公开(公告)号：US09702056B2

公开(公告)日：2017-07-11

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 ,  Hidemitsu Sakamoto

发明人： Kazuhito Kamei ,  Kazuhiko Kusunoki ,  Nobuyoshi Yashiro ,  Nobuhiro Okada ,  Hironori Daikoku ,  Motohisa Kado ,  Hidemitsu Sakamoto

IPC分类号： C30B15/10 ,  C30B35/00 ,  C30B19/02 ,  C30B29/36 ,  C30B17/00 ,  C30B19/08

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.

公开(公告)号：US09512540B2

公开(公告)日：2016-12-06

申请号：US13883350

申请日：2011-11-04

申请人： Kazuhiko Kusunoki ,  Kazuhito Kamei ,  Nobuyoshi Yashiro ,  Kouji Moriguchi ,  Nobuhiro Okada ,  Katsunori Danno ,  Hironori Daikoku

发明人： Kazuhiko Kusunoki ,  Kazuhito Kamei ,  Nobuyoshi Yashiro ,  Kouji Moriguchi ,  Nobuhiro Okada ,  Katsunori Danno ,  Hironori Daikoku

IPC分类号： C30B15/20 ,  C30B17/00 ,  C30B19/02 ,  C30B29/36 ,  C30B15/10 ,  C30B15/30 ,  C30B15/36

CPC分类号： C30B15/20 ,  C30B15/10 ,  C30B15/30 ,  C30B15/36 ,  C30B17/00 ,  C30B19/02 ,  C30B29/36

摘要： A method for manufacturing an n-type SiC single crystal, enables the suppression of the variation in nitrogen concentration among a plurality of n-type SiC single crystal ingots manufactured. A method includes the steps of: providing a manufacturing apparatus (100) including a chamber (1) having an area in which a crucible (7) is to be disposed; heating the area in which the crucible (7) is to be disposed and evacuating the gas in the chamber (1); filling, after the evacuation, the chamber (1) with a mixed gas containing a noble gas and nitrogen gas; heating and melting a starting material housed in the crucible (7) disposed in the area to produce a SiC solution (8) containing silicon and carbon; and immersing a SiC seed crystal into the SiC solution under the mixed gas atmosphere to grow an n-type SiC single crystal on the SiC seed crystal.

摘要翻译： 制造n型SiC单晶的方法能够抑制制造的多个n型SiC单晶锭中的氮浓度的变化。 一种方法包括以下步骤：提供一种制造装置（100），该制造装置（100）包括具有坩埚（7）将被设置的区域的腔室（1） 加热要安置坩埚（7）的区域并抽空腔室（1）中的气体; 在排气之后用包含惰性气体和氮气的混合气体填充室（1）; 加热和熔化容纳在所述区域中的坩埚（7）中的原料以产生含有硅和碳的SiC溶液（8）; 并在混合气体气氛下将SiC晶种浸入SiC溶液中，以在SiC晶种上生长n型SiC单晶。

公开(公告)号：US09388508B2

公开(公告)日：2016-07-12

申请号：US13997766

申请日：2011-12-26

申请人： Kazuhito Kamei ,  Kazuhiko Kusunoki ,  Nobuyoshi Yashiro ,  Nobuhiro Okada ,  Motohisa Kado ,  Hidemitsu Sakamoto ,  Hironori Daikoku

发明人： Kazuhito Kamei ,  Kazuhiko Kusunoki ,  Nobuyoshi Yashiro ,  Nobuhiro Okada ,  Motohisa Kado ,  Hidemitsu Sakamoto ,  Hironori Daikoku

IPC分类号： C30B11/04 ,  C30B15/32 ,  C30B19/06 ,  C30B29/36

CPC分类号： C30B15/32 ,  C30B19/06 ,  C30B29/36 ,  Y10T117/1032 ,  Y10T117/1072

摘要： A manufacturing apparatus of a SiC single crystal which can suppress the generation of a polycrystal is provided. A jig (41) and a crucible (6) are accommodated in a chamber (1). A SiC solution (8) is housed in the crucible (6). The jig (41) includes a seed shaft (411) and a cover member (412). The seed shaft (411) can move up and down, and a SiC seed crystal (9) is attached to the lower surface thereof. The cover member (412) is attached to the lower end portion of the seed shaft (411). The cover member (412) is a housing which has an opening at its lower end, wherein the lower end portion of the seed shaft (411) is disposed in the cover member (412).

摘要翻译： 提供了可以抑制多晶体的产生的SiC单晶的制造装置。 夹具（41）和坩埚（6）容纳在腔室（1）中。 将SiC溶液（8）容纳在坩埚（6）中。 夹具（41）包括种子轴（411）和盖构件（412）。 种子轴（411）可以上下移动，并且其SiC晶种（9）附着到其下表面。 盖构件（412）附接到种子轴（411）的下端部。 盖构件（412）是在其下端具有开口的壳体，其中种子轴（411）的下端部设置在盖构件（412）中。

公开(公告)号：US20130305981A1

公开(公告)日：2013-11-21

申请号：US13997766

申请日：2011-12-26

申请人： Kazuhito Kamei ,  Kazuhiko Kusunoki ,  Nobuyoshi Yashiro ,  Nobuhiro Okada ,  Motohisa Kado ,  Hidemitsu Sakamoto ,  Hironori Daikoku

发明人： Kazuhito Kamei ,  Kazuhiko Kusunoki ,  Nobuyoshi Yashiro ,  Nobuhiro Okada ,  Motohisa Kado ,  Hidemitsu Sakamoto ,  Hironori Daikoku

IPC分类号： C30B15/32

CPC分类号： C30B15/32 ,  C30B19/06 ,  C30B29/36 ,  Y10T117/1032 ,  Y10T117/1072

摘要： A manufacturing apparatus of a SiC single crystal which can suppress the generation of a polycrystal is provided. A jig (41) and a crucible (6) are accommodated in a chamber (1). A SiC solution (8) is housed in the crucible (6). The jig (41) includes a seed shaft (411) and a cover member (412). The seed shaft (411) can move up and down, and a SiC seed crystal (9) is attached to the lower surface thereof. The cover member (412) is attached to the lower end portion of the seed shaft (411). The cover member (412) is a housing which has an opening at its lower end, wherein the lower end portion of the seed shaft (411) is disposed in the cover member (412).

摘要翻译： 提供了可以抑制多晶体的产生的SiC单晶的制造装置。 夹具（41）和坩埚（6）容纳在腔室（1）中。 将SiC溶液（8）容纳在坩埚（6）中。 夹具（41）包括种子轴（411）和盖构件（412）。 种子轴（411）可以上下移动，并且其SiC晶种（9）附着到其下表面。 盖构件（412）附接到种子轴（411）的下端部。 盖构件（412）是在其下端具有开口的壳体，其中种子轴（411）的下端部设置在盖构件（412）中。

公开(公告)号：US07659033B2

公开(公告)日：2010-02-09

申请号：US11686204

申请日：2007-03-14

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： H01M4/58 ,  C01B31/04

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/μm and not more than 1500/μm, 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。

公开(公告)号：US07635413B2

公开(公告)日：2009-12-22

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： C30B23/00 ,  C30B28/12

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。

公开(公告)号：US20070154812A1

公开(公告)日：2007-07-05

申请号：US11686204

申请日：2007-03-14

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： H01M4/58 ,  C01B31/04

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/μm and not more than 1500/μm, 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. forgraphization and subsequently firterheat-treating the graphized material at a temperature exceeding a temperature of the oxidating heat treatnent 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 通过（1）在碳化之前或之后以高速粉碎的碳材料进行热处理，以在温度下进行石墨化，制造小于100 / mum且不大于1500 / mum，d 002优选不大于3.3650 超过1500℃，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，然后在超过氧化热处理温度的温度下对石墨化材料进行热处理， 惰性气体中的热处理。

公开(公告)号：US20060134523A1

公开(公告)日：2006-06-22

申请号：US10826233

申请日：2004-04-16

申请人： Koji Moriguchi ,  Mitsuharu Yonemura ,  Kazuhito Kamei ,  Masaru Abe ,  Hideya Kaminaka ,  Noriyuki Negi ,  Atsuo Omaru ,  Masayuki Nagamine

发明人： Koji Moriguchi ,  Mitsuharu Yonemura ,  Kazuhito Kamei ,  Masaru Abe ,  Hideya Kaminaka ,  Noriyuki Negi ,  Atsuo Omaru ,  Masayuki Nagamine

IPC分类号： H01M4/58 ,  C01B31/04

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/μm and not more than 1500/μm, 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. forgraphization 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℃的温度下热处理，然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， 惰性气体中的热处理。

公开(公告)号：US09631295B2

公开(公告)日：2017-04-25

申请号：US14006640

申请日：2011-07-27

申请人： Hironori Daikoku ,  Kazuhito Kamei

发明人： Hironori Daikoku ,  Kazuhito Kamei

IPC分类号： C30B15/22 ,  C30B29/36 ,  C30B19/04 ,  C30B19/06 ,  C30B19/12 ,  C30B17/00

CPC分类号： C30B15/22 ,  C30B17/00 ,  C30B19/04 ,  C30B19/061 ,  C30B19/12 ,  C30B29/36 ,  Y10T117/1032

摘要： Provided is a method for producing SiC single crystals while maintaining a temperature gradient such that the temperature decreases from within an Si solution inside a graphite crucible toward the solution surface, with the SiC seed crystals that have contacted the solution surface serving as the starting point for crystal seed growth, wherein when the crystal growth surface of the SiC seed crystals, which serves as the starting point for SiC single crystal growth, contacts the solution surface, the height by which the solution rises to the side of the SiC seed crystals is within the range where the SiC single crystals that have grown from the crystal growth surface and the SiC single crystals that have grown from the side grow as one SiC single crystal unit. Also provided is a device for producing an SiC single crystal comprising a graphite crucible, a heating device for heating and melting base materials in the crucible to form a base material solution and maintaining a temperature gradient required for growth of SiC single crystal, a support rod which holds a SiC seed crystal at its bottom end, and a holding structure which maintains the holding by the support rod so that a height by which the solution rises to the side of the SiC seed crystal is within a range where the SiC single crystal that have grown from the crystal growth surface and the SiC single crystal that have grown from the side grow as one SiC single crystal unit.

公开(公告)号：US09222198B2

公开(公告)日：2015-12-29

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： C30B19/02 ,  H01L21/02 ,  H01L21/16 ,  C30B29/36 ,  C30B19/04 ,  C30B19/06

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。