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

Journal Article · · Advanced Materials
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  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)
+ Show Author Affiliations

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.

Research Organization:
Brookhaven National Laboratory (BNL), Upton, NY (United States)
Sponsoring Organization:
USDOE Office of Energy Efficiency and Renewable Energy (EERE), Vehicle Technologies Office (EE-3V); National Nature Science Foundation of China (NNSFC); USDOE
Grant/Contract Number:
SC0012704; DE‐SC0012704
OSTI ID:
1507700
Alternate ID(s):
OSTI ID: 1513307
Report Number(s):
BNL-211557-2019-JAAM
Journal Information:
Advanced Materials, Vol. 31, Issue 28; ISSN 0935-9648
Publisher:
WileyCopyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 304 works
Citation information provided by
Web of Science

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Low-temperature performance of Li-ion batteries: The behavior of lithiated graphite journal May 2015
Lithium plating in lithium-ion batteries at sub-ambient temperatures investigated by in situ neutron diffraction journal December 2014
Demonstrating the Feasibility of Al as Anode Current Collector in Li-Ion Batteries via In Situ Neutron Depth Profiling journal January 2016
Irreversible lithium storage during lithiation of amorphous silicon thin film electrodes studied by in-situ neutron reflectometry journal August 2017
Solid Electrolyte Interphase in Li-Ion Batteries: Evolving Structures Measured In situ by Neutron Reflectometry journal May 2012
Neutron Imaging of Lithium Concentration in LFP Pouch Cell Battery journal January 2011
Expansion of Lithium Ion Pouch Cell Batteries: Observations from Neutron Imaging journal January 2013
Direct measurement of lithium transport in graphite electrodes using neutrons journal April 2012
Raman Microspectrometry Applied to the Study of Electrode Materials for Lithium Batteries journal March 2010
In situ methods for Li-ion battery research: A review of recent developments journal August 2015
Memoir on inventing the confocal scanning microscope journal January 1988
In situ Raman spectroscopic–electrochemical studies of lithium-ion battery materials: a historical overview journal October 2013
In Situ Raman Study on Electrochemical Li Intercalation into Graphite journal January 1995
In situ Roman Study of Electrochemical Lithium Insertion into Mesocarbon Microbeads Heat-Treated at Various Temperatures journal January 1996
A transmission electron microscopy study of crack formation and propagation in electrochemically cycled graphite electrode in lithium-ion cells journal October 2011
An in situ Raman study of the intercalation of supercapacitor-type electrolyte into microcrystalline graphite journal October 2006
Design and comparison of ex situ and in situ devices for Raman characterization of lithium titanate anode material journal April 2011
In Situ Raman Study on Single- and Double-Walled Carbon Nanotubes as a Function of Lithium Insertion journal May 2006
Modified Coin Cells for In situ Raman Spectroelectrochemical Measurements of Li x V 2 O 5 for Lithium Rechargeable Batteries journal May 2006
Li + -Ion Extraction/Insertion of Ni-Rich Li 1+ x (Ni y Co z Mn z ) w O 2 (0.005< x <0.03; y : z =8:1, w ≈1) Electrodes: In Situ XRD and Raman Spectroscopy Study journal July 2015
In situ measurement of lithiation-induced stress in silicon nanoparticles using micro-Raman spectroscopy journal April 2016
Development of In Situ Cross-Sectional Raman Imaging of LiCoO<sub>2</sub> Cathode for Li-ion Battery journal January 2015
In Situ, Time-Resolved Raman Spectromicrotopography of an Operating Lithium-Ion Battery journal January 2004
Time and/or space resolved laser Raman spectroscopy journal January 1982
Raman microprobe and microscope with laser excitation journal February 1975
Correlations between structural and electrical properties of BaCeO3 studied by coupled in-situ Raman scattering and impedance spectroscopy journal June 1995
Raman Spectroelectrochemistry of a Lithium/Polymer Electrolyte Symmetric Cell journal January 1998
In situ surface enhanced Raman spectroscopic studies of solid electrolyte interphase formation in lithium ion battery electrodes journal June 2014
In situ Raman spectroscopy of carbon-coated ZnFe 2 O 4 anode material in Li-ion batteries – investigation of SEI growth journal January 2016
In Situ, Real-Time Raman Microscopy of Embedded Single Particle Graphite Electrodes journal January 2002
Lithium Insertion into Anatase Nanotubes journal November 2012
Ultrafast-Charging and Long-Life Li-Ion Battery Anodes of TiO 2 -B and Anatase Dual-Phase Nanowires journal October 2017
Copper-Coated Amorphous Silicon Particles as an Anode Material for Lithium-Ion Batteries journal March 2012
In situ Raman microscopy during discharge of a high capacity silicon–carbon composite Li-ion battery negative electrode journal January 2009
Large Impact of Particle Size on Insertion Reactions. A Case for Anatase Li x TiO 2 journal April 2007
Evolution of the electrochemical interface in sodium ion batteries with ether electrolytes journal February 2019
Length-Scale-Dependent Phase Transformation of LiFePO 4 : An In situ and Operando Study Using Micro-Raman Spectroscopy and XRD journal June 2015
Advanced in situ methods for the characterization of practical electrodes in lithium-ion batteries journal September 2000
In situ Raman spectroscopic studies of electrochemical intercalation in LixMn2O4-based cathodes journal September 1999
Application of Operando X-ray Diffraction and Raman Spectroscopies in Elucidating the Behavior of Cathode in Lithium-Ion Batteries journal July 2018
In situ and Operando Raman Spectroscopy of Layered Transition Metal Oxides for Li-ion Battery Cathodes journal August 2018
Direct Visualization of the Reversible O 2− /O − Redox Process in Li-Rich Cathode Materials journal February 2018
Label-Free Biomedical Imaging with High Sensitivity by Stimulated Raman Scattering Microscopy journal December 2008
Operando and three-dimensional visualization of anion depletion and lithium growth by stimulated Raman scattering microscopy journal July 2018
Electrochemical cycling behaviour of lithium carbonate (Li2CO3) pre-treated graphite anodes – SEI formation and graphite damage mechanisms journal October 2014
In Situ Study of Li Intercalation into Highly Crystalline Graphitic Flakes of Varying Thicknesses journal October 2016
Studying lithium intercalation into graphite particles via in situ Raman spectroscopy and confocal microscopy journal August 2004
Dopant Modulated Li Insertion in Si for Battery Anodes: Theory and Experiment journal August 2011
Electrochemical lithium insertion into anatase-type TiO2: An in situ Raman microscopy investigation journal May 2007
Investigation of effects of carbon coating on the electrochemical performance of Li4Ti5O12/C nanocomposites journal January 2013
In situ Raman spectroscopic study of LixCoO2 electrodes in propylene carbonate solvent systems journal October 1997
Spectroelectrochemical studies on highly polarized LiCoO2 electrode in organic solutions journal November 2000
Visualization of the State-of-Charge Distribution in a LiCoO 2 Cathode by In Situ Raman Imaging journal January 2013
Raman spectro-electrochemistry of LiCoxMn2−xO4 thin film electrodes for 5 V lithium batteries journal April 2004
In situ Raman spectroscopic studies of LiNi x Mn 2 − x O 4 thin film cathode materials for lithium ion secondary batteries journal January 2002
In Situ Raman Microscopy of Individual LiNi 0.8 Co 0.15 Al 0.05 O 2 Particles in a Li-Ion Battery Composite Cathode journal January 2005
Electrochemical activation of Li2MnO3 at elevated temperature investigated by in situ Raman microscopy journal October 2013
High energy xLi2MnO3–(1−x)LiNi2/3Co1/6Mn1/6O2 composite cathode for advanced Li-ion batteries journal January 2015
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 journal June 2014
In situ Raman microspectrometry investigation of electrochemical lithium intercalation into sputtered crystalline V2O5 thin films journal November 2009
Lithium Insertion in Channel-Structured β-AgVO 3 : In Situ Raman Study and Computer Simulation journal November 2007
Controlling Electrochemical Lithiation/Delithiation Reaction Paths for Long-cycle Life Nanochain-structured FeS2 Electrodes journal September 2016
Characterization of a model solid electrolyte interphase/carbon interface by combined in situ Raman/Fourier transform infrared microscopy journal September 2013
Infrared Spectroscopy journal January 1996
In-Situ Infrared Spectroscopic Studies of Electrochemical Energy Conversion and Storage journal December 2011
Solvation and Dynamics of Lithium Ions in Carbonate-Based Electrolytes during Cycling Followed by Operando Infrared Spectroscopy: The Example of NiSb 2 , a Typical Negative Conversion-Type Electrode Material for Lithium Batteries journal November 2017
Spectroscopic Insight into Li-Ion Batteries during Operation: An Alternative Infrared Approach journal November 2015
A Catalytic Path for Electrolyte Reduction in Lithium-Ion Cells Revealed by in Situ Attenuated Total Reflection-Fourier Transform Infrared Spectroscopy journal February 2015
In-operando FTIR Spectroscopy for Composite Electrodes of Lithium-ion Batteries journal January 2015
In Situ FTIR Spectroscopy Study of Li/LiNi[sub 0.8]Co[sub 0.15]Al[sub 0.05]O[sub 2] Cells with Ionic Liquid-Based Electrolytes in Overcharge Condition journal January 2010
Dynamic in situ fourier transform infrared measurements of chemical bonds of electrolyte solvents during the initial charging process in a Li ion battery journal December 2013
Combined In Situ Raman and IR Microscopy at the Interface of a Single Graphite Particle with Ethylene Carbonate/Dimethyl Carbonate journal January 2014
In-Situ Spectro-electrochemical Insight Revealing Distinctive Silicon Anode Solid Electrolyte Interphase Formation in a Lithium-ion Battery journal March 2016
Lithiation Mechanism of Methylated Amorphous Silicon Unveiled by Operando ATR-FTIR Spectroscopy journal January 2018
In-situ Fourier transform infrared spectroscopic analysis on dynamic behavior of electrolyte solution on LiFePO4 cathode journal October 2013
In Situ DRIFTS Analysis of Solid-Electrolyte Interphase Formation on Li-Rich Li 1.2 Ni 0.2 Mn 0.6 O 2 and LiCoO 2 Cathodes during Oxidative Electrolyte Decomposition journal November 2015
Nanoscale Measurements of Lithium-Ion-Battery Materials using Scanning Probe Techniques journal November 2016
Looking at cell mechanics with atomic force microscopy: Experiment and theory: CELL MECHANICS WITH AFM journal August 2014
Progress of electrode/electrolyte interfacial investigation of Li-ion batteries via in situ scanning probe microscopy journal May 2015
Direct Observation of Inhomogeneous Solid Electrolyte Interphase on MnO Anode with Atomic Force Microscopy and Spectroscopy journal January 2012
In Situ and Quantitative Characterization of Solid Electrolyte Interphases journal February 2014
In Situ AFM Study of Surface Film Formation on the Edge Plane of HOPG for Lithium-Ion Batteries journal December 2011
In Situ AFM Imaging of Solid Electrolyte Interfaces on HOPG with Ethylene Carbonate and Fluoroethylene Carbonate-Based Electrolytes journal November 2015
Direct Visualization of Nucleation and Growth Processes of Solid Electrolyte Interphase Film Using in Situ Atomic Force Microscopy journal June 2017
In Situ Observation of Electrolyte-Concentration-Dependent Solid Electrolyte Interphase on Graphite in Dimethyl Sulfoxide journal April 2015
Facet dependent SEI formation on the LiNi 0.5 Mn 1.5 O 4 cathode identified by in situ single particle atomic force microscopy journal January 2014
In Situ and Operando Investigations of Failure Mechanisms of the Solid Electrolyte Interphase on Silicon Electrodes journal September 2016
Single Nanowire Electrode Electrochemistry of Silicon Anode by in Situ Atomic Force Microscopy: Solid Electrolyte Interphase Growth and Mechanical Properties journal October 2014
In-situ investigation of solid-electrolyte interphase formation on the anode of Li-ion batteries with Atomic Force Microscopy journal November 2014
Effect of sulfur-containing additives on the formation of a solid-electrolyte interphase evaluated by in situ AFM and ex situ characterizations journal January 2017
In situ quantification of interphasial chemistry in Li-ion battery journal November 2018
Combined AFM/SECM Investigation of the Solid Electrolyte Interphase in Li-Ion Batteries journal May 2015
In situ and operando atomic force microscopy of high-capacity nano-silicon based electrodes for lithium-ion batteries journal January 2016
Enhanced Lithiation Cycle Stability of ALD-Coated Confined a-Si Microstructures Determined Using In Situ AFM journal January 2016
Real-Time Observation of Li Deposition on a Li Electrode with Operand Atomic Force Microscopy and Surface Mechanical Imaging journal February 2017
A Flexible Solid Electrolyte Interphase Layer for Long-Life Lithium Metal Anodes journal January 2018
In Situ Visualized Cathode Electrolyte Interphase on LiCoO 2 in High Voltage Cycling journal May 2017
Nanoscale Mapping of Lithium-Ion Diffusion in a Cathode within an All-Solid-State Lithium-Ion Battery by Advanced Scanning Probe Microscopy Techniques journal January 2013
In situ studies of lithium-ion diffusion in a lithium-rich thin film cathode by scanning probe microscopy techniques journal January 2015
Elucidating the Phase Transformation of Li 4 Ti 5 O 12 Lithiation at the Nanoscale journal March 2016
Scanning Electrochemical Microscopy: A Comprehensive Review of Experimental Parameters from 1989 to 2015 journal October 2016
Review—Advances in Scanning Electrochemical Microscopy (SECM) journal December 2015
Scanning electrochemical microscopy of Li-ion batteries journal January 2015
In situ visualization of Li-ion intercalation and formation of the solid electrolyte interphase on TiO2 based paste electrodes using scanning electrochemical microscopy journal January 2013
Spatiotemporal Changes of the Solid Electrolyte Interphase in Lithium-Ion Batteries Detected by Scanning Electrochemical Microscopy journal July 2014
Comparison of Electron Transfer Properties of the SEI on Graphite Composite and Metallic Lithium Electrodes by SECM at OCP journal January 2015
In Situ Quantification of the Swelling of Graphite Composite Electrodes by Scanning Electrochemical Microscopy journal October 2015
Layer Number Dependence of Li + Intercalation on Few-Layer Graphene and Electrochemical Imaging of Its Solid–Electrolyte Interphase Evolution journal March 2016
Understanding surface reactivity of Si electrodes in Li-ion batteries by in operando scanning electrochemical microscopy journal January 2016
Scanning Electrochemical Microscopy Applied to the Investigation of Lithium (De-)Insertion in TiO 2 journal March 2015
Solid Electrolyte Interphase (SEI) at TiO 2 Electrodes in Li-Ion Batteries: Defining Apparent and Effective SEI Based on Evidence from X-ray Photoemission Spectroscopy and Scanning Electrochemical Microscopy journal January 2017
In situ electrochemical studies for Li+ ions dissociation from the LiCoO2 electrode by the substrate-generation/tip-collection mode in SECM journal February 2011
Rapid SECM probing of dissolution of LiCoO2 battery materials in an ionic liquid journal November 2012
Determination of the formation and range of stability of the SEI on glassy carbon by local electrochemistry journal January 2015
In-operando evaluation of the effect of vinylene carbonate on the insulating character of the solid electrolyte interphase journal September 2015
Scanning Electrochemical Microscopy for the In Situ Characterization of Solid-Electrolyte Interphases: Highly Oriented Pyrolytic Graphite versus Graphite Composite journal June 2016
Investigation of the Electron Transfer at Si Electrodes: Impact and Removal of the Native SiO 2 Layer journal December 2015
Lithium Ion Quantification Using Mercury Amalgams as in Situ Electrochemical Probes in Nonaqueous Media journal October 2014
Do imaging techniques add real value to the development of better post-Li-ion batteries? journal January 2018
In situ Raman spectroscopy of LiFePO 4 : size and morphology dependence during charge and self-discharge journal September 2013
Development and evaluation of in-situ instrumentation for cylindrical Li-ion cells using fibre optic sensors journal April 2018
Advances in Understanding Materials for Rechargeable Lithium Batteries by Atomic Force Microscopy journal March 2018
Scanning electrochemical microscopy at the nanometer level journal January 2018
Reviving the lithium metal anode for high-energy batteries journal March 2017
Electrolytes and Interphases in Li-Ion Batteries and Beyond journal October 2014
State-of-the-art characterization techniques for advanced lithium-ion batteries journal March 2017
Sustainability and in situ monitoring in battery development journal December 2016
In Situ Quantification and Visualization of Lithium Transport with Neutrons journal July 2014
Quantifying microstructural dynamics and electrochemical activity of graphite and silicon-graphite lithium ion battery anodes text January 2016
Strain Coupling of Conversion‐type Fe 3 O 4 Thin Films for Lithium Ion Batteries journal May 2017
Rapid mapping of lithiation dynamics in transition metal oxide particles with operando X-ray absorption spectroscopy text January 2016
A Flexible Solid Electrolyte Interphase Layer for Long-Life Lithium Metal Anodes journal January 2018
Gas Evolution in Operating Lithium-Ion Batteries Studied in Situ by Neutron Imaging text January 2015
Combining operando synchrotron X-ray tomographic microscopy and scanning X-ray diffraction to study lithium ion batteries text January 2016

Cited By (3)

Application of Alternating Current Scanning Electrochemical Microscopy in Lithium‐Ion Batteries: Local Visualization of the Electrode Surface journal September 2019
Understanding the cathode electrolyte interface formation in aqueous electrolyte by scanning electrochemical microscopy journal January 2019
Unraveling the Formation of Amorphous MoS 2 Nanograins during the Electrochemical Delithiation Process journal August 2019

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25 ENERGY STORAGE
characterization techniques
in situ-operando
lithium battery