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1. 发明授权

US08236453B2 Carbon-coated Li-containing powders and process for production thereof 有权
标题翻译：含碳的含碳粉末及其生产方法
公开(公告)号：US08236453B2
公开(公告)日：2012-08-07
申请号：US13042653
申请日：2011-03-08
申请人： Albane Audemer , Calin Wurm , Mathieu Morcrette , Sylvain Gwizdala , Christian Masquelier
发明人： Albane Audemer , Calin Wurm , Mathieu Morcrette , Sylvain Gwizdala , Christian Masquelier
IPC分类号： H01M4/58
CPC分类号： H01M4/5825 , C01B25/37 , C01B25/375 , C01B25/45 , H01M4/131 , H01M4/1391 , H01M4/36 , H01M4/366 , H01M4/62 , H01M4/624 , H01M4/625 , H01M6/185 , H01M10/052 , H01M10/0562 , H01M2004/021 , H01M2004/028
摘要： The invention provides a new route for the synthesis of carbon-coated powders having the olivine or NASICON structure, which form promising classes of active products for the manufacture of rechargeable lithium batteries. Carbon-coating of the powder particles is necessary to achieve good performances because of the rather poor electronic conductivity of said structures. For the preparation of coated LiFePO4, sources of Li, Fe and phosphate are dissolved in an aqueous solution together with a polycarboxylic acid and a polyhydric alcohol. Upon water evaporation, polyesterification occurs while a mixed precipitate is formed containing Li, Fe and phosphate. The resin-encapsulated mixture is then heat treated at 700° C. in a reducing atmosphere. This results in the production of a fine powder consisting of an olivine LiFePO4, phase, coated with conductive carbon. When this powder is used as active material in a lithium insertion-type electrode, fast charge and discharge rates are obtained at room temperature and an excellent capacity retention is observed.
摘要翻译：本发明提供了一种用于合成具有橄榄石或NASICON结构的碳涂覆粉末的新途径，其形成用于制造可再充电锂电池的有希望的活性产品类别。由于所述结构的电子导电性差，所以粉末颗粒的碳涂层是必需的，以获得良好的性能。为了制备涂覆的LiFePO 4，将Li，Fe和磷酸盐源与多元羧酸和多元醇一起溶解在水溶液中。当水蒸发时，在形成含有Li，Fe和磷酸盐的混合沉淀物的同时发生聚酯化。然后将树脂包封的混合物在还原气氛中在700℃下进行热处理。这导致生产由用导电碳涂覆的橄榄石LiFePO 4相的细粉末。当这种粉末用作锂插入型电极中的活性材料时，在室温下能够获得快速的充放电率，并且观察到优异的容量保持率。

2. 发明申请

US20090072203A1 Carbon-Coated Li-Containing Powders and Process for Production Thereof 有权
标题翻译：含碳酸钙的粉末及其生产工艺
公开(公告)号：US20090072203A1
公开(公告)日：2009-03-19
申请号：US12270969
申请日：2008-11-14
申请人： Albane AUDEMER , Calin Wurm , Mathieu Morcrette , Sylvain Gwizdala , Christian Masquelier
发明人： Albane AUDEMER , Calin Wurm , Mathieu Morcrette , Sylvain Gwizdala , Christian Masquelier
IPC分类号： H01B1/24
CPC分类号： H01M4/5825 , C01B25/37 , C01B25/375 , C01B25/45 , H01M4/131 , H01M4/1391 , H01M4/36 , H01M4/366 , H01M4/62 , H01M4/624 , H01M4/625 , H01M6/185 , H01M10/052 , H01M10/0562 , H01M2004/021 , H01M2004/028
摘要： The invention provides a new route for the synthesis of carbon-coated powders having the olivine or NASICON structure, which form promising classes of active products for the manufacture of rechargeable lithium batteries. Carbon-coating of the powder particles is necessary to achieve good performances because of the rather poor electronic conductivity of said structures. For the preparation of coated LiFePO4, sources of Li, Fe and phosphate are dissolved in an aqueous solution together with a polycarboxylic acid and a polyhydric alcohol. Upon water evaporation, polyesterification occurs while a mixed precipitate is formed containing Li, Fe and phosphate. The resin-encapsulated mixture is then heat treated at 700° C. in a reducing atmosphere. This results in the production of a fine powder consisting of an olivine LiFePO4 phase, coated with conductive carbon. When this powder is used as active material in a lithium insertion-type electrode, fast charge and discharge rates are obtained at room temperature and an excellent capacity retention is observed.
摘要翻译：本发明提供了一种用于合成具有橄榄石或NASICON结构的碳涂覆粉末的新途径，其形成用于制造可再充电锂电池的有希望的活性产品类别。由于所述结构的电子导电性差，所以粉末颗粒的碳涂层是必需的，以获得良好的性能。为了制备涂覆的LiFePO 4，将Li，Fe和磷酸盐源与多元羧酸和多元醇一起溶解在水溶液中。当水蒸发时，在形成含有Li，Fe和磷酸盐的混合沉淀物的同时发生聚酯化。然后将树脂包封的混合物在还原气氛中在700℃下进行热处理。这导致由导电碳涂覆的由橄榄石LiFePO 4相组成的细粉末的生产。当这种粉末用作锂插入型电极中的活性材料时，在室温下能够获得快速的充放电率，并且观察到优异的容量保持率。

3. 发明授权

US07618747B2 Carbon-coated Li-containing powders and process for production thereof 失效
标题翻译：含碳的含碳粉末及其生产方法
公开(公告)号：US07618747B2
公开(公告)日：2009-11-17
申请号：US10518560
申请日：2003-06-19
申请人： Albane Audemer , Calin Wurm , Mathieu Morcrette , Sylvain Gwizdala , Christian Masquelier
发明人： Albane Audemer , Calin Wurm , Mathieu Morcrette , Sylvain Gwizdala , Christian Masquelier
IPC分类号： C01B25/00 , H01M4/58
CPC分类号： H01M4/5825 , C01B25/37 , C01B25/375 , C01B25/45 , H01M4/131 , H01M4/1391 , H01M4/36 , H01M4/366 , H01M4/62 , H01M4/624 , H01M4/625 , H01M6/185 , H01M10/052 , H01M10/0562 , H01M2004/021 , H01M2004/028
摘要： The invention provides a new route for the synthesis of carbon-coated powders having the olivine or NASICON structure, which form promising classes of active products for the manufacture of rechargeable lithium batteries. Carbon-coating of the powder particles is necessary to achieve good performances because of the rather poor electronic conductivity of said structures. For the preparation of coated LiFePO4, sources of Li, Fe and phosphate are dissolved in an aqueous solution together with a polycarboxylic acid and a polyhydric alcohol. Upon water evaporation, polyesterification occurs while a mixed precipitate is formed containing Li, Fe and phosphate. The resin-encapsulated mixture is then heat treated at 700° C. in a reducing atmosphere. This results in the production of a fine powder consisting of an olivine LiFePO4 phase, coated with conductive carbon. When this powder is used as active material in a lithium insertion-type electrode, fast charge and discharge rates are obtained at room temperature and an excellent capacity retention is observed.
摘要翻译：本发明提供了一种用于合成具有橄榄石或NASICON结构的碳涂覆粉末的新途径，其形成用于制造可再充电锂电池的有希望的活性产品类别。由于所述结构的电子导电性差，所以粉末颗粒的碳涂层是必需的，以获得良好的性能。为了制备涂覆的LiFePO 4，将Li，Fe和磷酸盐源与多元羧酸和多元醇一起溶解在水溶液中。当水蒸发时，在形成含有Li，Fe和磷酸盐的混合沉淀物的同时发生聚酯化。然后将树脂包封的混合物在还原气氛中在700℃下进行热处理。这导致由导电碳涂覆的由橄榄石LiFePO 4相组成的细粉末的生产。当这种粉末用作锂插入型电极中的活性材料时，在室温下能够获得快速的充放电率，并且观察到优异的容量保持率。

4. 发明授权

US07923154B2 Carbon-coated Li-containing powders and process for production thereof 有权
标题翻译：含碳的含碳粉末及其生产方法
公开(公告)号：US07923154B2
公开(公告)日：2011-04-12
申请号：US12270969
申请日：2008-11-14
申请人： Albane Audemer , Calin Wurm , Mathieu Morcrette , Sylvain Gwizdala , Christian Masquelier
发明人： Albane Audemer , Calin Wurm , Mathieu Morcrette , Sylvain Gwizdala , Christian Masquelier
IPC分类号： H01M4/58
CPC分类号： H01M4/5825 , C01B25/37 , C01B25/375 , C01B25/45 , H01M4/131 , H01M4/1391 , H01M4/36 , H01M4/366 , H01M4/62 , H01M4/624 , H01M4/625 , H01M6/185 , H01M10/052 , H01M10/0562 , H01M2004/021 , H01M2004/028
摘要： The invention provides a new route for the synthesis of carbon-coated powders having the olivine or NASICON structure, which form promising classes of active products for the manufacture of rechargeable lithium batteries. Carbon-coating of the powder particles is necessary to achieve good performances because of the rather poor electronic conductivity of said structures. For the preparation of coated LiFePO4, sources of Li, Fe and phosphate are dissolved in an aqueous solution together with a polycarboxylic acid and a polyhydric alcohol. Upon water evaporation, polyesterification occurs while a mixed precipitate is formed containing Li, Fe and phosphate. The resin-encapsulated mixture is then heat treated at 700° C. in a reducing atmosphere. This results in the production of a fine powder consisting of an olivine LiFePO4 phase, coated with conductive carbon. When this powder is used as active material in a lithium insertion-type electrode, fast charge and discharge rates are obtained at room temperature and an excellent capacity retention is observed.
摘要翻译：本发明提供了一种用于合成具有橄榄石或NASICON结构的碳涂覆粉末的新途径，其形成用于制造可再充电锂电池的有希望的活性产品类别。由于所述结构的电子导电性差，所以粉末颗粒的碳涂层是必需的，以获得良好的性能。为了制备涂覆的LiFePO 4，将Li，Fe和磷酸盐源与多元羧酸和多元醇一起溶解在水溶液中。当水蒸发时，在形成含有Li，Fe和磷酸盐的混合沉淀物的同时发生聚酯化。然后将树脂包封的混合物在还原气氛中在700℃下进行热处理。这导致由导电碳涂覆的由橄榄石LiFePO 4相组成的细粉末的生产。当这种粉末用作锂插入型电极中的活性材料时，在室温下能够获得快速的充放电率，并且观察到优异的容量保持率。

5. 发明申请

US20060035150A1 Carbon-coated li-containing powders and process for production thereof 失效
标题翻译：含碳的含Li粉末及其生产方法
公开(公告)号：US20060035150A1
公开(公告)日：2006-02-16
申请号：US10518560
申请日：2003-06-19
申请人： Albane Audemer , Calin Wurm , Mathieu Morcrette , Sylvain Gwizdala , Christain Masquelier
发明人： Albane Audemer , Calin Wurm , Mathieu Morcrette , Sylvain Gwizdala , Christain Masquelier
IPC分类号： H01M4/58 , B05D5/12
CPC分类号： H01M4/5825 , C01B25/37 , C01B25/375 , C01B25/45 , H01M4/131 , H01M4/1391 , H01M4/36 , H01M4/366 , H01M4/62 , H01M4/624 , H01M4/625 , H01M6/185 , H01M10/052 , H01M10/0562 , H01M2004/021 , H01M2004/028
摘要： The invention provides a new route for the synthesis of carbon-coated powders having the olivine or NASICON structure, which form promising classes of active products for the manufacture of rechargeable lithium batteries. Carbon-coating of the powder particles is necessary to achieve good performances because of the rather poor electronic conductivity of said structures. For the preparation of coated LiFePO4, sources of Li, Fe and phosphate are dissolved in an aqueous solution together with a polycarboxylic acid and a polyhydric alcohol. Upon water evaporation, polyesterification occurs while a mixed precipitate is formed containing Li, Fe and phosphate. The resin-encapsulated mixture is then heat treated at 700° C. in a reducing atmosphere. This results in the production of a fine powder consisting of an olivine LiFePO4 phase, coated with conductive carbon. When this powder is used as active material in a lithium insertion-type electrode, fast charge and discharge rates are obtained at room temperature and an excellent capacity retention is observed.
摘要翻译：本发明提供了一种用于合成具有橄榄石或NASICON结构的碳涂覆粉末的新途径，其形成用于制造可再充电锂电池的有希望的活性产品类别。由于所述结构的电子导电性差，所以粉末颗粒的碳涂层是必需的，以获得良好的性能。为了制备涂覆的LiFePO 4，将Li，Fe和磷酸盐源与多元羧酸和多元醇一起溶解在水溶液中。当水蒸发时，在形成含有Li，Fe和磷酸盐的混合沉淀物的同时发生聚酯化。然后将树脂包封的混合物在还原气氛中在700℃下进行热处理。这导致生产由导电碳涂覆的由橄榄石LiFePO 4 N 4相组成的细粉末。当这种粉末用作锂插入型电极中的活性材料时，在室温下能够获得快速的充放电率，并且观察到优异的容量保持率。

6. 发明授权

US07371482B2 Lithium transition-metal phosphate powder for rechargeable batteries 有权
标题翻译：用于充电电池的锂过渡金属磷酸盐粉末
公开(公告)号：US07371482B2
公开(公告)日：2008-05-13
申请号：US10719134
申请日：2003-11-21
申请人： Calin Wurm , Mathieu Morcrette , Sylvain Gwizdala , Christian Masquelier
发明人： Calin Wurm , Mathieu Morcrette , Sylvain Gwizdala , Christian Masquelier
IPC分类号： H01M4/58 , C01B25/30
CPC分类号： H01M4/136 , C01B25/375 , C01B25/377 , C01B25/45 , H01M4/1397 , H01M4/5825 , H01M10/052
摘要： Methods of manufacture and use of phosphates of transition metals are described as positive electrodes for secondary lithium batteries, including a process for the production of LiMPO4 with controlled size and morphology, M being FexCoyNizMnw, where 0≦x≦1,0≦y≦1, 0≦w≦1, and x+y+z+w=1. According to an exemplary embodiment, a process is described for the manufacture of LiFePO4 including the steps of providing an equimolar aqueous solution of Li1+, Fe3+ and PO43−, evaporating water from the solution to produce a solid mixture, decomposing the solid mixture at a temperature of below 500° C. to form a pure homogeneous Li and Fe phosphate precursor, and annealing the precursor at a temperature of less than 800° C. in a reducing atmosphere to produce the LiFePO4 powder. The obtained powders can have a particle size of less than 1 μm, and can provide superior electrochemical performance when mixed for an appropriate time with an electrically conductive powder.
摘要翻译：过渡金属的磷酸盐的制造和使用方法被描述为二次锂电池的正电极，包括用于制备具有受控尺寸和形态的LiMPO 4的方法，M是Fe x x 其中0 <= x <= 1,0 <= y <= 1，0

7. 发明申请

US20090111024A1 Lithium transition-metal phosphate powder for rechargeable batteries 有权
标题翻译：用于充电电池的锂过渡金属磷酸盐粉末
公开(公告)号：US20090111024A1
公开(公告)日：2009-04-30
申请号：US11786334
申请日：2007-04-11
申请人： Calin Wurm , Mathieu Morcrette , Sylvain Gwizdala , Christian Masquelier
发明人： Calin Wurm , Mathieu Morcrette , Sylvain Gwizdala , Christian Masquelier
IPC分类号： H01M4/58 , C01B25/26 , H01B1/04 , H01M4/90
CPC分类号： H01M4/136 , C01B25/375 , C01B25/377 , C01B25/45 , H01M4/1397 , H01M4/5825 , H01M10/052
摘要： Methods of manufacture and use of phosphates of transition metals are described as positive electrodes for secondary lithium batteries, including a process for the production of LiMPO4 with controlled size and morphology, M being FexCoyNizMnw, where 0≦x≦1, 0≦y≦1, 0≦w≦1, and x+y+z+w=1. According to an exemplary embodiment, a process is described for the manufacture of LiFePO4 including the steps of providing an equimolar aqueous solution of Li1+, Fe3+ and PO43−, evaporating water from the solution to produce a solid mixture, decomposing the solid mixture at a temperature of below 500° C. to form a pure homogeneous Li and Fe phosphate precursor, and annealing the precursor at a temperature of less than 800° C. in a reducing atmosphere to produce the LiFePO4 powder. The obtained powders can have a particle size of less than 1 μm, and can provide superior electrochemical performance when mixed for an appropriate time with an electrically conductive powder.
摘要翻译：将过渡金属的磷酸盐的制造和使用方法描述为二次锂电池的正电极，包括用于制备具有受控尺寸和形态的LiMPO4的方法，M是FexCoyNizMnw，其中0≤x≤1,0< y <= 1，0 <= w <= 1，x + y + z + w = 1。根据一个示例性实施方案，描述了制备LiFePO 4的方法，其包括以下步骤：提供Li1 +，Fe3 +和PO43-的等摩尔水溶液，从溶液中蒸发水以产生固体混合物，并在一定温度下分解固体混合物在500℃以上以形成纯均匀的Li和Fe磷酸盐前体，并在还原气氛中在小于800℃的温度下退火前体以产生LiFePO 4粉末。得到的粉末的粒径可以小于1μm，并且当与导电粉末混合适当的时间时，可提供优异的电化学性能。

8. 发明授权

US07670721B2 Process for making lithium transition metal phosphate powder for battery electrode 有权
标题翻译：制备电池电极用锂过渡金属磷酸盐粉末的方法
公开(公告)号：US07670721B2
公开(公告)日：2010-03-02
申请号：US11786334
申请日：2007-04-11
申请人： Calin Wurm , Mathieu Morcrette , Sylvain Gwizdala , Christian Masquelier
发明人： Calin Wurm , Mathieu Morcrette , Sylvain Gwizdala , Christian Masquelier
IPC分类号： C01B25/00
CPC分类号： H01M4/136 , C01B25/375 , C01B25/377 , C01B25/45 , H01M4/1397 , H01M4/5825 , H01M10/052
摘要： Methods of manufacture and use of phosphates of transition metals are described as positive electrodes for secondary lithium batteries, including a process for the production of LiMPO4 with controlled size and morphology, M being FexCoyNizMnw, where 0≦x≦1, 0≦y≦1, 0≦w≦1, and x+y+z+w=1. According to an exemplary embodiment, a process is described for the manufacture of LiFePO4 including the steps of providing an equimolar aqueous solution of Li1+, Fe3+ and PO43−, evaporating water from the solution to produce a solid mixture, decomposing the solid mixture at a temperature of below 500° C. to form a pure homogeneous Li and Fe phosphate precursor, and annealing the precursor at a temperature of less than 800° C. in a reducing atmosphere to produce the LiFePO4 powder. The obtained powders can have a particle size of less than 1 μm, and can provide superior electrochemical performance when mixed for an appropriate time with an electrically conductive powder.
摘要翻译：过渡金属磷酸盐的制造和使用方法被描述为二次锂电池的正电极，包括用于制备具有受控尺寸和形态的LiMPO4的方法，M是FexCoyNizMnw，其中0＆nlE; x＆nlE; 1,0＆amp; nlE; y＆nlE; 1 ，0＆nlE; w＆nlE; 1，x + y + z + w = 1。根据一个示例性实施方案，描述了制备LiFePO 4的方法，其包括以下步骤：提供Li1 +，Fe3 +和PO43-的等摩尔水溶液，从溶液中蒸发水以产生固体混合物，并在一定温度下分解固体混合物在500℃以上以形成纯均匀的Li和Fe磷酸盐前体，并在还原气氛中在小于800℃的温度下退火前体以产生LiFePO 4粉末。得到的粉末可以具有小于1μm的粒度，并且当与导电粉末混合适当的时间时，可提供优异的电化学性能。

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