TWI506158B - 由二矽烷前驅物進行之遠端電漿化學氣相沈積的高品質氧化矽膜 - Google Patents

由二矽烷前驅物進行之遠端電漿化學氣相沈積的高品質氧化矽膜 Download PDF

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TWI506158B
TWI506158B TW097140531A TW97140531A TWI506158B TW I506158 B TWI506158 B TW I506158B TW 097140531 A TW097140531 A TW 097140531A TW 97140531 A TW97140531 A TW 97140531A TW I506158 B TWI506158 B TW I506158B
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nitrogen
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ruthenium
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Abhijit Basu Mallick
Srinivas D Nemani
Ellie Yieh
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Applied Materials Inc
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Description

由二矽烷前驅物進行之遠端電漿化學氣相沈積的高品質氧化矽膜
本發明大體上涉及用於製造半導體裝置的氧化矽膜形成方法，尤其涉及利用乙矽烷前驅物之遠端電漿CVD的高品質氧化矽膜。
諸如淺溝槽隔離結構(STI)等間隙和溝槽通常被用來電性隔離半導體裝置上的元件。STI可包括形成在半導體基板隔離區域中填有介電材料的溝槽或間隙，用以防止鄰近的裝置結構(例如電晶體、二極體等)的電耦合。隨著積體電路上的裝置密度持續增加，在裝置結構之間的尺寸和距離也逐漸減小。但是，STI溝槽的垂直高度的減小通常不會與水平寬度一樣快，這導致間隙和溝槽具有較大的高寬比，即較高的深寬比(aspect ratio)。
雖然使裝置結構具有增加的深寬比的能力允許在半導體晶片基板的相同表面積上設置更多的結構(例如電晶體、電容、二極體等)，但也產生了製造問題。其中一個問題是在填充製程期間，難以完全填充這些結構中的間隙和溝槽卻不產生孔洞或縫隙(seam)。必須用介電材料(例如氧化矽)填充間隙和溝槽，以將鄰近的裝置結構相互電性隔離，而使電雜訊和漏電流降至最小。隨著深寬比的增加，更加難以填充該些深且狹窄的溝槽又不會在填充溝槽的介電材料中產生孔洞或縫隙。
介電層中的孔洞和縫隙在半導體裝置製造期間和已完成的裝置中都會引起問題。孔洞和縫隙在介電材料中隨機形成且具有不可預知的尺寸、形狀、位置和密度。這會導致不可預知且不一致的膜層沈積後處理，例如不均勻的蝕刻、研磨、退火等。完成的裝置中的孔洞和縫隙也會使裝置結構中之間隙和溝槽的介電品質產生變化。其他問題中，這會導致由於電性互相干擾、電荷泄漏以及在某情況下裝置中發生短路而產生不穩定或低劣的裝置性能。
已經開發出可在高深寬比結構上沈積介電材料期間使形成的孔洞和縫隙減至最少的技術。這些技術包括減慢介電材料的沈積速度，以使介電材料可與溝槽的側壁和底部更加共形。更加共形的沈積能夠降低溝槽頂部上的材料堆積以及介電材料過早封住溝槽頂部而形成孔洞的機會(此問題有時被稱作「麵包塊現象(breadloafing)」)。但不幸的是，減慢沈積速度也意味著增加沈積時間，這降低了處理效率以及產率。
控制孔洞形成的另一種技術是增加所沈積介電材料的可流動性。具有更大可流動性的材料能夠更快速地填充孔洞或縫隙，並防止孔洞或縫隙變成填充容積內的永久缺陷。例如，通常採用高流動性的旋塗玻璃(SOG)前驅物(例如PSZ膜、SAM24、BTBAS等)以良好的共形性來填充溝槽。但是，利用此類習知SOG膜來增加氧化矽介電材料的可流動性通常會導致所沉積的膜層具有低膜密度，這是因為殘留有碳和矽烷醇基團所引起。增加膜密度的其中一種手段是將SOG膜固化成為氧化矽膜的時候使用高溫退火。但是，用來去除殘留碳和OH基團的高溫退火，也會引起相當大程度的膜體積收縮。在STI應用的狹窄溝槽中，所沈積之膜的收縮受到侷限且不穩定，從而產生具有多孔性結構或含孔洞結構的低密度膜。
因此，仍需要一種用於增加具有高深寬比之溝槽、間隙和其他裝置結構中之介電膜層密度的改良方法，以實現無孔洞的間隙填充。亦需要一種對於能夠以高速度和良好流動性來沈積介電材料又不會對完成間隙填充的品質造成不良影響的介電沈積製程。本發明主要著重於介電膜沈積的上述和其他態樣。
本發明涉及一種用於製造半導體裝置的氧化矽膜形成方法，實施例包括形成可流動介電膜的方法，包括進行化學氣相沈積(CVD)而由矽前驅物形成Si-N(H)-Si鍵，該矽前驅物具有一個或多個Si-Si鍵以與在遠端電漿中產生的自由基氮前驅物(例如-N、-NH、-NH2)反應。固化所沈積的膜，以將Si-N(H)-Si基團轉換成氧化矽(例如Si-O-Si)，並且在沈積後的退火過程(例如水蒸汽退火，steam anneal)中增加該膜的緻密度。該方法能用於形成STI(淺溝槽隔離)結構的高品質氧化矽膜，但將意識到，其具有更廣泛的應用。
實施例還包括在基板上沈積一含矽和氮之膜的方法。該方法包括將含矽前驅物引入一含有基板的沈積室。含矽前驅物可包括至少兩個矽原子。該方法還可包括使用位於沈積室外部的遠端電漿系統產生至少一個自由基氮前驅物。此外，該方法可包括將該自由基氮前驅物引入該沈積室中，在該沉積室中，該自由基氮和該含矽前驅物反應並且在基板上沈積該含矽和氮的膜。
實施例可能還包括在基板上形成氧化矽膜的方法。該方法包括在沈積室中提供基板，以及利用耦合至該沈積室的遠端電漿系統來產生活化(activated)的氮物種，例如氮氫自由基(hydronitrene radicals)。此外，該方法包括將含矽前驅物引入沈積室中。該含矽前驅物包含至少一個Si-Si鍵。該方法更包括將活化的氮物種引入該沈積室中，在該沉積室中，活化的氮物種與含矽前驅物反應並且在基板上沈積第一膜。該第一層膜包含多個Si-N(H)-Si鍵。而且，該方法包括在蒸汽氛圍中退火該第一膜，以及在基板上形成第二膜。該第二層膜包含多個Si-O-Si鍵。
在以下的描述出列出部分的其他實施例和特徵，且本領域技術人員藉由閱讀本案說明書以及通過實踐本發明而可明白以及學習到該些額外的實施例和特徵。可借助於說明書中描述的手段、組合和方法來實現和獲得本發明的特徵和優點。
本發明涉及一種用於製造半導體裝置的氧化矽膜形成方法。實施例包括形成可流動介電膜的化學氣相沈積方法，該介電膜包括由具有一個或多個Si-Si鍵的矽前驅物與在遠端電漿中形成的自由基氮前驅物(例如，-N、-NH、-NH2)反應而得的Si-N(H)-Si鍵。該方法還包括利用沈積後退火(例如蒸汽退火)來固化該流動性的介電膜，以將Si-N(H)-Si鍵轉換成更加緻密的Si-O-Si鍵。在其他應用中，該方法可用來形成高品質的氧化矽間隙填充(例如，形成STI結構)。
第1圖示意性示出了根據本發明實施例將矽前驅物中的Si-Si鍵轉換成Si-N(H)-Si鍵之後，在進一步轉換成Si-O-Si鍵的化學反應過程。該圖僅僅是一範例，這不應過度地限制本案請求項的範圍。本領域技術人員將可領會到其他變化、改進和替換態樣。如圖所示，該化學反應是CVD(化學氣相沈積)製程，期間具有至少一個Si-Si鍵的含矽前驅物與由遠端電漿(也就是，與流動性Si-N(H)-Si膜之沈積製程分開形成的電漿)解離產生的自由基氮混合。該CVD製程使該矽前驅物(或多個前驅物)中的Si-Si鍵轉換成Si-N(H)-Si鍵。在隨後的退火步驟中，將Si-N(H)-Si鍵轉換成Si-O-Si鍵，其中可在例如水蒸汽(即是H2 O蒸汽)環境中執行該退火。由於氧原子的原子體積比氮原子更大，因此在退火期間形成氧化矽會導致介電膜膨脹。
上述CVD製程包括將至少兩種反應物單獨引入沈積室中，並且使它們在預定條件下反應。在一實施例中，第一反應物可以是選自於由烷氧基乙矽烷、烷氧基烷基乙矽烷、烷氧基乙醯氧基乙矽烷和聚矽烷所構成之群組中的一種前驅物。例如，烷氧基乙矽烷包括Si2 (EtO)6 的乙氧基乙矽烷類、Si2 (MeO)6 的甲氧基乙矽烷類，以及Si6 (MeO)12 的甲氧基環己矽烷類，這裏Et表示乙基(C2 H6 )，以及Me表示甲基(CH3 )。在另一範例中，烷氧基烷基乙矽烷可能包括Si2 (EtO)4 (Me)2 的四乙氧基二甲基乙矽烷、Si2 (EtO)4 (Et)2 的四乙氧基二乙基乙矽烷、Si2 (EtO)2 (Me)4 的二乙氧基四甲基乙矽烷、Si2 (MeO)4 (Me)2 的四甲氧基二甲基乙矽烷、和Si4 O2 (Me)3 的甲基環己矽氧、Si6 (MeO)6 (Me)6 的甲氧基甲基環己矽烷、Si4 O2 (H2 )4 的氫化環己矽氧。在又一範例中，烷氧基乙醯氧基乙矽烷包括Si2 (AcO)6 的乙醯氧基乙矽烷、Si2 (Me)4 (AcO)2 的四甲基二乙醯氧基乙矽烷和Si2 (Me)2 (AcO)4 的二甲基四乙醯氧基乙矽烷，這裏，Ac表示乙醯基(acetyl group)。在又一範例中，聚矽烷可包括環戊矽烷或其他替代物。在不遇到任何CVD製程其他反應物的情況下，將任一種上述前驅物供應到沈積室中。
在另一實施例中，用於上述CVD製程的其他反應物是第二反應物，其包括由遠端氨電漿產生的自由基氮物種(radical nitrogen species)。例如，自由基氮物種可包括氮離子、氮氫自由基NHx (hydronitrene)，其中x=1或2。由於在這些乙矽烷或聚矽烷基前驅物的分子骨架中存在至少一個高反應性的Si-Si鍵，因此，CVD製程會產生含有多個Si-N(H)-Si鍵的產物，且還含有羥基(hydroxyl group)和碳系物種。例如，產物是沈積在基板上的碳氮化矽膜。由於存在這些羥基和碳系物種，因此CVD沈積的碳氮化矽膜是無定形的且可流動性的。
在又一實施例中，在水蒸汽環境中進行後續熱處理引起碳氮化矽膜和H2 O蒸汽之間的另一化學反應。該反應是氧化過程，會將碳氮化矽膜中的Si-N(H)-Si鍵轉換成Si-O-Si鍵，而形成氧化矽膜。一種副產物可能包括氨(NH3 )，可利用為該沉積室建立的排氣系統立即泵出該副產物。
第2圖示出根據本發明實施例在基板上形成氧化矽膜的方法簡化流程圖。如圖所示，該方法200利用第1圖中所描述的化學反應過程來形成氧化矽膜。示範性方法200包括非窮舉性(non-exhaustive)的一系列步驟，其可添加額外步驟(未示出)。本領域技術人員可領會到多種變化、修改和替換方式。在所示出的實施例中，方法200包括在沈積室中提供基板(步驟210)。該方法200還包括將分子骨架中具有至少一個Si-Si鍵的一種或多種含矽前驅物引入沈積室中(步驟220)。該方法還包括產生一種或多種自由基氮前驅物(步驟230)。例如，可在耦合到沈積室的遠端氨電漿系統中產生一種或多種自由基氮前驅物。
該方法200還包括將一種或多種自由基氮前驅物引入沈積室中以與該一種或多種含矽前驅物反應(步驟240)，而在基板上沈積具有Si-N(H)-Si鍵的可流動性介電膜。此外，方法200可包括蒸汽退火(steam annealing)以將CVD沈積的可流動性介電膜氧化成氧化矽膜(步驟250)。該蒸汽氧化製程(步驟250)可能包括由於將Si-N(H)-Si鍵轉換成Si-O-Si鍵所導致的膜膨脹，這會與從CVD沈積膜中去除一些羥基所導致的膜收縮相互抵消。結果，膜膨脹和收縮作用的平衡導致了產生緻密且無孔的氧化矽膜，也降低了在沈積和退火期間引入應力而導致膜破裂的可能性。
在一實施例中，用於CVD製程的一種或多種含矽前驅物在其分子骨架中包含多個羥基。羥基會保留在CVD沈積的膜中，而為該膜提供與習知SOG(旋塗玻璃)膜相似的流動特性。由於具有流動特性，依據於方法200所形成的CVD沈積膜在沈積過程中易於聚集在基板間隙或溝槽的底部中，因此減少在間隙填充或STI溝槽中心附近產生孔洞的機率。在另一實施例中，在分子骨架中具有至少一個Si-Si鍵的一種或多種含矽前驅物包括乙矽烷和/或聚矽烷前驅物。乙矽烷在其分子結構中具有單個的Si-Si單元，而聚矽烷具有多個Si-Si鍵。例如，可使用具有不同取代基的乙矽烷，包括烷氧基乙矽烷、烷氧基烷基乙矽烷和烷氧基乙醯氧基乙矽烷。在其他實例中，也可使用更高階同系物(higher homologue)的乙矽烷。當然，本領域技術人員可領會到對於乙矽烷和聚矽烷前驅物的選擇可有很多替換方式、變化和修改。
上述的CVD沈積製程與2006年5月30日申請、Ingle等人共同轉讓且名稱為「使用氧原子和含矽前驅物化學氣相沉積高品質之流動性二氧化矽(CHEMICAL VAPOR DEPOSITION OF HIGH QUALITY FLOW-LIKE SILICON DIOXIDE USING A SILICON CONTANTING PRECURSOR AND ATOMIC OXYGEN)」的美國專利申請案60/803,493號中描述的製程相似，在此引入其整體內容作為參考。但是，在方法200中，使用利用電漿解離氨而產生的自由基氮來代替原子氧，以與一種或多種含矽前驅物反應，從而產生因存在有羥基(例如矽醇基)而具有流動特性的含矽和氮之膜。
如上所述，可藉著在遠端電漿系統中引入氨(NH3 )來產生用於方法200中的反應物種(例如，-N、-NH、-NH2 )。遠端電漿系統可包括耦合到沈積室的一獨立腔室。用於將氨解離成NH/N/H自由基的電漿條件可包括：使用3kW至15kW範圍內的RF功率、在1Torr(托)至10托範圍內的腔室壓力下以及在室溫(room temperature)至約200℃範圍內的腔室溫度下產生電漿。在遠端電漿系統中解離氨而產生自由基氮前驅物，例如氮氫自由基(hydronitrene)，如NH或NH2 。也可產生原子氫(H)自由基。例如，在方法200的步驟230中產生氮氫自由基和氫自由基。隨後將自由基氮前驅物輸送到沈積室，並且該沉積室中已經單獨引入了一種或多種含矽前驅物。例如，可透過一噴頭來輸送該反應性氮前驅物，而通過多個帶槽的噴嘴來引入該矽前驅物。
第3圖示意性示出根據本發明實施例利用乙矽烷和/或聚矽烷前驅物與利用氨遠端電漿產生的自由基氮前驅物反應形成碳氮化矽(Si:C:N:H)膜的化學反應步驟。第3圖是一示意性實例，且不應過度限制本案請求項的範圍。本領域技術人員將可領會到其他變化、修改和替換態樣。
如圖所示，在過程310中利用氨電漿來產生氮氫(NH)自由基和氫(H)自由基。當氮氫(NH)自由基和氫(H)自由基在沈積室中遇到乙矽烷或聚矽烷前驅物時，乙矽烷或聚矽烷前驅物中高反應性的Si-Si鍵通常會斷裂，而形成矽-氫氧自由基與-NH2 重新鍵合，如第3圖的反應過程320所示。或者，乙矽烷或聚矽烷前驅物中的Si-Si鍵會斷裂以形成直接與-H重新鍵合的矽-氫氧自由基，如第3圖中的支系過程(side process)325所示的。當然，本領域技術人員將可領會到多種替換、變化和修改態樣。
在所示出的實例中，與-NH2 自由基鍵合的矽-羥基可藉著釋出醇基而解離成矽-氮氫自由基(silicon-hydronitrene radical)。例如，在原始含矽前驅物中的羥基會抓住鍵結在氮原子的H原子，以形成甲醇(CH3 OH)，如第3圖的過程330所示。利用真空泵輕易地去除所產生的甲醇能，而促進形成另外的甲醇。反應物的剩餘部分變成包含具有兩個懸鍵(dangling bond)之Si-NH鍵的自由基。隨後，兩個懸鍵快速地再次鍵合，而形成具有Si=NH雙鍵的二甲基矽亞胺自由基(dimethylsilanimine radical)，如第3圖的過程340所示。當然，本領域技術人員將領會到很多替換、變化和修改態樣。
在另一實施例中，化學反應進一步涉及在含矽前驅物中之Si-C鍵與二甲基矽亞胺自由基之間的反應。如第3圖的過程350中所示，該反應是一種鍵插入反應(bond insertion process)，其中二甲基矽亞胺自由基直接插入Si原子和C原子之間以產生碳氮化矽產物。當然，本領域技術人員將領會到很多替換、變化和修改態樣。
第4圖示出根據本發明實施例沈積可流動性含矽和氮之膜的方法簡化流程圖。該圖僅僅是實例，不應當過度限制本案請求項的範圍。本領域中具有通常知識者將領會到其他變化、修改和替換態樣。如圖所示，方法400是CVD製程，用於在基板上沈積具有流動特性的無定形碳氮化矽膜。方法400可包括在沈積室中提供基板(步驟410)。沈積室耦合到一遠端電漿系統。該方法400也可包括將氨引入該遠端電漿系統中，以在遠端電漿中使氨解離而產生自由基氮前驅物。所產生的自由基氮前驅物可包括氮氫(NH)自由基和氫(H)自由基。當然，還存在其他的替換、變化和修改態樣。
此外，方法400包括將氮氫(NH)自由基和氫(H)自由基輸送到沈積室中(步驟420)。在一實施例中，透過一噴頭來輸送氮氫(NH)自由基和氫(H)自由基，該噴頭以流體可流通的方式來耦合沈積室和遠端電漿系統。例如，反應性氮自由基(並且伴隨著載氣)可通過擋板或噴頭進入沈積室，該擋板或噴頭諸如在2007年5月29日申請、名稱為「用於介電間隙填充的製程腔室(PROCESS CHAMBER FOR DIELECTRIC GAPFILL)」且由Lubomirsky等人共同轉讓的美國專利申請案11/754,924號中所示出者，在此引入其全部內容作為參考。
方法400還包括將具有至少一個Si-Si鍵的一種或多種含矽前驅物引入沈積室中(步驟430)。在一實施例中，含矽前驅物被單獨引導到沈積室中。例如，這些前驅物是來自一個或多個分離的CVD氣體源，並且在被引入沈積室之前不會遇到任何的氨電漿。在另一實施例中，含矽前驅物包括在其分子骨架中具有單個Si-Si單元的乙矽烷和/或具有多個Si-Si單元的聚矽烷。例如，含矽前驅物是具有如第3圖所示之乙基羥基的乙矽烷。
方法400還包括執行CVD製程，以在沈積室中的基板上沈積可流動性碳氮化矽膜(步驟440)。當含矽前驅物在沈積室中遇到氮氫NH自由基和氫H自由基時，前驅物中的Si-Si鍵具有高反應性，使得具有Si-Si鍵的乙矽烷或聚矽烷前驅物斷裂成矽-氮氫自由基。而且，在甲醇解離和重新鍵結反應過程中，矽-氮氫自由基會轉變成二甲基矽亞胺自由基。二甲基矽亞胺自由基隨後藉著鍵插入反應而與前驅物中的Si-C鍵反應，形成碳氮化矽分子。
舉例而言，可在沈積室中於下列製程條件下進行CVD製程440：1)前驅物流速設定為1mgm/min至15gm/min；2)將沈積室保持在約1毫托至約600托範圍內的壓力下；3)腔室溫度控制在約0℃至約400℃之間。形成矽-氮氫自由基在第3圖的過程320中發生。涉及上述CVD製程440的其他化學反應過程可能包括第3圖所示的反應步驟330、340或350。所產生的碳氮化矽分子接著沈積在基板上以形成固體膜。該膜本質上是無定形的(amorphous)，並且因為在其分子骨架中具有羥基而具有可流動特性。
可流動性的沈積膜形成具有很低密度的無孔間隙填充，用於裝置的介電隔離。方法400還包括在氧化環境中退火該可流動性碳氮化矽膜，以形成緻密的氧化矽膜(步驟450)。與其他可流動性介電膜(例如習知的SOG膜)相似，高溫退火引起羥基和殘留的碳解離成水和/或甲醇蒸氣，其被立即泵出，並且導致明顯的膜收縮和緻密化。在特定實施例中，退火步驟450是在蒸汽(水蒸汽)氛圍內的氧化環境中進行的熱退火。例如，在約200℃至高達約1050℃的基板溫度下進行蒸汽退火。在退火期間的水蒸氣壓力約在1托至1大氣壓(atm，即約760托)的範圍內。
在替換實施例中，退火步驟450是將基板保持在室溫(room temperature)至高達約600℃下的臭氧處理。臭氧處理可進一步與UV光照射結合。在另一替換實施例中，退火步驟450是包括從室溫至約900℃的分子氧處理或從室溫至高達約600℃的原子氧處理的膜固化製程。當然，本領域技術人員將可領會到多種替換、變化和修改態樣。
在另一特定實施例中，由於在所沈積的碳氮化矽膜中存在著Si-N(H)-Si鍵，氧化步驟450將造成這些Si-N(H)-Si鍵轉換成Si-O-Si鍵。由於氧的原子體積比氮要大，因此此種轉換自然造成該膜膨脹。例如，鍵轉換過程與第1圖中描述的化學反應過程相同。該膜膨脹與由於未反應的碳和OH物種損失所導致的膜收縮相互抵消。平衡膜膨脹和收縮的淨效果導致產生較高品質的氧化矽膜，其具有較少整體收縮，但膜密度卻增加，同時保持無孔洞的間隙填充。
在另一實施例中，退火該可流動性碳氮化矽膜是在包括水蒸氣和酸性蒸汽的氛圍中進行。當CVD沈積膜包含具有烷氧基取代基乙矽烷時，在沈積期間，酸性環境有助於催化該些未反應之有機部分(organic moieties)的反應。第5圖示意性示出根據本發明實施例，酸性催化處理所沈積之介電膜的化學繪圖(chemical drawing)。該圖僅是示範範例，不應當過度限制本案請求項的範圍。本領域技術人員將領會到其他變化、修改和替換態樣。如圖所示，藉著在退火過程中添加酸性蒸汽，未反應的羥基會受到酸的親電子攻擊，也就是藉著從氧原子取出一個電子給氫原子，來自酸的H+ 離子會將未反應的CH3 O基團轉換成反應性的CH3 OH基團。其顯示於第5圖的過程510中。
此時水蒸氣與反應性的CH3 OH基團反應，如過程520所示。反應導致形成矽醇基(Si-OH)，並且從膜中釋出甲醇分子(CH3 OH)。所形成的矽醇Si-OH基團進行縮合(即，兩個矽醇(Si-OH)結合而釋放出水)導致在膜中形成氧化矽網狀結構(network)。在一實施例中，利用酸處理的退火有助於去除碳物種而增加膜密度，並且經由其他方式移除羥基而有助於降低孔洞形成的可能性。當然，存在其他替換、變化和修改態樣。
在其他實施例中，在包括水蒸氣和鹼性蒸汽(例如，氨(NH3 ))的氛圍中退火該可流動性碳氮化矽膜。對於CVD沈積膜包含具有烷氧基取代基的乙矽烷，鹼性環境有助於在沈積期間催化該些未反應之有機部分的反應。
第6A至6B圖示意性示出所沈積介電膜之鹼性催化處理的兩個化學反應機制。於第6A圖所示的第一個機制包括利用包含氨的鹼性蒸汽進行烷基的親核性攻擊。該機制中，矽烷氧基的烷基部分會轉移給氨，在轉移過程中亦釋放出質子(H+ )。由於烷基的轉移也包括水分子，因此其貢獻出一質子來取代該離開的烷基，並且形成矽醇(-Si-OH)基。在隨後的反應中，會發生矽醇縮合反應，而將固化的介電氧化膜中的-Si-OH基轉換成-Si-O-Si-基。
第6B圖示出的第二個反應機制包括利用含有氨的鹼性蒸汽進行矽烷氧中之矽原子的親核性攻擊。反應包括用氨分子來取代連接在矽上的烷氧基，而形成矽烷基胺(silyl amine)。烷氧基與水分子所貢獻的質子反應而形成醇類。在隨後的反應中，矽烷基胺可被水解以形成矽醇並且重新產生氨。接著，與第6A圖中描述的機制相似，矽醇基團進行縮合反應，而將固化的介電氧化膜中的-Si-OH基轉換成-Si-O-Si基。
應當理解，在第6A-6B圖中描述的鹼性催化反應原理僅是可能的反應機制中的兩個範例，且不應過度地限制本案請求項的範圍。本領域中具有通常知識人員將可領會到可用於如此沈積之矽烷氧物種的鹼性催化處理的其他變化、修改和替換態樣。
用於從可流動性有機矽膜中鹼性催化去除碳(諸如烷基和烷氧基)的示範性製程條件可包括在含有水和鹼性蒸汽的環境中進行膜層的沈積後固化處理。例如，如果鹼性蒸汽含有氨作為鹼性催化劑，則所沈積的膜可被加熱至約300℃同時被暴露到壓力為約1托至約40托的潮濕氨氣氛圍中達約2分鐘至約5分鐘。在另外的實施例中，氨氣氛圍也可包含氧氣(O2 )和/或利用氮前驅物(例如NH3 )進行遠端電漿離解所產生的原子氮(N)。
參考第7圖，示出根據本發明實施例的示範性處理系統700的截面圖。系統700包括沈積室701，在沈積室701中，前驅物進行化學反應並且在基板晶圓702上沈積可流動性的介電膜。晶圓702(例如200mm、300mm、400mm等直徑的半導體基板晶圓)可耦合到可旋轉的基板底座704上，該底座可垂直移動，以將基板702定位在更接近或更遠離上方的前驅物分配系統706。基座可以約1rpm至約2000rpm(例如約10rpm至約120rpm)的旋轉速度來旋轉基板晶圓。基座可以垂直移動基板一段距離，例如離該前驅物分配系統之該些側噴嘴708約0.5mm至約100mm的距離。
前驅物分配系統706包括多個徑向分佈的側噴嘴708，其每一個噴嘴都具有兩種不同長度的其中一種。在另外的實施例(未示出)中，可去掉該些側噴嘴，而留下環繞著沈積室壁而成環狀分佈的多個開口。前驅物通過這些開口流入腔室中。
分配系統706也可包括一圓錐形頂部擋板710，其與基板底座704的中心共軸。流體通道712可通過擋板710中心，以提供與向下流至該擋板之外側引導表面的前驅物成分不同的前驅物或載氣。
管道714圍繞著擋板710的外部表面，該管道714用來引導來自沈積室701上方之反應性物種產生系統(未示出)的反應性前驅物。導管714可以是直線圓形管，其一端開口在擋板710的外部表面上，並且其相反端耦合到該反應性物種產生系統。
反應性物種產生系統可以是遠端電漿產生系統(RPS)，其將較穩定的起始材料暴露於電漿中而產生反應性物種。例如，起始材料可以是包括分子氧(或臭氧)的混合物。將起始材料暴露於來自RPS的電漿會造成一部分的分子氧解離成原子氧，一種可在較低溫度下(例如低於100℃)與有機矽前驅物(例如TMOS、OMCTS)發生化學反應的高反應性自由基物種，以在基板表面上形成可流動的介電膜。由於在反應性物種產生系統中所產生的反應性物種通常即使在室溫下也可與其他沈積前驅物高度反應，因此在與其他沈積前驅物混合之前，該反應性物種在一隔離的氣體混合物向下游導管714中輸送，並在藉由擋板710將其分配到反應室701中。
系統700也可包括纏繞在沈積室701之圓頂716周圍的RF線圈(未示出)。這些線圈能在沈積室701中產生電感耦合電漿，進一步增強反應性物種前驅物和其他前驅物的反應性，從而在基板上沈積流體性介電膜。例如，利用RF線圈可將藉由擋板710而分配到該腔室中的含反應性原子氧之氣流，以及來自通道712和/或一個或多個側噴嘴708的有機矽前驅物氣流，引導至形成在基板702上方的電漿中。原子氧和有機矽前驅物甚至在低溫下也能在電漿中快速反應，而在基板表面上形成高流動性的介電膜。
利用底座704使基板表面本身也可旋轉，以增強所沈積膜的均勻性。旋轉平面與晶圓沈積表面平行，或者該兩個平面可能部分地不對準。當該些平面不對準時，基板702的旋轉可能產生搖擺，而在沈積表面上方的空間中產生流體擾動。在一些情況下，這種擾動也會促進沈積在基板表面上之介電膜的均勻性。底座704也可包括用來創造出真空夾盤的多個凹槽及/或其他結構，以當當底座移動時可將晶圓保持在底座上的適當位置處。典型的室內沈積壓力是介於約0.05托至約200托範圍內的腔室總壓力(例如1托)，這讓真空夾盤得以將晶圓保持在適當位置。
馬達718設置在沈積室701下方且可旋轉地耦合至支撐著底座704的軸720，而可利用馬達718來驅動底座旋轉。軸720也可包含多個內部通道(未示出)，用以將來自沈積室(未示出)下方之冷卻/加熱系統的冷卻流體和/或電線攜帶底座704。這些通道可從底座中心向週邊延伸，以為上方基板晶圓702提供均勻冷卻和/或加熱。該些通道也可設計成當軸720和基板底座704正在旋轉和/或傳送的時候進行操作。例如，在沈積可流動性氧化膜期間，可操作冷卻系統而在底座旋轉的時後保持基板晶圓702的溫度低於100℃。
系統700還包括設置在圓頂716上方的照射系統722。照射系統722的多個燈(未示出)可照射下方的基板702，以烘烤或退火基板上的沈積膜。在沈積期間，也可啟動該些燈，以促進膜前驅物或沈積膜中的反應。至少圓頂716的頂部部分是由能夠使一部分該些燈所發出的光線穿過的半透明材料製成。
當文中提供了數值範圍時，應當明白，除非文中另有清楚指示，否則，亦視為本文揭示了介於該範圍之上限和下限值之間且下至單位之十分之一的每一個數值。所述範圍內的任何所述值或其內數值與該範圍內的任一其他所述值或其內數值之間的每個較小範圍皆為本發明所涵蓋。這些較小範圍的上限值和下限值可各自包含在該範圍中或從該範圍中排除，並且依據所述範圍中是否有任何特別排除的限值，該些不含任一上下限值、包含其中一個限值、或是上下兩個限值都包含的每一個較小範圍也屬於本發明的涵蓋範圍內。當所述範圍包括其中一個或兩個限值，該些排除了其中一個限值或兩個限值的範圍也包括在本發明中。
如文中以及後附申請專利範圍中所使用的，除非文中另有清楚說明，否則單數形式的用語「一」、「一個」和「該」包括複數形式之意。因此，例如「一製程」可能包括多個這類製程，以及「該噴嘴」可能包括一種或多種噴嘴以及本領域技術人員知悉的等效物。
又，當說明書以及後附申請專利範圍中使用「包括」、「包括有」、「含有」、「具有」和「包含」等用語時，該些用語是意欲指出存在著所述特徵、整體、部件或步驟，但是不排除存在或添加一個或多個其他的特徵部件、整體、部件、步驟或基團。
200、400．．．方法
210、220、230、240、250．．．步驟
310．．．電漿誘導化學反應過程
320、325、330、340、350．．．過程
410、420、430、440、450．．．步驟
510、520、330、340．．．過程
700．．．處理系統
701．．．沈積室
702．．．基板晶圓
704．．．基板底座
706．．．前驅物分配系統
708．．．側噴嘴
710．．．擋板
712．．．流體通道
714．．．管道
716．．．圓頂
718．．．馬達
720．．．軸
722．．．照射系統
第1圖示意性示出根據本發明實施例，矽前驅物中的Si-Si鍵與反應性氮物種反應，以形成含Si-N(H)-Si的組化合物，並且之後將該化合物氧化成含Si-O-Si之化合物的化學反應過程；
第2圖是示出根據本發明實施例在基板上形成氧化矽膜之方法的簡化流程圖；
第3圖示意性示出根據本發明實施例，使用乙矽烷或聚矽烷前驅物以及在遠端電漿中解離氨所產生的自由基氮前驅物，來形成碳氮化矽Si:C:N:H的化學反應步驟；
第4圖是根據本發明實施例沈積可流動性且含矽和氮之膜層的方法簡化流程圖；
第5圖示意性示出根據本發明實施例，利用酸催化以去除所沈積之介電膜中之碳系物種的化學反應機制；
第6A-B圖示出根據本發明實施例，利用鹼催化來去除在所沈積之介電膜中之碳系物種的化學反應機制；以及
第7圖示出根據本發明實施例，用於在基板上形成氧化矽膜的示範性製程系統的截面圖。

Claims (38)

  1. 一種在一基板上沈積一含矽和氮之薄膜的方法，該方法包括：將含矽前驅物引入至含有該基板的一沈積室中，其中該含矽前驅物包括至少兩個矽原子；利用設置在該沈積室外部的一遠端電漿系統產生至少一種自由基氮前驅物；以及將該自由基氮前驅物引入該沈積室中，其中該自由基氮和該含矽前驅物反應，並且在該基板上沈積該含矽和氮的膜，其中該含矽和氮的膜在沈積過程期間為可流動的。
  2. 如申請專利範圍第1項所述的方法，其中該產生原子氮的步驟包括將氨暴露於該遠端電漿系統中的一電漿，其中至少一部分的氨解離成該自由基氮前驅物。
  3. 如申請專利範圍第1項所述的方法，其中該自由基氮前驅物具有化學式NHx ，其中x是0、1或2。
  4. 如申請專利範圍第1項所述的方法，其中該含矽前驅物包括乙矽烷前驅物或聚矽烷前驅物。
  5. 如申請專利範圍第1項所述的方法，其中該含矽前驅 物選自於由烷氧基乙矽烷、烷氧基烷基乙矽烷和聚矽烷構成的群組中。
  6. 如申請專利範圍第1項所述的方法，其中該含矽和氮的膜包括碳氮化矽膜。
  7. 如申請專利範圍第1項所述的方法，其中該含矽和氮的膜包括一含有Si-N(H)-Si鍵的膜。
  8. 如申請專利範圍第1項所述的方法，其中該方法更包括對該含矽和氮的膜進行退火，以形成氧化矽膜。
  9. 如申請專利範圍第8項所述的方法，其中在一包含蒸汽(steam)的環境中執行該退火。
  10. 如申請專利範圍第8項所述的方法，其中在一包含酸性蒸汽的環境中執行該退火。
  11. 如申請專利範圍第8項所述的方法，其中在約20℃至約900℃範圍內的一溫度下執行該退火。
  12. 如申請專利範圍第8項所述的方法，其中在一包含臭氧(O3 )的氛圍中執行該退火。
  13. 如申請專利範圍第12項所述的方法，其中該退火更包括在約20℃至約600℃範圍內的一溫度下，將該基板暴露於紫外光。
  14. 如申請專利範圍第8項所述的方法，其中在包含分子氧(O2 )的氛圍中執行該退火。
  15. 如申請專利範圍第8項所述的方法，其中在包含原子氧(O)的氛圍中且在約20℃至約600℃範圍內的一溫度下執行該退火。
  16. 如申請專利範圍第8項所述的方法，其中在約200℃到約1050℃範圍的一溫度下執行該退火。
  17. 一種在一基板上形成氧化矽膜的方法，該方法包括：在一沈積室中提供一基板；利用耦合到該沈積室的一遠端電漿系統產生多個氮氫自由基(hydronitrene radicals)；將含矽前驅物引入該沈積室，該含矽前驅物包括至少一個Si-Si鍵；將該多個氮氫自由基引入該沈積室，其中該些氮氫自由基和該含矽前驅物反應，並且在該基板上沈積一第一膜，該第一膜包含多個Si-N(H)-Si鍵且在沈積過程期間為可流動的； 在一蒸汽氛圍中對該第一膜進行退火；以及在該基板上形成一第二膜，該第二膜包含多個Si-O-Si鍵。
  18. 如申請專利範圍第17項所述的方法，其中該產生多個氮氫自由基的步驟包括將氨暴露到該遠端電漿系統中的一電漿，其中至少一部分的氨解離成該多個氫氮自由基。
  19. 如申請專利範圍第17所述的方法，其中該含矽前驅物包括乙矽烷前驅物或聚矽烷前驅物。
  20. 如申請專利範圍第17項所述的方法，其中該第一膜更包含具有可流動特性的羥基。
  21. 如申請專利範圍第17項所述的方法，其中對該第一膜進行退火的步驟是在約20℃至約900℃範圍內的一溫度下執行。
  22. 如申請專利範圍第17項所述的方法，其中該蒸汽氛圍包含水蒸汽和酸性蒸汽。
  23. 如申請專利範圍第22項所述的方法，其中該形成一第二膜的步驟包括使用水蒸汽將該第一膜中至少一部分 的該多個Si-N(H)-Si鍵轉換成多個Si-O-Si鍵的至少第一部分。
  24. 如申請專利範圍第22項所述的方法，其中該形成一第二膜的步驟更包括使用一酸性蒸汽，以催化未反應的羥基與水蒸氣反應，以形成反應性的OH基，產生該多個Si-O-Si鍵的至少第二部分。
  25. 如申請專利範圍第22項所述的方法，其中該酸性蒸汽包括氫氯酸或醋酸。
  26. 如申請專利範圍第17項所述的方法，其中該第二膜的密度比該第一膜要高。
  27. 一種固化一基板上之氧化矽膜的方法，該方法包括：提供一半導體處理室和一基板；形成氧化矽層以覆蓋至少一部分的該基板，該氧化矽層包含多個碳物種的副產物；將一鹼性蒸汽引入該半導體處理室中，該鹼性蒸汽與該氧化矽層反應，以從該氧化矽層中去除該些碳物種；以及從該半導體處理室中移除該鹼性蒸汽，其中該鹼性蒸汽包括水蒸氣、鹼蒸汽及分子氧(O2 )。
  28. 如申請專利範圍第27項所述的方法，其中該鹼性蒸汽包括氨。
  29. 如申請專利範圍第27項所述的方法，其中該矽層使用烷氧基矽烷製程沈積而得。
  30. 如申請專利範圍第27項所述的方法，其中該氧化矽層使用電漿CVD製程沈積而得。
  31. 如申請專利範圍第27項所述的方法，其中該引入一鹼性蒸汽的步驟更包括將氨氣流入該半導體處理室中。
  32. 如申請專利範圍第27項所述的方法，其中該鹼性蒸汽做為催化劑，以使該氧化矽層中的反應完全。
  33. 如申請專利範圍第27項所述的方法，其中該蒸汽是酸和水的混合物。
  34. 如申請專利範圍第27項所述的方法，其中該蒸汽更包括遠端產生的自由基原子氮。
  35. 如申請專利範圍第27項所述的方法，其中該鹼性蒸汽和該氧化矽層之間的該反應在約60℃至約600℃之間進行。
  36. 如申請專利範圍第26項所述的方法，其中該反應在約300℃執行。
  37. 如申請專利範圍第27項所述的方法，其中在與氧化矽層反應期間，該處理室具有約1托至760托的壓力。
  38. 如申請專利範圍第37項所述的方法，其中該處理室具有約40托的壓力。
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US7867923B2 (en) 2011-01-11
SG152183A1 (en) 2009-05-29
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US20090104755A1 (en) 2009-04-23

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