TWI654335B - 製造用於填充表面特徵的低ｋ膜的前驅物及流動ｃｖｄ方法 - Google Patents

製造用於填充表面特徵的低ｋ膜的前驅物及流動ｃｖｄ方法

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TWI654335B
TWI654335B TW106129394A TW106129394A TWI654335B TW I654335 B TWI654335 B TW I654335B TW 106129394 A TW106129394 A TW 106129394A TW 106129394 A TW106129394 A TW 106129394A TW I654335 B TWI654335 B TW I654335B
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branched
linear
plasma
silicon
situ
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TW106129394A
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TW201816178A (zh
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李建恒
雷蒙 尼克勞斯 孟提
羅伯特 戈登 瑞吉威
滿超 蕭
新建 雷
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美商慧盛材料美國責任有限公司
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Abstract

一種用以沈積含矽膜的方法，該方法包括：將一包含至少一種表面特徵的基材放進溫度在約-20℃至約400℃下之流動CVD反應器中；將至少一種具有至少一個醯氧基的含矽化合物引進該反應器中，讓該至少一種含矽化合物至少部分進行反應而形成一可流動的液體寡聚物，其中該可流動的液體寡聚物會在該基材上形成一氧化矽塗層及至少部分填充該至少一種表面特徵的至少一部分。一旦硬化，該氧化矽塗層具有低k及優良的機械性質。

Description

製造用於填充表面特徵的低K膜的前驅物及流動CVD方法
本申請案主張2016年8月30日提出之申請案案號62/381222的利益。該申請案案號62/381222之揭示內容以參考方式併入本文。
本發明係關於一種製造用於填充表面特徵的低k膜的前驅物及流動CVD方法。
本文描述出一種用以製造電子裝置的方法。更特別是，本文描述出一種用於沈積方法，諸如例如，流動化學氣相沈積法來形成含矽膜的組成物。可使用本文所描述的組成物及方法進行沈積之範例性含矽膜包括氧化矽、氮化矽、氧氮化矽、或摻雜碳的氧化矽、或摻雜碳的氮化矽膜。
流動氧化物沈積方法典型使用烷氧基矽烷化合物作為含矽膜的前驅物，且該方法係藉由經控制的水解及縮合反應進行沈積。此等膜可例如藉由將水與烷氧基矽烷之混合物，選擇性與 溶劑及/或諸如界面活性劑及多孔質(porogens)之其它添加劑施加到基材上而沈積到基材上。這些混合物的典型施加方法包括旋轉塗佈法、浸沾塗佈法、噴灑塗佈法、絹版印刷法、共縮合法及噴墨印刷法。在施加至基材後及在施加諸如例如熱、電漿及/或其它來源之一或多種能量來源後，於該混合物內的水可與烷氧基矽烷反應而水解該烷氧化物及/或芳基氧化物基團及產生一矽烷醇物種，其進一步與其它已水解的分子縮合及形成一寡聚性或網狀結構。
除了將該前驅物物理沈積或施加至基材外，已經描述出使用水與含矽蒸氣來源之氣相沈積方法用於流動介電質沈積(FCVD)，例如，在美國專利案號7,541,297、8,449,942、8,629,067、8,741,788、8,481,403、8,580,697、8,685,867、7,498,273、7,074,690、7,582,555、7,888,233及7,915,131，和美國公開案號2013/0230987 A1中，此等揭示以參考之方式併入本文。典型的方法普遍關於藉由在間隙中形成一流動液體膜，以固體介電質材料填充在基材上之間隙。該流動膜係藉由讓一可具有Si-C鍵的介電質前驅物與一氧化劑反應形成該介電質材料而形成。在某些具體實例中，該介電質前驅物會凝結及隨後與氧化劑反應而形成介電質材料。在某些具體實例中，該氣相反應物進行反應而形成凝結的流動膜。因為Si-C鍵對與水的反應呈相當惰性，所產生之網狀物可有益地由將對所產生的膜授予想要的化學及物理性質之有機官能基官能化。例如，將碳加入該網狀物可降低所產生的膜之介電常數。
另一種使用流動化學氣相沈積方法來沈積氧化矽膜之方法係氣相聚合。例如，先述技藝已聚焦在使用諸如三矽基胺 (TSA)之化合物來沈積含Si、H、N寡聚物，隨後使用臭氧曝露將其氧化成SiOx膜。此等方法之實施例包括美國公開案號2014/0073144、美國公開案號2013/230987、美國專利案號7,521,378、US 7,557,420及8,575,040及美國專利案號7,825,040，此等揭示以參考之方式併入本文。
考慮到使用三矽基胺(TSA)的方法，TSA典型以氣體傳遞進該反應艙中與氨混合，及在遠程電漿反應器中活化以產生NH2、NH、H及或N自由基或離子。TSA與經電漿活化的氨反應及開始寡聚化以形成較高分子量的TSA二聚物及三聚物或包括Si、N及H的其它物種。將該基材放置在反應器中，及於某一艙壓及TSA/經活化的氨混合物下冷卻至範圍約0至約50℃之一或多種溫度，該寡聚物開始以其可”流動”以填充該溝槽表面特徵之此方式凝結在晶圓表面上。以此方式將一包括Si、N及H的材料沈積到晶圓上及填充該溝槽。在某些具體實例中，進行預退火步驟以允許該膜更像SiN。想要具有SiN材料，因為下一個製程步驟係在範圍100-700℃之一或多種溫度下，使用臭氧或水進行氧化。因為SiN的鍵距及角度，已知當SiN氧化成SiO2時，會有單位晶胞體積增加而防止膜收縮。
雖然技藝的最近活動係關於流動化學氣相沈積及其它膜沈積方法，但問題仍然存在。這些問題之一係關於膜組成物。例如，使用氣相聚合方法從三矽基胺(TSA)前驅物所沈積的流動氧化物膜會產生具有高Si-H鍵密度之膜，其在稀HF溶液中之溼式蝕刻速率係比高品質熱氧化物快2.2至2.5倍。此膜不合適於低k膜應用。
在許多情況中，可對該流動膜施加一硬化製程，包括熱退火、UV硬化或離子/自由基緻密化。該硬化製程可從該已沈積的材料移除碳基團、羥基及較小分子量物種。現在參照圖1，此經常會在該硬化材料中留下空洞、裂痕或間隔。此膜亦不合適於低k膜應用。
因此，有需要提供另一種前驅物化合物，以便經由流動CVD技術製造出具有機械完整性(mechanical integrity)及多孔洞性之含矽膜，以便能成功地作用為含低k氧化矽的膜材料。
於本文中所描述的組成物或調配物及使用其之方法係藉由在至少一部分的基材表面上沈積一含矽膜克服先述技藝的問題，其中該含矽膜在沈積後處理後提供想要之膜性質。本發明可提供一種具有下列性質的含矽膜：i)機械完整性，就Young’s模數來說，其係約2至約15GPa，約4至約12及在某些情況中，約6至約10；ii)多孔洞性，其係約10至約30體積%，約12至約25及在某些情況中，約16至約22(例如，如藉由偏振光橢圓計(elipsometric)孔隙度測量法測量)；及iii)介電常數，其係約2.2至約3.0，約2.4至約2.8及在某些情況中，約2.5至約2.7。
在一個態樣中，於本文中所描述的發明提供一種用以沈積含矽膜的方法，該方法包括：將一包含至少一種表面特徵的基材放進溫度在約-20℃至約400℃下的反應器中；將至少一種具有至少一個醯氧基的含矽化合物引進該反應器中，其中該至少一種含矽化合物係選自於由下列所組成之群： I(a).具有式(RCOO)mR1 nSiHp的醯氧基矽烷，其中R係選自於氫、線性或分枝的C1至C6烷基；R1係選自於線性或分枝的C1至C6烷基、線性或分枝的C2至C6烯基、線性或分枝的C2至C6炔基；m=2或3；n=1或2；p=0或1；及m+n+p=4；I(b).具有式(RCOO)m(R2O)nSiHpR1 q的醯氧基烷氧基矽烷，其中R係選自於氫、線性或分枝的C1至C6烷基；R1係選自於線性或分枝的C1至C6烷基、線性或分枝的C2至C6烯基、線性或分枝的C2至C6炔基；R2係選自於線性或分枝的C1至C6烷基；m=2或3；m=1或2；p=0或1；q=0或1及m+n+p+q=4；及I(c).具有式(RCOO)m(R3R4NO)nSiHpR1 q的醯氧基胺氧基矽烷，其中R係選自於氫、線性或分枝的C1至C6烷基；R1係選自於線性或分枝的C1至C6烷基、線性或分枝的C2至C6烯基、線性或分枝的C2至C6炔基；及R3係選自於氫、線性或分枝的C1至C10烷基；R4係選自於線性或分枝的C1至C6烷基；m=2或3；n=1或2；p=0或1；q=0或1及m+n+p+q=4；及對該反應器提供一電漿以讓該至少一種含矽化合物至少部分反應而形成一可流動的液體寡聚物，其中該可流動的液體寡聚物會在該基材上形成一塗層及至少部分填充該至少一種表面特徵的至少一部分。
在另一個態樣中，本發明的方法進一步包括一讓該塗層於約100℃至約1000℃間之一或多種溫度下接受熱處理的步驟，以緻密化該塗層的至少一部分及形成一硬化層。
在又另一個態樣中，本發明的方法進一步包含一將該硬化層曝露至選自於由電漿、紅外光、化學處理、電子束或UV 光所組成之群的能量之步驟，以形成最後的含矽膜。
本發明的另一個態樣係關於一種包含至少一種具有至少一個醯氧基的含矽化合物之前驅物組成物，其中該至少一種含矽化合物係選自於由下列所組成之群：I(a).具有式(RCOO)mR1 nSiHp的醯氧基矽烷，其中R係選自於氫、線性或分枝的C1至C6烷基；R1係選自於線性或分枝的C1至C6烷基、線性或分枝的C2至C6烯基、線性或分枝的C2至C6炔基；m=2或3；n=1或2；p=0或1；及m+n+p=4；I(b).具有式(RCOO)m(R2O)nSiHpR1 q的醯氧基烷氧基矽烷，其中R係選自於氫、線性或分枝的C1至C6烷基；R1係選自於線性或分枝的C1至C6烷基、線性或分枝的C2至C6烯基、線性或分枝的C2至C6炔基；R2係選自於線性或分枝的C1至C6烷基；m=2或3；m=1或2；p=0或1；q=0或1及m+n+p+q=4；及I(c).具有式(RCOO)m(R3R4NO)nSiHpR1 q的醯氧基胺氧基矽烷，其中R係選自於氫、線性或分枝的C1至C6烷基；R1係選自於線性或分枝的C1至C6烷基、線性或分枝的C2至C6烯基、線性或分枝的C2至C6炔基；及R3係選自於氫、線性或分枝的C1至C10烷基；R4係選自於線性或分枝的C1至C6烷基；m=2或3；n=1或2；p=0或1；q=0或1及m+n+p+q=4。
本發明的另一個態樣係關於一種藉由本發明的方法及組成物獲得之膜。
將從下列較佳具體實例的更詳細說明與一起採用作為例示以闡明本發明之原理的伴隨圖形明瞭本發明的其它特徵及優點。
本發明的具體實例及特徵可單獨或彼此組合著使用。
於此之後，本發明將與所附加的圖形一起進行說明，其中類似的元件以類似的數字表示：圖1顯示出先述技藝在基材的溝槽中形成之氧化矽膜的SEM顯微圖，其中於硬化製程期間形成空洞；圖2顯示出根據本發明的方法，經由沈積二乙醯氧基二甲基矽烷與O2所形成之氧化矽膜的SEM顯微圖；圖3顯示出圖2之氧化矽膜在根據本發明的方法於300℃下熱退火5分鐘後之SEM顯微圖；及圖4顯示出圖3之氧化矽膜在根據本發明的方法於400℃下UV曝光10分鐘後之SEM顯微圖。
接著發生之詳細說明僅提供較佳的範例性具體實例及不意欲限制本發明之範圍、可行性或組態。而是，接著發生之較佳範例性具體實例的詳細說明將提供熟習該項技術者一能夠執行本發明的較佳範例性具體實例之說明。可在元素的功能及安排上製得不同變化而沒有離開本發明如在附加的申請專利範圍中所提出之精神及範圍。
在申請專利範圍中，可使用字母來鑑別所主張的方法步驟(例如，a、b及c)。這些字母係使用來輔助指出方法步驟 而不意欲指示出進行所主張的步驟之順序，除非此順序在申請專利範圍中有特別敘述及僅有至此程度。
於本文中所描述的組成物或調配物及使用其之方法係藉由在該基材表面的至少一部分上沈積一含矽膜克服先述技藝的問題，其中該含矽膜在沈積後處理後提供想要的膜性質。
本發明係針對一種半導體薄膜製程技術。本發明描述出一種用以改良介電膜品質且形態適應於多種裝置結構的方法及系統。更特別的是，本發明之具體實例提供一種形成具有增加的氧化矽膜密度之方法及系統，以對具有高縱深比率之溝槽達成無空洞的間隙填充。例如，除了別的應用以外，本發明係應用來形成用以填充窄的STI溝槽之高品質氧化矽膜。
此外，在一個態樣中，本開發提供一種用以沈積含矽膜的方法，該方法包括：將一包含至少一種表面特徵的基材放進溫度在約-20℃至約400℃下的反應器中；將至少一種具有至少一個醯氧基的含矽化合物引進該反應器中，其中該至少一種含矽化合物係選自於由下列所組成之群：I(a).具有式(RCOO)mR1 nSiHp的醯氧基矽烷，其中R係選自於氫、線性或分枝的C1至C6烷基；R1係選自於線性或分枝的C1至C6烷基、線性或分枝的C2至C6烯基、線性或分枝的C2至C6炔基；m=2或3；n=1或2；p=0或1；及m+n+p=4；I(b).具有式(RCOO)m(R2O)nSiHpR1 q的醯氧基烷氧基矽烷，其中R係選自於氫、線性或分枝的C1至C6烷基；R1係選自於線性或分枝的C1至C6烷基、線性或分枝的C2至C6烯基、線性或分枝的C2至C6炔基；R2係選自於線性或分枝的C1至C6烷基；m=2或3； m=1或2；p=0或1；q=0或1及m+n+p+q=4；及I(c).具有式(RCOO)m(R3R4NO)nSiHpR1 q的醯氧基胺氧基矽烷，其中R係選自於氫、線性或分枝的C1至C6烷基；R1係選自於線性或分枝的C1至C6烷基、線性或分枝的C2至C6烯基、線性或分枝的C2至C6炔基；及R3係選自於氫、線性或分枝的C1至C10烷基；R4係選自於線性或分枝的C1至C6烷基；m=2或3；n=1或2；p=0或1；q=0或1及m+n+p+q=4；及對該反應器提供一電漿以讓該至少一種含矽化合物至少部分反應而形成一可流動的液體寡聚物，其中該可流動的液體寡聚物會在該基材上形成一塗層及至少部分填充該至少一種表面特徵的至少一部分。
”可流動的液體寡聚物”意謂著在沈積條件下可流動之聚矽氧烷材料，其中該聚矽氧烷係經由FTIR測量。在硬化後，該可流動的液體寡聚物會形成一摻雜固體碳的多孔OSG。
該含矽膜係選自於由下列所組成之群：氮化矽、碳化矽、氧化矽、摻雜碳的氮化矽、氧氮化矽及摻雜碳的氧氮化矽膜。該組成物可係預混合的組成物、預混合物(在使用於該沈積製程前混合)或原地混合物(在沈積製程期間混合)。因此，在本揭示中，用語”混合物”、”調配物”及”組成物”可互換。
遍及本說明，如於本文中所使用的用語”氧化矽”指為包含矽及氧的膜，其係選自於由化學計量或非化學計量的氧化矽、摻雜碳的氧化矽、羧基氮化矽及於此其混合物所組成之群。
在本開發的方法中，典型來說，該第一步驟係將一包含至少一種表面特徵的基材放進溫度在約-20℃至約400℃下 之反應器中。合適的基材包括但不限於半導體材料，諸如砷化鎵(”GaAs”)、硼氮化(”BN”)矽及包括矽的組成物，諸如結晶矽、多晶矽、非晶矽、磊晶矽、二氧化矽(”SiO2”)、碳化矽(”SiC”)、氧碳化矽(”SiOC”)、氮化矽(”SiN”)、碳氮化矽(”SiCN”)、有機矽酸鹽玻璃(”OSG”)、有機氟矽酸鹽玻璃(”OFSG”)、氟矽酸鹽玻璃(”FSG”)及其它適當的基材或其混合物。該基材可進一步包含多種層，諸如例如，抗反射塗層、光阻、有機聚合物、多孔有機及無機材料；金屬，諸如銅及鋁；或擴散障敝層，例如，TiN、Ti(C)N、TaN、Ta(C)N、Ta、W、WN、TiSiN、TaSiN、SiCN、TiSiCN、TaSiCN或W(C)N，其中可對該些層施加該膜。本發明的有機矽酸鹽玻璃膜較佳為能充分黏附至前述材料之至少一種且能通過習知的拉力測試，諸如ASTM D3359-95a膠帶拉力測試。
在某些具體實例中，該基材可係單晶矽晶圓、碳化矽晶圓、氧化鋁(藍寶石)晶圓、薄片玻璃、金屬箔、有機聚合物膜或可係聚合物、玻璃、矽或金屬3維物件。該基材可塗佈以多種技藝熟知的材料，包括氧化矽、氮化矽、非晶相碳、氧碳化矽、氧氮化矽、碳化矽、砷化鎵、氮化鎵及其類似材料。這些塗層可完全被覆該基材、可係不同材料的多重層及可經部分蝕刻以曝露出下面的材料層。該表面亦可在其上面具有一已經進行圖案曝光且顯影而部分被覆該基材之光阻材料。
在某些具體實例中，該基材包含一表面特徵。如於本文中所使用，用語”表面特徵”意謂著該基材或經部分製造的基材包含下列孔洞、溝槽、淺溝隔絕層(STI)、通道、凹腔特徵或其類似特徵之一或多種。在一個特別的具體實例中，該表面特徵具有寬 度100微米或較少，寬度1微米或較少，或寬度0.5微米或較少，或寬度50奈米或較少。在此或其它具體實例中，若存在時，該表面特徵的縱深比率(深度對寬度比率)係0.1：1或較大，或1：1或較大，或10：1或較大，或20：1或較大，或40：1或較大。
該使用來形成於本文中所描述的膜或塗層之方法係流動化學沈積方法。合適於本文所揭示的方法之沈積方法的實施例包括但不限於熱化學氣相沈積(CVD)或電漿輔助循環(plasma enhanced cyclic)CVD(PECCVD)方法。範例性流動CVD反應器係揭示在美國公開案號2014/0073144中，其藉此以參考方式併入本文。如於本文中所使用，用語”流動化學氣相沈積方法”指為進行下列製程之任何方法：讓一基材曝露至一或多種揮發性前驅物，且在基材表面上讓其反應及/或分解以提供可流動的寡聚性含矽物種，然後在進一步處理後產生該固體膜或材料。雖然於本文中所使用的前驅物、試劑及來源有時可描述為”氣體”，要了解的是，該前驅物可係液體或固體，其係經由直接蒸發、吹氣泡或昇華且以或不以惰性氣體運輸進反應器中。在某些情況中，該已蒸發的前驅物可通過一電漿產生器。在一個具體實例中，該膜係使用電漿基底的(例如，遠距產生或原地)CVD方法沈積。如於本文中所使用，用語”反應器”包括但不限於反應艙或沈積艙。
在某些具體實例中，可將該基材曝露至一或多種預沈積處理，諸如但不限於電漿處理、熱處理、化學處理、紫外光曝光、電子束曝露及其組合以影響該膜的一或多種性質。這些預沈積處理可在選自於惰性、氧化及/或還原性環境下發生。
雖然於本文中所使用的化學試劑有時可描述為” 氣體”，要了解的是，該化學試劑可如為氣體直接傳遞；如為來自蒸發的液體之蒸氣、或使用諸如氮、氦或氬的載體氣體吹氣泡之液體、來自昇華的固體之蒸氣傳遞至反應器；及/或藉由惰性載體氣體運輸進反應器中。
本開發的方法包括一將具有至少一個醯氧基的含矽化合物(於本文中亦指為”前驅物”)引進該反應器中的步驟，其中該至少一種第二化合物係選自於由下列式I(a)至I(c)所組成之群：I(a).具有式(RCOO)mR1 nSiHp的醯氧基矽烷，其中R及R1各自獨立地選自於線性或分枝的C1至C6烷基；m=2或3；n=1或2；p=0或1；及m+n+p=4；I(b).具有式(RCOO)m(R1O)nSiHp的醯氧基烷氧基矽烷，其中R及R1各自獨立地選自於線性或分枝的C1至C6烷基；m=2或3；m=1或2；p=0或1；及m+n+p=4；及I(c).具有式(RCOO)m(R2R3NO)nSiHp的醯氧基胺氧基矽烷，其中R係選自於線性或分枝的C1至C6烷基；R2係選自於氫、分枝的C1至C10烷基及C4至C10芳基；及R3係選自於線性或分枝的C1至C10烷基；m=2或3；n=1或2；p=0或1；及m+n+p=4。
在上述及遍及本說明的式中，用語”線性烷基”指示為具有1至10、3至10、或1至6個碳原子之線性官能基。在上述及遍及本說明的式中，用語”分枝的烷基”指示為具有3至10、或1至6個碳原子的線性官能基。範例性線性烷基包括但不限於甲基、乙基、丙基、丁基、戊基及己基。範例性分枝烷基包括但不限於異丙基、異丁基、二級丁基、三級丁基、異戊基、三級戊基、異己基及新己基。在某些具體實例中，該烷基可具有一或多個官能基接附 於此，諸如但不限於烷氧基、二烷基胺基或其組合。在其它具體實例中，該烷基不具有一或多個官能基接附於此。該烷基可係飽和，或任擇地，不飽和。
在上述及遍及本說明的式中，用語”芳基”指示為具有3至10個碳原子、5至10個碳原子、或6至10個碳原子的芳香族環狀官能基。範例性芳基包括但不限於苯基、苄基、氯苄基、甲苯基及鄰-茬基。
在上述及遍及本說明的式中，用語”烯基”指示為具有一或多個碳碳雙鍵且具有2至12、2至10、或2至6個碳原子的基團。範例性烯基包括但不限於乙烯基或烯丙基。
用語”炔基”指示為具有一或多個碳碳三鍵且具有2至10或2至6個碳原子的基團。範例性烯基包括但不限於乙炔基。
在某些具體實例中，於式中之一或多個烷基或芳基可”經取代”或具有一或多個原子或原子基團取代置換例如氫原子。範例性取代基包括但不限於氧、硫、鹵素原子(例如，F、Cl、I或Br)、氮、烷基及磷。在其它具體實例中，於式中之一或多個烷基、烯基、炔基、芳香族及/或芳基可未經取代。
在某些具體實例中，於上述式中的取代基R1、R2及R3之任何一或多個當它們非為氫時，其可與在上述式中的C-C鍵連結而形成一環結構。如將由熟練人士了解，該取代基可選自於線性或分枝的C1至C10伸烷基部分；C2至C12伸烯基部分；C2至C12伸炔基部分；C4至C10環烷基部分；及C6至C10伸芳基部分。在這些具體實例中，該環結構可不飽和，諸如例如，環烷基環；或飽和，例如，芳基環。再者，在這些具體實例中，該環結構亦可經 取代或經取代。在其它具體實例中，取代基R1、R2及R3之任何一或多個未連結。
在該含矽前驅物包含具有式I(a)之化合物的具體實例中，該前驅物的實施例包括下列：
式I(a)之化合物的實施例包括二乙醯氧基二甲基矽烷、二乙醯氧基甲基矽烷、三乙醯氧基甲基矽烷、二乙醯氧基二乙烯基矽烷、二乙醯氧基甲基乙烯基矽烷、三乙醯氧基乙烯基矽烷、二乙醯氧基二乙炔基矽烷、二乙醯氧基甲基乙炔基矽烷及三乙醯氧基乙炔基矽烷。
在該含矽前驅物包含具有式I(b)之化合物的具體實例中，該前驅物的實施例包括下列：
該式I(b)的化合物之實施例包括二乙醯氧基甲氧基甲基矽烷、二乙醯氧基二甲氧基矽烷及三乙醯氧基甲氧基矽烷。
在該含矽前驅物包含具有式I(c)之化合物的具體實例中：
該式I(c)之化合物的實施例包括二乙醯氧基二甲基胺氧基甲基矽烷、二乙醯氧基二(甲基乙基)胺氧基甲基矽烷及二乙醯氧基二乙基胺氧基甲基矽烷。
可以多種方式將本文所描述的含矽前驅物化合物傳遞至反應艙，諸如CVD或ALD反應器。在一個具體實例中，可使用液體傳遞系統。在任擇的具體實例中，可使用結合的液體傳遞與急驟蒸發製程單元，諸如例如，由MSP Corporation of Shoreview，MN製造的渦輪蒸發器，以便讓低揮發性材料能夠定體積地傳遞，此導致可再現的運輸及沈積而沒有該前驅物的熱分解。在液體傳遞調配物中，於本文中所描述的前驅物可以純淨液體形式傳遞，或任擇地，可以包含其之溶劑調配物或組成物使用。因此，在某些具體實例中，該前驅物調配物可包括具有如可在所提供的末端使用應用中想要且優良之合適特徵的溶劑組分，以在基材上形成一膜。
該含矽前驅物化合物較佳為實質上無鹵化物離子，諸如氯化物；或金屬離子，諸如Al。如於本文中所使用，用語”實質上無”當其係關於鹵化物離子(或鹵化物)或金屬離子，諸如例如，氯化物、氟化物、溴化物、碘化物、Al3+離子、Fe2+、Fe3+、Ni2+、Cr3+時，其意謂著每種鹵化物或金屬離子少於5ppm(以重量計)，較佳為少於3ppm及更佳為少於1ppm，及最佳為0ppm。 氯化物或金屬離子已知作用為矽前驅物的分解觸媒。在最後產物中，明顯的氯化物程度可造成該矽前驅物降解。該矽前驅物逐漸降解可直接衝擊該膜沈積方法，使得半導體製造商難以滿足膜規格。此外，閑置壽命或穩定性將由該矽前驅物的較高降解速率而有負面衝擊，因此使得保證1-2年的閑置壽命有困難。再者，已知矽前驅物會在分解後形成易燃及/或可自燃的氣體，諸如氫及矽烷。包含本前驅物化合物的組成物實質上無此分解產物。因此，相關於形成這些易燃及/或可自燃的氣體副產物，該含矽前驅物之加速分解存在有安全性及性能關注。
可藉由下列方法達成實質上無鹵化物之根據本發明的含矽前驅物：(1)減少或消除在化學合成期間的氯化物來源，及/或(2)執行有效的純化方法以從粗產物移除氯化物，以便最後的純化產物實質上無氯化物。可藉由使用不包括鹵化物諸如氯二矽烷類、溴二矽烷類或碘二矽烷類的試劑來減少在合成期間之氯化物來源，因此避免產生包括鹵化物離子的副產物。此外，前述提及的試劑應該實質上無氯化物雜質，如此所產生的粗產物係實質上無氯化物雜質。以類似的方式，該合成應該不使用包括不能接受的高鹵化物污染物程度之鹵化物基底的溶劑、觸媒或溶劑。該粗產物亦可藉由多種純化方法進行處理以提供實質上無鹵化物諸如氯化物之最後產物。此等方法在先述技藝中有充分描述，及可包括但不限於純化方法，諸如蒸餾或吸附。通常利用沸點差異，使用蒸餾從想要的產物分離出雜質。亦可使用吸附，利用組分的不同吸附性質達成分離，如此最後產物實質上無鹵化物。可使用諸如例如可商業購得的MgO-Al2O3摻合物之吸附劑來移除鹵化物諸如氯化物。
對與包含溶劑與至少一種於本文中描述的含矽化合物之組成物相關的那些具體實例來說，所選擇的溶劑或其混合物不與該矽化合物反應。在該組成物中之溶劑量的範圍以重量計百分比係0.5重量%至99.5%或10重量%至75%。在此或其它具體實例中，該溶劑具有沸點(b.p.)類似於式I(a)、I(b)及I(c)之前驅物的b.p.，或在溶劑的b.p.與式I(a)、I(b)及I(c)之矽前驅物的b.p.間之差異係40℃或較少，30℃或較少，或20℃或較少，10℃或較少，或5℃或較少。任擇地，在沸點間之差異範圍係下列終點的任何一或多種：0、10、20、30或40℃。合適的b.p.差異範圍之實施例包括但不限於0℃至40℃，20℃至30℃，或10℃至30℃。在該組成物中，合適的溶劑之實施例包括但不限於醚(諸如1,4-二氧六圜、二丁基醚)、三級胺(諸如吡啶、1-甲基哌啶、1-乙基哌啶、N,N’-二甲基哌、N,N,N’,N’-四甲基乙二胺)、腈(諸如苯甲腈)、烷基烴(諸如辛烷、壬烷、十二烷、乙基環己烷)、芳香烴(諸如甲苯、脒)、三級胺基醚(諸如雙(2-二甲基胺基乙基)醚)或其混合物。
在一個特別的具體實例中，將該至少一種含矽化合物引進該反應器中，其係於範圍-20℃至1000℃，或約400℃至約1000℃，或約400℃至約600℃，或約-20℃至約400℃之一或多種溫度下進行該引進步驟。在這些或其它具體實例中，該基材包括一包含表面特徵的半導體基材。
本發明的方法包括一提供原地電漿或遠程電漿來源之步驟，以讓該至少一種含矽化合物至少部分進行反應而形成一可流動的液體寡聚物，其中該可流動的液體寡聚物會在該基材上形成一塗層及至少部分填充該至少一種表面特徵的至少一部分。將能 量施加至該至少一種含矽化合物、含氮來源(若使用時)、氧來源、其它前驅物或其組合以引發反應及在該基材上形成含矽膜或塗層。此能量可由下列提供但不限於：熱、電漿、脈衝電漿、螺旋電漿、高密度電漿、誘導耦合電漿、X射線、e束、光子、遠程電漿方法及其組合。在某些具體實例中，可使用二次RF頻率來源來修改在基材表面處的電漿特徵。在該沈積包括電漿的具體實例中，該電漿產生方法可包含直接電漿產生方法，其中該電漿係直接在該反應器中產生；或任擇地，遠距電漿產生方法，其中該電漿係在該反應器外部產生及供應進該反應器中。
該前驅物對含氧或氮來源的體積流動比率範圍可係約40：1至約0.2：1，約20：1至約1：1，及在某些情況中，約6：1至約2：1。在本發明的一個具體實例中，該組成物包含本發明的含矽前驅物與含氧或氮來源之至少一種。在本發明的另一個具體實例中，該組成物包含一從本發明的前驅物與含氧或氮來源之至少一種所獲得的寡聚物。
在一個特別的具體實例中，該電漿係選自於由下列所組成之群，但不限於：氮電漿、包含氮及氦的電漿、包含氮及氬的電漿、氨電漿、包含氨及氦的電漿、包含氨及氬的電漿、氦電漿、氬電漿、氫電漿、包含氫及氦的電漿、包含氫及氬的電漿、包含氨及氫的電漿、有機胺電漿、包含氧的電漿、包含氧及氫的電漿、及其混合物。
在另一個具體實例中，該電漿來源係選自於由碳來源電漿所組成之群，但不限於，包括：烴電漿、包含烴及氦的電漿、包含烴及氬的電漿、二氧化碳電漿、一氧化碳電漿、包含烴及 氫的電漿、包含烴及氮來源的電漿、包含烴及氧來源的電漿、及其混合物。
如先前提到，該方法在包含一表面特徵的基材之至少一部分表面上沈積一膜。將該基材放進該反應器中及將該基材維持在範圍約-20℃至約400℃的一或多種溫度下。在一個特別的具體實例中，該基材之溫度係低於艙壁。將該基材溫度保持在溫度低於100℃，較佳溫度為低於25℃及最佳為低於10℃及高於-20℃。
在某些具體實例中，該反應器係在壓力低於大氣壓或750托耳(105巴斯卡(Pa))或較低下，或100托耳(13332巴斯卡)或較低。在其它具體實例中，將該反應器的壓力範圍維持在約0.1托耳(13巴斯卡)至約10托耳(1333巴斯卡)下。
於電漿能量存在下，該含矽化合物彼此反應及形成寡聚物，其在基材表面上凝結如為液體(液體寡聚物)及至少部分填充在該基材的特徵中。但是，直接使用如所沈積的膜可產生一太多孔且不具有適當的機械強度之介電質。因此，本開發的某些具體實例係應用來對如所沈積的氧化矽層進行進一步處理以改良膜品質且具有增加的密度及仍然達成無空洞的間隙填充。”無空洞”意謂著藉由觀看該經沈積及硬化的膜之SEM或TEM所獲得之視覺決定。
在較佳具體實例中，於範圍約100℃至約1000℃之一或多種溫度下熱退火該可流動的液體寡聚物以緻密化該材料的至少一部分，接著在溫度範圍100℃至1000℃下進行寬帶UV處理。
為了防止空洞化形成，需要在處理期間進行交聯。例如，當加熱二乙醯氧基二甲基矽烷時，會損失醋酸酐分子及形成Si-O-Si鍵。損失醋酸酐分子導致奈米尺度孔洞產生。因為在 每個矽原子上有二個乙醯氧基，該交聯形成將導致長鏈。為了產生3D交聯，需要具有三個乙醯氧基官能基的前驅物。在其它具體實例中，較佳為加入氧化劑(O2或CO2)來產生3D交聯。對氧化矽或摻雜碳的氧化矽來說，膜密度之範圍典型為1.5至2.0克/立方公分；及對氮化矽或摻雜碳的氮化矽來說，1.8至2.8克/立方公分。因此，此等膜係合適於使用作為低k材料應用。對摻雜碳的氧化矽來說，所達成的介電常數k之範圍典型為2.5至2.8，或2.5至3.0。
在某些具體實例中，可將所產生的含矽膜或塗層曝露至沈積後處理以影響該膜的一或多種性質，諸如但不限於電漿處理，其包括但不限於氫電漿、氦電漿、氬電漿、氨電漿、水(H2O)電漿、氧電漿、臭氧(O3)電漿、NO電漿、N2O電漿、一氧化碳(CO)電漿、二氧化碳(CO2)電漿及其組合；化學處理、紫外光曝光、紅外線曝光、電子束曝露及/或其它處理。
在某些具體實例中，將該熱處理後材料曝露至電漿、紅外光、化學處理、電子束或UV光以形成一緻密膜。
上述步驟定義出於本文中所描述的方法之一個循環；及可重覆該循環直到獲得想要的含矽膜厚度。在此或其它具體實例中，要了解的是，可以多種順序、可相繼地或同時地(例如，在另一個步驟的至少一部分期間)及其任何組合進行於本文中所描述的方法之步驟。可藉由變化該化合物及其它試劑的各別步驟之供應時間週期來進行供應，以改變所產生的含矽膜之組成物化學計量。
在本發明的一個具體實例中，可於本發明的含矽膜上形成或沈積下列膜或特徵之至少一種：i)接受平坦化，ii)銅(例如，填充通道)，及iii)介電質膜。在一個態樣中，本發明包括一包 含具有至少一種特徵(例如，通道或溝槽)之圖形化結構的基材，在其上面沈積本發明的膜(例如，摻雜碳的氧化矽)及在本發明的膜上沈積一包含阻障層之膜(例如，鈷、碳氮化矽、氮化矽、氧氮化碳、TiN及TaN之至少一種)。
為了進一步闡明本發明的目的提供下列實施例，但是決不意欲限制本發明。
實施例
將流動化學氣相沈積(FCVD)膜沈積到中電阻率(8-12歐姆公分)單晶矽晶圓基材及Si圖案晶圓上。在某些實施例中，可將所產生的含矽膜或塗層曝露至預沈積處理以影響該膜之一或多種性質，諸如但不限於電漿處理、熱處理、化學處理、紫外光曝光、紅外線曝光、電子束曝露及/或其它處理。
可在Applied Materials Precision 5000系統上之經修改的FCVD艙中，使用矽烷或TEOS製程成套工具進行沈積。該艙具有直接液體注入(DLI)傳遞能力。該前驅物係液體，其傳遞溫度係與該前驅物的沸點相依。
為了沈積初始可流動之摻雜碳的氧化物膜，典型的液體前驅物流速係100-5000毫克/分鐘，氧(或任擇地二氧化碳)流速係20-40sccm，原地電漿功率密度係0.25-3.5瓦/平方公分，壓力係0.75-12托耳。為了緻密化如所沈積的流動膜，在真空中，使用經修改的PECVD艙，於100~1000℃，較佳為300~400℃下熱退火及/或UV硬化該膜。藉由SCI反射儀或Woollam偏振光橢圓計測量厚度及在632奈米處的折射率(RI)。典型的膜厚度範圍係 10至2000奈米。藉由Nicolet穿透式傅立葉(Fourier)轉換紅外線光譜(FTIR)工具測量及分析該以矽為基底的膜之鍵結性質及氫含量(Si-H、C-H及N-H)。使用X射線反射性(XRR)完成全部的密度測量。進行X射線光電子光譜(XPS)及二次離子質譜儀(SIMS)分析以決定該膜的元素組成物。藉由截面掃描式電子顯微鏡(SEM)，使用Hitachi S-4800系統，在2.0奈米解析度下觀察於圖形化晶圓上的流動能力及間隙填充效應。藉由偏振光橢圓計(ellipsometric)孔隙度測量法來測量該膜的多孔洞性。
使用實驗設計(DOE)方法進行流動CVD沈積。該實驗設計包括：前驅物流係100至5000毫克/分鐘，較佳為500至2000毫克/分鐘；氧(或CO2)流係0sccm至1000sccm，較佳為0至100sccm；壓力係0.75至12托耳，較佳為6至10托耳；RF功率(13.56MHz)係50至1000瓦，較佳為100~500瓦；低頻率(LF)功率係0至100瓦；及沈積溫度範圍係-20至400℃，較佳為-20℃至40℃。使用DOE實驗來決定何種製程參數將產生具有好的流動能力之最理想的膜。
以二乙醯氧基二甲基矽烷作為前驅物沈積低k膜
在此實驗中，使用如下之製程條件來沈積具有最適宜的膜性質之可流動的多孔低k膜：功率=200瓦，間隔=200密耳，壓力=6~10托耳，溫度=30~35℃，二乙醯氧基二甲基矽烷=1500~2000毫克/分鐘，He=200sccm，O2=40~60sccm。在300℃下熱退火該流動膜5分鐘，接著為400℃的UV硬化10分鐘。
在毯覆基材上獲得具有RI係1.37及k係2.6~2.7 的膜。該膜的多孔洞性係19~20%。在8托耳的加工壓力下，該膜之模數係10.4GPa；硬度係1.84GPa。該模數及硬度係與習知的PECVD多孔低k膜一致。
現在參照圖2，圖2顯示出截面SEM，其指示出藉由沈積二乙醯氧基二甲基矽烷與O2達成好的間隙填充。現在參照圖3，圖3顯示出圖2的膜之截面SEM，其係在300℃下熱退火5分鐘及在400℃下UV硬化10分鐘(圖4)。現在參照圖4，圖4顯示出圖3的氧化矽膜在400℃下UV曝光10分鐘後之SEM顯微圖。
雖然本發明之原理已於上述與較佳具體實例連結進行說明，要清楚了解的是，此說明僅製得實施例及不作為本發明的範圍之限制。

Claims (14)

  1. 一種用以沈積含矽膜的方法，該方法包含下列步驟：將一包含至少一種表面特徵的基材放進溫度在約-20℃至約400℃下的反應器中；將至少一種具有至少一個醯氧基的含矽化合物引進該反應器中，其中該至少一種含矽化合物係選自於由下列所組成之群：I(b). 具有式(RCOO)m(R2O)nSiR1 q的醯氧基烷氧基矽烷，其中R係選自於氫、線性或分枝的C1至C6烷基；R1係選自於線性或分枝的C1至C6烷基、線性或分枝的C2至C6烯基、線性或分枝的C2至C6炔基；R2係選自於線性或分枝的C1至C6烷基；m=2,n=1，及q=1；或m=3,n=1，及q=0；及I(c). 具有式(RCOO)m(R3R4NO)nSiHpR1 q的醯氧基胺氧基矽烷，其中R係選自於氫、線性或分枝的C1至C6烷基；R1係選自於線性或分枝的C1至C6烷基、線性或分枝的C2至C6烯基、線性或分枝的C2至C6炔基；及R3係選自於氫、線性或分枝的C1至C10烷基；R4係選自於線性或分枝的C1至C6烷基；m=2或3；n=1或2；p=0或1；q=0或1及m+n+p+q=4；及對該反應器提供一電漿來源以讓該至少一種含矽化合物至少部分進行反應而形成一可流動的液體寡聚物，其中該可流動的液體寡聚物會在該基材上形成一塗層及至少部分填充該至少一種表面特徵的至少一部分。
  2. 如請求項1之方法，其中該電漿係選自於由下列所組成之群：包含氮之原地或遠程電漿來源基底的電漿、包含氮及氦之原地或遠程電漿來源基底的電漿、包含氮及氬之原地或遠程電漿來源基底的電漿、包含氨之原地或遠程電漿來源基底的電漿、包含氨及氦之原地或遠程電漿來源基底的電漿、包含氨及氬之原地或遠程電漿來源基底的電漿、氦電漿、氬電漿、氫電漿、包含氫及氦之原地或遠程電漿來源基底的電漿、包含氫及氬之原地或遠程電漿來源基底的電漿、包含氨及氫之原地或遠程電漿來源基底的電漿、原地或遠程電漿來源基底的有機胺電漿、包含氧之原地或遠程電漿來源基底的電漿、包含氧及氫之原地或遠程電漿來源基底的電漿、及其混合物。
  3. 如請求項1之方法，其中該電漿係選自於由下列所組成之群：包含碳或烴之原地或遠程電漿來源基底的電漿、包含烴及氦之原地或遠程電漿來源基底的電漿、包含烴及氬之原地或遠程電漿來源基底的電漿、包含二氧化碳之原地或遠程電漿來源基底的電漿、包含一氧化碳之原地或遠程電漿來源基底的電漿、包含烴及氫之原地或遠程電漿來源基底的電漿、包含烴及氮之原地或遠程電漿來源基底的電漿、包含烴及氧之原地或遠程電漿來源基底的電漿、及其混合物。
  4. 如請求項1之方法，更包含一在約100℃至約1000℃間之一或多種溫度下讓該塗層接受熱處理的步驟，以緻密化該塗層的至少一部分及形成硬化層。
  5. 如請求項4之方法，更包含一讓該硬化層曝露至選自於由電漿、紅外光、化學處理、電子束或UV光所組成之群的能量之步驟，以形成該最後的含矽膜。
  6. 如請求項5之方法，其中上述步驟定義出該方法的一個循環及可重覆該循環直到獲得想要的厚度之含矽膜。
  7. 如請求項1之方法，其中該具有式I(b)的醯氧基烷氧基矽烷係選自於由下列所組成之群：其中R係選自於由下列所組成之群：甲基、乙基、正丙基、異丙基、三級丁基、正丁基、二級丁基及異丁基；R1係選自於由下列所組成之群：甲基、乙基、乙烯基、烯丙基及乙炔基；及R2係選自於由下列所組成之群：甲基、乙基、正丙基、異丙基、三級丁基、正丁基、二級丁基及異丁基。
  8. 如請求項1之方法，其中該醯氧基胺氧基矽烷具有式I(c)：其中R及R1各自獨立地選自於由下列所組成之群：甲基、乙基、正丙基、異丙基、三級丁基、正丁基、二級丁基及異丁基；R1係選自於由甲基、乙基、乙烯基、烯丙基及乙炔基所組成之群；及R3及R4各自獨立地選自於由甲基及乙基所組成之群。
  9. 如請求項1之方法，其中該含矽膜具有介電常數<3.0，如藉由電容-電壓測量決定；多孔洞性>10%，如藉由偏振光橢圓計孔隙度測量法測量。
  10. 一種包含至少一種含矽化合物的含矽膜前驅物，其係選自於由下列所組成之群：I(b). 具有式(RCOO)m(R2O)nSiR1 q的醯氧基烷氧基矽烷，其中R係選自於氫、線性或分枝的C1至C6烷基；R1係選自於線性或分枝的C1至C6烷基、線性或分枝的C2至C6烯基、線性或分枝的C2至C6炔基；R2係選自於線性或分枝的C1至C6烷基；m=2,n=1，及q=1；或m=3,n=1，及q=0；及I(c). 具有式(RCOO)m(R3R4NO)nSiHpR1 q的醯氧基胺氧基矽烷，其中R係選自於氫、線性或分枝的C1至C6烷基；R1係選自於線性或分枝的C1至C6烷基、線性或分枝的C2至C6烯基、線性或分枝的C2至C6炔基；及R3係選自於氫、線性或分枝的C1至C10烷基；R4係選自於線性或分枝的C1至C6烷基；m=2或3；n=1或2；p=0或1；q=0或1及m+n+p+q=4；其中該含矽化合物與電漿反應以形成該含矽膜。
  11. 如請求項10之前驅物，更包含至少一種溶劑。
  12. 如請求項10之前驅物，更包括含氧來源及含氮來源之至少一種。
  13. 如請求項10之前驅物，更包含該至少一種含矽化合物的至少一種寡聚物。
  14. 一種含矽膜，其係藉由如請求項1之方法在具有至少一種表面特徵的基材上獲得，其具有介電常數<3.0，如藉由電容-電壓測量決定；多孔洞性>10體積%，如藉由偏振光橢圓計孔隙度測量法測量。
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