CN115084471A - 层状卤化物双钙钛矿锂离子电池负极材料及其制备方法 - Google Patents
层状卤化物双钙钛矿锂离子电池负极材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种层状卤化物双钙钛矿锂离子电池负极材料,属于锂离子电池领域,其原料组成物及摩尔百分比为CsCl21.05~57.14%、MnCl25.26~75%、BiCl310.53~28.57%、LiCl 0~63.16%;本发明负极材料通过简单的研磨法即能制得,本发明制得的锂离子电池负极材料,经测试有着较高的容量和较为优异的循环稳定性,适于工业化生产制备和商业化推广应用。
Description
技术领域
本发明涉及一种层状卤化物双钙钛矿锂离子电池负极材料及其制备方法,属于锂离子电池领域。
技术背景
近些年由于便携式电子设备如手机、摄像机和手提电脑的普及以及电动汽车等新兴领域的飞速发展,锂离子电池市场扩展迅速,锂离子电池的技术水平也在不断提高。目前已有的锂离子电池负极材料可分为两大类,一类是碳基负极材料如天然石墨、人造石墨和改性石墨等;另一类是非碳基负极材料如硅、金属合金以及各种金属氧化物等。但都有些各自的弊端,碳基负极材料会由于锂离子的嵌入和脱嵌导致石墨的体积发生变化,循环稳定性降低。而非碳基负极材料中的硅电极主要面临的问题就是体积的巨大变化,导致容量的快速损失和库伦效率的下降;而对于合金以及金属氧化物来说,在合金脱合金的过程中体积变化很大,使得活性物质粉碎和聚集,电子传导性较差。
为了使现在的锂离子电池跟得上需求的脚步,扩大锂离子电池负极材料库,所以寻找新型稳定可靠的锂离子电池负极材料显得更加重要。
发明内容
针对锂离子电池负极材料体系单一,本发明提供了一种层状卤化物双钙钛矿锂离子电池负极材料,本发明通过掺杂不同的锂离子浓度,采用了极为简单的研磨法制备了一种比容量高且循环稳定性强的层状卤化物双钙钛矿锂离子电池负极材料。
本发明高循环稳定性锂离子电池负极材料的组成物及摩尔百分比为CsCl21.05~57.14%、MnCl2 5.26~14.29% 、BiCl3 10.53~28.57%、LiCl 0~63.16%。
上述高循环稳定性锂离子电池负极材料的制备是将原材料混合,置于玛瑙研钵中干磨或加入水磨20~100min,混合物在40~120℃下烘干,取出研磨1~5min,即得层状卤化物双钙钛矿锂离子电池负极材料。
本发明的有益效果是:
相比于传统的锂离子电池负极材料,本发明层状卤化物双钙钛矿锂离子电池负极材料,拓宽了现有的锂离子电池负极材料体系,锂离子可以进入层状双钙钛矿晶格间隙而不破坏其晶格结构,并且锂离子可以在层状卤化物双钙钛矿中的层间快速迁移,大大提高了锂离子的迁移速率,倍率充放电性能优异;并且在材料中掺杂了不同浓度的锂离子,实现了较高的比容量,且制备方法极为简单,适于工业化生产和商业化推广应用。
附图说明
图1为实施例1用研磨法制备的负极材料的XRD图谱;
图2为实施例1用研磨法制备的负极材料的电镜图;
图3为实施例1用沉淀制备的负极材料的XRD图谱;
图4为实施例1研磨法制备的负极材料在电流密度为75mAh g-1时的循环比容量和库伦效率图;
图5为实施例1研磨法制备的负极材料在电流密度为150mAh g-1时的循环比容量和库伦效率图;
图6为实施例1沉淀法制备的负极材料在电流密度为75mAh g-1时的循环比容量和库伦效率图;
图7为实施例2制备的负极材料在电流密度为75mAh g-1时的循环比容量和库伦效率图;
图8为实施例3制备的负极材料在电流密度为75mAh g-1时的循环比容量和库伦效率图;
图9为实施例4制备的负极材料在电流密度为75mAh g-1时的循环比容量和库伦效率图;
图10为实施例5用研磨法制备的负极材料的XRD图谱;
图11为实施例5制备的负极材料在电流密度为75mAh g-1时的循环比容量和库伦效率图。
具体实施方式
下面将结合实例进一步阐释本发明的内容,但这些实例并不限制本发明的保护范围。
实施例1:本层状卤化物双钙钛矿锂离子电池负极材料的组成物及摩尔百分比为CsCl57.14%、MnCl214.29%、BiCl328.57%;
将上述原材料混合,并置于玛瑙研钵中干磨30min,所得浆料在60℃下烘干60min,待烘干后取出研磨2min,即得层状卤化物双钙钛矿锂离子电池负极材料,其XRD图谱如图1,与标准卡片对比可以看出是纯相。图2为研磨法制备的负极材料电镜形貌图,从图中可以看出负极材料是由片层状堆积形成的,为层状材料。
同时采用共沉淀法制备负极材料:将原材料MnCl2、BiCl3装入玻璃瓶或烧杯等容器中,将原材料CsCl装入另一个玻璃瓶或烧杯等容器中,在2个容器中分别注入10mL浓盐酸,搅拌或使用超声处理使其充分溶解,将两个容器中的溶液混和生成沉淀物,沉淀物使用丙酮溶液清洗4次后在80℃下烘干,即得卤化物双钙钛矿锂离子电池负极材料,其XRD图谱如图3;
以N-甲基-2-吡咯烷酮(NMP)为溶剂,将上述制得的负极材料、导电炭黑(Super-P)和聚偏二氟乙烯(PVDP,Sigma-Aldrich)按重量比8:1:1的比例混合,然后放进球磨罐中混合1h,得到均匀的浆料;用刮刀将浆料涂布在铜箔上,在80℃真空干燥12h;切割成直径16mm的电极片,用作结构研究和电化学分析的工作电极。
采用2032型纽扣电池,以锂金属箔作为对电极和参比电极,聚丙烯微孔(celgard2320)作为隔膜;1mol/L六氟磷酸锂(LiPF6)溶液为电解液[溶剂为体积比1:1:1的EC(碳酸乙烯酯)、EMC(碳酸甲乙酯)、DMC(碳酸二甲酯)的混合物],在充满Ar2的手套箱中进行电池的组装,得到用以电性能测试的电池。
通过对电池(研磨法制备的负极材料)的电性能测试,发现在循环30次后趋于稳定,电池稳定后其库伦效率接近98%,当电流密度为75mAh g-1时,其首次放电比容为396mAhg-1,循环65次后,比容量为174 mAh g-1,如图4;当电流密度为150mAh g-1时,其首次放电比容为318mAh g-1,循环140次后,比容量为179mAh g-1,如图5;
沉淀法制备的负极材料按上述方法制成电池,对电池的电性能测试,结果见图6,当电流密度为75mAh g-1时,其首次放电比容为118 mAh g-1,循环100次后,比容量为69mAhg-1,效果明显低于研磨法制备的负极材料。
实施例2:本新型层状卤化物双钙钛矿锂离子电池负极材料的组成物及摩尔百分比为:CsCl44.44%、MnCl211.12%、BiCl322.22%、LiCl22.22%。
将精确称量过的原材料混合,并置于玛瑙研钵中干磨30min,所得浆料在60℃下烘干120min后取出研磨1min,即得层状卤化物双钙钛矿锂离子电池负极材料;
本实施例中电池的制备方法同实施例1;
通过对电池的电性能测试,当电流密度为75mAh g-1时,其首次放电比容为878mAhg-1,且循环40次后循环比容量依旧为192mAhg-1,其库伦效率接近98%,如图7。
实施例3:本层状卤化物双钙钛矿锂离子电池负极材料的组成物及摩尔百分比为:CsCl36.36%、MnCl29.10%、BiCl318.18%、LiCl36.36%;
将精确称量过的原材料混合,并置于玛瑙研钵中干磨60min,所得浆料在80℃下烘干120min后取出研磨2min,即得新型层状卤化物双钙钛矿锂离子电池负极材料。
本实施例中电池的制备方法同实施例1;
通过对电池的电性能测试,电池其库伦效率接近98%,当电流密度为75mAh g-1时,首次放电比容为681mAh g-1,且经40次循环后,循环比容量维持在211mAhg-1,有着较高的容量,如图8。
实施例4:本层状卤化物双钙钛矿锂离子电池负极材料的组成物及摩尔百分比为:CsCl26.67%、MnCl26.67%、BiCl313.33%、LiCl53.33%;
将精确称量过的原材料混合,并置于玛瑙研钵中干磨60min,所得浆料在80℃下烘干120min后取出研磨2min,即得层状卤化物双钙钛矿锂离子电池负极材料。
本实施例中电池的制备方法同实施例1;
通过对电池的电性能测试,当电流密度为75mAh g-1时,其首次放电比容为917mAhg-1,循环30次后容量为269mAhg-1,如图9。
实施例5:本新型层状卤化物双钙钛矿锂离子电池负极材料的组成物及摩尔百分比:CsCl21.05%、MnCl25.26%、BiCl310.53%、LiCl63.16%;
将精确称量过的原材料混合,并置于玛瑙研钵中干磨80min,所得浆料在110℃下烘干50min后取出研磨2min,即得层状卤化物双钙钛矿锂离子电池负极材料,样品的XRD图谱如图10;
本实施例中电池的制备方法同实施例1;
通过对电池的电性能测试,当电流密度为75mAh g-1时,其首次放电比容为1394mAhg-1,循环50次后的容量为137mAhg-1,其效率待稳定后一直接近98%,保持着较好的电化学性能,如图11,且在掺杂较多锂离子的情况下,XRD图谱并未发生明显的变化,说明材料拥有者较好的容忍度。
Claims (2)
1.一种层状卤化物双钙钛矿锂离子电池负极材料,其特征在于:原料组成物及摩尔百分比为CsCl21.05~57.14%、MnCl25.26~14.29%、BiCl310.53~28.57%、LiCl 0~63.16%。
2.权利要求1所述的层状卤化物双钙钛矿锂离子电池负极材料的制备方法,其特征在于:将原料组成物混合,置于玛瑙研钵中干磨或加入水磨20~100min,混合物在40~120℃下烘干,取出研磨1~5min,即得层状卤化物双钙钛矿锂离子电池负极材料。
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