TW200927979A - High quality silicon oxide films by remote plasma CVD from disilane precursors - Google Patents

High quality silicon oxide films by remote plasma CVD from disilane precursors Download PDF

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TW200927979A
TW200927979A TW097140531A TW97140531A TW200927979A TW 200927979 A TW200927979 A TW 200927979A TW 097140531 A TW097140531 A TW 097140531A TW 97140531 A TW97140531 A TW 97140531A TW 200927979 A TW200927979 A TW 200927979A
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film
ruthenium
precursor
nitrogen
substrate
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Abhijit Basu Mallick
Srinivas D Nemani
Ellie Yieh
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Applied Materials Inc
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/56—After-treatment
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    • H01L21/02326—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment introduction of substances into an already existing insulating layer introduction of oxygen into a nitride layer, e.g. changing SiN to SiON

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200927979 六、發明說明： 【發明所屬之技術領域】 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。 【先前技術】 ❹ 諸如歲/冓槽隔離結構（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 2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 ^間的尺寸和距離也逐漸減小。但是，STI溝槽的垂直 4的減小it會與水平寬度—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如⑷。 雖然使裝置結構具有增加的深寬比的能力允許在半 :體晶片基板的相同表面積上設置更多的結構（例如電 體電各、二極體等），但也産生了製造問題。其中一 2題是在填充製程期間，難以完全填充這些結構中的 二和溝槽卻不產生孔洞或縫隙（seam)。必須用介電材 相1 I化石夕）填充間隙和溝槽，以將鄰近的裝置結構 電&隔離’而使電雜訊和漏電流降至最小。隨著深 、、曰加更加難以填充該些深且狹窄的溝槽又不會 200927979 在填充溝槽的介電材料中産生孔洞或縫隙β 介電層中的孔洞和縫隙在半導體裝置製造期間和已 元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β 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t比結構上沈積彳電材料期間 使形成的孔洞和缝隙減至最少的技術。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 ❿ 的機會（此問題有時被稱作「麵包塊現象 (breadloafing)」）。但不幸&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，並防止孔洞或缝隙變成填充容積内的永 久缺陷。例如，通常採用高流動性的旋塗玻璃（S〇G) 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 200927979 碎介電材料的可流動性通常會導致所沉積的媒層具有低 膜密度’廷是因為殘留有碳和石夕院醇基團所引起。增加 膜密度的其巾—種手段是將sqg膜m化成爲氧化梦膜的 時，使用高溫退火。但是，用來去除殘留碳和OH基團 的，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彳電材才斗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。 【發明内容】 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臈的方法，包括進 行化學氣相沈積（CVD)而由矽前驅物形成Si_N(H卜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_0-Si)，並且在沈積後的退火過程（例如 水蒸汽退火，steam armed)中增加該膜的緻密度。該方 6 200927979 法能用於形成STI (淺溝槽隔離）結構的高品質氧化珍 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;5夕和I之膜的方 法。該方法包括將含碎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I前驅 ❾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 積至的遠端電漿系統來産生活化（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_〇_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 月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#中描述的手段、組合和方法來實現和獲得本 7 200927979 發明的特徵和優點。 【實施方式】
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@化該流動性的 介電膜，謂Si-N(H)_Si鍵轉換成更加緻密的si-〇_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珍前驅物 中的Si-Si鍵轉換成Si_N(H)_Si鍵之後，在進—步轉換成 HSi鍵的化學反應過程。_僅僅是—制，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-個si_si 鍵的切前㈣與㈣端電漿（也就是，與流動性 SMHMi膜之沈積製程分開形成的電幻解離產生的 自由基氮混合。該CVD製程使該♦前驅物（或多個前驅 物）中的Si-Si鍵轉換成Si_N叫81鍵。在隨後的退火步 驟中，將Si-N(H)-Si鍵轉換成队⑽鍵，其中可在例 8 200927979 如水蒸汽（即是HsO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 積至中’並且使匕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、烷氧基乙酿氧基乙矽烷和聚矽烷所構成之群組 ❹ 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、SiAMeO)6的甲氧基乙矽烷類，以及 SWMeO)!2的甲氧基環己矽烷類，這裏价表示乙基 (C2H6 )，以及Me表示甲基（CH3 )。在另一範例中，烷 氧基烧基乙矽烷可能包括Si2(Et〇)4(Me)2的四乙氧基二 曱基乙矽烷、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石夕烧、 Si2(MeO)4(Me)2的四甲氧基二曱基乙矽烷、和Si4〇2(Me)8 ❹ 的甲基環己矽氧、Si6(Me〇)6(Me)6的甲氧基甲基環己矽 烷、SUOdH2)4的氫化環己矽氧。在又一範例中，烧氧基 乙酿氧基乙矽烷包括SidAcO)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 SiAMeMAcO)4的二甲基四乙醯氧基乙矽烷，這裏，Ae 表示乙醯基（acetyl group)。在又一範例中，聚碎烧可包 括環戊梦烧或其他替代物。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 9 200927979 是第二反應物’其包括由遠端氨電漿産生的自由基氮物 種（radical nitrogen species)。例如，自由基氮物種可包 括氮離子、氮1氫自由基NHX (hydronitrene)，其中χ=ι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 在至少一個尚反應性的Si-Si鍵，因此，CVD製程會產 生含有多個Si-N(H)-Si鍵的産物，且還含有羥基 (hydroxyl group)和碳系物種。例如，産物是沈積在基板 上的碳氮化矽膜。由於存在這些羥基和碳系物種，因此 Ο η 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H2〇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-0-Si鍵，而形成氧化矽膜。一種副産物可能包括氨 (NH3)，可利用爲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2〇〇利用第工 圖中所描述的化學反應過程來形成氧化矽膜。示範性方 法2〇〇包括非窮舉性（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 2〇〇包括在沈積室中提供基板（步驟21〇)。該方法別〇 還包括將分子骨架中具有至少-個Si-Si鍵的—種或多 種含矽前驅物引入沈積室中（步驟22〇)。該方法還包括 200927979 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産生一種或多種自 由基氮前驅物。
❹ 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碎前驅物反應（步驟 240 )，而在基板上沈積具有以_；^(11)_以鍵的可流動性介 電膜。此外’方法200可包括蒸汽退火（stearn 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25〇 )可能包括由於將 Si-N(H)-Si鍵轉換成Si-0-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，而爲該膜提供與習知s〇G (旋塗玻璃）膜 相似的流動特性❺由於具有流動特性，依據於方法2〇〇 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冑爪溝槽中 心附近産生孔洞的機率。在另—實施例中，在分子^架 中具有至少-個S⑷鍵的—種或多種切前驅物包括 乙石夕燒和/或聚㈣前驅物。乙㈣在其分子結構中具 有單個的Si-Si單元，而聚石夕烧具有多個s⑷鍵。例如， 11 200927979 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)的乙石夕 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曰申請、Ingle 等人共同轉讓且名稱爲「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 AT0MIC 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 内容作爲參考。但是，在方法200中，使用利用電漿解 離氨而産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，一N、一 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範圍内的RF功率、在1 Torr (托）至 10托範圍内的腔室壓力下以及在室溫（ro〇m temperature) 至約200°C範圍内的腔室溫度下産生電漿。在遠端電漿 系統中解離氨而産生自由基氮前驅物，例如氮氫自由基 12 200927979 (hydr〇nitrene)，如NH或NH2。也可産生原子氫（H)自 由基。例如，在方法2GG的步驟23G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人了—種或多種切前驅物。 例如，可透過一噴頭來輸送該反應性氮前驅物，而通過 • 多個帶槽的喷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/ ❹ 或聚矽烷前驅物與利用氨遠端電漿産生的自由基氮前驅 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中利用氨電漿來産生氮氫（NH) 自由基和氫（Η)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 ❹ 聚矽烷前驅物中高反應性的Si-Si鍵通常會斷裂，而形成 石夕一氫氧自由基與一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一Η重新鍵合的矽—氫氡自由 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，與一NH2自由基鍵合的矽—羥 基可藉著釋出醇基而解離成石夕一氮氫自由基 13 200927979 (silicon-hydronitrene radical)。例如，在原始含石夕前驅物 中的羥基會抓住鍵結在氮原子的Η原子，以形成甲醇 (CH3〇H)，如第3圖的過程33〇所示。利用真空泵輕易 地去除所產生的曱醇能，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雙鍵的二曱基矽亞胺自由基 (dimethylsilanimine radical)，如第 3 圖的過程 340 所示。 ❹ §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（b〇nd insertion process)，其中二甲基矽亞胺自由基直接插入 Si原子和C原子之間以産生碳氮化矽産物。當然，本領 〇 域技術人員將領會到假多替換、變化和修改態樣。 第4圖不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 疋CVD製程，用於在基板上沈積具有流動特性的無定形 碳氮切膜。方法4GG可包括在沈積室巾提供基板（步 驟41〇)。沈積室耗合到一遠端電製系統。該方法4〇〇也 可匕括將氨引入該遠端電漿系統中’以在遠端電漿中使 14 200927979 氨解離而產生自由基氣前驅物。所産生的自由基氮前驅 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包括將氮氳（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 喷頭來輸送氮氫（NH)自由基和氫（H)自由基，該喷頭以流 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）可通過擋板或喷頭 ® 進入沈積室，該擋板或喷頭諸如在2007年5月29日申 請、名稱爲「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’在此引入其全部内容作爲參考。 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43〇)。在一實施例中’ 〇 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C：VD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 矽則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44〇 當含矽前驅 物在沈積室中遇到氮氫NH自由基和氫Η自由基時，前 15 200927979 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一氮氫自由基。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。二曱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 )前驅物流速設定爲1 mgm/ min至 Ο 1 5gm/ min ; 2 )將沈積室保持在約1毫托至約6〇〇托範 圍内的壓力下；3 )腔室溫度控制在約〇〇c至約4〇〇〇c之 間。形成矽一氮氩自由基在第3圖的過程32〇中發生。 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35(^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4〇〇還包括在氧化環境 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450八與其他可流動性介電膜（例如習知的s〇g 膜）相似，高溫退火引起羥基和殘留的碳解離成水和/或 甲酵蒸氣’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45〇是在蒸汽（水蒸 汽）说圍内的氧化環境中進行的熱退火。例如，在約彻 200927979 °c至高達約丨050°c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（atin，即約760 托）的範圍内。 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。〇下的臭氧處理。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1該膜膨脹與 Ο 由於未反應的碳和〇H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 含具有燒氧基取代基乙石夕烧時’在沈積期間，酸性環境 有助於催化該些未反應之有機部分（organie m〇ieties)的 反應。第5圖示意性示出根據本發明實施例，酸性催化 17 200927979 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 CHjO基團轉換成反應性的cHsOH基團。其顯示於第5 圖的過程510中。 ❹ 此時水蒸氣與反應性的CH3〇H基團反應，如過程 520所示。反應導致形成矽醇基（Si_〇H)，並且從膜中釋 出甲醇分子（CHsOH)。所形成的矽酵Si_0I1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 形成氧化梦網狀結構（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 φ 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（ΝΑ ))的氛圍中退火該可流動性碳氮化砍膜。對於 CVD沈積膜包含具有烷氧基取代基的乙矽烷，驗性環境 有助於在沈積期間催化該些未反應之有機部分的反應。 第6 A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 包括利用包含氨的驗性蒸汽進行烧基的親核性攻擊。該 機制中，矽烷氧基的烷基部分會轉移给氨，在轉移過程 18 200927979 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，並且形成發 醇（-Si-OH )基。在隨後的反應中，會發生石夕醇縮合反 應’而將固化的介電氧化膜中的-Si-ΟΗ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，而形成砍院基 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 醇並且重新産生氨。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-0-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 烧基和絲基）的*範性t程條件可包括在含有水和驗 性蒸汽的環境中進行膜層的沈積後固化處理。例如’如 果驗性蒸汽含有氨作爲驗催化劑，則所沈積的膜可被 加熱至約3(HTC同時被暴露到壓力爲約i托至約4〇托的 潮濕氨氣氛圍中達約2分鐘$幼ς八μ , _ . _ 200927979 氨氣氛圍也可包含氧氣（〇2)和/或利用氮前驅 歹•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。系统7〇〇包括沈積冑7〇1，在沈積 ❹
室701中，前驅物進行化學反應並且在基板晶圓了们上 沈積可流動性的介電膜。晶圓7〇2(例如鳩随、細職、 4〇〇mm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7〇2定位 在更接近或更遠離上方的前驅物分配系統7〇6。基座可 以約Irpm至約2000 rpm (例如約1〇rpm至約12〇rpm) 的旋轉速度來旋轉基板晶圓。基座可以垂直移動基板一 丰又距離，例如離該前驅物分配系統之該些側喷嘴7 〇 8約 〇.5mm至約100mm的距離。 刖媒物分配系統7 0 6包括多個徑向分佈的側喷嘴 708’其每一個喷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71〇，其 與基板底座704的中心共軸。流體通道712可通過擋板 71 〇中心’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圍繞著擔板710的外部表面，該管道714 用來引導來自沈積室70 1上方之反應性物種産生系統 20 200927979 (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産生系統。 反應性物種産生系統可以是遠端電漿産生系統 (RPS)’其將較穩定的起始材料暴露於電漿中而産生反 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 φ 邠刀的刀子氧解離成原子氧，一種可在較低溫度下（例 如低於100 c )與有機矽前驅物（例如TM〇s、〇MCTS ) 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 産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7〇1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7〇1中産 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71〇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 或多個侧喷嘴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 21 200927979 流動性的介電琪。 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的旋轉可能産生搖擺’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7〇4也可包 @ 括用來創造出真空失盤的多個凹槽及/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。 典型的室内沈積壓力是介於約〇〇5托至約2〇〇托範圍内 的腔室總麼力（例如1托）’這讓真空夹盤得以將晶圓保 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。轴720也可包含多個内部通道（未示出），用以 參 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7〇4。這些通道可從底座中心 向週邊延伸，以爲上方基板晶圓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1 〇〇。(：。 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 22 200927979 板7〇2,以烘烤或退火基板上的沈積臈。在沈積期間， 也可啟動該些燈，以促進膜前驅物或沈積膜令的反應。 至》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。
‘文中k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。 所述範圍内的任何所述值或其内數值與該範圍内的任一 其他所述值或其内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 該祀圍_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内。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 多種喷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、 23 200927979 驟仁疋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。 【圖式簡單說明】 第1圖示意性不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_〇_si之化合物 的化學反應過程； 〇 … 第2圖是不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産生的自由基 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氣 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 _化硬膜的示範性製程系統的截面_圖。 【主要元件符號說明】 24 200927979 200 ' 400 方法 步驟 過程 步驟 210 ' 220 ' 230 、 240 、 250 310電漿誘導化學反應過程 320 、 325 ' 330 、 340 ' 350 410 、 420 、 430 、 440 ' 450 510、520、330、340 過程 700處理系統 701沈積室 7 0 2基板晶圓 704基板底座 706前驅物分配系統 708側喷嘴 710擋板 712流體通道 714管道 716圓頂 7 1 8馬達 720軸 722照射系統 25

Claims (1)

  1. 200927979 七、申請專利範圍： 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一基板的一沈積室中，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産生至 少一種自由基氮前驅物；以及 ❹ 將該自由基氮前驅物引入該沈積室中，其中該自由 基氣和該含梦前驅物反應，並且在該基板上沈積該含矽 和氮的膜。 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·如申睛專利範圍第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是〇、1或2。 4_如申凊專利範圍第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.如申凊專利範圍第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 26 200927979 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，以形成氧化石夕膜。 9.如申請專利範圍第8項所述的方法 汽（steam)的環境中執行該退火。 ’其中在一包含蒸 10.如申請專利範圍第8項所述的方法 性蒸汽的環境中執行該退火。 ’其中在一包含酸 11 ·如申請專利範圍第 約900°c範圍内的_ ; ;8項所述时法，其巾細2〇°C至 溫度下執行該退火。 12 ·如申請專利範圍第 氧（〇3)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 27 200927979 匕括在，約20°c至、約600°c範圍内的—溫度下，將該基板 暴露於紫外光。 如申請專利範圍第8項所述的方法，其中在包含分子 氧（〇2)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（〇)的氛圍中且在約2〇°C至約6〇(TC範圍内的一溫度下 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2〇〇t： 到約1050 °C範圍的一溫度下執行該退火。 17·—種在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産生多個氮 氫自由基（hydronitrene radicals); 將含梦前驅物引入該沈積室，該含石夕前驅物包括至 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 —膜，該第一膜包含多個Si-N(H)-Si鍵； 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 28 200927979 S i Ο S i 鍵0 18.如申請專利範圍第17 項所述的方法
    | w万法，其中該産生多 & m露到該遠端電漿系統中 部分的氣解離成該多個氫氮自由 所述的方法，其中該含矽前驅 ΐ9·如申請專利範圍第17 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經基。 21. 如申請專利粑圍第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90(rc範圍内的一溫 ❹ 度下執行。 22. 如申請專利範圍第π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-0-Si鍵的至少第 一部分。 29 200927979 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，以形成反應性的〇H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 汽包括氫氣酸或醋酸。 ❹ 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. —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 ❹ 矽層包含多個碳物種的副産物； 將一鹼性蒸汽引入該半導體處理室中，該鹼性蒸汽 與該氧化石夕層反應，以從該氧化碎層巾去除該些碳物 種；以及 從該半導體處理室中移除該鹼性蒸汽。 28. 如中請專利錢第27項所述的方法，其中該驗性蒸 汽包括氨。 30 200927979 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㈣圍第27項所述的方法，其中該氧化石夕 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，其令該引入一 驗性蒸汽的步㈣包括冑氨氣流入該半導體處理室中。 如申請專利範圍第27項所述的方法，其中該驗性蒸 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 包括分子氧（〇2p 其中該蒸汽更 =申請專利範圍帛27項所述的方法，其中該蒸汽 已括遠端産生的自由基原子氮 Γ和如申請專利範圍第27項所述的方法，其"驗性蒸 二，化矽層之間的該反應在約，c至約鑛之間 31 200927979 37. 如申請專利範圍第26項所述的方法，其中該反應在 約3 00°C執行。 38. 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。 39. 如申請專利範圍第38項所述的方法，其中該處理室 具有約40托的壓力。 32
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US8242031B2 (en) 2012-08-14
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