Nanoscale Detection of Intermediate Solid Solutions in Equilibrated LixFePO4 Microcrystals

May, Brian M.; Yu, Young-Sang; Holt, Martin V.; Strobridge, Fiona C.; Boesenberg, Ulrike; Grey, Clare P.; Cabana, Jordi

doi:10.1021/acs.nanolett.7b03086

Title: Nanoscale Detection of Intermediate Solid Solutions in Equilibrated Li_xFePO₄ Microcrystals

Abstract

Redox-driven phase transformations in solids determine the performance of lithium-ion batteries, crucial in the technological transition from fossil fuels. Couplings between chemistry and strain define reversibility and fatigue of an electrode. The accurate definition of all phases in the transformation, their energetics, and nanoscale location within a particle produces fundamental understanding of these couplings needed to design materials with ultimate performance. In this paper we demonstrate that scanning X-ray diffraction microscopy (SXDM) extends our ability to image battery processes in single particles. In LiFePO₄ crystals equilibrated after delithiation, SXDM revealed the existence of domains of miscibility between LiFePO₄ and Li_0.6FePO₄. These solid solutions are conventionally thought to be metastable, and were previously undetected by spectromicroscopy. The observation provides experimental verification of predictions that the LiFePO₄–FePO₄ phase diagram can be altered by coherency strain under certain interfacial orientations. Finally, it enriches our understanding of the interaction between diffusion, chemistry, and mechanics in solid state transformations.

Authors:

May, Brian M. ^[1]; Yu, Young-Sang ^[2]; Holt, Martin V. ^[3]; Strobridge, Fiona C. ^[4]; Boesenberg, Ulrike ^[5];

^[4];

^[1]

Univ. of Illinois, Chicago, IL (United States). Dept. of Chemistry
Univ. of Illinois, Chicago, IL (United States). Dept. of Chemistry; Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Environmental Energy Technologies Division
Argonne National Lab. (ANL), Argonne, IL (United States). Center for Nanoscale Materials
Univ. of Cambridge (United Kingdom). Dept. of Chemistry
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Environmental Energy Technologies Division

Publication Date:: Wed Nov 22 00:00:00 EST 2017

Research Org.:: Argonne National Laboratory (ANL), Argonne, IL (United States); Univ. of Illinois, Chicago, IL (United States); Energy Frontier Research Centers (EFRC) (United States). Northeastern Center for Chemical Energy Storage (NECCES)

Sponsoring Org.:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

OSTI Identifier:: 1461313

Grant/Contract Number:: AC02-06CH11357; AC02-76SF00515; SC0012583

Resource Type:: Accepted Manuscript

Journal Name:: Nano Letters

Additional Journal Information:: Journal Volume: 17; Journal Issue: 12; Journal ID: ISSN 1530-6984

Publisher:: American Chemical Society

Country of Publication:: United States

Language:: English

Subject:: 25 ENERGY STORAGE; Li-ion battery materials; LiFePO4; nanoscale chemical imaging; redox phase transitions

Citation Formats


                    May, Brian M., Yu, Young-Sang, Holt, Martin V., Strobridge, Fiona C., Boesenberg, Ulrike, Grey, Clare P., and Cabana, Jordi. Nanoscale Detection of Intermediate Solid Solutions in Equilibrated LixFePO4 Microcrystals.  United States: N. p., 2017. 
Web.  doi:10.1021/acs.nanolett.7b03086.

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                    May, Brian M., Yu, Young-Sang, Holt, Martin V., Strobridge, Fiona C., Boesenberg, Ulrike, Grey, Clare P., & Cabana, Jordi. Nanoscale Detection of Intermediate Solid Solutions in Equilibrated LixFePO4 Microcrystals.  United States.  https://doi.org/10.1021/acs.nanolett.7b03086

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                    May, Brian M., Yu, Young-Sang, Holt, Martin V., Strobridge, Fiona C., Boesenberg, Ulrike, Grey, Clare P., and Cabana, Jordi. Wed .  
"Nanoscale Detection of Intermediate Solid Solutions in Equilibrated LixFePO4 Microcrystals".  United States.  https://doi.org/10.1021/acs.nanolett.7b03086.  https://www.osti.gov/servlets/purl/1461313.

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@article{osti_1461313,

  title        = {Nanoscale Detection of Intermediate Solid Solutions in Equilibrated LixFePO4 Microcrystals},

  author       = {May, Brian M. and Yu, Young-Sang and Holt, Martin V. and Strobridge, Fiona C. and Boesenberg, Ulrike and Grey, Clare P. and Cabana, Jordi},

  abstractNote = {Redox-driven phase transformations in solids determine the performance of lithium-ion batteries, crucial in the technological transition from fossil fuels. Couplings between chemistry and strain define reversibility and fatigue of an electrode. The accurate definition of all phases in the transformation, their energetics, and nanoscale location within a particle produces fundamental understanding of these couplings needed to design materials with ultimate performance. In this paper we demonstrate that scanning X-ray diffraction microscopy (SXDM) extends our ability to image battery processes in single particles. In LiFePO4 crystals equilibrated after delithiation, SXDM revealed the existence of domains of miscibility between LiFePO4 and Li0.6FePO4. These solid solutions are conventionally thought to be metastable, and were previously undetected by spectromicroscopy. The observation provides experimental verification of predictions that the LiFePO4–FePO4 phase diagram can be altered by coherency strain under certain interfacial orientations. Finally, it enriches our understanding of the interaction between diffusion, chemistry, and mechanics in solid state transformations.},

  doi          = {10.1021/acs.nanolett.7b03086},

  journal      = {Nano Letters},

  number       = 12,

  volume       = 17,

  place        = {United States},

  year         = {Wed Nov 22 00:00:00 EST 2017},

  month        = {Wed Nov 22 00:00:00 EST 2017}

}

Copy to clipboard

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https://doi.org/10.1021/acs.nanolett.7b03086

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Title: Nanoscale Detection of Intermediate Solid Solutions in Equilibrated LixFePO4 Microcrystals

Abstract

Citation Formats

The existence of a temperature-driven solid solution in LixFePO4 for 0 ≤ x ≤ 1 journal, February 2005

Design criteria for electrochemical shock resistant battery electrodes journal, January 2012

Dependence on Crystal Size of the Nanoscale Chemical Phase Distribution and Fracture in Li x FePO 4 journal, June 2015

Capturing metastable structures during high-rate cycling of LiFePO4 nanoparticle electrodes journal, June 2014

Direct view on the phase evolution in individual LiFePO4 nanoparticles during Li-ion battery cycling journal, September 2015

The Role of Coherency Strains on Phase Stability in Li[sub x]FePO[sub 4]: Needle Crystallites Minimize Coherency Strain and Overpotential journal, January 2009

Metastable Solid-Solution Phases in the LiFePO[sub 4]∕FePO[sub 4] System journal, January 2007

Direct Observation of Lithium Staging in Partially Delithiated LiFePO 4 at Atomic Resolution journal, April 2011

Visualization of Electrochemical Reactions in Battery Materials with X-ray Microscopy and Mapping journal, April 2017

Electron-beam-induced reduction of Fe3+ in iron phosphate dihydrate, ferrihydrite, haemosiderin and ferritin as revealed by electron energy-loss spectroscopy journal, July 2010

Fast determination of phases in LixFePO4 using low losses in electron energy-loss spectroscopy journal, March 2009

Chemical composition mapping with nanometre resolution by soft X-ray microscopy journal, September 2014

A hard X-ray nanoprobe beamline for nanoscale microscopy journal, September 2012

Nanoscale Hard X-Ray Microscopy Methods for Materials Studies journal, July 2013

Quantitative Nanoscale Imaging of Lattice Distortions in Epitaxial Semiconductor Heterostructures Using Nanofocused X-ray Bragg Projection Ptychography journal, September 2012

Mesoscale Phase Distribution in Single Particles of LiFePO 4 following Lithium Deintercalation journal, April 2013

Intercalation Pathway in Many-Particle LiFePO 4 Electrode Revealed by Nanoscale State-of-Charge Mapping journal, February 2013

Dichotomy in the Lithiation Pathway of Ellipsoidal and Platelet LiFePO 4 Particles Revealed through Nanoscale Operando State-of-Charge Imaging journal, May 2015

Antiferromagnetism in LiFePO4 journal, March 1967

IR Near-Field Spectroscopy and Imaging of Single Li x FePO 4 Microcrystals journal, December 2014

Electron Microscopy Study of the LiFePO[sub 4] to FePO[sub 4] Phase Transition journal, January 2006

Phase Change in Li[sub x]FePO[sub 4] journal, January 2005

The source of first-cycle capacity loss in LiFePO4 journal, July 2001

Phase Diagram of Li[sub x]FePO[sub 4] journal, January 2006

Phase Transformation and Lithiation Effect on Electronic Structure of Li x FePO 4 : An In-Depth Study by Soft X-ray and Simulations journal, August 2012

MAS NMR Study of the Metastable Solid Solutions Found in the LiFePO 4 /FePO 4 System † journal, February 2010

Current-induced transition from particle-by-particle to concurrent intercalation in phase-separating battery electrodes journal, September 2014

Kinetics of non-equilibrium lithium incorporation in LiFePO4 journal, July 2011

The thermodynamic stability of intermediate solid solutions in LiFePO 4 nanoparticles journal, January 2016

Direct Observation of a Metastable Crystal Phase of Li x FePO 4 under Electrochemical Phase Transition journal, April 2013

Elucidation of the Na 2/3 FePO 4 and Li 2/3 FePO 4 Intermediate Superstructure Revealing a Pseudouniform Ordering in 2D journal, June 2014

Size-Dependent Lithium Miscibility Gap in Nanoscale Li[sub 1−x]FePO[sub 4] journal, January 2007

Lithium ion conductivity in single crystal LiFePO4 journal, October 2008

3D elemental sensitive imaging using transmission X-ray microscopy journal, February 2012

Three-dimensional imaging of chemical phase transformations at the nanoscale with full-field transmission X-ray microscopy journal, July 2011

X-ray Microscopy book, January 2019

X-ray microscopy journal, July 1965

Title: Nanoscale Detection of Intermediate Solid Solutions in Equilibrated Li_xFePO₄ Microcrystals

The existence of a temperature-driven solid solution in LixFePO4 for 0 ≤ x ≤ 1
journal, February 2005

Design criteria for electrochemical shock resistant battery electrodes
journal, January 2012

Dependence on Crystal Size of the Nanoscale Chemical Phase Distribution and Fracture in Li _x FePO ₄
journal, June 2015

Capturing metastable structures during high-rate cycling of LiFePO4 nanoparticle electrodes
journal, June 2014

Direct view on the phase evolution in individual LiFePO4 nanoparticles during Li-ion battery cycling
journal, September 2015

The Role of Coherency Strains on Phase Stability in Li[sub x]FePO[sub 4]: Needle Crystallites Minimize Coherency Strain and Overpotential
journal, January 2009

Metastable Solid-Solution Phases in the LiFePO[sub 4]∕FePO[sub 4] System
journal, January 2007

Direct Observation of Lithium Staging in Partially Delithiated LiFePO ₄ at Atomic Resolution
journal, April 2011

Visualization of Electrochemical Reactions in Battery Materials with X-ray Microscopy and Mapping
journal, April 2017

Electron-beam-induced reduction of Fe3+ in iron phosphate dihydrate, ferrihydrite, haemosiderin and ferritin as revealed by electron energy-loss spectroscopy
journal, July 2010

Fast determination of phases in LixFePO4 using low losses in electron energy-loss spectroscopy
journal, March 2009

Chemical composition mapping with nanometre resolution by soft X-ray microscopy
journal, September 2014

A hard X-ray nanoprobe beamline for nanoscale microscopy
journal, September 2012

Nanoscale Hard X-Ray Microscopy Methods for Materials Studies
journal, July 2013

Quantitative Nanoscale Imaging of Lattice Distortions in Epitaxial Semiconductor Heterostructures Using Nanofocused X-ray Bragg Projection Ptychography
journal, September 2012

Mesoscale Phase Distribution in Single Particles of LiFePO ₄ following Lithium Deintercalation
journal, April 2013

Intercalation Pathway in Many-Particle LiFePO ₄ Electrode Revealed by Nanoscale State-of-Charge Mapping
journal, February 2013

Dichotomy in the Lithiation Pathway of Ellipsoidal and Platelet LiFePO ₄ Particles Revealed through Nanoscale Operando State-of-Charge Imaging
journal, May 2015

Antiferromagnetism in LiFePO4
journal, March 1967

IR Near-Field Spectroscopy and Imaging of Single Li _x FePO ₄ Microcrystals
journal, December 2014

Electron Microscopy Study of the LiFePO[sub 4] to FePO[sub 4] Phase Transition
journal, January 2006

Phase Change in Li[sub x]FePO[sub 4]
journal, January 2005

The source of first-cycle capacity loss in LiFePO4
journal, July 2001

Phase Diagram of Li[sub x]FePO[sub 4]
journal, January 2006

Phase Transformation and Lithiation Effect on Electronic Structure of Li _x FePO ₄ : An In-Depth Study by Soft X-ray and Simulations
journal, August 2012

MAS NMR Study of the Metastable Solid Solutions Found in the LiFePO ₄ /FePO ₄ System ^†
journal, February 2010

Current-induced transition from particle-by-particle to concurrent intercalation in phase-separating battery electrodes
journal, September 2014

Kinetics of non-equilibrium lithium incorporation in LiFePO4
journal, July 2011

The thermodynamic stability of intermediate solid solutions in LiFePO ₄ nanoparticles
journal, January 2016

Direct Observation of a Metastable Crystal Phase of Li _x FePO ₄ under Electrochemical Phase Transition
journal, April 2013

Elucidation of the Na _2/3 FePO ₄ and Li _2/3 FePO ₄ Intermediate Superstructure Revealing a Pseudouniform Ordering in 2D
journal, June 2014

Size-Dependent Lithium Miscibility Gap in Nanoscale Li[sub 1−x]FePO[sub 4]
journal, January 2007

Lithium ion conductivity in single crystal LiFePO4
journal, October 2008

3D elemental sensitive imaging using transmission X-ray microscopy
journal, February 2012

Three-dimensional imaging of chemical phase transformations at the nanoscale with full-field transmission X-ray microscopy
journal, July 2011

X-ray Microscopy
book, January 2019

X-ray microscopy
journal, July 1965