磷酸铁锂具有热稳定性好、充放电效率高、环境友好、价格便宜的特点,被认为是极有潜力的锂离子电池,特别是动力锂离子电池正极材料。目前,研究者们广泛采用高温固相法、液相法、共沉淀法、微波加热等方法来合成磷酸铁锂,并通过碳包覆或掺杂等方式来提高材料的电导率以发问其电化学性能。喷雾干燥法是从料液中获得超微干粉的一种较好的方法这种由液态经过雾化和干燥在瞬间直接变成粉体的过程,已经广泛应用于食品、医药、电子和材料等一些与原材料颗粒大小密切相关的领域。与其他一些粉末生产相比较,喷雾干燥法具有如下一些优点︰
1.可以保证组分分布均匀,精确控制化学计量比,适合制备多组分的复合粉末;
2.保证粉末具有较高的纯度和活性;
3.喷雾赤豆工序简单,生产过程连续,产能大,生产效率高,有利于工业化生产;
4.喷雾干燥的颗粒大都呈规则的球形,有利于提高粉末的振实密度。
二、实验用品
(一)器材
(1)喷雾干燥机。
(2)球磨机。
(二)试剂
葡萄糖
(三)材料
磷酸铁碳酸锂。
三、LiFePO4/C材料合成。
具体工艺流程如下:
1.按化学计量比称取正磷酸铁和碳酸锂,以葡萄糖为还原剂和碳添加剂,添加适量葡萄糖;
2.以去离子水为介质球磨1h,球磨转速为120r/min;将球磨后的物料进行喷雾干燥﹔
3.将喷雾干燥后所得的粉末装入瓷舟,置于高纯氮气保护的管式电炉中,于600~800度下
热处理数小时;
4.冷却至室温,所得灰黑色粉末即为LiFePO4/C材料。
四、料液浓度的影响。
颗粒粒径随着料液固含量的降低而减小,当固含量降低到20%以下时,颗粒粒径随固含量的变化比较缓慢。固含量越低,越有利于合成颗粒细小的磷酸铁锂材料,这是因为料液浓度越高,其粘度也越高,在喷雾干燥过程中形成的雾滴也变大。这使得雾化后的液滴与气体接触的面积减小,干燥后形成的颗粒粒径就变大。同时,高浓度的料液还容易导致颗粒团聚结块现象的发生,其原因在于雾滴过大,尚末干燥就被高速离心雾化器甩到干燥塔内壁,导致颗粒结块和沾壁,在固含量30%时这种现象比较明显。
五、进料速度对粒度的影响
随着进料速度的增大,颗粒粒径逐渐变大。进料速度的增大引起雾滴的变大和雾滴数量的增加,雾滴在干燥前相互碰撞发生聚合,导致成核数量的减少,产品粒径变大。
五、结果与分析
1.采用喷雾干燥-热还原法合成了磷酸铁锂材料,喷雾干燥能有效抑制组分的偏析和颗粒的长大,保证物料实现很好的混合均匀度,有利于合成更纯更细的磷酸铁锂正极材料;
⒉喷雾干燥过程对材料颗粒有较大的影响,低固含量,低进料速率有利小粒径材料的合成;
3喷雾干燥所得到的材料形状规则,颗粒细小且成球状,对改善材料的电化学性能有很大意义。
喷雾干燥机。"]]},"spaceId":"300000000$dqxcFOHabtRz","type":"text","updatedAt":1714459143895,"updatedBy":"144115210452899165","version":1}}}}},{"blockId":"kXji9HMnQz4dwAQ8bDw0FL","blockSubtree":{"block":{"kXji9HMnQz4dwAQ8bDw0FL":{"role":"editor","value":{"createdAt":1714459143896,"createdBy":"144115210452899165","enabled":true,"id":"kXji9HMnQz4dwAQ8bDw0FL","parentId":"1N2ZYyXqTmc0GXSti8n9MW","parentTable":"block","props":{"title":[["(2)球磨机。"]]},"spaceId":"300000000$dqxcFOHabtRz","type":"text","updatedAt":1714459143896,"updatedBy":"144115210452899165","version":1}}}}},{"blockId":"PvxOuCqmP40IRF8SK224mM","blockSubtree":{"block":{"PvxOuCqmP40IRF8SK224mM":{"role":"editor","value":{"createdAt":1714459143898,"createdBy":"144115210452899165","enabled":true,"id":"PvxOuCqmP40IRF8SK224mM","parentId":"1N2ZYyXqTmc0GXSti8n9MW","parentTable":"block","props":{"title":[["(二)试剂"]]},"spaceId":"300000000$dqxcFOHabtRz","type":"text","updatedAt":1714459143898,"updatedBy":"144115210452899165","version":1}}}}},{"blockId":"s0eVi3XKVoI1zsAaBrymhO","blockSubtree":{"block":{"s0eVi3XKVoI1zsAaBrymhO":{"role":"editor","value":{"createdAt":1714459143899,"createdBy":"144115210452899165","enabled":true,"id":"s0eVi3XKVoI1zsAaBrymhO","parentId":"1N2ZYyXqTmc0GXSti8n9MW","parentTable":"block","props":{"title":[["葡萄糖"]]},"spaceId":"300000000$dqxcFOHabtRz","type":"text","updatedAt":1714459143899,"updatedBy":"144115210452899165","version":1}}}}},{"blockId":"G2dYwAbJRPf8R43xSyuMkS","blockSubtree":{"block":{"G2dYwAbJRPf8R43xSyuMkS":{"role":"editor","value":{"createdAt":1714459143900,"createdBy":"144115210452899165","enabled":true,"id":"G2dYwAbJRPf8R43xSyuMkS","parentId":"1N2ZYyXqTmc0GXSti8n9MW","parentTable":"block","props":{"title":[["(三)材料"]]},"spaceId":"300000000$dqxcFOHabtRz","type":"text","updatedAt":1714459143900,"updatedBy":"144115210452899165","version":1}}}}},{"blockId":"OB2cPXMbRoOhE4TRSHMO86","blockSubtree":{"block":{"OB2cPXMbRoOhE4TRSHMO86":{"role":"editor","value":{"createdAt":1714459143901,"createdBy":"144115210452899165","enabled":true,"id":"OB2cPXMbRoOhE4TRSHMO86","parentId":"1N2ZYyXqTmc0GXSti8n9MW","parentTable":"block","props":{"title":[["磷酸铁碳酸锂。"]]},"spaceId":"300000000$dqxcFOHabtRz","type":"text","updatedAt":1714459143901,"updatedBy":"144115210452899165","version":1}}}}},{"blockId":"UTFQo4AmFNe5QNS56YSdna","blockSubtree":{"block":{"UTFQo4AmFNe5QNS56YSdna":{"role":"editor","value":{"createdAt":1714459153069,"createdBy":"144115210452899165","enabled":true,"id":"UTFQo4AmFNe5QNS56YSdna","parentId":"1N2ZYyXqTmc0GXSti8n9MW","parentTable":"block","props":{"title":[["三、LiFePO4/C材料合成。"]]},"spaceId":"300000000$dqxcFOHabtRz","type":"text","updatedAt":1714459154661,"updatedBy":"144115210452899165","version":4}}}}},{"blockId":"FZ8UxtjdtL5r3Rdv3ak5ZZ","blockSubtree":{"block":{"FZ8UxtjdtL5r3Rdv3ak5ZZ":{"role":"editor","value":{"createdAt":1714459154656,"createdBy":"144115210452899165","enabled":true,"id":"FZ8UxtjdtL5r3Rdv3ak5ZZ","parentId":"1N2ZYyXqTmc0GXSti8n9MW","parentTable":"block","props":{"title":[["具体工艺流程如下:"]]},"spaceId":"300000000$dqxcFOHabtRz","type":"text","updatedAt":1714459154656,"updatedBy":"144115210452899165","version":1}}}}},{"blockId":"BkK3xqEABQZ6qJ8GnTdA67","blockSubtree":{"block":{"BkK3xqEABQZ6qJ8GnTdA67":{"role":"editor","value":{"createdAt":1714459154657,"createdBy":"144115210452899165","enabled":true,"id":"BkK3xqEABQZ6qJ8GnTdA67","parentId":"1N2ZYyXqTmc0GXSti8n9MW","parentTable":"block","props":{"title":[["1.按化学计量比称取正磷酸铁和碳酸锂,以葡萄糖为还原剂和碳添加剂,添加适量葡萄糖;"]]},"spaceId":"300000000$dqxcFOHabtRz","type":"text","updatedAt":1714459154657,"updatedBy":"144115210452899165","version":1}}}}},{"blockId":"U5DEKfWoEwZvHj8VnmN5wR","blockSubtree":{"block":{"U5DEKfWoEwZvHj8VnmN5wR":{"role":"editor","value":{"createdAt":1714459154658,"createdBy":"144115210452899165","enabled":true,"id":"U5DEKfWoEwZvHj8VnmN5wR","parentId":"1N2ZYyXqTmc0GXSti8n9MW","parentTable":"block","props":{"title":[["2.以去离子水为介质球磨1h,球磨转速为120r/min;将球磨后的物料进行喷雾干燥﹔"]]},"spaceId":"300000000$dqxcFOHabtRz","type":"text","updatedAt":1714459154658,"updatedBy":"144115210452899165","version":1}}}}},{"blockId":"TFNUphLdK4oY1uEfaw37Rj","blockSubtree":{"block":{"TFNUphLdK4oY1uEfaw37Rj":{"role":"editor","value":{"createdAt":1714459154659,"createdBy":"144115210452899165","enabled":true,"id":"TFNUphLdK4oY1uEfaw37Rj","parentId":"1N2ZYyXqTmc0GXSti8n9MW","parentTable":"block","props":{"title":[["3.将喷雾干燥后所得的粉末装入瓷舟,置于高纯氮气保护的管式电炉中,于600~800度下"]]},"spaceId":"300000000$dqxcFOHabtRz","type":"text","updatedAt":1714459154659,"updatedBy":"144115210452899165","version":1}}}}},{"blockId":"oApoRuvZ0uSWP5ftTMpxf0","blockSubtree":{"block":{"oApoRuvZ0uSWP5ftTMpxf0":{"role":"editor","value":{"createdAt":1714459166196,"createdBy":"144115210452899165","enabled":true,"id":"oApoRuvZ0uSWP5ftTMpxf0","parentId":"1N2ZYyXqTmc0GXSti8n9MW","parentTable":"block","props":{"title":[["热处理数小时;"]]},"spaceId":"300000000$dqxcFOHabtRz","type":"text","updatedAt":1714459167869,"updatedBy":"144115210452899165","version":4}}}}},{"blockId":"yW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