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Synchrotron X-ray Analytical Techniques for Studying Materials Electrochemistry in Rechargeable Batteries

Journal Article · · Chemical Reviews
 [1];  [2];  [3];  [4];  [5];  [5];  [6];  [7];  [4];  [8];  [9];  [10];  [2];  [7];  [4]
  1. Virginia Polytechnic Inst. and State Univ. (Virginia Tech), Blacksburg, VA (United States). Dept. of Chemistry
  2. SLAC National Accelerator Lab., Menlo Park, CA (United States). Stanford Synchrotron Radiation Lightsource (SSRL)
  3. Brookhaven National Lab. (BNL), Upton, NY (United States). Dept. of Chemistry; Chinese Academy of Sciences (CAS), Beijing (China). Inst. of Physics. Beijing National Lab. for Condensed Matter Physics (BNLCP-CAS)
  4. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Energy Storage and Distributed Resources Division
  5. Univ. of California, San Diego, CA (United States). Dept. of Physics
  6. Brookhaven National Lab. (BNL), Upton, NY (United States). Center for Functional Nanomaterials (CFN)
  7. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Advanced Light Source (ALS)
  8. Center for High Pressure Science & Technology Advanced Research, Shanghai (China)
  9. Brookhaven National Lab. (BNL), Upton, NY (United States). Dept. of Chemistry
  10. Univ. of California, San Diego, CA (United States). Dept. of NanoEngineering
+ Show Author Affiliations

Rechargeable battery technologies have ignited major breakthroughs in contemporary society, including but not limited to revolutions in transportation, electronics, and grid energy storage. The remarkable development of rechargeable batteries is largely attributed to in-depth efforts to improve battery electrode and electrolyte materials. There are, however, still intimidating challenges of lower cost, longer cycle and calendar life, higher energy density, and better safety for large scale energy storage and vehicular applications. Further progress with rechargeable batteries may require new chemistries (lithium ion batteries and beyond) and better understanding of materials electrochemistry in the various battery technologies. In the past decade, advancement of battery materials has been complemented by new analytical techniques that are capable of probing battery chemistries at various length and time scales. Synchrotron X-ray techniques stand out as one of the most effective methods that allows for nearly nondestructive probing of materials characteristics such as electronic and geometric structures with various depth sensitivities through spectroscopy, scattering, and imaging capabilities. This article begins with the discussion of various rechargeable batteries and associated important scientific questions in the field, followed by a review of synchrotron X-ray based analytical tools (scattering, spectroscopy and imaging) and their successful applications (ex situ, in situ, and in operando) in gaining fundamental insights into these scientific questions. Furthermore, electron microscopy and spectroscopy complement the detection length scales of synchrotron X-ray tools, and are also discussed towards the end. We highlight the importance of studying battery materials by combining analytical techniques with complementary length sensitivities, such as the combination of X-ray absorption spectroscopy and electron spectroscopy with spatial resolution, because a sole technique may lead to biased and inaccurate conclusions. We then discuss the current progress of experimental design for synchrotron experiments and methods to mitigate beam effects. Finally, a perspective is provided to elaborate how synchrotron techniques can impact the development of next-generation battery chemistries.

Research Organization:
Brookhaven National Laboratory (BNL), Upton, NY (United States). National Synchrotron Light Source II
Sponsoring Organization:
USDOE Office of Energy Efficiency and Renewable Energy (EERE), Vehicle Technologies Office (EE-3V); USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22); Chinese Academy of Sciences (CAS)
Grant/Contract Number:
SC0012704; SC0001805; AC02-76SF00515
OSTI ID:
1377367
Alternate ID(s):
OSTI ID: 1437475
OSTI ID: 1437973
OSTI ID: 1474323
Report Number(s):
BNL--114217-2017-JA; VT1201000
Journal Information:
Chemical Reviews, Journal Name: Chemical Reviews Journal Issue: 21 Vol. 117; ISSN 0009-2665
Publisher:
American Chemical SocietyCopyright Statement
Country of Publication:
United States
Language:
English

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  • Wiaderek, Kamila M.; Borkiewicz, Olaf J.; Castillo-Martínez, Elizabeth
  • Journal of the American Chemical Society, Vol. 135, Issue 10 https://doi.org/10.1021/ja400229v
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Lithium deintercalation in LiFePO4 nanoparticles via a domino-cascade model journal July 2008
Structure and bonding at the atomic scale by scanning transmission electron microscopy journal April 2009
The thermodynamic origin of hysteresis in insertion batteries journal April 2010
Direct imaging of hydrogen-atom columns in a crystal by annular bright-field electron microscopy journal February 2011
Kinetics of non-equilibrium lithium incorporation in LiFePO4 journal July 2011
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Reversible anionic redox chemistry in high-capacity layered-oxide electrodes journal July 2013
Origin of additional capacities in metal oxide lithium-ion battery electrodes journal November 2013
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Current-induced transition from particle-by-particle to concurrent intercalation in phase-separating battery electrodes journal September 2014
Direct mapping of Li-enabled octahedral tilt ordering and associated strain in nanostructured perovskites journal August 2015
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Anionic redox processes for electrochemical devices journal January 2016
Coherent lensless X-ray imaging journal November 2010
Nanoscale X-ray imaging journal December 2010
Determination of total x-ray absorption coefficient using non-resonant x-ray emission journal December 2011
In Situ Ambient Pressure X-ray Photoelectron Spectroscopy Studies of Lithium-Oxygen Redox Reactions journal October 2012
11 nm hard X-ray focus from a large-aperture multilayer Laue lens journal December 2013
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Unsupervised Data Mining in nanoscale X-ray Spectro-Microscopic Study of NdFeB Magnet journal September 2016
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In operando X-ray studies of the conversion reaction in Mn 3 O 4 lithium battery anodes journal January 2013
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Insitu nanotomography and operando transmission X-ray microscopy of micron-sized Ge particles journal January 2014
Profiling the nanoscale gradient in stoichiometric layered cathode particles for lithium-ion batteries journal January 2014
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In situ high-energy synchrotron X-ray diffraction studies and first principles modeling of α-MnO 2 electrodes in Li–O 2 and Li-ion coin cells journal January 2015
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Direct observation of the energetics at a semiconductor/liquid junction by operando X-ray photoelectron spectroscopy journal January 2015
Aqueous solution/metal interfaces investigated in operando by photoelectron spectroscopy journal January 2015
Future generations of cathode materials: an automotive industry perspective journal January 2015
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Li-alloy based anode materials for Li secondary batteries journal January 2010
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A new in situ synchrotron X-ray diffraction technique to study the chemical delithiation of LiFePO4 journal January 2011
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Multi-scale study of thermal stability of lithiated graphite journal January 2011
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Experimental visualization of lithium conduction pathways in garnet-type Li7La3Zr2O12 journal January 2012
High rate delithiation behaviour of LiFePO4 studied by quick X-ray absorption spectroscopy journal January 2012
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In situ chemical mapping of a lithium-ion battery using full-field hard X-ray spectroscopic imaging journal January 2013
Electronic structure of ions and molecules in solution: a view from modern soft X-ray spectroscopies journal January 2013
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Update on Na-based battery materials. A growing research path journal January 2013
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Full-field XANES analysis of Roman ceramics to estimate firing conditions—A novel probe to study hierarchical heterogeneous materials journal January 2013
Phase transition kinetics of LiNi0.5Mn1.5O4 electrodes studied by in situ X-ray absorption near-edge structure and X-ray diffraction analysis journal January 2013
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Quantitative X-ray projection microscopy: phase-contrast and multi-spectral imaging: QUANTITATIVE X-RAY PROJECTION MICROSCOPY journal August 2002
Synchrotron x‐ray diffraction studies of the structural properties of electrode materials in operating battery cells journal July 1996
A hard x-ray scanning microprobe for fluorescence imaging and microdiffraction at the advanced photon source conference January 2000
Kinetics of Phase Change. I General Theory journal December 1939
In situ x-ray absorption spectroscopic study of the Li[Ni1∕3Co1∕3Mn1∕3]O2 cathode material journal June 2005
Focusing of hard x-rays to 16 nanometers with a multilayer Laue lens journal June 2008
Plastic deformation in Al (Cu) interconnects stressed by electromigration and studied by synchrotron polychromatic x-ray microdiffraction journal July 2008
A dedicated superbend x-ray microdiffraction beamline for materials, geo-, and environmental sciences at the advanced light source journal March 2009
Solid and liquid spectroscopic analysis (SALSA)–a soft x-ray spectroscopy endstation with a novel flow-through liquid cell journal December 2009
A new white beam x-ray microdiffraction setup on the BM32 beamline at the European Synchrotron Radiation Facility journal March 2011
Applications of Hard X‐ray Full‐Field Transmission X‐ray Microscopy at SSRL conference January 2011
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A high resolution and large solid angle x-ray Raman spectroscopy end-station at the Stanford Synchrotron Radiation Lightsource journal April 2012
Fast microtomography using bright monochromatic x-rays journal September 2012
Role of joule heating effect and bulk-surface phases in voltage-driven metal-insulator transition in VO 2 crystal journal August 2013
Nanoscale strain mapping in battery nanostructures journal February 2014
Modular soft x-ray spectrometer for applications in energy sciences and quantum materials journal January 2017
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One hundred years of diffuse scattering journal July 2015
Experiments and Theory of In situ and Operando Soft X-ray Spectroscopy for Energy Storage journal September 2014
In situ synchrotron x-ray studies of battery and fuel cell materials journal May 1998
Atomic-resolution spectroscopic imaging of oxide interfaces journal December 2010
Recent advances in synchrotron-based hard x-ray phase contrast imaging journal November 2013
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Ordered subsets algorithms for transmission tomography journal October 1999
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New avenues in x-ray microbeam experiments journal February 2000
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Single-nanometer focusing of hard x-rays by Kirkpatrick–Baez mirrors journal September 2011
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Soft x-ray spectroscopy for probing electronic and chemical states of battery materials journal January 2016
Full-field transmission x-ray microscopy for bio-imaging journal September 2009
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Precision Method for Obtaining Absolute Values of Atomic Binding Energies journal March 1957
X-ray-absorption studies of organodisulfide redox polymeric electrodes journal March 1992
Determination of absorption coefficients for concentrated samples by fluorescence detection journal June 1993
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Beyond the ensemble average: X-ray microdiffraction analysis of single SiGe islands journal June 2008
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Direct Determination of the Chemical Bonding of Individual Impurities in Graphene journal November 2012
New Technique for Investigating Noncrystalline Structures: Fourier Analysis of the Extended X-Ray—Absorption Fine Structure journal November 1971
Band gaps and electronic structure of transition-metal compounds journal July 1985
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Three-Dimensional Imaging of Microstructure in Au Nanocrystals journal April 2003
Hard-X-Ray Lensless Imaging of Extended Objects journal January 2007
Extended x-ray absorption fine structure—its strengths and limitations as a structural tool journal October 1981
Theoretical approaches to x-ray absorption fine structure journal July 2000
Resonant inelastic x-ray scattering studies of elementary excitations journal June 2011
A Swagelok-type in situ cell for battery investigations using synchrotron radiation journal September 2005
The AMPIX electrochemical cell: a versatile apparatus for in situ X-ray scattering and spectroscopic measurements journal November 2012
Polychromatic X-ray microdiffraction studies of mesoscale structure and dynamics journal February 2005
Three-dimensional imaging of chemical phase transformations at the nanoscale with full-field transmission X-ray microscopy journal July 2011
TXM-Wizard : a program for advanced data collection and evaluation in full-field transmission X-ray microscopy journal January 2012
A hard X-ray nanoprobe beamline for nanoscale microscopy journal September 2012
The Bionanoprobe: hard X-ray fluorescence nanoprobe with cryogenic capabilities journal December 2013
Diffraction-limited storage rings – a window to the science of tomorrow journal August 2014
Pushing the limits: an instrument for hard X-ray imaging below 20 nm journal January 2015
Maximum Likelihood Reconstruction for Emission Tomography journal October 1982
LSO-Based Single Crystal Film Scintillator for Synchrotron-Based Hard X-Ray Micro-Imaging journal June 2009
Novel Fast Lithium Ion Conduction in Garnet-Type Li 5 La 3 M 2 O 12 (M = Nb, Ta) journal March 2003
Li6ALa2Nb2O12 (A=Ca, Sr, Ba): A New Class of Fast Lithium Ion Conductors with Garnet-Like Structure journal February 2005
Identifying and managing radiation damage during in situ transmission x-ray microscopy of Li-ion batteries conference September 2013
Prior image constrained compressed sensing (PICCS): A method to accurately reconstruct dynamic CT images from highly undersampled projection data sets: Prior image constrained compressed sensing (PICCS) journal January 2008
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Atomic-Scale Chemical Imaging of Composition and Bonding by Aberration-Corrected Microscopy journal February 2008
High-Resolution Scanning X-ray Diffraction Microscopy journal July 2008
In Situ Observation of the Electrochemical Lithiation of a Single SnO2 Nanowire Electrode journal December 2010
Visualization and Quantification of Electrochemical and Mechanical Degradation in Li Ion Batteries journal October 2013
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In situ visualization of Li/Ag2VP2O8 batteries revealing rate-dependent discharge mechanism journal January 2015
Topological defect dynamics in operando battery nanoparticles journal June 2015
Beyond crystallography: Diffractive imaging using coherent x-ray light sources journal April 2015
Cycling Li-O2 batteries via LiOH formation and decomposition journal October 2015
Visualization of O-O peroxo-like dimers in high-capacity layered oxides for Li-ion batteries journal December 2015
Origin and hysteresis of lithium compositional spatiodynamics within battery primary particles journal August 2016
Residual stress preserved in quartz from the San Andreas Fault Observatory at Depth journal February 2015
Handbook of Solid State Batteries and Capacitors book May 1995
Layered Cathode Materials Li[Ni[sub x]Li[sub (1/3−2x/3)]Mn[sub (2/3−x/3)]]O[sub 2] for Lithium-Ion Batteries journal January 2001
In Situ Investigation of Phase Transitions of Li[sub 1+y]Mn[sub 2]O[sub 4] Spinel during Li-Ion Extraction and Insertion journal January 2002
Li Conductivity in Li[sub x]MPO[sub 4] (M = Mn, Fe, Co, Ni) Olivine Materials journal January 2004
Reaction Mechanism of Tin Phosphide Anode by Mechanochemical Method for Lithium Secondary Batteries journal January 2004
Li-Storage via Heterogeneous Reaction in Selected Binary Metal Fluorides and Oxides journal January 2004
Synchrotron X-Ray Absorption Study of LiFePO[sub 4] Electrodes journal January 2005
Phospho-olivines as Positive-Electrode Materials for Rechargeable Lithium Batteries journal April 1997
Structural Evolution of Li[sub x]Mn[sub 2]O[sub 4] in Lithium-Ion Battery Cells Measured In Situ Using Synchrotron X-Ray Diffraction Techniques journal January 1998
Time-Resolved XRD Study on the Thermal Decomposition of Li[sub 1−x]Ni[sub 0.8]Co[sub 0.15]Al[sub 0.05]O[sub 2] Cathode Materials for Li-Ion Batteries journal January 2005
Degradation of Sodium β″‐Alumina: Effect of Microstructure journal May 1983
Electron Microscopy Study of the LiFePO[sub 4] to FePO[sub 4] Phase Transition journal January 2006
Electronic Structure of the Electrochemically Delithiated Li[sub 1−x]FePO[sub 4] Electrodes Investigated by P K-edge X-Ray Absorption Spectroscopy journal January 2006
Alloy Design for Lithium-Ion Battery Anodes journal January 2007
Si Electrodes for Li-Ion Batteries—A New Way to Look at an Old Problem journal January 2008
Silicon/Graphite Composite Electrodes for High-Capacity Anodes: Influence of Binder Chemistry on Cycling Stability journal January 2008
An Electrochemical Cell for Operando Study of Lithium Batteries Using Synchrotron Radiation journal January 2010
Surface Modification of Li-Excess Mn-based Cathode Materials journal January 2010
Morphological and Structural Studies of Composite Sulfur Electrodes upon Cycling by HRTEM, AFM and Raman Spectroscopy journal January 2010
Structural and Electrochemical Investigation of Li(Ni[sub 0.4]Co[sub 0.15]Al[sub 0.05]Mn[sub 0.4])O[sub 2] Cathode Material journal January 2010
Study of the Conversion Reaction Mechanism for Copper Borate as Electrode Material in Lithium-Ion Batteries journal January 2011
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Photoelectron Spectroscopy for Lithium Battery Interface Studies journal November 2015
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Phase Transition Analysis between LiFePO 4 and FePO 4 by In-Situ Time-Resolved X-ray Absorption and X-ray Diffraction journal January 2013
Review—Nano-Silicon/Carbon Composite Anode Materials Towards Practical Application for Next Generation Li-Ion Batteries journal January 2015
Review—Advances in Anode and Electrolyte Materials for the Progress of Lithium-Ion and beyond Lithium-Ion Batteries journal January 2015
Degradation Mechanism of LiNi 0.82 Co 0.15 Al 0.03 O 2 Positive Electrodes of a Lithium-Ion Battery by a Long-Term Cycling Test journal January 2014
An Electrochemical, Microtopographical and Ambient Pressure X-Ray Photoelectron Spectroscopic Investigation of Si/TiO 2 /Ni/Electrolyte Interfaces journal November 2015
A Critical Review of Li∕Air Batteries journal January 2012
Energy Dispersive X-ray Diffraction Profiling of Prototype LiMn 2 O 4 -Based Coin Cells journal January 2013
Review—Practical Challenges Hindering the Development of Solid State Li Ion Batteries journal January 2017
A General Discussion of Li Ion Battery Safety journal January 2012
A Review on the Structural Studies of Batteries and Host Materials by X-Ray Absorption Spectroscopy journal January 2013
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Emerging operando and x-ray pair distribution function methods for energy materials development journal March 2016
Materials Challenges Facing Electrical Energy Storage journal April 2008
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Non-invasive 3D-Visualization with Sub-micron Resolution Using Synchrotron-X-ray-tomography journal January 2008

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Rechargeable aqueous electrolyte batteries: from univalent to multivalent cation chemistry journal January 2019
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