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Title: Review of Recent Development of in situ/operando Characterization Techniques for Lithium Battery Research

Abstract

The increasing demands on energy storage requires significant improvement of current Li-ion battery electrode materials and development of advanced electrode materials. This necessitates in-depth understanding of the reaction processes, degradation mechanism, and thermal decomposition mechanisms of electrode materials under realistic operation conditions. This can be achieved by in situ/operando characterization techniques that provide information of the structure evolution, redox mechanism, solid-electrolyte interphase (SEI) formation, side reactions and Li-ion transport properties under operating conditions. In this review, recent progress of in situ/operando techniques employed for the investigation of the structural stability, dynamic properties, chemical environment changes and morphological evolution during electrochemical processes are described and summarized in detail. The experimental approaches reviewed in this paper include X-ray, Electron, Neutron, Optical, and Scanning probes. Each advanced technique has unique capabilities to study specific properties of electrode materials within specific limitations. The experimental methods and operating principles, and especially the in situ cell designs are described in detail. To illustrate the possibilities of each technique representative studies making use of these in situ/operando techniques are discussed and summarized. Finally, the major current challenges and future opportunities of the in situ/operando techniques are outlined. Several important battery challenges are anticipated to profit from thesemore » in situ/operando techniques, including the inhomogeneous reactions of high energy density cathodes, the development of safe and reversible Li metal plating and the development of stable SEI on electrodes.« less

Authors:
 [1];  [1];  [1];  [1];  [1];  [1];  [1];  [2];  [1]; ORCiD logo [3];  [3];  [3];  [4];  [5];  [5];  [5];  [6]
  1. Tsinghua Univ., Shenzhen (China). Engineering Lab. for the Next Generation Power and Energy Storage Batteries, Graduate School at Shenzhen
  2. Tsinghua Univ., Shenzhen (China). Engineering Lab. for the Next Generation Power and Energy Storage Batteries, Graduate School at Shenzhen; Tsinghua Univ., Shenzhen (China). Nano Energy Materials Lab. (NEM), Tsinghua-Berkeley Shenzhen Inst. (TBSI)
  3. Brookhaven National Lab. (BNL), Upton, NY (United States). Chemistry Dept.
  4. Tsinghua Univ., Shenzhen (China). Nano Energy Materials Lab. (NEM), Tsinghua-Berkeley Shenzhen Inst. (TBSI)
  5. Delft Univ. of Technology (Netherlands). Dept. of Radiation Science and Technology
  6. Hong Kong Polytechnic Univ. (Hong Kong)
Publication Date:
Research Org.:
Brookhaven National Laboratory (BNL), Upton, NY (United States)
Sponsoring Org.:
USDOE Office of Energy Efficiency and Renewable Energy (EERE), Vehicle Technologies Office (EE-3V); National Nature Science Foundation of China (NNSFC); USDOE
OSTI Identifier:
1507700
Alternate Identifier(s):
OSTI ID: 1513307
Report Number(s):
BNL-211557-2019-JAAM
Journal ID: ISSN 0935-9648
Grant/Contract Number:  
SC0012704; DE‐SC0012704
Resource Type:
Accepted Manuscript
Journal Name:
Advanced Materials
Additional Journal Information:
Journal Volume: 31; Journal Issue: 28; Journal ID: ISSN 0935-9648
Publisher:
Wiley
Country of Publication:
United States
Language:
English
Subject:
25 ENERGY STORAGE; characterization techniques; in situ-operando; lithium battery

Citation Formats

Liu, Dongqing, Qian, K., Li, H., Wang, S.W., Yu, Q. P., Qin, X.Y., Yang, Q.-H., Kang, F.Y., Li, B. H., Shadike, Zulipiya, Lin, R. Q., Yang, X.-Q., Qian, K., Liu, M., Ganapathy, S., Wagemaker, M., and Li, K. K. Review of Recent Development of in situ/operando Characterization Techniques for Lithium Battery Research. United States: N. p., 2019. Web. doi:10.1002/adma.201806620.
Liu, Dongqing, Qian, K., Li, H., Wang, S.W., Yu, Q. P., Qin, X.Y., Yang, Q.-H., Kang, F.Y., Li, B. H., Shadike, Zulipiya, Lin, R. Q., Yang, X.-Q., Qian, K., Liu, M., Ganapathy, S., Wagemaker, M., & Li, K. K. Review of Recent Development of in situ/operando Characterization Techniques for Lithium Battery Research. United States. https://doi.org/10.1002/adma.201806620
Liu, Dongqing, Qian, K., Li, H., Wang, S.W., Yu, Q. P., Qin, X.Y., Yang, Q.-H., Kang, F.Y., Li, B. H., Shadike, Zulipiya, Lin, R. Q., Yang, X.-Q., Qian, K., Liu, M., Ganapathy, S., Wagemaker, M., and Li, K. K. Tue . "Review of Recent Development of in situ/operando Characterization Techniques for Lithium Battery Research". United States. https://doi.org/10.1002/adma.201806620. https://www.osti.gov/servlets/purl/1507700.
@article{osti_1507700,
title = {Review of Recent Development of in situ/operando Characterization Techniques for Lithium Battery Research},
author = {Liu, Dongqing and Qian, K. and Li, H. and Wang, S.W. and Yu, Q. P. and Qin, X.Y. and Yang, Q.-H. and Kang, F.Y. and Li, B. H. and Shadike, Zulipiya and Lin, R. Q. and Yang, X.-Q. and Qian, K. and Liu, M. and Ganapathy, S. and Wagemaker, M. and Li, K. K.},
abstractNote = {The increasing demands on energy storage requires significant improvement of current Li-ion battery electrode materials and development of advanced electrode materials. This necessitates in-depth understanding of the reaction processes, degradation mechanism, and thermal decomposition mechanisms of electrode materials under realistic operation conditions. This can be achieved by in situ/operando characterization techniques that provide information of the structure evolution, redox mechanism, solid-electrolyte interphase (SEI) formation, side reactions and Li-ion transport properties under operating conditions. In this review, recent progress of in situ/operando techniques employed for the investigation of the structural stability, dynamic properties, chemical environment changes and morphological evolution during electrochemical processes are described and summarized in detail. The experimental approaches reviewed in this paper include X-ray, Electron, Neutron, Optical, and Scanning probes. Each advanced technique has unique capabilities to study specific properties of electrode materials within specific limitations. The experimental methods and operating principles, and especially the in situ cell designs are described in detail. To illustrate the possibilities of each technique representative studies making use of these in situ/operando techniques are discussed and summarized. Finally, the major current challenges and future opportunities of the in situ/operando techniques are outlined. Several important battery challenges are anticipated to profit from these in situ/operando techniques, including the inhomogeneous reactions of high energy density cathodes, the development of safe and reversible Li metal plating and the development of stable SEI on electrodes.},
doi = {10.1002/adma.201806620},
journal = {Advanced Materials},
number = 28,
volume = 31,
place = {United States},
year = {Tue Apr 30 00:00:00 EDT 2019},
month = {Tue Apr 30 00:00:00 EDT 2019}
}

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Studying the Kinetics of Crystalline Silicon Nanoparticle Lithiation with In Situ Transmission Electron Microscopy
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Reversible Nanopore Formation in Ge Nanowires during Lithiation–Delithiation Cycling: An In Situ Transmission Electron Microscopy Study
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Direct Mapping of Charge Distribution during Lithiation of Ge Nanowires Using Off-Axis Electron Holography
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Nanovoid Formation and Annihilation in Gallium Nanodroplets under Lithiation–Delithiation Cycling
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Leapfrog Cracking and Nanoamorphization of ZnO Nanowires during In Situ Electrochemical Lithiation
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Revealing the conversion mechanism of CuO nanowires during lithiation–delithiation by in situ transmission electron microscopy
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In Situ Transmission Electron Microscopy Study of Electrochemical Lithiation and Delithiation Cycling of the Conversion Anode RuO 2
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Transitions from Near-Surface to Interior Redox upon Lithiation in Conversion Electrode Materials
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Real-time Observation of Deep Lithiation of Tungsten Oxide Nanowires by In Situ Electron Microscopy
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Atomistic Conversion Reaction Mechanism of WO 3 in Secondary Ion Batteries of Li, Na, and Ca
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Strain Coupling of Conversion-type Fe 3 O 4 Thin Films for Lithium Ion Batteries
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Study on the Electrochemical Reaction Mechanism of ZnFe2O4 by In Situ Transmission Electron Microscopy
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In situ TEM observation of the structural transformation of rutile TiO 2 nanowire during electrochemical lithiation
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In Situ Transmission Electron Microscopy Observation of Electrochemical Behavior of CoS 2 in Lithium-Ion Battery
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In Situ Observation of Divergent Phase Transformations in Individual Sulfide Nanocrystals
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High-Resolution Tracking Asymmetric Lithium Insertion and Extraction and Local Structure Ordering in SnS 2
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In Situ Investigations of Li-MoS 2 with Planar Batteries
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In Situ Study of Lithiation and Delithiation of MoS 2 Nanosheets Using Electrochemical Liquid Cell Transmission Electron Microscopy
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Lithiation-Induced Shuffling of Atomic Stacks
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In Situ TEM Observation of Local Phase Transformation in a Rechargeable LiMn 2 O 4 Nanowire Battery
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Phase Transitions in a LiMn 2 O 4 Nanowire Battery Observed by Operando Electron Microscopy
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In Situ Atomic-Scale Imaging of Phase Boundary Migration in FePO 4 Microparticles During Electrochemical Lithiation
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In Situ Observation of Random Solid Solution Zone in LiFePO 4 Electrode
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Asynchronous Crystal Cell Expansion during Lithiation of K + -Stabilized α-MnO 2
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The influence of large cations on the electrochemical properties of tunnel-structured metal oxides
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Direct characterization of the Li intercalation mechanism into α-V 2 O 5 nanowires using in-situ transmission electron microscopy
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Controlling the Lithiation-Induced Strain and Charging Rate in Nanowire Electrodes by Coating
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The effect of metallic coatings and crystallinity on the volume expansion of silicon during electrochemical lithiation/delithiation
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Surface-Coating Regulated Lithiation Kinetics and Degradation in Silicon Nanowires for Lithium Ion Battery
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Mesoscale Origin of the Enhanced Cycling-Stability of the Si-Conductive Polymer Anode for Li-ion Batteries
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Sandwich-Lithiation and Longitudinal Crack in Amorphous Silicon Coated on Carbon Nanofibers
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Lithiation of SiO 2 in Li-Ion Batteries: In Situ Transmission Electron Microscopy Experiments and Theoretical Studies
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Dynamics of Electrochemical Lithiation/Delithiation of Graphene-Encapsulated Silicon Nanoparticles Studied by In-situ TEM
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Tailoring Lithiation Behavior by Interface and Bandgap Engineering at the Nanoscale
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A Yolk-Shell Design for Stabilized and Scalable Li-Ion Battery Alloy Anodes
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In Situ TEM Study of Lithiation Behavior of Silicon Nanoparticles Attached to and Embedded in a Carbon Matrix
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Engineering Heteromaterials to Control Lithium Ion Transport Pathways
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Interconnected hollow carbon nanospheres for stable lithium metal anodes
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Lithium Electrodeposition Dynamics in Aprotic Electrolyte Observed in Situ via Transmission Electron Microscopy
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Observation and Quantification of Nanoscale Processes in Lithium Batteries by Operando Electrochemical (S)TEM
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Nanoscale Imaging of Fundamental Li Battery Chemistry: Solid-Electrolyte Interphase Formation and Preferential Growth of Lithium Metal Nanoclusters
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Direct Observation of Li-Ion Transport in Electrodes under Nonequilibrium Conditions Using Neutron Depth Profiling
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In Situ Neutron Depth Profiling: A Powerful Method to Probe Lithium Transport in Micro-Batteries
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Operando Neutron Depth Profiling to Determine the Spatial Distribution of Li in Li-ion Batteries
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Gas Evolution in Operating Lithium-Ion Batteries Studied In Situ by Neutron Imaging
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Probing Multiscale Transport and Inhomogeneity in a Lithium-Ion Pouch Cell Using In Situ Neutron Methods
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In situ visualization of the electrolyte solvent filling process by neutron radiography
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The LiMn2O4 to λ-MnO2 phase transition studied by in situ neutron diffraction
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A New Null Matrix Electrochemical Cell for Rietveld Refinements of In-Situ or Operando Neutron Powder Diffraction Data
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Circular in situneutron powder diffraction cell for study of reaction mechanism in electrode materials for Li-ion batteries
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New in-situ neutron diffraction cell for electrode materials
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An In-Situ Electrochemical Cell for Neutron Diffraction Studies of Phase Transitions in Small Volume Electrodes of Li-Ion Batteries
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In-situ neutron diffraction study of the MoS2 anode using a custom-built Li-ion battery
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A Cylindrical Cell for Operando Neutron Diffraction of Li-Ion Battery Electrode Materials
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A custom battery for operando neutron powder diffraction studies of electrode structure
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Visualizing the chemistry and structure dynamics in lithium-ion batteries by in-situ neutron diffraction
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Neutron depth profiling of Li-ion cell electrodes with a gas-controlled environment
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Nano-morphology of lithiated thin film TiO2 anatase probed with in situ neutron reflectometry
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Lithium Migration in Li 4 Ti 5 O 12 Studied Using in Situ Neutron Powder Diffraction
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Correlating cycling history with structural evolution in commercial 26650 batteries using in operando neutron powder diffraction
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Structural changes in a commercial lithium-ion battery during electrochemical cycling: An in situ neutron diffraction study
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In-situ observation of inhomogeneous degradation in large format Li-ion cells by neutron diffraction
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Degradation analysis of 18650-type lithium-ion cells by operando neutron diffraction
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In operando neutron diffraction study of a commercial graphite/(Ni, Mn, Co) oxide-based multi-component lithium ion battery
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Understanding structural changes in NMC Li-ion cells by in situ neutron diffraction
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The Origin of Capacity Fade in the Li 2 MnO 3 ·Li M O 2 ( M = Li, Ni, Co, Mn) Microsphere Positive Electrode: An Operando Neutron Diffraction and Transmission X-ray Microscopy Study
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Low-temperature performance of Li-ion batteries: The behavior of lithiated graphite
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Lithium plating in lithium-ion batteries at sub-ambient temperatures investigated by in situ neutron diffraction
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Demonstrating the Feasibility of Al as Anode Current Collector in Li-Ion Batteries via In Situ Neutron Depth Profiling
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Direct measurement of lithium transport in graphite electrodes using neutrons
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In Situ Raman Study on Single- and Double-Walled Carbon Nanotubes as a Function of Lithium Insertion
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Copper-Coated Amorphous Silicon Particles as an Anode Material for Lithium-Ion Batteries
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Evolution of the electrochemical interface in sodium ion batteries with ether electrolytes
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In situ and Operando Raman Spectroscopy of Layered Transition Metal Oxides for Li-ion Battery Cathodes
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Investigations on Electrochemical Behavior and Structural Stability of Li 1.2 Mn 0.54 Ni 0.13 Co 0.13 O 2 Lithium-Ion Cathodes via in-Situ and ex-Situ Raman Spectroscopy
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In situ Raman microspectrometry investigation of electrochemical lithium intercalation into sputtered crystalline V2O5 thin films
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Lithium Insertion in Channel-Structured β-AgVO 3 : In Situ Raman Study and Computer Simulation
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A Catalytic Path for Electrolyte Reduction in Lithium-Ion Cells Revealed by in Situ Attenuated Total Reflection-Fourier Transform Infrared Spectroscopy
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In-operando FTIR Spectroscopy for Composite Electrodes of Lithium-ion Batteries
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In-Situ Spectro-electrochemical Insight Revealing Distinctive Silicon Anode Solid Electrolyte Interphase Formation in a Lithium-ion Battery
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Lithiation Mechanism of Methylated Amorphous Silicon Unveiled by Operando ATR-FTIR Spectroscopy
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In Situ Observation of Electrolyte-Concentration-Dependent Solid Electrolyte Interphase on Graphite in Dimethyl Sulfoxide
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Facet dependent SEI formation on the LiNi 0.5 Mn 1.5 O 4 cathode identified by in situ single particle atomic force microscopy
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In Situ and Operando Investigations of Failure Mechanisms of the Solid Electrolyte Interphase on Silicon Electrodes
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Single Nanowire Electrode Electrochemistry of Silicon Anode by in Situ Atomic Force Microscopy: Solid Electrolyte Interphase Growth and Mechanical Properties
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In-situ investigation of solid-electrolyte interphase formation on the anode of Li-ion batteries with Atomic Force Microscopy
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Effect of sulfur-containing additives on the formation of a solid-electrolyte interphase evaluated by in situ AFM and ex situ characterizations
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In situ quantification of interphasial chemistry in Li-ion battery
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Combined AFM/SECM Investigation of the Solid Electrolyte Interphase in Li-Ion Batteries
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In situ and operando atomic force microscopy of high-capacity nano-silicon based electrodes for lithium-ion batteries
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Enhanced Lithiation Cycle Stability of ALD-Coated Confined a-Si Microstructures Determined Using In Situ AFM
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A Flexible Solid Electrolyte Interphase Layer for Long-Life Lithium Metal Anodes
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In Situ Visualized Cathode Electrolyte Interphase on LiCoO 2 in High Voltage Cycling
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Elucidating the Phase Transformation of Li 4 Ti 5 O 12 Lithiation at the Nanoscale
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Scanning Electrochemical Microscopy: A Comprehensive Review of Experimental Parameters from 1989 to 2015
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Review—Advances in Scanning Electrochemical Microscopy (SECM)
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Scanning electrochemical microscopy of Li-ion batteries
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Do imaging techniques add real value to the development of better post-Li-ion batteries?
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In situ Raman spectroscopy of LiFePO 4 : size and morphology dependence during charge and self-discharge
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Works referencing / citing this record:

Understanding the cathode electrolyte interface formation in aqueous electrolyte by scanning electrochemical microscopy
journal, January 2019

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Unraveling the Formation of Amorphous MoS 2 Nanograins during the Electrochemical Delithiation Process
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