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Construction of a High‑Performance composite solid electrolyte Through In‑Situ Polymerization within a Self‑Supported Porous Garnet Framework

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Nano-Micro Letters 2024年第5期16卷 56-70页

作者： An‑Giang Nguyen Min‑Ho Lee Jaekook Kim Chan‑Jin Park Department of Materials Science and Engineering Chonnam National University77 Yongbong‑roBuk‑guGwangju 61186South Korea

composite solid electrolytes(CSEs)have emerged as promising candidates for safe and high-energy–density solid-state lithium metal batteries(SSLMBs).However,concurrently achieving exceptional ionic conductivity and interface compatibility between the electrolyte and electrode presents a significant challenge in the development of high-performance CSEs for SSLMBs.To overcome these challenges,we present a method involving the in-situ polymerization of a monomer within a self-supported porous Li_(6.4)La_(3)Zr_(1.4)Ta_(0.6)O_(12)(LLZT)to produce the CSE.The synergy of the continuous conductive LLZT network,well-organized polymer,and their interface can enhance the ionic conductivity of the CSE at room temperature.Furthermore,the in-situ polymerization process can also con-struct the integration and compatibility of the solid electrolyte–solid electrode interface.The synthesized CSE exhibited a high ionic conductivity of 1.117 mS cm^(-1),a significant lithium transference number of 0.627,and exhibited electrochemical stability up to 5.06 V vs.Li/Li+at 30℃.Moreover,the Li|CSE|LiNi_(0.8)Co_(0.1)Mn_(0.1)O_(2) cell delivered a discharge capacity of 105.1 mAh g^(-1) after 400 cycles at 0.5 C and 30℃,corresponding to a capacity retention of 61%.This methodology could be extended to a variety of ceramic,polymer electrolytes,or battery systems,thereby offering a viable strategy to improve the electrochemical properties of CSEs for high-energy–density SSLMBs.

关键词： Scalable tape-casting method Self-supported porous Li_(6.4)La_(3)Zr_(1.4)Ta_(0.6)O_(12) composite solid electrolyte LiF-and B-rich interphase layers

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Flexible,solid-state,fiber-network-reinforced composite solid electrolyte for long lifespan solid lithium-sulfurized polyacrylonitrile battery

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Nano Research 2022年第4期15卷 3290-3298页

作者： Shiqiang Luo Enyou Zhao Yixuan Gu Nagahiro Saito Zhengxi Zhang Li Yang Shin-ichi Hirano School of Chemistry and Chemical Engineering Frontiers Science Center for Transformative MoleculesShanghai Jiao Tong UniversityShanghai 200240China Department of Chemical Systems Engineering Nagoya UniversityNagoya 4648603Japan Shanghai Electrochemical Energy Devices Research Center Shanghai 200240China Hirano Institute for Materials Innovation Shanghai Jiao Tong UniversityShanghai 200240China

solid lithium-sulfur batteries(SLSBs)show potential for practical application due to their possibility for high energy density.However,SLSBs still face tough challenges such as the large interface impedance and lithium dendrite formation.Herein,a highperformance SLSB is demonstrated by using a fiber network reinforced Li_(6.75)La_(3)Zr_(1.75)Ta_(0.25)O_(12)(LLZTO)based composite solid electrolyte(CSE)in combination with sulfurized polyacrylonitrile(SPAN)cathode.The CSE consisting of an electrospun polyimide(PI)film,LLZTO ionically conducting filler and polyacrylonitrile(PAN)matrix,which is named as PI-PAN/LLZTO CSE,possesses high room-temperature ionic conductivity(2.75×10^(-4)S/cm),high Li^(+)migration number(tLi+)of 0.67 and good interfacial wettability.SPAN is utilized due to its unique electrochemical properties:reasonable electronic conductivity and no polysulfides shuttle effect.The CSE enables a highly stable Li plating/stripping cycle for over 600 h and good rate performance.Moreover,the assembled SLSB exhibits good cycle performance of accomplishing 120 cycles at 0.2 C with the capacity retention of 474 mAh/g,good rate properties and excellent long-term cycling stability with a high capacity retention of 86.49%from 15^(th)to 1,000^(th)cycles at 1.0 C.This work rationalizes our design concept and may guide the future development of SLSBs.

关键词： solid lithium-sulfur battery composite solid electrolyte sulfurized polyacrylonitrile cathode interfacial wettability dendritefree

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Scalable,thin asymmetric composite solid electrolyte for high-performance all-solid-state lithium metal batteries

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Interdisciplinary Materials 2022年第3期1卷 434-444页

作者： Guoxu Wang Yuhao Liang Hong Liu Chao Wang Dabing Li Li-Zhen Fan Beijing Key Laboratory for Advanced Energy Materials and Technologies Beijing Advanced Innovation Center for Materials Genome EngineeringUniversity of Science and Technology BeijingBeijingChina

All-solid-state Li metal batteries(ASSLMBs)have been considered the most promising candidates for next-generation energy storage devices owing to their high-energy density and safety.However,some obstacles such as thick solid electrolyte(SSEs)and unstable interface between the solid-state electrolytes(SSEs)and the electrodes have restricted the practical application of ASSLBs.Here,the scalable polyimide(PI)film reinforced asymmetric ultrathin(~20μm)composite solid electrolyte(AU-CSE)with a ceramic-rich layer and polymer-rich layer is fabricated by a both-side casting method and rolling process.The ceramic-rich layer not only acts as a“securer”to inhibit the lithium dendrite growth but also redistributes Li-ions uniform deposition,while the polymer-rich layer improves the compatibility with cathode materials.As a result,the obtained AU-CSE demonstrates an ionic conductivity of 1.44×10^(−4)S cm^(−1)at 35°C.The PI-reinforced AU-CSE enables Li/Li symmetric cell stable cycling over 1200 h at_(0.2)mA cm^(−2)and_(0.2)mAh cm^(−2).Li/LiNi_(0.6)Co_(0.2)Mn_(0.2)O2 and Li/LiFePO4 ASSLMBs achieve superior performances at 35°C.This study provides a new way of solving the interface problems between SSEs and electrodes and developing high-energy-density ASSLMBs for practical applications.

关键词： all-solid-state lithium batteries asymmetric composite solid electrolyte ultra-thin

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High-conductivity free-standing Li_(6)PS_(5)Cl/poly(vinylidene difluoride)composite solid electrolyte membranes for lithium-ion batteries

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Journal of Materiomics 2020年第1期6卷 70-76页

作者： Shuo Wang Xue Zhang Sijie Liu Chengzhou Xin Chuanjiao Xue Felix Richter Liangliang Li Lizhen Fan Yuanhua Lin Yang Shen Jurgen Janek Ce-Wen Nan State Key Laboratory of New Ceramics and Fine Processing School of Materials Science and EngineeringTsinghua UniversityBeijing100084China Institute of Physical Chemistry&Center for Materials Research Justus-Liebig-University GiessenHeinrich-Buff-Ring 17D-35392GiessenGermany Institute of Advanced Materials and Technology University of Science and Technology BeijingBeijing100083China

Bulk-type all-solid-state batteries(ASSBs)using sulfide solid electrolyte are considered as a promising alternative to commercial lithium-ion batteries owing to their high energy density and safety.However,cell energy density is often comparatively low due to use of a thick solid electrolyte separator and a lithium alloy as anode.For achieving high-performance ASSBs,creating a thin free-standing electrolyte with high-conductivity and good cycling stability against lithium anode is essential.In this work,we present Li_(6)PS_(5)Cl/poly(vinylidene difluoride)(LPSCl/PVDF)composite electrolytes prepared by a slurry method.The influence of the PVDF content on the microstructure,morphology,ionic conductivity and activation energy of the LPSCl/PVDF electrolytes is systematically investigated.Free-standing LPSCl/PVDF membranes with a thickness of 100-120 mm and a high ionic conductivity of about 1·10^(-3) S cm^(-1) at 25℃ are obtained.After adding PVDF to the LPSCl electrolyte,the cycling stability of the LPSCl electrolyte against lithium metal improves significantly.Therefore,LPSCl/PVDF composite electrolytes are promising candidates to be used in ASSBs.

关键词： composite solid electrolyte Li_(6)PS_(5)Cl Poly(vinylidene difluoride)

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Highly Efficient Aligned Ion‑Conducting Network and Interface Chemistries for Depolarized All‑solid‑State Lithium Metal Batteries

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Nano-Micro Letters 2024年第5期16卷 102-119页

作者： Yongbiao Mu Shixiang Yu Yuzhu Chen Youqi Chu Buke Wu Qing Zhang Binbin Guo Lingfeng Zou Ruijie Zhang Fenghua Yu Meisheng Han Meng Lin Jinglei Yang Jiaming Bai Lin Zeng Shenzhen Key Laboratory of Advanced Energy Storage Southern University of Science and TechnologyShenzhen 518055People’s Republic of China Department of Mechanical and Energy Engineering Southern University of Science and TechnologyShenzhen 518055People’s Republic of China SUSTech Energy Institute for Carbon Neutrality Southern University of Science and TechnologyShenzhen 518055People’s Republic of China Department of Mechanical and Aerospace Engineering Hong Kong University of Science and TechnologyKowloon 997077Hong Kong Special Administrative Region of ChinaPeople’s Republic of China HKUST Shenzhen-Hong Kong Collaborative Innovation Research Institute FutianShenzhenPeople’s Republic of China

Improving the long-term cycling stability and energy density of all-solid-state lithium(Li)-metal batteries(ASSLMBs)at room temperature is a severe challenge because of the notorious solid–solid interfacial contact loss and sluggish ion transport.solid electrolytes are generally studied as two-dimensional(2D)structures with planar interfaces,showing limited interfacial contact and further resulting in unstable Li/electrolyte and cathode/electrolyte interfaces.Herein,three-dimensional(3D)architecturally designed composite solid electrolytes are developed with independently controlled structural factors using 3D printing processing and post-curing treatment.Multiple-type electrolyte films with vertical-aligned micro-pillar(p-3DSE)and spiral(s-3DSE)structures are rationally designed and developed,which can be employed for both Li metal anode and cathode in terms of accelerating the Li+transport within electrodes and reinforcing the interfacial adhesion.The printed p-3DSE delivers robust long-term cycle life of up to 2600 cycles and a high critical current density of 1.92 mA cm^(−2).The optimized electrolyte structure could lead to ASSLMBs with a superior full-cell areal capacity of 2.75 mAh cm^(−2)(LFP)and 3.92 mAh cm^(−2)(NCM811).This unique design provides enhancements for both anode and cathode electrodes,thereby alleviating interfacial degradation induced by dendrite growth and contact loss.The approach in this study opens a new design strategy for advanced composite solid polymer electrolytes in ASSLMBs operating under high rates/capacities and room temperature.

关键词： All-solid-state lithium metal batteries composite solid electrolyte 3D printing Areal capacity Interfacial degradation

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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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Integrated interface between composite electrolyte and cathode with low resistance enables ultra-long cycle-lifetime in solid-state lithium-metal batteries

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Science China Chemistry 2021年第4期64卷 673-680页

作者： Zhuo Li Xin Guo State Key Laboratory of Material Processing and Die&Mould Technology Laboratory of Solid State IonicsSchool of Materials Science and EngineeringHuazhong University of Science and TechnologyWuhan 430074China

We report a three-dimensional(3D)nanofiber-reinforced solid composite electrolyte with a 3D Li^(+)-conducting ceramic network of Li_(6.2)5Ga_(0.25)La_(3)Zr_(2)O_(12)(LLZO)nanofibers.Benefiting from the 3D structure,the composite shows a high ionic conductivity of 3.2×10^(-4)S cm^(-1)and Li-ion transference number of 0.32 at room temperature.The interfacial resistance between the composite solid electrolyte and cathode is mitigated by creating an integrated interfacial structure,in which the polyethylene oxide(PEO)-lithiumbis(trifluoromethylsulphonyl)imide(LiTFSI)binder and ionic liquids(ILs)form a viscoelastic interface.Therefore,intimate contact,low interfacial impedance,and fast ion-transport between the cathode and the solid electrolyte are simultaneously achieved.solid-state lithium metal batteries with the Li Fe PO_(4) cathode deliver a superior capacity(158.0 m A h g^(-1))and significant capacity retention(90.4%retention after 800 cycles)at 60℃.Moreover,the smooth and uniform Li surface after long-term cycling confirms the successful suppression of the dendrite formation.The integrated interfacial structure provides a solution to the interfacial problem and improves the cycling performance in solid-state Li-metal batteries.

关键词： composite solid electrolyte Li_(7)La_(3)Zr_(2)O_(12)nanofiber interfacial resistance solid-state battery

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Lithiated Nafion-garnet ceramic composite electrolyte membrane for solid-state lithium metal battery

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Journal of Energy Chemistry 2020年第7期29卷 237-247,I0008页

作者： Jing Gao Qinjun Shao Jian Chen Advanced Rechargeable Battery Laboratory Dalian Institute of Chemical PhysicsChinese Academy of SciencesDalian 116023LiaoningChina University of Chinese Academy of Sciences Beijing 100049China

Single-ion conducting solid polymer electrolytes are expected to play a vital role in the realization of solid-state Li metal batteries.In this work,a lithiated Nafion(Li-Nafion)-garnet ceramic Li6.25La3 Zr2 Al0.25O12(LLZAO)composite solid electrolyte(CSE)membrane with 30μm thickness was prepared for the first time.By employing X-ray photoelectron spectroscopy and transmission electron microscope,the interaction between LLZAO and Li-Nafion was investigated.It is found that the LLZAO interacts with the Li-Nafion to form a space charge layer at the interface between LLZAO and Li-Nafion.The space charge layer reduces the migration barrier of Li-ions and improves the ionic conductivity of the CSE membrane.The CSE membrane containing 10 wt%LLZAO exhibits the highest ionic conductivity of2.26×10-4 S cm-1 at 30℃among the pristine Li-Nafion membrane,the membrane containing 5 wt%,20 wt%,and 30 wt%LLZAO,respectively.It also exhibits a high Li-ion transference number of 0.92,and a broader electrochemical window of 0-+4.8 V vs.Li+/Li than that of 0-+4.0 V vs.Li+/Li for the pristine Li-Nafion membrane.It is observed that the CSE membrane not only inhibits the growth of Li dendrites but also keeps excellent electrochemical stability with the Li electrode.Benefitting from the above merits,the solid-state LiFePO4/Li cell fabricated with the CSE membrane was practically charged and discharged at 30℃.The cell exhibits an initial reversible discharge specific capacity of 160 mAh g-1 with 97%capacity retention after 100 cycles at 0.2 C,and maintains discharge specific capacity of 126 mAh g-1 after500 cycles at 1 C.The CSE membrane prepared with Li-Nafion and LLZAO is proved to be a promising solid electrolyte for advanced solid-state Li metal batteries.

关键词： Single-ion conductor composite solid electrolyte Lithiated Nafion Garnet ceramic solid-state Li metal battery

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High-Performance 3-D Fiber Network composite electrolyte Enabled with Li-Ion Conducting Nanofibers and Amorphous PEO-Based Cross-Linked Polymer for Ambient All-solid-State Lithium-Metal Batteries

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Advanced Fiber Materials 2019年第1期1卷 46-60页

作者： Chaoyi Yan Pei Zhu Hao Jia Jiadeng Zhu R.Kalai Selvan Ya Li Xia Dong Zhuang Du Indunil Angunawela Nianqiang Wu Mahmut Dirican Xiangwu Zhang Fiber and Polymer Science Program Department of Textile EngineeringChemistry and ScienceWilson College of TextilesNorth Carolina State UniversityRaleighNC 27695-8301USA Department of Physics and Organic and Carbon Electronics Lab North Carolina State UniversityRaleighNC 27695-8301USA Department of Mechanical and Aerospace Engineering West Virginia UniversityMorgantownWV 26506USA

solid electrolytes have gained attention recently for the development of next-generation Li-ion batteries since they can fun-damentally improve the battery stability and safety.Among various types of solid electrolytes,composite solid electrolytes(CSEs)exhibit both high ionic conductivity and excellent interfacial contact with the electrodes.Incorporating active nanofib-ers into the polymer matrix demonstrates an effective method to fabricate CSEs.However,current CSEs based on traditional poly(ethylene oxide)(PEO)polymer suffer from the poor ionic conductivity of PEO and agglomeration effect of inorganic fillers at high concentrations,which limit further improvements in Li+conductivity and electrochemical stability.Herein,we synthesize a novel PEO based cross-linked polymer(CLP)as the polymer matrix with naturally amorphous structure and high room-temperature ionic conductivity of 2.40×10^(−4)S cm^(−1).Li_(0.3)La_(0.557)TiO_(3)(LLTO)nanofibers are incorporated into the CLP matrix to form composite solid electrolytes,achieving enhanced ionic conductivity without showing filler agglomeration.The high content of Li-conductive nanofibers improves the mechanical strength,ensures the conductive network,and increases the total Li+conductivity to 3.31×10^(−4)S cm^(−1).The all-solid-state Li|LiFePO_(4)batteries with LLTO nanofiber-incorporated CSEs are able to deliver attractive specific capacity of 147 mAh g^(−1)at room temperature,and no evident dendrite is found at the anode/electrolyte interface after 100 cycles.

关键词： Cross-linked PEO polymer Li_(0.33)La_(0.55)TiO_(3)nanofibers composite solid electrolyte All-solid-state batteries Ambient working temperature

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LiF and LiNO_(3) as synergistic additives for PEO-PVDF/LLZTO-based composite electrolyte towards high-voltage lithium batteries with dualinterfaces stability

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Journal of Energy Chemistry 2022年第2期31卷 319-328页

作者： Liansheng Li Yuanfu Deng Huanhuan Duan Yunxian Qian 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 Shenzhen CAPCHEM Technol Co Ltd. Shenzhen 518118GuangdongChina Department of Mechanical Engineering The Hong Kong Polytechnic UniversityHung HomKowloonHong KongChina

solid electrolytes with desirable properties such as high ionic conductivity,wide electrochemical stable window,and suitable mechanical strength,and stable electrode-electrolyte interfaces on both cathode and anode side are essential for high-voltage all-solid-state lithium batteries(ASSLBs)to achieve excellent cycle stability.In this work,a novel strategy of using LiF and LiNO_(3) as synergistic additives to boost the performance of PEO-PVDF/LLZTO-based composite solid electrolytes(CSEs)is developed,which also promotes the assembled high-voltage ASSLBs with dual-interfaces stability characteristic.Specifically,LiF as an inactive additive can increase the electrochemical stability of the CSE under high cut-off voltage,and improve the high-voltage compatibility between cathode and CSE,thus leading to a stable cathode/CSE interface.LiNO_(3) as an active additive can lead to an enhanced ionic conductivity of CSE due to the increased free-mobile Li+and ensure a stable CSE/Li interface by forming stable solid electrolyte interphase(SEI)on Li anode surface.Benefiting from the improved performance of CSE and stable dualinterfaces,the assembled NCM622/9[PEO_(15)-LiTFSI]-PVDF-15 LLZTO-2 LiF-3 LiNO_(3)/Li cell delivers a high rate capacity of 102.1 mAh g^(-1) at 1.0 C and a high capacity retention of 77.4%after 200 cycles at 0.5 C,which are much higher than those of the ASSLB assembled with additive-free CSE,with only 60.0 mAh g^(-1) and 52.0%,respectively.Furthermore,novel cycle test modes of resting for 5 h at different charge states after every 5 cycles are designed to investigate the high-voltage compatibility between cathode and CSE,and the results suggest that LiF additive can actually improve the high-voltage compatibility of cathode and CSE.All the obtained results confirm that the strategy of using synergistic additives in CSE is an effective way to achieve high-voltage ASSLBs with dual-interfaces stability.

关键词： Synergistic additives composite solid electrolyte Dual-interfaces stability High-voltage cathode Lithium metal battery

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