公开(公告)号：US10077282B2

公开(公告)日：2018-09-18

申请号：US15558262

申请日：2016-05-09

Applicant: TANAKA KIKINZOKU KOGYO K.K.

Inventor： Ryosuke Harada ,  Toshiyuki Shigetomi ,  Kazuharu Suzuki ,  Shunichi Nabeya ,  Akiko Kumakura ,  Tatsutaka Aoyama ,  Takayuki Sone

IPC: H01L21/31 ,  C07F15/00 ,  C23C16/18 ,  H01L21/285 ,  C09D5/24

CPC classification number: C07F15/0086 ,  C07F15/00 ,  C09D5/24 ,  C23C16/18 ,  H01L21/285 ,  H01L21/28568 ,  H01L21/31

Abstract: The present invention relates to a raw material for chemical deposition shown in a formulae below and including an organoplatinum compound in which diimine containing two imines and an alkyl anion are coordinated to divalent platinum. In the formulae, each of substituents R1 to R4 on the diimine represents a hydrogen atom, an alkyl group or the like and has a carbon number of 5 or less. Each of alkyl anions R5 and R6 is an alkyl group having a carbon number of 1 or more and 3 or less. The raw material has high vapor pressure and low decomposition temperature, and thus it is possible to manufacture a platinum thin film at low temperature.

公开(公告)号：US10465283B2

公开(公告)日：2019-11-05

申请号：US15558057

申请日：2016-05-09

Applicant: TANAKA KIKINZOKU KOGYO K.K.

Inventor： Ryosuke Harada ,  Toshiyuki Shigetomi ,  Kazuharu Suzuki ,  Shunichi Nabeya ,  Akiko Kumakura ,  Rumi Kobayashi ,  Takayuki Sone

IPC: C07F15/00 ,  C23C16/18 ,  C07C211/21 ,  H01L21/285 ,  C23C16/46 ,  H01L49/02

Abstract: An organoplatinum compound with the following formula for use as a raw material in the chemical deposition of platinum compound thin films. In the formula, n is 1 or more and 5 or less. Each of substituents R1 to R5 on the alkenyl amine is a hydrogen atom, an alkyl group or the like and has a carbon number of 4 or less. Each of alkyl anions R6 and R7 is an alkyl group having a carbon number of 1 or more and 3 or less. The vapor pressure of the organoplatinum compound is high enough to allow for the manufacturing of a platinum thin film at low temperature. It also has moderate thermal stability.

公开(公告)号：US10131987B2

公开(公告)日：2018-11-20

申请号：US15514778

申请日：2015-09-24

Applicant: TANAKA KIKINZOKU KOGYO K.K.

Inventor： Ryosuke Harada ,  Toshiyuki Shigetomi ,  Kazuharu Suzuki ,  Shunichi Nabeya ,  Takayuki Sone ,  Akiko Kumakura

IPC: C23C16/18 ,  C07F15/00 ,  H01L21/28 ,  H01L21/285 ,  C07F17/02 ,  C09D1/00

Abstract: The invention provides a raw material for chemical deposition having properties required for a CVD compound, that is, which has a high vapor pressure, can be formed into a film at low temperatures (about 250° C. or less), and also has moderate thermal stability. The invention relates to a raw material for chemical deposition, for producing a ruthenium thin film or a ruthenium compound thin film by a chemical deposition method, the raw material for chemical deposition including an organoruthenium compound represented by the following formula, in which a cyclohexadienyl group or a derivative thereof and a pentadienyl group or a derivative thereof are coordinated to ruthenium: wherein the substituents R1 to R12 are each independently a hydrogen atom, a linear or cyclic hydrocarbon, an amine, an imine, an ether, a ketone, or an ester, and the substituents R1 to R12 each have 6 or less carbon atoms.

公开(公告)号：US10526698B2

公开(公告)日：2020-01-07

申请号：US16277789

申请日：2019-02-15

Applicant: TANAKA KIKINZOKU KOGYO K.K.

Inventor： Ryosuke Harada ,  Toshiyuki Shigetomi ,  Shunichi Nabeya ,  Kazuharu Suzuki ,  Akiko Kumakura ,  Tatsutaka Aoyama ,  Takayuki Sone

IPC: C23C16/18 ,  C07F13/00 ,  C07F15/00 ,  C07F15/02 ,  C07F15/06 ,  C07F17/00 ,  C07F19/00 ,  C23C16/06 ,  C07F15/04

Abstract: The present invention relates to a chemical deposition raw material including a heterogeneous polynuclear complex in which a cyclopentadienyl and a carbonyl are coordinated to a first transition metal and a second transition metal as central metals, the chemical deposition raw material being represented by the following formula. In the following formula, the first transition metal (M1) and the second transition metal (M2) are mutually different. The number of cyclopentadienyls (L) is 1 or more and 2 or less, and to the cyclopentadienyl is coordinated one of a hydrogen atom and an alkyl group with a carbon number of 1 or more and 5 or less as each of substituents R1 to R5. With the chemical deposition raw material of the present invention, a composite metal thin film or a composite metal compound thin film containing plural metals can be formed from a single raw material.

公开(公告)号：US10407450B2

公开(公告)日：2019-09-10

申请号：US15558011

申请日：2016-05-09

Applicant: TANAKA KIKINZOKU KOGYO K.K.

Inventor： Ryosuke Harada ,  Toshiyuki Shigetomi ,  Shunichi Nabeya ,  Kazuharu Suzuki ,  Akiko Kumakura ,  Tatsutaka Aoyama ,  Takayuki Sone

IPC: C07F13/00 ,  C07F15/00 ,  C23C16/16 ,  C07F15/06 ,  C07F19/00 ,  C07C251/08 ,  C23C16/18 ,  H01L21/285 ,  H01L21/31 ,  C23C16/06 ,  C23C16/46 ,  H01L21/02

Abstract: A heterogeneous polynuclear complex for use as a raw material in the chemical deposition of composite metal or composite metal thin films with the below formula. In the formula, M1 and M2 are mutually different transition metals, x is an integer of 0 or more and 2 or less, y is in integer of 1 or more and 2 or less, z is an integer of 1 or more and 10 or less, R1 to R4 are each one of a hydrogen atom and an alkyl group with a carbon number of 1 or more and 5 or less, and R5 is a hydrogen atom, a carbonyl, an alkyl group with a carbon number of 1 or more and 7 or less, an allyl group or an allyl derivative. The heterogeneous polynuclear complex allows a composite metal thin film or a composite metal compound thin film containing a plurality of metals to be formed from a single raw material.

公开(公告)号：US09783429B2

公开(公告)日：2017-10-10

申请号：US15312355

申请日：2015-06-02

Applicant: TANAKA KIKINZOKU KOGYO K.K.

Inventor： Hirofumi Nakagawa ,  Tasuku Ishizaka ,  Hirofumi Ishida ,  Akiko Kumakura

IPC: C01G55/00

CPC classification number: C01G55/008 ,  C01P2002/88 ,  C01P2006/80 ,  C07F15/00 ,  C23C16/16

Abstract: 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.

公开(公告)号：US09499411B2

公开(公告)日：2016-11-22

申请号：US15030084

申请日：2014-10-14

Applicant: Tanaka Kikinzoku Kogyo K.K.

Inventor： Hirofumi Nakagawa ,  Tasuku Ishizaka ,  Hirofumi Ishida ,  Ken Hagiwara ,  Akiko Kumakura

IPC: C01G55/00 ,  B01D7/00 ,  C23C16/16

CPC classification number: C01G55/008 ,  B01D7/00 ,  C01P2006/80 ,  C23C16/16

Abstract: The present invention provides a method for producing DCR that can efficiently sublimate a large amount of crude DCR to stably supply DCR. Also, the present invention relates to a sublimation apparatus applicable to the production method. The method for producing an organoruthenium compound for a chemical vapor deposition raw material containing dodecacarbonyl triruthenium (DCR) includes the step for purifying DCR by separating impurity elements from crude DCR by a sublimation method, and in the purification step, crude DCR is heated and sublimated in an atmosphere having a carbon monoxide concentration of 30 to 100% and then cooled to precipitate DCR. According to the present invention, a large amount of crude DCR can be efficiently sublimated, and thus a large amount of DCR can be supplied stably.

Abstract translation: 本发明提供一种能够有效地升华大量粗制DCR以稳定地供应DCR的DCR的制造方法。 此外，本发明涉及适用于生产方法的升华装置。 用于含有十二羰基三钌（DCR）的化学气相沉积原料的有机钌化合物的制备方法包括通过升华法从粗DCR中分离杂质元素来纯化DCR的步骤，在纯化步骤中，将粗DCR加热升华 在一氧化碳浓度为30〜100％的气氛中，然后冷却以沉淀DCR。 根据本发明，能够有效地升华大量的粗制DCR，能够稳定地供给大量的DCR。