TW201736261A - 經摻雜之組成物及其製造方法與用途 - Google Patents

經摻雜之組成物及其製造方法與用途 Download PDF

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TW201736261A
TW201736261A TW105141072A TW105141072A TW201736261A TW 201736261 A TW201736261 A TW 201736261A TW 105141072 A TW105141072 A TW 105141072A TW 105141072 A TW105141072 A TW 105141072A TW 201736261 A TW201736261 A TW 201736261A
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史蒂芬 楚勞特
歐朵 溫尼克
麥瑟斯 帕茲
米利安 梅爾契
哈洛德 史都格
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贏創德固賽有限責任公司
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Abstract

本發明係關於包含至少一種通式SinHm(其中n□5且m=(2n)及(2n+2))之氫矽烷及至少一種式HnB(OR)3-n(其中R=C1-C10-烷基、C6-C10-芳基、C7-C14-芳烷基、鹵素，n=0、1、2)之化合物的組成物；其製備方法及其用途。

Description

經摻雜之組成物及其製造方法與用途
本發明係關於經摻雜之組成物、其製造方法、及其用途。
特別是對於半導體工業，含矽層的製造是令人感興趣的。含矽層可在真空室中自氣相沉積，例如經由PECVD。然而，氣相法係技術複雜且經常無法產生所欲品質的層。為此，對於含矽層的製造，液相法經常是較佳的。
為此，可用來經由液相法製造含矽層之組成物是令人大感興趣的。
在本上下文中，令人感興趣的不僅是用於製造本質(即未摻雜)含矽層的液相法。特別是用於製造p或n型摻雜之含矽層、製造經摻雜之含矽層的方法及用於其中之組成物是令人感興趣的。
關於製造p型摻雜，尤其是經硼摻雜，之含矽層，已有多種可用於此目的之液相法及組成物。舉例而 言，US 5,866,471 A揭示製造p型摻雜之含矽層的方法，其中將未摻雜之塗覆組成物施加到基板上並在含p型摻雜物氛圍的存在下轉化成經摻雜之含矽層。然而，此方法的不利之處在於它非常複雜，尤其是在設備方面。
US 5,866,471 A另亦揭示製造經摻雜之含矽層的純液相法，其中將包含摻雜物和含矽前驅物之調配物施加到基板上，並接著轉化成半導體層。然而，所使用的摻雜物係摻雜物之烷基化/芳基化化合物(例如BPh3、BMePh2或B(t-Bu)3)，或是在矽原子和摻雜物原子之間具有鍵結的化合物(例如B(SiMe3)3、PhB(SiMe3)2或Cl2B(SiMe3)。然而，前者化合物由於該等化合物的烷基/芳基而導致不利的含碳層。所提到的後者化合物非為商業上可獲得的並因此必須先以複雜的方式合成。再者，若彼等係經烷基化/芳基化，則其由於已提到的原因是不利的。
EP 1 715 509 B1及EP 1 085 579 A1亦揭示製造經摻雜之含矽層的方法，其中使用了包含式SiaXbYc(其中Y可為硼原子)之化合物的組成物。然而，這些化合物亦必須先以複雜的方式合成。
EP 1 640 342 A1及EP 1 357 154 A1揭示矽形成(silicon-forming)組成物，其可包含矽烷聚合物及有機溶劑以及隨意地含有第3主族之元素(其中之一為硼)的物質。說明性化合物為那些在JP 2000-031066 A中具體指明的化合物，即B2H6、B4H10、B5H9、B6H10、B10H14、 B(CH3)3、B(C2H5)3、及B(C6H5)3。然而，如同已陳述的，對應的烷基化或芳基化硼化合物會導致不利的含碳層。使用所提到的硼烷因為其高毒性是額外不利的。
US 2008/0022897 A1尤其亦揭示矽形成組成物，其可包含摻雜物來源。所描述的含硼摻雜物可為含硼雜環矽烷化合物或其他具有硼-矽鍵之化合物，其具有已描述之必須先以複雜方式合成的不利之處。亦揭示了含氫烷基化、芳基化或芳烷基化硼化合物，彼等因其已被提及之毒性，或是因其導致含碳層之傾向，故而是不利的。
DE 10 2010 040 231 A1另描述適於製造p型摻雜之含矽層且包含矽化合物及至少一種來自氫硼化劑之組群的化合物(其可為BH3與選自由THF、NR3及SR‘2所組成組群之錯合劑的錯合物)之調配物。然而，由於所提到的化合物之介穩性，無法確保受控添加該等摻雜物。
因此本發明所提出的課題係避免先前技藝的缺點。更特定而言，本發明所提出的課題係提供包含摻雜物之調配物，以該調配物，即可獲得且穩定的低毒性化合物亦可用來有效地製造無碳含矽層。
因此所提出的課題係令人驚訝地藉由本發明之組成物來解決，該組成物包含至少一種通式SinHm(其中n5且m=(2n)至(2n+2))之氫矽烷，以及至少一種式HnB(OR)3-n(其中R=C1-C10-烷基、C6-C10-芳基、C7-C14- 芳烷基、鹵素，n=0、1、2)之化合物，其相應地被稱為硼酸酯、亞硼酸酯或次硼酸酯類之衍生物，又有時在文獻中亦被稱為單、二或三烷氧基硼烷或硼酸酯類。
通式SinHm之氫矽烷在m=2n的情況下為環狀氫矽烷，而在m=2n+2的情況下為直鏈或支鏈氫矽烷。製備氫矽烷的方法是熟習此項技術者已知的。存在於根據本發明之組成物中的氫矽烷另具有至少5個Si原子，即n5。
氫矽烷是由矽和氫原子所組成並具有優於含碳有機矽烷或含氫和碳有機矽烷的優點：彼等在轉化時反應產生沉積矽(隨意地帶有有益於電子性質之殘餘氫含量)及氣態氫，而沒有碳含量。
氫矽烷之含量，以總調配物為基準計，可為0.1重量%至99重量%，較佳為1重量%至30重量%。
有利的是，根據本發明之氫矽烷為可由至少一種通式SixH2x+2(其中x3)之氫矽烷或通式SixH2x(其中x5)之環狀氫矽烷製備之氫矽烷寡聚物，較佳的是可由直鏈或支鏈氫矽烷製備之氫矽烷寡聚物。氫矽烷寡聚物被理解為意指可由具有相對較低分子量之氫矽烷經由寡聚合而製備的氫矽烷。氫矽烷寡聚物因此亦為氫矽烷。
可能以特別有效的方式使用相應的通式SixH2x+2(其中x3)之直鏈或支鏈氫矽烷，藉由熱途徑，來製備可有利地使用的氫矽烷。更佳而言，該氫矽烷可經由包含基本上至少一種式SixH2x+2(其中x3-20)之氫矽 烷作為氫矽烷的組成物，在無催化劑的存在下，於低於235℃的溫度下熱寡聚合而得到。相應之製備這些化合物的方法係揭示於WO 2011/104147 A1。這些化合物典型地具有290至5000g/mol之重量平均分子量(經由GPC對照聚苯乙烯標準物測量)。可能藉由根據本發明之方法，以特別有效的方式，製備特別適合用於根據本發明之組成物且具有重量平均分子量為500-3500g/mol之氫矽烷寡聚物。
具有特別好的適用性之組成物為那些包含已藉由熱方法由支鏈氫矽烷，最佳由Si(SiH3)4(新五矽烷)，所製備之通式SinHm之氫矽烷的組成物。
然而，可有利地使用之通式SinHm之氫矽烷亦可由通式SixH2x(其中x=5)之環狀氫矽烷(環五矽烷)製備。
該組成物進一步包含至少一種式HnB(OR)3-n(其中R=C1-C10-烷基、C6-C10-芳基、C7-C14-芳烷基、鹵素；n=0、1、2)之化合物。相應化合物為隨意經烷基化、芳基化、芳烷基化、鹵化及/或氫化之硼酸酯、亞硼酸酯或次硼酸酯類。
迄今並不知道硼酸酯、亞硼酸酯或次硼酸酯類可用於摻雜，因為認為其中所存在的氧對產生的層之電子性質具有不利的影響。DE 695 05 268 T2揭示了在至少一種硼化合物(其亦可包含經烷基取代之硼酸衍生物)的存在下，從聚烷基氫矽烷及/或聚芳基氫矽烷製造基於碳化 矽之陶瓷材料的方法。然而，其中所描述的方法及所揭示的為了製造陶瓷材料之組成物並不適合用於製造半導體工業之含矽層。因此已令人驚訝地發現，該穩定的硼酸酯、亞硼酸酯或次硼酸酯類係適合作為所界定之用於含矽層之摻雜的起始化合物，並導致相應之適用於半導體工業之含矽層的良好導電性。
硼酸酯、亞硼酸酯或次硼酸酯類之含量，以總調配物為基準計，有利地為0.0001重量%至20重量%，較佳為0.001重量%至10重量%，且更佳為0.01重量%至5重量%。
最佳的通式HnB(OR)3-n之化合物為化合物HnB(O(n-Bu))3-n(其中n=1、2)。此等化合物導致可用各組成物製備之含矽層具有非常特別好的電子性質。
通式HnB(OR)3-n(其中R=C1-C10-烷基、C6-C10-芳基、C7-C14-芳烷基、鹵素，n=0、1、2)之相應的硼酸酯、亞硼酸酯或次硼酸酯類可商業上購得，或是，例如，以受控的方式原位從適合的前驅化合物製備。
適合用於原位製備硼酸酯、亞硼酸酯或次硼酸酯類之前驅化合物為BH3、B2H6與通式RHC=O之醛類、通式RR'C=O之酮類、通式R-O-R'之醚類(其中R、R‘=C1-C10-烷基、C6-C10-芳基、C7-C14-芳烷基)、或是基於烷基或芳族基礎骨架之鄰或1,2二醇(例如2,3-二甲基丁烷-2,3-二醇、兒茶酚)併用；較佳為與通式(CH2)nO(n=2-10)之環狀醚類併用，且最佳為與四氫呋喃(CH2)4O併 用。
根據本發明之組成物可僅由所提到的氫矽烷及所提到的硼酸酯、亞硼酸酯或次硼酸酯類組成，或是還具有進一步的成分。
為了達成有利的性質，其較佳包含進一步的成分。
因此，該組成物較佳包含至少一種溶劑。較佳的溶劑為脂族和芳族烴。進一步較佳的是來自由下列所組成之組群的溶劑：具有1至12個碳原子之直鏈、支鏈及環狀，飽和、不飽和及芳族烴(隨意地經部分或全部鹵化)、醇類、醚類、羧酸類、酯類、腈類、胺類、醯胺類、亞碸類及水。特佳的是正戊烷、正己烷、正庚烷、正辛烷、正癸烷、十二烷、環己烷、環辛烷、環癸烷、二環戊烷、苯、甲苯、間二甲苯、對二甲苯、對稱三甲苯、茚烷、茚、四氫萘、十氫萘、二乙基醚、二丙基醚、乙二醇二甲基醚、乙二醇二乙基醚、乙二醇甲基乙基醚、二乙二醇二甲基醚、二乙二醇二乙基醚、二乙二醇甲基乙基醚、四氫呋喃、對二烷、乙腈、二甲基甲醯胺、二甲亞碸、二氯甲烷及氯仿。
為了達成有利的性質，以總調配物為基準計，溶劑之比例可為0.1重量%至99.9重量%，較佳為25重量%至95重量%。
尤其是當具有重量平均分子量為290-5000g/mol之氫矽烷係可經由包含基本上至少一種式SixH2x+2 (其中x3-20)之氫矽烷作為氫矽烷的組成物，在無催化劑的存在下，於低於235℃的溫度下熱寡聚合而得到，在該調配物進一步包含通式SinH2n+2(其中n=5-9)之氫矽烷時，其可能達成具有特別好的性質的層。
通式SinH2n+2(其中n=5-9)之氫矽烷的比例，以所存在之氫矽烷的質量為基準計，較佳為0.1重量%至90重量%，更佳為1重量%至30重量%。
本發明之組成物較佳為適於液相法之塗覆組成物。最佳而言，根據本發明之組成物係印刷油墨。
本發明進一步提供製造根據本發明之組成物的方法，其中將該至少一種氫矽烷、該至少一種通式HnB(OR)3-n之化合物及任何進一步的成分彼此混合。
本發明同樣提供了根據本發明之組成物用於製造含矽層的用途。較佳的是根據本發明之組成物用於製造經摻雜之矽層的用途。尤佳者為根據本發明之組成物用於製造p型摻雜(尤其是經硼摻雜)之矽層的用途。
相應地，本發明同樣提供了製造經摻雜之含矽層(較佳為經摻雜之矽層)的方法，其中將至少一種根據本發明之組成物施加到基板上，並經熱轉化及/或以電磁輻射成經摻雜之含矽層(較佳為矽層)。
根據本發明之組成物係有利地適合在許多種基板上製造含矽層，較佳為經摻雜之矽層。在本發明之上下文中，含矽層被理解為意指不僅是基本上純的矽層，而且還指除了矽之外也包含另外的半導體金屬(例如鍺)的 層；以及另外還有包含氧化矽、碳化矽或氮化矽的層。
較佳之基板由玻璃、石英玻璃、石墨、金屬、氧化矽、矽、或是存在於熱穩定支撐物上之矽、氧化矽、銦錫氧化物、ZnO：F、ZnO：Al或SnO2：F層所組成。較佳之金屬為鋁、不鏽鋼、Cr鋼、鈦、鉻或鉬。亦可能使用例如PEEK、PEN、PET或聚醯亞胺之聚合物膜作為基板。
該組成物較佳係經由選自下列之方法施加：印刷或塗覆法，尤其是快乾/凹版印刷、奈米-或微米壓印、噴墨印刷、平版印刷、數位平版印刷及網版印刷、噴霧法、氣溶膠輔助化學氣相沉積、直接液體注入化學氣相沉積、旋塗法、浸塗法、以及選自彎月面塗覆(meniscus coating)、狹縫塗覆、狹縫式模具塗覆及簾塗覆之方法。
在施加該組成物後以及在轉化之前，可還經塗覆之基板乾燥以移除任何存在的溶劑。為此目的之相應的措施及條件為熟習此項技藝者已知者。為了僅移除溶劑，在加熱乾燥操作的情況中，加熱溫度應低於200℃。
此外，該組成物之初步交聯可在基板上以UV照射進行。
該轉化較佳係在200-1000℃，較佳為250至750℃，尤佳為300至700℃的溫度下進行。在經塗覆基板的熱處理中，轉化係在0.1ms-360min的期間進行。轉化時間較佳係在介於0.1ms和10min之間，尤佳在介於1s和120s之間。
若在各預熱或加溫狀態中需要，此比較快速的高能製程方法可，例如，藉由使用IR燈、加熱板、烘箱、閃光燈、具有不同氣體組成之電漿、RTP系統或微波系統進行。
轉化同樣可藉由以UV光照射來進行。轉化時間較佳可在介於1s和360min之間。
在轉化之後，可例如：以反應性氫藉由熱線法、以含氧電漿(遠距離或直接地在減壓下或大氣壓下)；或是供給氫藉由電暈處理(電暈處理被理解為意指聚合物膜之表面處理方法)，來以氫進行含矽層之富集，其稱為對含矽層中由於未滿足的"懸"鍵所造成之缺陷的"氫鈍化"。或者，如前所述之乾燥及/或轉化可在富集氫的氣氛中進行，使得材料在一開始即富含氫。
所描述之塗覆操作可進行多於一次；同時或隨後沉積，在此情況下，該等膜彼此部分或全部疊置。此外，該基板可經雙面塗覆。
根據本發明之組成物適用於許多用途。其特別好的適合-單獨或與其他成分呈組成物的形式-用於製造電子或光電子含矽成分層。
如同以下實施例1和2及比較例之描述所揭示，上述根據本發明之組成物的使用導致了在所謂無光導電性之技術特徵上的明顯改善。在本發明之上下文中，無光導電性係摻雜品質的測量，作為在各情況中所描述之基板之較低缺陷密度的結果。
值得注意的是根據實施例2所達到的無光導電性，比使用三烷基硼烷衍生物B(Et)3的比較例高出了5個數量級。在實施例2中，與硼酸酯類亦同時一起存在之亞硼酸酯及次硼酸酯類的重要性，其已經由NMR光譜術測量檢測，藉著與實施例1相比而變得清楚明白。在實施例1中，摻雜係僅由硼酸酯B(O-n-Bu)3進行並導致紀錄的無光導電性十倍高於使用三烷基硼烷衍生物B(Et)3的比較例。然而，根據實施例2之經包覆的基板具有的無光導電性，與實施例1相比高出了4個數量級。此技術效果是不可從先前技術預見到的。
以下實施例旨在對本發明之用途提供進一步額外的說明，它們本身不具有任何限制作用：
- 異質發射極太陽能電池
- HIT太陽能電池
- 選擇性發射極太陽能電池
- 背接觸太陽能電池
- 場效電晶體、薄膜電晶體
- 微電子組件中之介電層
- 半導體材料之表面鈍化
所使用的縮寫：
NPS=新五矽烷或四矽基矽烷或Si(SiH3)4
NPO=新五矽烷基矽烷寡聚物
THF=四氫呋喃
RTP=快速熱處理
HIT=帶有本質薄層之異質接面
實施例
實施例1
於1g之NPO(Mw~2200g/mol)中，加入0.124g之B(O-n-Bu)3，並在30℃進行寡聚合180min。將0.1g所產生的p型摻雜之NPO與0.069g之環辛烷及0.161g之甲苯一起調配，然後將該調配物施加到玻璃基板上。在6000rpm之塗覆操作及隨後在500℃/60s之轉化操作中，可能得到152nm之p型摻雜之a-Si層。無光導電性為2×10-7S/cm。
實施例2
將二硼烷(10%於N2中)導入1g之NPS和0.035g之THF的混合物中，並在30℃進行寡聚合一段210min的時間。於0.1g所產生的p型摻雜之NPO中，加入0.05g之環辛烷及0.452g之甲苯。以11B NMR光譜術分析所產生的調配物，並觀察到B(O-n-Bu)3(δ(11B)=19ppm(s))、HB(O-n-Bu)2(δ(11B)=27ppm(d，1JBH=160Hz))、及H2B(O-n-Bu)(δ(11B)=8ppm(t，1JBH=124Hz))。此外，將該調配物施加到玻璃基板上。在2000rpm之塗覆操作及隨後在500℃/60s之轉化操作中，可能得到60nm之p型摻雜之a-Si層。無光導電性為1.1×10-3S/cm。
比較例：
於5g之NPS中，加入2.587g之B(Et)3(1M於THF中)，並在30℃進行寡聚合120min。將0.1g所產生的p型摻雜之NPO與0.05g之環辛烷和0.45g之甲苯一起調配，然後將該調配物施加到玻璃基板上。在6000rpm之塗覆操作及隨後在500℃/60s之轉化操作中，可能得到37nm之p型摻雜之a-Si層。無光導電性為2×10-8S/cm。
實驗：
所有研究均係在M.Braun Inertgas-Systeme GmbH所製造的手套箱中或以標準Schlenk方法學(D.F.Shriver、M.A.Drezdzon，The manipulation of air sensitive compounds，1986，Wiley VCH，New York，USA)，於乾燥氮(N2；O2含量：<10ppm；H2O含量：<10ppm)的惰性氣氛下進行。無水無氧溶劑(環辛烷、甲苯)係藉由M.Braun Inertgas-Systeme GmbH所製造的MB-SPS-800-自動型溶劑乾燥系統製備。氘化苯(C6D6)係來自於Sigma-Aldrich,Coorp.，並且為了乾燥的目的，在使用前於分子篩(4Å)上貯存至少2天。NMR譜係在室溫下以來自Varian有限公司之Varian INOVA 300(11B：96.2MHz)型光譜儀測量。化學位移係與外參考物(BF3*Et2O)比較報導。所描述的調配物係在室溫下組成，然後藉由PE注射器(包含注射器過濾器：1μm)施加到基板(來自Corning有限公司之EagleXG玻璃)上。濕膜係在25℃下 以來自SCS Specialty Coating Systems有限公司之Spincoat G3P-8旋塗器製造。濕膜之轉化係在來自HARRY GESTIGKEIT GmbH之標準實驗室加熱板上進行。層厚度係藉由來自SENTECH Gesellschaft für Sensortechnik mbH之SENpro橢圓偏光計以界定之介於40°和90°之間(5°步)之入射角測量。與所製造的層之接觸連接係藉由用來自Quorum Technologies股份有限公司之Emscope model SC 500型濺射系統施加銀接觸點來達成。測定無光導電性之測量係在25℃下，於N2氣氛中及在密閉金屬容器中之暗處，以來自Keithley Instruments有限公司之兩點測量系統進行。

Claims (10)

  1. 一種組成物，其包含：- 至少一種通式SinHm之氫矽烷- 其中n5且- m=(2n)至(2n+2)，及- 至少一種式HnB(OR)3-n之化合物- 其中R=C1-C10-烷基、C6-C10-芳基、C7-C14-芳烷基、鹵素，- n=0、1、2。
  2. 根據申請專利範圍第1項之組成物，其中該至少一種氫矽烷係可由通式SixH2x+2(其中x3)之氫矽烷或通式SixH2x(其中x5)之環狀氫矽烷製備的氫矽烷寡聚物。
  3. 根據申請專利範圍第2項之組成物，其中該氫矽烷寡聚物可經由包含基本上至少一種式SixH2x+2(其中x3-20)之氫矽烷作為氫矽烷的組成物，在無催化劑的存在下，於低於235℃的溫度下熱寡聚合而得到。
  4. 根據申請專利範圍第3項之組成物，其中該式SixH2x+2之氫矽烷係新五矽烷。
  5. 根據申請專利範圍第2項之組成物， 其中該式SixH2x(其中x5)之氫矽烷係環五矽烷。
  6. 根據申請專利範圍第1項之組成物，其中該式HnB(OR)3-n之化合物具有通式HnB(OC4H9)3-n(其中n=1、2)。
  7. 根據申請專利範圍第1至6項中任一項之組成物，其中其亦包含至少一種溶劑。
  8. 根據申請專利範圍第3項之組成物，其中該調配物進一步包含通式SinH2n+2(其中n=5-9)之氫矽烷。
  9. 一種製備根據申請專利範圍第1至8項中任一項之組成物的方法，其特徵在於將該至少一種氫矽烷、該至少一種通式HnB(OR)3-n之化合物及任何進一步的成分彼此混合。
  10. 一種根據申請專利範圍第1至8項中任一項之組成物的用途，其係用於製造含矽層。
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