CN101848917B - 金属化合物、含有其的化学气相沉积用原料以及含有金属的薄膜的制造方法 - Google Patents
金属化合物、含有其的化学气相沉积用原料以及含有金属的薄膜的制造方法 Download PDFInfo
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- CN101848917B CN101848917B CN2008801147932A CN200880114793A CN101848917B CN 101848917 B CN101848917 B CN 101848917B CN 2008801147932 A CN2008801147932 A CN 2008801147932A CN 200880114793 A CN200880114793 A CN 200880114793A CN 101848917 B CN101848917 B CN 101848917B
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Abstract
本发明涉及一种由下述通式(1)表示的新型金属化合物、含有其的化学气相沉积用原料以及基于使用了该原料的化学气相沉积法的含有金属的薄膜的制造方法。作为该金属化合物,优选下述通式(1)中X为氯原子的化合物,这是因为原料便宜,挥发性高;当M为钛原子时,优选m为1的化合物,这是因为挥发温度(蒸汽温度)与薄膜沉积温度(反应温度)之差较大,可获得较宽的制程范围。下述式中,M表示钛、锆或铪,X表示卤原子,m表示1或2,
Description
技术领域
本发明涉及具有特定的结构的新型金属化合物、含有其的化学气相沉积用原料以及使用了该原料的含有金属的薄膜的制造方法。
背景技术
含有钛、锆或铪的薄膜被用作高电介质电容器、强电介质电容器、门极膜、阻挡膜、门极绝缘膜等电子部件的电子构件或光波导、光开关、光放大器等光通信用设备的光学构件。
作为上述薄膜的制造方法,可以列举出涂布热分解法或凝胶溶胶法等MOD法、CVD法或ALD法等化学气相沉积法等,由于组成控制性、阶梯覆盖性优良、适合于量产化以及能够实现混合集成等具有很多优点,所以CVD法、ALD法等使前体气化后使用的化学气相沉积法是最合适的制造工艺。作为CVD法、ALD法的前体,使用利用了有机配位体的金属化合物。
金属原子为钛、锆或铪的氮化金属系薄膜被作为用于提高切割工具等的的硬度和强度的涂布层、半导体元件的门极薄膜、阻挡膜来使用,并且对于通过化学气相沉积法来制造这些薄膜的技术已有大量报道。
例如,在专利文献1中公开了一种使用了钛、锆、铪、钒、铌或钽的卤化物的氮化金属和/或碳化金属薄膜的制造方法;在专利文献2中公开了一种基于CVD法的氮化钛薄膜的制造方法,在该CVD法中使用了四氯化钛和氨气。
在专利文献3~5中公开了一种含有4族金属的薄膜的制造方法,该制造方法中使用了以有机胺作为配位体的二烷基氨基金属化合物作为钛、锆或铪的前体,并且还公开了使用乙基甲基胺作为有机胺配位体的金属化合物。
但是,在使用以四氯化钛为代表的氯化物的方法中,薄膜形成至少需要500℃左右的温度,在用于门极膜等半导体元件的制造时是不适合的。另外, 以有机胺作为配位体的有机酰胺系金属化合物尽管能够进行低温下的氮化金属薄膜的制造,但由于使用它而得到的薄膜的残留碳成分较多,所以难以实现所期待的电特性,特别是难以作为要求导电性的门极膜、阻挡膜、电极膜来应用。
在专利文献6中公开了一种基于CVD法的氮化钛薄膜的制造方法,在该CVD法中使用了Ti(N(CH3)2)3X、Ti(N(CH3)2)2X2、Ti(N(C2H5)2)3X、Ti(N(C2H5)2)2X2(X为卤原子)。其中公开有,上述钛化合物的热分解性高,能够适宜用作门极薄膜材料。但是,以专利文献6为代表所使用的Ti(N(CH3)2)3Cl是固体,作为CVD材料使用时必须将原料保持在熔点以上的温度。它们的热分解性良好,但热稳定性不良,所以如果为了长时间保持液体状态而加热的话,则有可能分解。另外,如果以固体状态使用,则在挥发量不足、经时变化等原料气体供给性或在线状态下的原料输送方面具有问题,还有颗粒污染的问题。另外,在使用将固体前体溶解于有机溶剂而得到的溶液的溶液CVD法等使用溶液的工艺中,由于气化装置中的温度变化或溶剂的部分挥发、浓度变化而发生固体析出,配管的堵塞等引起的供给量的经时变化或颗粒污染的问题还无法完全解决。
专利文献1:日本特开2003-64475号公报
专利文献2:日本特开平7-201779号公报
专利文献3:韩国专利156980号公报
专利文献4:日本特开2006-45083号公报
专利文献5:日本特开2006-182709号公报
专利文献6:日本特开2000-36473号公报
发明内容
本发明要解决的课题是提供一种金属化合物,该金属化合物能够提供残留碳较少的良好的含有金属的薄膜,并且对于成膜速度或薄膜组成控制能够提供稳定的工艺。此外,本发明中的化学气相沉积用原料只要是没有特别进行区别,则表示CVD用原料或ALD用原料这两者。
本发明者等人经过反复研究,结果发现具有特定的结构的金属化合物能够解决上述课题,从而完成了本发明。
本发明提供一种由下述通式(1)表示的金属化合物。
(式中,M表示钛、锆或铪,X表示卤原子,m表示1或2。)
另外,本发明提供一种化学气相沉积用原料,其含有上述金属化合物。
另外,本发明提供一种含有金属的薄膜的制造方法,其利用了化学气相沉积法,该化学气相沉积法中使用了上述化学气相沉积用原料。
附图说明
图1是表示本发明的薄膜的制造方法中使用的CVD装置的一个例子的概略图。
具体实施方式
以下,根据优选的实施形态详细地说明本发明。
本发明的金属化合物是上述通式(1)表示的新型化合物。
上述通式(1)中,作为X表示的卤原子,可以列举出氟、氯、溴、碘。这些卤原子中,由于原料便宜,挥发性高,因而优选氯。
另外,m为1的化合物的挥发性大于m为2的化合物,m为2的化合物的热分解温度低于m为1的化合物。当作为化学气相沉积用原料来使用时,挥发温度(蒸汽温度)与薄膜沉积温度(反应温度)之差较大的化合物由于可获得较宽的制程范围(process margin),所以容易使用。因此,对于m来说,选择制程范围较大者即可。例如,当M是钛原子时,m为1的金属化合物由于可取得较大的制程范围,因而优选。
X为氯、M为钛时,尽管作为类似的化合物的ClnTi(N(CH3)2)4-n(n为1或2)是在70~95℃的范围内具有熔点的固体,但本发明的金属化合物由于是液体,所以特别适合作为化学气相沉积用原料来使用。
作为本发明的金属化合物的具体例子,可以列举出下述化合物No.1~24。
化合物No.1 化合物No.2 化合物No.3 化合物No.4
化合物No.5 化合物No.6 化合物No.7 化合物No.8
化合物No.9 化合物No.10 化合物No.11 化合物No.12
化合物No.13 化合物No.14 化合物No.15 化合物No.16
化合物No.17 化合物No.18 化合物No.19 化合物No.20
化合物No.21 化合物No.22 化合物No.23 化合物No.24
本发明的金属化合物不受其制造方法的特别限制,可以应用众所周知的反应来制造。作为其制造方法,可以列举出例如基于MX4(M、X的定义与上述通式(1)相同)与提供所期望的m所需要的量的乙基甲基胺之间的反应的方法、基于MX4与提供所期望的m所需要的量的M(NEtMe)4之间的反应的方法。在为前者的情况下,优选如下方法:使用烷基锂作为反应剂,经由作为反应性中间体的乙基甲基氨基锂,使其与MX4反应。在为后者的情况下,优选如下方法:将MX4和M(NEtMe)4进行混合,并在反应所需要的温度下进行搅拌。另外,本发明的金属化合物的制造要在将水分、氧、二氧化碳等反应活性种尽可能从体系内排除的环境下进行。
本发明的化学气相沉积用原料是指将上述通式(1)表示的金属化合物作为薄膜的前体,其形态可根据所使用的化学气相沉积法的输送供给方法等手法来适当选择。
作为上述的输送供给方法,有如下方法:在原料容器中通过加热和/或减压化学气相沉积用原料而使其气化,并与根据需要所使用的氩、氮、氦等载气一起导入至沉积反应部的气体输送法;以液体或溶液的状态将化学气相沉积用原料输送至气化室,在气化室中通过加热和/或减压使其气化,并导入至沉积反应部的液体输送法。在为气体输送法的情况下,上述通式(1)表示的金属化合物本身成为化学气相沉积用原料,在为液体输送法的情况下,上述通式(1)表示的金属化合物本身或在有机溶剂中溶解有该金属化合物的溶液成为化学气相沉积用原料。
另外,在制造多成分体系薄膜时使用的多成分体系化学气相沉积法中,有如下方法:使化学气相沉积用原料的各成分独立地气化并供给的方法(以下有时也记载为单源法);以及将多成分原料预先按照所期望的组成混合,使该混合原料气化并供给的方法(以下有时也记载为混合源法)。在为混合源法的情况下,仅由上述通式(1)表示的金属化合物形成的混合物或在这些混合物中加入了有机溶剂的混合溶液、上述通式(1)表示的金属化合物与其它的前体的混合物或在这些混合物中加入了有机溶剂的混合溶液是化学气相沉积用原料。
作为上述的化学气相沉积用原料中使用的有机溶剂,没有特别限制,可以使用众所周知的普通的有机溶剂中与本发明的金属化合物不反应的溶剂。作为该有机溶剂,可以列举出例如乙酸乙酯、乙酸丁酯、乙酸甲氧基乙酯等乙酸酯类;四氢呋喃、四氢吡喃、吗啉、乙二醇二甲基醚、二乙二醇二甲基醚、三乙二醇二甲基醚、二丁基醚、二噁烷等醚类;甲基丁基酮、甲基异丁基酮、乙基丁基酮、二丙基酮、二异丁基酮、甲基戊基酮、环己酮、甲基环己酮等酮类;己烷、环己烷、甲基环己烷、二甲基环己烷、乙基环己烷、庚烷、辛烷、甲苯、二甲苯等烃类;乙腈、1-氰基丙烷、1-氰基丁烷、1-氰基己烷、氰基环己烷、氰基苯、1,3-二氰基丙烷、1,4-二氰基丁烷、1,6-二氰基己烷、1,4-二氰基环己烷、1,4-二氰基苯等具有氰基的烃类;吡啶、二甲吡啶。根据溶质的溶解性、使用温度与沸点及燃点的关系等,上述溶剂单独或以二种以上的混合溶剂的形式来使用。在使用上述有机溶剂时,该有机溶剂中的本发明的金属化合物成分的总量优选设定为0.01~2.0摩尔/升,特别优选设定为0.05~1.0摩尔/升。
另外,在使用了单源法或混合源法的多成分体系的化学气相沉积法中,作为与本发明的上述通式(1)表示的金属化合物一起使用的其它前体,不受特别限制,可以使用众所周知的普通的前体。
作为上述的其它前体,可以列举出选自醇化合物、二醇化合物、β-二酮化合物、环戊二烯化合物以及有机胺化合物等用作有机配位体的化合物中的一种或二种以上与硅、硼、磷或金属的化合物。作为金属种,可以列举出锂、钠、钾、铷、铯等1族元素;铍、镁、钙、锶、钡等2族元素;钪、钇、镧系元素(镧、铈、镨、钕、钷、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥)、锕系元素等3族元素;钛、锆、铪等4族元素;钒、铌、钽的5族元素;铬、钼、钨的6族元素;锰、锝、铼的7族元素;铁、钌、锇的8族元素;钴、铑、铱的9族元素;镍、钯、铂的10族元素;铜、银、金的11族元素;锌、镉、汞的12族元素;铝、镓、铟、铊的13族元素;锗、锡、铅的14族元素;砷、锑、铋的15族元素;钋的16族元素。
作为用作有机配位体的上述醇化合物,可以列举出甲醇、乙醇、丙醇、异丙醇、丁醇、2-丁醇、异丁醇、叔丁醇、戊醇、异戊醇、叔戊醇等烷基醇类;2-甲氧基乙醇、2-乙氧基乙醇、2-丁氧基乙醇、2-(2-甲氧基乙氧基)乙醇、2-甲氧基-1-甲基乙醇、2-甲氧基-1,1-二甲基乙醇、2-乙氧基-1,1-二甲基乙醇、2-异丙氧基-1,1-二甲基乙醇、2-丁氧基-1,1-二甲基乙醇、2-(2-甲氧基乙氧基)-1,1-二甲基乙醇、2-丙氧基-1,1-二乙基乙醇、2-仲丁氧基-1,1-二乙基乙醇、3-甲氧基-1,1-二甲基丙醇等醚醇类;二烷基氨基醇等。
作为用作有机配位体的上述二醇化合物,可以列举出1,2-乙二醇、1,2-丙二醇、1,3-丙二醇、2,4-己二醇、2,2-二甲基-1,3-丙二醇、2,2-二乙基-1,3-丙二醇、1,3-丁二醇、2,4-丁二醇、2,2-二乙基-1,3-丁二醇、2-乙基-2-丁基-1,3-丙二醇、2,4-戊二醇、2-甲基-1,3-丙二醇、2-甲基-2,4-戊二醇、2,4-己二醇、2,4-二甲基-2,4-戊二醇等。
作为用作有机配位体的上述β-二酮化合物,可以列举出乙酰丙酮、己烷-2,4-二酮、5-甲基己烷-2,4-二酮、庚烷-2,4-二酮、2-甲基庚烷-3,5-二酮、5-甲基庚烷-2,4-二酮、6-甲基庚烷-2,4-二酮、2,2-二甲基庚烷-3,5-二酮、2,6-二甲基庚烷-3,5-二酮、2,2,6-三甲基庚烷-3,5-二酮、2,2,6,6-四甲基庚烷-3,5-二酮、辛烷-2,4-二酮、2,2,6-三甲基辛烷-3,5-二酮、2, 6-二甲基辛烷-3,5-二酮、2,9-二甲基壬烷-4,6-二酮、2-甲基-6-乙基癸烷-3,5-二酮、2,2-二甲基-6-乙基癸烷-3,5-二酮等烷基取代β-二酮类;1,1,1-三氟戊烷-2,4-二酮、1,1,1-三氟-5,5-二甲基己烷-2,4-二酮、1,1,1,5,5,5-六氟戊烷-2,4-二酮、1,3-二全氟己基丙烷-1,3-二酮等氟取代烷基β-二酮类;1,1,5,5-四甲基-1-甲氧基己烷-2,4-二酮、2,2,6,6-四甲基-1-甲氧基庚烷-3,5-二酮、2,2,6,6-四甲基-1-(2-甲氧基乙氧基)庚烷-3,5-二酮等醚取代β-二酮类。
作为用作有机配位体的上述环戊二烯化合物,可以列举出环戊二烯、甲基环戊二烯、乙基环戊二烯、丙基环戊二烯、异丙基环戊二烯、丁基环戊二烯、仲丁基环戊二烯、异丁基环戊二烯、叔丁基环戊二烯、二甲基环戊二烯、四甲基环戊二烯、五甲基环戊二烯等。
作为用作有机配位体的上述有机胺化合物,可以列举出甲基胺、乙基胺、丙基胺、异丙基胺、丁基胺、叔丁基胺、仲丁基胺、异丁基胺、二甲基胺、二乙基胺、二丙基胺、二异丙基胺、乙基甲基胺、丙基甲基胺、异丙基甲基胺等。
有关多成分体系化学气相沉积法中的上述其它前体,在为单源法的情况,优选对薄膜组成变化的反应或分解行为与本发明的金属化合物类似的化合物。另外,在为ALD法的情况,优选对所形成的分子水平的层(本发明的金属化合物层或其反应而形成的中间体层)具有反应活性的化合物。在为混合源法的情况,优选对薄膜组成变化的行为类似、而且在混合时不会发生化学反应引起变质的化合物。
另外,在本发明的化学气相沉积用原料中,根据需要为了赋予本发明的金属化合物以及其它的前体的稳定性,还可以含有亲核性试剂。作为该亲核性试剂,可以列举出甘醇二甲醚、二甘醇二甲醚、三甘醇二甲醚、四甘醇二甲醚等乙二醇醚类;18-冠-6、二环己基-18-冠-6,24-冠-8、二环己基-24-冠-8、二苯并-24-冠-8等冠醚类;乙二胺、N,N’-四甲基乙二胺、二亚乙基三胺、三亚乙基四胺、四亚乙基五胺、五亚乙基六胺、1,1,4,7,7-五甲基二亚乙基三胺、1,1,4,7,10,10-六甲基三亚乙基四胺、三乙氧基三亚乙基胺等多胺类,1,4,8,11-四氮杂环十四烷、1,4,7,10-四氮杂环十二烷等环状多胺类;吡啶、吡咯烷、哌啶、吗啉、N-甲基吡咯烷、N-甲基哌啶、N- 甲基吗啉、四氢呋喃、四氢吡喃、1,4-二噁烷、噁唑、噻唑、噁噻烷等杂环化合物类。作为稳定剂的上述亲核性试剂的使用量是,相对于1摩尔本发明的金属化合物优选在0.05摩尔~10摩尔的范围内使用,更优选在0.1~5摩尔的范围内使用。
本发明的化学气相沉积用原料尽量不要含有其构成成分以外的杂质金属元素成分、氯成分等杂质卤素、以及杂质有机成分。杂质金属元素成分优选为每种元素都为100ppb以下,更优选为10ppb以下。总量优选为1ppm以下,更优选为100ppb以下。特别是在将金属氧化物、与硅的复合金属氧化物、氮化物、与硅的氮化氧化物等用作LSI的门极绝缘膜、门极膜、阻挡层时,必须减少对所得到的薄膜的电特性有影响的碱金属元素、碱土类金属元素及同族元素(钛、锆或铪)的含量。杂质卤素成分优选为100ppm以下,更优选为10ppm以下,进一步优选为1ppm以下。杂质有机成分的总量优选为500ppm以下,更优选为50ppm以下,进一步优选为10ppm以下。此外,由于水分将引起CVD原料中的颗粒的发生或化学气相沉积法中的颗粒的发生,所以对于金属化合物、有机溶剂以及亲核性试剂来说,为了减少各自的水分,使用时最好预先尽可能地除去水分。金属化合物、有机溶剂以及亲核性试剂各自的水分量优选为10ppm以下,更优选为1ppm以下。
另外,为了降低或防止所制造的薄膜的颗粒污染,本发明的化学气相沉积用原料在液相中用光散射式液中粒子检测器得到的颗粒测定中,优选的是,大于0.3μm的粒子的数量在1ml液相中为100个以下,更优选的是,大于0.2μm的粒子的数量在1ml液相中为1000个以下,进一步优选的是,大于0.2μm的粒子的数量在1ml液相中为100个以下。
本发明的薄膜的制造方法是基于如下的化学气相沉积法:使本发明的金属化合物以及根据需要使用的其它前体气化,将气化得到的蒸汽以及根据需要使用的反应性气体导入至基板上,然后使前体在基板上分解和/或反应,从而使薄膜生长并沉积于基板上。有关原料的输送供给方法、沉积方法、制造条件、制造装置等,不受特别限制,可以使用众所周知的普通的条件、方法。
作为上述的根据需要而使用的反应性气体,例如作为制造氧化物时的反应性气体,可以列举出作为氧化性气体的氧、臭氧、二氧化氮、一氧化氮、水蒸汽、过氧化氢、甲酸、乙酸、乙酸酐等,作为还原性的反应性气体,可 以列举出氢,此外,作为制造氮化物时的反应性气体,可以列举出单烷基胺、二烷基胺、三烷基胺、亚烷基二胺等有机胺化合物,肼,氨,氮等。
另外,作为上述的输送供给方法,可以列举出上述的气体输送法、液体输送法、单源法、混合源法等。
另外,作为上述的沉积方法,可以列举出:仅通过热使原料气体或原料气体及反应性气体反应,从而使薄膜沉积的热CVD;使用热和等离子体的等离子体CVD;使用热和光的光CVD;使用热、光和等离子体的光等离子体CVD;将CVD的沉积反应划分为基本过程,以分子水平阶段性地进行沉积的ALD(原子层沉积,Atomic Layer Deposition)。
另外,作为上述的制造条件,可以列举出反应温度(基板温度)、反应压力、沉积速度等。有关反应温度,优选为本发明的金属化合物可充分反应的温度即150℃以上,更优选为250℃~450℃。另外,有关反应压力,如果是热CVD或光CVD的情况,则优选为大气压~10Pa,在使用等离子体的情况下,优选为10Pa~2000Pa。另外,沉积速度可以通过原料的供给条件(气化温度、气化压力)、反应温度、反应压力来控制。沉积速度如果较大,则得到的薄膜的特性有可能恶化,如果较小,则有可能在生产率方面产生问题,因而优选为0.5~5000nm/分钟,更优选为1~1000nm/分钟。另外,如果是ALD的情况,通过循环的次数来进行控制以获得所期望的膜厚。此外,通过本发明的化学气相沉积用原料而形成的薄膜的厚度可根据用途来适当选择,但优选从0.1~1000nm中选择。
本发明的金属化合物由于可提供残留碳等杂质含量较小的金属氮化物,所以优选用于氮化金属系薄膜的制造。另外,使用本发明的化学气相沉积用原料来制造氮化金属系薄膜时的优选的方法是ALD。ALD是如下方法:向沉积部交替进行原料和根据需要使用的反应性气体、根据需要使用的其它前体的供给,将其设定为1个循环,阶段性地沉积所期望的薄膜的分子层。此外在各个循环中还可以任意地导入下述工序,即,在供给原料气体和/或反应性气体后通过不活泼气体进行清洗和/或通过减压而排气,从而除去未反应的原料气体和/或反应性气体。ALD与其它的CVD法相比具有的特征是,能够获得膜厚薄且均匀的良好的薄膜。另外,从其成膜机理来看,能够将薄膜沉积温度抑制得较低,且不被基体的耐热性、向基体中的元素扩散性等所左右, 能够进行广泛应用。此外,ALD还能够与热、光、等离子体并用。
另外,在本发明的薄膜的制造方法中,为了在薄膜沉积后获得更良好的电特性,也可以在不活泼气氛下、氧化性气氛下或还原性气氛下进行退火处理,在需要阶梯覆盖的情况下,也可以设置回流工序。退火、回流的温度为在用途上可允许的温度内。通常为300~1200℃,优选为400~600℃。
通过使用了本发明的化学气相沉积法用原料的本发明的薄膜的制造方法而制造的薄膜通过适当选择其它成分的前体、反应性气体以及制造条件,可以形成金属氧化物系薄膜、金属氮化物系薄膜、玻璃等所期望种类的薄膜。作为所制造的薄膜的组成,例如作为金属氧化物系薄膜,可以列举出氧化钛、氧化锆、氧化铪、铋-钛复合氧化物、铋-稀土类元素-钛复合氧化物、硅-钛复合氧化物、硅-锆复合氧化物、硅-铪复合氧化物、铪-铝复合氧化物、铪-稀土类元素复合氧化物、硅-铋-钛复合氧化物、硅-铪-铝复合氧化物、硅-铪-稀土类元素复合氧化物、钛-锆-铅复合氧化物、钛-铅复合氧化物、锶-钛复合氧化物、钡-钛复合氧化物、钡-锶-钛复合氧化物等。作为金属氮化物系薄膜,可以列举出氮化钛、氮化锆、氮化铪、钛-铝复合氮化膜、硅-铪复合氧化氮化物(HfSiON)、钛复合氧化氮化物。作为上述薄膜的用途,可以列举出高电介质电容器膜、门极绝缘膜、门极膜、电极膜、阻挡膜、强电介质电容器膜、电容器膜等电子部件的构件、光纤、光波导、光放大器、光开关等光学玻璃构件。
实施例
以下,通过实施例、评价例和比较例来更详细地说明本发明。但是,本发明不受以下的实施例等的任何限制。
[实施例1]化合物No.2的制造
在干燥氩气气氛下向反应烧瓶中加入四氯化钛(TiCl4)43.0g、脱水己烷500ml,冷却至-10℃。以使反应体系的温度不超过-5℃的方式向其中滴加四(乙基甲基胺)钛(Ti[N(CH3)(C2H5)]4)191g和脱水己烷500ml的混合溶液。滴加结束后,在室温下搅拌8小时,然后在减压下馏去己烷。将残渣进行减压蒸馏,由压力为100Pa、馏出温度为82℃的馏分得到收率为90%的目标物即化合物No.2。得到的化合物No.2的鉴定是通过元素分析和1H-NMR来进 行。其结果如下所示。
(1)元素分析(金属分析:原子吸收、氯分析:硝酸银滴定法)
Ti:18.5质量%(理论值18.59质量%)
氯:13.4质量%(理论值13.76质量%)
(2)1H-NMR(溶剂∶氘代苯)(化学位移∶多重态∶H数比)
(3.096∶s∶3)(3.429∶q∶2)(1.003∶t∶3)
[实施例2]化合物No.6的制造
在干燥氩气气氛下向反应烧瓶中加入四氯化钛(TiCl4)55.7g、脱水甲苯300ml,冷却至-10℃。以使反应体系的温度不超过-5℃的方式向其中滴加四(乙基甲基胺)钛(Ti[N(CH3)(C2H5)]4)82.3g和脱水甲苯300ml的混合溶液。滴加结束后,在室温下搅拌8小时,然后在减压下馏去甲苯。将残渣进行减压蒸馏,由压力为100Pa、馏出温度为85℃的馏分得到收率为90%的目标物即化合物No.6。得到的化合物No.6的鉴定是通过元素分析和1H-NMR来进行。其结果如下所示。
(1)元素分析(金属分析:原子吸收、氯分析:硝酸银滴定法)
Ti:20.3质量%(理论值20.38质量%)
氯:30.1质量%(理论值30.17质量%)
(2)1H-NMR(溶剂∶氘代苯)(化学位移∶多重态∶H数比)
(3.021∶s∶3)(3.470∶q∶2)(1.003∶t∶3)
[评价例]
对于上述的实施例1和2中得到的化合物No.2、6、表1、2所示的比较化合物,进行了20℃下的状态(如果是固体,则熔点为利用DTA测定而得到的熔点的吸热开始温度)和热分解性的评价。其结果示于表1或表2中。热分解性是指,从将化合物密闭于不锈钢容器中,加热1小时后的减压下(10torr)的TG-DTA测定的结果,确认到了超过0.5质量%的分解物时的加热温度。有关加热温度,除TiCl4以外,均是按照每10℃的间隔从80℃至200℃选择,TiCl4是选择250℃~300℃。例如,在130℃加热1小时后的减压下的TG-DTA测定的结果是,大致全部挥发,在140℃加热1小时后的减压下的TG-DTA测定的结果是,并未全部挥发,质量减少结束时产生了超过0.5质量%的残渣,此时将热分解性记作140℃。
表1
金属化合物 | 状态 | 热分解性 |
化合物No.2 | 液体 | 140℃ |
TiCl4 | 液体 | >300℃ |
TiCl[N(CH3)2]3 | 固体(mp70℃) | 140℃ |
Ti[N(CH3)(C2H5)]4 | 液体 | 200℃ |
从上述的评价例可知,作为本发明的金属化合物的化合物No.2与作为类似化合物的TiCl[N(CH3)2]3不同,由于室温下是液体,所以适合作为化学气相沉积用原料。此外,热分解性也比TiCl4、Ti[N(CH3)(C2H5)]4良好。该结果暗示了可以提供更加低温下的薄膜制造,且将其作为前体而得到的薄膜的膜质良好。特别是,由于薄膜中的残留碳所带来的对电特性的影响较小,所以适合于以氮化钛为代表的LSI的门极薄膜、阻挡薄膜、电极膜的用途。
表2
金属化合物 | 状态 | 热分解性 |
化合物No.6 | 液体 | 100℃ |
TiCl2[N(CH3)2]2 | 固体(mp83℃) | 100℃ |
从上述的评价例可知,作为本发明的金属化合物的化合物No.6与作为类似化合物的TiCl2[N(CH3)2]2不同,由于室温下是液体,所以适合作为化学气相沉积用原料。此外,热分解性也是同等的。将化合物No.2与化合物No.6比较,虽然可以确认化合物No.6在低温下分解,但分解温度为100℃,其与挥发温度的制程范围较小。考虑到气化工序的温度与成膜温度的范围,化合物No.2比化合物No.6更适合用于化学气相沉积法。
[实施例3]氮化钛薄膜的制造
将上述实施例1中得到的金属化合物No.2作为化学气相沉积用原料,使用图1所示的装置,通过以下的条件的ALD在硅晶片上制造氮化钛薄膜。用荧光X射线对得到的薄膜进行膜厚测定、薄膜组成的确认,结果膜厚为60nm,膜组成为氮化钛,碳含量为1.3atom%。(条件)
反应温度(基板温度):300℃、反应性气体:NH3
(工序)
将下述(1)~(4)构成的一系列工序作为一个循环,重复300个循环。
(1)将在气化室温度为120℃、气化室压力为250Pa的条件下气化的CVD原料的蒸汽导入,在体系压力为250Pa的条件下使其沉积3秒钟。
(2)通过3秒钟的氩气清洗而除去未反应原料。
(3)导入反应性气体,在体系压力为250Pa的条件下使其反应3秒钟。
(4)通过2秒钟的氩气清洗除去未反应原料。
[比较例1]
将Ti[N(CH3)(C2H5)]4作为化学气相沉积用原料,通过与上述实施例2同样条件的ALD法在硅晶片上制造氮化钛薄膜。用荧光X射线对得到的薄膜进行膜厚测定、薄膜组成的确认,结果膜厚为50nm,膜组成为氮化钛,碳含量为7.0atom%。
根据本发明,可以提供一种金属化合物,其具有适合于含有金属的薄膜、特别是氮化金属系薄膜的制造中使用的化学气相沉积用原料的物性。
Claims (6)
1.一种金属化合物,其由下述通式(1)表示,
式中,M表示钛原子,X表示氯原子,m表示1或2。
2.根据权利要求1所述的金属化合物,其中,在所述通式(1)中,m为1。
3.一种化学气相沉积用原料,其含有权利要求1或2所述的金属化合物。
4.根据权利要求3所述的化学气相沉积用原料,其是在基体上通过化学气相沉积法来形成氮化金属系薄膜的原料。
5.一种含有金属的薄膜的制造方法,其利用了化学气相沉积法,该化学气相沉积法中使用了权利要求3或4所述的化学气相沉积用原料。
6.一种氮化金属系薄膜的制造方法,其利用了化学气相沉积法,该化学气相沉积法中使用了权利要求4所述的化学气相沉积用原料。
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