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Electrolyte-dependent formation of solid electrolyte interphase and ion intercalation revealed by in situ surface characterizations

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Journal of Energy Chemistry 2022年第4期31卷 718-726页

作者： Shiwen Li Chao Wang caixia meng Yanxiao Ning Guohui Zhang Qiang Fu State Key Laboratory of Catalysis iChEMDalian Institute of Chemical PhysicsChinese Academy of SciencesDalian 116023LiaoningChina University of Chinese Academy of Sciences Beijing 100049China Dalian National Laboratory for Clean Energy Dalian Institute of Chemical PhysicsChinese Academy of SciencesDalian 116023LiaoningChina

The formation of solid electrolyte interphase(SEI) and ion intercalation are two key processes in rechargeable batteries, which need to be explored under dynamic operating conditions. In this work, both planar and sandwich model lithium batteries consisting of Li metal | ionic liquid electrolyte | graphite electrode have been constructed and investigated by a series of in situ surface analysis platforms including atomic force microscopy, Raman and X-ray photoelectron spectroscopy. It is found that the choice of electrolyte, including the concentration and contents, has a profound effect on the SEI formation and evolution, and the subsequent ion intercalation. A smooth and compact SEI is preferably produced in highconcentration electrolytes, with FSI^(-) salt superior to TFSI^(-) salt, facilitating the lithiation/delithiation to achieve high capacity and excellent cycle stability, while suppressing the co-intercalation of electrolyte solvent ions. The innovative research scenario of well-defined model batteries in combination with multiple genuinely in situ surface analysis methods presented herein leads to insightful results, which provide valuable strategies for the rational design and optimization of practical batteries, and energy storage devices in general.

关键词： Lithium ion batteries Solid electrolyte interphase Ion intercalation In situ surface characterization Ionic liquid electrolyte

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Visualizing surface-enriched Li storage with a nanopore-array model battery

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Nano Research 2023年第4期16卷 5026-5032页

作者： Shiwen Li Guohui Zhang Chao Wang caixia meng Xianjin Li Yanxiao Ning Qiang Fu State Key Laboratory of Catalysis iChEMDalian Institute of Chemical PhysicsChinese Academy of SciencesDalian 116023China University of Chinese Academy of Sciences Beijing 100049China Department of Chemical Physics University of Science and Technology of ChinaHefei 230026China Dalian National Laboratory for Clean Energy Dalian Institute of Chemical PhysicsChinese Academy of SciencesDalian 116023China

The coupling of model batteries and surface-sensitive techniques provides an indispensable platform for interrogating the vital surface/interface processes in battery systems.Here,we report a sandwich-format nanopore-array model battery using an ultrathin graphite electrode and an anodized aluminum oxide(AAO)film.The porous framework of AAO regulates the contact pattern of the electrolyte with the graphite electrode from the inner side,while minimizing contamination on the outer surface.This model battery facilitates repetitive charge-discharge processes,where the graphite electrode is reversibly intercalated and deintercalated,and also allows for the in-situ characterizations of ion intercalation in the graphite electrode.The ion distribution profiles indicate that the intercalating Li ions accumulate in both the inner and outer surface regions of graphite,generating a high capacity of~455 mAh·g^(-1)(theory:372 mAh·g^(-1)).The surface enrichment presented herein provides new insights towards the mechanistic understanding of batteries and the rational design strategies.

关键词： lithium ion batteries nanopore-array model battery in-situ surface characterization techniques ion intercalation surface enrichment effect

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Revealing the effect of electrolyte coordination structures on the intercalation chemistry of batteries

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Journal of Energy Chemistry 2023年第6期81卷 149-156,I0006页

作者： Chao Wang Xianjin Li Guiming Zhong caixia meng Shiwen Li Guohui Zhang Yanxiao Ning Xianfeng Li Qiang Fu State Key Laboratory of Catalysis iChEMDalian Institute of Chemical PhysicsChinese Academy of SciencesDalian 116023LiaoningChina University of Chinese Academy of Sciences Beijing 100049China Department of Chemical Physics University of Science and Technology of ChinaHefei 230026AnhuiChina Laboratory of Advanced Spectro-electrochemistry and Li-ion Batteries Dalian Institute of Chemical Physics Chinese Academy of SciencesDalian116023LiaoningChina Division of Energy Storage Dalian National Laboratory for Clean Energy Dalian Institute of Chemical PhysicsChinese Academy of SciencesDalian 116023LiaoningChina Dalian National Laboratory for Clean Energy Dalian Institute of Chemical Physics Chinese Academy of SciencesDalian 116023LiaoningChina

In-depth understanding of the electrolyte-dependent intercalation chemistry in batteries through direct operando/in situ characterizations is crucial for the development of the high-performance batteries.Herein,taking the Al/graphite battery as a model system,the effect of electrolyte coordination structure on the intercalation processes has been investigated over the batteries with either 1-hexyl-3-methylimidazolium chloride(HMICl)-AlCl_(3) or 1-ethyl-3-methylimidazolium chloride(EMICl)-AlCl_(3) ionic liquid electrolyte using operando X-ray photoelectron spectroscopy(XPS)and X-ray diffraction.With a weaker anion-cation interaction in HMI-based electrolyte,the XPS-derived atomic ratio between cointercalated N and intercalated Al is 0.9,which is lower than 1.6 for EMI-based electrolyte.Attributed to the additional de-solvation process,the batteries with the HMI-based electrolyte show a lower ionic diffusion rate,capacity,and cycling performance,which agree with the operando characterization results.Our findings highlight the critical role of the electrolyte coordination structure on the(co-)intercalation chemistry.

关键词： Operando surface characterization Electrolyte coordination structure De-solvation Intercalation chemistry

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Low-temperature and high-voltage planar micro-supercapacitors based on anti-freezing hybrid gel electrolyte

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Journal of Energy Chemistry 2022年第9期31卷 195-202,I0006页

作者： Manning Chen Xiaoyu Shi Xiaolei Wang Hanqing Liu Sen Wang caixia meng Yu Liu Liangzhu Zhang Yuanyuan Zhu Zhong-Shuai Wu College of Chemistry and Environment Shenyang University of TechnologyShenyang 110870LiaoningChina State Key Laboratory of Catalysis Dalian Institute of Chemical PhysicsChinese Academy of SciencesDalian 116023LiaoningChina University of Chinese Academy of Sciences Beijing 100049China Dalian National Laboratory for Clean Energy Chinese Academy of SciencesDalian 116023LiaoningChina

Micro-supercapacitors(MSCs)are considered as highly competitive power sources for miniaturized electronics.However,narrow voltage window and poor anti-freezing properties of MSCs in conventional aqueous electrolytes lead to low energy density and limited environmental adaption.Herein,we report the construction of low-temperature and high-energy-density MSCs based on anti-freezing hybrid gel electrolytes(HGE)through introducing ethylene glycol(EG)additives into aqueous LiCl electrolyte.Since EG partially destroys hydrogen bond network among water molecules,the HGE exhibits maximum electrochemical stability window of 2.7 V and superior anti-freezing features with a glass transition temperature of-62.8℃.Further,the optimized MSCs using activated carbon microelectrodes possess impressive volumetric capacitance of 28.9 F cm^(-3)and energy density of 10.3 mWh cm^(-3)in the voltage of 1.6 V,2.6 times higher than MSCs tested in 1.2 V.Importantly,the MSCs display 68.3%capacitance retention even at-30℃ compared to the value at 25℃,and ultra-long cyclability with 85.7%of initial capacitance after 15,000 times,indicating extraordinary low-temperature performance.Besides,our devices offer favorable flexibility and modular integration.Therefore,this work provides a general strategy of realizing flexible,safe and anti-freezing microscale power sources,holding great potential towards subzero-temperature microelectronic applications.

关键词： Hybrid gel electrolyte Micro-supercapacitors Low temperature High voltage Graphene

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Intercalation-etching of graphene on Pt(111) in H_2 and O_2 observed by in-situ low energy electron microscopy

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中国科学：化学英文版 2017年第5期60卷 656-662页

作者： Wei Wei caixia meng Qiang Fu Xinhe Bao Department of Chemical Physics University of Science and Technology of China State Key Laboratory of Catalysis iChEM Dalian Institute of Chemical Physics the Chinese Academy of Sciences

Graphene layers are often exposed to gaseous environments in their synthesis and application processes, and interactions of graphene surfaces with molecules particularly H_2 and O_2 are of great importance in their physico-chemical properties. In this work, etching of graphene overlayers on Pt(111) in H_2 and O_2 atmospheres were investigated by in-situ low energy electron microscopy. Significant graphene etching was observed in 10^(-5) Torr H_2 above 1023 K, which occurs simultaneously at graphene island edges and interiors with a determined reaction barrier at 5.7 eV. The similar etching phenomena were found in 10.7 Torr O_2 above 973 K, while only island edges were reacted between 823 and 923 K. We suggest that etching of graphene edges is facilitated by Pt-aided hydrogenation or oxidation of edge carbon atoms while intercalation-etching is attributed to etching at the interiors at high temperatures. The different findings with etching in O_2 and H_2 depend on competitive adsorption, desorption, and diffusion processes of O and H atoms on Pt surface, as well as intercalation at the graphene/Pt interface.

关键词： graphene etching intercalation LEEM oxidation hydrogenation

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Step-confined thin film growth via near-surface atom migration

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Nano Research 2020年第6期13卷 1552-1557页

作者： caixia meng Junfeng Gao Rongtan Li Yanxiao Ning Yuan Chang Rentao Mu Qiang Fu Xinhe Bao State Key Laboratory of Catalysis Dalian Institute of Chemical PhysicsChinese Academy of SciencesDalian116023China University of Chinese Academy of Sciences Beijing100039China Key Laboratory of Materials Modification by Laser Ion and Electron BeamsDalian University of TechnologyMinistry of EducationDalian116024China University of Science and Technology of China Hefei230026China

Understanding of thin film growth mechanism is crucial for tailoring film growth behaviors,which in turn determine physicochemical properties of the resulting films.Here,vapor-growth of tungsten carbide overlayers on W(110)surface is investigated by real time low energy electron microscopy.The surface growth is strongly confined by surface steps,which is in contrast with overlayer growth crossing steps in a so-called carpet-like growth mode for example in graphene growth on metal surfaces.Density functional theory calculations indicate that the step-confined growth is caused by the strong interaction of the forming carbide overlayer with the substrate blocking cross-step growth of the film.Furthermore,the tungsten carbide growth within each terrace is facilitated by the supply of carbon atoms from near-surface regions at high temperatures.These findings suggest the critical role of near-surface atom diffusion and step confinement effects in the thin film growth,which may be active in many film growth systems.

关键词： thin film growth tungsten carbide near-surface dopant low-energy electron microscopy(LEEM) step confinement

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Pt@h-BN core-shell fuel electrocatalysis confined cell electrocatalysts wit under outer shells

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Nano Research 2018年第6期11卷 3490-3498页

作者： mengmeng Sun Jinchao Dong Yang Lv Siqin Zhao caixia meng Yujiang Song Guoxiong Wang Jianfeng Li Qiang Fu Zhongqun Tian Xinhe Bao State Key Laboratory of Catalysis iChEM Dalian Institute of Chemical Physics Chinese Academy of Sciences Dalian 116023 China University of Chinese Academy of Sciences Beijing 100049 China MOE Key Laboratory of Spectrochemical Analysis and Instrumentation State Key Laboratory of Physical Chemistry of Solid Surfaces iChEM College of Chemistry and Chemical Engineering Xiamen University Xiamen 361005 China State Key Laboratory of Fine Chemicals School of Chemical Engineering Dalian University of Technology Dalian 116024 China

Two-dimensional （2D） materials such as graphene and hexagonal boron nitride （h-BN） can be used as robust and flexible encapsulation overlayers, which effectively protect metal cores but allow reactions to occur between inner cores and outer shells. Here, we demonstrate this concept by showing that Pt@h-BN core-shell nanocatalysts present enhanced performances in H2/O2 fuel cells. Electrochemical （EC） tests combined with operando EC-Raman characterizations were performed to monitor the reaction process and its intermediates, which confirm that Pt-catalyzed electrocatalytic processes happen under few-layer h-BN covers. The confinement effect of the h-BN shells prevents Pt nanoparticles from aggregating and helps to alleviate the CO poisoning problem. Accordingly, embedding nanocatalysts within ultrathin 2D material shells can be regarded as an effective route to design high-performance electrocatalysts.

关键词： electrocatalysis two-dimensional materials core-shell confinement catalysis operando Raman

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改进YOLOv5s的铁路异物入侵检测算法

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小型微型计算机系统 2024年第4期45卷 879-886页

作者：孟彩霞王兆楠石磊高宇飞卫琳郑州大学计算机与人工智能学院郑州450001 郑州大学网络空间安全学院郑州450002 铁道警察学院图像与网络侦查系郑州450053

行人、车辆等异物侵入铁路界线,严重威胁行人安全和铁路交通安全.针对传统铁路异物入侵检测方法精度低、时效性差等问题,提出改进YOLOv5s算法的铁路异物入侵检测模型SD-YOLO.本文提出SSA混合注意力机制,加强模型的局部表征能力,提高小... 详细信息

行人、车辆等异物侵入铁路界线,严重威胁行人安全和铁路交通安全.针对传统铁路异物入侵检测方法精度低、时效性差等问题,提出改进YOLOv5s算法的铁路异物入侵检测模型SD-YOLO.本文提出SSA混合注意力机制,加强模型的局部表征能力,提高小目标识别效果;提出DW-Decoupled Head解耦检测头,加快网络收敛速度;引入边界框回归损失函数SIoU,提高了模型的检测精度;使用转置卷积作为采样方法,采样更适合铁路侵限障碍物特征的尺寸和比例.在数据集RS和Pascal VOC 2012进行实验验证,与基线YOLOv5s算法相比,平均精度mAP@0.5分别提高了2.7%、1.8%,mAP@.5:.95分别提高了2.9%、2.1%,检测速度分别达到79 FPS和78 FPS,表明该算法在检测精度和速度上均取得良好的性能,有效改善了漏检、误检问题,提高了小目标识别能力.

关键词：铁路入侵检测混合注意力机制解耦头损失函数上采样

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Creating one-line hybrid crops by synthetic apomixis

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Molecular Plant 2024年第1期17卷 16-18页

作者： Ronghong Liang caixia Gao New Cornerstone Science Laboratory Center for Genome EditingInstitute of Genetics and Developmental BiologyChinese Academy of SciencesBeijing100101China College of Advanced Agricultural Sciences University of Chinese Academy of SciencesBeijing100049China

Hybrid breeding plays an important role in increasing crop yields by taking advantage of hybrid vigor,which helps crops grow with superior yields across various climates and contributes to ensuring secure food production.Hybrid seed production is relatively straightforward and simple in cross-pollinating plants such as maize but is difficult in self-pollinating plants such as rice,wheat,and soybean.Therefore,breeders have developed a three-line breeding strategy,utilizing a sterile line,a maintainer line,and a restorer line,for breeding hybrid rice(Figure 1A;Yuan,1966).

关键词： breeding crops sterile

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Self assembled electron blocking and lithiophilic interface towards dendrite-free solid-state lithium battery

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Chinese Chemical Letters 2024年第4期35卷 220-225页

作者： caixia Li Yi Qiu Yufeng Zhao Wuliang Feng Institute for Sustainable Energy&College of Sciences Shanghai UniversityShanghai 200444China Key Laboratory of Advanced Energy Materials Chemistry(Ministry of Education) Nankai UniversityTianjin 300071China

The poor interfacial contact is one of the biggest challenges that solid-state lithium batteries suffer from.Reducing the solid-state electrolyte surface energy by transforming the interface from lithiophobic to lithiophilic is effective to promote the interfacial contact, but electronic conductive interphases usually increase the risk of electron attack, thus leading to uncontrollable Li dendrite growth. Herein, we propose a self-assembled thermodynamic stable Li I interphase to simultaneously improve the interfacial contact between the garnet electrolyte Li_7La_(3)Zr_(2)O_(12)(LLZO) and Li anode, and prohibit the electron attack. The direct contact between LLZO and Li and the high temperature Li melting process was ascribed to Zr4+reduction, which facilitated Li dendrite formation and propagation. With the modification of the high lithiophilic I_(2) thin film, the area specific interfacial resistance of LLZO/Li was reduced from 1525 Ω/cm^(2) to 57 Ω/cm^(2). More importantly, LLZO was protected from being reduced due to the outstanding electronic insulativity of the Li I interphase, which leaded to a high critical current density of 1.2/7.0 m A/cm^(2) in the time/capacity-constant modes, respectively.

关键词： Li_7La_(3)Zr_(2)O_(12) LiI interphase Interfacial contact Li dendrite Thermodynamic stable

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