公开(公告)号：US10538543B2

公开(公告)日：2020-01-21

申请号：US16331978

申请日：2017-10-12

Applicant: NATIONAL INSTITUTE OF ADVANCED INDUSTRIAL SCIENCE AND TECHNOLOGY ,  TANAKA KIKINZOKU KOGYO K.K.

Inventor： Hideo Konno ,  Junichi Taniuchi ,  Rumi Kobayashi ,  Yasushi Masahiro

IPC: C07F15/00

Abstract: The present invention provides a method for producing a cyclometalated iridium complex, the method including producing a cyclometalated iridium complex by reacting a cyclometalated iridium complex raw material including an organoiridium material with an aromatic heterocyclic bidentate ligand capable of forming an iridium-carbon bond and an iridium-nitrogen bond, and using as the raw material an organoiridium material represented by the following general formula (1). The present invention allows a cyclometalated iridium complex to be produced with a high yield without by-production of a halogen-crosslinked iridium dimer.

公开(公告)号：US10533027B2

公开(公告)日：2020-01-14

申请号：US16060105

申请日：2016-12-22

Applicant: TANAKA KIKINZOKU KOGYO K.K. ,  NATIONAL INSTITUTE OF ADVANCED INDUSTRIAL SCIENCE AND TECHNOLOGY

Inventor： Hideo Konno ,  Junichi Taniuchi ,  Ryosuke Harada ,  Toshiyuki Shigetomi ,  Rumi Kobayashi ,  Yasushi Masahiro

IPC: C07F15/00 ,  C09K11/06 ,  H01L51/00 ,  H01L51/50

Abstract: The present invention provides a method for producing a cyclometalated iridium complex by use of a non-chlorine iridium raw material. The method for producing a cyclometalated iridium complex includes producing a cyclometalated iridium complex by reacting a raw material including an iridium compound with an aromatic heterocyclic bidentate ligand capable of forming an iridium-carbon bond, the raw material being non-halogenated iridium having a conjugated base of a strong acid as a ligand. Here, the non-halogenated iridium is preferably one containing a conjugated base of a strong acid having a pKa of 3 or less as a ligand.

公开(公告)号：US09793499B2

公开(公告)日：2017-10-17

申请号：US15314648

申请日：2015-06-09

Applicant: Tanaka Kikinzoku Kogyo K.K. ,  Osaka Prefecture University Public Corporation

Inventor： Yasushi Masahiro ,  Shigeyuki Yagi ,  Junichi Taniuchi

IPC: C07F15/00 ,  H01L51/50 ,  H01L51/00 ,  C09K11/02 ,  C09K11/06

CPC classification number: H01L51/0085 ,  C07F15/0033 ,  C09K11/025 ,  C09K11/06 ,  C09K2211/1007 ,  C09K2211/1011 ,  C09K2211/1029 ,  C09K2211/1088 ,  C09K2211/1092 ,  C09K2211/185 ,  H01L51/5016

Abstract: The present invention provides an organic metal complex having high heat resistance while making it possible to realize electroluminescence with high quantum efficiency as a light-emitting material for organic electroluminescent (EL) element. The present invention relates to an organic iridium complex for an organic EL element, wherein a C—N ligand including a substituent of a tricyclic-based structure obtained by condensing a heterocyclic ring and two benzene rings, and a β-diketone ligand composed of a propane-1,3-dione having two tert-butyl-substituted phenyl groups are coordinated with an iridium atom. The complex of the present invention has high heat resistance and contributes to lifetime prolongation of the organic EL element.

公开(公告)号：US20170215279A1

公开(公告)日：2017-07-27

申请号：US15448485

申请日：2017-03-02

Applicant: TANAKA KIKINZOKU KOGYO K.K.

Inventor： Hitoshi Kubo ,  Yusuke Ohshima ,  Noriaki Nakamura ,  Hiroshi Noguchi ,  Junichi Taniuchi ,  Yuichi Makita

IPC: H05K1/09 ,  C09D11/52 ,  B22F1/00 ,  B22F9/30 ,  H01B1/22 ,  H05K3/12

CPC classification number: H05K1/097 ,  B22F1/0044 ,  B22F1/0062 ,  B22F9/30 ,  B22F2001/0066 ,  B22F2998/10 ,  C09D11/52 ,  H01B1/22 ,  H05K3/1291 ,  Y10T428/268 ,  B22F3/10

Abstract: Provided are a fine silver particle ink composed of hexylamine, dodecylamine, oleic acid, fine silver particles and a solvent, in which the volume resistivity of a sintered body at 100° C. obtained after the ink is applied on a substrate by spin coating is 8 to 25 μΩ cm, a sintered body thereof, and a method for producing a fine silver particle ink. When a fine silver particle ink containing coated fine silver particles is produced by a silver-amine complex decomposition method, production can be carried out smoothly. The fine silver particle ink can be sintered even at a low temperature, and a sintered body thereof has a mirror surface and low volume resistance.

公开(公告)号：US10125158B2

公开(公告)日：2018-11-13

申请号：US15503822

申请日：2015-08-28

Applicant: TANAKA KIKINZOKU KOGYO K.K.

Inventor： Yasushi Masahiro ,  Toshiyuki Shigetomi ,  Junichi Taniuchi ,  Ryosuke Harada

IPC: C07C45/77 ,  C07F15/00 ,  C07C49/92 ,  C09K11/06 ,  C23C16/18 ,  H01L51/00 ,  H01L51/50

Abstract: A method for manufacturing tris(β-diketonato)iridium by reacting β-diketone with an iridium compound, in which an activation treatment including (a) an alkali treatment and (b) an acid treatment described below is applied to the iridium compound to activate the iridium compound, and to subsequently react the β-diketone, (a) an alkali treatment: a treatment of adding alkali to a solution of the iridium compound to raise pH of the solution to a more alkaline side than that before the alkali addition and to not less than 10, and (b) an acid treatment: a treatment of adding acid to the solution subjected to the alkali treatment to lower pH of the solution to a more acidic side than that before the acid addition and to make the pH difference between solutions before and after the acid addition be not less than 0.1 and not more than 10. The present invention allows manufacture of tris(β-diketonato)iridium utilizing a wide variety of β-diketones.

公开(公告)号：US09674953B2

公开(公告)日：2017-06-06

申请号：US14614196

申请日：2013-07-11

Applicant: TANAKA KIKINZOKU KOGYO K.K.

Inventor： Hitoshi Kubo ,  Yusuke Ohshima ,  Noriaki Nakamura ,  Hiroshi Noguchi ,  Junichi Taniuchi ,  Yuichi Makita

IPC: H05K1/09 ,  H01B1/22 ,  B22F1/00 ,  C09D11/52 ,  B22F9/30

CPC classification number: H05K1/097 ,  B22F1/0044 ,  B22F1/0062 ,  B22F9/30 ,  B22F2001/0066 ,  B22F2998/10 ,  C09D11/52 ,  H01B1/22 ,  H05K3/1291 ,  Y10T428/268 ,  B22F3/10

Abstract: Provided are a fine silver particle ink composed of hexylamine, dodecylamine, oleic acid, fine silver particles and a solvent, in which the volume resistivity of a sintered body at 100° C. obtained after the ink is applied on a substrate by spin coating is 8 to 25 μΩcm, a sintered body thereof, and a method for producing a fine silver particle ink. When a fine silver particle ink containing coated fine silver particles is produced by a silver-amine complex decomposition method, production can be carried out smoothly. The fine silver particle ink can be sintered even at a low temperature, and a sintered body thereof has a mirror surface and low volume resistance.

公开(公告)号：US09607922B2

公开(公告)日：2017-03-28

申请号：US14778684

申请日：2014-03-03

Applicant: Tanaka Kikinzoku Kogyo K.K.

Inventor： Kenji Matsuda ,  Dai Shinozaki ,  Yuichi Makita ,  Hitoshi Kubo ,  Yusuke Ohshima ,  Hidekazu Matsuda ,  Junichi Taniuchi

IPC: H01L23/34 ,  H01L23/367 ,  H01L23/00 ,  H01L23/373 ,  H01L23/36 ,  H05K7/20

CPC classification number: H01L23/367 ,  H01L23/34 ,  H01L23/36 ,  H01L23/373 ,  H01L23/3736 ,  H01L24/01 ,  H01L2924/0002 ,  H05K7/20409 ,  H01L2924/00

Abstract: A semiconductor device includes a semiconductor chip which can be a heat-generating semiconductor chip or a semiconductor relay substrate in which an integrated circuit or wiring is built in. A sintered-silver-coated film is adhered on a surface layer part of the semiconductor substrate, interposed by a silicon oxide film. A heat-dissipating fin (heat sink), which may be copper or aluminum, is bonded on the sintered-silver-coated film, interposed by an adhesive layer.

公开(公告)号：US20150237742A1

公开(公告)日：2015-08-20

申请号：US14429702

申请日：2013-09-27

Applicant: TANAKA KIKINZOKU KOGYO K.K. ,  A SCHOOL CORPORATION KANSAI UNIVERSITY

Inventor： Noriaki Nakamura ,  Junichi Taniuchi ,  Hitoshi Kubo ,  Yuusuke Ohshima ,  Tomoko Ishikawa ,  Shoso Shingubara ,  Fumihiro Inoue

IPC: H05K3/42 ,  H05K3/38

CPC classification number: H05K3/422 ,  C23C18/1893 ,  C23C18/208 ,  C23C18/2086 ,  C23C18/30 ,  C23C18/34 ,  H05K3/387 ,  H05K3/389 ,  H05K3/426

Abstract: The present invention provides a method for treating a substrate that supports metal fine particles for forming a plating layer on a circuit pattern or TSVs in various substrates, in which further micronization treatment is enabled compared with the conventional methods, and the formation of a stable plating layer is enabled. The present invention is a method for treating a substrate, the method including bringing a substrate into contact with a colloidal solution containing metal particles in order to support the metal particles that serve as a catalyst for forming a plating layer on the substrate, in which the colloidal solution contains metal particles formed of Pd and having a particle size of 0.6 nm to 4.0 nm and a face-to-face dimension of the (111) plane of 2.254 Å or more. When an organic layer such as SAM is formed on a surface of the substrate before this treatment, the binding force of the Pd particles can be increased.

Abstract translation: 本发明提供一种处理基板的方法，该基板用于在各种基板上的电路图形或TSV上支撑用于形成镀层的金属微粒，与常规方法相比，能够进一步进行微粉化处理，并形成稳定的电镀 层被启用。 本发明是一种处理基板的方法，该方法包括使基板与含有金属颗粒的胶体溶液接触，以便支撑用作在基板上形成镀层的催化剂的金属颗粒，其中 胶体溶液含有由Pd形成的并且具有0.6nm至4.0nm的粒径和（111）面的面对面尺寸为2.254或更大的金属颗粒。 当在该处理之前在基板的表面上形成诸如SAM的有机层时，可以增加Pd颗粒的结合力。

公开(公告)号：US09901985B2

公开(公告)日：2018-02-27

申请号：US14891725

申请日：2014-05-20

Applicant: Tanaka Kikinzoku Kogyo K.K.

Inventor： Yuichi Makita ,  Yuusuke Ohshima ,  Hidekazu Matsuda ,  Noriaki Nakamura ,  Junichi Taniuchi ,  Hitoshi Kubo

IPC: B22F9/30 ,  B22F1/00

CPC classification number: B22F9/30 ,  B22F1/0018 ,  B22F2301/255 ,  B22F2304/054 ,  B22F2304/056 ,  B22F2999/00

Abstract: The present invention provides a method for producing silver particles, the method capable of adjusting the particle diameter to be within the range of several tens of nanometers to several hundreds of nanometers and also producing silver particles with a uniform particle diameter. The present invention relates to a method for producing silver particles by heating of a reaction system containing a thermally-decomposable silver-amine complex precursor, including a process of producing a silver-amine complex, a process of adding an organic compound having an amide (carboxylic amide) as a skeleton to a reaction system, and a process of heating the reaction system, in which a water content in the reaction system before the heating is 20 to 100 parts by weight relative to 100 parts by weight of the silver compound. The present invention can produce uniform silver particles while the particle diameter is controlled.

公开(公告)号：US09565776B2

公开(公告)日：2017-02-07

申请号：US14429702

申请日：2013-09-27

Applicant: Tanaka Kikinzoku Kogyo K.K. ,  A School Corporation Kansai University

Inventor： Noriaki Nakamura ,  Junichi Taniuchi ,  Hitoshi Kubo ,  Yuusuke Ohshima ,  Tomoko Ishikawa ,  Shoso Shingubara ,  Fumihiro Inoue

IPC: B05D5/12 ,  H05K3/42 ,  H05K3/38

CPC classification number: H05K3/422 ,  C23C18/1893 ,  C23C18/208 ,  C23C18/2086 ,  C23C18/30 ,  C23C18/34 ,  H05K3/387 ,  H05K3/389 ,  H05K3/426

Abstract: The present invention provides a method for treating a substrate that supports metal fine particles for forming a plating layer on a circuit pattern or TSVs in various substrates, in which further micronization treatment is enabled compared with the conventional methods, and the formation of a stable plating layer is enabled. The present invention is a method for treating a substrate, the method including bringing a substrate into contact with a colloidal solution containing metal particles in order to support the metal particles that serve as a catalyst for forming a plating layer on the substrate, in which the colloidal solution contains metal particles formed of Pd and having a particle size of 0.6 nm to 4.0 nm and a face-to-face dimension of the (111) plane of 2.254 Å or more. When an organic layer such as SAM is formed on a surface of the substrate before this treatment, the binding force of the Pd particles can be increased.

Abstract translation: 本发明提供一种处理基板的方法，该基板用于在各种基板上的电路图形或TSV上支撑用于形成镀层的金属微粒，与常规方法相比，能够进一步进行微粉化处理，并形成稳定的电镀 层被启用。 本发明是一种处理基板的方法，该方法包括使基板与含有金属颗粒的胶体溶液接触，以便支撑用作在基板上形成镀层的催化剂的金属颗粒，其中 胶体溶液含有由Pd形成的并且具有0.6nm至4.0nm的粒径和（111）面的面对面尺寸为2.254或更大的金属颗粒。 当在该处理之前在基板的表面上形成诸如SAM的有机层时，可以增加Pd颗粒的结合力。