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Recent progress of in-situ characterization of LiNi_(1−x−y)Co_(x)Mn_(y)O_(2) cathodes for lithium metal batteries: A mini review

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Nano Research 2024年第3期17卷 1384-1401页

作者： Huanzhu Lv Xiaoqi Zhu Jun Mei Yuanhua Xia Bin Wang Institute of Fundamental and Frontier Science University of Electronic Science and Technology of ChinaChengdu 611731China Chengdu Development Center of Science and Technology China Academy of Engineering PhysicsChengdu 610200China Key Laboratory of Neutron Physics and Institute of Nuclear Physics and Chemistry China Academy of Engineering Physics(CAEP)Mianyang 621999China

In the context of the gradual popularity of electric vehicles(EVs),the development of lithium battery systems with high energy density and power density is regarded as the foremost way to improve the range of EVs.LiNi_(1-x-y)Co_(x)Mn_(y)O_(2)(NCM)cathodes have been the focus of researchers due to their high energy density,excellent power performance,and low-temperature resistance.However,the elaboration of the decay mechanism of NCM cathode based on lithium metal batteries(LMBs)is still being restricted to the primary level.In the past decades,the development and application of advanced in-situ characterization tools have facilitated researchers'understanding of the internal operation mechanism of batteries during charging and discharging.In this minireview,the latest progress of in-situ observation of the NCM cathode by X-ray diffraction(XRD),fourier transform infrared(FT-IR)spectroscopy,Raman spectroscopy,atomic force microscopy(AFM),transmission electron microscope(TEM),optical microscope,and other characterization tools is summarized.The mechanisms of structural degradation,cathode-electrolyte interfaces(CEIs)composition,and dynamic changes of NCM,electrolyte breakdown,and gas production are elaborated.Finally,based on the existing research progress,the opportunities and challenges for future in-situ characterization technology in the study of the mechanism of LMBs are discussed in depth.Therefore,the purpose of this minireview is to summarize recent work that focuses on the outstanding application of in-situ characterization techniques in the mechanistic study of LMBs,and pointing the way to the future development of high energy density and power density LMBs systems.

关键词： lithium metal batteries(LMBs) in-situ characterization LiNi_(1-x-y)Co_(x)Mn_(y)O_(2)(NCM)

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Pd-based nanocatalysts for oxygen reduction reaction:Preparation,performance,and in-situ characterization

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Chinese Journal of Structural Chemistry 2023年第11期42卷 55-68页

作者： Guan-Nan Xing Di-Ye Wei Hua Zhang Zhong-Qun Tian Jian-Feng Li College of Materials State Key Laboratory of Physical Chemistry of Solid SurfacesMOE Key Laboratory of Spectrochemical Analysis and InstrumentationCollege of Chemistry and Chemical EngineeringiChEMFujian Key Laboratory of Advanced MaterialsXiamen UniversityXiamen361005China Shenzhen Research Institute of Xiamen University Shenzhen518000China

Electrochemical energy devices such as fuel cells have received extensive concern in recent decades.However,the commercial applications of fuel cells have been restricted by the slow kinetics of oxygen reduction reaction(ORR).Pd-based fuel cell catalysts are strong candidates for enhanced ORR activities,especially under alkaline conditions.Therefore,extensive exploration has been made to improve the performance of Pd-based nano-catalysts for oxygen reduction reaction.This paper reviews the research progress of preparation,electrocatalytic performance,and in-situ characterization of various Pd-based oxygen reduction catalysts,from zero-dimensional nanoparticles,to one-dimensional nanowires,to two-dimensional nanosheets,and to Pd single-atom catalysts.It may provide some help for improving the activity of Pd-based catalysts and understanding the reaction mecha-nisms and structure-activity relationships.

关键词： Pd-based nanocatalyst Oxygen reduction reaction Electrocatalysis in-situ characterization

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Metal organic frameworks-based cathode materials for advanced Li-S batteries: A comprehensive review

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Nano Research 2024年第4期17卷 2592-2618页

作者： Zhengkun Xie Boyong Cao Xiyan Yue Ruixue Wang Ziqian Xue Jiajia Wang Guoqing Guan Weihua Chen College of Chemistry Zhengzhou UniversityZhengzhou 450001China School of Ecology and Environment Zhengzhou UniversityZhengzhou 450001China School of Materials Science and Engineering Henan Polytechnic UniversityJiaozuo 454003China Laboratory of Energy Conversion Engineering Institute of Regional InnovationHirosaki University3 Bunkyo-choHirosakiAomori 036-8561Japan Institute for Integrated Cell-Material Sciences(iCeMS) Kyoto UniversitySakyo-kuKyoto 606-8501Japan Key Laboratory of Advanced Energy Materials Chemistry(Ministry of Education) Nankai UniversityTianjin 300071China

Li-S batteries(LSBs)have been considering as new and promising energy storage systems because of the high theoretical energy density and low price.Nevertheless,their practical application is inhibited by several factors,including poor electrical conductivity of electrode materials,greatly volumetric variation,as well as the polysulfide formation upon the cycling.To address these problems,it is imperative to develop and design effective and suitable sulfur host anode materials.Metal organic frameworks(MOFs)-based cathode materials,possessing their good conductivity and easy morphology design,have been extensively studied and exhibited enormously potential in LSBs.In this review,a comprehensive overview of MOFs-based sulfur host materials is provided,including their electrochemical reaction mechanisms,related evaluation parameters,and their performances used in LSBs in the past few years.In particular,the recent advances using in-situ characterization technologies for investigating the electrochemical reaction mechanism in LSBs are presented and highlighted.Additionally,the challenges and prospects associated with future research on MOF-related sulfur host materials are discussed.It is anticipated to offer the guidance for the identification of suitable MOFs-based sulfur cathode materials for high-performance LSBs,thereby contributing for the achievement of a sustainable and renewable society.

关键词： lithium metal anode sulfur cathode metal organic frameworks host energy density in-situ characterization

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in-situ characterization of Non-aqueous Nano-dispersion Systems by Freeze-etching TEM and Comparative Study with Laser Scattering Method

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Journal of Wuhan University of Technology(Materials Science) 2010年第3期25卷 432-436页

作者：欧忠文 Department of Architecture and Civil Engineering Logistics Engineering University

in-situ characterization of non-aqueous nano-dispersion systems（NANDS） by freeze-etching transmission electron microscope（FETEM） was reported.To improve just-for-once successive rate of specimen preparation and get good characterization results,an improving specimen preparation method of freezing etching was developed.Size,distribution and morphology of NANDS were directly visualized.Some information of particle dispersion feature and particle density can also be obtained.Reproductivity of the FETEM characterization is excellent.Comparing with laser scattering method,which is liable to give positive error especially for small size particle anchoring disperser,FETEM characterization can give more accurate measurement of particle size.Moreover,FETEM can give dispersion feature of nanoparticle in non-aqueous medium.

关键词： non-aqueous nano-dispersion system dispersion state in-situ characterization freeze-etching laser scattering method

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Promotion effects of alkali metals on iron molybdate catalysts for CO_(2)catalytic hydrogenation

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Journal of Energy Chemistry 2023年第10期85卷 291-300,I0009页

作者： Yong Zhou Aliou Sadia Traore Deizi V.Peron Alan J.Barrios Sergei A.Chernyak Massimo Corda Olga V.Safonova Achim Iulian Dugulan Ovidiu Ersen Mirella Virginie Vitaly V.Ordomsky Andrei Y.Khodakov University of Lille CNRSCentrale LilleUniversity of ArtoisUMR 8181-UCCS-Unitéde Catalyse et Chimie du SolideLille F-59000France IPCMS UMR 7504 CNRSUniversitéde Strasbourg23 rue du LoessBP 43Cedex 267034 StrasbourgFrance PSI CH-5232 VilligenSwitzerland Fundamental Aspects of Materials and Energy Group Delft University of TechnologyMekelweg 15Delft 2629 JBNetherlands

CO_(2)hydrogenation is an attractive way to store and utilize carbon dioxide generated by industrial processes,as well as to produce valuable chemicals from renewable and abundant resources.Iron catalysts are commonly used for the hydrogenation of carbon oxides to hydrocarbons.Iron-molybdenum catalysts have found numerous applications in catalysis,but have been never evaluated in the CO_(2)hydrogenation.In this work,the structural properties of iron-molybdenum catalysts without and with a promoting alkali metal(Li,Na,K,Rb,or Cs)were characterized using X-ray diffraction,hydrogen temperatureprogrammed reduction,CO_(2)temperature-programmed desorption,in-situ^(57)Fe Mossbauer spectroscopy and operando X-ray adsorption spectroscopy.Their catalytic performance was evaluated in the CO_(2)hydrogenation.During the reaction conditions,the catalysts undergo the formation of an iron(Ⅱ)molybdate structure,accompanied by a partial reduction of molybdenum and carbidization of iron.The rate of CO_(2)conversion and product selectivity strongly depend on the promoting alkali metals,and electronegativity was identified as an important factor affecting the catalytic performance.Higher CO_(2)conversion rates were observed with the promoters having higher electronegativity,while low electronegativity of alkali metals favors higher light olefin selectivity.

关键词： CO_(2)utilization Iron molybdate catalysts Promotion Alkali metals Light olefins in-situ characterization

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Engineering Cu^(+)/CeZrO_(x) interfaces to promote CO_(2) hydrogenation to methanol

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Journal of Energy Chemistry 2023年第2期77卷 45-53,I0002页

作者： Jingpeng Zhang Xiaohang Sun Congyi Wu Wenquan Hang Xu Hu Dawei Qiao Binhang Yan Department of Chemical Engineering Tsinghua UniversityBeijing 100084China School of Science China University of GeosciencesBeijing 10084China Jiangsu Huadian Jurong Power Station Co.LTD Zhenjiang 212000JiangsuChina

Cu-based catalysts are widely employed for CO_(2) hydrogenation to methanol,which is expected as a promising process to achieving carbon neutrality.However,most Cu-based catalysts still suffer from low methanol yield with a passable CO_(2) conversion and lack insight into its reaction mechanism for guiding the design of catalysts.In this work,Cu^(+)/CeZrO_(x) interfaces are engineered by employing a series of ceria-zirconia solid solution catalysts with various Ce/Zr ratios,forming a Cu^(+)-O_(v)-Ce^(3+)structure where Cu^(+)atoms are bonded to the oxygen vacancies(O_(v))of ceria.Compared to Cu/CeO_(2) and Cu/ZrO_(2),the optimized catalyst(i.e.,Cu_(0.3)Ce_(0.3)Zr_(0.7))exhibits a much higher mass-specific methanol formation rate(192g_(MeOH)/kg_(cat)/h)at 240℃and 3 MPa.Through a series of in-situ and ex-situ characterization,it is revealed that oxygen vacancies in solid solutions can effectively assist the activation of CO_(2) and tune the electronic state of copper to promote the formation of Cu^(+)/CeZrO_(x) interfaces,which stabilizes the key*CO intermediate,inhibits its desorption and facilitates its further hydrogenation to methanol via the reverse watergas-shift(RWGS)+CO-Hydro pathway.Therefore,the concentration of*CO or the apparent Cu^(+)/(Cu^(+)+Cu^(0))ratio could be employed as a quantitative descriptor of the methanol formation rate.This work is expected to give a deep insight into the mechanism of metal/support interfaces in CO_(2) hydrogenation to methanol,offering an effective strategy to develop new catalysts with high performance.

关键词： CO_(2)hydrogenation Methanol synthesis in-situ characterization Cu^(+)/CeZrO_(x)interfaces Oxygen vacancies

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Plasmonic Core-Shell Nanostructures Enhanced Spectroscopies

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Chinese Journal of Chemistry 2022年第3期40卷 392-406页

作者： Jun Zhou Di-Ye Wei Yu-Jin Zhang Hua Zhang Jian-Feng Li State Key Laboratory of Physical Chemistry of Solid Surfaces College of Chemistry and Chemical EngineeringCollege of MaterialsCollege of EnergyFujian Key Laboratory of Advanced MaterialsXiamen UniversityXiamenFujian 361005China College of Optical and Electronic Technology China Jiliong UniversityHangzhouZhejiang 310018China

Core-shell nanostructures constituted by a plasmonic core and an ultrathin shell have drawn enormous attentions in enhanced spectroscopies,catalysis,energy,and other fields because of their splendid properties such as multifunctionality,stability,and adjustability.In this article,we summarized the endeavors made by our group in the past decade about the core-shell nanostructures in the shell-isolated nanoparticle-enhanced Raman spectroscopy(SHINERS)and plasmon-enhanced spectroscopies.Meanwhile,the potential challenges and perspectives about core-shell nanostructures in spectroscopies have also been proposed.Thus,we believe this article would provide an avenue for a comprehensive understanding of enhanced spectroscopies with core-shell nanostructures.

关键词： Raman spectroscopy Nanostructures Electrochemistry Heterogeneous catalysis in-situ characterization

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In-situ/operando techniques to identify active sites for thermochemical conversion of CO_(2) over heterogeneous catalysts

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Journal of Energy Chemistry 2021年第11期30卷 153-171,I0004页

作者： Kai Feng Yaning Wang Man Guo Jingpeng Zhang Zhengwen Li Tianyu Deng Zhihe Zhang Binhang Yan Department of Chemical Engineering Tsinghua UniversityBeijing 100084China

The catalytic conversion of CO_(2) to fuels or chemicals is considered to be an effective pathway to mitigate the greenhouse effect. To develop new types of efficient and durable catalysts, it is critical to identify the catalytic active sites, surface intermediates, and reaction mechanisms to reveal the relationship between the active sites and catalytic performance. However, the structure of a heterogeneous catalyst usually dynamically changes during reaction, bringing a great challenge for the identification of catalytic active sites and reaction pathways. Therefore, in-situ/operando techniques have been employed to real-time monitor the dynamic evolution of the structure of active sites under actual reaction conditions to precisely build the structure–function relationship. Here, we review the recent progress in the application of various in-situ/operando techniques in identifying active sites for catalytic conversion of CO_(2) over heterogeneous catalysts. We systematically summarize the applications of various optical and X-ray spectroscopy techniques, including Raman spectroscopy, Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and X-ray absorption spectroscopy (XAS), in identifying active sites and determining reaction mechanisms of the CO_(2) thermochemical conversion with hydrogen and light alkanes over heterogeneous catalysts. Finally, we discuss challenges and opportunities for the development of in-situ characterization in the future to further enlarge the capability of these powerful techniques.

关键词： in-situ characterization Spectroscopy techniques Active sites CO_(2)conversion Heterogeneous catalysis

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Ordered lithium ion channels of covalent organic frameworks with lithiophilic groups enable uniform and efficient Li plating/stripping

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Journal of Energy Chemistry 2021年第10期30卷 135-140,I0004页

作者： Xuyan Ni Jie Liu Haoqing Ji Libao Chen Tao Qian Chenglin Yan College of Energy Key Laboratory for Advanced Carbon Materials and Wearable Energy Technologies of Jiangsu ProvinceSoochow UniversitySuzhou 215006JiangsuChina State Key Laboratory for Powder Metallurgy Central South UniversityChangsha 410083HunanChina Light Industry Institute of Electrochemical Power Sources Suzhou 215006JiangsuChina

Covalent organic frameworks(COFs)are a kind of materials composed of organic blocks linked through robust covalent bonds[1,2].In these materials,the organic blocks are integrated into symmetric structures that extend infinitely under the guidance of topological diagram,founded by periodic skeletons and nanopores[3-5].On account of the extensive building blocks,variety of topology design diagram and the variety of linkages,various COFs with different functionalities can be designed and synthesized for versatile applications.

关键词： Lithium metal anodes Lithiophilic covalent organic frameworks Dendrite-free in-situ characterization

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