CN1042377C - 一种合成锂离子电池中正极材料的方法 - Google Patents

一种合成锂离子电池中正极材料的方法 Download PDF

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CN1042377C
CN1042377C CN96104965A CN96104965A CN1042377C CN 1042377 C CN1042377 C CN 1042377C CN 96104965 A CN96104965 A CN 96104965A CN 96104965 A CN96104965 A CN 96104965A CN 1042377 C CN1042377 C CN 1042377C
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严宏伟
陈立泉
黄学杰
薛荣坚
黄宏
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Abstract

本发明属于高能电池技术领域，特别是合成锂离子电池用的正极材料的技术领域。本发明的目的为了节约能源和提高劳动生产率，和减少制备过程中锂盐的挥发，使配方得以准确控制，从而提供一种将锂和过渡金属Co、Ni、Mn、Cr的氢氧化物或氧化物或它们的盐按Li0.5-1M1-yMy′O2称料混合，放入保温容器内，置微波炉中用微波频率在0.3-300GHz下，加热600-900℃，保温1-60分钟合成。该方法简单，防止锂盐挥发，重复性好。

Description

一种合成锂离子电池中正极材料的方法
本发明属于高能电池制备技术领域，特别是合成锂离子电池中正极材料的技术领域。
用作锂离予电池正极材料的过渡金属氧化物如LiCoO2、LiNiO2、LiMn2O4，其常规合成方法是固相反应法，通常是以锂的氢氧化物或盐和含过渡金属的氢氧化物或盐为原料；在700-900℃高温下长时间煅烧、并重复数次而成，所获得的材料其电化学可逆容量在120-140mAh/g之间，如参考文献：
1.K.Mizushima,P.C.Jones,P.J.Wiseman and
  J.B.Goodenough,Mat.Res.Bull.15,783(1980).
2.M.G.S.R.Thomas,W.I.F.David,J.B.
  Goodenough and P.Groves,Mat.Res.Bull.20,
  1137(1985).
3.M.M.Thackeray,W.I.F.David,P.G.Bruce and
  J.B.Goodenough,Mat.Res.Bull.18,461(1983)所描述的：由于固相反应合成温度高、保温时间长，造成以下几个缺点；
(1)能源的巨大消耗，生产效率低；
(2)锂盐的大量挥发，通常在反应过程中需要添加过量的锂盐来以补充，而这又造成配方控制上的困难；
(3)获得的正极材料晶粒度较大，在制备锂离子电池正极膜之前，必须充分磨细；
(4)材料的均匀性差。
本发明的目的在于克服上述已有技术的缺点和不足，为了节约能源和提高劳动生产率。
本发明的目的，还在于减少制备过程中锂盐的挥发，使配方得以准确控制，生产重复性好；获得均匀微晶正极材料，允许大电流放电。从而提供一种将锂和过渡金属如Co、Ni、Mn、Cr的氢氧化物或氧化物或它们的盐类的混合物在微波炉中加热的合成方法。该方法使用频率在0.3-300GHz的微波进行合成，温度在600-900℃，保温时间1至60分钟。其正极材料循环性好，并可耐大电流充放电。
本发明的目的是这样实现的：本发明的合成热源是微波炉，使用微波频率在0.3-300GHz之间，把原料按组成配方均匀混合后，置于能被微波穿透的保温材料如莫来石泡沫保温砖或叶蜡石，耐高温玻璃等容器中，然后放入频率为2.45GHz或28GHz或60GHz单模微波炉或多模微波炉如家用微波炉中，使用微波频率在0.3-300GHz范围内，在600-900℃合成，保温时间1至60分钟，然后随炉冷却，制备出组成为LixM1-yMy＇O2其中x=0.5-1y=0-1,M=Co、Ni、Mn,M＇=Co、Ni、Mn、Cr等的锂离予电池用正极材料。
本发明使用微波频率在0.3-300GHz范围的电磁波，相应波长在1m-1mm之间，具有波长短、频率高、穿透能力强、量子特性明显等特性，作为一种新能源，可以对材料实现快速加热和快速烧结。微波加热完全不同于常规加热，它是依靠物体吸收微波能转换成热能自身升温至一定温度，热量产生于材料内部而不是来源于外部加热源，是一种体加热方式，材料吸收微波能转化为内部分子的动能和热能后，整体同时均匀加热。由于材料对微波能的吸收率与温度成正比，导致加热温度里指数形式升高，从而产生极高的加热速率。
本发明的优点在于用微波加热合成锂离子电池正极材料，可以明显降低合成温度，缩短合成时间；由于在极短的时间内完成了合成，全过程锂量的挥发可以忽略；同时晶粒生长也得以有效控制。制备的正极材料的电化学容量高，其他性能优于或不亚于常规方法合成的正极材料，尤其是可以大电流充放电。
下面结合实施例和附图对本发明进行详细说明：
实施例1：正极材料LiCoO2的合成：锂盐采用化学纯氢氧化锂，钴盐用化学纯的三氧化二钴，将两种原料按重量比1∶3.47均匀混合、压片后置于莫来石泡沫保温砖容器中；放于微波频率为2.45GHz的单模微波炉中进行合成。合成温度为800℃，保温10分钟，然后随炉冷却，整个过程共用20分钟左右。合成的LiCoO2晶粒度为1-2微米，而常规合成的LiCoO2其粒度则为10-20微米。从XRD谱图中可以发现，微波合成的LiCoO2具有很高的纯度，观察不到其它杂相的存在。其电化学可逆容量为140mAh/g，循环性能良好。
实施例2：正极材料LiNiO2的合成：锂盐采用化学纯硝酸锂，镍盐采用分析纯氢氧化镍，将两种原料按重量比1∶0.75均匀混合，合成方法同上，合成温度为700℃，保温10分钟，然后随炉冷却。合成的LiNiO2晶粒度为1-2微米。其电化学可逆容量为1500mAh/g，循环性能良好。
实施例3：正极材料Li0.9NiO2的合成：将同上原料按重量比1∶0.83均匀混合、压片后在同上条件下进行合成。合成温度为700℃，保温10分钟。其电化学可逆容量为120mAh/g，循环性能良好。
实施例4：正极材料LiNi0.91Co0.09O2的合成：锂盐采用化学纯氢氧化锂，镍盐采用化学纯三氧化二镍，钴盐用化学纯三氧化二钴，将三种原料按重量比1∶3.14∶0.31均匀混合、压片后置于莫来石泡沫保温砖容器中，放于微波频率为2.45GHz的单模微波炉中进行合成。合成温度为700℃，保温10分钟，然后随炉冷却。产物为单相，其电化学可逆容量为150mAh/g，循环性能良好。
实施例5：正极材料LiMn2O4的合成：用化学纯氢氧化锂和化学纯二氧化锰为原料，按重量比1∶7.26均匀混合、压片后置于莫来石泡沫保温砖容器中，放于28GHz单模家用微波炉中，用高加热档加热20分钟，然后随炉冷却。所得的LiMn2O4晶粒均匀，为1-2微米，相纯度高，其电化学可逆容量为130mAh/g，循环性能良好。
实施例6：正极材料LiCr0.4Mn1.6O4的合成：用化学纯氢氧化锂，化学纯三氧化二铬和化学纯二氧化锰为原料，按重量比1∶1.27∶5.81均匀混合、压片后置于莫来石泡沫保温砖容器中，放于60GHz单模家用微波炉中，用高加热档加热20分钟，然后随炉冷却。产物的电化学可逆容量为100mAh/g。

Claims (2)

1．一种合成锂离子电池中正极材料的方法，其特征在于：用锂和过渡金属Co、Ni、Mn、Cr的氢氧化物或氧化物或它们的盐按比例混合均匀，其原料混合比例按LixM1-yM’yO2称料，
其中x=0.5-1；
    y=0-1；
M为Co、Ni或Mn；
M’为Co、Ni、Mn或Cr；
将混合均匀的原料放入能被微波穿透的保温材料容器内，置于微波炉中，微波炉使用频率为2.45GHz-60GHz，加热温度在600-900℃范围内，保温1-60分钟，然后随炉温冷却后取出。
2．按权力要求1所述的合成锂离子电池中正极材料的方法，其特征在于：所述的能被微波穿透的保温材料包括莫来石泡沫保温砖、叶蜡石、玻璃。
CN96104965A 1996-05-10 1996-05-10 一种合成锂离子电池中正极材料的方法 Expired - Fee Related CN1042377C (zh)

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JP9540354A JPH11511290A (ja) 1996-05-10 1997-05-04 マイクロ波エネルギーを用いたリチウム二次電池用陽極材料の調製方法
EP97920486A EP0913876A4 (en) 1996-05-10 1997-05-04 PROCESS FOR THE PREPARATION OF POSITIVE MATERIALS FOR LITHIUM SECONDARY BATTERIES USING MICROWAVE ENERGY
PCT/CN1997/000039 WO1997043794A1 (fr) 1996-05-10 1997-05-04 Procede de preparation de materiaux positifs pour piles secondaires au lithium au moyen d'energie micro-ondes
DE0913876T DE913876T1 (de) 1996-05-10 1997-05-04 Verfahren zur herstellung von positivmaterial für lithiumsekundärzelle mittels mikrowellenenergie

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CN1324731C (zh) * 2003-07-15 2007-07-04 新乡无氧铜材总厂 一种锂离子电池用锂锰氧化物正极材料的制备工艺
CN106573795A (zh) * 2014-07-03 2017-04-19 科学与工业研究理事会 层状锂‑锰‑镍‑钴氧化物材料的制备

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JP4678452B2 (ja) * 2000-05-15 2011-04-27 株式会社豊田中央研究所 リチウム二次電池正極活物質用リチウムマンガン複合酸化物の製造方法
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