CN110831950B - 钨化合物、薄膜形成用原料和薄膜的制造方法 - Google Patents
钨化合物、薄膜形成用原料和薄膜的制造方法 Download PDFInfo
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- CN110831950B CN110831950B CN201880042110.0A CN201880042110A CN110831950B CN 110831950 B CN110831950 B CN 110831950B CN 201880042110 A CN201880042110 A CN 201880042110A CN 110831950 B CN110831950 B CN 110831950B
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- tungsten
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- 150000003658 tungsten compounds Chemical class 0.000 title claims abstract description 60
- 239000010409 thin film Substances 0.000 title claims description 117
- 238000004519 manufacturing process Methods 0.000 title claims description 37
- 239000000463 material Substances 0.000 title description 15
- 239000002994 raw material Substances 0.000 claims description 65
- 239000010408 film Substances 0.000 claims description 32
- 239000000758 substrate Substances 0.000 claims description 21
- 230000008016 vaporization Effects 0.000 claims description 16
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical group [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 13
- 125000000217 alkyl group Chemical group 0.000 abstract description 13
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 abstract description 12
- 125000004432 carbon atom Chemical group C* 0.000 abstract description 11
- 125000004435 hydrogen atom Chemical group [H]* 0.000 abstract description 9
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 abstract description 7
- 125000001973 tert-pentyl group Chemical group [H]C([H])([H])C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 abstract description 5
- 125000005843 halogen group Chemical group 0.000 abstract description 4
- 238000000034 method Methods 0.000 description 57
- 239000002243 precursor Substances 0.000 description 35
- 239000007789 gas Substances 0.000 description 33
- 238000005229 chemical vapour deposition Methods 0.000 description 29
- 150000001875 compounds Chemical class 0.000 description 27
- 238000006243 chemical reaction Methods 0.000 description 21
- 229910052751 metal Inorganic materials 0.000 description 21
- 239000002184 metal Substances 0.000 description 21
- 239000000203 mixture Substances 0.000 description 20
- 238000000231 atomic layer deposition Methods 0.000 description 19
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- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 19
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- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
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- 239000002904 solvent Substances 0.000 description 7
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- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 6
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45553—Atomic layer deposition [ALD] characterized by the use of precursors specially adapted for ALD
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F11/00—Compounds containing elements of Groups 6 or 16 of the Periodic Table
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F17/00—Metallocenes
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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Abstract
Description
技术领域
本发明涉及新的钨化合物,含有该化合物的薄膜形成用原料以及使用该薄膜形成用原料的薄膜的制造方法。
背景技术
含钨薄膜用于制造LSI时使用的MOSFET栅极、与源极/漏极的接触,存储器的字线等。
作为上述的薄膜的制造方法,可举出溅射法、离子镀法、涂布热解法、溶胶-凝胶法等MOD法、化学气相沉积法等。由于具有组成控制性、梯度覆盖性优异、适合量产化、可混合集成等众多优点,包括原子层沉积(ALD(Atomic Layer Deposition))法在内的化学气相沉积(以下,有时简记为“CVD”)法是最佳的制造方法。
作为用于化学气相沉积法的钨原子供给源,大量报道了各种原料。例如,在专利文献1中,作为可用作根据CVD法的薄膜形成用原料的钨原子供给源,公开了WCl2、WCl4、WCl5和WCl6及其混合物这样的氯化钨。另外,在专利文献2中,作为可用于CVD法和ALD法的钨原子供给源,公开了包含二氮杂丁二烯钨化合物的由式W(R1-N=CR3-CR4=N-R2)3(式中,R1、R2、R3和R4各自独立地选自H,C1~C6直链、支链或环状的烷基,C1~C6直链、支链或环状的烷基甲硅烷基,C1~C6直链、支链或环状的烷基氨基,以及C1~C6直链、支链或环状的氟代烷基)表示的化合物。然而,专利文献1和2均没有具体记载本发明的钨化合物。
现有技术文献
专利文献
专利文献1:日本特开2015-221940号
专利文献2:日本特开2014-534952号
发明内容
发明要解决的课题
不限于钨化合物,在根据CVD法等使化合物气化而形成薄膜的方法中使用的化合物(前体)所要求的性质中,包括低熔点、在液体状态下可运输、蒸气压大、容易气化。另外,在所形成的薄膜中,为了制造碳残渣这类不期望的杂质的浓度低的、高品质的含钨膜,要求可适用于ALD法的钨化合物。然而,对于以往的钨化合物来说,在这些方面还不能充分令人满意。
因此,本发明的目的是得到一种新的钨化合物,其可以用作根据CVD法的薄膜形成用原料,具有高的蒸气压,并且可以在常温下或者通过轻微加热而变成液体。
解决课题的手段
本发明人等进行了反复研究,结果发现,特定的钨化合物可以解决上述课题,从而完成了本发明。
即,本发明提供下述通式(1)表示的钨化合物:
[化1]
(式中,X表示卤原子,R1~R5各自独立地表示氢原子或碳数1~5的烷基,R6表示叔丁基或叔戊基,R7表示碳数1~5的烷基;但是,当R1~R5全部为氢原子且R6为叔丁基时、以及当R1~R5全部为甲基且R6为叔丁基时,R7表示碳数1~3或5的烷基。)
另外,本发明提供一种薄膜形成用原料,其含有通式(1)表示的钨化合物。
进而,本发明提供一种薄膜的制造方法,其包括以下工序:将使上述薄膜形成用原料气化而得到的含有上述通式(1)表示的钨化合物的蒸气引入设置有基体的成膜室内,使该钨化合物分解和/或发生化学反应,以在该基体的表面形成含有钨原子的薄膜。
发明效果
根据本发明,可以得到蒸气压高并且在常温下或者通过轻微加热而变为液体的新的钨化合物。通过将该钨化合物用作根据CVD法的薄膜形成用原料,在根据CVD法的含钨薄膜的制造过程中,前体的运输性优异,容易控制其向基板的供给量,并且能够稳定地供给。因此,能够以高生产率制造高品质的含钨薄膜。另外,由于该钨化合物可适用于ALD法,因此特别适合作为用于ALD法的薄膜形成用原料。
附图说明
[图1]是示出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例的概要图。
[图2]是示出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的概要图。
[图3]是示出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的概要图。
[图4]是示出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的概要图。
具体实施方式
本发明的钨化合物由上述通式(1)表示,适合用作包括CVD法等气化工序的薄膜制造方法中的前体,也可以使用ALD法形成薄膜。
在上述通式(1)中,X表示卤原子。作为卤原子,可举出氯原子、氟原子、溴原子等。其中,优选氯原子。
在上述通式(1)中,R1~R5各自独立地表示氢原子或碳数1~5的烷基,R6表示叔丁基或叔戊基,R7表示碳数1~5的烷基。
作为碳数1~5的烷基,可举出甲基、乙基、丙基、正丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基、正戊基、异戊基、仲戊基和叔戊基等。
在上述通式(1)中,当R1~R5全部为氢原子且R6为叔丁基时、以及当R1~R5全部为甲基且R6为叔丁基时,R7表示碳数1~3或5的烷基。
作为碳数1~3或5的烷基,可举出甲基、乙基、正丙基、异丙基、正戊基、异戊基、仲戊基和叔戊基等。
在上述通式(1)中,当R1为甲基、乙基或异丙基、且R2~R5均为氢原子时,在使用蒸气压高、熔点低的本发明的薄膜形成用原料制造薄膜时,能够以高生产率制造高品质的薄膜,因而是优选的。其中,当R1为异丙基时,这些效果更高,因而是更优选的,进而,当R1为异丙基且X为氯原子时,这些效果显著提高,因而是进一步优选的。
另外,在上述通式(1)中,当R1~R5均相同或全部为氢原子或碳数1~3的直链或支链烷基时,这些效果高,因而是优选的。
作为通式(1)表示的钨化合物的优选具体例,可举出由下述化学式No.1~No.44表示的化合物。予以说明,在下述化学式No.1~No.44中,“Me”表示甲基,“Et”表示乙基,“nPr”表示正丙基,“iPr”表示异丙基,“nBu”表示正丁基,“tBu”表示叔丁基。
[化2]
[化3]
[化4]
[化5]
[化6]
[化7]
本发明的钨化合物不受其制造方法的特别限制,可应用周知的反应来制造。例如,当以氯化钨为原料时,可举出下述式(2)和(3)所示的方法。予以说明,在式(2)和(3)中,“tAm”表示叔戊基。
[化8]
作为制造本发明钨化合物的其他方法,当以单环戊二烯基三羰基单氢钨为原料时,可举出下述式(4)和(5)所示的方法。关于下述式(4)和(5)中的单环戊二烯基三羰基单氢钨,可以使用单烷基环戊二烯基三羰基单氢钨。
[化9]
本发明的薄膜形成用原料是指将上文说明的本发明的钨化合物作为薄膜的前体,其形态根据该薄膜形成用原料所应用的制造工艺的不同而不同。例如,在制造仅含有钨作为金属原子的薄膜时,本发明的薄膜形成用原料不含上述钨化合物以外的金属化合物或半金属化合物。另一方面,在制造含有包括钨的2种以上的金属和/或半金属作为金属原子的薄膜时,本发明的薄膜形成用原料除了包含上述钨化合物以外,还包含含有期望金属的化合物和/或含有期望半金属的化合物(以下也称为“其他前体”)。如下文所述,本发明的薄膜形成用原料还可以含有有机溶剂和/或亲核试剂。对于本发明的薄膜形成用原料而言,如上所述,作为前体的钨化合物的物性适于CVD法、ALD法,因而本发明的薄膜形成用原料特别是作为化学气相沉积用原料(以下有时称为“CVD用原料”)是有用的。
当本发明的薄膜形成用原料是化学气相沉积用原料时,其形态可根据所使用的CVD法中的输送供给方法等方法适当地选择。
作为上述输送供给方法,包括如下方法:气体输送法,其中,通过在储存有CVD用原料的容器(以下有时简称为“原料容器”)中加热和/或减压该原料而使之气化成为蒸气,将该蒸气与根据需要使用的氩气、氮气和氦气等载气一起导入设置有基体的成膜室(以下有时称为“沉积反应部”)内;以及液体输送法,其中,将CVD用原料以液体或溶液的状态输送到气化室中,通过在气化室中加热和/或减压而使之气化成为蒸气,将该蒸气导入成膜室内。当使用气体输送法时,上述通式(I)表示的钨化合物本身可用作CVD用原料。当使用液体输送法时,上述通式(I)表示的钨化合物本身或将该化合物溶解在有机溶剂中而得到的溶液可用作CVD用原料。这些CVD用原料还可以包括其他前体、亲核试剂等。
另外,在多成分体系的CVD法中,包括如下方法:独立地气化和供给CVD用原料的各成分的方法(以下有时称为“单一来源法”),气化和供给将多成分原料以预先期望的组成混合的混合原料的方法(以下有时称为“鸡尾酒式来源法”)。当使用鸡尾酒式来源法时,本发明的钨化合物和其他前体的混合物、或将该混合物溶解在有机溶剂中的混合溶液可用作CVD用原料。该混合物或混合溶液还可以含有亲核试剂等。
上述有机溶剂可以不受特别限制地使用公知的通常的有机溶剂。作为该有机溶剂,例如可举出: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、二甘醇二甲醚、三甘醇二甲醚、二丁基醚、二烷等醚类;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、二甲基吡啶等。根据溶质的溶解性、使用温度、沸点和闪点之间的关系等,这些溶剂可以单独使用或混合2种以上使用。在使用这些有机溶剂的情况下,CVD用原料中的前体的总量为0.01~2.0mol/升,特别优选为0.05~1.0mol/升,所述CVD用原料是将前体溶解在有机溶剂中的溶液。当本发明的薄膜形成用原料不含本发明的钨化合物以外的金属化合物和半金属化合物时,前体的总量是指本发明的钨化合物的量。当本发明的薄膜形成用原料除了该钨化合物,还含有包含其他金属的化合物和/或包含半金属的化合物时,前体的总量是指本发明的钨化合物和其他前体的合计量。
另外,在多成分体系的CVD法的情况下,作为与本发明的钨化合物一起使用的其他前体,没有特别限制,可以使用在CVD用原料中使用的通常公知的前体。
作为上述其他前体,例如可举出选自以下化合物中的1种或2种以上的硅或金属的化合物,所述化合物具有氢化物、氢氧化物、卤化物、叠氮化物、烷基、烯基、环烷基、芳基、炔基、氨基、二烷基氨基烷基、单烷基氨基、二烷基氨基、二胺、二(甲硅烷基-烷基)氨基、二(烷基-甲硅烷基)氨基、二甲硅烷基氨基、烷氧基、烷氧基烷基、肼基、膦基、腈、二烷基氨基烷氧基、烷氧基烷基二烷基氨基、甲硅烷氧基、二酮基、环戊二烯基、甲硅烷基、吡唑基、胍基、磷酸胍、脒基、磷酸脒基、酮亚胺基、二酮亚胺基、羰基、或磷酸脒基作为配体的化合物。
予以说明,作为前体的金属种类,例如可举出:镁、钙、锶、钡、镭、钪、钇、钛、锆、铪、铌、钽、铬、钼、钨、锰、铁、锇、钴、铑、铱、镍、钯、铂、铜、银、金、锌、镉、铝、镓、铟、锗、锡、铅、锑、铋、镧、铈、镨、钕、钷、钐、铕、钆、铽、镝、钬、铒、铥、镱。
上述其他前体在本技术领域中是公知的,其制造方法也是公知的。若举出制造方法的一例,例如,在使用醇化合物作为有机配体的情况下,可以通过使上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,可举出金属的卤化物、硝酸盐等,作为碱金属醇盐,可举出醇钠、醇锂、醇钾等。
在单源法的情况下,上述其他前体优选是与本发明钨化合物的热和/或氧化分解的表现类似的化合物,在鸡尾酒式来源法的情况下,上述其他前体优选除了热和/或氧化分解的表现类似以外,而且在混合时也不会因化学反应等而引起改性的化合物。
另外,本发明的薄膜形成用原料可以根据需要含有亲核试剂,以向本发明的钨化合物和其他前体赋予稳定性。作为该亲核试剂,可举出: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;环拉胺、三环烯等环状多胺类;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、1,4-二烷、唑、噻唑、氧硫杂环戊烷等杂环化合物类;乙酰乙酸甲酯、乙酰乙酸乙酯、乙酰乙酸-2-甲氧基乙酯等β-酮酸酯类;或者乙酰丙酮、2,4-己二酮、2,4-庚二酮、3,5-庚二酮、二戊酰基甲烷等β-二酮类。这些亲核试剂的使用量相对于前体的总量1摩尔,优选为0.1~10摩尔的范围,更优选为1~4摩尔的范围。
在本发明的薄膜形成用原料中,需要使构成其的成分以外的杂质金属元素成分、杂质氯等杂质卤素成分、以及杂质有机成分的量最小化。关于杂质金属元素成分的含量,每种杂质金属元素成分的含量优选为100ppb以下,更优选为10ppb以下,其总量优选为1ppm以下,更优选为100ppb以下。特别是,在用作LSI的栅极绝缘膜、栅极膜、阻挡层的情况下,必须减少影响所得薄膜的电特性的碱金属元素和碱土金属元素的含量。杂质卤素成分的含量优选为100ppm以下,更优选为10ppm以下,最优选为1ppm以下。杂质有机成分的总量优选为500ppm以下,更优选为50ppm以下,最优选为10ppm以下。另外,由于水分会在化学气相沉积用原料中引起颗粒产生、并且在薄膜形成中引起颗粒产生,因此为了减少金属化合物、有机溶剂和亲核试剂的每一种中的水分,优选在使用时预先尽可能地除去水分。金属化合物、有机溶剂和亲核试剂的各自的水分含量优选为10ppm以下,更优选为1ppm以下。
另外,在本发明的薄膜形成用原料中,为了减少或防止所形成的薄膜的颗粒污染,优选尽可能地不含颗粒。具体而言,在通过在液相中的光散射式液体中的颗粒检测器进行的颗粒测定中,优选大于0.3μm的颗粒的数量在1ml液相中为100个以下,更优选大于0.2μm的颗粒的数量在1ml液相中为1000个以下,最优选大于0.2μm的颗粒的数量在1ml液相中为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,是基于CVD法的方法,所述CVD法如下所述:将使本发明的薄膜形成用原料气化的蒸气、以及根据需要使用的(任选的)反应性气体引入设置有基体的成膜室内,接着,使前体在基体上分解和/或发生化学反应,以使含有金属的薄膜在基体表面上生成并沉积。关于原料的输送供给方法、沉积方法、制造条件、制造装置等,不受特殊限制,可以使用公知的通常的条件和方法。
作为上述的根据需要使用的反应性气体,例如,作为具有氧化性的气体,可举出氧气、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,作为具有还原性的气体,可举出氢气,另外,作为制造氮化物的物质,可举出单烷胺、二烷胺、三烷胺、亚烷基二胺等有机胺化合物,肼,氨等,可以使用其中的1种或2种以上。
另外,作为上述的输送供给方法,可举出上述的气体输送法、液体输送法、单源法、鸡尾酒式来源法。
另外,作为上述的沉积方法,可举出:仅通过加热而使原料气体反应或者原料气体与反应性气体反应来沉积薄膜的热CVD法,使用热和等离子体的等离子体CVD法,使用热和光的光CVD法,使用热、光和等离子体的光等离子体CVD法,以及将CVD的沉积反应分为基本过程并在分子水平上进行逐步沉积的ALD法。
作为上述基体的材质,例如可举出硅,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,金属钌等金属。作为基体的形状,可举出板状、球状、纤维状、鳞片状。基体的表面既可以是平面的,也可以是沟槽结构等三维结构。
另外,作为上述的制造条件,可举出反应温度(基体温度)、反应压力、沉积速度等。关于反应温度,优选为能够使本发明的钨化合物充分反应的温度,即100℃以上,更优选为150~500℃。本发明的钨化合物具有300℃以上的热稳定性,因此,特别优选为250~450℃。另外,在热CVD法或光CVD法的情况下,反应压力优选为大气压~10Pa,在使用等离子体的情况下,反应压力优选为2000~10Pa。
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)、反应温度和反应压力来控制。当沉积速度大时,有时得到的薄膜的特性劣化,当沉积速度小时,有时生产率会产生问题,因此,沉积速度优选为0.01~100nm/分钟,更优选为1~50nm/分钟。另外,在ALD法的情况下,通过控制循环数来得到期望的膜厚。
作为上述的制造条件,还可举出将薄膜形成用原料气化成蒸气时的温度和压力。将薄膜形成用原料气化成蒸气的工序既可以在原料容器内进行,也可以在气化室内进行。在任一种情况下,本发明的薄膜形成用原料优选在0~150℃下蒸发。另外,在将薄膜形成用原料在原料容器内或气化室内气化为蒸气时,原料容器内的压力和气化室内的压力均优选为1~10000Pa。
本发明的薄膜的制造方法当采用ALD法时,可以包括以下工序:通过上述的输送供给方法,使薄膜形成用原料气化成蒸气,将该蒸气引入成膜室内的原料引入工序,除此以外,还可以包括以下工序:通过该蒸气中的上述钨化合物,在上述基体的表面上形成前体薄膜的前体薄膜成膜工序;将未反应的钨化合物气体排出的排气工序;以及,使该前体薄膜与反应性气体发生化学反应,以在该基体的表面上形成含有上述金属的薄膜的含金属薄膜形成工序。
以下,关于各工序,以形成金属氧化物薄膜的情况为例进行详细说明。在通过ALD法形成金属氧化物薄膜的情况下,首先,进行上述的原料引入工序。使薄膜形成用原料成为蒸气时的优选的温度和压力与上述说明的相同。接着,通过引入到沉积反应部中的钨化合物,在基体表面上形成前体薄膜(前体薄膜形成工序)。此时,可以加热基体或加热沉积反应部以施加热。在该工序中形成的前体薄膜是金属氧化物薄膜、或者是通过使钨化合物的一部分发生分解和/或反应而生成的薄膜,具有与目标的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200~500℃。进行本工序时的体系(成膜室内)的压力优选为1~10000Pa,更优选为10~1000Pa。
接着,将未反应的钨化合物气体和副产的气体从沉积反应部中排出(排气工序)。理想地是,未反应的钨化合物气体和副产的气体从沉积反应部中完全排出,但未必需要完全排出。作为排气方法,可举出用氮气、氦气、氩气等非活性气体吹扫体系内的方法,通过将体系内减压来进行排气的方法,以及将它们组合的方法等。减压时的减压度优选为0.01~300Pa,更优选为0.01~100Pa。
接着,向沉积反应部中引入氧化性气体,通过该氧化性气体的作用或者氧化性气体和热的作用,从由先前的前体薄膜形成工序中得到的前体薄膜来形成金属氧化物薄膜(含金属氧化物薄膜形成工序)。在本工序中作用热时的温度优选为室温~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1~10000Pa,更优选为10~1000Pa。由于本发明的钨化合物与氧化性气体的反应性良好,因此可以得到金属氧化物薄膜。另外,由于本发明的钨化合物与氨气等还原性气体的反应性也良好,因此也可以得到金属钨薄膜。
在本发明的薄膜的制造方法中,在如上所述采用ALD法的情况下,将通过包括上述的原料引入工序、前体薄膜形成工序、排气工序和含金属氧化物薄膜形成工序在内的一系列操作所进行的薄膜沉积设为1个循环,可以重复多次该循环,直至得到必要膜厚的薄膜。在这种情况下,优选的是,在进行1个循环之后,与上述排气工序同样操作,将未反应的钨化合物气体和反应性气体(形成金属氧化物薄膜时,为氧化性气体)、以及副产的气体从沉积反应部中排出,然后进行下一个循环。
另外,在通过ALD法的金属氧化物薄膜的形成中,既可以施加等离子体、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没有特殊限定,例如,该时期可以是原料引入工序中的钨化合物气体引入时、前体薄膜形成工序或含有金属氧化物的薄膜形成工序(含金属氧化物薄膜形成工序)中的加温(加热)时、排气工序中的体系内的排气时、含有金属氧化物的薄膜形成工序中的氧化性气体引入时,也可以在上述的各工序之间。
另外,在本发明的薄膜的制造方法中,在薄膜沉积后,为了得到更良好的电特性,可以在非活性气氛下、氧化性气氛下或还原性气氛下进行退火处理,在需要台阶覆盖的情况下,可以设计回流工序。此时的温度为200~1000℃,优选为250~500℃。
使用本发明的薄膜形成用原料制造薄膜的装置可以使用公知的化学气相沉积用装置。作为具体装置的例子,可举出如图1所示的能够通过鼓泡供给前体来进行的装置,和如图2所示那样具有气化室的装置。另外,可举出如图3和图4所示那样能够对反应性气体进行等离子体处理的装置。不限于图1~图4所示那样的单片式装置,也可以使用采用分批式炉的能够同时处理多片的装置。
通过适当地选择其他前体、反应性气体和制造条件,使用本发明的薄膜形成用原料制造的薄膜可以被制成金属、氧化物陶瓷、氮化物陶瓷等期望种类的薄膜。已知该薄膜显示出各种电特性和光学特性等,可应用于各种用途。例如,可用作在制造LSI时使用的MOSFET栅极、与源极/漏极的接触,存储器的字线等。
实施例
以下,参考实施例和评价例,更详细地描述本发明。但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.1的制造
在Ar气氛下,向500ml四口烧瓶中加入7.80g(0.019mol)甲基环戊二烯基四氯化钨和72ml甲苯。一边在冰浴下冷却,一边使用100ml滴液漏斗滴加16.8g(0.193mol)叔戊胺,然后将混合物在室温下搅拌。过滤反应溶液,将滤液在略微减压下蒸馏除去溶剂,然后在减压下蒸馏出滤液,得到1.2g收量的黑黄色液体(收率13%)。
(分析值)
(1)1H NMR(溶剂:重苯)(化学位移:多重度:H数)
(5.88~5.89:m:2)(5.61~5.62:m:2)(2.15:s:3)(1.46~1.61:m:4)(1.25:s:6)(1.18:s:6)(0.98:t:6)
(2)元素分析(金属分析:ICP-AES,氯分析:TOX)
W:38.7质量%,C:41.3质量%,H:6.5质量%,N:6.0质量%,Cl:7.2质量%(理论值:W:39.2质量%,C:41.0质量%,H:6.2质量%,N:6.0质量%,Cl:7.6质量%)
(3)常压TG-DTA
质量减少50%时的温度:227℃(Ar流速:100ml/分钟,升温速度:10℃/分钟)
(4)减压TG-DTA
质量减少50%时的温度:152℃(10托,Ar流速:50ml/分钟,升温速度:10℃/分钟)
[实施例2]化合物No.4的制造
在Ar气氛下,向500ml四口烧瓶中加入31.2g(0.072mol)异丙基环戊二烯基四氯化钨和287ml甲苯。一边在冰浴下冷却,一边使用100ml滴液漏斗滴加69.8g(0.801mol)叔戊胺,然后将混合物在室温下搅拌。过滤反应溶液,将滤液在略微减压下蒸馏除去溶剂,然后在减压下蒸馏出滤液,得到13.9g收量的黑黄色液体(91Pa,峰值温度137℃)(收率39%)。
(分析值)
(1)1H NMR(溶剂:重苯)(化学位移:多重度:H数)
(5.87~5.88:m:2)(5.80~5.81:m:2)(3.11:sept:1)(1.47~1.62:m:4)(1.26:s:6)(1.19:s:6)(1.17:d:6)(1.00:t:6)
(2)元素分析(金属分析:ICP-AES,氯分析:TOX)
W:37.2质量%,C:43.8质量%,H:6.4质量%,N:5.5质量%,Cl:7.5质量%(理论值:W:37.0质量%,C:43.5质量%,H:6.7质量%,N:5.7质量%,Cl:7.1质量%)
(3)常压TG-DTA
质量减少50%时的温度:240℃(Ar流速:100ml/分钟,升温速度:10℃/分钟)
(4)减压TG-DTA
质量减少50%时的温度:162℃(10托,Ar流速:50ml/分钟,升温速度:10℃/分钟)
[实施例3]化合物No.36的制造
在Ar气氛下,向50ml二口烧瓶中加入1.50g(0.003mol)异丙基环戊二烯基四氯化钨和40ml甲苯。使用注射器向其中滴加2.52g(0.034mol)叔丁胺,然后将混合物在室温下搅拌。过滤反应溶液,将滤液在略微减压下蒸馏除去溶剂,然后在减压下蒸馏出滤液,得到0.18g收量的黑黄色液体(收率11%)。
(分析值)
(1)1H NMR(溶剂:重苯)(化学位移:多重度:H数)
(1.16:d:6)(1.26:s:18)(3.08:sept:1)(5.81:t:2)(5.88:t:2)
(2)元素分析(金属分析:ICP-AES,氯分析:TOX)
W:43.2质量%,C:34.8质量%,H:7.0质量%,N:6.2质量%,Cl:8.0质量%(理论值:W:43.7质量%,C:34.3质量%,H:6.9质量%,N:6.7质量%,Cl:8.4质量%)
(3)常压TG-DTA
质量减少50%时的温度:227℃(Ar流速:100ml/分钟,升温速度:10℃/分钟)
(4)减压TG-DTA
质量减少50%时的温度:143℃(10托,Ar流速:50ml/分钟,升温速度:10℃/分钟)
[评价例1]钨化合物的物性评价
关于本发明的钨化合物No.1、4和36、以及以下所示的比较化合物1,目测观察常压和20℃下的化合物的状态。结果示于表1。
[化10]
比较化合物1
[表1]
化合物 | 状态(20℃) |
化合物No.1 | 液体 |
化合物No.4 | 液体 |
化合物No.36 | 液体 |
比较化合物1 | 固体 |
由表1的结果可知,比较化合物1在20℃的条件下为固体化合物,与此相比,化合物No.1、4和36是在20℃的条件下为液体的低熔点的化合物。熔点低的化合物是优异的,因为当用作化学气相沉积用原料时,它可以以液体状态稳定且容易地运输。
[实施例4]根据ALD法的氧化钨薄膜的制造
使用钨化合物No.1作为化学气相沉积用原料,使用图1所示的ALD装置,根据以下条件的ALD法,在氮化钛基板上制造氧化钨薄膜。对得到的薄膜,进行通过X射线反射率法的膜厚测定、通过X射线衍射法和X射线光电子能谱法的薄膜结构和薄膜组成的确认,结果,膜厚为8nm,膜组成为氧化钨(WO3)。碳含量和氯含量小于检测下限0.1原子%。平均1个循环得到的膜厚为0.08nm。
(条件)
反应温度(基板温度):350℃
反应性气体:臭氧气体
(工序)
将包括下述(1)~(4)的一系列工序设为1个循环,并重复100个循环:
(1)引入在原料容器加热温度:100℃的条件下气化的化学气相沉积用原料的蒸气,在体系压力:100Pa下沉积10秒;
(2)用氩气吹扫30秒,除去未反应的原料;
(3)引入反应性气体,在体系压力:100Pa下反应30秒;
(4)用氩气吹扫30秒,除去未反应的原料。
[实施例5]根据ALD法的氧化钨薄膜的制造
使用钨化合物No.4作为化学气相沉积用原料,除此以外,在与实施例4同样的条件下,在氮化钛基板上制造氧化钨薄膜。对得到的薄膜,进行通过X射线反射率法的膜厚测定、通过X射线衍射法和X射线光电子能谱法的薄膜结构和薄膜组成的确认,结果,膜厚为9nm,膜组成为氧化钨(WO3)。碳含量和氯含量小于检测下限0.1原子%。平均1个循环得到的膜厚为0.09nm。
[实施例6]根据ALD法的氧化钨薄膜的制造
使用钨化合物No.36作为化学气相沉积用原料,除此以外,在与实施例4同样的条件下,在氮化钛基板上制造氧化钨薄膜。对得到的薄膜,进行通过X射线反射率法的膜厚测定、通过X射线衍射法和X射线光电子能谱法的薄膜结构和薄膜组成的确认,结果,膜厚为6nm,膜组成为氧化钨(WO3)。碳含量和氯含量小于检测下限0.1原子%。平均1个循环得到的膜厚为0.06nm。
[比较例1]根据ALD法的氧化钨薄膜的制造
使用比较化合物1作为化学气相沉积用原料,除此以外,在与实施例4同样的条件下,在氮化钛基板上制造氧化钨薄膜。对得到的薄膜,进行通过X射线反射率法的膜厚测定、通过X射线衍射法和X射线光电子能谱法的薄膜结构和薄膜组成的确认,结果,膜厚为3nm,膜组成为氧化钨(WO3)。碳含量为1原子%,氯含量小于检测下限0.1原子%。平均1个循环得到的膜厚为0.03nm。
由实施例4~6和比较例1的结果可知,通过使用钨化合物No.1、4和36作为薄膜形成用原料,可以制造氧化钨薄膜,进而,得到的氧化物薄膜与使用比较化合物1作为薄膜形成用原料的情况相比,在一个循环中得到的氧化钨薄膜的膜厚多2倍以上,并且所得到的膜中的碳杂质的量也为1/10以下。特别是已知,当使用钨化合物No.4作为薄膜形成用原料时,与使用比较化合物1作为薄膜形成用原料的情况相比,在一个循环中得到的氧化钨薄膜的膜厚多3倍以上,特别是能够以高生产率制造氧化钨薄膜。
因此可知,当使用本发明的钨化合物作为薄膜形成用原料来制造氧化物薄膜时,能够以高生产率制造高品质的氧化钨薄膜。
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