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1. 发明授权

US09783911B2 Apparatus for producing SiC single crystal by solution growth method, and method for producing SiC single crystal by using the production apparatus and crucible used in the production apparatus 有权
公开(公告)号：US09783911B2
公开(公告)日：2017-10-10
申请号：US14410969
申请日：2013-07-15
申请人： Nobuyoshi Yashiro , Kazuhito Kamei , Kazuhiko Kusunoki , Nobuhiro Okada , Koji Moriguchi , Hironori Daikoku , Hidemitsu Sakamoto , Motohisa Kado
发明人： Nobuyoshi Yashiro , Kazuhito Kamei , Kazuhiko Kusunoki , Nobuhiro Okada , Koji Moriguchi , Hironori Daikoku , Hidemitsu Sakamoto , Motohisa Kado
IPC分类号： C30B19/02 , C30B15/10 , C30B19/04 , C30B19/06 , C30B29/36 , C30B15/32
CPC分类号： C30B15/10 , C30B15/32 , C30B19/04 , C30B19/067 , C30B29/36 , Y10T117/1032
摘要： A production apparatus is used for a solution growth method. The production apparatus includes a seed shaft and a crucible. The seed shaft has a lower end surface to which an SiC seed crystal is attached. The crucible contains an SiC solution. The crucible includes a cylindrical portion, a bottom portion, and an inner lid. The bottom portion is disposed at a lower end of the cylindrical portion. The inner lid is disposed in the cylindrical portion. The inner lid has a through hole and is positioned below a liquid surface of the SiC solution when the SiC solution is contained in the crucible.

2. 发明申请

US20140116325A1 PRODUCTION APPARATUS OF SiC SINGLE CRYSTAL BY SOLUTION GROWTH METHOD, METHOD FOR PRODUCING SiC SINGLE CRYSTAL USING THE PRODUCTION APPARATUS, AND CRUCIBLE USED IN THE PRODUCTION APPARATUS 有权
标题翻译：通过溶液生长方法生产SiC单晶的生产方法，使用生产设备生产SiC单晶的方法，以及在生产设备中使用的可溶性碳纳米管
公开(公告)号：US20140116325A1
公开(公告)日：2014-05-01
申请号：US14126942
申请日：2012-06-11
申请人： Kazuhito Kamei , Kazuhiko Kusunoki , Nobuyoshi Yashiro , Nobuhiro Okada , Hironori Daikoku , Motohisa Kado , Hidamisu Kasamoto
发明人： Kazuhito Kamei , Kazuhiko Kusunoki , Nobuyoshi Yashiro , Nobuhiro Okada , Hironori Daikoku , Motohisa Kado , Hidamisu Kasamoto
IPC分类号： C30B15/10
CPC分类号： C30B15/10 , C30B17/00 , C30B19/02 , C30B19/08 , C30B29/36 , C30B35/00 , Y10T117/1032
摘要： A region of an SiC solution in the vicinity of an SiC seed crystal is cooled while suppressing the temperature variation in a peripheral region of the SiC solution. An apparatus includes a seed shaft and a crucible for an SiC solution. The seed shaft has a lower end surface for attachment to an SiC seed crystal. The crucible comprises a main body, an intermediate cover, and a top cover. The main body includes a first cylindrical portion and a bottom portion at a lower end portion of the first cylindrical portion. The intermediate cover is within the first cylindrical portion and above the liquid level of the SiC solution in the main body. The intermediate cover has a first through hole for the seed shaft. The top cover is disposed above the intermediate cover and has a second through hole for the seed shaft to pass through.
摘要翻译：在SiC晶种附近的SiC溶液的区域被冷却，同时抑制SiC溶液的周边区域的温度变化。一种装置包括种子轴和用于SiC溶液的坩埚。种子轴具有用于连接到SiC晶种的下端表面。坩埚包括主体，中间盖和顶盖。主体包括在第一圆筒部的下端部的第一圆筒部和底部。中间盖在主体内的第一圆柱形部分内和SiC溶液的液面之上。中间盖具有用于种子轴的第一通孔。顶盖设置在中间盖的上方，并且具有用于种子轴穿过的第二通孔。

3. 发明授权

US08492774B2 Method and apparatus for manufacturing a SiC single crystal film 有权
标题翻译： SiC单晶膜的制造方法和装置
公开(公告)号：US08492774B2
公开(公告)日：2013-07-23
申请号：US13033767
申请日：2011-02-24
申请人： Kazuhiko Kusunoki , Kazuhito Kamei , Nobuyoshi Yashiro , Ryo Hattori
发明人： Kazuhiko Kusunoki , Kazuhito Kamei , Nobuyoshi Yashiro , Ryo Hattori
IPC分类号： H01L29/15
CPC分类号： C30B29/36 , C30B19/02 , C30B19/04 , C30B19/10 , Y10T117/1024
摘要： A manufacturing method for a SiC single crystal film which allows stable growth of a SiC epitaxial film with a low doping concentration on a substrate with a diameter of at least 2 inches by the LPE method using a SiC solution in solvent of a melt includes an evacuation step in which the interior of a crystal growth furnace is evacuated with heating until the vacuum pressure at the crystal growth temperature is 5×10−3 Pa or lower prior to introducing a raw material for the melt into the furnace. Then, a crucible containing a raw material for the melt is introduced into the furnace, a SiC solution is formed, and a SiC epitaxial film is grown on a substrate immersed in the solution.
摘要翻译：一种SiC单晶膜的制造方法，其通过LPE法在熔体溶剂中使用SiC溶液，使具有低掺杂浓度的SiC外延膜在直径至少为2英寸的基板上稳定地生长，其包括抽真空在将熔体原料引入炉内之前，将晶体生长炉的内部加热抽真空直到晶体生长温度下的真空压力为5×10 -3 Pa以下的步骤。然后，将含有熔体原料的坩埚引入炉内，形成SiC溶液，在沉积在溶液中的基板上生长SiC外延膜。

4. 发明申请

US20120211769A1 Sic single crystal wafer and process for production thereof 有权
标题翻译： Sic单晶晶片及其制造方法
公开(公告)号：US20120211769A1
公开(公告)日：2012-08-23
申请号：US13385566
申请日：2012-02-27
申请人： Kazuhiko Kusunoki , Kazuhito Kamei , Nobuyoshi Yashiro , Junichi Koike
发明人： Kazuhiko Kusunoki , Kazuhito Kamei , Nobuyoshi Yashiro , Junichi Koike
IPC分类号： H01L29/16 , B32B3/02 , C30B19/04 , H01L21/20 , C01B31/36 , B32B5/00 , B32B9/04 , B82Y30/00
CPC分类号： C30B29/36 , C30B19/02 , C30B19/04 , C30B19/062 , Y10T428/21 , Y10T428/265
摘要： A SiC single crystal wafer on which a good quality epitaxial film by suppressing defects derived from the wafer can be grown has an affected surface layer with a thickness of at most 50 nm and a SiC single crystal portion with an oxygen content of at most 1.0×1017 atoms/cm3. This SiC single crystal wafer is manufactured from a high purity SiC bulk single crystal obtained by the solution growth method using raw materials with an oxygen content of at most 100 ppm and a non-oxidizing atmosphere having an oxygen concentration of at most 100 ppm.
摘要翻译：通过抑制从晶片产生的缺陷可以生长出其质量良好的外延膜的SiC单晶晶片具有厚度至多为50nm的受影响的表面层和氧含量至多为1.0×x的SiC单晶部分 1017原子/ cm3。该SiC单晶晶片由使用氧含量为100ppm以下的原料和氧浓度为100ppm以下的非氧化性气氛的溶液生长法得到的高纯度SiC体单晶制造。

5. 发明申请

US20110200833A1 METHOD OF MANUFACTURING A SILICON CARBIDE SINGLE CRYSTAL 有权
标题翻译：制造单晶碳化硅单晶的方法
公开(公告)号：US20110200833A1
公开(公告)日：2011-08-18
申请号：US13036101
申请日：2011-02-28
申请人： Kazuhito KAMEI , Kazuhiko Kusunoki , Nobuyoshi Yashiro , Akihiro Yauchi , Shinji Shimosaki
发明人： Kazuhito KAMEI , Kazuhiko Kusunoki , Nobuyoshi Yashiro , Akihiro Yauchi , Shinji Shimosaki
IPC分类号： C30B19/04 , C30B29/36
CPC分类号： C30B19/04 , C30B9/10 , C30B19/02 , C30B19/10 , C30B29/36
摘要： A method capable of stably manufacturing a SiC single crystal in the form of a thin film or a bulk crystal having a low carrier density of at most 5×1017/cm3 and preferably less than 1×1017/cm3 and which is suitable for use in various devices by liquid phase growth using a SiC solution in which the solvent is a melt of a Si alloy employs a Si alloy having a composition which is expressed by SixCryTiz wherein x, y, and z (each in atomic percent) satisfy 0.50
摘要翻译：一种能够稳定地制造低载体密度至多为5×1017 / cm3，优选小于1×1017 / cm3的薄膜或本体晶体形式的SiC单晶的方法，其适用于使用其中溶剂是Si合金的熔体的SiC溶液的液相生长的各种装置采用具有由SixCryTiz表示的组成的Si合金，其中x，y和z（以原子百分比计）满足0.50

6. 发明申请

US20110198614A1 METHOD AND APPARATUS FOR MANUFACTURING A SiC SINGLE CRYSTAL FILM 有权
标题翻译：用于制造SiC单晶膜的方法和装置
公开(公告)号：US20110198614A1
公开(公告)日：2011-08-18
申请号：US13033767
申请日：2011-02-24
申请人： Kazuhiko KUSUNOKI , Kazuhito Kamei , Nobuyoshi Yashiro , Ryo Hattori
发明人： Kazuhiko KUSUNOKI , Kazuhito Kamei , Nobuyoshi Yashiro , Ryo Hattori
IPC分类号： H01L29/161 , C30B19/04 , C30B19/06 , C30B19/12
CPC分类号： C30B29/36 , C30B19/02 , C30B19/04 , C30B19/10 , Y10T117/1024
摘要： A manufacturing method for a SiC single crystal film which allows stable growth of a SiC epitaxial film with a low doping concentration on a substrate with a diameter of at least 2 inches by the LPE method using a SiC solution in solvent of a melt includes an evacuation step in which the interior of a crystal growth furnace is evacuated with heating until the vacuum pressure at the crystal growth temperature is 5×10−3 Pa or lower prior to introducing a raw material for the melt into the furnace. Then, a crucible containing a raw material for the melt is introduced into the furnace, a SiC solution is formed, and a SiC epitaxial film is grown on a substrate immersed in the solution.
摘要翻译：一种SiC单晶膜的制造方法，其通过LPE法在熔体溶剂中使用SiC溶液，使具有低掺杂浓度的SiC外延膜在直径至少为2英寸的基板上稳定地生长，其包括抽真空在将熔体原料引入炉内之前，将晶体生长炉的内部加热抽真空直到晶体生长温度下的真空压力为5×10 -3 Pa以下的步骤。然后，将含有熔体原料的坩埚引入炉内，形成SiC溶液，在沉积在溶液中的基板上生长SiC外延膜。

7. 发明授权

US07520930B2 Silicon carbide single crystal and a method for its production 有权
标题翻译：碳化硅单晶及其制造方法
公开(公告)号：US07520930B2
公开(公告)日：2009-04-21
申请号：US10967070
申请日：2004-10-15
申请人： Kazuhiko Kusunoki , Shinji Munetoh , Kazuhito Kamei
发明人： Kazuhiko Kusunoki , Shinji Munetoh , Kazuhito Kamei
IPC分类号： C30B1/00 , C30B28/02 , C30B25/00
CPC分类号： C30B29/36 , C30B11/00
摘要： A bulk silicon carbide single crystal of good crystalline quality which includes a minimized number of structural defects and is free from micropipe defects can be produced by crystal growth in a melt of an alloy comprising Si, C, and M (wherein M is either Mn or Ti) and having an atomic ratio between Si and M in which the value of x, when express as Si1-xMx, is 0.1≦x≦0.7 in the case where M is Mn or 0.1≦x≦0.25 in the case where M is Ti at a temperature of the melt which is below 2000° C. The C component is preferably supplied into the melt by dissolution of a graphite crucible which contains the melt such that the melt is free from undissolved C. One method of crystal growth is performed by cooling the melt after a seed substrate is immersed in the melt.
摘要翻译：具有最小数量的结构缺陷并且没有微管缺陷的良好结晶质量的块状碳化硅单晶可以通过在包含Si，C和M的合金的熔体中的晶体生长（其中M为Mn或 Ti），并且在M和Mn之间的原子比在X表示为Si1-xMx时的x的值为0.1≤x≤0.7，在M为Mn或0.1≤x≤0.25的情况下在熔体温度低于2000℃时M为Ti的情况。优选通过溶解包含熔体的石墨坩埚使熔融物不溶解C而将C成分供入熔体中。一种方法晶种生长通过在种子基底浸入熔体中之后冷却熔融物来进行。

8. 发明申请

US20070209573A1 Method for preparing silicon carbide single crystal 有权
标题翻译：碳化硅单晶的制备方法
公开(公告)号：US20070209573A1
公开(公告)日：2007-09-13
申请号：US11712841
申请日：2007-03-01
申请人： Kazuhiko Kusunoki , Kazuhito Kamei , Nobuyoshi Yashiro , Akihiro Yauchi , Yoshihisa Ueda , Yutaka Itoh , Nobuhiro Okada
发明人： Kazuhiko Kusunoki , Kazuhito Kamei , Nobuyoshi Yashiro , Akihiro Yauchi , Yoshihisa Ueda , Yutaka Itoh , Nobuhiro Okada
IPC分类号： C30B15/00 , C30B19/00
CPC分类号： C30B9/06 , C30B9/10 , C30B15/305 , C30B17/00 , C30B19/02 , C30B19/04 , C30B29/36 , Y10T117/10 , Y10T117/1004 , Y10T117/1008 , Y10T117/1016 , Y10T117/1072
摘要： A SiC single crystal is produced by the solution growth method in which a seed crystal attached to a seed shaft is immersed in a solution of SiC dissolved in a melt of Si or a Si alloy and a SiC single crystal is allowed to grow on the seed crystal by gradually cooling the solution or by providing a temperature gradient therein. To this method, accelerated rotation of a crucible is applied by repeatedly accelerating to a prescribed rotational speed and holding at that speed and decelerating to a lower rotational speed or a 0 rotational speed. The rotational direction of the crucible may be reversed each acceleration. The seed shaft may also be rotated synchronously with the rotation of the crucible in the same or opposite rotational as the crucible. A large, good quality single crystal having no inclusions are produced with a high crystal growth rate.
摘要翻译：通过溶液生长法生产SiC单晶，其中将种子轴附着的晶种浸入溶解在Si或Si合金熔体中的SiC溶液中，使SiC单晶在种子上生长通过逐渐冷却溶液或通过在其中提供温度梯度来制备。对于这种方法，通过反复加速到规定的转速并以该速度保持并且减速到较低的转速或0转速来施加坩埚的加速旋转。坩埚的旋转方向可以反转每个加速度。种子轴也可以与坩埚的旋转同步旋转，与坩埚相同或相反。以高的晶体生长速率生产不含夹杂物的大质量好的单晶。

9. 发明申请

US20050183657A1 Silicon carbide single crystal and a method for its production 有权
标题翻译：碳化硅单晶及其制造方法
公开(公告)号：US20050183657A1
公开(公告)日：2005-08-25
申请号：US10967070
申请日：2004-10-15
申请人： Kazuhiko Kusunoki , Shinji Munetoh , Kazuhito Kamei
发明人： Kazuhiko Kusunoki , Shinji Munetoh , Kazuhito Kamei
IPC分类号： C30B11/00 , C30B29/36 , C30B1/00
CPC分类号： C30B29/36 , C30B11/00
摘要： A bulk silicon carbide single crystal of good crystalline quality which includes a minimized number of structural defects and is free from micropipe defects can be produced by crystal growth in a melt of an alloy comprising Si, C, and M (wherein M is either Mn or Ti) and having an atomic ratio between Si and M in which the value of x, when express as Si1-xMx, is 0.1≦×≦0.7 in the case where M is Mn or 0.1≦×≦0.25 in the case where M is Ti at a temperature of the melt which is below 2000° C. The C component is preferably supplied into the melt by dissolution of a graphite crucible which contains the melt such that the melt is free from undissolved C. One method of crystal growth is performed by cooling the melt after a seed substrate is immersed in the melt.
摘要翻译：具有最小数量的结构缺陷并且没有微管缺陷的良好结晶质量的块状碳化硅单晶可以通过在包含Si，C和M的合金的熔体中的晶体生长（其中M为Mn或 Ti），并且具有Si和M之间的原子比，其中当x 1表示为Si 1-x M x x时，x的值为0.1 <= x <= 0.7 在熔体温度低于2000℃时M为Ti的情况下，M为Mn或0.1 <= x <= 0.25的情况。优选通过溶解石墨坩埚将C成分供入熔体中其包含熔体，使得熔体不含未溶解的C.晶种生长的一种方法是在种子基底浸入熔体中之后冷却熔体。

10. 发明授权

US06764767B2 Graphite powders suited for negative electrode material of lithium ion secondary battery 失效
标题翻译：适用于锂离子二次电池负极材料的石墨粉
公开(公告)号：US06764767B2
公开(公告)日：2004-07-20
申请号：US09292834
申请日：1999-04-16
申请人： Koji Moriguchi , Mitsuhara Yonemura , Kazuhito Kamei , Masaru Abe , Hideya Kaminaka , Noriyuki Negi , Atsuo Omaru , Masayuki Nagamine
发明人： Koji Moriguchi , Mitsuhara Yonemura , Kazuhito Kamei , Masaru Abe , Hideya Kaminaka , Noriyuki Negi , Atsuo Omaru , Masayuki Nagamine
IPC分类号： C01B3104
CPC分类号： H01M10/0525 , C01B32/20 , C01P2002/60 , C01P2002/72 , C01P2006/80 , H01M4/133 , H01M4/587 , H01M2004/021 , Y10T428/30
摘要： A graphite powder suitable for a negative electrode material of a lithium ion secondary battery which assures a high discharging capacity not lower than 320 mAh/g is to be manufactured at a lower cost. Specifically, a graphite powder containing 0.01 to 5.0 wt % of boron and having a looped closure structure at an end of a graphite c-planar layer on the surface of a powder, with the density of the interstitial planar sections between neighboring closure structures being not less than 100/&mgr;m and not more than 1500/&mgr;m, and with d002 being preferably not larger than 3.3650 Å, is manufactured by (1) heat-treating a carbon material pulverized at an elevated speed before or after carbonization for graphization at temperature exceeding 1500° C. or by (2) heat-treating the carbon material pulverized before or after carbonization at a temperature exceeding 1500° C. for graphization and subsequently further heat-treating the graphized material at a temperature exceeding a temperature of the oxidating heat treatment and the heat treatment in the inert gas.
摘要翻译：以更低的成本制造适合于确保高放电容量不低于320mAh / g的锂离子二次电池的负极材料的石墨粉末。具体地说，在粉末表面上，在石墨c平面层的端部含有0.01〜5.0重量％的硼并且具有环状封闭结构的石墨粉末，相邻闭合结构之间的间隙平面部分的密度不是小于100 /小时且不超过1500 / mum，d002优选不大于3.3650，通过以下方法制造：（1）在碳化之前或之后以高速粉碎的碳材料进行热处理，以在超过或者（2）在碳化之前或之后粉碎的碳材料在超过1500℃的温度下进行热处理，以进行石墨化，随后在超过氧化热处理温度的温度下进一步热处理石墨化材料并在惰性气体中进行热处理。

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