公开(公告)号：US09108997B2

公开(公告)日：2015-08-18

申请号：US14396861

申请日：2013-06-06

Applicant: TANAKA KIKINZOKU KOGYO K.K.

Inventor： Ryosuke Harada ,  Shunichi Nabeya ,  Toshiyuki Shigetomi ,  Masayuki Saito

IPC: C07F17/02 ,  C07F15/00 ,  B01J23/44 ,  C07C45/79 ,  C07C45/85 ,  B01J23/42 ,  B01J23/46 ,  B01J25/02

CPC classification number: C07F15/0046 ,  B01J23/42 ,  B01J23/44 ,  B01J23/462 ,  B01J25/02 ,  C07C45/79 ,  C07C45/85 ,  C07C49/92

Abstract: The present invention is a method for recycling an organic ruthenium compound for chemical vapor deposition, wherein an unreacted organic ruthenium compound is extracted from a used raw material through a thin film formation process. The method includes the following steps (a) to (c). (a) A modification step in which the used raw material and a hydrogenation catalyst are brought into contact with each other in a hydrogen atmosphere, thereby hydrogenating an oxidized organic ruthenium compound in the used raw material. (b) An adsorption step in which the used raw material and an adsorbent are brought into contact with each other, thereby removing impurities in the used raw material. (c) A restoration step in which the used raw material is heated at a temperature that is not lower than −100° C. and not higher than −10° C. with respect to the decomposition temperature of the organic ruthenium compound for eight hours or more, thereby adjusting the ratio of the isomers of the organic ruthenium compound in the used raw material.

Abstract translation: 本发明是一种用于化学气相沉积的有机钌化合物的再循环方法，其中通过薄膜形成方法从使用的原料中提取未反应的有机钌化合物。 该方法包括以下步骤（a）至（c）。 （a）在氢气氛中使使用的原料和氢化催化剂彼此接触的改性步骤，从而使所使用的原料中的氧化的有机钌化合物氢化。 （b）使原料和吸附剂相互接触的吸附工序，除去原料中的杂质。 （c）将有机钌化合物的分解温度在不低于-100℃且不高于-10℃的温度下加热8小时的恢复步骤 以上，由此调整所使用的原料中的有机钌化合物的异构体的比例。

公开(公告)号：US20150225437A1

公开(公告)日：2015-08-13

申请号：US14422292

申请日：2013-08-19

Applicant: Tanaka Kikinzoku Kogyo K.K.

Inventor： Ryosuke Harada ,  Naoki Nakata ,  Masayuki Saito

IPC: C07F15/00 ,  C23C16/46 ,  C23C16/18

CPC classification number: C07F15/0046 ,  C23C16/18 ,  C23C16/46

Abstract: The present invention provides a raw material, formed of a ruthenium complex, for producing a ruthenium thin film or a ruthenium compound thin film by a chemical deposition method, wherein the ruthenium complex is a ruthenium complex represented by the following formula, in which carbonyl groups and a fluoroalkyl derivative of a polyene are coordinated to ruthenium. The present invention provides a raw material for chemical deposition having a preferable decomposition temperature, and the production cost therefor is low: (nR-L)Ru(CO)3  [Chemical Formula 1] wherein L is a polyene having a carbon number of from 4 to 8 and 2 to 4 double bonds, wherein the polyene L has n (n≧1) pieces of substituents Rs, wherein the substituents Rs are each a fluoroalkyl group having a carbon number of from 1 to 6 and a fluorine number of from 1 to 13, and in the case when the polyene L has two or more (n≧2) of the substituents Rs, the carbon numbers and the fluorine numbers of the substituents Rs may be different in the same molecule.

Abstract translation: 本发明提供一种由钌络合物形成的原料，用于通过化学沉积法制备钌薄膜或钌化合物薄膜，其中钌络合物是下式表示的钌络合物，其中羰基 多烯的氟烷基衍生物与钌配位。 本发明提供了具有优选的分解温度的化学沉积用原料，其制造成本低：（nR-L）Ru（CO）3 [化学式1]其中L是碳原子数为 4〜8个和2〜4个双键，其中多烯L具有n（n≥1）个取代基R s，其中取代基R 5各自为碳原子数1〜6的氟代烷基， 在多烯L具有两个以上（n≥2）个取代基Rs的情况下，取代基Rs的碳数和氟数在同一分子中可能不同。