公开(公告)号：US20100000872A1

公开(公告)日：2010-01-07

申请号：US12443766

申请日：2007-04-02

申请人： Tetsuya Shimizu ,  Hisayoshi Tajima ,  Seizo Miyata ,  Masato Sone

发明人： Tetsuya Shimizu ,  Hisayoshi Tajima ,  Seizo Miyata ,  Masato Sone

IPC分类号： C25D21/14

CPC分类号： C25D15/02 ,  C25D3/38 ,  C25D5/003 ,  H01L21/2885 ,  H01L21/76877

摘要： The surface of a metal base is electroplated by utilizing an induction codeposition phenomenon using at least one of carbon dioxide and inert gas, an electroplating liquid containing a metal powder dispersed therein, and a surfactant in a supercritical state or a subcritical state. The concentration of the metal in the electroplating liquid is in a saturated or supersaturated state. Accordingly, the dissolution speed of the metal base can be suppressed, and, at the same time, a plating layer having a smooth surface can be formed in a short time by utilizing an induction codeposition phenomenon. The electroplating method can be applied even when the metal base is formed of a metallic thin film provided on a surface of an insulating film provided on the substrate, or even when the metal is copper, zinc, iron, nickel, or cobalt. The above constitution can provide an electroplating method which, in electroplating on the surface of a metal base, can prevent the dissolution of the metal base to realize normal electroplating even in the case of a very thin metal base.

摘要翻译： 使用二氧化碳和惰性气体中的至少一种，含有分散在其中的金属粉末的电镀液体和超临界状态或亚临界状态的表面活性剂，利用感应共沉淀现象对金属基体的表面进行电镀。 电镀液中金属的浓度处于饱和或过饱和状态。 因此，可以抑制金属基体的溶解速度，并且同时可以通过利用感应共沉积现象在短时间内形成具有光滑表面的镀层。 即使当金属基底由设置在基板上的绝缘膜的表面上设置的金属薄膜形成时，或甚至当金属为铜，锌，铁，镍或钴时，也可以应用电镀方法。 上述结构可以提供一种电镀方法，即使在非常薄的金属基底的情况下，在金属基体表面的电镀中也能够防止金属基体的溶解，从而实现正常的电镀。

公开(公告)号：US20100092661A1

公开(公告)日：2010-04-15

申请号：US12447013

申请日：2007-10-24

申请人： Tetsuya Shimizu ,  Hisayoshi Tajima ,  Seizo Miyata ,  Masato Sone

发明人： Tetsuya Shimizu ,  Hisayoshi Tajima ,  Seizo Miyata ,  Masato Sone

IPC分类号： B05D1/12

CPC分类号： C23C18/00 ,  C23C18/1682 ,  C23C18/1685 ,  C23C18/31 ,  H01L21/288 ,  H01L21/76877

摘要： This invention provides an electroless plating method comprising electrolessly plating the surface of a metal base sample using a supercritical fluid or a subcritical fluid in such a state that a metal powder is dispersed in an electroless plating liquid. According to this method, a homogeneous and thick plating layer is formed in a short time by taking advantage of an induction eutectoid phenomenon. In the electroless plating method, the metal powder may have an average particle diameter of not less than 1 nm and not more than 100 &mgr;m, and the electroless plating method may also be applied to a damascene process or a dual damascene process which is a method for forming a fine metal wiring within a semiconductor element. The above constitution can provide an electroless plating method which can realize the formation of an even film by electroless plating in a short time using a subcritical fluid or a supercritical fluid by taking advantage of an induction eutectoid phenomenon.

摘要翻译： 本发明提供了一种化学镀方法，其包括使金属粉末分散在无电镀液中的状态，使用超临界流体或亚临界流体对金属基体样品的表面进行无电镀。 根据该方法，通过利用感应共析现象，在短时间内形成均匀且厚的镀层。 在化学镀方法中，金属粉末的平均粒径可以不小于1nm且不大于100μm，并且化学镀方法也可以应用于镶嵌工艺或双镶嵌工艺，其为 一种在半导体元件内形成精细金属布线的方法。 上述结构可以提供一种化学镀方法，其可以通过利用诱导共析现象利用亚临界流体或超临界流体在短时间内通过无电解电镀实现均匀的膜的形成。

公开(公告)号：US07857952B2

公开(公告)日：2010-12-28

申请号：US11981136

申请日：2007-10-31

申请人： Hideo Yoshida ,  Seizo Miyata ,  Masato Sone ,  Nobuyoshi Sato

发明人： Hideo Yoshida ,  Seizo Miyata ,  Masato Sone ,  Nobuyoshi Sato

IPC分类号： C25D17/06

CPC分类号： B08B3/14 ,  C25D5/00 ,  C25D5/08 ,  C25D17/00 ,  C25D21/04 ,  H01L21/02052 ,  H01L21/2885 ,  H01L21/32134

摘要： An apparatus for treating the surface of an object to be treated comprising introducing a surface treatment fluid into a reaction vessel (4) capable of receiving an object, introducing the surface treatment fluid into a separation vessel (14) after the object is subjected to surface treatment, and circulating the surface treatment fluid, from which a contaminant has already been removed, to the reaction vessel (4). At the time of treatment on the surface of the object, a circulation passage for the surface treatment fluid including the reaction vessel (4) is communicated and the surface treatment fluid is constantly circulated through the circulation passage.

摘要翻译： 一种用于处理待处理物体的表面的装置，包括将表面处理流体引入到能够接收物体的反应容器（4）中，在物体经受表面之后将表面处理流体引入分离容器（14） 处理，并且将已经从其中除去污染物的表面处理流体循环到反应容器（4）。 在物体表面处理时，包括反应容器（4）的表面处理流体的循环通道连通，表面处理流体不断循环通过循环通道。

公开(公告)号：US07323096B2

公开(公告)日：2008-01-29

申请号：US10416678

申请日：2002-10-29

申请人： Hideo Yoshida ,  Seizo Miyata ,  Masato Sone ,  Nobuyoshi Sato

发明人： Hideo Yoshida ,  Seizo Miyata ,  Masato Sone ,  Nobuyoshi Sato

IPC分类号： C25D21/18

CPC分类号： B08B3/14 ,  C25D5/00 ,  C25D5/08 ,  C25D17/00 ,  C25D21/04 ,  H01L21/02052 ,  H01L21/2885 ,  H01L21/32134

摘要： A method for treating the surface of an object to be treated includes introducing a surface treatment fluid into a reaction vessel (4) capable of receiving an object, introducing-the surface treatment fluid into a separation vessel (14) after the object is subjected to surface treatment, and circulating the surface treatment fluid, from which a contaminant has already been removed, to the reaction vessel (4).At the time of treatment on the surface of the object, a circulation passage for the surface treatment fluid including the reaction vessel (4) is communicated and the surface treatment fluid is constantly circulated through the circulation passage.

摘要翻译： 处理被处理物的表面的方法包括将表面处理流体引入到能够接收物体的反应容器（4）中，在所述物体经受所述物体后将所述表面处理流体引入分离容器（14） 表面处理，并将表面处理流体（已经从中除去污染物）循环到反应容器（4）中。 在物体表面处理时，包括反应容器（4）的表面处理流体的循环通道连通，表面处理流体不断循环通过循环通道。

公开(公告)号：US06793793B2

公开(公告)日：2004-09-21

申请号：US10070516

申请日：2002-03-04

申请人： Hideo Yoshida ,  Seizo Miyata ,  Yoshihiro Asai ,  Masato Sone ,  Fumiko Iwao ,  Hiroe Asai

发明人： Hideo Yoshida ,  Seizo Miyata ,  Yoshihiro Asai ,  Masato Sone ,  Fumiko Iwao ,  Hiroe Asai

IPC分类号： C25D500

CPC分类号： C25D3/02 ,  B23H3/08 ,  C23C18/1685 ,  C23C22/18 ,  C23C22/24 ,  C25D5/003 ,  C25D5/34 ,  C25D5/48 ,  C25D11/005 ,  C25D11/02 ,  C25D11/04 ,  C25D13/00 ,  C25D17/02 ,  C25F3/00

摘要： A novel method of electrochemical treatment such as electroplating, etc. and an electrochemical reaction apparatus thereof which is high in reactability and able to be electrochemically reacted efficiently, which is small or zero in amount of generation of liquid waste such as electrolytic solution and cleaning liquid and therefore, amicable to the environment, and in which it is no more required to clean the electrode, etc. with cleaning liquid after reaction. Electrochemical reaction is executed in a reaction vessel (6) containing matter (5) which is in a supercritical or subcritical state and an electrolytic solution (1), and after reaction, the supercritical or subcritical matter (5) is shifted into a state of the matter (5) before being shifted into a critical state.

摘要翻译： 电化学等电化学处理的新方法及其电化学反应装置，其反应性高，能够高效电化学反应，电解液和清洗液等液体废液的产生量小或为零 因此与环境友好，反应后用清洗液清洗电极等不再需要。 在含有超临界或亚临界状态的物质（5）和电解液（1）的反应容器（6）中进行电化学反应，反应后，将超临界或亚临界物质（5）转移到 事情（5）在转入危急状态之前。

公开(公告)号：US20080210554A1

公开(公告)日：2008-09-04

申请号：US11981136

申请日：2007-10-31

申请人： Hideo Yoshida ,  Seizo Miyata ,  Masato Sone ,  Nobuyoshi Sato

发明人： Hideo Yoshida ,  Seizo Miyata ,  Masato Sone ,  Nobuyoshi Sato

IPC分类号： C25B9/00

CPC分类号： B08B3/14 ,  C25D5/00 ,  C25D5/08 ,  C25D17/00 ,  C25D21/04 ,  H01L21/02052 ,  H01L21/2885 ,  H01L21/32134

摘要： An apparatus for treating the surface of an object to be treated comprising introducing a surface treatment fluid into a reaction vessel (4) capable of receiving an object, introducing the surface treatment fluid into a separation vessel (14) after the object is subjected to surface treatment, and circulating the surface treatment fluid, from which a contaminant has already been removed, to the reaction vessel (4). At the time of treatment on the surface of the object, a circulation passage for the surface treatment fluid including the reaction vessel (4) is communicated and the surface treatment fluid is constantly circulated through the circulation passage.

摘要翻译： 一种用于处理待处理物体的表面的装置，包括将表面处理流体引入到能够接收物体的反应容器（4）中，在物体经受表面之后将表面处理流体引入分离容器（14） 处理，并且将已经从其中除去污染物的表面处理流体循环到反应容器（4）。 在物体表面处理时，包括反应容器（4）的表面处理流体的循环通道连通，表面处理流体不断循环通过循环通道。

公开(公告)号：US08172916B2

公开(公告)日：2012-05-08

申请号：US13046372

申请日：2011-03-11

申请人： Tadamasa Fujimura ,  Masato Sone ,  Valeri Yu Dolmatov ,  Shigeru Shiozaki

发明人： Tadamasa Fujimura ,  Masato Sone ,  Valeri Yu Dolmatov ,  Shigeru Shiozaki

IPC分类号： B24D3/02 ,  C09C1/68 ,  C09K3/14 ,  B01J3/08 ,  C01B31/06

CPC分类号： C25D15/02 ,  Y10S428/935 ,  Y10T428/12493 ,  Y10T428/12625 ,  Y10T428/25

摘要： An aqueous suspension liquid of finely divided diamond particles comprising 0.05 to 160 parts by weight of a finely divided diamond particles in 1000 parts of water, wherein; (i) the finely divided diamond particles have an element composition consisting mainly of 72 to 89.5% by weight of carbon, 0.8 to 1.5% of hydrogen, 1.5 to 2.5% of nitrogen, and 10.5 to 25.0% of oxygen; (ii) and, almost all of said diamond particles are in the range of 2 mu to 50 nm in diameters thereof (80% or more by number average, 70% or more by weight average), (iii) and, said finely divided diamond particles exhibit a strongest peak of the intensity of the Bragg angle at 43.9° (20±20), strong and characteristic peaks at 73.5° (20±20) and 95° (20±2°), a warped halo at 17′ (20±2′), and no peak at 26.5°, by X-ray diffraction (XRD) spectrum analysis using Cu-Ku radiation when dried, (iv) and, specific surface area of said diamond particles when dry state powder is not smaller than 1.50×105 m2/kg, and substantially all the surface carbon atoms of said particles are bonded with hetero atoms, and the total absorption space of said powder is 0.5 m3/kg or more, when dried. The diamond particles are very active and dispersible in aqueous liquid in stable, and have essentially same mechanical properties as that of usual diamonds.

摘要翻译： 一种细碎金刚石颗粒的水性悬浮液，其包含0.05至160重量份在1000份水中的细碎金刚石颗粒，其中： （i）细碎金刚石颗粒具有主要由碳原子数为72〜89.5重量％，氢为0.8〜1.5％，氮为1.5〜2.5％，氧为10.5〜25.0％的元素组成。 （ii），并且几乎所有的所述金刚石颗粒的直径在2至50nm的范围内（数均为80％或更多，平均为70％或更多），（iii），并且所述细分 金刚石颗粒在43.9°（20±20）处呈现出最强的布拉格角强度峰值，73.5°（20±20）°和95°（20±2°）处的强特征峰，17' （20±2'），26.5°没有峰，通过干燥后使用Cu-Ku辐射的X射线衍射（XRD）光谱分析，（iv）当干态粉末不是时，所述金刚石颗粒的比表面积 小于1.50×105m2 / kg，并且所述颗粒的基本上所有的表面碳原子与杂原子键合，并且当干燥时，所述粉末的总吸收空间为0.5m 3 / kg以上。 金刚石颗粒在水性液体中是非常活泼和可分散的，并且具有与通常的钻石基本上相同的机械性能。

公开(公告)号：US07300527B2

公开(公告)日：2007-11-27

申请号：US10297878

申请日：2002-11-06

申请人： Hideo Yoshida ,  Nobuyoshi Sato ,  Takeshi Sako ,  Masato Sone ,  Kentaro Abe ,  Kiyohito Sakon

发明人： Hideo Yoshida ,  Nobuyoshi Sato ,  Takeshi Sako ,  Masato Sone ,  Kentaro Abe ,  Kiyohito Sakon

IPC分类号： B08B3/02

CPC分类号： B08B3/04 ,  B08B3/02 ,  B08B7/02 ,  C25D5/34 ,  Y10S134/902

摘要： A method for activating the surface of a base material and an apparatus thereof, which is suited to be utilized for pretreatment in electrochemical treatment such as, for example, electroplating or the like, in which the surface of a base material such as metal can be subjected to degreasing treatment and oxide film removing treatment simultaneously, efficiently and rationally, in which productivity can be enhanced and the equipment cost can be reduced, and in which a waste solution can be rationalized so that the solution can be reutilized and the environmental pollution can be prevented. A method for activating the surface of a base material in which the surface of a member to be treated is subjected to degreasing treatment or oxide film removing treatment. Pressurized carbon dioxide is dissolved in a predetermined quantity of water, thereby preparing an oxide film removing solution having a predetermined acidic concentration.

摘要翻译： 用于激活基材表面的方法及其装置，其适用于电化学处理例如电镀等中的预处理，其中诸如金属的基材的表面可以是 同时进行脱脂处理和氧化膜除去处理，能够高效合理地提高生产性，并且可以降低设备成本，并且其中废溶液可以合理化以使溶液可再利用并且环境污染可以 被阻止 一种激活基材的表面的方法，其中待处理部件的表面进行脱脂处理或氧化膜去除处理。 将加压的二氧化碳溶解在预定量的水中，从而制备具有预定酸性浓度的氧化膜去除溶液。

公开(公告)号：US07201972B2

公开(公告)日：2007-04-10

申请号：US10460660

申请日：2003-06-13

申请人： Shigeru Shiozaki ,  Masato Sone ,  Hideo Yoshida ,  Kiyohito Sakon ,  Tadamasa Fujimura

发明人： Shigeru Shiozaki ,  Masato Sone ,  Hideo Yoshida ,  Kiyohito Sakon ,  Tadamasa Fujimura

IPC分类号： B32B5/16 ,  B32B5/02 ,  B32B15/00 ,  C25C5/00

CPC分类号： C25D15/02 ,  Y10T428/12486

摘要： There is provided a metal thin film comprising a metal plate and a diamond particle dispersed in the metal plate. According to the present invention, the metal thin film has a film thickness of 5 nm to 35000 nm. The diamond particle is dispersed almost homogeneously over the direction of the film thickness of the metal thin film. The metal thin film has the diamond particle at a concentration of 1 to 12%. According to the present invention, based on conversion into an equivalent circle, the diamond particle has a first particle size distribution with respect to a first particle of a first particle size of 16 nm or less, at a first number average existence rate of 50% or more; the diamond particle has a second particle size distribution with respect to a second particle having a second particle size of 50 nm or more, at a second number average existence rate of substantially 0%; and the diamond particle has a third particle size distribution with respect to a third particle having a third particle size of 2 nm or less, at a third number average existence rate of substantially 0%.

摘要翻译： 提供了金属薄膜，其包括分散在金属板中的金属板和金刚石颗粒。 根据本发明，金属薄膜的膜厚为5nm〜35000nm。 金刚石颗粒在金属薄膜的膜厚方向上几乎均匀地分散。 金属薄膜的浓度为1〜12％的金刚石粒子。 根据本发明，基于转换为等效圆，金刚石颗粒相对于第一粒径为16nm或更小的第一粒子以第一数均分子存在率为50％具有第一粒度分布， 或者更多; 所述金刚石颗粒相对于具有第二粒径为50nm或更大的第二颗粒的​​第二粒度分布，其第二数均分子存在率基本为0％; 并且所述金刚石颗粒相对于第三粒径为2nm以下的第三粒子具有基本上为0％的第三数均分率的第三粒度分布。

公开(公告)号：US20110209642A1

公开(公告)日：2011-09-01

申请号：US13046372

申请日：2011-03-11

申请人： Tadamasa Fujimura ,  Masato Sone ,  Valeri Yu Dolmatov ,  Shigeru Shiozaki

发明人： Tadamasa Fujimura ,  Masato Sone ,  Valeri Yu Dolmatov ,  Shigeru Shiozaki

IPC分类号： C09D1/00 ,  B82Y30/00

CPC分类号： C25D15/02 ,  Y10S428/935 ,  Y10T428/12493 ,  Y10T428/12625 ,  Y10T428/25

摘要： An aqueous suspension liquid of finely divided diamond particles comprising 0.05 to 160 parts by weight of a finely divided diamond particles in 1000 parts of water, wherein; (i) the finely divided diamond particles have an element composition consisting mainly of 72 to 89.5% by weight of carbon, 0.8 to 1.5% of hydrogen, 1.5 to 2.5% of nitrogen, and 10.5 to 25.0% of oxygen; (ii) and, almost all of said diamond particles are in the range of 2 mu to 50 nm in diameters thereof (80% or more by number average, 70% or more by weight average), (iii) and, said finely divided diamond particles exhibit a strongest peak of the intensity of the Bragg angle at 43.9° (20±20), strong and characteristic peaks at 73.5° (20±20) and 95° (20±2°), a warped halo at 17′(20±2′), and no peak at 26.5°, by X-ray diffraction (XRD) spectrum analysis using Cu-Ku radiation when dried, (iv) and, specific surface area of said diamond particles when dry state powder is not smaller than 1.50×105 m2/kg, and substantially all the surface carbon atoms of said particles are bonded with hetero atoms, and the total absorption space of said powder is 0.5 m3/kg or more, when dried. The diamond particles are very active and dispersible in aqueous liquid in stable, and have essentially same mechanical properties as that of usual diamonds.

摘要翻译： 一种细碎金刚石颗粒的水性悬浮液，其包含0.05至160重量份在1000份水中的细碎金刚石颗粒，其中： （i）细碎金刚石颗粒具有主要由碳原子数为72〜89.5重量％，氢为0.8〜1.5％，氮为1.5〜2.5％，氧为10.5〜25.0％的元素组成。 （ii），并且几乎所有的所述金刚石颗粒的直径在2至50nm的范围内（数均为80％或更多，平均为70％或更多），（iii），并且所述细分 金刚石颗粒在43.9°（20±20）处呈现出最强的布拉格角强度峰值，73.5°（20±20）°和95°（20±2°）处的强特征峰，17' （20±2'），26.5°没有峰，通过干燥后使用Cu-Ku辐射的X射线衍射（XRD）光谱分析，（iv）当干态粉末不是时，所述金刚石颗粒的比表面积 小于1.50×105m2 / kg，并且所述颗粒的基本上所有的表面碳原子与杂原子键合，并且当干燥时，所述粉末的总吸收空间为0.5m 3 / kg以上。 金刚石颗粒在水性液体中是非常活泼和可分散的，并且具有与通常的钻石基本上相同的机械性能。