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Green recycling of short-circuited garnet-type electrolyte for high-performance solid-state lithium batteries

Journal of Energy Chemistry 2023年第5期80卷 492-500,I0012页

作者： Yongxian Huang Zhiwei Qin Cheng Shan Yuming Xie Xiangchen Meng Delai Qian Gang He Dongxin Mao Long Wan state Key Laboratory of Advanced Welding and Joining Harbin Institute of TechnologyHarbin 150001HeilongjiangChina Zhengzhou Research Institute Harbin Institute of TechnologyZhengzhou 450046HenanChina School of Materials Science and Engineering Harbin Institute of TechnologyHarbin 150001HeilongjiangChina

solid-state lithium batteries(SSLBs)solve safety issues and are potentially energy-dense alternatives to next-generation energy storage systems.Battery green recycling routes are responsible for the widespread use of SSLBs due to minimizing environmental contamination,reducing production costs,and providing a sustainable solution for resources,e.g.,saving rare earth elements(La,Ta,etc.).Herein,a solid-state recycling strategy is proposed to achieve green recycling of the crucial component solidstate electrolytes(SSEs)in spent SSLBs.The short-circuited garnet Li_(6.5)La_(3)Zr_(1.5)Ta_(0.5)O_(12)(LLZTO)is broken into fine particles and mixed with fresh particles to improve sintering activity and achieve high packing density.The continuous Li absorption process promotes sufficient grain fusion and guarantees the transformation from tetragonal phase to pure cubic phase for high-performance recycled LLZTO.The Li-ion conductivity reaches 5.80×10^(-4)S cm-1with a relative density of 95.9%.Symmetric Li cell with asrecycled LLZTO shows long-term cycling stability for 700 h at 0.3 mA cm^(-2)without any voltage hysteresis.Full cell exhibits an excellent cycling performance with a discharge capacity of 141.5 mA h g^(-1)and a capacity retention of 92.1%after 400 cycles(0.2C).This work develops an environmentally friendly and economically controllable strategy to recycle SSE from spent SSLBs,guiding future directions of SSLBs large-scale industrial application and green recycling study.

关键词： solid-state electrolytes Li-garnet Green recycling solid-state lithium batteries Cycling stability

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In situ analysis of dynamic evolution of the additive-regulated cathode processes in quasi-solid-state lithium-metal batteries

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Science China Chemistry 2023年第10期66卷 2921-2928页

作者： Jian-Xin Tian Hui-Juan Guo Jing Wan Gui-Xian Liu Rui Wen Li-Jun Wan CAS Key Laboratory of Molecular Nanostructure and Nanotechnology CAS Research/Education Center for Excellence in Molecular SciencesBeijing National Laboratory for Molecular ScienceInstitute of ChemistryChinese Academy of SciencesBeijing 100190China University of Chinese Academy of Sciences Beijing 100049China

The implementation of high-energy-density storage devices can be facilitated by the built-in situ cathode electrolyte interphase(CEI)between Ni-rich cathodes and gel polymer electrolytes,as it improves interfacial compatibility and enhances security.Understanding the interphase processes of cathode materials,including the structural evolution and the formation of cathode electrolyte interphase upon charging/discharging,is crucial for the design of solid-state lithium batteries.Here,we employed in situ atomic force microscopy(AFM)to investigate the effects of lithium difluoro(oxalato)borate(Li DFOB)on the dynamic evolution of the cathode interphase.In the presence of Li DFOB,the adhesion of nanoparticles and a thin amorphous film on the cathode surface resulted in the formation of a homogeneous CEI,inducing the production of LixPFyas byproducts.Furthermore,the stable CEI formed between the cathode and electrolyte helps maintain the integrity of the composition and structure,reduces interfacial resistance,and improves the cycle stability of the batteries.The visualization of in situ AFM in quasi-solid-state lithium-metal batteries provides valuable insights into the distinct nanostructures and growth dynamics of Li DFOB-mediated CEI on the LiNi_(6)Co_(2)Mn_(2)O_(2) cathode,thus offering a universal and convenient technique for interfacial analysis and a mechanistic understanding of solid-state batteries.

关键词： atomic force microscopy electrochemistry interfacial dynamics solid-state lithium batteries cathode electrolyte interphase

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In-situ interfacial passivation and self-adaptability synergistically stabilizing all-solid-state lithium metal batteries

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Journal of Energy Chemistry 2024年第1期88卷 282-292,I0007页

作者： Huanhui Chen Xing Cao Moujie Huang Xiangzhong Ren Yubin Zhao Liang Yu Ya Liu Liubiao Zhong Yejun Qiu Shenzhen Engineering Lab of Flexible Transparent Conductive Films School of Materials Science and EngineeringHarbin Institute of TechnologyShenzhen 518055GuangdongChina Guangdong Provincial Key Laboratory of Semiconductor Optoelectronic Materials and Intelligent Photonic Systems School of Materials Science and EngineeringHarbin Institute of TechnologyShenzhen 518055GuangdongChina College of Chemistry and Environmental Engineering Shenzhen UniversityShenzhen 518060GuangdongChina School of Resource and Environmental Sciences Wuhan UniversityWuhan 430072HubeiChina

The function of solid electrolytes and the composition of solid electrolyte interphase(SEI)are highly significant for inhibiting the growth of Li dendrites.Herein,we report an in-situ interfacial passivation combined with self-adaptability strategy to reinforce Li_(0.33)La_(0.557)TiO_(3)(LLTO)-based solid-state batteries.Specifically,a functional SEI enriched with LiF/Li_(3)PO_(4) is formed by in-situ electrochemical conversion,which is greatly beneficial to improving interface compatibility and enhancing ion transport.While the polarized dielectric BaTiO_(3)-polyamic acid(BTO-PAA,BP)film greatly improves the Li-ion transport kinetics and homogenizes the Li deposition.As expected,the resulting electrolyte offers considerable ionic conductivity at room temperature(4.3 x 10~(-4)S cm^(-1))and appreciable electrochemical decomposition voltage(5.23 V)after electrochemical passivation.For Li-LiFePO_(4) batteries,it shows a high specific capacity of 153 mA h g^(-1)at 0.2C after 100 cycles and a long-term durability of 115 mA h g^(-1)at 1.0 C after 800 cycles.Additionally,a stable Li plating/stripping can be achieved for more than 900 h at 0.5 mA cm^(-2).The stabilization mechanisms are elucidated by ex-situ XRD,ex-situ XPS,and ex-situ FTIR techniques,and the corresponding results reveal that the interfacial passivation combined with polarization effect is an effective strategy for improving the electrochemical performance.The present study provides a deeper insight into the dynamic adjustment of electrode-electrolyte interfacial for solid-state lithium batteries.

关键词： solid-state lithium batteries Composite solid electrolyte In-situ polymerization Interfacial passivation layer Self-adaptability

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solid-state lithium batteries: Safety and prospects

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eScience 2022年第2期2卷 138-163页

作者： Yong Guo Shichao Wu Yan-Bing He Feiyu Kang Liquan Chen Hong Li Quan-Hong Yang Nanoyang Group State Key Laboratory of Chemical EngineeringSchool of Chemical Engineering and TechnologyTianjin UniversityTianjin300072China Joint School of National University of Singapore and Tianjin University International Campus of Tianjin UniversityBinhai New CityFuzhou350207China Haihe Laboratory of Sustainable Chemical Transformations Tianjin300192China Key Laboratory of Advanced Energy Materials Chemistry(Ministry of Education) College of ChemistryNankai UniversityTianjin300071China Shenzhen Geim Graphene Center Tsinghua Shenzhen International Graduate SchoolTsinghua UniversityShenzhen518055China Institute of Physics Chinese Academy of SciencesBeijing100190China

solid-state lithium batteries are flourishing due to their excellent potential energy density.Substantial efforts have been made to improve their electrochemical performance by increasing the conductivity of solid-state electrolytes(SEs)and designing a compatible battery configuration.The safety of a solid lithium battery has generally been taken for granted due to the nonflammability and strength of SEs.However,recent results have shown the release of dangerous gases and intense heat due to the formation of lithium dendrites,indicating the safety of solid-state lithium batteries may have been overestimated.In this review,we introduce a safety evaluation methodology,then focus on the garnet Li_(7)La_(3)Zr_(2)O_(12)(LLZO)and sulfide-based SEs,summarizing their structure,conductivity,compatibility with a lithium metal anode,electrochemical/chemical stability,and mechanical/thermal stability,which correlate closely with battery safety.We also evaluate the safety of all-solid-state lithium batteries,then conclude by discussing future avenues for improving the safety of SE-based batteries.

关键词： solid-state lithium batteries Safety evaluation Electrochemical/chemical stability Mechanical/thermal stability

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A flexible solid polymer electrolyte enabled with lithiated zeolite for high performance lithium battery

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Nano Research 2023年第7期16卷 9443-9452页

作者： Zhiyu Ding Qiming Tang Qi Zhang Penghui Yao Xingjun Liu Junwei Wu Shenzhen Key Laboratory of Advanced Materials Department of Materials Science and EngineeringHarbin Institute of Technology(Shenzhen)Shenzhen 518055China Maryland Energy Innovation Institute University of MarylandCollege ParkMD 20742USA Department of Chemical and Metallurgical Engineering Aalto UniversityKemistintie 1Aalto FI-00076Finland

solid-state lithium batteries using composite polymer electrolytes(CPEs)have attracted much attention owing to their higher safety compared to liquid electrolytes and flexibility compared to ceramic electrolytes.However,their unsatisfactory lithium-ion conductivity still limits their development.Herein,a high ion conductive CPE with multiple continuous lithium pathways is designed.This new electrolyte consists of poly(vinylidene fluorideco-hexafluoropropylene)(PVDF-HFP)and lithiated X type zeolite(Li-X),which possesses a high ionic conductivity(1.98×10^(-4)S/cm),high lithium transference number(t_(Li^(+))=0.55),wide electrochemical window(4.7 V),and excellent stability against the lithium anode.Density functional theory(DFT)calculation confirms that the Lewis acid sites in zeolite can graft with N,N-dimethylformamide(DMF)and PVDF-HFP chains,resulting in decreased crystallinity of polymer and providing rapid Li+transmission channels.When used in a full cell,the solid Li|Li-X-3%|LiFePO_(4) cell displays excellent cycling stability and rate performance at room temperature and 60℃.Furthermore,pouch cells with the Li-X-3%electrolyte exhibit brilliant safety under extreme conditions,such as folding and cutting.Thus,this proposed zeolite-PVDF-HFP CPE represents a promising potential in the application of making a safer,higher performing,and flexible solid-state lithium battery.

关键词： solid-state lithium batteries composite polymer electrolytes zeolite poly(vinylidene fluorideco-hexafluoropropylene)(PVDF-HFP) flexible

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Transformation of Undesired Li_(2)CO_(3)into Lithiophilic Layer Via Double Replacement Reaction for Garnet Electrolyte Engineering

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Energy & Environmental Materials 2022年第3期5卷 962-968页

作者： Jiaxu Zhang Ruohan Yu Jun Li Huiyu Zhai Gangjian Tan Xinfeng Tang state Key Laboratory of Advanced Technology for Materials Synthesis and Processing Wuhan University of TechnologyWuhan 430070China International School of Materials Science and Engineering Wuhan University of TechnologyWuhan 430070China

Garnet-type solid-state electrolytes(SSEs)are a remarkable Li-ion electrolyte for the realization of next-generation all-solid-state lithium batteries due to their excellent stability against Li metal as well as high ionic conductivities at room temperature.However,garnet electrolytes always contain undesired and hardly removable Li_(2)CO_(3) contaminations that have persistently large resistance and unstable interface contact with Li metal.This is a critical bottleneck for the practical application of garnet electrolytes.Here,we design a novel strategy to completely root out Li_(2)CO_(3) both inside and on the surface of garnet.This is achieved by a so-called double replacement reaction between Li_(2)CO_(3) and SiO_(2) during one-step hot press process for garnet electrolyte densification.It leads to in-situ transformation of LixSiOy(LSO)mostly locating around the grain boundaries of garnet.Due to the higher ion conductivity and better electrochemistry stability of LSO than Li_(2)CO_(3),the modified garnet electrolyte shows much improved electrochemical performance.Moreover,the wettability between modified garnet electrolyte and lithium metals was significantly enhanced in the absence of surface Li_(2)CO_(3).As a proof of concept,an assembled Li symmetric cell with modified garnet electrolyte displays a high critical current density(CCD)of 0.7 mA cm^(-2)and a low interfacial impedance(5Ωcm^(2))at 25℃.These results indicate that the upcycling of Li_(2)CO_(3)is a promising strategy to well-address the degradation and interfacial issue associated with garnet electrolytes.

关键词： double replacement reaction garnet electrolytes lithiophilic layer solid-state lithium batteries

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Nuclear magnetic resonance studies of organic-inorganic composite solid electrolytes

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Magnetic Resonance Letters 2021年第2期1卷 142-152页

作者： Xueyan Zhang Hua Huo MIIT Key Laboratory of Cnitical Materials Technology for New Energy Conversion and Storage School of Chemistry and Chermical EngineeringHarbin Institute of TechnologyNo.92 West Da Zhi StreetHarbin150001China

solid electrolytes have received widespread attention due to their higher safety than liquid electrolytes in the past decades.In particular,organic-inorganic composite solid electro-lytes(CSEs)in which inorganic fllers dispersed in polymer solid electrolytes are consid-ered to be one of the most promising candidate electrolytes for high-performance solid-state lithium batteries.Understanding the local environments and the conduction pathway/dynamics of Lit is essential for the design of high-performance CSEs.Nuclear magnetic resonance(NMR)is a non-invasive quantitative technique that has unique ca-pabilities in providing molecular structure information,morphological evolution,and measuring the movement of ions at different time scales.Therefore,for battery re-searchers,an accurate and comprehensive under standing of the basic principles and experimental design of solid-state NMR(SSNMR)is of great significance for investigating the abundant molecular structure and dynamics information in CSEs.The specific appli-cations of the SSNMR technique in CSEs are briefly introduced in this present review.

关键词： Composite solid electrolytes(CSEs) Conduction pathway solid-state NMR(SSNMR) solid-state lithium batteries

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