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1. 发明公开

EP2027956A1 PROCESS FOR PRODUCTION OF COLLOIDAL GOLD AND COLLOIDAL GOLD 有权
标题翻译： VERFAHREN ZUR HERSTELLUNG VON KOLLOIDALEM GOLD
公开(公告)号：EP2027956A1
公开(公告)日：2009-02-25
申请号：EP07744338.0
申请日：2007-05-29
申请人： Tanaka Kikinzoku Kogyo K.K.
发明人： TANIUCHI, Junichi , NAKAGAWA, Hirofumi , OKAMOTO, Koji
IPC分类号： B22F9/24 , B01J13/00
CPC分类号： B01J13/0043 , B22F1/0022 , B22F9/24 , B82Y30/00 , Y10S977/896
摘要： It is an object of the present invention to provide a method for producing gold colloid having a targeted particle size, a sharp particle size distribution and a uniform and perfect spherical shape. The present invention relates to a method for producing gold colloid including a nucleation step of forming nuclear colloidal particles by adding a first reducing agent to a first gold salt solution; and a growth step of growing nuclear colloid by adding a second gold salt and a second reducing agent to the solution of the nuclear colloidal particles, characterized in that the growth step is performed at least once; a citrate is used as the first reducing agent and an ascorbate is used as the second reducing agent; and the addition of the ascorbate in the growth step is performed simultaneously with addition of the second gold salt. According to the method for producing gold colloid of the present invention, gold colloid having a sharp particle size distribution and a uniform and perfect spherical shape can be obtained.
摘要翻译：本发明的目的是提供一种具有目标粒度，尖锐的粒度分布和均匀且完美的球形形状的金胶体的制造方法。本发明涉及一种生产金胶体的方法，包括通过向第一金盐溶液中加入第一还原剂形成核胶体颗粒的成核步骤; 以及通过向核胶体粒子的溶液中添加第二金盐和第二还原剂来生长核胶体的生长步骤，其特征在于，所述生长步骤至少进行一次; 使用柠檬酸盐作为第一还原剂，使用抗坏血酸作为第二还原剂; 并且在添加第二金盐的同时进行生长步骤中的抗坏血酸盐的添加。根据本发明的金胶体的制造方法，可以获得具有尖锐的粒度分布和均匀且完美的球形的金胶体。

2. 发明授权

EP2027956B1 PROCESS FOR PRODUCTION OF COLLOIDAL GOLD 有权
标题翻译：生产胶体金的方法
公开(公告)号：EP2027956B1
公开(公告)日：2017-07-05
申请号：EP07744338.0
申请日：2007-05-29
申请人： Tanaka Kikinzoku Kogyo K.K.
发明人： TANIUCHI, Junichi , NAKAGAWA, Hirofumi , OKAMOTO, Koji
IPC分类号： B22F9/24 , B01J13/00 , B82Y30/00 , B22F1/00
CPC分类号： B01J13/0043 , B22F1/0022 , B22F9/24 , B82Y30/00 , Y10S977/896

3. 发明公开

EP3153473A1 METHOD FOR PURIFYING DODECACARBONYL TRIRUTHENIUM 审中-公开
标题翻译： VERFAHREN ZUR REINIGUNG VON DODECACARBONYLTRIRUTHENIUM
公开(公告)号：EP3153473A1
公开(公告)日：2017-04-12
申请号：EP15802466.1
申请日：2015-06-02
申请人： Tanaka Kikinzoku Kogyo K.K.
发明人： NAKAGAWA, Hirofumi , ISHIZAKA, Tasuku , ISHIDA, Hirofumi , KUMAKURA, Akiko
IPC分类号： C01G55/00 , C07F15/00 , C23C16/16
CPC分类号： C01G55/008 , C01P2002/88 , C01P2006/80 , C07F15/00 , C23C16/16
摘要： An object of the present invention is to provide a purification method to give dodecacarbonyl triruthenium (DCR) which serves as a raw material for chemical vapor deposition and does not cause the contamination of a thin film with impurities even when used to form a ruthenium thin film. The present invention relates to a method in which the dissolved oxygen concentration in the solvent is made 0.2 mg/L or less in at least a dissolution stage, and an organic ruthenium compound including DCR as a raw material for chemical vapor deposition is purified by a recrystallization method. The present invention allows a trace amount of impurities to be separated from DCR. When a ruthenium thin film is formed by use of DCR thus obtained, the formed film is hardly contaminated with impurities. Additionally, the purification method of the present invention is also applicable for recovering/purifying DCR after being used for the formation of a ruthenium thin film.
摘要翻译：本发明的目的是提供一种提供用作化学气相沉积原料的十二羰基三钌（DCR）的纯化方法，即使在形成钌薄膜时也不会引起杂质的杂质污染。本发明涉及至少在溶解阶段将溶剂中的溶解氧浓度设定为0.2mg / L以下的方法，将包含作为化学气相沉积原料的DCR的有机钌化合物通过重结晶法。本发明允许微量的杂质与DCR分离。当通过使用由此获得的DCR形成钌薄膜时，形成的膜几乎不被杂质污染。此外，本发明的纯化方法也适用于在用于形成钌薄膜后回收/纯化DCR。

4. 发明授权

EP2740816B1 ORGANIC RUTHENIUM COMPOUND FOR CHEMICAL VAPOR DEPOSITION RAW MATERIAL AND PRODUCTION METHOD FOR SAID ORGANIC RUTHENIUM COMPOUND 有权
标题翻译：用于CVD原料，有机钌方法生产该有机钌
公开(公告)号：EP2740816B1
公开(公告)日：2016-05-04
申请号：EP12819564.1
申请日：2012-07-24
申请人： Tanaka Kikinzoku Kogyo K.K.
发明人： SAITO, Masayuki , TANIUCHI, Junichi , NAKAGAWA, Hirofumi
IPC分类号： C23C16/18 , H01L21/28 , H01L21/285 , C07F15/00 , C01G55/00
CPC分类号： C23C16/16 , C07F15/0046 , C23C16/30 , H01L21/28556

5. 发明公开

EP2740816A1 ORGANIC RUTHENIUM COMPOUND FOR CHEMICAL VAPOR DEPOSITION RAW MATERIAL AND PRODUCTION METHOD FOR SAID ORGANIC RUTHENIUM COMPOUND 有权
标题翻译：用于CVD原料，有机钌方法生产该有机钌
公开(公告)号：EP2740816A1
公开(公告)日：2014-06-11
申请号：EP12819564.1
申请日：2012-07-24
申请人： Tanaka Kikinzoku Kogyo K.K.
发明人： SAITO, Masayuki , TANIUCHI, Junichi , NAKAGAWA, Hirofumi
IPC分类号： C23C16/18 , H01L21/28 , H01L21/285
CPC分类号： C23C16/16 , C07F15/0046 , C23C16/30 , H01L21/28556
摘要： The present invention is an organoruthenium compound for a chemical vapor deposition raw material, including dodecacarbonyl triruthenium represented by the following chemical formula, wherein the iron (Fe) concentration is 1 ppm or less. The DCR in the present invention can be produced by obtaining crude DCR by directly carbonylating ruthenium through allowing a ruthenium salt and carbon monoxide to react with each other and by purifying the crude DCR by a sublimation method. In the synthesis step, the concentration of Fe in the obtained crude DCR is preferably set at 10 ppm or less.
摘要翻译：本发明是一种用于化学气相沉积原料的有机钌化合物，包括由以下化学式表示的十二羰基三钌，worin的铁（Fe）浓度为1ppm或更少。在本发明的DCR可以通过通过允许钌盐和一氧化碳与海誓山盟反应并通过升华法纯化粗DCR直接羰基化获得钌粗DCR来制造。在合成步骤中，Fe中所得到的粗DCR的浓度优选设定为10 ppm以下。

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