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1. 发明授权

US10400147B2 Method for producing purified active silicic acid solution and silica sol 有权
公开(公告)号：US10400147B2
公开(公告)日：2019-09-03
申请号：US13617453
申请日：2012-09-14
申请人： Kiyomi Ema , Noriyuki Takakuma , Tohru Nishimura , Naoki Kawashita , Kouji Yamaguchi
发明人： Kiyomi Ema , Noriyuki Takakuma , Tohru Nishimura , Naoki Kawashita , Kouji Yamaguchi
IPC分类号： C09K3/14 , C09K13/04 , C01B33/143 , C01B33/148 , C01B33/141
摘要： A method for producing an active silicic acid solution in which the existing amount of foreign matters as plate-like fine particles is reduced and a method for producing a silica sol in which such foreign matters are reduced. The method fulfills the following condition: the existing amount of plate-like fine particles having a length of one side of 0.2 to 4.0 μm and a thickness of 1 to 100 nm is measured to be 0% to 30% in accordance with measuring method A, the method including the steps of: preparing an active silicic acid solution by subjecting an alkali silicate aqueous solution having a silica concentration of 0.5% by mass to 10.0% by mass to cation-exchange to remove alkaline components; and filtering the active silicic acid solution through a filter whose removal rate of particles having a primary particle size of 1.0 μm is 50% or more.

2. 发明授权

US09108855B2 Method for producing purified alkali silicate aqueous solution and silica sol 有权
标题翻译：纯碱性硅酸盐水溶液和硅溶胶的制备方法
公开(公告)号：US09108855B2
公开(公告)日：2015-08-18
申请号：US13603715
申请日：2012-09-05
申请人： Kiyomi Ema , Noriyuki Takakuma , Tohru Nishimura , Naoki Kawashita , Kouji Yamaguchi
发明人： Kiyomi Ema , Noriyuki Takakuma , Tohru Nishimura , Naoki Kawashita , Kouji Yamaguchi
IPC分类号： B24D3/00 , B24D3/02 , B24D11/00 , B24D18/00 , C09K3/14 , C09C1/68 , C01B33/148 , C01B33/143 , B82Y30/00
CPC分类号： C01B33/1485 , B82Y30/00 , C01B33/1435 , C01P2004/64 , C09K3/1463
摘要： To provide a method for producing an alkali silicate aqueous solution containing a reduced amount of foreign substance of plate-like fine particles and a method for producing a silica sol containing a reduced amount of foreign substance of plate-like fine particles. A method for producing an alkali silicate aqueous solution fulfilling the following condition: the existing amount of plate-like fine particles having a length of one side of 0.2 to 4.0 μm and a thickness of 1 to 100 nm is determined to be 0 to 30%. The method for producing an alkali silicate aqueous solution includes the steps of adjusting a silica concentration of an alkali silicate aqueous solution to 0.5 to 10.0% by mass and filtering the alkali silicate aqueous solution through a filter having a removal rate of particles with a primary particle size of 1.0 μm of 50% or more.
摘要翻译：提供一种含有少量板状微粒的异物的碱金属硅酸盐水溶液的制造方法以及含有少量的板状微粒的异物的二氧化硅溶胶的制造方法。一种满足以下条件的碱金属硅酸盐水溶液的制造方法：将一边长度为0.2〜4.0μm，厚度为1〜100nm的板状微粒的存在量确定为0〜30％。碱土金属硅酸盐水溶液的制造方法包括将碱土金属硅酸盐水溶液的二氧化硅浓度调整为0.5〜10.0质量％的步骤，通过具有一次粒子的粒子去除率的过滤器过滤碱金属硅酸盐水溶液 1.0μm的尺寸为50％以上。

3. 发明申请

US20080156908A1 Method of milling cerium compound by means of ball mill 审中-公开
标题翻译：通过球磨机研磨铈化合物的方法
公开(公告)号：US20080156908A1
公开(公告)日：2008-07-03
申请号：US12071785
申请日：2008-02-26
申请人： Isao Ota , Kenji Tanimoto , Gen Yamada , Noriyuki Takakuma
发明人： Isao Ota , Kenji Tanimoto , Gen Yamada , Noriyuki Takakuma
IPC分类号： B02C17/20
CPC分类号： B02C17/00 , B02C17/20 , C09K3/1409
摘要： A method of milling cerium compound by means of a ball mill using a milling medium, characterized in that ratio Hb/r of radius r of a cylindrical ball mill container and depth Hb of the milling medium in the ball mill container disposed horizontally ranges from 1.2 to 1.9, and the ball mill container is rotated at a rotational speed which is 50% or less of critical rotational speed Nc=299/r1/2 of the ball mill container converted from the radius r expressed in centimeter. The milling method can be carried out in a wet or dry process, and the cerium compound is preferably cerium oxide. The method can be also applied for producing a cerium compound slurry.
摘要翻译：一种通过使用研磨介质的球磨机研磨铈化合物的方法，其特征在于，圆柱形球磨机容器的半径r与深度H b b的比值H b / 水平设置的球磨机容器中的研磨介质的SUB> 1.2〜1.9，球磨容器以临界旋转速度N C = 50％以下的转速旋转，从以半径r表示的半径r转换的球磨机容器的299 / r 1/2倍。研磨方法可以在湿法或干法中进行，铈化合物优选为氧化铈。该方法也可用于制备铈化合物浆料。

4. 发明申请

US20090042393A1 Production method of polishing composition 失效
标题翻译：抛光组合物的生产方法
公开(公告)号：US20090042393A1
公开(公告)日：2009-02-12
申请号：US12285498
申请日：2008-10-07
申请人： Noriyuki Takakuma , Isao Ota , Kenji Tanimoto
发明人： Noriyuki Takakuma , Isao Ota , Kenji Tanimoto
IPC分类号： H01L21/306
CPC分类号： C01G25/02 , B82Y30/00 , C01P2004/64 , C09K3/1409 , C09K3/1463
摘要： A production method of a semiconductor device including: producing a polishing composition containing zirconium oxide sol; and planarizing a substrate having an uneven surface with said polishing composition, wherein the polishing composition containing zirconium oxide is produced by the steps comprising: baking at a temperature ranging from 400 to 1000° C., a zirconium compound having d50 (where d50 represents a particle diameter meaning that the number of particles having this particle diameter or less is 50% of the total number of particles) of zirconium compound particles of 5 to 25 μm and d99 (where d99 represents a particle diameter meaning that the number of particles having this particle diameter or less is 99% of the total number of particles) of zirconium compound particles of 60 μm or less, wherein d50 and d99 are measured by measuring a slurry of the zirconium compound by a laser diffractometry; and wet-grinding a powder of zirconium oxide obtained in the above baking in an aqueous medium until d50 of zirconium oxide particles becomes 80 to 150 nm and d99 of zirconium oxide particles becomes 150 to 500 nm, wherein d50 and d99 are measured by measuring a slurry of the zirconium compound by a laser diffractometry.
摘要翻译：一种半导体器件的制造方法，包括：制造含有氧化锆溶胶的研磨用组合物; 并且用所述抛光组合物平坦化具有不平坦表面的衬底，其中所述包含氧化锆的抛光组合物通过以下步骤制备，所述步骤包括：在400至1000℃的温度下焙烧具有d50的锆化合物（其中d50表示粒径为5〜25μm的锆化合物粒子和d99（d99表示具有该粒子的粒子的粒子数）的粒子总数的50％）粒径为99％以下的锆化合物粒子为60μm以下，其中d50和d99通过激光衍射法测定锆化合物的浆料来测量; 在水性介质中湿式研磨上述焙烧得到的氧化锆粉末，直到氧化锆粒子的d50为80〜150nm，氧化锆粒子的d99为150〜500nm，其中d50和d99为锆化合物的浆料通过激光衍射法。

5. 发明授权

US07484679B2 Method of milling cerium compound by means of ball mill 失效
标题翻译：通过球磨机研磨铈化合物的方法
公开(公告)号：US07484679B2
公开(公告)日：2009-02-03
申请号：US10518769
申请日：2003-07-03
申请人： Isao Ota , Kenji Tanimoto , Gen Yamada , Noriyuki Takakuma
发明人： Isao Ota , Kenji Tanimoto , Gen Yamada , Noriyuki Takakuma
IPC分类号： B02C1/00 , B02C11/08 , B02C21/00 , B02C23/00
CPC分类号： B02C17/00 , B02C17/20 , C09K3/1409
摘要： A method of milling cerium compound by means of a ball mill using a milling medium, characterized in that ratio Hb/r of radius r of a cylindrical ball mill container and depth Hb of the milling medium in the ball mill container disposed horizontally ranges from 1.2 to 1.9, and the ball mill container is rotated at a rotational speed which is 50% or less of critical rotational speed Nc=299/r1/2 of the ball mill container converted from the radius r expressed in centimeter. The milling method can be carried out in a wet or dry process, and the cerium compound is preferably cerium oxide. The method can be also applied for producing a cerium compound slurry.
摘要翻译：一种通过使用研磨介质的球磨机研磨铈化合物的方法，其特征在于，圆柱形球磨机容器的半径r的比率Hb / r和水平设置的球磨机容器中的研磨介质的深度Hb范围为1.2 到1.9，球磨容器以从以半径r表示的半径r转换的球磨机容器的临界转速Nc = 299 / r1 / 2的50％以下的转速旋转。研磨方法可以在湿法或干法中进行，铈化合物优选为氧化铈。该方法也可用于制备铈化合物浆料。

6. 发明申请

US20080254718A1 Production Method of Polishing Composition 失效
标题翻译：抛光组合物的生产方法
公开(公告)号：US20080254718A1
公开(公告)日：2008-10-16
申请号：US11920532
申请日：2006-05-10
申请人： Noriyuki Takakuma , Isao Ota , Kenji Tanimoto
发明人： Noriyuki Takakuma , Isao Ota , Kenji Tanimoto
IPC分类号： C09K3/14 , C01G25/02 , B24B29/00 , B02C23/18 , H01L21/304
CPC分类号： C01G25/02 , B82Y30/00 , C01P2004/64 , C09K3/1409 , C09K3/1463
摘要： [Problems to Be Solved] To provide a method for obtaining a polishing composition by which a polishing speed is high and the polished surface has little surface failure.[Means to Solve the Problems] The present invention relates to a production method of a polishing composition containing zirconia oxide sol including: baking at a temperature ranging from 400 to 1000° C., a zirconium compound having d50 (where d50 represents a particle diameter meaning that the number of particles having this particle diameter or less is 50% of the total number of particles) of zirconium compound particles of 5 to 25 μm and d99 (where d99 represents a particle diameter meaning that the number of particles having this particle diameter or less is 99% of the total number of particles) of zirconium compound particles of 60 μm or less, wherein d50 and d99 are measured by measuring a slurry of the zirconium compound by a laser diffractometry; and wet-grinding a powder of zirconium oxide obtained in the above baking in an aqueous medium until d50 of zirconium oxide particles becomes 80 to 150 nm and d99 of zirconium oxide particles becomes 150 to 500 nm, wherein d50 and d99 are measured by measuring the slurry of the zirconium compound by a laser diffractometry.
摘要翻译： [待解决的问题]提供一种获得抛光速度高的抛光组合物和抛光表面几乎没有表面破坏的方法。解决问题的方法本发明涉及包含氧化锆氧化物溶胶的抛光组合物的制造方法，其包括：在400〜1000℃的温度下焙烧具有d50的锆化合物（d50表示粒径意味着具有5〜25μm的锆化合物粒子和d99的d99（其中d99表示具有该粒径的粒子的数量的粒径的粒子的总数的50％）或更少为总数的99％）的锆化合物颗粒，其中d50和d99通过激光衍射测量锆化合物的浆料来测量; 在水性介质中湿式研磨上述焙烧得到的氧化锆粉末，直到氧化锆粒子的d50为80〜150nm，氧化锆粒子的d99为150〜500nm，通过测定d50和d99 锆化合物的浆料通过激光衍射法。

7. 发明授权

US07431758B2 Cerium oxide particles and production method therefor 失效
标题翻译：氧化铈颗粒及其制备方法
公开(公告)号：US07431758B2
公开(公告)日：2008-10-07
申请号：US10532316
申请日：2003-10-28
申请人： Isao Ota , Kenji Tanimoto , Noriyuki Takakuma
发明人： Isao Ota , Kenji Tanimoto , Noriyuki Takakuma
IPC分类号： C09G1/02 , B01J23/00 , C01F17/00 , B24D3/02
CPC分类号： C01F17/0043 , C01P2004/52 , C09K3/1409 , C09K3/1463
摘要： The production method for cerium oxide particles of the present invention is a method of producing a cerium oxide particle by heating a cerium compound from a normal temperature to a temperature range of 400° C. to 1200° C., and comprises at least a temperature raising stage of a temperature rise speed of 2° C./hour to 60° C./hour, or proceeds via a stage of heating while supplying a humidified gas in a temperature raising process. By the method of the present invention, a cerium oxide powder whose particle diameter distribution of primary particles is narrow can be obtained. An aqueous cerium oxide slurry produced from the powder enables an improvement in the productivity and a reduction in the cost of a polishing step, because if it is used as an abrasive a high-quality polished face is obtained without deteriorating the polishing speed. The aqueous cerium oxide slurry of the present invention is particularly useful as an abrasive for final finish of a substrate whose main component is silica.
摘要翻译：本发明的氧化铈粒子的制造方法是通过将铈化合物从常温加热至400〜1200℃的温度范围来制造氧化铈粒子的方法，至少包含温度升温速度为2℃/小时至60℃/小时，或者在升温过程中供给加湿气体的同时进行加热阶段。通过本发明的方法，可以获得一次颗粒的粒径分布窄的氧化铈粉末。由粉末制造的二氧化铈水泥浆能够提高生产率和降低抛光步骤的成本，因为如果将其用作磨料，则不会降低抛光速度而获得高质量的抛光面。本发明的水氧化铈浆料特别可用作主要成分为二氧化硅的基材的最终光洁度的研磨剂。

8. 发明授权

US08323368B2 Production method of polishing composition 失效
标题翻译：抛光组合物的生产方法
公开(公告)号：US08323368B2
公开(公告)日：2012-12-04
申请号：US11920532
申请日：2006-05-10
申请人： Noriyuki Takakuma , Isao Ota , Kenji Tanimoto
发明人： Noriyuki Takakuma , Isao Ota , Kenji Tanimoto
IPC分类号： B24D3/02 , C09C1/68 , C09K3/14
CPC分类号： C01G25/02 , B82Y30/00 , C01P2004/64 , C09K3/1409 , C09K3/1463
摘要： [Problems to Be Solved]To provide a method for obtaining a polishing composition by which a polishing speed is high and the polished surface has little surface failure.[Means to Solve the Problems]The present invention relates to a production method of a polishing composition containing zirconia oxide sol including: baking at a temperature ranging from 400 to 1000° C., a zirconium compound having d50 (where d50 represents a particle diameter meaning that the number of particles having this particle diameter or less is 50% of the total number of particles) of zirconium compound particles of 5 to 25 μm and d99 (where d99 represents a particle diameter meaning that the number of particles having this particle diameter or less is 99% of the total number of particles) of zirconium compound particles of 60 μm or less, wherein d50 and d99 are measured by measuring a slurry of the zirconium compound by a laser diffractometry; and wet-grinding a powder of zirconium oxide obtained in the above baking in an aqueous medium until d50 of zirconium oxide particles becomes 80 to 150 nm and d99 of zirconium oxide particles becomes 150 to 500 nm, wherein d50 and d99 are measured by measuring the slurry of the zirconium compound by a laser diffractometry.[Selected Drawings]None.
摘要翻译： [待解决的问题]提供一种获得抛光速度高的抛光组合物和抛光表面几乎没有表面破坏的方法。解决问题的方法本发明涉及包含氧化锆氧化物溶胶的抛光组合物的制造方法，其包括：在400〜1000℃的温度下焙烧具有d50的锆化合物（d50表示粒径意味着具有5〜25μm的锆化合物粒子的粒径的总数的50％），d99（其中d99表示具有该粒径的粒子的数量的粒径）或更少为总数为99％的锆化合物颗粒），其中d50和d99通过激光衍射测量锆化合物的浆料来测量; 在水性介质中湿式研磨上述焙烧得到的氧化锆粉末，直到氧化锆粒子的d50为80〜150nm，氧化锆粒子的d99为150〜500nm，通过测定d50和d99 锆化合物的浆料通过激光衍射法。 [所选图纸]无。

9. 发明申请

US20070240366A1 Composition for Polishing 审中-公开
标题翻译：抛光组合
公开(公告)号：US20070240366A1
公开(公告)日：2007-10-18
申请号：US11596389
申请日：2005-05-16
申请人： Isao Ota , Kenji Tanimoto , Noriyuki Takakuma
发明人： Isao Ota , Kenji Tanimoto , Noriyuki Takakuma
IPC分类号： C09G1/02 , C09K3/14
CPC分类号： C09K3/1463 , C09G1/02 , C09K3/1409
摘要： [Problems] To provide a polishing agent for use in polishing for planarization in semiconductor device production steps and for use in a semiconductor device isolation process. [Means for Solving Problems]The composition for polishing comprises a component (A), which is a water-soluble organic compound containing a carboxyl group or a salt thereof; and a component (B), which is an aqueous sol of cerium oxide particles obtained by calcining a cerium compound by holding it in at least two different calcining temperature ranges and wet-milling the resultant cerium oxide powder until the ratio of the mean particle size (b1) measured in the aqueous sol by the laser diffraction method to the particle size (b2) as determined from the specific surface area measured by the gas adsorption method is in the range of either 1 to 4 or 15 to 40. The component (A) is ammonium acrylate, ammonium methacrylate, an amino acid or a derivative thereof. The component (B) is obtained by a process in which the cerium compound is calcined by holding it in two calcining temperature ranges, that is, a range of 200 to 350° C. and a range of 400 to 550° C. or 700 to 850° C., and the resultant cerium oxide powder is wet-milled.
摘要翻译： [问题]提供一种用于半导体器件制造步骤中用于平面化的抛光的抛光剂并用于半导体器件隔离工艺中。 [解决问题的方法]抛光用组合物是含有羧基的水溶性有机化合物或其盐的成分（A）和组分（B），其是通过将铈化合物保持在至少两个不同的煅烧温度范围内并将所得的氧化铈粉末进行湿磨以获得的氧化铈颗粒的水性溶胶，直到平均粒径通过激光衍射法在水性溶胶中测定的（b 1）与通过气体吸附法测定的比表面积确定的粒径（b 2）在1〜4或15〜40的范围内。组分（A）是丙烯酸铵，甲基丙烯酸铵，氨基酸或其衍生物。组分（B）通过将铈化合物保持在两个煅烧温度范围，即200-350℃，400-550℃或700℃范围内煅烧的方法获得至850℃，并将所得的氧化铈粉末湿磨。

10. 发明申请

US20060150526A1 Cerium oxide particles and process for the production therefor 失效
标题翻译：氧化铈颗粒及其生产方法
公开(公告)号：US20060150526A1
公开(公告)日：2006-07-13
申请号：US10532316
申请日：2003-10-28
申请人： Isao Ota , Kenji Tanimoto , Noriyuki Takakuma
发明人： Isao Ota , Kenji Tanimoto , Noriyuki Takakuma
IPC分类号： C09G1/02 , C01F17/00 , C09K3/14
CPC分类号： C01F17/0043 , C01P2004/52 , C09K3/1409 , C09K3/1463
摘要： The production method for cerium oxide particles of the present invention is a method of producing a cerium oxide particle by heating a cerium compound from a normal temperature to a temperature range of 400° C. to 1200° C., and comprises at least a temperature raising stage of a temperature rise speed of 2° C./hour to 60° C./hour, or proceeds via a stage of heating while supplying a humidified gas in a temperature raising process. By the method of the present invention, a cerium oxide powder whose particle diameter distribution of primary particles is narrow can be obtained. An aqueous cerium oxide slurry produced from the powder enables an improvement in the productivity and a reduction in the cost of a polishing step, because if it is used as an abrasive a high-quality polished face is obtained without deteriorating the polishing speed. The aqueous cerium oxide slurry of the present invention is particularly useful as an abrasive for final finish of a substrate whose main component is silica.
摘要翻译：本发明的氧化铈粒子的制造方法是通过将铈化合物从常温加热至400〜1200℃的温度范围来制造氧化铈粒子的方法，至少包含温度升温速度为2℃/小时至60℃/小时，或者在升温过程中供给加湿气体的同时进行加热阶段。通过本发明的方法，可以获得一次颗粒的粒径分布窄的氧化铈粉末。由粉末制造的二氧化铈水泥浆能够提高生产率和降低抛光步骤的成本，因为如果将其用作磨料，则不会降低抛光速度而获得高质量的抛光面。本发明的水氧化铈浆料特别可用作主要成分为二氧化硅的基材的最终光洁度的研磨剂。

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