CN115626659B - 一种三维网状二硫化锡复合硫氮掺杂石墨烯的制备及其在锂离子电池的应用 - Google Patents
一种三维网状二硫化锡复合硫氮掺杂石墨烯的制备及其在锂离子电池的应用 Download PDFInfo
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Abstract
本发明涉及一种三维网状二硫化锡复合硫氮掺杂石墨烯的制备及其在锂离子电池的应用。以二水合氯化亚锡、L‑半胱氨酸、乙醇酸、氧化石墨烯为原料，制备三维网状二硫化锡复合硫氮掺杂石墨烯S‑SnS2/NSG。所制备的三维网状二硫化锡复合硫氮掺杂石墨烯化合物电池负极材料具有高的比容量和循环稳定性，在电流密度5 A/g时充放电1000圈，容量稳定在790 mAh/g。该方法工艺简单，电池倍率性能、循环性能较好，有良好的发展前景。
Description
技术领域
本发明属于电化学领域，具体涉及一种三维网状二硫化锡复合硫氮掺杂石墨烯的制备及其在锂离子电池的应用。
背景技术
90年代初，Sony公司首先发现研制出以碳材料为负极，以LiCoO2作正极的锂电池。该电池在充放电过程中，没有金属锂的存在，只有锂离子，又称为锂离子电池。但是要得到循环性能好，比容量高，大电流充放电性能好的锂离子电池负极材料一直以来是科学家的研究重点。根据与锂离子不同的反应类型，可将负极材料分为嵌入型，合金型，转化型等，而目前使用的商业化石墨负极材料就属于嵌入型，在充放电过程中，锂离子在石墨的晶格嵌入和脱出，但其理论容量仅为372 mA h/g，同时它还存在倍率性能差，循环寿命短，存在安全隐患等问题。金属硫化物和石墨同属二维材料，其在充放电过程中不仅发生脱嵌锂反应，同时它还与锂离子发生转换反应，大大提高了其理论容量。不同于大部分半导体过渡金属硫化物，二硫化锡作为二维材料的一员，它具有良好的导电性，更有利于电化学反应过程中电荷的传输。基于此，本发明提供一种三维网状二硫化锡复合硫氮掺杂石墨烯的制备及其在锂离子电池的应用。目前还未有制备三维网状二硫化锡复合硫氮掺杂石墨烯化合物的相关专利报道。
发明内容
本发明的目的在于提供一种三维网状二硫化锡复合硫氮掺杂石墨烯的制备及其在锂离子电池的应用。
为实现上述目的，本发明采用如下技术方案：
制备方法：将0.225 克二水合氯化亚锡，0.4克L-半胱氨酸，0.6克乙醇酸，4毫升氧化石墨烯分散液（10毫克每毫升）加入到16毫升去离子水和10毫升乙醇中，搅拌均匀后，移入50mL的反应釜中，置于200度的烘箱中，反应18小时。将所得产物用无水乙醇与去离子水洗涤离心三遍以上，再用真空烘箱烘干80℃得到S-SnS2/NSG。
锂电池组装：按质量比S-SnS2/NSG ：乙炔黑：聚丙烯酸＝7：2：1混合研磨后均匀地涂在铜箔上做负极，参比电极和对电极均为金属锂，电解质由1M LiPF6的EC+DEC (EC/DEC=1/1 v/v)，添加体积百分数分别为10%和1%的FEC和VC的溶液。所有组装均在手套箱里进行。
本发明的优点在于：
（1）本发明提供了一种三维网状二硫化锡复合硫氮掺杂石墨烯化合物的制备方法，该方法工艺简单，成本廉价，重现性好，性能优异。
（2）一种三维网状二硫化锡复合硫氮掺杂石墨烯的S-SnS2/NSG，由于在水热过程中引入乙醇酸，乙醇酸的加入可以抑制石墨烯之间的键合进而使石墨烯卷曲成三维管状结构，从而使得此材料具有独特的疏松三维结构，此结构可以促进锂离子与电子的扩散，同时乙醇酸酸性的存在使得二硫化锡可以产生硫空位，极大的提高材料的电化学性能。并且，乙醇酸的加入不仅促进了二硫化锡与石墨烯的键合，还因为抑制了前驱体（二水合氯化亚锡）的水解从而使得二硫化锡呈现出很小的纳米片状。对比样SnS2/NSG由于没有加入乙醇酸就是简单石墨烯和球状二硫化锡的复合，呈现不了卷曲石墨烯的形貌，对比样SnS2/NSG中的石墨烯呈现出堆叠形貌（图2），主样S-SnS2/NSG中因为二硫化锡尺寸很小，所以呈现的是石墨烯的形貌，而且乙醇酸的键合可以使得石墨烯卷曲，没有加乙醇酸就是二硫化锡呈现球状，球状二硫化锡与片状石墨烯的杂乱堆叠。
（3）将S-SnS2/NSG用作锂电池负极，得到的锂电池具有很高的比容量和循环稳定性，在电流密度为5 A/g时充放电循环1000圈容量稳定在790 mA h/g。
附图说明
图1中a是S-SnS2/NSG材料的XRD、b是S-SnS2/NSG材料的扫描电镜、c是SnS2/NSG材料的扫描电镜、d是S-SnS2/NSG材料的透射电镜图。可以看到S-SnS2/NSG材料呈现出卷曲石墨烯的独特三维结构，从TEM图中可以看出，材料呈现出二硫化锡紧密键合在石墨烯上，其中二硫化锡为小纳米片状；而未添加乙醇酸的材料呈现出二硫化锡纳米片插层组成的球状结构负载在堆叠的片状石墨烯上。
图2是对比例1制备的SnS2/NSG材料的扫描电镜。可以看出，未添加乙醇酸，石墨烯呈现出片状堆叠形貌。
图3是S-SnS2/NSG和SnS2/NSG材料的循环性能以及倍率性能图。可以看到S-SnS2/NSG材料的循环性能与倍率性能都很优异，在0.1, 0.2, 0.5, 1, 2, 5 A g-1的电流密度下，材料的倍率性能分别为1156.5, 1108.9, 1027.2, 977.9, 908.4, 790.2 mA h g-1，在5A g-1的电流密度下，循环1000圈容量还能保持790 mA h g-1，展现出良好的循环稳定性和优异的长循环性能；而未添加乙醇酸的样品SnS2/NSG循环及倍率性能较差，在0.1, 0.2,0.5, 1, 2, 5 A g-1的电流密度下，没有添加乙醇酸的SnS2/NSG材料的倍率性能分别为1002.4, 934.7, 864.5, 757.2,655.1,580.9 mA h g-1，在5A g-1的电流密度下，循环1000圈容量仅为544 mA h g-1。
具体实施方式
为让本发明的上述特征和优点能更明显易懂，下文特举实施例，作详细说明。本发明的方法如无特殊说明，均为本领域常规方法。
实施例1三维网状二硫化锡复合硫氮掺杂石墨烯的S-SnS2/NSG的制备
将0.225 克二水合氯化亚锡，0.4克L-半胱氨酸，0.6克乙醇酸，4毫升氧化石墨烯分散液（10毫克每毫升）加入到16毫升去离子水和10毫升乙醇中，搅拌均匀后，移入50mL的反应釜中，置于200℃的烘箱中，反应18小时。将所得产物用无水乙醇与去离子水洗涤离心三遍，再用真空烘箱烘干80℃得到S-SnS2/NSG。其中，氮含量约为3.2wt%，硫含量约为4.5wt%，二硫化锡含量约为73.8 wt%
对比例1二硫化锡复合硫氮掺杂石墨烯的SnS2/NSG的制备
将0.225 克二水合氯化亚锡，0.4克L-半胱氨酸，4毫升氧化石墨烯分散液（10毫克每毫升）加入到16毫升去离子水和10毫升乙醇中，搅拌均匀后，移入50mL的反应釜中，置于200℃的烘箱中，反应18小时。将所得产物用无水乙醇与去离子水洗涤离心三遍，再用真空烘箱烘干80℃得到SnS2/NSG。
应用例
锂电池组装：按质量比S-SnS2/NSG （或SnS2/NSG）：乙炔黑：聚丙烯酸＝7：2：1混合研磨后均匀地涂在铜箔上做负极，参比电极和对电极均为金属锂，电解质由1M LiPF6的EC+DEC (EC/DEC =1/1 v/v)，添加体积百分数分别为10%和1%的FEC和VC的溶液。所有组装均在手套箱里进行。
以上所述仅为本发明的较佳实施例，凡依本发明申请专利范围所做的均等变化与修饰，皆应属本发明的涵盖范围。
Claims (3)
1.一种三维网状二硫化锡复合硫氮掺杂石墨烯的制备方法，其特征在于，包括以下步骤：
（1）将二水合氯化亚锡，L-半胱氨酸，乙醇酸，氧化石墨烯分散液加入到去离子水和乙醇中，搅拌均匀后，移入反应釜中，置于200℃的烘箱中，反应18小时；
（2）将所得产物用无水乙醇与去离子水洗涤离心三遍以上，再用真空烘箱烘干，得到三维网状二硫化锡复合硫氮掺杂石墨烯S-SnS2/NSG；
二水合氯化亚锡的用量为0.225 g，L-半胱氨酸的用量为0.4g，乙醇酸的用量为0.6g，氧化石墨烯分散液的用量为4ml，氧化石墨烯的浓度为10mg/ml；
步骤（1）中去离子水的用量为16m，乙醇的用量为10ml。
2.根据权利要求1所述的制备方法制得的三维网状二硫化锡复合硫氮掺杂石墨烯S-SnS2/NSG。
3.根据权利要求2所述的三维网状二硫化锡复合硫氮掺杂石墨烯S-SnS2/NSG在锂电池中的应用，其特征在于，所述的三维网状二硫化锡复合硫氮掺杂石墨烯S-SnS2/NSG用于制备锂电池负极，具体锂电池的组装为：按质量比S-SnS2/NSG ：乙炔黑：聚丙烯酸＝7：2：1混合研磨后均匀地涂在铜箔上做负极，参比电极和对电极均为金属锂，电解质由1M LiPF6的EC+DEC、添加体积百分数分别为10%和1%的FEC和VC的溶液，所有组装均在手套箱里进行。
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