。在將上述循環重複m次之後(m為1至3000，較佳1至1000之整數)，起始PEALD，其包含分別實質上對應於圖4中說明之「饋送」、「排空1」、「RF」及「排空2」的「饋送3」、「排空3」、「RF」、及「排空4」。上述循環可重複n次(n為1至1000，較佳1至150之整數)。n/m之比可在0.1至3，較佳0.2至2之範圍內。在此序列中，可最小化或實質上地抑制壓力波動，並提高可控制性。
製程循環可使用(例如)包括圖1A中所說明之設備的任何合適設備執行。圖1A係可用於本發明之一些具體例中之理想地結合經程式設計以進行下文所述序列之控制來熱ALD及電漿增強型ALD(PEALD)沉積氧化物膜之ALD(原子層沉積)設備之示意性表示圖。在此圖中，藉由在反應室3之內部11(反應區)中設置彼此平行且面對的一對導電(電容耦合)之平板電極4、2，施加HRF功率(13.56MHz或27MHz)25至一側，及將另一側12電接地，在該等電極之間激發電漿。一溫度調節器係設置於下部載台2(下部電極)中，且置放於其上之基板1之溫度在給定溫度下保持恆定。上部電極4亦充當噴灑板，且前驅體氣體及反應物氣體(及稀有氣體)係分別經由氣體管線21及氣體管線22及經由PEALD之噴灑板4引入至反應室3中。另外，在反應室3中，設置了具有排氣管線7之圓管13，經由該排氣管線，反應室3之內部11中之氣體被排出。另外，安置於反應室3下之轉移室5具備密封氣體管線24以經由轉移室5之內部16(轉移區)將密封氣體引入至反應室3之內部11，其中設置有用於將反應區與轉移區隔開之分隔板14(自此圖省略閘閥，晶圓係經由該閘閥轉移至轉移室5中或自該轉移室轉移)。該轉移室亦具備排氣管線6。在一些具體例中，多元素膜沉積及表面處理係 在同一反應空間中執行，使得所有步驟可連續地進行，而不會將基板暴露於空氣或其他含氧氛圍。
在一些具體例中，針對藉由熱ALD之第一氧化物膜，使用與用於藉由PEALD之第二氧化物膜者不同的前驅體及反應物，儘管第一氧化物膜及第二氧化物膜構成(單一膜類型的)單一連續氧化物膜。在熱ALD中，前驅體及反應物傾向於在其接觸時相互反應，且因此，在一些具體例中，使用不同於用來供應PEALD之反應物的埠將反應物供應至反應室。在圖1A中說明之設備中，可藉由通過位在設置於反應室3內部之噴灑頭4上游之氣體管線27將反應物引入至歧管管道23，及/或藉由通過設置於噴灑頭4中之氣體埠18於噴灑頭4處引入反應物，及/或藉由通過設置於反應室3之側壁中的氣體埠17(密閉穿透過圓管13)於噴灑頭4與其上放置基鈑1的基座2之間引入反應物，來將用於熱ALD之反應物供應至反應室。針對熱ALD，當使用不同前驅體時，通過氣體管線26將前驅體供應至歧管管道23。在一些具體例中，可使用遠端電漿單元，藉由將經激發氣體供應至歧管導管23來激發氣體。
在一些具體例中，在圖1A中所描繪之設備中，可使用圖1B中所說明(較早所描述)的切換不活潑氣體之流動與前驅體氣體之流動的系統來在脈衝中引入前驅體氣體，而不使反應室之壓力實質上地波動。
在一些具體例中，可使用雙腔室反應器(用於處理彼此緊密地安置之晶圓的兩個區段或隔室)，其中反應物氣體及稀有氣體可經由共用管線來供應，而前驅體氣體係經由非共用管線來供應。
熟悉技術者應瞭解，該設備包括一或多個控制器(未圖示)，其經程式設計或另外組構以使如本文中別處所描述之沉積及反應器清潔製程進行。如熟悉技術者應瞭解，控制器係與反應器之各種電源、加熱系統、泵、機器人及氣流控制器或閥通信。
圖7為可用於本發明之另一具體例中的用於熱ALD及電漿 增強型ALD(PEALD)沉積介電質膜之ALD設備之示意性表示圖。在此設備中，氣體管線31、32、33、及34對應於圖1A中說明之設備的氣體管線21、22、26、及27；RF源51對應於圖1A中之RF源25；歧管管道41對應於圖1A中之歧管管道23；噴灑頭44對應於圖1A中之噴灑頭4；反應室52對應於圖1A中之反應室3；排氣管線45對應於圖1A中之排氣管線6；及基座43對應於圖1A中之基座2。圖1A中所指示之任何結構可設置於圖7中所說明之設備中。閘閥42係用於遠端電漿單元之閘閥。在此設備中，可將觸媒供應至反應室52。由於觸媒可與前驅體反應，因此在一些具體例中，未在噴灑頭44之上游將觸媒與前驅體混合，而將其直接供應至反應室52。例如，藉由與如圖1A中說明之具有用於前驅體之孔洞之氣體通道分開地提供如圖7中所說明之於噴灑頭44中具有其他孔洞37之另一氣體通道，可通過氣體管線35將觸媒供應至於噴灑頭44中具有孔洞37的氣體通道，以致可將觸媒不與前驅體接觸地饋送至反應室直至觸媒進入反應室52之內部中為止(雖然圖7顯示通道具有僅靠近噴灑頭之外圍分佈的孔洞37，但孔洞37可均勻地分佈遍及噴灑頭之整個表面)。替代地或另外地，可通過設置於反應室52之側壁中的氣體埠36將觸媒饋送至反應室52。
在一些具體例中，可如圖3中所說明在下表1中顯示的條件下連續地進行熱ALD循環及PEALD循環。
Figure 107103230-A0202-12-0015-1
Figure 107103230-A0202-12-0016-2
Figure 107103230-A0202-12-0017-4
上文所指示的用於300-mm晶圓之RF功率可經轉換至W/cm2(每晶圓單位面積之瓦數)，其可適用於具有不同直徑(諸如200mm或450mm)之晶圓。
通常，第一氧化物膜之厚度係在約1nm至約7nm之範圍內，而第二氧化物膜之厚度係在約5nm至約30nm之範圍內，其中第二氧化物膜之厚度係大於第一氧化物膜之厚度(期望的膜厚度可根據應用及膜用途等適當地選擇)。經組合的氧化物膜可藉由沉積於碳膜(例如，非晶形碳)上而用於雙重圖案化或可藉由沉積於模板(例如，矽基板)上而用作中間層介電膜。
在一些具體例中，可如圖6中所說明在下表2中顯示的條件下連續地進行熱ALD循環及PEALD循環。
Figure 107103230-A0202-12-0017-5
Figure 107103230-A0202-12-0018-6
第一氧化物膜及第二氧化物膜可具有下表3中顯示的性質。
Figure 107103230-A0202-12-0018-7
以上，第一氧化物膜之WER低於第二氧化物膜之WER，且第一氧化物膜之膜密度亦低於第二氧化物膜之膜密度。
參考以下工作實施例來進一步說明本發明。然而，該等實施例不欲限制本發明。在實施例中未規定條件及/或結構之處，熟悉本技藝者可鑒於本揭示內容根據常規實驗容易地提供此等條件及/或結構。此外，特定實施例中所應用之數字可經修改至少±50%之範圍，且在一些具體例中，該等數字為近似值。
實施例
實施例1至5
使用圖3或4中說明之序列藉由熱ALD及PEALD之組合 製程將氧化矽膜形成於非晶形碳膜(厚度為100nm)上，該非晶形碳膜係形成於具有縱橫比為1之寬溝槽(開口寬度為100nm)及縱橫比為3.5之窄溝槽(開口寬度為30nm)的矽基板(直徑為300mm且厚度為0.7mm)上，其之一個循環係使用圖1A中說明之ALD設備及圖1B中說明之氣體供應系統(FPS)利用表5中指示的特定條件及序列在下表4(製程循環)中顯示的一般條件下進行。通過圖1A中說明的歧管管道將第一反應物饋送至反應室。
Figure 107103230-A0202-12-0019-8
Figure 107103230-A0202-12-0020-9
Figure 107103230-A0202-12-0020-10
在表5中，具有「*」之實施例編號表示比較例。評估每一所獲得之膜。表6展示評估之結果。
Figure 107103230-A0202-12-0020-11
Figure 107103230-A0202-12-0021-12
在表6中，「碳膜收縮率」表示於沉積氧化物膜後減少之碳膜厚度相對於沉積氧化物膜前之碳膜厚度之比率的百分比；「側壁覆蓋率」表示於窄溝槽之側壁處之氧化物膜厚度相對於基板頂表面處之氧化物膜厚度之比率的百分比；「圖案負載率」表示於窄溝槽之側壁處之氧化物膜厚度相對於寬溝槽之側壁處之氧化物膜厚度之比率的百分比；「熱ALD GPC」表示每個循環的生長速率。
如表6中所示，當完全藉由PEALD來沉積氧化矽膜時，下方碳膜會受損並顯示顯著的膜收縮率(實施例1)，而當先藉由熱ALD沉積氧化矽膜作為保護層，然後再藉由PEALD連續沉積作為本體層時，下方碳膜的損傷大大地減小並顯示顯著較低的膜收縮率(實施例2-5)。此外，作為保護層，使用TICS藉由熱ALD的氧化矽膜(實施例3及5)看來較佳於使用BDEAS者(實施例2及4)。另外，藉由PEALD製程沉積之氧化矽膜的等形性(實施例1)與藉由熱ALD及PEALD之組合製程沉積之氧化矽膜的等形性(實施例2-5)並無顯著不同(其皆顯示高於90%之等形性)。
實施例6至11
以與實施例1至5中描述者實質上類似的方式將氧化矽膜形成於矽基板上，僅除了氧化物膜係利用表7中指示的特定條件及序列直接沉積於不具有碳膜的矽基板上。
Figure 107103230-A0202-12-0021-13
Figure 107103230-A0202-12-0022-14
在表7中，具有「*」之實施例編號表示比較例。評估每一所獲得之膜。表8展示評估之結果。
Figure 107103230-A0202-12-0022-15
表8中，「經氧化Si基板之厚度」表示基於在沉積氧化物膜後之觀察之經氧化矽基板的厚度。
如表8中所示，當完全藉由PEALD來沉積氧化矽膜時，下方矽層會受損並被氧化(實施例6)，而當先藉由熱ALD沉積氧化矽膜作為保護層，然後再藉由PEALD連續沉積作為本體層時，下方矽層的損傷大大地減小並被氧化(實施例7-11)。此外，作為保護層，使用TICS藉由熱ALD的氧化矽膜(實施例9)看來較使用OMCTS者(實施例10及11)佳，此外，厚度為5nm之氧化矽膜(實施例9)較厚度為2nm者(實施例8)佳。使用OMCTS藉由熱ALD沉積之氧化矽膜(實施例10及11)顯示較使用TICS藉由熱ALD 沉積之氧化矽膜(實施例9)顯著更高的GPC(乃因烷氧化物矽烷具有高反應性)。另外，藉由PEALD製程沉積之氧化矽膜的等形性(實施例6)與藉由熱ALD及PEALD之組合製程沉積之氧化矽膜的等形性(實施例7-11)並無顯著不同(其皆顯示高於90%)。
實施例12至17
以與實施例1至5實質上類似的方式，將氧化矽膜形成於非晶形碳膜上，僅除了1st反應物係連續地饋送，及觸媒係使用圖2、4、5、或6中說明之序列添加，其之一個循環係利用表10中指示的特定條件及序列在下表9(製程循環)中顯示的一般條件下進行。觸媒係經由圖7中說明之不同氣體通道通過噴灑頭饋送至反應室。
Figure 107103230-A0202-12-0023-16
Figure 107103230-A0202-12-0024-17
Figure 107103230-A0202-12-0024-18
在表10中，具有「*」之實施例編號表示比較例。評估每一所獲得之膜。表11展示評估之結果。
Figure 107103230-A0202-12-0024-19
Figure 107103230-A0202-12-0025-20
在表11中，術語係對應於表6中所使用者。在「熱ALD GPC」中，括號中之數字顯示藉由PEALD之GPC。
如表11中所示，當完全藉由PEALD來沉積氧化矽膜時，下方碳膜會受損並顯示顯著的膜收縮率(實施例12)，而當先藉由熱ALD沉積氧化矽膜作為保護層，然後再藉由PEALD連續沉積作為本體層時(實施例15-17)，及當完全藉由熱ALD來沉積氧化矽膜時(實施例13及14)，下方碳膜的損傷大大地減小並顯示顯著較低的膜收縮率。此外，出人意料地，即使當藉由PEALD沉積第二氧化矽膜時，在沉積第二氧化矽膜之前藉由利用熱ALD以1nm至3nm之厚度沉積第一氧化矽膜作為保護膜(實施例15-17)，可完全避免電漿對下方膜所產生的不利效應(實施例15-17中之碳膜收縮率與僅實施熱ALD之實施例13-14相比為實質上相等或更低)。以上結果亦可於實施例4(表6)中與實施例13(未使用觸媒)相比而觀察到。此外，當於一脈衝中添加觸媒同時於熱ALD中連續地饋送反應物時，與當未添加觸媒且於一脈衝中饋送反應物時獲得的GPC相比(實施例13)，GPC經顯著地提高(實施例14至17)。此外，當藉由熱ALD沉積之第一氧化矽膜的厚度為3nm時，與厚度1nm的第一氧化矽膜(實施例16)相比，實質上未偵測得膜收縮率(實施例15)。另外，完全藉由PEALD製程沉積之氧化矽膜的等形性(實施例12)、完全藉由熱ALD製程沉積之氧化矽膜的等形性(實施例13及14)、及藉由熱ALD及PEALD之組合製程沉積之氧化矽膜的等形性(實 施例15-17)，並無顯著不同(其等皆顯示高於90%之等形性)。
實施例18至21
以與實施例12至17中描述者實質上類似的方式將氧化矽膜形成於矽基板上，僅除了氧化物膜係利用表12中指示的特定條件及序列直接沉積於不具有碳膜的矽基板上。
Figure 107103230-A0202-12-0026-21
在表12中，具有「*」之實施例編號表示比較例。評估每一所獲得之膜。表13展示評估之結果。
Figure 107103230-A0202-12-0026-22
在表13中，術語係對應於表8中所使用者。在「熱ALD GPC」中，括號中之數字顯示藉由PEALD之GPC。
如表13中所示，當完全藉由PEALD來沉積氧化矽膜時， 下方矽層會受損並被氧化(實施例18)，而當先藉由熱ALD沉積氧化矽膜作為保護層，然後再藉由PEALD連續沉積作為本體層時，下方層的損傷大大地減小並被氧化(實施例19-21)。此外，當於一脈衝中添加觸媒同時於熱ALD中連續地饋送反應物時，與當未添加觸媒且於一脈衝中饋送反應物時獲得的GPC相比(表8中之實施例7)，GPC經顯著地提高(實施例21)。此外，當藉由熱ALD沉積之第一氧化矽膜的厚度為3nm時，與厚度1nm的第一氧化矽膜(實施例20)相比，實質上未偵測得下方矽層的氧化(實施例19)。另外，完全藉由PEALD製程沉積之氧化矽膜的等形性(實施例18)、及藉由熱ALD及PEALD之組合製程沉積之氧化矽膜的等形性(實施例19-21)並無顯著不同(其皆顯示高於90%之等形性)。
鑒於前述，經證實藉由根據明確地、必要地、或內在地揭示於文中之具體例之熱ALD及PEALD之組合連續製程，可實質地沉積高品質氧化物膜，而不會因電漿導致損傷下方層。
熟悉技藝人士當明瞭可進行許多及各種修改而不脫離本發明之精神。因此，應清楚明瞭本發明之形式僅為說明性而非意欲限制本發明之範疇。
1‧‧‧基板
2‧‧‧導電平板電極；基座
3‧‧‧反應室
4‧‧‧導電平板電極；噴灑頭
5‧‧‧轉移室
6‧‧‧排氣管線
7‧‧‧排氣管線
21‧‧‧氣體管線
22‧‧‧氣體管線
23‧‧‧歧管管道
24‧‧‧密封氣體管線
25‧‧‧RF源
26‧‧‧氣體管線
27‧‧‧氣體管線
11‧‧‧反應室3之內部
12‧‧‧電接地之一側
13‧‧‧圓管
14‧‧‧分隔板
16‧‧‧轉移室5之內部(轉移區)
17‧‧‧氣體埠
18‧‧‧氣體埠

Claims (15)

  1. 一種藉由熱ALD及PEALD於基板上沉積氧化物膜之方法，包括：於反應室中提供基板；於該反應室中藉由熱ALD於該基板上沉積第一氧化物膜；及不中斷真空，於該反應室中藉由PEALD於該第一氧化物膜上連續沉積第二氧化物膜；其中該熱ALD之循環包括藉由將該反應物引入至設置於該反應室內部之噴灑頭上游之歧管管道，藉由於該噴灑頭處引入該反應物，及/或藉由於該噴灑頭與其上放置該基板之基座之間引入該反應物而將反應物饋送至該反應室。
  2. 如請求項1之方法，其中該熱ALD之循環包括將前驅體饋送至該反應室，該前驅體係選自由胺基矽烷、矽烷胺、異氰酸酯矽烷、羥乙磺酸酯矽烷、無機矽烷、含矽烷氫氧化物、及含矽烷烷氧化物所組成之群之至少一種化合物的氣體。
  3. 如請求項1之方法，其中該熱ALD之循環包括將反應物饋送至該反應室，該反應物係選自由H2O、醚、醇、H2及O2之混合物、及H2O2所組成之群之至少一種氣體。
  4. 如請求項1之方法，其中該PEALD之循環包括使用連續流至該反應室之載氣來於一脈衝中饋送前驅體，且將反應物連續饋送至該反應室。
  5. 如請求項4之方法，其中該反應物係選自由O2、CO2、及N2O組成之群的至少一種氣體。
  6. 如請求項1之方法，其進一步包括於藉由該熱ALD及該PEALD進行沉積之後清潔該反應室。
  7. 如請求項6之方法，其中該清潔係使用清潔氣體藉由在混合前驅體及反應物之位置的上游饋送該清潔氣體來實施。
  8. 如請求項7之方法，其中該清潔氣體係藉由在該反應室上游之遠端電漿單元來激發或使用含氟氣體原位激發。
  9. 如請求項1之方法，其中該熱ALD之循環包括在整個循環連續地將反應物饋送至該反應室，該反應物係選自由乙醇、H2O、及O3組成之群的至少一種氣體。
  10. 如請求項1之方法，其中該熱ALD之循環包括於一脈衝中將催化氣體饋送至該反應室，該催化氣體係除前驅體及反應物外之氣體並且能夠促進氧化物膜於循環中之沉積。
  11. 如請求項1之方法，其中該催化氣體係選自由吡啶、烷基金屬、吡啶基矽烷、矽烷胺、及矽氮烷組成之群之至少一種化合物的氣體。
  12. 如請求項1之方法，其中該第一氧化物膜具有1至7nm之厚度，及該第二氧化物膜具有5至30nm之厚度，其中該第二氧化物膜較厚於該第一氧化物膜。
  13. 如請求項1之方法，其中其上沉積該第一氧化物膜之該基板的表面係由非晶形碳所構成。
  14. 如請求項1之方法，其中其上沉積該第一氧化物膜之該基板的表面係由矽所構成。
  15. 如請求項1之方法，其中該基板具有圖案化凹部，且該第一及該第二氧化物膜係沉積於該等凹部上。
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