TWI498447B - 使用胺基金屬與鹵化金屬前驅物組合之含金屬氮化物之薄膜沈積 - Google Patents

使用胺基金屬與鹵化金屬前驅物組合之含金屬氮化物之薄膜沈積 Download PDF

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TWI498447B
TWI498447B TW100111512A TW100111512A TWI498447B TW I498447 B TWI498447 B TW I498447B TW 100111512 A TW100111512 A TW 100111512A TW 100111512 A TW100111512 A TW 100111512A TW I498447 B TWI498447 B TW I498447B
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Katsuko Higashino
Kazutaka Yanagita
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Description

使用胺基金屬與鹵化金屬前驅物組合之含金屬氮化物之薄膜沈積
相關申請案之交叉引用
本申請案主張2010年4月1日申請之美國臨時申請案第61/320,236號的權利，該案之全部內容以引用的方式併入本文中。
揭示自胺基金屬前驅物與鹵化金屬前驅物之組合形成含金屬氮化物之薄膜，較佳自胺基矽烷前驅物與氯矽烷前驅物之組合形成含SiN之薄膜的方法。變化胺基金屬前驅物與鹵化金屬前驅物之順序反應實現了具有變化之化學計量的含金屬氮化物之薄膜的形成。另外，含金屬氮化物之薄膜的組成可基於胺基金屬前驅物之結構而加以修飾。所揭示製程可為熱製程或低溫下的電漿製程。
諸如氮化矽(SiN)薄膜之含金屬氮化物之薄膜廣泛用於半導體器件及超大規模積體(ULSI)電路中。根據日益需要較高LSI安裝密度的電子器件之小型化及增長的複雜性，需要SiN薄膜改良其對抗電流洩漏的薄膜品質。另外，亦將SiCN薄膜用作用於Cu佈線之雙鑲嵌結構中的蝕刻擋止器。
氮化矽(SiN)薄膜已被研究以在線後端(BEOL)製程中應用為鑲嵌內之蝕刻終止/襯墊層。在浮閘電晶體內，閘間介電層可包含(例如)SiO2 或SiN。另外，摻雜碳之SiN層提供高的抗蝕刻性。
當大規模整合(LSI)之尺寸按比例縮小時，薄膜深度應較薄，從而需要更精確控制之製程(例如，原子層沈積(ALD))。另外，需要沈積溫度降低。ALD廣泛用於許多製程(例如，SiO2 、SiN及金屬薄膜)。參見(例如)美國專利第7648927號。然而，沈積速率趨於低於化學氣相沈積(CVD)。當沈積溫度較低時，SiN之沈積速率及薄膜品質較差。
許多文章已報告，藉由PECVD、PEALD藉由使用氯矽烷及活性NH3 以及引入胺、CH4 或C2 H4 作為碳源而沈積高品質SiN及SiCN薄膜(參見(例如)WO2009/149167及US2008/0213479)。
仍需要更精確控制之製程來沈積含金屬氮化物之薄膜。
記法及命名
某些縮寫、符號及術語遍及以下描述及申請專利範圍被使用並包括：縮寫「A」指代埃且1埃=100微微米；縮寫「PECVD」指代電漿增強型化學氣相沈積；縮寫「CVD」指代化學氣相沈積；縮寫「RF」指代射頻，縮寫「DR」指代沈積速率，且縮寫「RI」指代折射率。
術語「烷基」指代排他地含有碳及氫原子之飽和官能基。此外，術語「烷基」指代直鏈、支鏈或環狀烷基。直鏈烷基之實例包括(不限於)甲基、乙基、丙基、丁基等。支鏈烷基之實例包括(不限於)第三丁基。環狀烷基之實例包括(不限於)環丙基、環丁基、環戊基、環己基等。
如本文中所使用，縮寫「Me」指代甲基；縮寫「Et」指代乙基；縮寫「Pr」指代丙基；縮寫「nPr」指代鏈丙基；縮寫「iPr」指代異丙基；縮寫「Bu」指代丁基(正丁基)；縮寫「tBu」指代第三丁基；縮寫「sBu」指代第二丁基；縮寫「iBu」指代異丁基；且縮寫「TMS」指代三甲基矽烷基。
本文中使用來自元素週期表之元素的標準縮寫。應理解，元素可由此等縮寫來指代(例如，Si指代矽，C指代碳，等)。
所揭示內容為形成含金屬氮化物之薄膜的方法。將鹵化金屬前驅物引入至含有至少一基板之ALD反應器中。隨後將多餘鹵化金屬前驅物自該反應器清除。將胺基金屬前驅物引入至該反應器中。隨後將多餘胺基金屬前驅物自該反應器清除。可視情況將反應物引入至該反應器中。隨後將多餘可選反應物自該反應器清除。鹵化金屬前驅物之金屬及胺基金屬前驅物之金屬可為相同或不同的。
所揭示內容亦為形成含金屬氮化物之薄膜的方法。將鹵化金屬前驅物引入至含有至少一基板之ALD反應器中。隨後將多餘鹵化金屬前驅物自該反應器清除。將胺基金屬前驅物引入至該反應器中。隨後將多餘胺基金屬前驅物自該反應器清除。將反應物引入至該反應器中。隨後將多餘反應物自該反應器清除。鹵化金屬前驅物之金屬及胺基金屬前驅物之金屬可為相同或不同的。
所揭示內容亦為形成含氮化矽之薄膜的方法。將氯矽烷前驅物引入至含有至少一基板之ALD反應器中。隨後將多餘氯矽烷前驅物自該反應器清除。將胺基矽烷前驅物引入至該反應器中。隨後將多餘胺基矽烷前驅物自該反應器清除。可視情況將反應物引入至該反應器中。隨後將多餘可選反應物自該反應器清除。
所揭示內容亦為形成含氮化矽之薄膜的方法。將氯矽烷前驅物引入至含有至少一基板之ALD反應器中。隨後將多餘氯矽烷前驅物自該反應器清除。將胺基矽烷前驅物引入至該反應器中。隨後將多餘胺基矽烷前驅物自該反應器清除。將反應物引入至該反應器中。隨後將多餘反應物自該反應器清除。
所揭示方法中之每一者可進一步包括以下態樣中之一或多者：
‧　反應物係選自由以下各物組成之群：N2 、NH3 、N2 H4 、NMeH2 、NEtH2 、NMe2 H、NEt2 H、NMe3 、NEt3 、MeHNNH2 、Me2 NNH2 、苯肼及其混合物；
‧　反應物為NH3 ；
‧　藉由使方法步驟之次序變化而產生具有指定化學計量的含金屬氮化物之薄膜；
‧　鹵化前驅物為氯化金屬前驅物；
‧　含金屬氮化物之薄膜為含有一種或兩種金屬之金屬碳氮化物薄膜；
‧　金屬係選自過渡金屬、金屬或非金屬元素；
‧　金屬為硼或磷；
‧　含金屬氮化物之薄膜為含氮化矽之薄膜；
‧　鹵化金屬前驅物為氯矽烷前驅物；
‧　胺基金屬前驅物為胺基矽烷前驅物；
‧　含氮化矽之薄膜為摻雜碳之SiN薄膜；
‧　氯矽烷前驅物具有式Sia Hb Clc ，其中b+c=2a+2；
‧　氯矽烷前驅物作為混合物而引入；
‧　胺基矽烷前驅物具有式H4-x Si(NR'R")x ，其中x=1、2、3或4，R'及R"獨立地選自H或烷基，且R'及R"可經鍵聯以形成環結構；
‧　胺基矽烷前驅物包含胺基氯矽烷或胺基烷基矽烷；
‧　胺基氯矽烷前驅物具有式Cl4-x Si(NR'R")x ，其中x=2或3，R'及R"獨立地選自H或烷基，且R'及R"可經鍵聯以形成環結構；及
‧　胺基烷基矽烷前驅物具有式R'''4-x Si(NR'R")x ，其中x=1、2或3，R'及R"獨立地選自H或烷基，R'及R"可經鍵聯以形成環結構，且R'''基為具有少於3個碳之烷基。
為進一步理解本發明之本質及目標，結合隨附圖式參考以下實施方式。
所揭示內容為使用胺基金屬前驅物及鹵化金屬前驅物之交替供應形成含金屬氮化物之薄膜的ALD方法。胺基金屬前驅物與鹵化金屬前驅物之順序反應產生緻密的富金屬薄膜。鹵化金屬前驅物之金屬可與胺基金屬前驅物之金屬相同或不同。
所揭示內容亦為在熱條件或低溫電漿條件下使用胺基矽烷前驅物及氯矽烷前驅物之交替供應形成含氮化矽之薄膜(較佳碳氮化矽薄膜)的ALD方法。胺基矽烷前驅物與氯矽烷前驅物之順序反應在低於許多先前技術氮化矽薄膜沈積製程之溫度的溫度下產生緻密的富矽薄膜。碳氮化矽薄膜或者可被稱為摻雜碳之氮化矽薄膜。一般熟習此項技術者將認識到，氮化矽薄膜中之碳的含量判定適當之命名，摻雜碳之氮化矽薄膜中碳的量典型地小於碳氮化矽薄膜中碳的量。然而，一般熟習此項技術者將進一步認識到，判定適當命名的薄膜中碳之準確百分比未被定義且將因人而異。
所揭示方法藉由ALD自胺基金屬及鹵化金屬前驅物形成含金屬氮化物之薄膜(諸如，SiN)或金屬碳氮化物薄膜(諸如，SiCN)。含金屬氮化物之薄膜可為含有一或兩種金屬之金屬碳氮化物薄膜。舉例而言，金屬碳氮化物薄膜可為SiHfCN薄膜。或者，SiN薄膜可摻雜碳。
如實施例2至4中將進一步詳細描述，具有指定化學計量之含金屬氮化物之薄膜可藉由使所揭示方法步驟的次序變化而產生。此外，所揭示方法步驟之持續時間亦可變化，以便「調諧」所得薄膜。
將鹵化金屬前驅物引入至含有一或多個基板之ALD反應器中。可在胺基金屬前驅物之前或之後將鹵化金屬前驅物引入至ALD反應器中。反應器內之條件准許鹵化金屬前驅物之至少部分自吸附於基板上。一般熟習此項技術者將認識到，基板性質將定義鹵化金屬前驅物在此步驟中是經歷物理吸附抑或化學吸附。舉例而言，若鹵化金屬前驅物在胺基金屬前驅物之後引入至反應器中，則鹵化金屬前驅物之至少部分將與在先前步驟中所沈積的胺基金屬前驅物之部分反應/化學吸附。將任何未吸附或「多餘」之鹵化金屬前驅物清除出反應器。鹵化金屬前驅物在低溫下與NH3 /胺基金屬前驅物發生反應。
鹵化金屬前驅物可為氯化金屬前驅物。鹵化金屬或氯化金屬前驅物之金屬可為如元素週期表上通常定義的任何過渡金屬、金屬或非金屬元素。較佳過渡金屬包括(但不限於)Hf。較佳金屬包括(但不限於)Zn。較佳非金屬包括(但不限於)B、Si及P。鹵化金屬前驅物可應用為兩種或兩種以上鹵化金屬前驅物之混合物。較佳地，鹵化金屬前驅物為氯矽烷前驅物。例示性氯矽烷前驅物具有式Sia Hb Clc ，其中b+c=2a+2。例示性氯矽烷前驅物包括六氯二矽烷(HCDS)、SiCl4 、SiHCl3 、Si2 H5 Cl等及其混合物，諸如，HCDS與SiCl4 或HCDS與SiHCl3 。較佳地，鹵化金屬前驅物包含HfCl4 或HCDS，且更佳為HCDS。
將胺基金屬前驅物引入至反應器中。反應器內之條件准許胺基金屬前驅物之至少部分自吸附於基板上。胺基金屬前驅物可在鹵化金屬前驅物之前或之後引入至ALD反應器中。再一次，一般熟習此項技術者將認識到，基板性質將定義胺基金屬前驅物在此步驟中是經歷物理吸附抑或化學吸附。舉例而言，若胺基金屬前驅物在鹵化金屬前驅物之後引入至反應器中，則胺基金屬前驅物之至少部分將與在先前步驟中所沈積的鹵化金屬前驅物之部分反應/化學吸附。接著將任何未吸附或「多餘」之胺基金屬前驅物清除出反應器。與僅充當N源之先前技術NH3 前驅物對比，胺基金屬前驅物可充當C源及N源兩者。胺基金屬前驅物之烷基胺基充當良好的離去基且產生良好的吸附。使胺基金屬前驅物之配位基變化提供修飾含金屬氮化物之薄膜之碳含量的能力。
胺基金屬前驅物之金屬可為如元素週期表上通常定義的任何過渡金屬、金屬或非金屬元素。較佳過渡金屬包括(但不限於)Hf。較佳金屬包括(但不限於)Zn。較佳非金屬包括(但不限於)B、Si及P。胺基金屬前驅物可應用為兩種或兩種以上胺基金屬前驅物之混合物。胺基金屬前驅物可為胺基矽烷前驅物。例示性胺基矽烷前驅物具有式H4-x Si(NR'R")x ，其中x=1、2、3或4，R'及R"獨立地選自H或烷基，且R'及R"可經鍵聯以形成環結構。或者，胺基矽烷前驅物可為胺基氯矽烷前驅物或胺基烷基矽烷前驅物。例示性胺基氯矽烷前驅物具有式Cl4-x Si(NR'R")x ，其中x=2或3，且R'及R"係如先前定義。例示性胺基烷基矽烷前驅物具有式R'''4-x Si(NR'R")x ，其中x=1、2或3，R'及R"係如先前定義，且R'''基為具有小於3個碳之烷基。較佳地，胺基金屬前驅物為雙(二乙基胺基)矽烷(BDEAS)、參(二甲基胺基)矽烷(3DMAS)、肆(二甲基胺基)矽烷(4DMAS)或肆(乙基甲基胺基)鉿，且更佳為3DMAS及/或4DMAS。
將鹵化金屬前驅物及胺基金屬前驅物(共同地稱為「前驅物」)以蒸氣形式各自個別地引入至反應器中。在此情形中，「個別地」及「各自」指代指定類別之前驅物，例如「鹵化金屬前驅物」，其可由一或多種鹵化前驅物組成。在以下段落中，個別地不意欲意謂僅一種鹵化金屬前驅物之蒸氣引入至反應器中。
前驅物可以液體狀態個別地饋飼至蒸發器，其中該等前驅物在引入至反應器中之前各自個別地蒸發。在蒸發之前，前驅物中之每一者可視情況與一或多種溶劑混合。該等溶劑可選自由以下各物組成之群；甲苯、乙苯、二甲苯、1,3,5-三甲苯、癸烷、十二烷、辛烷、己烷、戊烷或其他。所得濃度可自約0.05 M變化至約2 M。
或者，前驅物可藉由將載氣傳遞至含有該等前驅物中之每一者的容器中或藉由使載氣起泡進入該等前驅物中之每一者中而個別地蒸發。該等前驅物中之每一者可視情況與一或多種溶劑在容器中混合。接著將載氣及個別前驅物作為蒸氣引入至反應器中。載氣可包括(但不限於)Ar、He、N2 及其混合物。藉由載氣起泡亦可移除存在於前驅物之溶液中的任何溶解氧。
必要時，可將容器加熱至准許前驅物處於液相並具有足夠之蒸氣壓力的溫度。容器可維持在(例如)0℃至150℃之範圍中之溫度下。熟習此項技術者認識到，可以已知方式調整容器之溫度以控制被蒸發之前驅物的量。
可將每一前驅物之蒸氣引入至反應器中歷時約0.01秒至約60秒、或約5秒至約25秒、或約10秒至約20秒之時間週期。
在一具體實例中，可將反應物引入至反應器中，在反應器處反應物與基板上之自吸附層反應。任何未反應或「多餘」之反應物接著被清除出反應器。反應物可為N2 、NH3 、N2 H4 、NMeH2 、NEtH2 、NMe2 H、NEt2 H、NMe3 、NEt3 、MeHNNH2 、Me2 NNH2 、苯肼及其混合物。較佳地，反應物為NH3 。然而，如隨後之實施例中將進一步詳細描述，可選反應物步驟之包括將取決於所得含金屬氮化物之薄膜中的元素之所要化學計量比。
反應物可藉由電漿來處理，以便將反應物分解成其自由基形式。電漿可產生或存在於反應器自身內。或者，(例如)在遠端定位之電漿系統中，電漿可一般處於遠離反應器的位置處。熟習此項技術者將認識到適於此電漿處理之方法及裝置。
舉例而言，可將反應物引入至直接電漿反應器(其在反應器中產生電漿)中，以在反應器中產生電漿處理之反應物。例示性直接電漿反應器包括由Trion技術所生產的TitanTM PECVD系統。可在電漿處理之前將反應物引入並保持於反應器中。或者，電漿處理可與反應物之引入同時發生。原位電漿典型地為在簇射頭與基板固持器之間所產生的13.56 MHz RF電容性耦合電漿。基板或簇射頭可取決於正離子碰撞是否發生而為帶電電極。原位電漿產生器中之典型施加電力為自約100 W至約1000 W。對於相同的電力輸入，使用原位電漿來解除關聯反應物典型地比不上使用遠端電漿源來達成反應物之解除關聯，且因此不如遠端電漿系統在反應物解除關聯方面有效，此可有益於在易於受電漿損壞的基板上沈積含金屬氮化物之薄膜。
或者，可在反應器之外部產生經電漿處理之反應物。MKS儀器之i活性氣體產生器可用以在傳遞至反應器中之前處理反應物。在2.45 GHz、7kW電漿電力及自約3托變化至約10托之壓力下操作，反應物NF3 可以超過96%分解效率分解成三個F- 基。較佳地，可以自約1 kW變化至約10 kW，更佳自約2.5 kW變化至約7.5 kW的電力產生遠端電漿。
ALD反應器可為具有安置於其內之至少一或多個基板的加熱之器皿。反應器具有如下出口：可連接至真空泵以允許副產物自反應器移除，或允許反應器內之壓力被修改或調節。合適之ALD反應器之實例包括(不限於)平行板型反應器、冷壁型反應器、熱壁型反應器、單晶圓反應器、多晶圓反應器、直接電漿反應器，或在適於使前驅物反應並形成多個層之條件下的其他類型之沈積系統。
一般而言，反應器含有上面將沈積含金屬氮化物之薄膜的一或多個基板。舉例而言，反應器可含有自1至200個具有自25.4 mm至450 mm之直徑的矽晶圓。基板可為用於半導體、光伏打、平板或LCD-TFT器件製造中的任何合適基板。基板可含有一或多個額外材料層，該一或多個層可自先前製造步驟而呈現。介電層及導電層為此等額外材料層之實例。在本申請案之範疇內，基板及沈積於基板上之任何層中的全部共同地包括於術語基板內。合適之基板的實例包括(不限於)金屬基板、金屬氮化物基板、矽基板、矽石基板、氮化矽基板、氮氧化矽基板、鎢基板及其組合。另外，可使用包含鎢或貴金屬(例如，鉑、鈀、銠或金)之基板。較佳地，基板為金屬薄膜或金屬氮化物薄膜。
反應器之溫度可藉由控制基板固持器之溫度或控制反應器壁之溫度來控制。此項技術中已知用以加熱基板之器件。反應器被加熱至足夠之溫度，以獲得在足夠生長速率下生長並具有所要物理狀態及組成的所要的含金屬氮化物之薄膜。可將反應器加熱至的非限制例示性溫度範圍包括自約200℃至約700℃。當利用電漿沈積製程時，沈積溫度可自約200℃變化至約550℃。或者，當執行熱製程時，沈積溫度可自約400℃變化至約600℃。
ALD反應器中之壓力為約0.1托(13帕)至約10托(1300帕)。
在一較佳具體實例中，所揭示方法利用氯矽烷前驅物(較佳HfCl4 或HCDS)及胺基矽烷前驅物(較佳3DMAS、4DMAS或肆(乙基甲基胺基)鉿)以形成含SiN或含SiCN之薄膜。所形成之薄膜具有極低(自約0至約5原子%)的氯或氧含量。
所揭示方法藉由低溫下的原子層沈積及含SiN之薄膜中的C插入而解決關於含SiN之薄膜之薄膜品質的問題。
所揭示方法提供勝於現有方法之以下優點：-　碳插入至具有胺基矽烷與氯矽烷之可調諧組合的SiN薄膜中原因為：-　組合之比率改變製成不同組成之薄膜。
實施例
提供以下非限制實施例以進一步說明本發明之具體實例。然而，該等實施例不欲包括全部且不欲限制本文中所描述之本發明的範疇。
實施例1
使用ALD方法以及三氯矽烷(3CS)及參(二甲基胺基)矽烷(3DMAS)前驅物來沈積緻密的SiCN薄膜。反應腔室被控制在5托、550℃下，且100 sccm之Ar連續地流動。沈積製程由以下步驟組成：1)將約1 sccm之3CS的脈衝供應至反應腔室歷時10秒，2)藉由100 sccm之Ar清除3CS前驅物歷時30秒，3)將約1 sccm之3DMAS的脈衝供應至反應腔室歷時10秒，4)藉由100 sccm之Ar清除3DMAS前驅物歷時30秒。重複序列1)至4)，直至沈積層達成合適之層厚度為止。
沈積薄膜展示沈積速率為約0.6埃/循環。折射率為2.1以上。
實施例2a
使用ALD方法藉由六氯二矽烷(HCDS)及參(二甲基胺基)矽烷(3DMAS)前驅物以及氨(NH3 )反應物來沈積緻密的SiCN薄膜。反應腔室被控制在5托、550℃下，且55 sccm之Ar連續地流動。沈積製程包含以下步驟：1)將約1 sccm之3DMAS的脈衝引入至反應腔室中歷時10秒，2)藉由55 sccm之Ar清除3DMAS前驅物歷時30秒，3)將約1 sccm之HCDS的脈衝引入至反應腔室中歷時10秒，4)藉由55 sccm之Ar清除HCDS前驅物歷時30秒，5)將約50 sccm之NH3 的脈衝引入至反應腔室中歷時10秒，及6)藉由55 sccm之Ar清除NH3 反應物歷時10秒。重複序列1)至6)，直至沈積層達成合適之層厚度為止。
圖1中展示沈積薄膜之沈積速率及折射率。所得薄膜中之矽及氮每一者的原子組成百分比大於40%但小於45%，而碳的原子組成百分比為約10%。所得薄膜中之氯及氧每一者的原子組成百分比為0%或更大但小於5%。所得薄膜由HF溶液蝕刻之濕式蝕刻速率為4.24埃/分鐘。
實施例2b
使用ALD方法藉由HCDS 3DMAS前驅物以及氨(NH3 )反應物來沈積緻密的SiCN薄膜。反應腔室被控制在5托、550℃下，且55 sccm之Ar連續地流動。沈積製程包含以下步驟：1)將約1 sccm之HCDS的脈衝引入至反應腔室中歷時10秒，2)藉由55 sccm之Ar清除HCDS前驅物歷時30秒，3)將約1 sccm之3DMAS的脈衝引入至反應腔室中歷時10秒，4)藉由55 sccm之Ar清除3DMAS前驅物歷時30秒，5)將約50 sccm之NH3 的脈衝引入至反應腔室中歷時10秒，及6)藉由55 sccm之Ar清除NH3 反應物歷時10秒。重複序列1)至6)，直至沈積層達合適層厚度為止。
圖2中展示沈積薄膜之沈積速率及折射率。所得薄膜中之矽的原子組成百分比大於45%但小於50%，所得薄膜中之氮的原子組成百分比大於30%但小於35%，且碳之原子組成百分比大於15%但小於20%。所得薄膜中之氯及氧每一者的原子組成百分比為0%或更大但小於5%。所得薄膜由HF溶液蝕刻之濕式蝕刻速率為0.54埃/分鐘。
實施例2c
使用ALD方法藉由HCDS及3DMAS前驅物來沈積緻密的SiCN薄膜。反應腔室被控制在5托、550℃下，且55 sccm之Ar連續地流動。沈積製程包含以下步驟：1)將約1 sccm之3DMAS的脈衝引入至反應腔室中歷時10秒，2)藉由55 sccm之Ar清除3DMAS前驅物歷時30秒，3)將約1 sccm之HCDS的脈衝引入至反應腔室中歷時10秒，及4)藉由55 sccm之Ar清除HCDS前驅物歷時30秒。重複序列1)至4)，直至沈積層達成合適之層厚度為止。
圖3中展示沈積薄膜之沈積速率及折射率。所得薄膜中之矽的原子組成百分比大於50%但小於55%，所得薄膜中之碳的原子組成百分比大於30%但小於35%，且氮之原子組成百分比為約10%。所得薄膜中之氯及氧每一者的原子組成百分比為1%或更大但小於5%。所得薄膜由HF溶液蝕刻之濕式蝕刻速率為0.04埃/分鐘。
實施例3a
使用ALD方法藉由六氯二矽烷(HCDS)及肆(二甲基胺基)矽烷(4DMAS)前驅物以及氨(NH3 )反應物來沈積緻密的SiCN薄膜。反應腔室被控制在5托、550℃下，且55 sccm之Ar連續地流動。沈積製程包含以下步驟：1)將約1 sccm之4DMAS的脈衝引入至反應腔室中歷時10秒，2)藉由55 sccm之Ar清除4DMAS前驅物歷時30秒，3)將約1 sccm之HCDS的脈衝引入至反應腔室中歷時10秒，4)藉由55 sccm之Ar清除HCDS前驅物歷時30秒，5)將約50 sccm之NH3 的脈衝引入至反應腔室中歷時10秒，及6)藉由55 sccm之Ar清除NH3 反應物歷時10秒。重複序列1)至6)，直至沈積層達成合適之層厚度為止。
圖4中展示沈積薄膜之沈積速率及折射率。所得薄膜中之氮的原子組成百分比為約45%，所得薄膜中之矽的原子組成百分比大於40%但小於45%，且碳之原子組成百分比大於5%但小於10%。所得薄膜中之氯及氧每一者的原子組成百分比為0%或更大但小於5%。所得薄膜由HF溶液蝕刻之濕式蝕刻速率為5.76埃/分鐘。
實施例3b
使用ALD方法藉由HCDS及4DMAS前驅物以及氨(NH3 )反應物來沈積緻密的SiCN薄膜。反應腔室被控制在5托、550℃下，且55 sccm之Ar連續地流動。沈積製程包含以下步驟：1)將約1 sccm之HCDS的脈衝引入至反應腔室中歷時10秒，2)藉由55 sccm之Ar清除HCDS前驅物歷時30秒，3)將約1 sccm之4DMAS的脈衝引入至反應腔室中歷時10秒，4)藉由55 sccm之Ar清除4DMAS前驅物歷時30秒，5)將約50 sccm之NH3 的脈衝引入至反應腔室中歷時10秒，及6)藉由55 sccm之Ar清除NH3 反應物歷時10秒。重複序列1)至6)，直至沈積層達成合適之層厚度為止。
圖5中展示沈積薄膜之沈積速率及折射率。所得薄膜中之矽的原子組成百分比大於40%但小於45%，所得薄膜中之氮的原子組成百分比為約40%，且碳之原子組成百分比大於10%但小於15%。所得薄膜中之氯及氧每一者的原子組成百分比為0%或更大但小於5%。所得薄膜由HF溶液蝕刻之濕式蝕刻速率為4.31埃/分鐘。
實施例3c
使用ALD方法藉由HCDS及4DMAS前驅物來沈積緻密的SiCN薄膜。反應腔室被控制在5托、550℃下，且55 sccm之Ar連續地流動。沈積製程包含以下步驟：1)將約1 sccm之4DMAS的脈衝引入至反應腔室中歷時10秒，2)藉由55 sccm之Ar清除4DMAS前驅物歷時30秒，3)將約1 sccm之HCDS的脈衝引入至反應腔室中歷時10秒，及4)藉由55 sccm之Ar清除HCDS前驅物歷時30秒。重複序列1)至4)，直至沈積層達成合適之層厚度為止。
圖6中展示沈積薄膜之沈積速率及折射率。所得薄膜中之矽的原子組成百分比大於50%但小於55%，所得薄膜中之碳的原子組成百分比大於30%但小於35%，且氮之原子組成百分比為約10%。所得薄膜中之氯及氧每一者的原子組成百分比為1%或更大但小於5%。所得薄膜由HF溶液蝕刻之濕式蝕刻速率為0.15埃/分鐘。
實施例4a
使用ALD方法藉由六氯二矽烷(HCDS)及雙(二乙基胺基)矽烷(BDEAS)前驅物以及氨(NH3 )反應物來沈積緻密的SiCN薄膜。反應腔室被控制在5托、550℃下，且55 sccm之Ar連續地流動。沈積製程包含以下步驟：1)將約1 sccm之BDEAS的脈衝引入至反應腔室中歷時10秒，2)藉由55 sccm之Ar清除BDEAS前驅物歷時30秒，3)將約1 sccm之HCDS的脈衝引入至反應腔室中歷時10秒，4)藉由55 sccm之Ar清除HCDS前驅物歷時30秒，5)將約50 sccm之NH3 的脈衝引入至反應腔室中歷時10秒，及6)藉由55 sccm之Ar清除NH3 反應物歷時10秒。重複序列1)至6)，直至沈積層達成合適之層厚度為止。
圖7中展示沈積薄膜之沈積速率及折射率。所得薄膜中之矽的原子組成百分比稍微大於約40%，所得薄膜中之氮的原子組成百分比稍微小於40%，且碳之原子組成百分比稍微大於15%。所得薄膜中之氯及氧每一者的原子組成百分比為0%或更大但小於5%。所得薄膜由HF溶液蝕刻之濕式蝕刻速率為1.65埃/分鐘。
實施例4b
使用ALD方法藉由HCDS及BDEAS前驅物以及氨(NH3 )反應物來沈積緻密的SiCN薄膜。反應腔室被控制在5托、550℃下，且55 sccm之Ar連續地流動。沈積製程包含以下步驟：1)將約1 sccm之HCDS的脈衝引入至反應腔室中歷時10秒，2)藉由55 sccm之Ar清除HCDS前驅物歷時30秒，3)將約1 sccm之BDEAS的脈衝引入至反應腔室中歷時10秒，4)藉由55 sccm之Ar清除BDEAS前驅物歷時30秒，5)將約50 sccm之NH3 的脈衝引入至反應腔室中歷時10秒，及6)藉由55 sccm之Ar清除NH3 反應物歷時10秒。重複序列1)至6)，直至沈積層達成合適之層厚度為止。
圖8中展示沈積薄膜之沈積速率及折射率。所得薄膜中之矽的原子組成百分比為約45%，所得薄膜中之氮的原子組成百分比為約30%，且碳之原子組成百分比為約20%。所得薄膜中之氯及氧每一者的原子組成百分比為0%或更大但小於5%。所得薄膜由HF溶液蝕刻之濕式蝕刻速率為0.54埃/分鐘。
實施例4c
使用ALD方法藉由HCDS及BDEAS前驅物來沈積緻密的SiCN薄膜。反應腔室被控制在5托、550℃下，且55 sccm之Ar連續地流動。沈積製程包含以下步驟：1)將約1 sccm之BDEAS的脈衝引入至反應腔室中歷時10秒，2)藉由55 sccm之Ar清除BDEAS前驅物歷時30秒，3)將約1 sccm之HCDS的脈衝引入至反應腔室中歷時10秒，及4)藉由55 sccm之Ar清除HCDS前驅物歷時30秒。重複序列1)至4)，直至沈積層達成合適之層厚度為止。
所得薄膜之碳含量過高以致不允許藉由橢圓對稱法來量測沈積速率及折射率。所得薄膜中之矽的原子組成百分比大於55%但小於60%，所得薄膜中之碳的原子組成百分比大於30%但小於35%，且氮之原子組成百分比稍微大於5%。所得薄膜中之氯及氧每一者的原子組成百分比為0%或更大但小於5%。所得薄膜由HF溶液蝕刻之濕式蝕刻速率為0.15埃/分鐘。
實施例5
申請者咸信，將使用所揭示之ALD方法藉由HfCl4 及3DMAS前驅物來沈積緻密的HfSiCN薄膜。申請者咸信，所揭示方法可用以更改所得薄膜中之化學計量比。
實施例6
申請者咸信，將使用所揭示之ALD方法藉由肆(乙基甲基胺基)鉿及HCDS前驅物來沈積緻密HfSiCN薄膜。申請者咸信，所揭示方法可用以更改所得薄膜中之化學計量比。
應理解，可在如附加申請專利範圍中所表達的本發明之原理及範疇內藉由熟習此項技術者進行在細節、材料、步驟及部件之配置方面的許多額外改變(其在本文中已被描述及說明以便解釋本發明之本質)。因此，本發明不欲限於上文所給出的實施例及/或附圖中之特定具體實例。
圖1為展示根據所揭示方法使用參(二甲基胺基)矽烷(3DMAS)及六氯二矽烷(HCDS)所沈積的SiCN薄膜之沈積速率及折射率對薄膜距入口之距離的曲線圖；
圖2為展示根據所揭示方法之一替代方法使用3DMAS及HCDS所沈積的SiCN薄膜之沈積速率及折射率對距離的曲線圖；
圖3為展示根據所揭示方法之第二替代方法使用3DMAS及HCDS所沈積的SiCN薄膜之沈積速率及折射率對距離的曲線圖；
圖4為展示根據所揭示方法使用肆(二甲基胺基)矽烷(4DMAS)及六氯二矽烷(HCDS)所沈積的SiCN薄膜之沈積速率及折射率對薄膜距入口之距離的曲線圖；
圖5為展示根據所揭示方法之一替代方法使用4DMAS及HCDS所沈積的SiCN薄膜之沈積速率及折射率對距離的曲線圖；
圖6為展示根據所揭示方法之第二替代方法使用4DMAS及HCDS所沈積的SiCN薄膜之沈積速率及折射率對距離的曲線圖；
圖7為展示根據所揭示方法使用雙(二乙基胺基)矽烷(BDEAS)及六氯二矽烷(HCDS)所沈積的SiCN薄膜之沈積速率及折射率對薄膜距入口之距離的曲線圖；及
圖8為展示根據所揭示方法之一替代方法使用BDEAS及HCDS所沈積的SiCN薄膜之沈積速率及折射率對距離的曲線圖。

Claims (4)

  1. 一種形成含氮化物之薄膜之方法，該方法包含以下步驟：a)控制ALD反應器在自約200℃至約600℃之溫度範圍內；b)將六氯二矽烷引入至含有至少一基板之該ALD反應器中；c)將多餘六氯二矽烷自該反應器清除；d)將雙(二乙基胺基)矽烷引入至該反應器中；e)將多餘雙(二乙基胺基)矽烷自該反應器清除；f)將NH3 引入至該反應器中；及g)將多餘NH3 自該反應器清除。
  2. 如申請專利範圍第1項之方法，其中變化該方法步驟(b)至(g)的次序產生具有指定化學計量之SiCN薄膜。
  3. 一種形成SiCN薄膜之方法，該方法包含以下步驟：a)控制ALD反應器在自約200℃至約600℃之溫度範圍內；b)將六氯二矽烷引入至含有至少一基板之該ALD反應器中；c)將多餘六氯二矽烷自該反應器清除；d)將肆(二甲基胺基)矽烷引入至該反應器中；e)將多餘肆(二甲基胺基)矽烷自該反應器清除；f)將NH3 引入至該反應器中，及g)將多餘NH3 自該反應器清除。
  4. 如申請專利範圍第3項之方法，其中變化該方法步驟(b)至(g)的次序產生具有指定化學計量之SiCN薄膜。
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