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Dynamic lithium-compensation mechanism for densification of garnet-type Li_(7)La_(3)Zr_(2)O_(12)electrolyte by Li_(2)O atmosphere buffer pair

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Nano Research 2024年第7期17卷 6184-6191页

作者： Chujun Zheng Ya Chen Haoxin Dong Yan Lu Jun Jin Zhaoyin Wen CAS Key Laboratory of Materials for Energy Conversion Shanghai Institute of CeramicsChinese Academy of ScienceShanghai 200050China State Key Lab High Performance Ceram and Superfine Shanghai Institute of CeramicsChinese Academy of SciencesShanghai 200050China Center of Materials Science and Optoelectronics Engineering University of Chinese Academy of SciencesBeijing 100049China

Solid-state lithium metal batteries are one of the most promising options for next-generation batteries pursuing high-energy density and ***,the inevitable volatilization of lithium compounds during sintering leads to low relative density and low ionic conductivity of solid-state ***,the dynamic lithium-compensation mechanism is proposed to facilitate the densification of Ta-substituted garnet-type electrolyte(Li_(6.5)La_(3)Zr_(1.5)Ta_(0.5)O_(12)(LLZT))through the reversible manipulating of Li_(2)O ***_(2)ZrO_(3)is used as mother powder additive,which reacts with Li_(2)O in sintering atmosphere and forms Li_(6)Zr_(2)O_(7).Li_(2)ZrO_(3)/Li_(6)Zr_(2)O_(7)buffer pair manipulates the sintering Li_(2)O atmosphere,which is vital for LLZT,within the Li_(2)O partial pressure range corresponding to Li_(2)ZrO_(3)and Li_(6)Zr_(2)O_(7).Furthermore,the reversibility mechanism of buffer pair for Li_(2)O absorption and release is *** obtained LLZT exhibits a relative density of over 96%and an ionic conductivity exceeding 7×10^(−4)S·cm^(−1)with no abnormal grain *** symmetric cell demonstrates an excellent lithium dendrite suppressing ability(stable cycling at a current density of 0.3 mA·cm^(−2)for over 1000 h).Such dynamic lithium-compensation strategy has been successfully applied in atmosphere manipulation of LLZT sintering process,which reduces the dependence of LLZT on the Li_(2)O atmosphere,making it conducive to large-scale preparation of electrolyte ceramics.

关键词： solid-state batteries garnet-type electrolyte high-density electrolyte dynamic lithium-compensation buffer pair

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Status and prospect of garnet/polymer solid composite electrolytes for all-solid-state lithium batteries

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Journal of Energy Chemistry 2020年第11期29卷 154-177页

作者： Liansheng Li Yuanfu Deng Guohua Chen The Key Laboratory of Fuel Cell for Guangdong Province School of Chemistry and Chemical EngineeringSouth China University of TechnologyGuangzhou 510640GuangdongChina Electrochemical Energy Engineering Research Center of Guangdong Province South China University of TechnologyGuangzhou 510640GuangdongChina Department of Mechanical Engineering The Hong Kong Polytechnic UniversityHung HomKowloonHong KongChina

Solid polymer electrolytes(SPEs), such as polyethylene oxide(PEO), are characteristic of good flexibility and excellent processability, but they suffer from low ionic conductivity and small Li+transference number at ambient temperature. Inorganic solid electrolytes(ISEs), garnet-type Li7La3Zr2O12 and its derivatives(LLZO-based) in particular, possess high ionic conductivity at room temperature, wide electrochemical stability window, large Li+transference number as well as good stability against Li metal ***, lithium dendrites growth, interfacial contact issue and brittle nature of LLZO-based ceramic electrolytes prevent their practical applications. In response to these shortcomings, LLZO-based/polymer solid composite electrolytes(SCEs), taking complementary advantages of two kinds of electrolytes, and thus simultaneously improving the electrode wettability, ionic conductivity and mechanical strength, have been made to develop high-performance SCEs in recent years. Herein, the intrinsic properties and research progress of LLZO-based/polymer SCEs, including LLZO-based/PEO SCEs(LLZO-based/PEO SCEs with uniform dispersion of LLZO-based fillers and LLZO-based/PEO layered SCEs) and LLZO-based/novel polymers SCEs, are summarized. Besides, comprehensive updates on their applications in solid-state batteries are also presented. Finally, challenges and perspectives of LLZO-based/polymer SCEs for advanced allsolid-state lithium batteries(ASSLBs) are suggested. This review paper aims to provide systematic research progress of LLZO-based/polymer SCEs, to allow for more efficient and target-oriented research on improving LLZO-based/polymer SCEs.

关键词： Solid polymer electrolyte garnet-type electrolyte Solid composite electrolyte All-solid-state battery

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Synthesis and ionic conductivity of Li_6La_3BiSnO_(12) with cubic garnet-type structure via solid-state reaction

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Journal of Central South University 2015年第8期22卷 2883-2886页

作者：彭红建肖理红曹远尼栾向峰 College of Chemistry and Chemical Engineering Central South University

The synthesis and transport properties of the Li6La3BiSnO1212 solid electrolyte by a solid-state reaction were reported. The condition to synthesize the Li6La3BiSnO1212 is 785 °C for 36 h in air. The refined lattice constant of Li6La3 BiSnO1212 is 13.007A. Qualitative phase analysis by X-ray powder diffraction patterns combined with the Rietveld method reveals garnet type compounds as major phases. The Li-ion conductivity of the prepared Li6La3BiSnO12 is 0.85×10^-4 S/cm at 22 °C, which is comparable with that of the Li5La3Bi2O12. The Li6La3BiSnO1212 compounds are chemically stable against Li CoO2 which is widely used as cathode material up to 700 °C but not against the Li Mn2O4 if the temperature is higher than 550 °C. The Li6La3 BiSnO1212 exhibits higher chemical stability than Li5La3Bi2O12, which is due to Sn substitution for Bi.

关键词： Li^+-ion solid electrolyte lithium battery garnet-type electrolyte solid-state reaction

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石榴石Li6.7La3Zr2Al0.1O12固体电解质表面改性研究

石榴石Li6.7La3Zr2Al0.1O12固体电解质表面改性研究

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作者：王道益福建师范大学

学位级别：硕士

因具有高比能量密度和高安全性等诸多优点,全固态锂电池被广泛认为是下一代储能电源的有力候选者之一。遗憾的是,固态电解质的本征电化学性能及其与正、负极的界面稳定性等诸多方面的问题限制了全固态电池的实际应用,尤其是固体电解质... 详细信息

因具有高比能量密度和高安全性等诸多优点,全固态锂电池被广泛认为是下一代储能电源的有力候选者之一。遗憾的是,固态电解质的本征电化学性能及其与正、负极的界面稳定性等诸多方面的问题限制了全固态电池的实际应用,尤其是固体电解质的低离子电导率、高界面阻抗和锂枝晶刺穿限制了电池的容量发挥和循环寿命。石榴石型立方相LiLaZrO（LLZO）具有较高的室温离子电导率和较宽的电化学窗口,其与聚氧化乙烯混合制成的复合固体电解质有望兼具高离子电导率、柔性和易加工等特点,同时LLZO大的杨氏模量和聚氧化乙烯的柔性也有利于抑制锂枝晶刺穿并降低界面阻抗,进而提升电池的安全性。正因如此,LLZO固态电解质是用于固态锂金属电池的最有前途的固体电解质材料之一并在近年来受到业界广泛关注。然而,在潮湿空气中LLZO表面自发形成的憎锂且低活性的LiCO,显著降低了LLZO固态电解质的离子导电性并增加了离子迁移势垒高度,最终恶化了固态电池的循环和倍率性能。改善LLZO的空气稳定性并有效去除LLZO表面LiCO杂质相,是提升LLZO基复合电解质离子迁移数和全电池性能的关键。针对上述LLZO固体电解质存在的问题,本论文提出硝酸刻蚀和AlO表面包覆两种途径去除LLZO表面LiCO杂质相,利用X射线粉末衍射、拉曼光谱、透射电子显微镜和X射线光电子能谱仪细致研究LLZO颗粒表面改性前后晶体结构和微结构变化。以Li Fe PO为正极、金属锂为负极、LLZO-PEO为电解质组装成固态电池,通过系统研究全电池电化学性能阐释表面改性增强电化学性能的机理。具体开展如下研究:（1）采用低浓度HNO-乙腈混合溶液,通过化学反应去除LLZO固态电解质表面LiCO相,并研究HNO刻蚀LLZO后,LLZO表面残余基团对锂离子迁移数和电池的影响。研究表明,HNO多次洗涤后可获得表面光滑且无LiCO残留的LLZO颗粒。同时,残余的NO根离子可与刻蚀后残留的Li络合,通过控制洗涤次数可以获得厚度不同的络合层。Li NO络合层生成可以增加LLZO颗粒界面Li的活性并更好地兼容聚合物,进而显著提升了复合电解质的离子电导率和离子迁移数。另外,循环后样品的XPS分析也表明,Li NO络合层可以促进电解质中锂盐的定向分解,并在金属锂负极侧形成了稳定的富Li F的固体电解质界面膜,进而抑制锂枝晶的无规生长。相比于无残留NO根离子的LLZO,利用残留有NO根离子的LLZO组装成的Li/LLZO-PEO/Li Fe PO全固态电池展现出了更好的电化学稳定性,在0.5C的倍率下循环200圈后仍具有140 m Ah/g的高放电比容量和97.4%的容量保持率。（2）为了提升LLZO的空气稳定性,通过原子层沉积技术在LLZO表面包覆上非晶AlO涂层。实验结果表明,包覆有11 nm AlO非晶层可以显著提升LLZO颗粒的空气稳定性,即使将LLZO颗粒在湿度高于90%的开放环境下暴露7天,LLZO样品表面也没有观测到LiCO杂质相。研究表明,非晶AlO涂层可以改善LLZO与PEO界面的空间电荷层,加速界面Li传导和降低电解质的本体阻抗。AlO的包覆的LLZO样品即便在潮湿的空气中暴露7天,所组装成的Li/LLZO-PEO/Li和Li/LLZO-PEO/Li Fe PO全固态电池依然具有较好的电化学稳定性和较高的比容量。本论文提出的HNO刻蚀阴离子残余法促进界面富Li F层生成、和利用非晶AlO包覆去除LiCO并增强LLZO空气稳定性。两种方法协同作用,不仅促进LLZO粉末的产业化生产和存储,也为高性能复合电解质的性能提升提供了借鉴。

关键词： All-solid-state battery garnet-type electrolyte Lithium carbonate Air stability Atomic layer deposition

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