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21.发明申请Graphite powders suited for negative electrode material of lithium ion secondary battery 失效适用于锂离子二次电池负极材料的石墨粉公开(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
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。
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22.发明申请Graphite powders suited for negative electrode material of lithium ion secondary battery 失效适用于锂离子二次电池负极材料的石墨粉公开(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
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。
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公开(公告)号：US08492774B2
公开(公告)日：2013-07-23
申请号：US13033767
申请日：2011-02-24
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。
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公开(公告)号：US20120211769A1
公开(公告)日：2012-08-23
申请号：US13385566
申请日：2012-02-27
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。
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公开(公告)号：US20110198614A1
公开(公告)日：2011-08-18
申请号：US13033767
申请日：2011-02-24
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。
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公开(公告)号：US07520930B2
公开(公告)日：2009-04-21
申请号：US10967070
申请日：2004-10-15
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。
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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
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。
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公开(公告)号：US20050183657A1
公开(公告)日：2005-08-25
申请号：US10967070
申请日：2004-10-15
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。
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29.发明授权Graphite powders suited for negative electrode material of lithium ion secondary battery 失效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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30.发明授权公开(公告)号：US06576369B1
公开(公告)日：2003-06-10
申请号：US09138561
申请日：1998-08-24
申请人： Koji Moriguchi , Mitsuharu Yonemura , Kazuhito Kamei , Noriyuki Negi , Masaru Abe , Hideya Kaminaka
发明人： Koji Moriguchi , Mitsuharu Yonemura , Kazuhito Kamei , Noriyuki Negi , Masaru Abe , Hideya Kaminaka
IPC分类号： C01B3104
CPC分类号： H01M4/583 , C01B32/20 , C01P2002/60 , C01P2006/12 , C01P2006/40 , H01M4/133 , H01M4/622 , H01M4/623 , H01M6/10 , H01M10/0525
摘要： A graphite powder has surface closed-end structures in which the graphite c-plane layers of the graphite layer crystal lattices have closed-ends on the surface of the graphite powder by linking the ends of one or more pairs of the c-plane layers, leaving interstices which are open on the surface of the graphite. The number of open interstices is at least 100 and at most 1500 per micrometer in a c-axis direction of the graphite. Preferably, the graphite powder has a specific surface area of 1.0 m2/g or less. Such a graphite powder can be prepared either by graphitizing a carbon material, which has been pulverized at a high speed under well-controlled conditions before and/or after the carbonization, or by subjecting a carbon material, which has been pulverized under well-controlled conditions before and/or after the carbonization, to graphitization and then to oxidative heat treatment at a temperature of 600-800° C. and finally to heat treatment at a temperature of 800° C. or higher in an inert gas. The graphite powder can be used to produce negative electrodes of lithium ion secondary batteries having a high discharge capacity of at least 320 mAh/g and a high charge/discharge coulombic efficiency of at least 90%.
摘要翻译： 石墨粉末具有表面封闭端结构，其中石墨层晶格的石墨c面层通过连接一对或多对c面层的端部而在石墨粉末的表面上具有封闭端， 留下在石墨表面开放的间隙。 在石墨的c轴方向上，开口间隙的数量为至少100个，最高为1500微米。 优选石墨粉的比表面积为1.0m 2 / g以下。 这样的石墨粉末可以通过在碳化之前和/或之后在良好控制的条件下高速粉碎的碳材料进行石墨化，或者通过将被粉碎的碳材料进行良好控制 在碳化之前和/或之后的条件进行石墨化，然后在600-800℃的温度下进行氧化热处理，最后在惰性气体中在800℃以上的温度下进行热处理。 该石墨粉末可用于制造具有至少320mAh / g的高放电容量和高充放电库仑效率至少为90％的锂离子二次电池的负极。
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