CN111276749B - 一种射频磁控溅射法制备高性能全固态薄膜锂电池的方法 - Google Patents
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Abstract
本发明公开了一种射频磁控溅射法制备高性能全固态薄膜锂电池的方法。该方法包括以下步骤:(1)设计在不同径向尺寸上相同电池形状的掩模版;(2)在衬底基片上覆盖掩模版,在磁控溅射设备上装样,安装靶材;(3)射频磁控溅射法溅射正极集流体、正极、电解质、负极、负极集流体,制备薄膜电池;(4)对不同径向尺寸上获得的电池分别进行充放电性能测试;(5)分析获得径向性能最优的区域。采用本发明的方法通过对不同径向尺寸上获得的薄膜电池进行性能分析,可以获得具有最佳性能的径向区域。
Description
技术领域
本发明涉及一种射频磁控溅射法制备高性能全固态薄膜锂电池的方法,属于锂离子电池技术领域。
背景技术
全固态薄膜锂电池具有高能量密度,低自放电率,高安全性、高循环寿命等优点,是锂离子电池研发的热点。射频磁控溅射法制备薄膜电池原理是基于在电场作用下Ar离子轰击靶材,靶材原子溅射沉积在衬底基片上。电池的形状与尺寸通常由覆盖在衬底基片上的掩模版控制。利用该方法在圆形衬底上沉积的原子层均匀性不一致,因而在不同区域镀覆得到的电池性能不同。
发明内容
本发明的目的在于提供一种射频磁控溅射法制备高性能全固态薄膜锂电池的方法,采用该方法通过对不同径向尺寸上获得的薄膜电池进行性能分析,可以获得具有最佳性能的径向区域。
为实现上述目的,本发明采用以下技术方案:
一种射频磁控溅射法制备高性能全固态薄膜锂电池的方法,该方法包括以下步骤:
(1)设计在不同径向尺寸上相同电池形状的掩模版;
(2)在衬底基片上覆盖掩模版,在磁控溅射设备上装样,安装靶材;
(3)射频磁控溅射法溅射正极集流体、正极、电解质、负极、负极集流体,制备薄膜电池;
(4)对不同径向尺寸上获得的电池分别进行充放电性能测试;
(5)分析获得径向性能最优的区域。
其中,所述掩模版的直径为52mm,其设计方式为:在半径为r=3.54mm,7.91mm,12.75mm,17.68mm,22.64mm的位置分别布局尺寸为Φ3(直径为3mm)的圆形电池。
所用衬底基片的尺寸与掩模版的尺寸相同,溅射过程中衬底基片的温度为室温。
所用靶材尺寸为3.2×60mm,铜背板尺寸为2×60mm。
所述步骤(3)中,正极集流体为Pt靶,正极靶材为LiMn2O4,电解质靶材为Li3PO4,负极靶材为Li4Ti5O12,负极集流体为Pt靶。
所述步骤(3)中,射频磁控溅射法制备薄膜电池时真空度为5×10-4,其中正极集流体、负极集流体、正极、负极镀覆过程中通入2Pa氩气,气体流量保持30sccm;电解质镀覆过程中通入2Pa氮气,气体流量保持30sccm。
所述步骤(3)中,正极集流体、正极、电解质、负极、负极集流体的溅射功率分别为70w,时长分别为20min,150min,180min,150min,20min。
本发明的优点在于:
采用本发明的方法通过对不同径向尺寸上获得的薄膜电池进行性能分析,可以获得具有最佳性能的径向区域。
本发明通过射频磁控溅射法成功优选得到了在直径为52mm的圆形衬底基片上镀覆电池的最佳性能区域,即r=4.7~19.4mm;并在r=12.75mm处得到了充电电压1.630V,可逆放电容量0.52μAh/4mm2,放电窗口1.505V的Φ3薄膜电池。
附图说明
图1为掩模版径向布局设计方式示意图。
图2为位于不同半径圆环上电池的充放电曲线。
图3为不同位置电池距中心的径向尺寸与输出电压关系拟合曲线。
图4为圆形硅片镀覆电池在不同径向区域的性能优劣示意图。
具体实施方式
以下结合附图和实施例对本发明进行进一步详细说明,但并不意味着对本发明保护范围的限制。
实施例
在直径为52mm的圆形不锈钢掩模版不同径向尺寸位置上布局Φ3的电池孔洞模型,径向尺寸位置分别为r=3.54mm,7.91mm,12.75mm,17.68mm,22.64mm,见图1。
将该掩模版覆盖在直径为52mm的圆形硅片上,在样品托上固定好后在JGP560C15型超高真空五靶磁控溅射镀膜系统上装样,同时安装靶材。
采用机械泵与分子泵两级真空泵抽真空,当样品仓内真空度达到5×10-4Pa时向仓室内通入2Pa氩气,气体流量保持30sccm。
射频磁控溅射法依次镀覆正极集流体Pt、正极LiMn2O4,电解质LiPON、负极Li4Ti5O12、负极集流体Pt,镀覆时长分别为20min,150min,180min,150min,20min。其中电解质靶材为Li3PO4,镀覆过程中需关闭氩气,改为通入2Pa氮气,气体流量同样保持在30sccm。以上各薄膜层溅射功率均为70w。
采用MACCOR MC16电池测试仪测试不同径向尺寸上电池的充放电性能。由图2的充电曲线可以看出r=7.91mm,r=12.75mm,r=17.68mm处的电池具有较好的充电平台,并在r=12.75mm处得到了充电电压1.630V,可逆放电容量0.52μAh/4mm2,放电窗口1.505V的Φ3薄膜电池。
同时由图3拟合曲线可看到各电池输出电量随径向尺寸增大先增大后减小,在r=12.75mm处存在最大值。在r为4.7~19.4mm范围内,所获得电池的输出电量均大于32nW。
由此可见,该区域镀覆得到的电池性能明显优于其它径向区域,见图4。在制备较小尺寸电池时可在该区域进行镀覆。
Claims (6)
1.一种射频磁控溅射法制备高性能全固态薄膜锂电池的方法,其特征在于,该方法包括以下步骤:
(1)设计在不同径向尺寸上相同电池形状的掩模版,所述掩模版的直径为52mm,其设计方式为:在半径为r=3.54mm,7.91mm,12.75mm,17.68mm,22.64mm的位置分别布局直径为3mm的圆形电池孔洞模型;
(2)在衬底基片上覆盖掩模版,在磁控溅射设备上装样,安装靶材;
(3)射频磁控溅射法溅射正极集流体、正极、电解质、负极、负极集流体,制备薄膜电池;
(4)对不同径向尺寸上获得的电池分别进行充放电性能测试;
(5)分析获得径向性能最优的区域。
2.根据权利要求1所述的射频磁控溅射法制备高性能全固态薄膜锂电池的方法,所用衬底基片的尺寸与掩模版的尺寸相同,溅射过程中衬底基片的温度为室温。
3.根据权利要求1所述的射频磁控溅射法制备高性能全固态薄膜锂电池的方法,所用靶材尺寸为3.2×60mm,铜背板尺寸为2×60mm。
4.根据权利要求1所述的射频磁控溅射法制备高性能全固态薄膜锂电池的方法,所述步骤(3)中,正极集流体为Pt靶,正极靶材为LiMn2O4,电解质靶材为Li3PO4,负极靶材为Li4Ti5O12,负极集流体为Pt靶。
5.根据权利要求1所述的射频磁控溅射法制备高性能全固态薄膜锂电池的方法,所述步骤(3)中,射频磁控溅射法制备薄膜电池时真空度为5×10-4,其中正极集流体、负极集流体、正极、负极镀覆过程中通入2Pa氩气,气体流量保持30sccm;电解质镀覆过程中通入2Pa氮气,气体流量保持30sccm。
6.根据权利要求1所述的射频磁控溅射法制备高性能全固态薄膜锂电池的方法,所述步骤(3)中,正极集流体、正极、电解质、负极、负极集流体的溅射功率分别为70w,时长分别为20min,150min,180min,150min,20min。
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