CN111344294A - 钌化合物、薄膜形成用原料以及薄膜的制造方法 - Google Patents
钌化合物、薄膜形成用原料以及薄膜的制造方法 Download PDFInfo
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- CN111344294A CN111344294A CN201880072963.9A CN201880072963A CN111344294A CN 111344294 A CN111344294 A CN 111344294A CN 201880072963 A CN201880072963 A CN 201880072963A CN 111344294 A CN111344294 A CN 111344294A
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- thin film
- compound
- raw material
- ruthenium
- ruthenium compound
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- 239000010409 thin film Substances 0.000 title claims abstract description 100
- 239000002994 raw material Substances 0.000 title claims abstract description 79
- 150000003304 ruthenium compounds Chemical class 0.000 title claims abstract description 44
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 37
- 150000001875 compounds Chemical class 0.000 claims abstract description 74
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims abstract description 32
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 11
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 5
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 5
- 239000000758 substrate Substances 0.000 claims description 23
- 230000008016 vaporization Effects 0.000 claims description 19
- 238000000151 deposition Methods 0.000 claims description 18
- 125000000539 amino acid group Chemical group 0.000 claims 2
- 229910052707 ruthenium Inorganic materials 0.000 abstract description 25
- 230000008018 melting Effects 0.000 abstract description 15
- 238000002844 melting Methods 0.000 abstract description 15
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- 238000000034 method Methods 0.000 description 56
- 239000002243 precursor Substances 0.000 description 45
- 239000007789 gas Substances 0.000 description 41
- 238000000231 atomic layer deposition Methods 0.000 description 28
- -1 ruthenium (ruthenium) carbonate compound Chemical class 0.000 description 25
- 238000006243 chemical reaction Methods 0.000 description 24
- 238000005229 chemical vapour deposition Methods 0.000 description 20
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Abstract
本发明的目的在于提供一种蒸气压高、熔点比以往已知的化合物低的钌化合物、含有该化合物的薄膜形成用原料以及使用该原料形成含有钌的薄膜的薄膜的制造方法。为了实现上述目的,提供一种下述通式所示的钌化合物、含有该钌化合物的薄膜形成用原料以及使用了该薄膜形成用原料的薄膜的制造方法。(式中,R1~R3分别独立地表示碳原子数1~5的烷基。其中,在R1为甲基的情况下,R2与R3为不同的基团。)
Description
技术领域
本发明涉及一种具有特定结构的新型钌化合物、含有该化合物的薄膜形成用原料以及使用该原料形成含有钌的薄膜的薄膜的制造方法。
背景技术
包含钌元素的薄膜形成用材料显示出特异的电特性,被应用于各种用途。例如,用作以DRAM(Dynamic Random Access Memory:动态随机存取存储器)元件为代表的存储器元件的电极材料、电阻膜、硬盘的记录层所使用的反磁性膜和固体高分子型燃料电池(polymer electrolyte fuel cell)用的催化剂材料等。
作为上述的薄膜的制造法,可列举出:溅射法、离子镀法、涂布热分解法、溶胶凝胶法等MOD(Metal Organic Deposition:金属有机沉积)法、化学气相沉积法等。在这些制造法中,由于具有组成控制性和台阶覆盖性(step coverage)优异、适于量产化、能混合集成(hybrid integration)等许多优点,因此,包括ALD(Atomic Layer Deposition:原子层沉积)法的化学气相沉积(以下,有时也简记为“CVD”)法是最佳的制造工艺。
作为用作CVD法用原料的钌化合物,以往已知各种钌化合物。例如,在专利文献1中公开了一种在钌上键合有两个羰基和两个具有特定结构的酮亚胺基的钌化合物,但没有关于本发明的钌化合物的记载。并且,专利文献1所公开的钌化合物的熔点为100℃以上,因此,不是能充分满足作为化学气相沉积用原料的化合物。
现有技术文献
专利文献
专利文献1:国际公开第2010/071364号
发明内容
发明所要解决的问题
在CVD法等使化合物气化来形成薄膜的方法中,对用作原料的化合物(前体(precursor))所要求的性质为:熔点低且能以液体的状态进行输送、液体的粘度低、蒸气压大且容易气化、热稳定性高。其中,在用于ALD法的情况下,要求具有被称为ALD窗口的能适用于ALD法的温度区域。特别是,对于用于ALD法的钌化合物,要求具有ALD窗口、蒸气压高、且熔点低的化合物,但对于以往的钌化合物,没有在这些方面能充分满足的化合物。
因此,本发明的目的在于提供一种蒸气压高、熔点比以往已知的化合物低的钌化合物、含有该化合物的薄膜形成用原料以及使用该原料形成含有钌的薄膜的薄膜的制造方法。
用于解决问题的方案
本发明人进行了反复研究,其结果是,发现了具有特定结构的钌化合物能解决上述问题,从而得到了本发明。
即,本发明涉及一种下述通式(1)所示的钌化合物:
(式中,R1~R3分别独立地表示碳原子数1~5的烷基。其中,在R1为甲基的情况下,R2与R3为不同的基团。)
此外,本发明提供一种含有上述通式(1)所示的钌化合物的薄膜形成用原料。
而且,本发明提供一种在基体的表面含有钌原子的薄膜的制造方法,其包括以下工序:使方案2所述的薄膜形成用原料气化,而得到含有所述钌化合物的蒸气的工序;将所述蒸气导入至处理气氛的工序;以及通过使该化合物分解、通过使该化合物进行化学反应、或通过使该化合物分解和使该化合物进行化学反应这两者,来使该化合物沉积于基体的工序。
发明效果
根据本发明,能得到一种蒸气压高且熔点低的钌化合物,该化合物适合作为CVD法用的薄膜形成用原料,尤其由于具有ALD窗口,因此可以优选作为ALD法用的薄膜形成用原料来使用。
附图说明
图1是表示在本发明的薄膜的制造方法中使用的化学气相沉积用装置的一个例子的概略图。
图2是表示在本发明的薄膜的制造方法中使用的化学气相沉积用装置的另一例子的概略图。
图3是表示在本发明的薄膜的制造方法中使用的化学气相沉积用装置的再一例子的概略图。
图4是表示在本发明的薄膜的制造方法中使用的化学气相沉积用装置的又一例子的概略图。
具体实施方式
本发明的钌化合物由上述通式(1)表示,是钌原子上加成有一氧化碳的化合物。本发明的钌化合物优选作为CVD法等具有气化工序的薄膜制造方法的前体,由于是能适用于ALD法的前体,因此特别优选作为用于ALD法的前体。
在上述通式(1)中,R1~R3分别独立地表示碳原子数1~5的烷基。其中,在R1为甲基的情况下,R2与R3为不同的基团。
在上述通式(1)中,作为R1~R3所表示的碳原子数1~5的烷基,例如可列举出:甲基、乙基、正丙基、异丙基、正丁基、仲丁基、叔丁基、异丁基、正戊基、仲戊基、叔戊基、异戊基、新戊基。
在上述通式(1)中,R1、R2以及R3根据所应用的薄膜的制造方法来适当选择。在用于具有使化合物气化的工序的薄膜的制造方法的情况下,R1、R2以及R3的组合优选在常温常压下成为液体状态,蒸气压大的组合。
具体而言,R1为甲基、乙基、正丙基的化合物的蒸气压高,因此优选,其中特别优选甲基或乙基。此外,R3为叔丁基的化合物的熔点低,因此优选,更优选R3为叔丁基,R2为甲基、乙基、正丙基、异丙基、正丁基、仲丁基的化合物,R3为叔丁基,R2为乙基的化合物的熔点特别低,因此优选。
此外,R1为甲基或乙基,R3为叔丁基,R2为乙基的化合物的蒸气压高,熔点也低,因此特别优选,R1为甲基,R3为叔丁基,R2为乙基的化合物的熔点特别低,25℃下的液体状态的粘度低,因此优选。另一方面,在利用不伴随有气化工序的MOD法的薄膜的制造方法的情况下,R1、R2以及R3可以根据对于所使用的溶剂的溶解性、薄膜形成反应等任意地选择。
作为本发明的钌化合物的优选的具体例,例如可列举出下述化合物No.1~No.217。
需要说明的是,下述化学式中的“Me”表示甲基,“Et”表示乙基,“nPr”表示正丙基,“iPr”表示异丙基,“sBu”表示仲丁基,“tBu”表示叔丁基,“tAm”表示叔戊基。
在上述化合物中,从熔点低的观点考虑,优选化合物No.10、31、46、74、214,更优选化合物No.10、31以及214。此外,从蒸气压的观点考虑,优选化合物No.10以及No.31。
本发明的钌化合物不受其制造方法的特别限制,可以通过使公知的以三羰基二氯化钌、十二碳三钌(dodecacarbonium triruthenium)为代表的碳钌(carboniumruthenium)化合物与对应结构的脒化合物、对应结构的脒化合物的碱金属盐反应来得到。
接着,本发明的薄膜形成用原料是将上述说明的本发明的钌化合物作为薄膜的前体的原料,其形态根据应用该薄膜形成用原料的制造工艺不同。例如,在制造作为金属仅包含钌的薄膜的情况下,本发明的薄膜形成用原料不含有本发明的钌化合物以外的金属化合物和半金属化合物。另一方面,在制造包含两种以上的金属和/或半金属的薄膜的情况下,本发明的薄膜形成用原料除本发明的钌化合物之外,还可以含有包含所期望的金属的化合物和/或包含半金属的化合物(以下,有时也记载为“其他前体”)。如后所述,本发明的薄膜形成用原料还可以含有有机溶剂和/或亲核性试剂。本发明的薄膜形成用原料如上所述,作为前体的本发明的钌化合物的物性适合于CVD法、ALD法,因此特别是作为化学气相沉积用原料(以下,有时也记载为“CVD用原料”)是有用的。
在本发明的薄膜形成用原料是化学气相沉积用原料的情况下,其形态根据所使用的CVD法的输送供给方法等方式来适当选择。
作为上述的输送供给方法,有气体输送法和液体输送法,气体输送法通过将CVD用原料在储存有该原料的容器(以下,有时也记载为“原料容器”)中进行加热和/或减压来使其气化而形成蒸气,将该蒸气与根据需要使用的氩、氮、氦等载气一起导入至设置有基体的成膜室内(以下,有时也记载为“沉积反应部”),液体输送法通过将CVD用原料以液体或溶液的状态输送至气化室,并在气化室进行加热和/或减压来使其气化而形成蒸气,将该蒸气导入至成膜室内。在气体输送法的情况下,能将上述通式(1)所示的钌化合物本身作为CVD原料。在液体输送法的情况下,能将上述通式(1)所示的钌化合物本身或者将该化合物溶于有机溶剂而成的溶液作为CVD用原料。这些CVD原料还可以含有其他前体、亲核性试剂等。
此外,在多成分体系的CVD法中,有以下方法:各成分独立地气化、供给CVD用原料的方法(以下,有时也记载为“单源法”);以及预先将多成分原料以所期望的组成进行混合而形成混合原料,气化、供给混合原料的方法(以下,有时也记载为“混合源(cocktailsource)法”)。在混合源法的情况下,能将本发明的钌化合物与其他前体的混合物或者将该混合物溶于有机溶剂而成的混合溶液作为CVD用原料。该混合物、混合溶液还可以包含亲核性试剂等。
作为上述的有机溶剂,不受特别限制,可以使用众所周知的一般的有机溶剂。作为该有机溶剂,例如可列举出: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、乙二醇二甲醚、二乙二醇二甲醚、三乙二醇二甲醚、二丁醚、二恶烷等醚类;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;1-氰基丙烷、1-氰基丁烷、1-氰基已烷、氰基环己烷、氰基苯、1,3-二氰基丙烷、1,4-二氰基丁烷、1,6-二氰基已烷、1,4-二氰基环己烷、1,4-二氰基苯等具有氰基的烃类;吡啶、二甲基吡啶等。这些可以根据溶质的溶解性、使用温度和沸点、闪点的关系等单独使用或者作为两种以上的混合溶剂来使用。
在使用这些有机溶剂的情况下,作为将前体溶于有机溶剂而成的溶液的CVD用原料中的前体整体的量为0.01~2.0摩尔/升,特别优选为0.05~1.0摩尔/升。在本发明的薄膜形成用原料不含有本发明的钌化合物以外的金属化合物和半金属化合物的情况下,前体整体的量是指本发明的钌化合物的量,在本发明的薄膜形成用原料除该钌化合物以外还含有包含其他金属的化合物和/或包含半金属的化合物的情况下,前体整体的量是指本发明的钌化合物和其他前体的合计量。
此外,在多成分体系的CVD法的情况下,作为与本发明的钌化合物一起使用的其他前体,不受特别限制,可以使用在CVD用原料中使用的众所周知一般的前体。
作为上述的其他前体,可列举出:选自由醇化合物、二醇化合物、β-二酮化合物、环戊二烯化合物、有机胺化合物等作为有机配体使用的化合物构成的组中的一种或两种以上与硅、金属的化合物。此外,作为前体的金属种类,可列举出:锂、钠、钾、镁、钙、锶、钡、钛、锆、铪、钒、铌、钽、铬、钼、钨、锰、铁、钌、钴、铑、铱、镍、钯、铂、铜、银、金、锌、铝、镓、铟、锗、锡、铅、锑、铋、钪、钇、镧、铈、镨、钕、钷、钐、铕、钆、铽、镝、钬、铒、铥、镱或镥。
作为用作上述的其他前体的有机配体的醇化合物,可列举出:甲醇、乙醇、丙醇、异丙醇、丁醇、仲丁醇、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-s-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;二甲基氨基乙醇、乙基甲基氨基乙醇、二乙基氨基乙醇、二甲基氨基-2-戊醇、乙基甲基氨基-2―戊醇、二甲基氨基-2-甲基-2―戊醇、乙基甲基氨基-2-甲基-2-戊醇、二乙基氨基-2-甲基-2-戊醇等二烷基氨基醇类;等。
作为用作上述的其他前体的有机配体的二醇化合物,可列举出:1,2-乙二醇、1,2-丙二醇、1,3-丙二醇、2,4-已二醇、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-已二醇、2,4-二甲基-2,4-戊二醇等。
此外,作为用作上述的其他前体的有机配体的β-二酮化合物,可列举出:乙酰丙酮、已烷-2,4-二酮、5-甲基已烷-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-5,5-二甲基已烷-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-甲氧基已烷-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;等。
此外,作为用作上述的其他前体的有机配体的环戊二烯化合物,可列举出: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、四甲基环戊二烯等。
作为用作上述的其他前体的有机配体的有机胺化合物,可列举出:甲胺、乙胺、丙胺、异丙胺、丁胺、仲丁胺、叔丁胺、异丁胺、二甲胺、二乙胺、二丙胺、二异丙胺、乙基甲基胺、丙基甲基胺、异丙基甲基胺等。
上述的其他前体是在该技术领域中公知的物质,其制造方法也是公知的。如果举出制造方法的一个例子,例如,在将醇化合物用作有机配体的情况下,可以通过使先前叙述的金属的无机盐或其水合物与该醇化合物的碱金属醇盐反应来制造前体。在此,作为金属的无机盐或其水合物,可以列举出:金属的卤化物、硝酸盐等,作为碱金属醇盐,可以列举出:醇钠、醇锂、醇钾等。
对于上述的其他前体,在单源法的情况下,优选热和/或氧化分解的行为与本发明的钌化合物类似的化合物,在混合源法的情况下,优选除了热和/或氧化分解的行为类似以外,在混合时还不会引起化学反应等导致的变质的物质。
此外,对于本发明的薄膜形成用原料,为了根据需要赋予本发明的钌化合物和其他前体的稳定性,也可以含有亲核性试剂。作为该亲核性试剂,可列举出:甘醇二甲醚(glyme)、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;环拉胺(cyclam)、轮环藤宁(cyclen)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、1,4-二恶烷、恶唑、噻唑、氧硫杂环戊烷(oxathiolane)等杂环化合物类;乙酰乙酸甲酯、乙酰乙酸乙酯、乙酰乙酸-2-甲氧基乙酯等β-酮酯类;或者乙酰丙酮、2,4-已烷二酮、2,4-庚烷二酮、3,5-庚烷二酮、二叔戊酰甲烷等β-二酮类。这些亲核性试剂的使用量相对于前体整体的量1摩尔优选为0.1摩尔~10摩尔的范围,更优选为1~4摩尔。
在本发明的薄膜形成用原料中,尽量不含有构成该原料的成分以外的杂质金属元素成分、杂质氯等杂质卤素成分以及杂质有机成分。杂质金属元素成分按每种元素计优选为100ppb以下,更优选为10ppb以下。按总量计,优选为1ppm以下,更优选为100ppb以下。特别是,在用作LSI(Large Scale Integration:大规模集成电路)的栅极绝缘膜、栅极膜、阻挡层的情况下,需要使对得到的薄膜的电特性有影响的碱金属元素和碱土金属元素的含量减少。杂质卤素成分优选为100ppm以下,更优选为10ppm以下,最优选为1ppm以下。杂质有机成分按总量计优选为500ppm以下,更优选为50ppm以下,最优选为10ppm以下。此外,由于水分成为在化学气相沉积用原料中的颗粒产生、薄膜形成中的颗粒产生的原因,因此,对于前体、有机溶剂以及亲核性试剂而言,为了减少各自的水分,最好在使用时预先尽可能地去除水分。前体、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。
此外,为了减少或防止所形成的薄膜的颗粒污染,本发明的薄膜形成用原料优选尽量不包含颗粒。具体而言,在液相中利用光散射式液体中粒子检测器进行的颗粒测定中,优选比0.3μm大的粒子的数量在液相1mL中为100个以下,更优选比0.2μm大的粒子的数量在液相1mL中为1000个以下,最优选比0.2μm大的粒子的数量在液相1mL中为100个以下。
作为使用本发明的薄膜形成用原料来制造薄膜的本发明的薄膜的制造方法,是将使本发明的薄膜形成用原料气化而得的蒸气和根据需要使用的反应性气体导入至设置有基体的成膜室内(处理气氛),接着,使前体在基体上分解、或使前体在基体上进行化学反应、或使前体在基体上分解和使前体在基体上进行化学反应这两者,由此使含有金属的薄膜生长、沉积于基体表面的基于CVD法的方法。对于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一般的条件和方法。
作为上述的根据需要使用的反应性气体,例如,作为氧化性气体,可列举出:氧、臭氧、二氧化氮、一氧化氮、水蒸气、过氧化氢、甲酸、乙酸、乙酸酐等,作为还原性气体,可列举出氢,此外,作为制造氮化物的物质,可列举出: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;氨等。它们可以使用一种或两种以上。其中,本发明的薄膜形成用原料与臭氧的反应性良好,因此在使用一种作为反应性气体的情况下,优选使用臭氧,在使用两种以上的混合气体作为反应性气体的情况下,优选至少包含臭氧。
此外,作为上述的输送供给方法,可列举出前述的气体输送法、液体输送法、单源法、混合源法等。
此外,作为上述的沉积方法,可列举出:仅通过热使原料气体或原料气体与反应性气体反应而沉积薄膜的热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、光以及等离子体的光等离子体CVD;将CVD的沉积反应分为基本过程(elementaryprocess),以分子水平阶段性进行沉积的ALD。
作为上述基体的材质,例如可列举出:硅;氮化硅、氮化钛、氮化钽、氧化钛、氮化钛、氧化钌、氧化锆、氧化铪、氧化镧等陶瓷;玻璃;金属钴等金属。作为基体的形状,可列举出:板状、球状、纤维状、鳞片状。基体表面可以为平面,也可以为沟槽(trench)结构等三维结构。
此外,作为上述的制造条件,可列举出反应温度(基体温度)、反应压力、沉积速度等。对于反应温度而言,优选为作为本发明的化合物充分反应的温度的100℃以上,更优选为150℃~400℃,特别优选为200℃~350℃。此外,对于反应压力而言,在热CVD或光CVD的情况下,优选为10Pa~大气压,在使用等离子体的情况下,优选为10Pa~2000Pa。
此外,对于沉积速度而言,可以根据原料的供给条件(气化温度、气化压力)、反应温度、反应压力进行控制。若沉积速度大,则有时得到的薄膜的特性会恶化,若沉积速度小,则有时生产率产生问题,因此优选0.01nm/分钟~100nm/分钟,更优选1nm/分钟~50nm/分钟。此外,在ALD法的情况下,为了得到所期望的膜厚,用循环的次数进行控制。
作为上述的制造条件,还可列举出:使薄膜形成用原料气化而成为蒸气时的温度、压力。使薄膜形成用原料气化而得到蒸气的工序可以在原料容器内进行,也可以在气化室内进行。无论在哪种情况下,本发明的薄膜形成用原料均优选在0℃~150℃下蒸发。此外,在原料容器内或气化室内使薄膜形成用原料气化而得到蒸气的情况下,原料容器内的压力和气化室内的压力均优选为1Pa~10000Pa。
本发明的薄膜的制造方法采用ALD法,除了通过上述的输送供给方法使薄膜形成用原料气化而成为蒸气,将该蒸气导入至成膜室内的原料导入工序之外,还可以具有:前体薄膜成膜工序,由该蒸气中的上述化合物在上述基体的表面形成前体薄膜;排气工序,将未反应的化合物气体排出;以及含金属的薄膜形成工序,使该前体薄膜与反应性气体进行化学反应,而在该基体的表面形成含有金属的薄膜。
以下,关于上述的ALD法的各工序,以形成金属氧化物薄膜的情况为例子进行详细说明。首先,进行上述的原料导入工序。使薄膜形成用原料成为蒸气时的优选的温度、压力与在利用CVD法的薄膜的制造方法中说明的相同。接着,导入至成膜室的蒸气与基体的表面接触,由此在基体表面形成前体薄膜(前体薄膜形成工序)。此时,可以对基体进行加热或对成膜室进行加热来施加热量。在该工序中成膜的前体薄膜是由本发明的化合物生成的薄膜,或本发明的化合物的一部分进行分解和/或反应而生成的薄膜,具有与目标金属氧化物薄膜不同的组成。进行本工序时的基体温度优选为室温~500℃,更优选为150℃~350℃。进行本工序时的体系(成膜室内)的压力优选为1Pa~10000Pa,更优选为10Pa~1000Pa。
接着,将未反应的化合物气体、副产的气体从成膜室排出(排气工序)。理想的是,未反应的化合物气体、副产的气体从成膜室完全排出,但不一定要完全排气。作为排气方法,可列举出:通过氮、氦、氩等惰性气体对体系内进行吹扫的方法;通过对体系内进行减压来排气的方法;将这些组合的方法;等。进行减压的情况下的减压度优选为0.01Pa~300Pa,更优选为0.01Pa~100Pa。
接着,向成膜室中导入氧化性气体作为反应性气体,通过该氧化性气体的作用或氧化性气体和热的作用,由在之前的前体薄膜形成工序中得到的前体薄膜形成金属氧化物薄膜(含金属氧化物的薄膜形成工序)。在本工序中使热进行作用的情况下的温度优选为室温~500℃,更优选为150~350℃。进行本工序时的体系(成膜室内)的压力优选为1Pa~10000Pa,更优选为10Pa~1000Pa。本发明的化合物与氧化性气体的反应性良好,因此能得到残留碳含量少的高品质的金属氧化物薄膜。
在本发明的薄膜的制造方法中,在如上所述采用了ALD法的情况下,可以将通过包括上述的原料导入工序、前体薄膜形成工序、排气工序以及含金属氧化物的薄膜形成工序的一系列操作实现的薄膜沉积设为一个循环,重复进行多次该循环,直至得到所需的膜厚的薄膜。在该情况下,优选的是,在进行一个循环后,与上述排气工序同样地,将未反应的化合物气体和反应性气体(在形成金属氧化物薄膜的情况下,为氧化性气体),进而副产的气体从沉积反应部排出后,进行下一个循环。
此外,在利用ALD法形成金属氧化物薄膜时,也可以施加等离子体、光、电压等能量,也可以使用催化剂。施加该能量的时期和使用催化剂的时期不特别限定。例如,可以在原料导入工序中的化合物气体导入时、在前体薄膜成膜工序或含金属氧化物的薄膜形成工序中的加热时、在排气工序中的体系内的排气时、在含金属氧化物的薄膜形成工序中的氧化性气体导入时,还可以在上述的各工序之间。
此外,在本发明的薄膜的制造方法中,在薄膜沉积之后,为了得到更良好的电特性,可以在惰性气氛下、氧化性气氛下或还原性气氛下进行退火处理,在需要埋入台阶的情况下,也可以设置回流(reflow)工序。该情况下的温度为200℃~1000℃,优选为250℃~500℃。
使用本发明的薄膜形成用原料来制造薄膜的装置可以使用众所周知的化学气相沉积法用装置。作为具体的装置的例子,可列举出:如图1那样的能通过鼓泡(bubbling)来供给前体的装置、如图2那样具有气化室的装置。此外,可列举出:如图3和图4那样能对反应性气体进行等离子体处理的装置。需要说明的是,不限于如图1~图4那样的单片式(singlewafer type)装置,也可以使用利用分批炉(batch furnace)能同时处理多片的装置。
使用本发明的薄膜形成用原料制造的薄膜通过适当选择其他前体、反应性气体以及制造条件,能制成金属、氧化物陶瓷、氮化物陶瓷、玻璃等所期望的种类的薄膜。已知该薄膜示出电特性和光学特性等,被应用于各种用途。例如,可列举出:金属钌薄膜、氧化钌薄膜、钌合金和含钌的复合氧化物薄膜等。作为钌合金,可列举出:Pt-Ru合金。作为含钌的复合氧化物薄膜,例如可列举出:SrRuO3。这些薄膜,例如被广泛用于制造以DRAM元件为代表的存储器元件的电极材料、电阻膜、硬盘的记录层所使用的反磁性膜和固体高分子型燃料电池用的催化剂材料等。
实施例
以下,以实施例、制造例、比较例以及评价例进一步对本发明进行详细说明。然而,本发明并不受以下的实施例等的任何限制。
[实施例1]化合物No.10的合成
向反应烧瓶中加入N’-(叔丁基)-N-乙基乙酰亚胺酰胺16g和脱水THF225mL,充分混合。在冰冷却下,向得到的溶液中滴加正丁锂的已烷溶液(1.55M)72.6mL,搅拌1小时。在向另外准备的反应烧瓶中添加三羰基二氯化钌13.1g和脱水THF511mL并充分混合后,在冰冷却下滴加前述的反应溶液。将反应溶液在室温下搅拌15小时后,在80℃下实施4小时加热回流。搅拌后,回到室温并进行过滤。对得到的滤液在减压下、油浴75℃下实施脱溶剂。将得到的钌络合物在油浴135℃、13Pa下进行蒸馏而得到了淡黄色粘状液体。
(分析值)
(1)常压TG-DTA
质量减少50%温度:216℃(760Torr,Ar流量:100ml/分钟,升温10℃/分钟)
(2)减压TG-DTA
质量减少50%温度:138℃(10Torr,Ar流量:50ml/分钟,升温10℃/分钟)
(3)1H-NMR(重苯)
1.01-1.08ppm(6H,多重峰),1.18-1.26ppm(18H,多重峰),1.48-1.53ppm(6H,多重峰),2.86-3.10ppm(4H,多重峰)
(4)元素分析(理论值)
C:49.4%(49.18%),H:7.8%(7.80%),N:12.7%(12.75%)
[实施例2]化合物No.31的合成
向反应烧瓶中添加N’-(叔丁基)-N-乙基丙酰亚胺酰胺10.35g和脱水THF120mL,充分混合。在冰冷却下向得到的溶液中滴加正丁锂的已烷溶液(1.55M)36.7ml,搅拌1小时。在向另外准备的反应烧瓶中添加三羰基二氯化钌7.0g和脱水THF273mL并充分混合后,在冰冷却下滴加前述的反应溶液。将反应溶液在室温下搅拌2小时后,在80℃下实施10小时加热回流。搅拌后,回到室温并进行过滤。对得到的滤液在减压下、油浴75℃下实施脱溶剂。将得到的钌络合物在油浴145℃、15Pa下进行蒸馏,得到了淡黄色粘状液体0.95g。
(分析值)
(1)常压TG-DTA
质量减少50%温度:224℃(760Torr,Ar流量:100ml/分钟,升温10℃/分钟)
(2)减压TG-DTA
质量减少50%温度:151℃(10Torr,Ar流量:50ml/分钟,升温10℃/分钟)
(3)1H-NMR(重苯)
0.86-0.97ppm(6H,多重峰),1.06-1.09ppm(6H,多重峰),1.21-1.30ppm(18H,多重峰),1.89-1.98ppm(4H,多重峰),2.83-3.11ppm(4H,多重峰)
(4)元素分析(理论值)
C:51.3%(51.37%),H:8.0%(8.19%),N:12.0%(11.98%)
[实施例3]化合物No.46的合成
向反应烧瓶中添加三羰基二氯化钌5.5g和脱水THF80mL,充分混合。在冰冷却下,向得到的悬浊液滴加由N,N’-二异丙基碳二亚胺5.7g与乙基锂1.58g制备出的N,N’-二异丙基-丙脒锂的THF溶液。在室温下搅拌19小时后,在减压下、油浴75℃下实施脱溶剂。将生成的钌络合物放入烧瓶,与kugelrohr提纯装置连接,在加热温度125℃、27Pa下进行蒸馏,得到了黄色粘性固体0.5g。
(分析值)
(1)常压TG-DTA
质量减少50%温度:222℃(760Torr,Ar流量:100ml/分钟,升温10℃/分钟)
(2)减压TG-DTA
质量减少50%温度:153℃(10Torr,Ar流量:50ml/分钟,升温10℃/分钟)
(3)1H-NMR(重苯)
0.82-0.86ppm(3H,三重峰),1.00-1.01(3H,双峰),1.15-1.16ppm(6H,双峰),1.22-1.24(3H,双峰),1.75-1.90ppm(2H,多重峰),3.29-3.38ppm(1H,七重峰),3.59-3.69ppm(1H,七重峰)
(4)元素分析(理论值)
C:51.5%(51.37%),H:8.2%(8.19%),N:11.8%(11.98%)
[实施例4]化合物No.74的合成
向反应烧瓶中添加三羰基二氯化钌5.2g和脱水THF80mL,充分混合。在冰冷却下,向得到的悬浊液中滴加由N,N’-二异丙基碳二亚胺5.4g和丙基氯化镁4.3g制备出的N,N’-二异丙基-丁脒基氯化镁的THF溶液。在室温下搅拌19小时后,在减压下、油浴75℃下实施脱溶剂。将生成的钌络合物放入烧瓶,与kugelrohr提纯装置连接,在加热温度145℃、42Pa下进行蒸馏,得到了褐色粘性液体(在室温下结晶化)0.6g。
(分析值)
(1)常压TG-DTA
质量减少50%温度:222℃(760Torr,Ar流量:100ml/分钟,升温10℃/分钟)
(2)减压TG-DTA
质量减少50%温度:157℃(10Torr,Ar流量:50ml/分钟,升温10℃/分钟)
(3)1H-NMR(重苯)
0.75-0.79ppm(3H,三重峰),1.02-1.04(3H,双峰),1.17-1.19ppm(6H,双峰-双峰),1.24-1.26(3H,双峰),1.31-1.41ppm(2H,六重峰),1.79-1.93ppm(2H,多重峰),3.34-3.43ppm(1H,七重峰),3.64-3.73ppm(1H,七重峰)
(4)元素分析(理论值)
C:53.4(53.31%),H:8.5%(8.54%),N:11.2(11.30%)
[实施例5]化合物No.214的合成
向反应烧瓶中添加三羰基二氯化钌4.9g和脱水THF80mL,充分混合。在冰冷却下向得到的悬浊液中滴加由N,N’-二异丙基碳二亚胺5.1g和正丁锂2.5g制备出的N,N’-二异丙基-戊基脒基锂的THF溶液。在室温下搅拌19小时后,在减压下、油浴75℃下实施脱溶剂。将生成的钌络合物放入烧瓶,与kugelrohr提纯装置连接,在加热温度150℃、55Pa下进行蒸馏,得到了褐色粘性液体0.5g。
(分析值)
(1)常压TG-DTA
质量减少50%温度:230℃(760Torr,Ar流量:100ml/分钟,升温10℃/分钟)
(2)减压TG-DTA
质量减少50%温度:162℃(10Torr,Ar流量:50ml/分钟,升温10℃/分钟)
(3)1H-NMR(重苯)
0.79-0.83ppm(3H,三重峰),1.04-1.06(3H,双峰),1.19-1.22ppm(8H,多重峰),1.26-1.28(3H,双峰),1.32-1.41ppm(2H,六重峰),1.86-2.00ppm(2H,多重峰),3.39-3.48ppm(1H,七重峰),3.69-3.78ppm(1H,七重峰)
(4)元素分析(理论值)
C:54.9(55.04%),H:8.8%(8.85%),N:10.8(10.70%)
[评价例1]钌化合物的物性评价
对于在实施例1~5中得到的本发明的化合物No.10、31、46、74以及214以及下述的比较化合物1和2,使用TG-DTA测定装置,确认了通过常压气氛(760torr)下的加热使样品质量减少50质量%的时间点的温度(L)。可以判断为:L低的化合物的蒸气压高,因此优选。此外,通过目视观察25℃下的状态。对于25℃下为固体的化合物,进行熔点测定。将这些结果示于表1。需要说明的是,在下述比较化合物1和比较化合物2的化学式中,“Me”表示甲基,“Et”表示乙基,“tBu”表示叔丁基。
[表1]
表1
化合物 | L/℃ | 25℃下的状态 | 熔点/℃ | |
评价例1-1 | 化合物No.10 | 215 | 液体 | - |
评价例1-2 | 化合物No.31 | 225 | 液体 | - |
评价例1-3 | 化合物No.46 | 220 | 固体 | 80 |
评价例1-4 | 化合物No.74 | 220 | 固体 | 75 |
评价例1-5 | 化合物No.214 | 230 | 液体 | - |
比较例1 | 比较化合物1 | 240 | 固体 | 120 |
比较例2 | 比较化合物2 | 250 | 固体 | 210 |
根据表1的结果,可知:化合物No.10、31、46、74以及214的蒸气压均高于比较化合物1和比较化合物2,熔点均低于比较化合物1和比较化合物2。其中,可知:化合物No.10、31以及214与具有类似结构的比较化合物相比,具有飞跃性低的熔点。除此之外,可知:化合物No.10以及31的蒸气压特别高。
[实施例6]金属钌薄膜的制造
将化合物No.10作为原子层沉积法用原料,使用图1所示的装置,通过以下条件的ALD法,在硅晶圆上制造出金属钌薄膜。
对所得到的薄膜通过X射线光电子能谱法确认薄膜组成,其结果是,所得到的薄膜为金属钌,残留碳含量少于1.0atom%。此外,通过X射线反射率法测定膜厚,计算出其平均值,其结果是,膜厚平均为26.4nm,每一个循环所得到的膜厚平均为0.05nm。
(条件)
基板:硅晶圆
反应温度(硅晶圆温度):350℃
反应性气体:氧
将包括下述(1)~(4)的一系列工序设为一个循环,重复进行500个循环:
(1)在原料容器温度:140℃、原料容器内压力:100Pa的条件下将气化了的原子层沉积法用原料导入至成膜室,使其在体系压力:100Pa下沉积30秒钟;
(2)通过15秒钟的氩吹扫,去除未沉积的原料;
(3)将反应性气体导入至成膜室,在体系压力:100Pa下使其反应5秒钟;
(4)通过15秒钟的氩吹扫,去除未反应的反应性气体和副产气体。
[实施例7]金属钌薄膜的制造
除了使用化合物No.31作为原子层沉积法用原料以外,在与实施例6相同的条件下制造出金属钌薄膜。对所得到的薄膜通过X射线光电子能谱法确认薄膜组成,其结果是,所得到的薄膜是金属钌,残留碳含量少于1.0atom%。此外,通过X射线反射率法测定膜厚,计算出其平均值,其结果是,膜厚平均为25.7nm,每一个循环所得到的膜厚平均为0.05nm。
[实施例8]金属钌薄膜的制造
除了使用化合物No.46作为原子层沉积法用原料以外,在与实施例6相同的条件下制造出金属钌薄膜。对所得到的薄膜通过X射线光电子能谱法确认薄膜组成,其结果是,所得到的薄膜为金属钌,残留碳含量少于1.0atom%。此外,通过X射线反射率法测定膜厚,计算出其平均值,其结果是,膜厚平均为26.3nm,每一个循环所得到的膜厚平均为0.05nm。
[实施例9]金属钌薄膜的制造
将化合物No.10作为原子层沉积法用原料,使用图1所示的装置,通过以下的条件的ALD法,在硅晶圆上制造出金属钌薄膜。
对所得到的薄膜通过X射线光电子能谱法确认薄膜组成,其结果是,所得到的薄膜为金属钌,残留碳含量少于1.0atom%。此外,通过X射线反射率法测定膜厚,计算出其平均值,其结果是,膜厚平均为15nm,每一个循环所得到的膜厚平均为0.03nm。
(条件)
基板:硅晶圆
反应温度(硅晶圆温度);350℃
反应性气体:氢
将包括下述(1)~(4)的一系列工序设为一个循环,重复进行500个循环。
(1)在原料容器温度:140℃、原料容器内压力:100Pa的条件下将气化了的原子层沉积法用原料导入至成膜室,使其在体系压力:100Pa下沉积30秒钟。
(2)通过15秒钟的氩吹扫,去除未沉积的原料。
(3)将反应性气体导入至成膜室,使其在体系压力:100Pa系下反应60秒钟。
(4)通过15秒钟的氩吹扫,去除未反应的第一的反应性气体和副产气体。
[比较例3]金属钌薄膜的制造
除了使用比较化合物2作为原子层沉积法用原料以外,在与实施例6相同的条件下制造出金属钌薄膜。对所得到的薄膜通过X射线光电子能谱法确认薄膜组成,其结果是,所得到的薄膜为金属钌,残留碳含量为6.0atom%。此外,通过X射线反射率法测定膜厚,计算出其平均值,其结果是,膜厚平均为10nm,每一个循环所得到的膜厚平均为0.02nm。
根据实施例6~9的结果,可知:均能制造残留碳含量低、品质良好的金属钌薄膜。另一方面,可知:比较例3中所得到的薄膜的残留碳含量非常高,得到了品质差的金属钌薄膜。此外,当将实施例6~8和比较例3的每一个循环所得到的膜厚进行比较时,可知:实施例6~8能生产率优于比较例3的2倍以上地制造金属钌薄膜。
根据以上结果可知:根据本发明,能通过ALD法以良好的生产率制造高品质的金属钌薄膜。
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