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Revealing the reason for the unsuccessful fabrication of Li_(3)Zr_(2)Si_(2)PO_(12) by solid state reaction

Chinese Journal of Structural Chemistry 2023年第11期42卷 13-18页

作者： Zizhuo Liang Fuming Du Ning Zhao xiangxin guo College of Physics Qingdao UniversityQingdao266071China Research Institute of Automobile Parts Technology Hunan Institute of TechnologyHengyang 421002China

NASICON type Li_(3)Zr_(2)Si_(2)PO_(12)can be synthesized via cation exchange method with Na_(3)Zr_(2)Si_(2)PO_(12)as precursor,which retains the skeleton structure and achieves an ionic conductivity higher than 3 mS cm^(-1)at room temperature.However,large-scale fabrication via cation exchange reaction seems unlikely considering the expensive precursors and complicated preparation process.Herein,the viability of solid-state reaction to prepare Li_(3)Zr_(2)Si_(2)PO_(12)is explored,which has important implication for its industrialization.The sintering was conducted using the raw materials of LiOH,SiO_(2),ZrO_(2)and NH_(4)H_(2)PO_(4)with the nominal stoichiometric ratio of Li_(3)Zr_(2)Si_(2)PO_(12).The results show that the final product is a Li_(3)PO_(4)·2ZrSiO_(4)composite with negligible Li+conductivity,other than the expected Li_(3)Zr_(2)Si_(2)PO_(12)with high Li+conductivity.Combined with thermodynamic calculations based on density functional theory(DFT),the competition between Li_(3)PO_(4)·2ZrSiO_(4)and Li_(3)Zr_(2)Si_(2)PO_(12)with NASICON phase is analyzed.It was found that the formation energy(AG)of Li_(3)PO_(4)·2ZrSiO_(4)is lower than that of Li_(3)Zr_(2)Si_(2)PO_(12).In addition,the decomposition of Li_(3)Zr_(2)Si_(2)PO_(12)with Li_(3)PO_(4)-2ZrSiO_(4)as products is a thermodynamically spontaneous reaction.The influences related to the coordination structures on the structural stability of NZSP are discussed as well.These results demonstrate that the fabrication of Li_(3)Zr_(2)Si_(2)PO_(12)through high-temperature sintering is difficult,and the development of a synthetic method with mild conditions is essential for the Li_(3)Zr_(2)Si_(2)PO_(12)preparation.

关键词： NASICON-Type solid electrolytes Na_(3)Zr_(2)Si_(2)PO_(12) Li_(3)Zr_(2)Si_(2)PO_(12) Thermodynamic analysis Coordination structure

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Evaluation of solid electrolytes: Development of conventional and interdisciplinary approaches

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Interdisciplinary Materials 2023年第4期2卷 529-568页

作者： Muhammad Khurram Tufail Pengbo Zhai Waquar Khokar Mengyang Jia Ning Zhao xiangxin guo College of Physics Qingdao UniversityQingdaoChina College of Materials Science and Engineering Qingdao UniversityQingdaoChina

Solid-state lithium batteries(SSLBs)have received considerable attention due to their advantages in thermal stability,energy density,and safety.Solid electrolyte(SE)is a key component in developing high-performance SSLBs.An in-depth understanding of the intrinsic bulk and interfacial properties is imperative to achieve SEs with competitive performance.This review first introduces the traditional electrochemical approaches to evaluating the fundamental parameters of SEs,including the ionic and electronic conductivities,activation barrier,electrochemical stability,and diffusion coefficient.After that,the characterization techniques to evaluate the structural and chemical stability of SEs are reviewed.Further,emerging interdisciplinary visualization techniques for SEs and interfaces are highlighted,including synchrotron X-ray tomography,ultrasonic scanning imaging,time-of-flight secondary-ion mass spectrometry,and three-dimensional stress mapping,which improve the understanding of electrochemical performance and failure mechanisms.In addition,the application of machine learning to accelerate the screening and development of novel SEs is introduced.This review article aims to provide an overview of advanced characterization from a broad physical chemistry view,inspiring innovative and interdisciplinary studies in solid-state batteries.

关键词： advanced characterization interdisciplinary techniques machine learning solid electrolytes solid-state batteries

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The evolution of local structure of Mo6S8 during Li+ electrochemical storage studied by in-situ tender X-ray absorption spectroscopy

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Progress in Natural Science:Materials International 2022年第6期32卷 739-744页

作者： Pengfei Yu Yujian Xia Xuefei Feng Shun Zheng guoxi Ren Nian Zhang Xiaosong Liu Cheng Chen xiangxin guo State Key Laboratory of Functional Materials for Informatics Shanghai Institute of Microsystem and Information Technology Chinese Academy of Sciences National Synchrotron Radiation Laboratory University of Science and Technology of China University of Chinese Academy of Sciences Tianmu Lake Institute of Advanced Energy Storage Technologies School of Physical Science and Technology Shanghai Tech University Shanghai BYD Co. Ltd. College of Physics Qingdao University

Chevrel phase Mo6S8has attracted great interest because of its capability to accommodate different types of small cations through reversible topotactic redox reactions.However,the intercalation mechanism of Mo6S8is still far from being fully understood owing to the complexity of the crystal structure and limitation of the probe tools.In our study,the reaction mechanism of Li+intercalation into Mo6S8was studied as a model by in-situ tender X-ray absorption spectroscopy(itXAS) in the viewpoint of local structure.According to the isobestic points of the 1st derivative,the discharge process is divided into five regions while the charge process is divided into four regions,where most of the regions are assigned to the two-phase transition reactions.The intensity change of the two spectroscopic features of the 1st derivative is found to be correlated,implying that the intercluster bond length directly affects the localization of the unoccupied states of the intracluster bond.The asymmetric evolution of the intensity of a’ and b’ as well as the asymmetric partition of reaction regions demonstrate the asymmetry of the reaction path in discharge and charge process.The results help to clarify the remaining debates on the phase transitions.Besides,itXAS is demonstrated to be a powerful tool to study the reaction mechanism of Mo6S8.which is complementary to NMR,XRD and so on.

关键词： Chevrel phases Cathode materials X-ray absorption In-situ measurement Local structure

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Long-Cycle Lithium Batteries with LiNi_(0.8)Co_(0.1)Mn_(0.1)O_(2) Cathodes above 4.5 V Enabled by Uniform Coating of Nanosized Garnet Electrolytes

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Chinese Physics Letters 2024年第7期41卷 161-175页

作者：王建群赵宁郭向欣 College of Physics Qingdao UniversityQingdao 266071China

The pursuit of high-energy cathode materials has been focused on raising the charging cutoff voltage of nickel (Ni)-rich layered oxide cathode such as LiNi_(0.8)Co_(0.1)Mn_(0.1)O2 (NCM811). However, the NCM811 suffers from rapid capacity fading upon cycling at cutoff voltage higher than 4.5 V, owing to their structural degradation and labile surface reactivity. Surface-coating with solid electrolytes has been recognized as an effective method to mitigate the performance failure of NCM811 at high voltage. Herein, the nano-sized Li_(6.4)La_(3)Ta_(0.6)Zr_(1.4)O_(12) (LLZTO) is uniformly coated on the surface of single-crystal NCM811 particles, accompanied with the long-range Ta^(5+) diffusion into the transition metal layer of NCM811 lattice. It is revealed that the LLZTO coating can not only inhibit the surface reactions of NCM811 with liquid electrolytes but also play an important role in suppressing the bulk microcracking within the NCM811 particles. The incorporation of Ta^(5+) ion expands the lattice spacing and thereby improves the homogeneity of the Li^(+) diffusion in the single-crystal NCM811, which alleviates the mechanical strain and intragranular cracks caused by nonuniform phases-transformation at high charging voltage. The synergy of surface protection and structural stabilization realized by LLZTO coating enables the NCM811-based lithium batteries to achieve a remarkable electrochemical performance. Typically, LLZTO coated NCM811 delivers a high reversible specific capacity of 202.1 mAh⋅g^(−1) with an excellent capacity retention as high as 70% over 1000 cycles upon charging to 4.5 V at 1 C.

关键词： coating cycling sized

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Tungsten oxide thin films for highly sensitive triethylamine detection

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Journal of Materiomics 2022年第2期8卷 408-416页

作者： Guanglu Lei Zishuo Li guocai Lu Jinyuan Hu Haochuan Shang Xiaolei Zhang Xianghong Liu Jun Zhang xiangxin guo College of Physics Center for Marine Observation and CommunicationsQingdao UniversityQingdao266071China Key Laboratory of Advanced Energy Materials Chemistry(Ministry of Education) Nankai UniversityTianjin300071China

Metal oxide semiconductor(MOS)thin films are promising sensing layer for integration in gas sensor devices for detecting toxic and harmful molecules.Herein,tungsten oxide(WO_(3))thin films are deposited on interdigital electrodes by vacuum thermal evaporation to realize batch fabrication of high-performance gas sensors.Subsequent annealing at different temperatures allows for regulation of the concentration of oxygen vacancies in the WO_(3) films,which has been found to exert a great influence on the sensor properties.In addition,the surface structure of WO_(3) films is also highly dependent on the annealing temperature.Gas sensing investigations show that the WO_(3) sensor annealed at 500℃ pos-sesses the best sensing properties for detecting triethylamine(TEA)including very high response,good selectivity,fast response,and low limit of detection(63 ppb).The excellent sensor performances are attributed to the enhanced adsorption of oxidative oxygen species due to the presence of abundant oxygen vacancies.The scalable fabrication of WO_(3) thin film gas sensors and the oxygen vacancy engi-neering strategy proposed herein may shed some light to developing high performance environmental sensors.

关键词： Thin film Tungsten oxide Thermal evaporation Oxygen vacancy Gas sensor

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全固态锂电池热安全性研究进展

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精细化工 2024年第5期41卷 960-970页

作者：冯振华邱祥云张涛戴作强郭向欣青岛大学机电工程学院山东青岛266071 电动汽车智能化动力集成技术国家地方联合工程研究中心(青岛) 山东青岛266071 山东威能环保电源科技股份有限公司山东潍坊262700 青岛大学物理科学学院山东青岛266071

随着液态锂电池的广泛应用,热失控现象时有发生,其热安全性成为亟待解决的问题。全固态锂电池以其优异的安全性显示出巨大的应用潜力。该文简要介绍了全固态锂电池的基本概念及组成结构,重点阐述了氧化物、硫化物以及聚合物固体电解质... 详细信息

随着液态锂电池的广泛应用,热失控现象时有发生,其热安全性成为亟待解决的问题。全固态锂电池以其优异的安全性显示出巨大的应用潜力。该文简要介绍了全固态锂电池的基本概念及组成结构,重点阐述了氧化物、硫化物以及聚合物固体电解质的最新研究进展,并对这3类全固态锂电池的热安全性差异进行了总结,包括固体电解质材料级别、固体电解质与活性材料或锂金属负极混合时界面级别以及全电池级别的热安全性。此外,锂枝晶现象对全固态锂电池安全性的影响仍不可忽视。目前,针对材料和界面级别的热安全性研究众多,但全电池级别的研究较少,且多集中在小容量电池,针对全电池级别的热安全性仍需进一步探究。最后,指出了未来高安全性全固态锂电池的商业化应用应着力于解决全固态锂电池中的关键界面问题以及锂枝晶问题。

关键词：全固态锂电池高比能热安全性固体电解质锂枝晶

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纳米石榴石固体电解质粉体在聚合物电解质中的均匀分散

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物理化学学报 2024年第3期40卷 46-47页

作者：吕寒梅陈昕孙麒富赵宁郭向欣青岛大学物理科学学院山东青岛266071

固态锂电池(SSLBs)因采用金属锂负极和固体电解质,具有提高能量密度和安全性的潜质。固体电解质作为固态锂电池的关键材料,对电池性能有重要影响。其中,聚合物-石榴石型复合固态电解质因结合了聚合物电解质的易加工性以及石榴石电解质... 详细信息

固态锂电池(SSLBs)因采用金属锂负极和固体电解质,具有提高能量密度和安全性的潜质。固体电解质作为固态锂电池的关键材料,对电池性能有重要影响。其中,聚合物-石榴石型复合固态电解质因结合了聚合物电解质的易加工性以及石榴石电解质的热稳定性和高离子电导率的优点,在固态电池规模化制造中具有良好的应用前景。然而,由于纳米固体电解质粉体的表面能高、与有机物的界面兼容性差,导致纳米锂镧锆氧颗粒在聚合物基体中容易发生团聚,进而导致复合电解质的离子电导率降低。本工作引入硅烷偶联剂3-缩水甘油氧基丙基三甲氧基硅烷(GPTMS)对Li_(6.4)La_(3)Zr_(1.4)Ta_(0.6)O_(12)(LLZTO)的表面进行改性,旨在改善LLZTO颗粒在溶剂和聚合物基体中的分散性。LLZTO纳米颗粒表面的羟基与GPTMS分子反应形成共价键,在颗粒表面形成一层厚度约5 nm的GPTMS修饰层。GPTMS中具有亲脂性的环氧基团,使改性后的LLZTO纳米颗粒(LLZTO@GPTMS)在有机溶剂中均匀分散。粒度分布实验表明,LLZTO纳米颗粒的分散性与溶剂的极性呈正相关。采用均匀分散的LLZTO悬浮液,制备的PEO:LLZTO复合电解质的室温离子电导率可以达到2.31×10^(-4)S·cm^(-1)。使用优化后的PEO:LLZTO@GPTMS电解质组装的锂对称电池以及以LiFePO_(4)(LFP)为正极、金属锂为负极的SSLBs均表现出更长的循环寿命。此外,GPTMS的修饰有助于LLZTO纳米颗粒在聚乙烯(Polyethylene,PE)隔膜上的均匀涂覆。采用LLZTO@GPTMS涂覆PE隔膜的LFP|Li电池比采用未修饰LLZTO涂覆PE隔膜的电池展现出更优异的循环稳定性。结果表明,GPTMS能够有效提高LLZTO纳米颗粒在有机溶剂和聚合物基质中的分散性,对其他有机-无机复合材料体系具有指导意义。

关键词：固态锂电池石榴石型电解质复合固体电解质硅烷偶联剂纳米粉体分散

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Heterogeneous electrolyte membranes enabling double-side stable interfaces for solid lithium batteries

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Journal of Energy Chemistry 2021年第9期30卷 162-168页

作者： Shuang Mu Weilin Huang Wuhui Sun Ning Zhao Mengyang Jia Zhijie Bi xiangxin guo College of Physics Qingdao UniversityQingdao 266071ShandongChina

The solid polymer electrolyte(SPE) is one of the most promising candidates for building solid lithium batteries with high energy density and safety due to its advantages of flexibility and light-weight.However,the conventional monolayered electrolytes usually exhibit unstable contacts with either high-voltage cathodes or Li-metal anodes during cell operation.Herein,heterogeneous dual-layered electrolyte membranes(HDEMs) consisting of the specific functional polymer matrixes united with the designed solid ceramic fillers are constructed to address the crucial issues of interfacial instability.The electrolyte layers composed of the high-conductivity and oxidation-resistance polyacrylonitrile(PAN) combined with Li_(0.33)La_(0.557)TiO_(3) nanofibers are in contact with the high-voltage cathodes,achieving the compatible interface between the cathodes and the electrolytes.Meanwhile,the electrolyte layers composed of the highstability and dendrite-resistance polyethylene oxide(PEO) with Li_(6.4)La_(3) Zr_(1.4)Ta_(0.6)O_(12) nanoparticles are in contact with the Li-metal anodes,aiming to suppress the dendrite growth,as well as avoid the passivation between the PAN and the Li-metal.Consequently,the solid LiNi_(0.6)Co_(0.2)Mn_(0.2)O2‖Li full cells based on the designed HDEMs show the good rate and cycling performance,i.***.the discharge capacity of 170.1 mAh g^(-1) with a capacity retention of 78.2% after 100 cycles at 0.1 C and 30℃.The results provide an effective strategy to construct the heterogeneous electrolyte membranes with double-side stable electrode/-electrolyte interfaces for the high-voltage and dendrite-free solid lithium batteries.

关键词： Solid electrolytes High-voltage cathodes Dendrite suppression Solid lithium batteries

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Sandwiched N-carbon@Co_(9)S_(8)@Graphene nanosheets as high capacity anode for both half and full lithium-ion batteries

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Journal of Energy Chemistry 2020年第12期29卷 62-71页

作者： Ningning Li Li Sun Kai Wana Sheng Xu Jun Zhang xiangxin guo Xianghong Liu College of Physics Qingdao UniversityQingdao 266071ShandongChina Key Laboratory of Advanced Energy Materials Chemistry(Ministry of Education) Nankai UniversityTianjin 300071China

Transition metal sulfides(TMSs) are promising candidates for replacing graphite anode in LIBs. However,the low conductivity and structural collapse caused by the large volume change during lithium insertion and extraction greatly limit its application. Herein, we report a unique design of a two-dimensional(2 D) sandwich structure of N-doped carbon@Co9 S8@graphene(N–C@Co9 S8@G) with multilayer structure. Electrochemical tests reveal that the N–C@Co9 S8@G nanosheets possess a high reversible capacity(1009 mAhg^(-1) at 0.1 Ag^(-1)), and excellent rate capability(422mAhg^(-1) at 10 Ag^(-1)) and long cycle life(853 m Ahg^(-1) at 1Ag^(-1) for 500 cycles). Experimental studies reveal that capacitive storage contributes to the high reversible capacity. The lithium storage kinetics are studied by Galvanostatic intermittent titration technique(GITT) and electrochemical impedance spectroscopy(EIS). Meanwhile, the potential of N–C@Co9 S8@G anode in a full cell using Li Co O2 as the cathode is also demonstrated, exhibiting a high reversible capacity of 300mAhg^(-1) cycles at 0.1Ag^(-1). The strategy proposed in this work paves the way to engineering high performance anodes in LIBs.

关键词： Cobalt sulfides Graphene Sandwich structure Anode Lithium-ion batteries

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Multilayered structure of N-carbonenvelopediron oxide/graphene nanocomposites as an improved anode for Li-ion battery

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Chinese Chemical Letters 2020年第9期31卷 2333-2338页

作者： Li Sun Kai Wang Ningning Li Jun Zhang xiangxin guo Xianghong Liu College of Physics Qingdao UniversityQingdao 266071China Key Laboratory of Advanced Energy Materials Chemistry(Ministry of Education) Nankai UniversityTianjin 300071China

Transition metal oxides with high capacity are considered a promising electrode material for lithium-ion batteries(LIBs).Nevertheless,the huge volume expansion and poor conductivity severely hamper their practical application.In this work,a carbon riveting method is reported to address the above issues by designing multilayered N-doped carbon(N-carbon) enveloped Fe3O4/graphene nanosheets.When evaluated as a negative electrode,the N-carbon/Fe3O4/graphene nanocomposites demonstrate greatly enhanced electrochemical properties compared with Fe3O4/graphene.The N-carbon/Fe3O4/graphene presents a superior reversible capacity(807 mAh/g) over Fe3O4/graphene(540 mAh/g).Furthermore,it affords a considerable capacity of 550 mAh/g at 1 A/g over 700 cycles,indicating supe rb cycling stability.The structure-property correlation studies reveal that the carbon riveting layer is essential for enhancing the lithium diffusion kinetics.The good electrochemical properties and effective structure design make the carbon riveting strategy quite general and reliable to manipulate high performance electrodes for future LIBs.

关键词： Fe3O4 Nanosheet N-doped carbon Anode Lithium-ion batteries

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