CN115304377A - Lgps陶瓷片及其制备方法、lgps陶瓷片的压制模具 - Google Patents
Lgps陶瓷片及其制备方法、lgps陶瓷片的压制模具 Download PDFInfo
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Abstract
本发明涉及固态电解质的制备技术领域,具体涉及一种LGPS陶瓷片及其制备方法、LGPS陶瓷片的压制模具,本发明提供的制备方法,包括以下步骤:将Li10GeP2S12粉末进行压制成型,得到所述Li10GeP2S12陶瓷片;所述压制成型的压力为0.5~3.0GPa,保压时间为3~10min。本发明采用高压力(0.5~3.0GPa)对Li10GeP2S12粉末进行压制,可以降低晶界处的气孔数目,形成区域晶粒间接触良好的“捷径”,降低晶界势垒和迁移路径,提高离子在固相中的迁移速率,从而提高了离子电导率。
Description
技术领域
本发明涉及固态电解质的制备技术领域,具体涉及一种LGPS陶瓷片及其制备方法、LGPS陶瓷片的压制模具。
背景技术
相对于液态锂电池来说,固态锂电池具有更高的能量密度和更好的安全稳定性,被认为是下一代电池体系的重要候选者。其中,固态电解质是全固态锂电池的核心部件。根据电解质的成分区分,电解质分为聚合物固态电解质和无机固态电解质。得益于自身高的锂离子电导率,良好的稳定性,无机固态电解质成为固态电解质重要的开发目标。然而,由于无机固态电解质内部晶界阻抗大以及电极/电解质之间界面阻抗高,导致无机固态电解质实际锂离子电导率低的问题。这个缺陷制约了全固态锂电池的发展,造成了电池差的电化学性能,限制了锂离子电池能量密度的发挥。
一直以来,国内外很多研究者通过元素替换和掺杂的方式来改善离子导电通道以及填隙离子或离子空位的浓度,提高无机固态电解质自身的离子电导率。然而,无机固态电解质材料的性质很大程度上取决于晶界的密度,较大的晶界电阻势必会降低无机固态电解质的离子电导性能,因此,调控晶界的微结构是从材料形貌角度提高离子电导率的关键。目前来讲,针对无机固态电解质,往往通过高温来影响晶界。虽然高温处理能够有效减少晶界处的气孔数目,提高晶粒间的接触,但是高温处理一方面能耗较高,另一方面经常会导致样品的非晶化或玻璃化,不仅破坏了材料的晶体结构,反而使得材料的电导率降低。
发明内容
有鉴于此,本发明提供了一种LGPS(Li10GeP2S12)陶瓷片及其制备方法、LGPS(Li10GeP2S12)陶瓷片的压制模具,本发明提供的制备方法,无需经过高温过程,且制备得到的Li10GeP2S12陶瓷片具有较高的电导率。
为了实现上述发明目的,本发明提供了一种Li10GeP2S12陶瓷片的制备方法,包括以下步骤:
将Li10GeP2S12粉末进行压制成型,得到所述Li10GeP2S12陶瓷片;
所述压制成型的压力为0.5~3.0GPa,保压时间为3~10min。
优选地,所述Li10GeP2S12粉末的粒径为0.1~1μm。
本发明还提供了上述所述的制备方法制备得到的Li10GeP2S12陶瓷片,所述Li10GeP2S12陶瓷片的电导率为2.5~5.0mS·cm-1。
本发明还提供了上述所述的Li10GeP2S12陶瓷片的压制模具,包括铜板1和可拆卸的样品成型环2;
所述铜板中央设有凹槽11;所述凹槽的中心为中空腔12;
所述中空腔12用于可拆卸地设置所述样品成型环2;
所述样品成型环2的厚度与所述中空腔12的高度相同。
优选地,还包括脱模件3。
优选地,所述脱模件3包括与所述凹槽11和中空腔12匹配的凸台。
优选地,所述样品成型环2的材质为叶腊石。
本发明提供了一种Li10GeP2S12陶瓷片的制备方法,包括以下步骤:将Li10GeP2S12粉末进行压制成型,得到所述Li10GeP2S12陶瓷片;所述压制成型的压力为0.5~3.0GPa,保压时间为3~10min。本发明采用高压力(0.5~3.0GPa)对Li10GeP2S12粉末进行压制成型,可以降低晶界处的气孔数目,形成区域晶粒间接触良好的“捷径”,降低晶界势垒和迁移路径,提高离子在固相中的迁移速率,从而提高了离子电导率。
附图说明
图1为Li10GeP2S12陶瓷片的压制模具,其中1-铜板,2-样品成型环,3-脱模件,11-凹槽,12-中空腔;
图2为实施例1在1.5GPa压力下和对比例1制备而成的陶瓷片的电导率测试图;
图3为实施例1在1.5GPa压力下和对比例1制备而成的陶瓷片的电镜扫描图;
图4为实施例1在1.5GPa压力下压制后的LGPS和对比例1制备得到的陶瓷片的比容量测试图。
具体实施方式
本发明提供了一种Li10GeP2S12陶瓷片的制备方法,包括以下步骤:
将Li10GeP2S12粉末进行压制成型,得到所述Li10GeP2S12陶瓷片。
在本发明中,如无特殊说明,本发明所用的原料均优选为市售产品。
在本发明中,所述Li10GeP2S12粉末的粒径优选为0.1~1μm,更优选为0.2~0.6μm。在本发明中,所述压制成型前,还包括所述Li10GeP2S12粉末进行球磨,本发明对所述球磨不作具体限定,采用本领域技术人员熟知的操作将球磨至上述粒径即可。
在本发明中,所述压制成型的压力为0.5GPa~3.0GPa,优选为1.5~2.0GPa。保压时间为3~10min,优选为5min;在本发明中,升温至所述压制成型的压力的升压速率优选为0.5GPa/min。
在本发明中,压制成型后,优选还包括退压。在本发明中,所述退压的方式优选为一次淬压。
本发明还提供了上述所述的制备方法制备得到的Li10GeP2S12陶瓷片。
在本发明中,所述Li10GeP2S12陶瓷片的电导率优选为2.5~5mS·cm-1,更优选为2.6~4.7mS·cm-1。
本发明所述的Li10GeP2S12陶瓷片的压制模具如图1所示,由图1可知,所述压制模具包括铜板1和可拆卸的样品成型环2;
所述铜板中央设有凹槽11;所述凹槽的中心为中空腔12;
所述中空腔12用于可拆卸地设置所述样品成型环2;
所述样品成型环2的厚度与所述中空腔12的高度相同。
在本发明中,所述压制模具包括铜板1,本发明对所述铜板1的尺寸不作具体限定,具体优选为长度为50mm,宽度为50mm,厚度为5mm的铜板。
在本发明中,所述铜板1中央设有凹槽11,所述凹槽11的形状优选为圆形凹槽或方形凹槽,更优选为圆形凹槽。在本发明中,所述圆形凹槽的直径具体优选为30mm,高度优选为4mm。
在本发明中,所述凹槽11的中心为中空腔12,所述中空腔12优选为方状中空腔或柱状中空腔;所述柱状中空腔的直径具体优选为16mm,厚度优选为1mm。
在本发明中,所述中空腔12用于可拆卸地设置所述样品成型环2。在本发明中,所述样品成型环2的材质优选为叶腊石。在本发明中,所述样品成型环优选为方环样品成型环或圆环样品成型环。在本发明中,所述圆环样品成型环的外径具体优选为22mm。在本发明中,所述样品成型环2的厚度与所述中空腔12的高度相同,在本发明中,具体优选为1mm。在本发明中,所述样品成型环能够同时起到封压以及方便脱模的作用。
在本发明中,所述压制模具优选还包括脱模件3,所述脱模件3优选包括与所述凹槽11和中空腔12匹配的凸台。在本发明中,所述脱模件3的材质优选为不锈钢。
在本发明中,对所述压制模具的使用方法不做具体限定,采用本领域技术人员熟知的使用方法将装载好样品的模具与油压机配合使用即可。
在本发明中,所述Li10GeP2S12的装载优选为将模具放置于垫块上后,于模具中添加所述Li10GeP2S12,进行预压成型。
在本发明中,所述垫块的材质优选为Cr钢;所述预压成型的压力优选为10~20MPa,在本发明中,所述预压成型的目的是将粉末状Li10GeP2S12压实在样品腔,便于后续与油压机配合使用。
下面结合实施例对本发明提供的技术方案进行详细地说明,但是不能把它们理解为对本发明保护范围的限定。
实施例1~7
油压机事先预设压力设置分别为0.5、1.0、1.5、2.0、2.5以及3.0GPa,升压速率和保压时间统一设置为0.5GPa/min和5min。
取300mg粒径为0.2μm的Li10GeP2S12陶瓷片粉末在真空手套箱内放入图1所示结构的模具中,(模具预先放置于Cr钢垫块),在10MPa下进行预压成型,然后将装载完样品的模具放入密封盒后从真空手套箱取出置于油压机按照预设加压程序进行压制成型,压制成型后进行退压,然后用脱模件将陶瓷片脱模,分别得到不同压制压力下的厚度1mm,直径16mm的Li10GeP2S12陶瓷片(简称为LGPS)。
对比例1
与实施例1的区别仅仅在于压力设置为0.03GPa。
测试例
将实施例1和对比例1制备得到的LGPS按照不锈钢/LGPS/不锈钢的叠加方式组装成对称型测试模型,采用交流阻抗谱法进行离子电导率测试,测试结果见图2。从图2可知:1.5GPa压力下制备而成的陶瓷片锂离子电导率表现为最高,为4.62mS·cm-1。
将实施例1在1.5GPa压力下和对比例1制备而成的陶瓷片进行电镜扫描,扫描电镜图见图3,其中图3a为对比例1制备而成的陶瓷片的扫描电镜图,图3b为1.5GPa压力下制备而成的陶瓷片的扫描电镜图。由图3可知:1.5GPa处理后的LGPS陶瓷片孔洞更少,颗粒之间更紧密。
将实施例1在1.5GPa压力下压制后的LGPS和对比例1制备得到的LGPS作为固态电解质,磷酸铁锂为正极,锂片为负极,组装成2032型纽扣电池(LFePO4/LGPS/Li),进行电化学性能(比容量)测试,测试结果见图4,从图4可知:LGPS陶瓷片与电极之间构建了很好的离子导电通道,界面阻抗更小,磷酸铁锂正极比容量可达143.9mAh/g。
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (7)
1.一种Li10GeP2S12陶瓷片的制备方法,其特征在于,包括以下步骤:
将Li10GeP2S12粉末进行压制成型,得到所述Li10GeP2S12陶瓷片;
所述压制成型的压力为0.5~3.0GPa,保压时间为3~10min。
2.根据权利要求1所述的制备方法,其特征在于,所述Li10GeP2S12粉末的粒径为0.1~1μm。
3.权利要求1或2所述的制备方法制备得到的Li10GeP2S12陶瓷片,其特征在于,所述Li10GeP2S12陶瓷片的电导率为2.5~5mS·cm-1。
4.用于权利要求3权利要求所述的Li10GeP2S12陶瓷片的压制模具,其特征在于,包括铜板(1)和可拆卸的样品成型环(2);
所述铜板中央设有凹槽(11);所述凹槽的中心为中空腔(12);
所述中空腔(12)用于可拆卸地设置所述样品成型环(2);
所述样品成型环(2)的厚度与所述中空腔(12)的高度相同。
5.根据权利要求4所述的压制模具,其特征在于,还包括脱模件(3)。
6.根据权利要求5所述的压制模具,其特征在于,所述脱模件(3)包括与所述凹槽(11)和中空腔(12)匹配的凸台。
7.根据权利要求4所述的压制模具,其特征在于,所述样品成型环(2)的材质为叶腊石。
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