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    Crystalline nanometric LiFePO4
    1.
    发明授权
    Crystalline nanometric LiFePO4 有权

    公开(公告)号：US09954227B2

    公开(公告)日：2018-04-24

    申请号：US11993925

    申请日：2006-06-15

    申请人： Charles Delacourt ,  Philippe Poizot ,  Christian Masquelier

    发明人： Charles Delacourt ,  Philippe Poizot ,  Christian Masquelier

    IPC分类号： C01B25/45 ,  H01M4/58 ,  C01B25/37 ,  H01M10/052 ,  H01M10/0565

    CPC分类号： H01M4/5825 ,  C01B25/37 ,  H01M10/052 ,  H01M10/0565 ,  Y10T428/2982

    摘要： The present invention relates to lithium secondary batteries and more specifically to positive electrode materials operating at potentials greater than 2.8 V vs. Li+/Li in nonaqueous electrochemical cells. In particular, the invention relates to crystalline nanometric carbon-free olivine-type LiFePO4 powders with enhanced electrochemical properties. A direct precipitation process is described for preparing crystalline LiFePO4powder, comprising the steps of: —providing a water-based mixture having at a pH between 6 and 10, containing a water-miscible boiling point elevation additive, and Li(I), Fe(II) and P(V) as precursor components; —heating said water-based mixture to a temperature less than or equal to its boiling point at atmospheric pressure, thereby precipitating crystalline LiFePO4 powder. An extremely fine 50 to 200 nm particle size is obtained, with a narrow distribution. The fine particle size accounts for excellent high-drain properties without applying any carbon coating. This allows for a significant increase in the active material content of the electrode. The narrow distribution facilitates the electrode manufacturing process and ensures a homogeneous current distribution within the battery.

    Room temperature single phase Li insertion/extraction material for use in Li-based battery
    3.
    发明授权
    Room temperature single phase Li insertion/extraction material for use in Li-based battery 有权
    室温单相Li插入/提取材料用于锂基电池

    公开(公告)号：US08641921B2

    公开(公告)日：2014-02-04

    申请号：US12530846

    申请日：2008-03-19

    申请人： Pierre Gibot ,  Christian Masquelier ,  Jean-Marie Tarascon ,  Stephane Levasseur ,  Philippe Carlach

    发明人： Pierre Gibot ,  Christian Masquelier ,  Jean-Marie Tarascon ,  Stephane Levasseur ,  Philippe Carlach

    IPC分类号： H01M4/88 ,  H01M4/02 ,  H01M4/00 ,  B32B15/02

    CPC分类号： H01M4/136 ,  C01B25/45 ,  H01M4/5825 ,  H01M10/0525 ,  H01M2004/021 ,  H01M2004/028 ,  Y10T428/2982

    摘要： The invention relates to active materials for the manufacture of Li-based batteries. A crystalline nanometric powdered material with formula Lix(M, M′)PO4, in particular LixFePO4 (O≦x≦1), is disclosed, exhibiting single phase Li insertion/extraction mechanism at room temperature when used as positive electrode material in Li-based batteries. Compared to current LiFePO4, the novel material results in smooth, sloping charge/discharge voltage curve greatly simplifying the monitoring of the state of charge of the batteries. The coexistence of mixed valence states for Fe (i.e. FeIIIVFeII) is believed to increase the electronic conductivity in the room temperature single phase LixFePO4 material, compared to state of the art two-phase materials. This, together with the nanometric size of the particles and their sharp monomodal size distribution, contributes to the exceptional high-rate capability demonstrated in batteries.

    摘要翻译： 本发明涉及用于制造锂基电池的活性材料。 公开了具有式Lix（M，M'）PO 4，特别是LixFePO 4（O @ x @）的结晶纳米粉末材料，当用作锂 - 正电极材料中的正极材料时，在室温下呈现单相Li插入/萃取机理， 基于电池。 与目前的LiFePO4相比，新型材料产生平滑，倾斜的充放电电压曲线，大大简化了电池充电状态监测。 与现有技术的两相材料相比，Fe（即FeIIIVFeII）的混合价态的共存被认为增加室温单相LixFePO 4材料中的电子传导性。 这与颗粒的纳米尺寸及其尖峰单峰尺寸分布一起，有助于在电池中展现出卓越的高速率能力。

    Carbon-Coated Li-Containing Powders and Process for Production Thereof
    9.
    发明申请
    Carbon-Coated Li-Containing Powders and Process for Production Thereof 有权
    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。

    Lithium transition-metal phosphate powder for rechargeable batteries
    10.
    发明授权
    Lithium transition-metal phosphate powder for rechargeable batteries 有权
    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