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1. 发明授权

US08187449B2 Cleaning method by electrolytic sulfuric acid and manufacturing method of semiconductor device 有权
标题翻译：电解硫酸的清洗方法及半导体装置的制造方法
公开(公告)号：US08187449B2
公开(公告)日：2012-05-29
申请号：US12459133
申请日：2009-06-26
申请人： Hiroki Domon , Yusuke Ogawa , Masaaki Kato , Takamichi Kishi , Naoya Hayamizu , Makiko Tange , Yoshiaki Kurokawa , Nobuo Kobayashi
发明人： Hiroki Domon , Yusuke Ogawa , Masaaki Kato , Takamichi Kishi , Naoya Hayamizu , Makiko Tange , Yoshiaki Kurokawa , Nobuo Kobayashi
IPC分类号： C25B1/28
CPC分类号： C11D11/007 , C11D7/08 , C11D11/0047 , C25B1/285 , G03F7/423 , H01L21/31133
摘要： The cleaning method by electrolytic sulfuric acid and the manufacturing method of semiconductor device comprising: the process in which the first sulfuric acid solution is supplied from outside to the sulfuric acid electrolytic cell to form the first electrolytic sulfuric acid containing oxidizing agent in the sulfuric acid electrolytic cell; the process in which the second sulfuric acid solution, which is higher in concentration than said the first sulfuric acid solution previously supplied, is supplied from outside to said sulfuric acid electrolytic cell; said the second sulfuric acid solution and the first electrolytic sulfuric acid are mixed in said sulfuric acid electrolytic cell; and electrolysis is performed to form the cleaning solution comprising the second electrolytic sulfuric acid containing sulfuric acid and oxidation agent in said sulfuric acid electrolytic cell and the process in which cleaning treatment is performed for the cleaning object with said cleaning solution.
摘要翻译：电解硫酸的清洗方法以及半导体装置的制造方法，其特征在于，包括：从硫酸电解槽向外部供给第一硫酸溶液，在硫酸电解液中形成含有第一电解硫酸的氧化剂的工序细胞; 其中比所述先前供应的所述第一硫酸溶液浓度高的第二硫酸溶液从外部供应到所述硫酸电解池的过程; 所述第二硫酸溶液和所述第一电解硫酸在所述硫酸电解池中混合; 并且进行电解以在所述硫酸电解池中形成包含含有硫酸和氧化剂的第二电解硫酸的清洗溶液，以及对所述清洁溶液进行清洁对象的清洁处理的处理。

2. 发明申请

US20110073490A1 CLEANING METHOD, CLEANING SYSTEM, AND METHOD FOR MANUFACTURING MICROSTRUCTURE 审中-公开
标题翻译：清洁方法，清洁系统和制造微结构的方法
公开(公告)号：US20110073490A1
公开(公告)日：2011-03-31
申请号：US12880549
申请日：2010-09-13
申请人： Naoya Hayamizu , Makiko Tange , Masaaki Kato , Hiroki Domon , Yusuke Ogawa , Yoshiaki Kurokawa , Nobuo Kobayashi
发明人： Naoya Hayamizu , Makiko Tange , Masaaki Kato , Hiroki Domon , Yusuke Ogawa , Yoshiaki Kurokawa , Nobuo Kobayashi
IPC分类号： C25F1/00 , C25F7/00
CPC分类号： C25B1/28 , G03F7/423
摘要： According to one embodiment, a cleaning method is disclosed. The method can produce an oxidizing solution including an oxidizing substance by electrolyzing a dilute sulfuric acid solution. In addition, the method can supply a highly concentrated inorganic acid solution individually, sequentially, or substantially simultaneously with the oxidizing solution to a surface of an object to be cleaned.
摘要翻译：根据一个实施例，公开了一种清洁方法。该方法可以通过电解稀硫酸溶液来产生包含氧化物质的氧化溶液。此外，该方法可以将高度浓缩的无机酸溶液与氧化溶液单独，依次或基本上同时地供给到待清洁物体的表面。

3. 发明申请

US20090325390A1 Cleaning method by electrolytic sulfuric acid and manufacturing method of semiconductor device 有权
标题翻译：电解硫酸的清洗方法及半导体装置的制造方法
公开(公告)号：US20090325390A1
公开(公告)日：2009-12-31
申请号：US12459133
申请日：2009-06-26
申请人： Hiroki Domon , Yusuke Ogawa , Masaaki Kato , Takamichi Kishi , Naoya Hayamizu , Makiko Tange , Yoshiaki Kurokawa , Nobuo Kobayashi
发明人： Hiroki Domon , Yusuke Ogawa , Masaaki Kato , Takamichi Kishi , Naoya Hayamizu , Makiko Tange , Yoshiaki Kurokawa , Nobuo Kobayashi
IPC分类号： H01L21/20 , C25B1/22 , C11D7/34
CPC分类号： C11D11/007 , C11D7/08 , C11D11/0047 , C25B1/285 , G03F7/423 , H01L21/31133
摘要： The cleaning method by electrolytic sulfuric acid and the manufacturing method of semiconductor device comprising: the process in which the first sulfuric acid solution is supplied from outside to the sulfuric acid electrolytic cell to form the first electrolytic sulfuric acid containing oxidizing agent in the sulfuric acid electrolytic cell; the process in which the second sulfuric acid solution, which is higher in concentration than said the first sulfuric acid solution previously supplied, is supplied from outside to said sulfuric acid electrolytic cell; said the second sulfuric acid solution and the first electrolytic sulfuric acid are mixed in said sulfuric acid electrolytic cell; and electrolysis is performed to form the cleaning solution comprising the second electrolytic sulfuric acid containing sulfuric acid and oxidation agent in said sulfuric acid electrolytic cell and the process in which cleaning treatment is performed for the cleaning object with said cleaning solution.
摘要翻译：电解硫酸的清洗方法以及半导体装置的制造方法，其特征在于，包括：从硫酸电解槽向外部供给第一硫酸溶液，在硫酸电解液中形成含有第一电解硫酸的氧化剂的工序细胞; 其中比所述先前供应的所述第一硫酸溶液浓度高的第二硫酸溶液从外部供应到所述硫酸电解池的过程; 所述第二硫酸溶液和所述第一电解硫酸在所述硫酸电解池中混合; 并且进行电解以在所述硫酸电解池中形成包含含有硫酸和氧化剂的第二电解硫酸的清洗溶液，以及对所述清洁溶液进行清洁对象的清洁处理的处理。

4. 发明申请

US20110073489A1 CLEANING LIQUID, CLEANING METHOD, CLEANING SYSTEM, AND METHOD FOR MANUFACTURING MICROSTRUCTURE 审中-公开
标题翻译：清洁液，清洁方法，清洁系统和制造微结构的方法
公开(公告)号：US20110073489A1
公开(公告)日：2011-03-31
申请号：US12880450
申请日：2010-09-13
申请人： Naoya Hayamizu , Makiko Tange , Yoshiaki Kurokawa , Nobuo Kobayashi , Masaaki Kato , Yusuke Ogawa , Hiroki Domon
发明人： Naoya Hayamizu , Makiko Tange , Yoshiaki Kurokawa , Nobuo Kobayashi , Masaaki Kato , Yusuke Ogawa , Hiroki Domon
IPC分类号： C25F1/00 , C25F7/00
CPC分类号： H01L21/31133 , G03F7/423 , H01L21/67051
摘要： According to embodiments, a cleaning liquid includes an oxidizing substance and hydrofluoric acid and exhibiting acidity. A cleaning method is disclosed. The method includes producing an oxidizing solution including an oxidizing substance by one selected from electrolyzing a sulfuric acid solution, electrolyzing hydrofluoric acid added to a sulfuric acid solution, and mixing a sulfuric acid solution with aqueous hydrogen peroxide. The method includes supplying the oxidizing solution and hydrofluoric acid to a surface of an object to be cleaned.
摘要翻译：根据实施方案，清洗液体包含氧化物质和氢氟酸并具有酸性。公开了一种清洁方法。该方法包括：通过选择电解硫酸溶液，电解加入到硫酸溶液中的氢氟酸，并将硫酸溶液与过氧化氢水溶液混合，制备包含氧化物质的氧化溶液。该方法包括将氧化溶液和氢氟酸供给到待清洁物体的表面。

5. 发明申请

US20090321272A1 Sulfuric acid electrolysis process 有权
标题翻译：硫酸电解过程
公开(公告)号：US20090321272A1
公开(公告)日：2009-12-31
申请号：US12459161
申请日：2009-06-26
申请人： Masaaki Kato , Yusuke Ogawa , Hiroki Domon , Naoya Hayamizu , Makiko Tange , Yoshiaki Kurokawa , Nobuo Kobayashi
发明人： Masaaki Kato , Yusuke Ogawa , Hiroki Domon , Naoya Hayamizu , Makiko Tange , Yoshiaki Kurokawa , Nobuo Kobayashi
IPC分类号： C25B15/00
CPC分类号： C25B1/285
摘要： Sulfuric acid electrolysis process wherein; a temperature of electrolyte containing sulfuric acid to be supplied to an anode compartment and a cathode compartment is controlled to 30 degree Celsius or more; a flow rate F1 (L/min.) of the electrolyte containing sulfuric acid to be supplied to said anode compartment is controlled to 1.5 times or more (F1/Fa≧1.5) a flow rate Fa (L/min.) of gas formed on an anode side as calculated from Equation (1) shown below and a flow rate F2(L/min.) of said electrolyte containing sulfuric acid to be supplied to said cathode compartment is controlled to 1.5 times or more (F2/Fc≧1.5) a flow rate Fe (L/min.) of gas formed on a cathode side as calculated from Equation (2) shown below. Fa=(I×S×R×T)/(4×Faraday constant) Equation (I) Fe=(I×S×R×T)/(2×Faraday constant) Equation (2) I: Electrolytic current (A)S: Time: 60 second (Fixed)R: Gas constant (0.082 1·atm/K/mol)K: Absolute temperature (273.15 degree Celsius+T degree Celsius)T: Electrolysis temperature (degree Celsius)Faraday constant: (C/mol)
摘要翻译：硫酸电解法其中; 供给阳极室和阴极室的含有硫酸的电解质的温度控制在30摄氏度以上; 将供给到阳极室的含有硫酸的电解质的流量F1（L / min）控制为气体的流量Fa（L / min）的1.5倍以上（F1 / Fa> 1.5）形成在阳极侧，由下述式（1）算出，将含有供给阴极室的硫酸的电解质的流量F2（L / min）控制在1.5倍以上（F2 / Fc> = 1.5）由下面所示的等式（2）计算的在阴极侧形成的气体的流速Fe（L / min）。 Fa =（IxSxRxT）/（4xFaraday常数）等式（I）Fe =（IxSxRxT）/（2xFaraday常数）等式（2）I：电解电流（A）S：时间：60秒（固定）R：气体常数（0.082 1.atm / K / mol）K：绝对温度（273.15摄氏度+ T摄氏度）T：电解温度（摄氏度）法拉第常数：（C / mol）

6. 发明授权

US08211287B2 Sulfuric acid electrolysis process 有权
标题翻译：硫酸电解过程
公开(公告)号：US08211287B2
公开(公告)日：2012-07-03
申请号：US12459161
申请日：2009-06-26
申请人： Masaaki Kato , Yusuke Ogawa , Hiroki Domon , Naoya Hayamizu , Makiko Tange , Yoshiaki Kurokawa , Nobuo Kobayashi
发明人： Masaaki Kato , Yusuke Ogawa , Hiroki Domon , Naoya Hayamizu , Makiko Tange , Yoshiaki Kurokawa , Nobuo Kobayashi
IPC分类号： C25B1/28
CPC分类号： C25B1/285
摘要： Sulfuric acid electrolysis process wherein; a temperature of electrolyte containing sulfuric acid to be supplied to an anode compartment and a cathode compartment is controlled to 30 degree Celsius or more; a flow rate F1 (L/min.) of the electrolyte containing sulfuric acid to be supplied to said anode compartment is controlled to 1.5 times or more (F1/Fa≧1.5) a flow rate Fa (L/min.) of gas formed on an anode side as calculated from Equation (1) shown below and a flow rate F2(L/min.) of said electrolyte containing sulfuric acid to be supplied to said cathode compartment is controlled to 1.5 times or more (F2/Fc≧1.5) a flow rate Fe (L/min.) of gas formed on a cathode side as calculated from Equation (2) shown below. Fa=(I×S×R×T)/(4×Faraday constant) Equation (1) Fe=(I×S×R×T)/(2×Faraday constant) Equation (2) I: Electrolytic current (A) S: Time: 60 second (Fixed) R: Gas constant (0.082 1·atm/K/mol) K: Absolute temperature (273.15 degree Celsius+T degree Celsius) T: Electrolysis temperature (degree Celsius) Faraday constant: (C/mol)
摘要翻译：硫酸电解法其中; 供给阳极室和阴极室的含有硫酸的电解质的温度控制在30摄氏度以上; 供给所述阳极室的含有硫酸的电解质的流量F1（L / min）被控制为形成的气体的流量Fa（L / min）的1.5倍以上（F1 /Fa≥1.5）在阳极侧，由下述式（1）计算，含有供给阴极室的硫酸的电解质的流量F2（L / min）被控制为1.5倍以上（F2 /Fc≥1.5 ）由如下所示的等式（2）计算的在阴极侧形成的气体的流速Fe（L / min）。 Fa =（I×S×R×T）/（4×法拉第常数）等式（1）Fe =（I×S×R×T）/（2×法拉第常数）等式（2）I：电解电流）S：时间：60秒（固定）R：气体常数（0.082 1·atm / K / mol）K：绝对温度（273.15摄氏度+ T摄氏度）T：电解温度（摄氏度）法拉第常数 / mol）

7. 发明申请

US20110143549A1 ETCHING METHOD, METHOD FOR MANUFACTURING MICROSTRUCTURE, AND ETCHING APPARATUS 审中-公开
标题翻译：蚀刻方法，制造微结构的方法和蚀刻装置
公开(公告)号：US20110143549A1
公开(公告)日：2011-06-16
申请号：US12963187
申请日：2010-12-08
申请人： Makiko TANGE , Naoya Hayamizu , Nobuyoshi Sato , Yuri Yonekura , Hideaki Hirabayashi , Yoshiaki Kurokawa , Nobuo Kobayashi , Masaaki Kato , Hiroki Domon
发明人： Makiko TANGE , Naoya Hayamizu , Nobuyoshi Sato , Yuri Yonekura , Hideaki Hirabayashi , Yoshiaki Kurokawa , Nobuo Kobayashi , Masaaki Kato , Hiroki Domon
IPC分类号： H01L21/302 , B44C1/22 , C23F1/00 , H01L21/02
CPC分类号： C25B1/22 , C25B9/08 , G03F1/80 , G03F7/423 , H01L21/02057 , H01L21/31133 , H01L21/6708
摘要： In one embodiment, an etching method is disclosed. The method can include producing an oxidizing substance by electrolyzing a sulfuric acid solution, and producing an etching solution having a prescribed oxidizing species concentration by controlling a produced amount of the produced oxidizing substance. The method can include supplying the produced etching solution to a surface of a workpiece.
摘要翻译：在一个实施例中，公开了蚀刻方法。该方法可以包括通过电解硫酸溶液来生产氧化物质，并通过控制生成的氧化物质的产生量来制备具有规定的氧化物质浓度的蚀刻溶液。该方法可以包括将所产生的蚀刻溶液供应到工件的表面。

8. 发明申请

US20130256150A1 ELECTRICALLY CONDUCTIVE DIAMOND ELECTRODE, AND SULFURIC ACID ELECTROLYSIS METHOD AND SULFURIC ACID ELECTROLYSIS APPARATUS EACH UTILIZING SAME 审中-公开
标题翻译：电导电钻石电极和硫酸电解法和硫酸电解设备每个使用一次
公开(公告)号：US20130256150A1
公开(公告)日：2013-10-03
申请号：US13993205
申请日：2011-11-21
申请人： Masaaki Kato , Hiroki Domon , Junko Kosaka
发明人： Masaaki Kato , Hiroki Domon , Junko Kosaka
IPC分类号： C25B11/04 , C25B1/28
CPC分类号： C25B11/0447 , C25B1/285 , C25B1/30
摘要： The present invention provides an electrically conductive diamond electrode comprising an electrically conductive substrate and an electrically conductive diamond layer coated on the surface of the electrically conductive substrate, featuring that: 1) the thickness of the electrically conductive diamond layer is 1˜25 μm, 2) the potential window fulfills Equation (1) and 3) the ratio (A/B) of the diamond component A and the non-diamond component B by the Raman spectroscopic analysis fulfills Equation (2). 2.1V≦potential window≦3.5V (1) 1.5
摘要翻译：本发明提供一种导电金刚石电极，其包括导电基底和涂覆在导电基底表面上的导电金刚石层，其特征在于：1）导电金刚石层的厚度为1〜25μm，2 ）潜在的窗口满足式（1）和3）通过拉曼光谱分析得到的金刚石成分A和非金刚石成分B的比（A / B）满足式（2）。 2.1V@potential window@3.5V（1）1.5

9. 发明申请

US20130334059A1 APPARATUS FOR ELECTROLYZING SULFURIC ACID AND METHOD FOR ELECTROLYZING SULFURIC ACID 审中-公开
标题翻译：用于电解硫酸的装置和用于电解硫酸的方法
公开(公告)号：US20130334059A1
公开(公告)日：2013-12-19
申请号：US14001636
申请日：2012-03-07
申请人： Hiroki Domon , Kouji Fujii , Junko Kosaka , Masaaki Kato
发明人： Hiroki Domon , Kouji Fujii , Junko Kosaka , Masaaki Kato
IPC分类号： C25B1/22 , C25B15/02
CPC分类号： C25B1/22 , C25B11/12 , C25B15/02 , C25B15/08
摘要： The present invention relates to an apparatus to produce oxidizing agent-rich sulfuric acid by electrolysis of sulfuric acid. More specifically, it relates to the apparatus by which dilute sulfuric acid of the specified temperature and concentration is formed within the electrolysis system and then, by electrolysis of the formed dilute sulfuric acid, electrolytic sulfuric acid containing richly oxidizing agent is formed at a high efficiency and safely under the temperature control.The apparatus for electrolyzing sulfuric acid and the method for electrolyzing sulfuric acid by the present invention comprise the anode side dilute sulfuric acid generation loop A in which concentrated sulfuric acid, as feed material, is diluted and controlled to the specified temperature and concentration, and the anode side electrolytic sulfuric acid generation loop B in which electrolytic sulfuric acid is formed by electrolysis of dilute sulfuric acid with the temperature and concentration controlled to the specified range in the anode side dilute sulfuric acid generation loop A, in, at least, the anode side electrolysis part of the apparatus for electrolyzing sulfuric acid having the anode side electrolysis part and the cathode side electrolysis part.
摘要翻译：本发明涉及通过电解硫酸生产富氧化剂硫酸的装置。更具体地说，涉及在电解系统内形成规定温度和浓度的稀硫酸的装置，然后通过电解形成的稀硫酸，以高效率形成含有浓氧化剂的电解硫酸并在温度控制下安全。本发明的硫酸电解装置及硫酸电解方法包括将作为原料的浓硫酸稀释至规定温度和浓度的阳极侧稀硫酸生成环A，阳极侧电解硫酸生成回路B，其中通过在阳极侧稀硫酸生成回路A中将温度和浓度控制在规定范围内的稀硫酸电解形成电解硫酸，至少在阳极侧用于电解具有阳极侧电解部分和阴极侧电解部分的硫酸的装置的电解部分。

10. 发明申请

US20130313129A1 METHOD FOR MEASURING TOTAL CONCENTRATION OF OXIDIZING AGENTS, CONCENTRATION METER FOR MEASURING TOTAL CONCENTRATION OF OXIDIZING AGENTS, AND SULFURIC ACID ELECTROLYSIS DEVICE EQUIPPED WITH SAME 审中-公开
标题翻译：用于测量氧化剂总浓度的方法，用于测量氧化剂总浓度的浓度计和装备有氧化剂的硫酸电解装置
公开(公告)号：US20130313129A1
公开(公告)日：2013-11-28
申请号：US13984451
申请日：2012-02-27
申请人： Junko Kosaka , Masaaki Kato , Hiroki Domon
发明人： Junko Kosaka , Masaaki Kato , Hiroki Domon
IPC分类号： G01N27/26 , G01N21/17 , G01N9/36 , G01N29/02
CPC分类号： G01N27/26 , G01N9/36 , G01N21/17 , G01N21/33 , G01N21/65 , G01N27/3277 , G01N29/02 , G01N31/228
摘要： Provided are: a method of measuring the total concentration of oxidizing agents, by which the total concentration can be determined in a single measurement with simple operations even in an evaluation solution containing multiple components such as persulfuric acid, perosulfate and hydrogen peroxide; a simple and inexpensive concentration meter for measuring the total concentration of oxidizing agents; and a sulfuric acid electrolysis device comprising the concentration meter.The method according to the present invention is a method of measuring the total concentration of oxidizing agent(s) in an evaluation solution containing at least one oxidizing agent. The method comprises at least the steps of: heat-treating the evaluation solution at 50 to 135° C.; and detecting hydrogen peroxide in the thus heat-treated evaluation solution.
摘要翻译：提供：测量氧化剂的总浓度的方法，即使在含有多种成分如过硫酸，过硫酸盐和过氧化氢的评价溶液中，也可以通过简单的操作在一次测量中确定总浓度; 用于测量氧化剂总浓度的简单廉价的浓度计; 和含有浓度计的硫酸电解装置。根据本发明的方法是测量含有至少一种氧化剂的评价溶液中的氧化剂的总浓度的方法。该方法至少包括以下步骤：在50至135℃下对评估溶液进行热处理; 并检测由此热处理的评估溶液中的过氧化氢。

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