TWI506157B - 含矽薄膜的電漿增強的循環性化學氣相沈積方法 - Google Patents

含矽薄膜的電漿增強的循環性化學氣相沈積方法 Download PDF

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TWI506157B
TWI506157B TW097106379A TW97106379A TWI506157B TW I506157 B TWI506157 B TW I506157B TW 097106379 A TW097106379 A TW 097106379A TW 97106379 A TW97106379 A TW 97106379A TW I506157 B TWI506157 B TW I506157B
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oxygen
plasma
substrate
group
chemical vapor
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TW097106379A
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TW200837213A (en
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Hareesh Thridandam
Manchao Xiao
Xinjian Lei
Thomas Richard Gaffney
Eugene Joseph Karwacki
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Air Prod & Chem
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Description

含矽薄膜的電漿增強的循環性化學氣相沈積方法 相關申請的相互引用
本申請要求於2007年2月27日提交的美國臨時專利申請No.60/903,734的優先權。
本發明公開了電漿增強循環性化學氣相沈積氮化矽、碳氮化矽、氧氮化矽、碳氧氮化矽和摻碳的氧化矽的方法。
電子裝置製造業已經把氮化矽、碳氮化矽和氧氮化矽的化學氣相沈積(CVD)、循環性化學氣相沈積(CCVD)或原子層沈積(ALD)用於製造積體電路中。該工業應用的實例包括：US 2003/0020111；US 2005/0048204 A1；US 4720395；US 7,166,516；Gumpher,J.,W.Bather,N.Mehta和D.Wedel.“Characterization of Low-Temperature Silicon Nitride LPCVD from Bis(tertiary-butylamino)silane and Ammonia.”Journal of The Electrochemical Society 151 (5)：(2004)G353-G359；US 2006/045986；US 2005/152501；US 2005/255714；US 7,129,187；US 2005/159017；US 6,391,803；US 5,976,991；US 2003/0059535；US 5,234,869；JP2006-301338；US 2006/087893；US 2003/26083；US 2004/017383；US 2006/0019032；US 2003/36097；US 2004/044958；US 6,881,636；US 6,963,101； US2001/0000476；和US2005/129862。如下所述，本發明提供在基材上將含矽膜如氮化矽、碳氮化矽、氧氮化矽和摻碳的氧化矽的CVD或ALD的現有工業方法的改進。
本發明是將含矽膜如氮化矽、碳氮化矽、氧氮化矽和摻碳的氧化矽沈積到基材上的方法。
本發明的實施方式之一是將氮化矽、碳氮化矽、氧氮化矽和碳氧氮化矽沈積到半導體基材上的方法，包括：a.在遠距電漿(remote plasma)條件下使含氮源與加熱的基材相接觸以在所述加熱的基材上吸收至少一部分含氮源，b.清除任何未吸收的含氮源，c.使所述加熱的基材與具有一個或多個Si-H3 片段的含矽源接觸以與所吸收的含氧源反應，其中所述含矽源含有選自以下組中的一個或多個H3 Si-NR0 2 (R0 =SiH3 ,R,R1 或R2 ，定義如下)基團，該組包括一種或多種的： 其中，式中的R和R1 代表具有2-10個碳原子的脂族基團，其中式A中的R和R1 也可以是環狀基團，且R2 選自單鍵、(CH2 )n 、環或SiH2 ，和 d.清除未反應的含矽源。
本發明的另一實施方式是將氧氮化矽、碳氧氮化矽和摻碳的氧化矽沈積到半導體基材上的方法，包括：a.在遠距電漿條件下使含氧源與加熱的基材相接觸以在所述加熱的基材上吸收至少一部分含氧源，b.清除任何未吸收的含氧源，c.使所述加熱的基材與具有一個或多個Si-H3 片段的含矽源接觸以與所吸收的含氧源反應，其中所述含矽源含有選自以下組中的一個或多個H3 Si-NR0 2 (R0 =SiH3 ,R,R1 或R2 ，定義如下)基團，該組包括一種或多種： 其中，式中的R和R1 代表具有2-10個碳原子的脂族基團，其中式A中的R和R1 也可以是環狀基團，且R2 選自單鍵、(CH2 )n 、環或SiH2 ，和d.清除未反應的含矽源。
本發明公開了由含有Si-H3 的烷胺基矽烷，優選式(R1 R2 N)SiH3 (其中R1 和R2 獨立地選自C2 -C10 )以及氮源(優選氨)進行電漿增強循環性化學氣相沈積氮化矽、碳氮化矽、氧氮化矽、碳氧氮化矽和摻碳的氧化矽的方法，使得膜與由熱化學氣相沈積獲得的膜相比具有改進的特 性，例如蝕刻速率、氫濃度和應力。或者，該方法可按照原子層沈積(ALD)、電漿輔助原子層沈積(PAALD)、化學氣相沈積(CVD)、低壓化學氣相沈積(LPCVD)、電漿增強化學氣相沈積(PECVD)或旋轉塗布沈積(Spin on deposition)(SOD)來進行。
電漿增強循環性化學氣相沈積氮化矽、碳氮化矽、氧氮化矽和碳氧氮化矽的典型循環示於圖1中。
遠距電漿室是Advanced Energy Industries公司製造的Litmas RPS。Litmas RPS是結合有固態RF功率輸出系統的圓柱形感應電漿源(石英室)。水冷線圈捲繞在室的周圍，為室提供冷卻並形成RF天線。頻率操作範圍在1.9MHz-3.2MHz。DC輸出功率範圍為100W-1500W。
ALD系統是Cambridge NanoTech公司製造的Savannah 100。ALD反應器是陽極化鋁且容納有100mm的矽基材。ALD反應器具有包埋的盤形加熱部件，其從底部加熱的基材。也有包埋在反應器壁內的管式加熱器。前驅物閥總管包封在加熱器中，加熱封套用於加熱前驅物容器。在前驅物閥總管中的ALD閥是三通閥，可向ALD反應器中連續地供給10-100sccm的惰性氣體。
氮化矽、碳氮化矽、氧氮化矽和碳氧氮化矽的沈積方法描述如下。
在方法的第一步驟中，安裝在沈積室上游約12英寸處的遠距電漿室內產生氨電漿(ammonia plasma)，並以預定體積流速、預定的時間供應到沈積室中。通常，通過開啟 遠距電漿頭和ALD反應器之間的門閥(gate valve)，經0.1-80秒的一段時間將氨電漿供給到ALD室中以使氨自由基被充分的吸附，使得基材表面飽和。沈積過程中，供給到遠距電漿室入口的氨的流速通常在1-100 sccm範圍內。電漿室中的PF功率在100W-1500W之間變化。沈積溫度是傳統的，範圍約200-600℃，對原子層沈積來說優選200-400℃，對循環性化學氣相沈積來說優選400-600℃。示例性的壓力從50 mtorr-100 torr。此外，氨中其他的含氮源能夠是氮、肼、單烷基肼、二烷基肼和其混合物。
在方法的第二步驟中，惰性氣體如Ar、N2 或He可用於從室中吹掃未反應的氨自由基。通常在循環沈積方法中，氣體如Ar、N2 或He以10-100 sccm的流速供入到室中，從而清除留在室中的氨自由基和任何的副産品。
在方法的第三步驟中，有機胺基矽烷諸如二乙基胺基矽烷(DEAS)、二異丙基胺基矽烷(DIPAS)、二第三丁基胺基矽烷(DTBAS)、二第二丁基胺基烷基、二第三戊基胺基矽烷和其混合物以預定摩爾體積(例如1-100微摩爾)、以預定一段時間(優選約0.005-10秒)導入到室中。矽前驅物與吸附在基材表面上的氨自由基反應導致氮化矽的形成。使用了傳統的沈積溫度200-500℃和壓力50 mtorr-100 torr。
在方法的第四步驟中，用惰性氣體如Ar、N2 或He從室中吹掃未反應的有機胺基矽烷。通常在循環沈積方法中，氣體如Ar、N2 或He以10-100 sccm的流速供入到室中， 從而清除留在室中的有機胺基矽烷和任何的副產品。
上述的四個方法步驟包括典型的ALD過程循環。該ALD過程循環重複若干次直到獲得所需的膜厚度。
圖2顯示了基材溫度爲400℃時的典型ALD飽和曲線。
電漿增強循環性化學氣相沈積氧氮化矽和摻碳的氧化矽的典型循環示於圖3中。
在方法的第一步驟中，安裝在沈積室上游約12英寸處的遠距電漿室內產生氧電漿(oxygen plasma)，並以預定體積流速、預定的時間供應到沈積室中。通常，通過開啟遠距電漿頭和ALD反應器之間的門閥，經0.1-80秒的一段時間將氧電漿供給到ALD室中以使含氧自由基被充分地吸附，使得基材表面飽和。沈積過程中，供給到遠距電漿室入口的氧流速通常在1-100 sccm範圍內。電漿室中的RF功率在100W-1500W之間變化。沈積溫度是傳統的，範圍約200-600℃，對原子層沈積來說優選200-400℃，對循環性化學氣相沈積來說優選400-600C。示例性的壓力從50 mtorr-100 torr。除氧以外，其他含氧源可以是臭氧、一氧化二氮和它們的混合物。
在方法的第二步驟中，惰性氣體如Ar、N2 或He可用於從室中吹掃未反應的含氧自由基。通常在循環沈積方法中，氣體如Ar、N2 或He以10-100 sccm的流速供入到室中，從而清除留在室中的含氧自由基和任何的副産品。
在方法的第三步驟中，有機胺基矽烷諸如二乙基胺基矽烷(DEAS)、二異丙基胺基矽烷(DIPAS)、二第三丁基胺 基矽烷(DTBAS)、二第二丁基胺基烷基、二第三戊基胺基矽烷和其混合物以預定摩爾體積(例如1-100微摩爾)、以一段預定時間(優選約0.005-10秒)導入到室中。矽前驅物與吸附在基材表面上的含氧自由基反應導致氧化矽的形成。使用了傳統的沈積溫度200-500℃和壓力50 mtorr-100 torr。
在方法的第四步驟中，用惰性氣體如Ar、N2 或He從室中吹掃未反應的有機胺基矽烷。通常在循環沈積方法中，氣體如Ar、N2 或He以10-100 sccm的流速供入到室中，從而清除留在室中的有機胺基矽烷和任何的副產品。
上述四個方法步驟包括ALD過程循環。該ALD過程循環重複若干次直到獲得所需的膜厚度。
實施例1
在將ALD反應器抽到～40mT真空度以下並用10 sccm的N2 清潔後，在ALD反應器中導入所述矽前驅物和NH3 。在溫度400℃進行沈積。遠距電漿也可用於降低所需的沈積溫度。在導入到反應器之前，將所述矽前驅物在加熱套包封的水浴瓶(bubbler)中預熱到40℃。結果總結在表1中。
由於在一次沈積期間僅使用極少量的化合物，所以來自水浴瓶的所述矽前驅物的流速(每單位時間量)在給定溫度下被認爲是恒定的。因此，加入ALD反應器中的所述矽前驅物的量與用於導入所述矽前驅物的脈衝時間成線性比 例。
從表1中可以看出，即使在沈積溫度和氮前驅物的數量保持相同時，形成氮化矽膜的速率隨著加入到反應器中所述矽前驅物的量的變化而變化。
同樣從表1中可以看出，當其他處理條件保持相同時，隨著所述矽前驅物的脈衝時間(或量)從0.01秒增加到0.05秒，形成氮化矽膜的速率開始從0.156A/循環增加。然而，隨後即使加入更多矽前驅物後，速率幾乎保持不變。這表明使用Si前驅物形成的膜確實是ALD膜。
實施例2
使用FTIP對所沈積的ALD膜進行分析。膜的FTIP光譜示於圖4中。從圖4中可以看出，1046cm-1 處存在有吸收峰，表明膜中存在氧化物。3371處的峰是N-H伸展(stretch)(有一些O-H)且在接近1130cm-1 的肩部具有相 應的搖擺(rock)。2218峰來自Si-H且其寬的形狀表明是低應力的膜。813的峰接近Si-N。沈積膜的EDX分析也證實了膜中Si和N的存在。
上述列出的包括試驗實施例的本發明的實施方式是對本發明所作的許多實施方式的示例。可以構想的是，可使用許多其他配置的方法並且方法中所用材料可選自除具體公開的那些以外的許多材料。簡言之，本發明已經針對特別的實施方式進行了闡述，但本發明的整個保護範圍應該由所附的權利要求加以確定。
圖1是典型的用於氮化矽、碳氮化物、氧氮化矽和碳氧氮化矽的電漿增強循環性化學氣相沈積的流程圖。
圖2是在下述PEALD試驗條件下DIPAS的沈積速率與脈衝時間圖：電漿功率為1.39kW的5sccm的NH3 、10sccm的吹掃氣體N2 、基材溫度400℃、不銹鋼容器中的DIPAS為40℃。
圖3是典型的用於氧氮化矽和摻碳的氧化矽的電漿增強循環性化學氣相沈積的流程圖。
圖4是實施例1所述的膜的FTIP光譜並在實施例2中進行討論。

Claims (5)

  1. 一種將氧氮化矽、碳氧氮化矽和摻碳的氧化矽沈積到半導體基材上的方法，其為電漿增強循環性化學氣相沈積法，包括：a.使含有含氧自由基的含氧電漿與加熱的基材相接觸一段脈衝時間以在所述加熱的基材上吸收至少一部分含氧自由基，其中該含氧電漿係在相對該基材的一遠距位置被產生；b.清除任何未被吸收的含氧自由基，c.使所述加熱的基材與具有一個或多個Si-H3 片段的含矽源接觸一段脈衝時間以與所吸收的含氧自由基反應，其中所述含矽源選自二異丙基胺基矽烷(DIPAS)、二第三丁基胺基矽烷(DTBAS)、二第二丁基胺基烷基、二第三戊基胺基矽烷和它們的混合物所組成的群組；及d.清除未反應的含矽源。
  2. 如申請專利範圍第1項所述的方法，其中，重複所述方法直到形成所需厚度的膜。
  3. 如申請專利範圍第1項所述的方法，其為原子層沈積法。
  4. 如申請專利範圍第1項所述的方法，其中，所述的基材溫度範圍為200-600℃。
  5. 如申請專利範圍第1項所述的方法，其中，所述含氧自由基藉由使一含氧氣體接受電漿能源而產生，其中該含氧氣體選自氧、一氧化二氮、臭氧和它們的混合物所組成的群組。
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