公开(公告)号：US08742153B2

公开(公告)日：2014-06-03

申请号：US13504573

申请日：2010-11-29

申请人： Atsushi Maniwa ,  Noriaki Oshima ,  Kazuhisa Kawano ,  Taishi Furukawa ,  Hirokazu Chiba ,  Toshiki Yamamoto

发明人： Atsushi Maniwa ,  Noriaki Oshima ,  Kazuhisa Kawano ,  Taishi Furukawa ,  Hirokazu Chiba ,  Toshiki Yamamoto

IPC分类号： C07F17/02 ,  C23C16/18 ,  H01L21/316

CPC分类号： C07F17/02 ,  C23C16/18 ,  H01L21/28088 ,  H01L21/28556 ,  H01L21/31695 ,  H01L21/32051 ,  H01L29/4966

摘要： For forming a thin ruthenium film of good quality by CVD method, it is necessary to form the thin film at low temperature. There hence is a desire for a ruthenium compound having a high reactivity to heat. This invention relates to a method of producing a ruthenium-containing film by CVD or the like using, as a raw material, a ruthenium complex mixture containing (2,4-dimethylpentadienyl)(ethyl-cyclopentadienyl)ruthenium and bis(2,4-dimethylpentadienyl)ruthenium, the amount of the latter compound being 0.1 to 100% by weight based on the weight of (2,4-dimethylpentadienyl)(ethylcyclopentadienyl)ruthenium, and the like.

摘要翻译： 为了通过CVD法形成质量好的薄钌膜，需要在低温下形成薄膜。 因此，需要具有高热反应性的钌化合物。 本发明涉及以含有（2,4-二甲基戊二烯基）（乙基 - 环戊二烯基）钌和双（2,4-二甲基戊二烯基）钌的钌络合物混合物为原料的CVD等制造含钌膜的方法， 二甲基戊二烯基）钌，后者化合物的量为（2,4-二甲基戊二烯基）（乙基环戊二烯基）钌的重量为0.1〜100重量％。

公开(公告)号：US20120227625A1

公开(公告)日：2012-09-13

申请号：US13504573

申请日：2010-11-29

申请人： Atsushi Maniwa ,  Noriaki Oshima ,  Kazuhisa Kawano ,  Taishi Furukawa ,  Hirokazu Chiba ,  Toshiki Yamamoto

发明人： Atsushi Maniwa ,  Noriaki Oshima ,  Kazuhisa Kawano ,  Taishi Furukawa ,  Hirokazu Chiba ,  Toshiki Yamamoto

IPC分类号： C07F15/00

CPC分类号： C07F17/02 ,  C23C16/18 ,  H01L21/28088 ,  H01L21/28556 ,  H01L21/31695 ,  H01L21/32051 ,  H01L29/4966

摘要： For forming a thin ruthenium film of good quality by CVD method, it is necessary to form the thin film at low temperature. There hence is a desire for a ruthenium compound having a high reactivity to heat. This invention relates to a method of producing a ruthenium-containing film by CVD or the like using, as a raw material, a ruthenium complex mixture containing (2,4-dimethylpentadienyl)(ethyl-cyclopentadienyl)ruthenium and bis(2,4-dimethylpentadienyl)ruthenium, the amount of the latter compound being 0.1 to 100% by weight based on the weight of (2,4-dimethylpentadienyl)(ethylcyclopentadienyl)ruthenium, and the like.

摘要翻译： 为了通过CVD法形成质量好的薄钌膜，需要在低温下形成薄膜。 因此，需要具有高热反应性的钌化合物。 本发明涉及以含有（2,4-二甲基戊二烯基）（乙基 - 环戊二烯基）钌和双（2,4-二甲基戊二烯基）钌的钌络合物混合物为原料的CVD等制造含钌膜的方法， 二甲基戊二烯基）钌，后者化合物的量为（2,4-二甲基戊二烯基）（乙基环戊二烯基）钌的重量为0.1〜100重量％。

公开(公告)号：US08748644B2

公开(公告)日：2014-06-10

申请号：US13129589

申请日：2009-12-21

申请人： Taishi Furukawa ,  Noriaki Oshima ,  Kazuhisa Kawano ,  Hirokazu Chiba

发明人： Taishi Furukawa ,  Noriaki Oshima ,  Kazuhisa Kawano ,  Hirokazu Chiba

IPC分类号： C07F17/02 ,  B01J31/00 ,  C07F15/00 ,  B01J31/22

CPC分类号： C07F17/02 ,  B01J31/2295 ,  C07F15/0046 ,  C23C16/18 ,  H01L28/65

摘要： This invention aims at providing (2,4-dimethylpentadienyl)-(ethylcyclopentadienyl)ruthenium which may contain its related structure compound, from which a ruthenium-containing thin film can be produced; a method of producing the same; a method of producing the ruthenium-containing thin film using the same; the ruthenium-containing thin film; and the like. The invention relates to producing the thin film using, as a precursor, (2,4-dimethylpentadienyl)(ethylcyclopentadienyl)ruthenium containing the related structure compound in an amount not more than 5% by weight, which can be obtained by separating the related structure compound from (2,4-dimethylpentadienyl)(ethylcyclopentadienyl)ruthenium containing the related structure compound.

摘要翻译： 本发明的目的在于提供可含有其相关结构化合物的（2,4-二甲基戊二烯基） - （乙基环戊二烯基）钌，由此可以制备含钌的薄膜; 其制造方法; 使用该含钌的薄膜的制造方法; 含钌的薄膜; 等等。 本发明涉及使用含有不超过5重量％的相关结构化合物作为前体的（2,4-二甲基戊二烯基）（乙基环戊二烯基）钌作为前体制备薄膜，其可以通过分离相关结构 含有相关结构化合物的（2,4-二甲基戊二烯基）（乙基环戊二烯基）钌的化合物。

公开(公告)号：US07906668B2

公开(公告)日：2011-03-15

申请号：US12439364

申请日：2007-08-20

申请人： Ken-ichi Tada ,  Taishi Furukawa ,  Koichiro Inaba ,  Tadahiro Yotsuya ,  Hirokazu Chiba ,  Toshiki Yamamoto ,  Tetsu Yamakawa ,  Noriaki Oshima

发明人： Ken-ichi Tada ,  Taishi Furukawa ,  Koichiro Inaba ,  Tadahiro Yotsuya ,  Hirokazu Chiba ,  Toshiki Yamamoto ,  Tetsu Yamakawa ,  Noriaki Oshima

IPC分类号： C07F9/00 ,  C23C16/00

CPC分类号： C23C16/18 ,  C01G33/00 ,  C01G35/00 ,  C01P2002/88 ,  C07C211/65 ,  C07C251/08 ,  C07F9/005 ,  C23C16/405

摘要： Objects of the present invention are to provide a novel niobium or tantalum complex having good vapor pressure and becoming a raw material for producing a niobium- or tantalum-containing thin film by a method such as CVD method, ALD method or the like, a method for producing the same, a metal-containing thin film using the same, and a method for producing the same. The present invention relates to producing an imide complex represented by the general formula (1) by, for example, the reaction between M1(NR1)X3(L)r (2) and an alkali metal alkoxide (3): (wherein M1 represents niobium atom or tantalum atom, R1 represents an alkyl group having from 1 to 12 carbon atoms, R2 represents an alkyl group having from 2 to 13 carbon atoms, X represents halogen atom, r is 1 when L is 1,2-dimethoxyethane ligand, r is 2 when L is pyridine ligand, and M2 represents an alkali metal), and producing a niobium- or tantalum-containing thin film by using the imide complex (1) as a raw material.

摘要翻译： 本发明的目的是提供一种具有良好蒸气压的新型铌或钽络合物，并且通过诸如CVD法，ALD法等的方法成为生产含铌或钽的薄膜的原料， 为了制造它们，使用该薄膜的含金属薄膜及其制造方法。 本发明涉及通过例如M1（NR1）X3（L）r（2）和碱金属醇盐（3）之间的反应来制备由通式（1）表示的酰亚胺络合物：（其中M1表示 铌原子或钽原子，R1表示碳原子数1〜12的烷基，R2表示碳原子数2〜13的烷基，X表示卤素原子，当L为1,2-二甲氧基乙烷配体时，r为1， 当L为吡啶配体时，r为2，M2表示碱金属，通过使用酰亚胺络合物（1）作为原料制造含有铌或钽的薄膜。

公开(公告)号：US20100010248A1

公开(公告)日：2010-01-14

申请号：US12439364

申请日：2007-08-20

申请人： Ken-ichi Tada ,  Taishi Furukawa ,  Koichiro Inaba ,  Tadahiro Yotsuya ,  Hirokazu Chiba ,  Toshiki Yamamoto ,  Tetsu Yamakawa ,  Noriaki Oshima

发明人： Ken-ichi Tada ,  Taishi Furukawa ,  Koichiro Inaba ,  Tadahiro Yotsuya ,  Hirokazu Chiba ,  Toshiki Yamamoto ,  Tetsu Yamakawa ,  Noriaki Oshima

IPC分类号： C07F19/00

CPC分类号： C23C16/18 ,  C01G33/00 ,  C01G35/00 ,  C01P2002/88 ,  C07C211/65 ,  C07C251/08 ,  C07F9/005 ,  C23C16/405

摘要： Objects of the present invention are to provide a novel niobium or tantalum complex having good vapor pressure and becoming a raw material for producing a niobium- or tantalum-containing thin film by a method such as CVD method, ALD method or the like, a method for producing the same, a metal-containing thin film using the same, and a method for producing the same. The present invention relates to producing an imide complex represented by the general formula (1) by, for example, the reaction between M1(NR1)X3(L)r (2) and an alkali metal alkoxide (3): (wherein M1 represents niobium atom or tantalum atom, R1 represents an alkyl group having from 1 to 12 carbon atoms, R2 represents an alkyl group having from 2 to 13 carbon atoms, X represents halogen atom, r is 1 when L is 1,2-dimethoxyethane ligand, r is 2 when L is pyridine ligand, and M2 represents an alkali metal), and producing a niobium- or tantalum-containing thin film by using the imide complex (1) as a raw material.

摘要翻译： 本发明的目的是提供一种具有良好蒸气压的新型铌或钽络合物，并且通过诸如CVD法，ALD法等的方法成为生产含铌或钽的薄膜的原料， 为了制造它们，使用该薄膜的含金属薄膜及其制造方法。 本发明涉及通过例如M1（NR1）X3（L）r（2）和碱金属醇盐（3）之间的反应来制备由通式（1）表示的酰亚胺络合物：（其中M1表示 铌原子或钽原子，R1表示碳原子数1〜12的烷基，R2表示碳原子数2〜13的烷基，X表示卤素原子，当L为1,2-二甲氧基乙烷配体时，r为1， 当L为吡啶配体时，r为2，M2表示碱金属，通过使用酰亚胺络合物（1）作为原料制造含有铌或钽的薄膜。

公开(公告)号：US08779174B2

公开(公告)日：2014-07-15

申请号：US12996690

申请日：2009-06-12

申请人： Ken-ichi Tada ,  Toshiki Yamamoto ,  Hirokazu Chiba ,  Kohei Iwanaga ,  Atsushi Maniwa ,  Tadahiro Yotsuya ,  Noriaki Oshima

发明人： Ken-ichi Tada ,  Toshiki Yamamoto ,  Hirokazu Chiba ,  Kohei Iwanaga ,  Atsushi Maniwa ,  Tadahiro Yotsuya ,  Noriaki Oshima

IPC分类号： C07F7/28

CPC分类号： H01L21/28556 ,  B01J21/063 ,  B01J31/1805 ,  B01J35/004 ,  B01J2531/46 ,  C07C209/54 ,  C07C209/66 ,  C07C211/65 ,  C07C251/08 ,  C07F7/003 ,  C23C16/405 ,  C23C16/45553 ,  H01L21/02186 ,  H01L21/02271

摘要： A subject for the invention is to provide novel titanium complexes which have a high vapor pressure and high thermal stability and serve as an excellent material for producing a titanium-containing thin film by a technique such as the CVD method or ALD method and to further provide processes for producing these complexes, titanium-containing thin films produced from the complexes, and a process for producing the thin films. The invention relates to producing a titanium complex represented by general formula (1): (wherein R1 and R4 each independently represent an alkyl group having 1-16 carbon atoms; R2 and R3 each independently represent a hydrogen atom or an alkyl group having 1-3 carbon atoms; and R5 represents an alkyl group which has 1-16 carbon atoms and may have been substituted with one or more fluorine atoms) and to producing a titanium-containing thin film using the complex.

摘要翻译： 本发明的主题是提供具有高蒸气压和高热稳定性的新型钛络合物，并且通过诸如CVD法或ALD法的技术制造含钛薄膜的优异材料，并进一步提供 用于制备这些络合物的方法，由络合物制备的含钛薄膜以及薄膜的制造方法。 本发明涉及制备由通式（1）表示的钛络合物：（其中R 1和R 4各自独立地表示具有1-16个碳原子的烷基; R 2和R 3各自独立地表示氢原子或具有1- 3个碳原子; R5表示具有1-16个碳原子并且可以被一个或多个氟原子取代的烷基），并使用该络合物制备含钛薄膜。

公开(公告)号：US20120029220A1

公开(公告)日：2012-02-02

申请号：US12996690

申请日：2009-06-12

申请人： Ken-ichi Tada ,  Toshiki Yamamoto ,  Hirokazu Chiba ,  Kohei Iwanaga ,  Atsushi Maniwa ,  Tadahiro Yotsuya ,  Noriaki Oshima

发明人： Ken-ichi Tada ,  Toshiki Yamamoto ,  Hirokazu Chiba ,  Kohei Iwanaga ,  Atsushi Maniwa ,  Tadahiro Yotsuya ,  Noriaki Oshima

IPC分类号： C07F7/28

CPC分类号： H01L21/28556 ,  B01J21/063 ,  B01J31/1805 ,  B01J35/004 ,  B01J2531/46 ,  C07C209/54 ,  C07C209/66 ,  C07C211/65 ,  C07C251/08 ,  C07F7/003 ,  C23C16/405 ,  C23C16/45553 ,  H01L21/02186 ,  H01L21/02271

摘要： A subject for the invention is to provide novel titanium complexes which have a high vapor pressure and high thermal stability and serve as an excellent material for producing a titanium-containing thin film by a technique such as the CVD method or ALD method and to further provide processes for producing these complexes, titanium-containing thin films produced from the complexes, and a process for producing the thin films. The invention relates to producing a titanium complex represented by general formula (1): (wherein R1 and R4 each independently represent an alkyl group having 1-16 carbon atoms; R2 and R3 each independently represent a hydrogen atom or an alkyl group having 1-3 carbon atoms; and R5 represents an alkyl group which has 1-16 carbon atoms and may have been substituted with one or more fluorine atoms) and to producing a titanium-containing thin film using the complex.

摘要翻译： 本发明的主题是提供具有高蒸气压和高热稳定性的新型钛络合物，并且通过诸如CVD法或ALD法的技术制造含钛薄膜的优异材料，并进一步提供 用于制备这些络合物的方法，由络合物制备的含钛薄膜以及薄膜的制造方法。 本发明涉及制备由通式（1）表示的钛络合物：（其中R 1和R 4各自独立地表示具有1-16个碳原子的烷基; R 2和R 3各自独立地表示氢原子或具有1- 3个碳原子; R5表示具有1-16个碳原子并且可以被一个或多个氟原子取代的烷基），并使用该络合物制备含钛薄膜。

公开(公告)号：US20090036697A1

公开(公告)日：2009-02-05

申请号：US12093389

申请日：2006-11-01

申请人： Ken-ichi Tada ,  Koichiro Inaba ,  Taishi Furukawa ,  Hirokazu Chiba ,  Tetsu Yamakawa ,  Noriaki Oshima

发明人： Ken-ichi Tada ,  Koichiro Inaba ,  Taishi Furukawa ,  Hirokazu Chiba ,  Tetsu Yamakawa ,  Noriaki Oshima

IPC分类号： C07F7/28

CPC分类号： C23C16/18 ,  C07C211/65 ,  C07C251/08 ,  C07F7/003 ,  C23C16/34 ,  C23C16/405

摘要： Objects of the present invention are to provide a novel titanium complex that has good vaporization characteristics and an excellent thermal stability, and becomes a raw material for forming a titanium-containing thin film by methods such as CVD method or ALD method, its production method, a titanium-containing thin film formed using the same, and its formation method. In the invention, a titanium complex represented by the general formula (1) is produced by reacting a diimine represented by the general formula (2) and metallic lithium, and then reacting a tetrakisamide complex represented by the general formula (3). (In the formulae, R1 and R4 represent an alkyl group having from 1 to 6 carbon atoms. R2 and R3 each independently represents a hydrogen atom or an alkyl group having from 1 to 3 carbon atoms. R5 and R6 each independently represents an alkyl group having from 1 to 4 carbon atoms.).

摘要翻译： 本发明的目的是提供具有良好的蒸发特性和优异的热稳定性的新颖的钛络合物，并且成为通过CVD法或ALD法等方法形成含钛薄膜的原料，其制造方法， 使用其形成的含钛薄膜及其形成方法。 在本发明中，由通式（1）表示的钛络合物通过使由通式（2）表示的二亚氨基与金属锂反应，然后使由通式（3）表示的四酰胺配合物反应来制备。 （式中，R 1和R 4表示碳原子数1〜6的烷基，R 2和R 3各自独立地表示氢原子或碳原子数1〜3的烷基，R 5和R 6各自独立地表示烷基 具有1至4个碳原子）。

公开(公告)号：US06605735B2

公开(公告)日：2003-08-12

申请号：US10236914

申请日：2002-09-09

申请人： Kazuhisa Kawano ,  Kenichi Sekimoto ,  Noriaki Oshima ,  Tetsuo Shibutami ,  Shuji Kumagai ,  Taishi Furukawa

发明人： Kazuhisa Kawano ,  Kenichi Sekimoto ,  Noriaki Oshima ,  Tetsuo Shibutami ,  Shuji Kumagai ,  Taishi Furukawa

IPC分类号： C07F1702

CPC分类号： C07F17/02 ,  C23C16/18

摘要： A ruthenium-containing thin film is produced by the chemical vapor deposition method etc. with the use of an organometallic ruthenium compound represented by the general formula (1), specific example of which is (2,4-dimethyl-pentadienyl)(ethylcyclopentadienyl)ruthenium: or an organometallic ruthenium compound represented by the general formula (7), specific example of which is carbonylbis(2-methyl-1,3-pentadiene)ruthenium: as the precursor.

摘要翻译： 通过使用由通式（1）表示的有机金属钌化合物的化学气相沉积法等制备含钌的薄膜，其具体实例为（2,4-二甲基 - 戊二烯基）（乙基环戊二烯基） 钌或由通式（7）表示的有机金属钌化合物，其具体实例是羰基双（2-甲基-1,3-戊二烯）钌：作为前体。

公开(公告)号：US07632958B2

公开(公告)日：2009-12-15

申请号：US12093389

申请日：2006-11-01

申请人： Ken-ichi Tada ,  Koichiro Inaba ,  Taishi Furukawa ,  Hirokazu Chiba ,  Tetsu Yamakawa ,  Noriaki Oshima

发明人： Ken-ichi Tada ,  Koichiro Inaba ,  Taishi Furukawa ,  Hirokazu Chiba ,  Tetsu Yamakawa ,  Noriaki Oshima

IPC分类号： C07F7/28 ,  C23C16/00

CPC分类号： C23C16/18 ,  C07C211/65 ,  C07C251/08 ,  C07F7/003 ,  C23C16/34 ,  C23C16/405

摘要： Objects of the present invention are to provide a novel titanium complex that has good vaporization characteristics and an excellent thermal stability, and becomes a raw material for forming a titanium-containing thin film by methods such as CVD method or ALD method, its production method, a titanium-containing thin film formed using the same, and its formation method. In the invention, a titanium complex represented by the general formula (1) is produced by reacting a diimine represented by the general formula (2) and metallic lithium, and then reacting a tetrakisamide complex represented by the general formula (3). (In the formulae, R1 and R4 represent an alkyl group having from 1 to 6 carbon atoms. R2 and R3 each independently represents a hydrogen atom or an alkyl group having from 1 to 3 carbon atoms. R5 and R6 each independently represents an alkyl group having from 1 to 4 carbon atoms.).

摘要翻译： 本发明的目的是提供具有良好的蒸发特性和优异的热稳定性的新颖的钛络合物，并且成为通过CVD法或ALD法等方法形成含钛薄膜的原料，其制造方法， 使用其形成的含钛薄膜及其形成方法。 在本发明中，由通式（1）表示的钛络合物通过使由通式（2）表示的二亚氨基与金属锂反应，然后使由通式（3）表示的四酰胺配合物反应来制备。 （式中，R 1和R 4表示碳原子数1〜6的烷基，R 2和R 3各自独立地表示氢原子或碳原子数1〜3的烷基，R 5和R 6各自独立地表示烷基 具有1至4个碳原子）。