CN108269980B - 一种制备高性能三氧化二铁/铁酸锌复合电极材料的方法 - Google Patents
一种制备高性能三氧化二铁/铁酸锌复合电极材料的方法 Download PDFInfo
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Abstract
本发明公开了一种制备高性能三氧化二铁/铁酸锌复合电极材料的方法。（1）分别以六水合硝酸锌和六水合氯化铁为锌源和铁源，以蔗糖为助剂，用去离子水溶解得到原料液；（2）在空气气氛下焙烧原料液，得到三氧化二铁/铁酸锌（Fe2O3/ZnFe2O4）复合电极材料。本发明方法十分简单、成本低、产率高、制备条件易于控制，制备的Fe2O3/ZnFe2O4复合材料作为锂离子电池负极材料具有高的储锂性能。
Description
技术领域
本发明涉及锂离子电池负极材料的技术领域，具体涉及一种高性能三氧化二铁/铁酸锌 (Fe2O3/ZnFe2O4)复合电极材料的制备方法。
技术背景
铁基尖晶石型双过渡金属氧化物ZnFe2O4由于具有嵌锂容量高(其理论比容量为1072 mAhg-1，传统石墨负极仅为372mAhg-1)，安全性好、环境友好、原料来源广泛、价格低廉等突出优点而被认为是非常具有应用前景的新一代锂离子电池负极材料之一。但是，ZnFe2O4作为锂离子电池负极材料在充放电过程中会发生明显的体积变化导致颗粒粉化，从而使其循环稳定性和倍率性能变差。Fe2O3/ZnFe2O4复合电极材料包含两个不同相，由于两相的协同效应，在充放电过程中能够缓解由于体积变化产生的内应力，从而提高ZnFe2O4电极材料嵌脱锂性能。ZnFe2O4基电极材料的制备方法有：水热法、聚合物裂解法、尿素燃烧法、均相沉淀法等。但大多数制备方法步骤多、条件要求苛刻。为此，本发明提出一种十分简单的制备高性能Fe2O3/ZnFe2O4复合电极材料的方法。
发明内容
本发明的目的在于提供一种制备高性能三氧化二铁/铁酸锌(Fe2O3/ZnFe2O4)复合电极材料的方法。
具体步骤为：
(1)将锌铁摩尔比为1:2的二价锌盐和三价铁盐混合。
(2)按蔗糖与三价铁盐的质量比为1:1的比例向步骤(1)的混合物中加入蔗糖，再向其中加入三价铁盐，步骤(2)加入的三价铁盐与步骤(1)加入的三价铁盐的摩尔比为1:32～1:2，然后加入去离子水使其全部溶解。
(3)将步骤(2)所得的混合溶液置于马弗炉中在空气气氛下，在600℃条件下烧结3小时，得到Fe2O3/ZnFe2O4复合电极材料。
所述二价锌盐为Zn(NO3)2·6H2O。
所述三价铁盐为FeCl3·6H2O。
本发明采用蔗糖辅助直接烧结法制备高性能Fe2O3/ZnFe2O4复合电极材料，方法十分简单、成本低、产率高、制备条件易于控制。
附图说明
图1为实施例1～3所得的铁酸锌电极材料的XRD图谱。
具体实施方式
下面结合具体实施例对本发明作进一步的说明，需要指出的是以下实施例是为了本领域的技术人员更好地理解本发明，而不是对本发明保护范围的限制，该领域的技术人员可以根据上述内容做出一些非本质的改进和调整。
实施例1：
(1)将1.1000g Zn(NO3)2·6H2O和2.0000g FeCl3·6H2O混合。
(2)向步骤(1)的混合物中加入2.0000g蔗糖，再向其中加入0.0625g FeCl3·6H2O(步骤(2) 加入的FeCl3·6H2O与步骤(1)加入的FeCl3·6H2O的摩尔比为1:32)，然后加入5mL去离子水使其全部溶解。
(3)将步骤(2)所得的混合溶液置于马弗炉中在空气气氛下，在600℃条件下烧结3小时，得到Fe2O3/ZnFe2O4复合电极材料。
实施例2：
(1)将1.1000g Zn(NO3)2·6H2O和2.0000g FeCl3·6H2O混合。
(2)向步骤(1)的混合物中加入2.0000g蔗糖，再向其中加入0.2500g FeCl3·6H2O(步骤(2) 加入的FeCl3·6H2O与步骤(1)加入的FeCl3·6H2O的摩尔比为1:8)，然后加入5mL去离子水使其全部溶解。
(3)将步骤(2)所得的混合溶液置于马弗炉中在空气气氛下，在600℃条件下烧结3小时，得到Fe2O3/ZnFe2O4复合电极材料。
实施例3：
(1)将1.1000g Zn(NO3)2·6H2O和2.0000g FeCl3·6H2O混合。
(2)向步骤(1)的混合物中加入2.0000g蔗糖，再向其中加入1.0000g FeCl3·6H2O(步骤(2) 加入的FeCl3·6H2O与步骤(1)加入的FeCl3·6H2O的摩尔比为1:2)，然后加入5mL去离子水使其全部溶解。
(3)将步骤(2)所得的混合溶液置于马弗炉中在空气气氛下，在600℃条件下烧结3小时，得到Fe2O3/ZnFe2O4复合电极材料。
电化学性能测试：分别将实施例中制备的Fe2O3/ZnFe2O4作为活性材料，导电炭黑(Super P)作为导电剂，聚偏氟乙烯(PVDF)作为粘结剂按质量比6:3:1的比例混合研磨均匀后，加入适量的N-甲基-2-吡咯烷酮(NMP)，调匀成浆后均匀涂覆在铜箔上，在80℃下干燥至恒重，冲裁后得到电极片。以铁酸锌电极片为工作电极，金属锂片为对电极，聚丙烯多孔膜(Celgard 2400)为隔膜，1mol/L LiPF6的碳酸乙烯酯(EC)、碳酸二甲酯(DMC)和碳酸二乙酯(DEC)的混合液(m(EC):m(DMC):m(DEC)＝1:1:1)为电解液，在充满氩气的手套箱中组装成CR2016型扣式电池。采用深圳新威公司的BTS-5V/10mA型充放电测试仪测试电池的恒流充放电及倍率性能，充放电电压范围为0.01～3.0V，其中倍率性能测试的电流密度分别为1、3、5、7和10A/g，循环性能测试的电流密度为1A/g，充放电循环500圈，具体测试结果列于表1中。
表1：实施例样品的性能测试结果
如图1所示，为实施例1～3制备的电极材料的XRD图谱。从图中可以看出，本发明制备的电极材料为Fe2O3/ZnFe2O4复合电极材料。
Claims (1)
1.一种制备高性能Fe2O3/ZnFe2O4复合电极材料的方法，其特征在于具体步骤为：
(1) 将锌铁摩尔比为1:2的二价锌盐和三价铁盐混合；
(2) 按蔗糖与三价铁盐的质量比为1:1的比例向步骤(1)的混合物中加入蔗糖，再向其中加入一定量的三价铁盐，步骤(2)加入的三价铁盐与步骤（1）加入的三价铁盐的摩尔比为1:32~1:2，然后加入去离子水使其全部溶解；
(3) 将步骤(2)所得的混合溶液置于马弗炉中在空气气氛下，在600 ℃条件下烧结3小时，得到Fe2O3/ZnFe2O4复合电极材料；
所述二价锌盐为Zn(NO3)2·6H2O；
所述三价铁盐为FeCl3·6H2O。
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