CN104080944A - 用于ald/cvd含硅薄膜应用的有机硅烷前体 - Google Patents
用于ald/cvd含硅薄膜应用的有机硅烷前体 Download PDFInfo
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Abstract
本发明公开了含Si薄膜形成前体、其合成方法及使用其以使用气相沉积法沉积含硅薄膜用于制造半导体、光伏装置、LCD-TFT、平板型装置、耐火材料或航空材料的方法。
Description
相关申请的交互引用
本申请主张2012年7月20日申请的美国临时申请第61/674,103号的优先权,该申请的全部内容引入本文供参考。
技术领域
公开含Si薄膜形成前体、其合成方法及使用其以使用气相沉积法沉积含硅薄膜用于制造半导体、光伏装置、LCD-TFT、平板型装置、耐火材料或航空材料的方法。
现有技术
含Si薄膜广泛用于半导体、光伏装置、LCD-TFT、平板型装置、耐火材料或航空行业中。含Si薄膜可例如用作具有电学性质的可绝缘的介电材料(SiO2、SiN、SiCN、SiCOH、MSiOx,其中M为Hf、Zr、Ti、Nb、Ta或Ge且x大于零),含Si薄膜可用作导电薄膜,如金属硅化物或金属硅氮化物。由于电学装置架构朝向纳米级(尤其低于28nm节点)降低尺寸所施加的严格要求,需要愈来愈精细调节的分子前体,这些分子前体除具有高沉积速率、所产生薄膜的保形性及坚实度以外也满足挥发性(对于ALD制程)、较低制程温度、与各种氧化剂的反应性及低薄膜污染的要求。
熟知硅烷(SiH4)可用于热CVD。然而,此分子具自燃性,由此使得此室温气体在安全处理方面面临挑战。已使用采用卤代硅烷(如二氯硅烷SiH2Cl2)的CVD方法。然而,这些方法可能需要较长吹扫时间,造成薄膜的卤素污染及粒子形成(由氯化铵盐形成),且甚至破坏某些基质,从而引起不希望的界面层形成。以烷基部分地替代卤素可得到一些改进,但代价是薄膜内产生不利的碳污染。
有机氨基硅烷已用作含Si薄膜的CVD的前体。Dussarrat等人的US7192626报导了使用三硅烷胺N(SiH3)3来沉积SiN薄膜。其他已报导的前体包括二异丙氨基硅烷[SiH3(NiPr2)]及类似SiH3(NR2)化合物(参见例如Thridandam等人的US 7875312)以及苯基甲基氨基硅烷[SiH3(NPhMe)]及相关经取代的硅烷苯胺(参见例如Xiao等人的EP 2392691)。
另一相关类别的用于含Si薄膜的CVD的Si前体由通式(R1R2N)xSiH4-x给出,其中x在1与4之间且R取代基独立地为H、C1-C6直链、分支链或环状碳链(参见例如Dussarrat等人的WO2006/097525)。
Hunks等人在US2010/0164057中公开诸多含Si前体,包括具有式R4-xSiLx的硅化合物,其中x为具有1-3的值的整数;R可选自H、分支链和未分支链C1-C6烷基、C3-C8环烷基和C6-C13芳基;且L可选自异氰酸酯基、甲基乙基酮肟、三氟乙酸酯、三氟甲磺酸酯、酰氧基、β-二酮亚胺(β-diketiminate)、β-二-亚胺(β-di-iminate)、脒、胍、烷氨基、氢化物、烷氧化物或甲酸酯配位体。Pinnavaia等人主张了一种由乙酰基丙酮酸硅和1,3-二酮硅(silicon 1,3-diketonate)前体制备多孔合成半结晶有机-无机杂合氧化硅组成物的方法(US6465387)。
尽管有诸多选择可用于含Si薄膜的沉积,但仍不断寻找其他前体以为装置工程师提供调节制造制程要求及达成具有所要电学和物理性质的薄膜的能力。
记法和命名法
贯穿以下说明书及申请专利范围使用某些缩写、符号和术语,且包括:
如本文所用,不定冠词“一(a/an)”意谓一个(种)或多个(种)。
如本文所用,术语“独立地”在用于描述R基团的情形中时应理解为表示所述R基团不仅相对于带有相同或不同下标或上标的其他R基团独立地选择,还相对于同一R基团的任何其他种类独立地选择。举例而言,在式MR1 x(NR2R3)(4-x)(其中x为2或3)中,两个或三个R1基团可但无需彼此或与R2或R3相同。另外,应了解,除非另外特定陈述,否则当用于不同式子中时R基团的值彼此独立。
如本文所用,术语“烷基”指排他性地含有碳和氢原子的饱和官能基。另外,术语“烷基”指直链、分支链或环状烷基。直链烷基的实例包括但不限于甲基、乙基、丙基、丁基等。分支链烷基的实例包括但不限于叔丁基。环状烷基的实例包括但不限于环丙基、环戊基、环己基等。
如本文所用,术语“芳基”指已自环中移除一个氢原子的芳环化合物。如本文所用,术语“杂环”指环状化合物,其具有至少两种不同元素的原子作为其环的成员。
如本文所用,缩写“Me”指甲基;缩写“Et”指乙基;缩写“Pr”指任何丙基(即正丙基或异丙基);缩写“iPr”指异丙基;缩写“Bu”指任何丁基(正丁基、异丁基、叔丁基、仲丁基);缩写“tBu”指叔丁基;缩写“sBu”指仲丁基;缩写“iBu”指异丁基;缩写“Ph”指苯基;缩写“Am”指任何戊基(异戊基、仲戊基、叔戊基);缩写“Cy”指环状烷基(环丁基、环戊基、环己基等);且缩写“R-amd”指R-N-C(Me)-N-R脒配位体,其中R为烷基(例如iPr-amd为iPr-N-C(Me)-N-iPr)。
如本文所用,首字母缩写词“SRO”表示氧化锶钌薄膜;首字母缩写词“HCDS”表示六氯二硅烷;且首字母缩写词“PCDS”表示五氯二硅烷。
本文使用元素周期表的元素的标准缩写。应了解,可用这些缩写来指代元素(例如Si指硅,N指氮,O指氧,C指碳等)。
附图简述
为了进一步理解本发明的性质和目的,应结合附图参考以下详细说明,其中相似组件由相同或类似参考编号指定且其中:
图1为热解重量分析(TGA)图,其显示SiH3(NiPr-amd)和SiH3(NtBu-amd)与DiPAS(二异丙基氨基硅烷)相比在温度变化下的重量损失百分比;且
图2为显示前体引入时间对比沉积速率和折射率的图。
发明内容
公开具有下式的有机硅烷分子:
其中R1和R2可各自独立地为H、C1-C6烷基或C3-C20芳基或杂环基且R3可为H、C1-C6烷基或C3-C20芳基或杂环基、氨基、烷氧基或卤素;
·R1与R2和/或R2与R3连接以形成环状链;
·有机硅烷分子具有下式:
其中R1和R2可各自独立地为C1-C6烷基;
·有机硅烷分子为H3Si(NiPr-amd);
·有机硅烷分子具有下式:
其中R1、R2、R3和R4可各自独立地为H、C1-C6烷基或C3-C20芳基或杂环;
·有机硅烷分子为H3Si(-(iPr)N-C(NMe2)-N(iPr)-);
·有机硅烷分子具有下式:
其中R1、R2和R3可各自独立地为H、C1-C6烷基或C3-C20芳基或杂环;
·有机硅烷分子为H3Si(-(iPr)N-C(OMe)-N(iPr)-);
·有机硅烷分子具有下式:
其中R1和R2可各自独立地为H、C1-C6烷基或C3-C20芳基或杂环;且X可为Cl、Br、I或F;且
·有机硅烷分子为H3Si(-(iPr)N-C(Cl)-N(iPr)-)。
还公开具有下式的含Si薄膜形成前体:
其中R1和R2可各自独立地为H、C1-C6烷基或C3-C20芳基或杂环基且R3可为H、C1-C6烷基、C3-C20芳基或杂环基、氨基、烷氧基或卤素;
·R1与R2和/或R2与R3连接以形成环状链;
·含Si薄膜形成前体具有下式:
其中R1和R2可各自独立地为C1-C6烷基;
·含Si薄膜形成前体为H3Si(NiPr-amd);
·含Si薄膜形成前体具有下式:
其中R1、R2、R3和R4可各自独立地为H、C1-C6烷基或C3-C20芳基或杂环;
·含Si薄膜形成前体为H3Si(-(iPr)N-C(NMe2)-N(iPr)-);
·含Si薄膜形成前体具有下式:
其中R1、R2和R3可各自独立地为H、C1-C6烷基或C3-C20芳基或杂环;且
·含Si薄膜形成前体为H3Si(-(iPr)N-C(OMe)-N(iPr)-);
·含Si薄膜形成前体具有下式:
其中R1和R2可各自独立地为H、C1-C6烷基或C3-C20芳基或杂环;且X可为Cl、Br、I或F;且
·含Si薄膜形成前体为H3Si(-(iPr)N-C(Cl)-N(iPr)-)。
还公开在基底上沉积含Si层的方法。
以上公开的至少一种有机硅烷前体引入其中安置有至少一个基底的反应器中。使用气相沉积法将至少一部分有机硅烷前体沉积至至少一个基底上以形成含Si层。所公开的方法可具有以下方面中的一种或多种:
·向反应器中引入包含至少一种第二前体的蒸气;
·至少一种第二前体的元素选自:第2族、第13族、第14族、过渡金属、镧系元素及其组合;
·至少一种第二前体的元素选自Mg、Ca、Sr、Ba、Zr、Hf、Ti、Nb、Ta、Al、Si、Ge、Y或镧系元素;
·向反应器中引入至少一种共反应物;
·共反应物选自:O2、O3、H2O、H2O2、NO、NO2、羧酸、其自由基及其组合;
·共反应物为经等离子处理的氧气;
·共反应物为臭氧;
·含Si层为氧化硅层;
·共反应物选自:H2、NH3、(SiH3)3N、氢化硅烷(如SiH4、Si2H6、Si3H8、Si4H10、Si5H10、Si6H12)、氯硅烷和氯聚硅烷(如SiHCl3、SiH2Cl2、SiH3Cl、Si2Cl6、Si2HCl5、Si3Cl8)、烷基硅烷(如Me2SiH2、Et2SiH2、MeSiH3、EtSiH3)、肼(如N2H4、MeHNNH2、MeHNNHMe)、有机胺(如NMeH2、NEtH2、NMe2H、NEt2H、NMe3、NEt3、(SiMe3)2NH)、吡唑啉、吡啶、含B分子(如B2H6、9-硼双环[3,3,1]壬烷、三甲基硼、三乙基硼、硼吖嗪(borazine))、烷基金属(如三甲基铝、三乙基铝、二甲基锌、二乙基锌)、其自由基物质及其混合物。
·共反应物选自:H2、NH3、SiH4、Si2H6、Si3H8、SiH2Me2、SiH2Et2、N(SiH3)3、其氢自由基及其混合物;
·共反应物经等离子处理;
·共反应物经远程等离子处理;
·共反应物不经等离子处理;
·共反应物为H2;
·共反应物为NH3;
·共反应物为HCDS;
·共反应物为PCDS;
·共反应物为四氯硅烷;
·共反应物为三氯硅烷;
·共反应物为六氯环六硅烷;
·气相沉积法为化学气相沉积法;
·气相沉积法为原子层沉积(ALD)法;
·气相沉积法为空间ALD法;
·含硅层为Si;
·含硅层为SiO2;
·含硅层为SiN;
·含硅层为SiON;
·含硅层为SiCN;且
·含硅层为SiCOH。
实施方式
公开了含Si薄膜形成前体、其合成方法及使用其以使用气相沉积法沉积含硅薄膜用于制造半导体、光伏装置、LCD-TFT、平板型装置、耐火材料或航空材料的方法。
所公开的有机硅烷前体具有下式:
脒
其中R1和R2可各自独立地为H、C1-C6烷基或C3-C20芳基或杂环基且R3可为H、C1-C6烷基、C3-C20芳基或杂环基、氨基、烷氧基或卤素。R1及R2和/或R2及R3可连接以形成环状链。
如该式中所说明,氮原子键结于硅原子,从而产生五配位Si(IV)中心。二齿单阴离子配位体的主链中的碳原子为sp2杂化,从而在配位体上产生非定域电荷。氮和碳原子可各自独立地经H、C1-C6烷基、芳基或杂环基取代。
所公开的有机硅烷前体由于硅原子处的超配位而可能比其他R4-xSiLx前体更具反应性。换言之,尽管硅原子为+IV,但三个氢键和单阴离子螯合配位体与硅原子形成总共5个键。
本领域技术人员应认识到使用氢或任何R基团中具有较少碳原子的烷基、芳基或杂环基(即H、C1或C2)与具有含较多碳(即C4+)的烷基、芳基或杂环基的分子相比将产生具有较高挥发性的分子。由于其在-N-C-N-配位体上的两个氮原子的氮含量增加,这些分子可用于产生还含有氮的含硅薄膜,如SiN、SiCN、SiON、MSiN或MSiON,其中M为如Hf、Zr、Ti、Nb、Ta或Ge的元素,或用于调节彼等薄膜中的氮的量。
当R3为Me时,所得前体为具有下式的含有脒的化合物:
其中R1和R2可各自独立地为H、C1-C6烷基或C3-C20芳基或杂环基。优选地,R1和R2各独立地为C1-C6烷基。
脒前体可如下合成:通过将SiXH3(其中X为Cl、Br、I或三氟甲磺酸根(SO3CF3 -))的烃溶液与纯配位体化合物(如Li[R1NC(R2)NR3]或Li(amd))或其烃溶液在氮气氛围下组合,混合烧瓶的出口与油起泡器连接以抑制空气及水分回流。
获得所公开的脒前体的第二合成途径为通过在惰性氛围下使质子化配位体(R1N=C(R2)-NRH3)与纯二烷基氨基硅烷[SiH3(NR2)]或其烃溶液反应。
或者,所公开的脒前体可如下合成:通过SiHnCl4-n与单一当量的配位体化合物(即Li[R1NC(R2)NR3]或Li(amd))反应,随后使用所选金属氢化物(如LAH(氢化锂铝))还原。
在所有三个合成途径中,可在室温下搅拌所得溶液过夜。适合于这些合成方法的例示性烃溶液包括乙醚、戊烷、己烷或甲苯。过滤所得悬浮液且蒸馏所得溶液以移除溶剂。分别通过蒸馏或升华来纯化所得液体或固体。除了配位体化合物Li(amd),所有起始材料均可在市面上购得。配位体化合物可通过将有机金属盐(即烷基锂)的烃溶液与适当碳化二亚胺(即R1N=C=NR3)的烃溶液组合来合成。其他合成细节提供于实施例中。
例示性脒前体包括:
优选地,脒前体为SiH3(NiPr-amd)。
当R3为氨基(即NR3R4)时,所得前体为具有下式的含有胍的化合物:
胍
其中R1、R2、R3和R4可各自独立地为H、C1-C6烷基、C3-C20芳基或杂环。由于其与其他分子相比时氮含量增加,这些分子可用于产生还含有氮的含硅薄膜(如SiN或SiON),或用于调节含有SiN或SiON的薄膜中的氮的量。
胍前体可如下合成:通过将SiXH3(其中X为Cl、Br、I或三氟甲磺酸根(SO3CF3 -))的烃溶液与纯配位体化合物(如Li[R1NC(NR3R4)NR2](或Li(gnd)))或其烃溶液在氮气氛围下组合,混合烧瓶的出口与油起泡器连接以抑制空气及水分回流。
获得所公开的胍前体的第二合成途径为通过在惰性氛围下使质子化配位体(R1N=C(NR3R4)-NR2H)与纯二烷基氨基硅烷[SiH3(NR2)]或其烃溶液反应。
或者,所公开的胍前体可如下合成:通过SiHnCl4-n与单一当量的配位体化合物(即Li[R1NC(NR3R4)NR2]或Li(gnd))反应,随后使用所选金属氢化物(如LAH(氢化锂铝))还原。
在所有三个合成途径中,可在室温下搅拌所得溶液过夜。适合于这些合成方法的例示性烃溶液包括乙醚、戊烷、己烷或甲苯。过滤所得悬浮液且蒸馏所得溶液以移除溶剂。分别通过蒸馏或升华来纯化所得液体或固体。除了配位体化合物Li(gnd),所有起始材料均可在市面上购得。配位体化合物可通过将有机金属盐(即氨基锂-Li(NR3R4))的烃溶液与适当碳化二亚胺(即R1N=C=NR2)的烃溶液组合来合成。
例示性胍前体包括:
优选地,胍前体为H3Si(-(iPr)N-C(NMe2)-N(iPr)-)。
当R3为烷氧基(即OR3)时,所得前体为具有下式的含有异脲的化合物:
异脲
其中R1、R2和R3可各自独立地为H、C1-C6烷基或C3-C20芳基或杂环。
由于其与其他分子相比时氧含量增加,这些分子可用于产生还含有氧的含硅薄膜(如SiO2或SiON),或用于调节含有SiO2或SiON的薄膜中的氧的量。
异脲前体可如下合成:通过将SiXH3(其中X为Cl、Br、I或三氟甲磺酸根(SO3CF3-))的烃溶液与纯配位体化合物(如Li[R1NC(OR3)NR2](或Li(iso)))或其烃溶液在氮气氛围下组合,混合烧瓶的出口与油起泡器连接以抑制空气和水分回流。
获得所公开的异脲前体的第二合成途径为通过在惰性氛围下使质子化配位体(R1N=C(OR3)-NR2H)与纯二烷基氨基硅烷[SiH3(NR2)]或其烃溶液反应。
或者,所公开的异脲前体可如下合成:通过SiHnCl4-n与单一当量的配位体化合物(即Li[R1NC(OR3)NR2]或Li(iso))反应,随后使用所选金属氢化物(如LAH(氢化锂铝))还原。
在所有三个合成途径中,可在室温下搅拌所得溶液过夜。适合于这些合成方法的例示性烃溶液包括乙醚、戊烷、己烷或甲苯。过滤所得悬浮液且蒸馏所得溶液以移除溶剂。分别通过蒸馏或升华来纯化所得液体或固体。除了配位体化合物Li(iso),所有起始材料均可在市面上购得。配位体化合物可通过将有机金属盐(即烷醇锂-Li(OR3))的烃溶液与适当碳化二亚胺(即R1N=C=NR2)的烃溶液组合来合成。
例示性异脲前体包括:
优选地,异脲前体为H3Si(-(iPr)N-C(OMe)-N(iPr)-)。
当R3为卤素(即X)时,所得前体为具有下式的含有α-卤基脒的化合物:
α-卤基脒
其中R1和R2可各自独立地为H、C1-C6烷基或C3-C20芳基或杂环且X可为Cl、Br、I或F。卤素原子可改进非晶硅的原子层沉积的保形性。
α-卤基脒前体可如下合成:通过组合经双取代的脲衍生物R1HN-(C=O)-NHR2的烃溶液与O=CX2的烃溶液,如Neubauer等人所述(Chemische Berichte,1964,97(5),1232-1245)。添加一摩尔当量的适当碱(如六甲基二硅烷氨基钾)的烃溶液至反应混合物中,且过滤所得悬浮液以移除金属盐副产物。所得溶液可与SiRH3反应,其中R为苯基、甲苯基或其他适当芳基取代基。所得混合物可通过分馏纯化。适合于这些合成方法的例示性烃溶液包括乙醚、戊烷、己烷或甲苯。所有起始材料均可在市面上购得。
例示性α-卤基脒前体包括:
优选地,α-卤基脒为H3Si(-(iPr)N-C(Cl)-N(iPr)-)。
还公开使用所公开的有机硅烷前体进行气相沉积法的方法。所公开的方法提供有机硅烷前体用于沉积含硅薄膜的用途。所公开的方法可适用于制造半导体、光伏装置、LCD-TFT或平板型装置。该方法包括:提供基底;提供包括所公开的有机硅烷前体中的至少一种的蒸气;及使蒸气与基底接触(且典型地将蒸气导引至基底)以在基底的至少一个表面上形成含硅层。
所公开的方法还可使用气相沉积法在基底上形成含双金属层且更特定言之沉积SiMOx薄膜,其中x为4且M为Ta、Hf、Nb、Mg、Al、Sr、Y、Ba、Ca、As、Sb、Bi、Sn、Pb、Co、镧系元素(如Er)或其组合。所公开的方法可适用于制造半导体、光伏装置、LCD-TFT或平板型装置。该方法包括:提供基底;提供包括所公开的有机硅烷前体中的至少一种的蒸气且使蒸气与基底接触(且典型地将蒸气导引至基底)以在基底的至少一个表面上形成含双金属的层。如O3、O2、H2O、NO、H2O2、乙酸、福尔马林、三聚甲醛、其氧自由基及其组合但优选O3或经等离子处理的O2的氧源也可与蒸气一起提供。
所公开的有机硅烷前体可用于使用本领域熟练技术人员已知的任何沉积方法沉积含硅薄膜。适合沉积方法的实例包括但不限于已知化学气相沉积(CVD)、低压化学气相沉积(LPCVD)、原子层沉积(ALD)、脉冲式化学气相沉积(P-CVD)、热ALD、热CVD、等离子增强式原子层沉积(PE-ALD)、等离子增强式化学气相沉积(PE-CVD)、空间ALD或其组合。优选地,沉积方法为ALD、空间ALD或PE-ALD。
将有机硅烷前体蒸气引入含有至少一个基底的反应室中。反应室内的温度和压力以及基底的温度保持在适合于将至少一部分有机硅烷前体气相沉积至基底上的条件下。换言之,在将汽化前体引入腔室中之后,腔室内的条件使得至少一部分汽化前体沉积至基底上以形成含硅薄膜。共反应物也可用于帮助形成含Si层。
反应室可为装置中进行沉积方法的任何封闭区域或腔室,如但不限于平行板型反应器、冷壁型反应器、热壁型反应器、单晶圆反应器、多晶圆反应器或其他此种类型的沉积体系。所有这些例示性反应室均能够充当ALD反应室。反应室可维持在约0.5毫托至约20托范围内的压力下。此外,反应室内的温度可在约20℃至约600℃范围内。本领域技术人员应认识到可仅经由实验来优化温度以达成所要结果。
可通过控制基底固持器的温度或控制反应器壁的温度来控制反应器温度。用于加热基底的装置为本领域中已知。将反应器壁加热至足以获得处于充足生长速率下且具有所要物理状态和组成的所要薄膜的温度。可将反应器壁加热至的非限制性例示性温度范围包括约20℃至约600℃。当使用等离子沉积法时,沉积温度可在约20℃至约550℃范围内。或者,当执行热制程时,沉积温度可在约300℃至约600℃范围内。
或者,可将基底加热至足以获得处于充足生长速率下且具有所要物理状态和组成的所要含硅薄膜的温度。可将基底加热至的非限制性例示性温度范围包括150℃至600℃。优选地,基底温度保持低于或等于500℃。
上面将沉积含硅薄膜的基底的类型将视预期的最终用途而不同。在一些具体实施方案中,基底可为由氢化碳(例如CHx,其中x大于零)制成的图案化光阻薄膜。在一些具体实施方案中,基底可选自在MIM、DRAM或FeRam技术中用作介电材料的氧化物(例如基于ZrO2的材料、基于HfO2的材料、基于TiO2的材料、基于稀土氧化物的材料、基于三元氧化物(ternary oxide)的材料等)或选自用作铜与低k层之间的氧障壁的基于氮化物的薄膜(例如TaN)。可使用其他基底来制造半导体、光伏装置、LCD-TFT或平板装置。此类基底的实例包括但不限于固体基底,如含有金属氮化物的基底(例如TaN、TiN、WN、TaCN、TiCN、TaSiN和TiSiN);绝缘体(例如SiO2、Si3N4、SiON、HfO2、Ta2O5、ZrO2、TiO2、Al2O3和钛酸钡锶);或包括这些材料的多种组合的其他基底。所使用的实际基底也可视所使用的特定前体具体实施方案而定。但在许多情况下,所使用的优选基底将选自氢化碳、TiN、SRO、Ru和Si型基底,如多晶硅或结晶硅基底。
所公开的有机硅烷前体可以纯形式或以与适合溶剂(如甲苯、乙苯、二甲苯、均三甲苯、癸烷、十二烷、辛烷、己烷、戊烷、叔胺、丙酮、四氢呋喃、乙醇、乙基甲基酮、1,4-二烷或其他溶剂)的掺混物形式供应。所公开的前体可以不同浓度存在于溶剂中。举例而言,所得浓度可在约0.05M至约2M范围内。
纯的或掺混的有机硅烷前体通过已知构件(如管道和/或流量计)以蒸气形式引入反应器中。可通过经由已知汽化步骤(如直接汽化、蒸馏、通过鼓泡或通过使用升华器(如Xu等人的PCT公开案WO2009/087609中所公开的升华器))使纯的或掺混的前体溶液汽化来产生呈蒸气形式的前体。纯的或掺混的前体可以液态装至汽化器中,在该汽化器中其经汽化随后将其引入反应器中。或者,可通过将载气通入含有前体的容器中或通过使载气鼓泡至前体中来使纯的或掺混的前体汽化。载气可包括但不限于Ar、He或N2及其混合物。用载气鼓泡也可移除存在于纯的或掺混的前体溶液中的任何溶解氧。接着,载气及前体以蒸气形式引入反应器中。
必要时,可将容器加热至允许有机硅烷前体呈其液相且具有充足蒸气压的温度。容器可维持在例如0-150℃范围内的温度下。本领域熟练技术人员认识到可以已知方式调节容器的温度以控制汽化的有机硅烷前体的量。
除所公开的前体以外,反应气体(即共反应物)也可引入反应器中。反应气体可为氧化剂,如以下中的一种:O2;O3;H2O;H2O2;含氧自由基,如O·或OH·;NO;NO2;羧酸,如甲酸、乙酸、丙酸;NO、NO2或羧酸的自由基物质;三聚甲醛;及其混合物。优选地,氧化剂选自:O2、O3、H2O、H2O2、其含氧自由基(如O·或OH·)及其混合物。优选地,当执行ALD制程时,共反应物为经等离子处理的氧气、臭氧或其组合。当使用氧化气体时,所得含硅薄膜也将含有氧。
或者,反应气体可为还原剂,如以下中的一种:H2、NH3、(SiH3)3N、氢化硅烷(如SiH4、Si2H6、Si3H8、Si4H10、Si5H10、Si6H12)、氯硅烷和氯聚硅烷(如SiHCl3、SiH2Cl2、SiH3Cl、Si2Cl6、Si2HCl5、Si3Cl8)、烷基硅烷(如(CH3)2SiH2、(C2H5)2SiH2、(CH3)SiH3、(C2H5)SiH3)、肼(如N2H4、MeHNNH2、MeHNNHMe)、有机胺(如N(CH3)H2、N(C2H5)H2、N(CH3)2H、N(C2H5)2H、N(CH3)3、N(C2H5)3、(SiMe3)2NH)、吡唑啉、吡啶、含B分子(如B2H6、9-硼双环[3,3,1]壬烷、三甲基硼、三乙基硼、硼吖嗪)、烷基金属(如三甲基铝、三乙基铝、二甲基锌、二乙基锌)、其自由基物质及其混合物。优选地,还原剂为H2、NH3、SiH4、Si2H6、Si3H8、SiH2Me2、SiH2Et2、N(SiH3)3、其氢自由基或其混合物。当使用还原剂时,所得含硅薄膜可为纯Si。
反应气体可经等离子处理,以便使反应气体分解成其自由基形式。当经等离子处理时N2也可用作还原剂。举例而言,可产生功率在约50W至约500W、优选约100W至约200W范围内的等离子。等离子可产生或存在于反应器自身内。或者,等离子可通常处于移离反应器的位置处,例如在远程定位的等离子体系中。本领域熟练技术人员将想到适合于该等离子处理的方法及装置。
所公开的有机硅烷前体也可与卤代硅烷或聚卤代硅烷(如六氯二硅烷、五氯二硅烷或四氯二硅烷)及一种或多种共反应物气体一起使用,以形成SiN或SiCN薄膜,如PCT公开案第WO2011/123792号中所公开,该公开案的全部内容引入本文供参考。
当所要含硅薄膜还含有另一元素(如但不限于Ta、Hf、Nb、Mg、Al、Sr、Y、Ba、Ca、As、Sb、Bi、Sn、Pb、Co、镧系元素(如Er)或其组合)时,共反应物可包括含金属前体,其选自但不限于金属烷基,如Ln(RCp)3或Co(RCp)2;金属胺,如Nb(Cp)(NtBu)(NMe2)3;及其任何组合。
有机硅烷前体及一种或多种共反应物可同时(化学气相沉积)、相继(原子层沉积)或以其他组合形式引入反应室中。举例而言,有机硅烷前体可在一次脉冲中引入且两种其他金属来源可在独立脉冲中一起引入[改进的原子层沉积]。或者,反应室在引入有机硅烷前体之前可能已含有共反应物。可使共反应物通过定位于反应室远程的等离子体系,且分解成自由基。或者,有机硅烷前体可连续引入反应室中,而其他金属来源通过脉冲引入(脉冲式化学气相沉积)。在各实施例中,可在脉冲之后进行吹扫或抽空步骤以移除所引入的过量组分。在各实施例中,脉冲可持续约0.01s至约10s,或者约0.3s至约3s,或者约0.5s至约2s范围内的时间。在另一替代方案中,有机硅烷前体及一种或多种共反应物可同时自淋浴喷头喷洒,在该淋浴喷头下固持若干晶圆的基座旋转(空间ALD)。
在一个非限制性例示性原子层沉积型制程中,有机硅烷前体的气相引入反应室中,在该反应室中其与适合基底接触。接着,可通过吹扫和/或抽空反应室来自反应室中移除过量有机硅烷前体。将氧源引入反应室中,在该反应室中其与所吸收的有机硅烷前体以自限制方式反应。通过吹扫和/或抽空反应室自反应室中移除任何过量氧源。若所要薄膜为氧化硅薄膜,则此两步制程可提供所要膜厚度或可重复直至已获得具有必需厚度的薄膜。
或者,若所要薄膜为硅金属氧化物薄膜(即SiMOx,其中x可为4且M为Ta、Hf、Nb、Mg、Al、Sr、Y、Ba、Ca、As、Sb、Bi、Sn、Pb、Co、镧系元素(如Er)或其组合),则可在以上两步制程之后将含金属前体的第二蒸气引入反应室中。含金属前体将基于所沉积的硅金属氧化物薄膜的性质来选择。在引入反应室中之后,含金属前体与基底接触。通过吹扫和/或抽空反应室自反应室中移除任何过量含金属前体。再次,可将氧源引入反应室中以与含金属前体反应。通过吹扫和/或抽空反应室自反应室中移除过量氧源。若已达成所要膜厚度,则制程可终止。然而,若需要较厚薄膜,则可重复整个四步骤制程。通过交替提供有机硅烷前体、含金属前体及氧源,可沉积具有所要组成及厚度的薄膜。
另外,通过改变脉冲次数,可获得具有所要化学计量M:Si比率的薄膜。举例而言,通过进行一次有机硅烷前体的脉冲及一次含金属前体的脉冲,且在各脉冲之后进行氧源的脉冲可获得SiMO2薄膜。然而,本领域技术人员应认识到为获得所要薄膜所需的脉冲次数可能不等于所得薄膜的化学计量比率。
在另一替代方案中,可经由ALD或改进的ALD制程使用所公开的化合物及具有式SiaH2a+2-bXb(其中X为F、Cl、Br或I;a=1至6;且b=1至(2a+2))的卤代硅烷化合物;或具有式-SicH2c-dXd-(其中X为F、Cl、Br、或I;c=3-8;且d=1至2c)的环状卤代硅烷化合物沉积Si或致密SiCN薄膜。优选地,卤代硅烷化合物为三氯硅烷、六氯二硅烷(HCDS)、五氯二硅烷(PCDS)、四氯二硅烷或六氯环六硅烷。本领域技术人员应认识到当必需为较低沉积温度时这些化合物中的Cl可经Br或I取代,此归因于Si-X键的较低键能(即Si-Cl=456kJ/mol;Si-Br=343kJ/mol;Si-I=339kJ/mol)。必要时,沉积可进一步使用含N反应物,如NH3。所公开的前体及卤代硅烷化合物的蒸气可视所要的最终薄膜浓度而相继或同时引入反应器。所选前体注入顺序将基于所要目的薄膜组成来确定。可重复前体引入步骤直至沉积层达成适合厚度。本领域技术人员应认识到当使用空间ALD装置时引导性脉冲(introductory pulse)可为同时的。如PCT公开案第WO2011/123792号中所描述,可改变前体引入顺序且可在存在或不存在NH3共反应物下执行沉积,以便调节SiCN薄膜中碳和氮的量。
由上文所论述的制程产生的含硅薄膜可包括Si、SiN、SiON、SiCN、SiCOH或MSiOx,其中M为如Hf、Zr、Ti、Nb、Ta或Ge的元素,且x可为4,当然视M的氧化态而定。本领域技术人员应认识到通过慎重选择适当有机硅烷前体和共反应物,可获得所要薄膜组成。
获得所要膜厚度后,可对薄膜进行进一步处理,如热退火、炉退火、快速热退火、UV或电子束固化和/或等离子气体暴露。本领域熟练技术人员可想到用于执行这些额外加工步骤的系统和方法。举例而言,含硅薄膜可在惰性氛围、含H氛围、含N氛围、含O氛围或其组合下暴露于约200℃至约1000℃范围内的温度,持续约0.1秒至约7200秒范围内的时间。最优选地,温度为400℃,在含H氛围下持续3600秒。所得薄膜可含有较少杂质,且因此可具有改进的效能特性。可在执行沉积制程的同一反应室中执行退火步骤。或者,可自反应室中移除基底,且在独立装置中执行退火/急骤退火制程。已发现以上后处理方法中的任一种、尤其热退火可有效减少含硅薄膜的碳和氮污染。
实施例
提供以下非限制性实施例以进一步说明本发明的具体实施方案。然而,这些实施例并不意欲包括所有且并不意欲限制本文所述的发明范畴。
实施例1
SiH3(NiPr-amd)的合成:在搅拌下,将甲基锂的乙醚溶液(91mL,1.6M,0.146mol)缓慢添加至N,N'-二异丙基碳化二亚胺(22.5mL,0.145mol)于乙醚(150mL)中的-40℃溶液中。添加完成后,使所得无色悬浮液升温至室温且搅拌三小时以形成无色溶液。在装备有-78℃(干冰/丙酮)冷凝器的独立烧瓶中装入乙醚(100mL)且冷却至-78℃。在搅拌下,一氯甲硅烷(13.2g,0.198mol)缓慢冷凝至第二烧瓶中,随后缓慢添加来自第一步骤的脒基锂溶液。最初观察到一定程度的发烟,随后形成无色沉淀。完成添加后,在剧烈搅拌过夜下使悬浮液缓慢达至室温。经含有硅藻土垫的中等玻璃粉过滤悬浮液且在大气压下使用维格罗管柱(Vigreux column)蒸馏所得无色溶液以移除溶剂。更换接收烧瓶且在-78℃浴中冷却,在25-28℃/200-300毫托下蒸馏得到呈无色液体状的所需产物。产量:7.9g(31.6%)。图1为显示此前体与DiPAS相比在温度变化下的重量损失百分比的TGA图。29Si NMR(80MHz,C6D6,25℃)δ(ppm)=-87.7;1H NMR(400MHz,C6D6,25℃)δ(ppm)=4.73(s,3H,SiH3),3.38(sept.,2H,1JH-H=8.0Hz,NCH(CH3)2),1.40(s,3H,CCH3),1.12(d,12H,1JH-H=8.0Hz,NCH(CH3)2)。
实施例2
SiH3(NtBu-amd)的合成:在装备有-78℃(干冰/丙酮)冷凝器的烧瓶中装入乙醚(100mL)且冷却至-78℃。在搅拌下,一氯甲硅烷(8.9g,0.134mol)缓慢冷凝至烧瓶中。在第二烧瓶中,将甲基锂的乙醚溶液(101mL,1.6M,0.162mol)缓慢添加至N,N'-二-叔丁基碳化二亚胺(25g,0.162mol)于乙醚(100mL)中的-40℃溶液中。添加完成后,使所得脒基锂无色悬浮液升温至室温且搅拌一小时以形成无色溶液。将所得Li-amd溶液冷却至0℃且由套管添加至一氯甲硅烷(MCS)于乙醚中的-78℃溶液中。最初观察到一定程度的发烟,随后形成无色沉淀。完成添加后,在剧烈搅拌下使悬浮液达至室温。
停止搅拌,且使固体沉降随后经具有硅藻土床的中等玻璃粉过滤。将所得无色溶液转移至含有干燥Amberlyst A21树脂(5g)的烧瓶中,略微搅拌且使其在室温下静置14小时。接着,过滤溶液且在大气压下使用短程管柱蒸馏以移除溶剂和高挥发物,从而得到高黏性浅黄色液体。更换接收烧瓶且冷却至-78℃,在55-61℃/100毫托下蒸馏得到呈无色液体状的所需产物,其在室温下静置之后缓慢结晶。产量:14.5g(54.1%)。MP=36℃,29SiNMR(80MHz,C6D6,25℃)δ(ppm)=-117.5;1H NMR(400MHz,C6D6,25℃)δ(ppm)=5.05(s,3H,SiH3),1.79(s,3H,CCH3),1.25(s,9H,NC(CH3)3)。
实施例3
SiH3(NiPr-amd)的ALD:使用实施例1中制备的SiH3(NiPr-amd)执行ALD测试,将该SiH3(NiPr-amd)置放于室温下的容器中。使用典型ALD条件,如在固定于约0.5托的反应器压力下使用臭氧。如图2中所示,在275℃下在纯硅晶圆上评估完全表面饱和及反应情况下的ALD特性。本领域技术人员应认识到不同沉积设备可在不同前体引入时间展现表面饱和。折射率为SiO2薄膜的特性(纯SiO2的折射率为1.46)。由前体引入时间变化引起的折射率变化指示薄膜中的杂质。
应了解,在如所附申请专利范围中所表述的本发明原理和范畴内,本领域熟练技术人员可对本文中已描述且说明以便解释本发明的性质的细节、材料、步骤和部件配置作出许多其他改变。因此,本发明并不意欲限于以上所提供的实施例和/或附图中的特定具体实施方案。
Claims (14)
1.一种含Si薄膜形成前体,其具有下式:
其中R1和R2可各自独立地为H、C1-C6烷基或C3-C20芳基或杂环基且R3可为H、C1-C6烷基、C3-C20芳基或杂环基、氨基、烷氧基或卤素。
2.根据权利要求1的含Si薄膜形成前体,其具有下式:
其中R1和R2可各自独立地为C1-C6烷基。
3.根据权利要求2的含Si薄膜形成前体,其中分子为SiH3(NiPr-amd)。
4.根据权利要求1的含Si薄膜形成前体,其具有下式:
其中R1、R2、R3和R4可各自独立地为H、C1-C6烷基或C3-C20芳基或杂环。
5.根据权利要求1的含Si薄膜形成前体,其具有下式:
其中R1、R2和R3可各自独立地为H、C1-C6烷基或C3-C20芳基或杂环。
6.根据权利要求1的含Si薄膜形成前体,其具有下式:
其中R1和R2可各自独立地为H、C1-C6烷基或C3-C20芳基或杂环且X可为Cl、Br、I或F。
7.一种在基底上沉积含Si层的方法,所述方法包括:
将至少一种根据权利要求1-6中任一项的有机硅烷前体引入其中安置有至少一个基底的反应器中;
使用气相沉积法将至少一部分有机硅烷前体沉积至至少一个基底上以形成含Si层。
8.根据权利要求7的方法,其进一步包含向反应器中引入至少一种共反应物。
9.根据权利要求8的方法,其中共反应物选自:O2、O3、H2O、H2O2、NO、NO2、羧酸、其自由基及其组合,优选经等离子处理的氧气或臭氧。
10.根据权利要求8的方法,其中共反应物选自:H2、NH3、(SiH3)3N、氢化硅烷(如SiH4、Si2H6、Si3H8、Si4H10、Si5H10、Si6H12)、氯硅烷和氯聚硅烷(如SiHCl3、SiH2Cl2、SiH3Cl、Si2Cl6、Si2HCl5、Si3Cl8)、烷基硅烷(如Me2SiH2、Et2SiH2、MeSiH3、EtSiH3)、肼(如N2H4、MeHNNH2、MeHNNHMe)、有机胺(如NMeH2、NEtH2、NMe2H、NEt2H、NMe3、NEt3、(SiMe3)2NH)、吡唑啉、吡啶、含B分子(如B2H6、9-硼双环[3,3,1]壬烷、三甲基硼、三乙基硼、硼吖嗪)、烷基金属(如三甲基铝、三乙基铝、二甲基锌、二乙基锌)、其自由基物质及其混合物。
11.根据权利要求10的方法,其中共反应物选自:H2、NH3、SiH4、Si2H6、Si3H8、SiH2Me2、SiH2Et2、N(SiH3)3、其氢自由基及其混合物。
12.根据权利要求10的方法,其中共反应物选自:SiHCl3、Si2Cl6、Si2HCl5、Si2H2Cl4和环-Si6H6Cl6。
13.根据权利要求7的方法,其中气相沉积法为化学气相沉积法。
14.根据权利要求7的方法,其中气相沉积法为原子层沉积法。
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US9371338B2 (en) | 2016-06-21 |
KR20150036114A (ko) | 2015-04-07 |
TW201412762A (zh) | 2014-04-01 |
TW201410690A (zh) | 2014-03-16 |
US20150166577A1 (en) | 2015-06-18 |
KR20150036122A (ko) | 2015-04-07 |
JP6242026B2 (ja) | 2017-12-06 |
US20150166576A1 (en) | 2015-06-18 |
JP2015528011A (ja) | 2015-09-24 |
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US9938303B2 (en) | 2018-04-10 |
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