Abstract
Characterization of microstructural properties in electrodes for Li-Ion batteries can be regarded a key factor to understand functionality and aging process in the cells. X-ray microscopy has proven extremely powerful to capture a number of morphological parameters such as porosity, tortuosity or particle size distribution but also chemical information regarding phase distribution, state of charge or elemental migration over a large range of length scales. With their high penetration power utilizing various contrast methods X-rays offer deep insight into the battery materials and microstructural characteristics.
Access this chapter
Tax calculation will be finalised at checkout
Purchases are for personal use only
References
Tanida H, Fukuda K, Murayama H et al (2014) RISING beamline (BL28XU) for rechargeable battery analysis. J Synchrotron Radiat 21:268–272. doi:10.1107/S1600577513025733
Stephenson DE, Walker BC, Skelton CB et al (2011) Modeling 3D microstructure and ion transport in porous li-ion battery electrodes. J Electrochem Soc 158:A781. doi:10.1149/1.3579996
Harris SJ, Lu P (2013) Effects of inhomogeneities—nanoscale to mesoscale—on the durability of li-ion batteries. J Phys Chem C 117:6481–6492
Ebner M, Marone F, Stampanoni M, Wood V (2013) Visualization and quantification of electrochemical and mechanical degradation in Li ion batteries. Science 342:716–720. doi:10.1126/science.1241882
Ebner M, Chung D-W, Garcia ER, Wood V (2014) Toruosity anisotropy in lithium-ion battery electrodes. Adv Energy Mater 4:1301278
Thiedmann R, Stenzel O, Spettl A et al (2011) Stochastic simulation model for the 3D morphology of composite materials in Li–ion batteries. Comput Mater Sci 50:3365–3376. doi:10.1016/j.commatsci.2011.06.031
Ender M, Joos J, Weber A, Ivers-Tiffée E (2014) Anode microstructures from high-energy and high-power lithium-ion cylindrical cells obtained by X-ray nano-tomography. J Power Sources 269:912–919
Shao M (2014) In situ microscopic studies on the structural and chemical behaviors of lithium-ion battery materials. J Power Sources 270:475–486. doi:10.1016/j.jpowsour.2014.07.123
Andrews JC, Weckhuysen BM (2013) Hard X-ray spectroscopic nano-imaging of hierarchical functional materials at work. ChemPhysChem 14:3655–3666
Shapiro DA, Yu Y-S, Tyliszczak T et al (2014) Chemical composition mapping with nanometre resolution by soft X-ray microscopy. Nat Photonics 1–5. doi:10.1038/nphoton.2014.207
Fitzgerald R (2000) Phase -sensitive X-ray imaging. Phys Today 23:23–26
Burvall A, Lundström U, Takman Pac et al (2011) Phase retrieval in X-ray phase-contrast imaging suitable for tomography. Opt Express 19:10359–10376
Schroer CG, Cloetens P, Rivers M et al (2004) High-resolution 3D imaging microscopy using hard X-rays. MRS Bull 29:157–165
Eastwood DS, Bradley RS, Tariq F et al (2014) The application of phase contrast X-ray techniques for imaging Li-ion battery electrodes. Nucl Instrum Methods Phys Res Sect B Beam Interact with Mater Atoms 324:118–123. doi:10.1016/j.nimb.2013.08.066
Lin C-N, Chen W-C, Song Y-F et al (2014) Understanding dynamics of polysulfide dissolution and re-deposition in working lithium-sulfur battery by in-operando transmission X-ray microscopy. J Power Sources 263:98–103
Bunker G (2010) Introduction to XAFS: a practical guide to X-ray absorption fine structure spectroscopy, 1st edn. Cambridge University Press, Cambridge
Koningsberger DC, Prins R (1988) X-Ray absorption: principles, applications, techniques of EXAFS, SEXAFS and XANES. Wiley-Interscience, New York
Shearing P, Wu Y, Harris SJ, Brandon N (2011) In situ X-Ray spectroscopy and imaging of battery materials. Electrochem Soc Interface 20:43–47
McBreen J, O’Grady WE, Pandya KI (1988) EXAFS: a new tool for the study of battery and fuel cell materials. J Power Sources 22:323–340. doi:10.1016/0378-7753(88)80027-2
Meirer F, Cabana J, Liu Y et al (2011) Three-dimensional imaging of chemical phase transformations at the nanoscale with full-field transmission X-ray microscopy. J Synchrotron Radiat 18:773–781. doi:10.1107/S0909049511019364
Liu Y, Meirer F, Williams Pa et al (2012) TXM-wizard: a program for advanced data collection and evaluation in full-field transmission X-ray microscopy. J Synchrotron Radiat 19:281–287. doi:10.1107/S0909049511049144
Dinnebier RE, Billinge SJL (2008) Powder diffraction—theory and practice. RSC Publishing
Reinsberg K-G, Schumacher C, Zastrow S et al (2013) Investigation on the homogeneity of pulsed electrochemically deposited thermoelectric films with synchrotron μ-XRF, μ-XRD and μ-XANES. J Mater Chem A 1:4215–4220. doi:10.1039/c3ta01480k
Janssens KHA, Adams FCV, Rindby A (1999) Microscopic X-ray fluorescence analysis. Wiley, New York
Radtke M, Buzanich G, Curado J et al (2014) Slicing—a new method for non destructive 3D elemental sensitive characterization of materials. J Anal At Spectrom 29:1339–1344. doi:10.1039/C4JA00085D
Scharf O, Ihle S, Ordavo I et al (2011) Compact pnCCD-based X-ray camera with high spatial and energy resolution: a color X-ray camera. Anal Chem 83:2532–2538
Boone MN, Garrevoet J, Tack P et al (2014) High spectral and spatial resolution X-ray transmission radiography and tomography using a color X-ray camera. Nucl Instrum Methods Phys Res A 735:644–648. doi:10.1016/j.nima.2013.10.044
Falcone R, Jacobsen C, Kirz J et al (2011) New directions in X-ray microscopy. Contemp Phys 52:293–318. doi:10.1080/00107514.2011.589662
Gonzalez-Jimenez ID, Cats K, Davidian T et al (2012) Hard X-ray nanotomography of catalytic solids at work. Angew Chem Int Ed Engl 51:11986–11990. doi:10.1002/anie.201204930
Sakdinawat A, Attwood D (2010) Nanoscale X-ray imaging. Nat Photonics 4:840–848. doi:10.1038/nphoton.2010.267
De Jonge MD, Vogt S (2010) Hard X-ray fluorescence tomography–an emerging tool for structural visualization. Curr Opin Struct Biol 20:606–614. doi:10.1016/j.sbi.2010.09.002
De Nolf W, Janssens K (2009) Micro X-ray diffraction and fluorescence tomography for the study of multilayered automotive paints. Surf Interface Anal 42:411–418
Larson BC, Yang W, Ice GE et al (2002) Three-dimensional X-ray structural microscopy with submicrometre resolution. Nature 415:887–890. doi:10.1038/415887a
Schropp A, Hoppe R, Patommel J et al (2012) Hard x-ray scanning microscopy with coherent radiation: beyond the resolution of conventional X-ray microscopes. Appl Phys Lett 100:253112. doi:10.1063/1.4729942
Dam HF, Andersen TR, Pedersen EBL et al (2014) Enabling flexible polymer tandem solar cells by 3D ptychographic imaging. Adv Energy Mater n/a–n/a. doi:10.1002/aenm.201400736
Holler M, Diaz A, Guizar-Sicairos M et al (2014) X-ray ptychographic computed tomography at 16Â nm isotropic 3D resolution. Sci Rep 4:3857. doi:10.1038/srep03857
Cotte M, Susini J, Dik J, Janssens K (2010) Synchrotron-based X-ray absorption spectroscopy for art conservation: looking back and looking forward. Acc Chem Res 43:705–714
Andrews JC, Almeida E, Van Der Meulen MCH et al (2010) Nanoscale X-Ray microscopic imaging of mammalian mineralized tissue. Microsc Microanal 16:327–336
Cocco AP, Nelson GJ, Harris WM et al (2013) Three-dimensional microstructural imaging methods for energy materials. Phys Chem Chem Phys 15:16377–16407. doi:10.1039/c3cp52356j
Liu Y, Meirer F, Wang J et al (2012) 3D elemental sensitive imaging using transmission X-ray microscopy. Anal Bioanal Chem 404:1297–1301. doi:10.1007/s00216-012-5818-9
Nelson J, Misra S, Yang Y et al (2012) In operando X-ray diffraction and transmission X-ray microscopy of lithium sulfur batteries. J Am Chem Soc 134:6337–6343. doi:10.1021/ja2121926
Kanitpanyacharoen W, Parkinson DY, De Carlo F et al (2013) A comparative study of X-ray tomographic microscopy on shales at different synchrotron facilities: ALS, APS and SLS. J Synchrotron Radiat 20:172–180. doi:10.1107/S0909049512044354
Yuan L-X, Wang Z-H, Zhang W-X et al (2011) Development and challenges of LiFePO4 cathode material for lithium-ion batteries. Energy Environ Sci 4:269. doi:10.1039/c0ee00029a
Shearing PR, Howard LE, Jørgensen PS et al (2010) Characterization of the 3-dimensional microstructure of a graphite negative electrode from a Li-ion battery. Electrochem Commun 12:374–377. doi:10.1016/j.elecom.2009.12.038
Shearing PR, Brandon NP, Gelb J et al (2012) Multi length scale microstructural investigations of a commercially available Li-ion battery electrode. J Electrochem Soc 159:A1023–A1027
Eastwood DS, Yufit V, Gelb J et al (2014) Lithiation-induced dilation mapping in a lithium-ion battery electrode by 3D X-Ray microscopy and digital volume correlation. Adv Energy Mater 4:1300506
Channagiri Sa, Nagpure SC, Babu SS et al (2013) Porosity and phase fraction evolution with aging in lithium iron phosphate battery cathodes. J Power Sources 243:750–757. doi:10.1016/j.jpowsour.2013.06.023
Chen-Wiegart YK, Liu Z, Faber KT et al (2013) 3D analysis of a LiCoO2–Li(Ni1/3Mn1/3Co1/3)O2 Li-ion battery positive electrode using x-ray nano-tomography. Electrochem Commun 28:127–130. doi:10.1016/j.elecom.2012.12.021
Chao S-C, Yen Y-C, Song Y-F et al (2011) In situ transmission X-ray microscopy study on working SnO anode particle of Li-ion batteries. J Electrochem Soc 158:A1335–A1339
Chao S-C, Yen Y-C, Song Y-F et al (2010) A study on the interior microstructures of working Sn particle electrode of Li-ion batteries by in situ X-ray transmission microscopy. Electrochem Commun 12:234–237. doi:10.1016/j.elecom.2009.12.002
Weker JN, Liu N, Misra S et al (2014) In situ nanotomography and operando transmission X-ray microscopy of micron-sized Ge particles. Energy Environ Sci 7:2771. doi:10.1039/C4EE01384K
Wang J, Chen-Wiegart YK, Wang J (2013) In situ chemical mapping of a lithium-ion battery using full-field hard X-ray spectroscopic imaging. Chem Commun (Camb) 49:6480–6482. doi:10.1039/c3cc42667j
Ebner M, Geldmacher F, Marone F et al (2013) X-Ray tomography of porous, transition metal oxide based lithium ion battery electrodes. Adv Energy Mater 3:845–850
Wang J, Chen-Wiegart YK, Wang J (2014) In situ three-dimensional synchrotron X-ray nanotomography of (de)lithiation processes in tin anodes. Angew Chem Int Ed 53:4460–4464
Zielke L, Hutzenlaub T, Wheeler DR et al (2014) A combination of X-ray tomography and carbon binder modeling: reconstructing the three phases of LiCoO2 Li-ion battery cathodes. Adv Energy Mater 4:1301617
Boesenberg U, Meirer F, Liu Y et al (2013) Mesoscale phase distribution in single particles of LiFePO4 following lithium deintercalation. Chem Mater 25:1664–1672. doi:10.1021/cm400106k
Chueh WC, El Gabaly F, Sugar JD et al (2013) Intercalation pathway in many-particle LiFePO(4) electrode revealed by nanoscale state-of-charge mapping. Nano Lett 13:866–872. doi:10.1021/nl3031899
Wang J, Chen-Wiegart YK, Wang J (2014) In operando tracking phase transformation evolution of lithium iron phosphate with hard X-ray microscopy. Nat Commun 5:1–10. doi:10.1038/ncomms5570
Chen-Wiegart YK, Wang J, Wang J (2013) Development of in situ full field spectroscopic imaging analysis and application on Li-ion battery using transmission X-ray microscopy. Proceediongs of the SPIE 8851, X-Ray Nanoimaging Instruments Methods. p 88510C
Yang F, Liu Y, Martha SK et al (2014) Nanoscale morphological and chemical changes of high voltage lithium-manganese rich NMC composite cathodes with cycling. Nano Lett 14:4334–4341. doi:10.1021/nl502090z
Sun Y-K, Chen Z, Noh H-J et al (2012) Nanostructured high-energy cathode materials for advanced lithium batteries. Nat Mater 11:942–947. doi:10.1038/nmat3435
Poulsen HF, Jensen DJ, Vaughan GBM (2004) Three-dimensional X-Ray diffraction microscopy using high-energy X-Rays. MRS Bull 29:166–169
Bleuet P, Welcomme E, Dooryhée E et al (2008) Probing the structure of heterogeneous diluted materials by diffraction tomography. Nat Mater 7:468–472. doi:10.1038/nmat2168
Liu J, Kunz M, Chen K et al (2010) Visualization of charge distribution in a lithium battery electrode. J Phys Chem Lett 1:2120–2123. doi:10.1021/jz100634n
Robert R, Zeng D, Lanzirotti A et al (2012) Scanning X-ray fluorescence imaging study of lithium insertion into copper based oxysulfides for Li-Ion batteries. Chem Mater 24:2684–2691
Singer A, Ulvestad A, Cho H et al (2014) Noequilibrium structural dynamics of nanoparticles in LiNi1/2Mn3/2O4 cathode under operando conditions. Nano Lett, ASAP
Ulvestad A, Singer A, Cho H-M et al (2014) Single Particle Nanomechanics in operando batteries via lensless strain mapping. Nano Lett. doi:10.1021/nl501858u
Fittschen U, Boesenberg U, Falk M et al (2014) Confocal XRF imaging of elemental deposition of Mn, Ni and Cu on the graphite anode in cycled LiNi0.5Mn1.5O4 /graphite full cells. Anka Annual Report
Menzel M, Schlifke A, Falk M et al (2013) Surface and in-depth characterization of lithium-ion battery cathodes at different cycle states using confocal micro-X-ray fluorescence-X-ray absorption near edge structure analysis. Spectrochim Acta Part B At Spectrosc 85:62–70. doi:10.1016/j.sab.2013.04.001
Boesenberg U, Falk M, Fittschen UEA et al (2015) Correlation between chemical and morphological heterogeneities in LiNi0.5Mn1.5O4 spinel composite electrodes for lithium-Ion batteries determined by Micro-X-ray Fluorescence Analysis, Chemistry of Materials, doi:10.1021/acs.chemmater.5b00119
Author information
Authors and Affiliations
Corresponding author
Editor information
Editors and Affiliations
Rights and permissions
Copyright information
© 2015 Springer International Publishing Switzerland
About this chapter
Cite this chapter
Boesenberg, U., Fittschen, U.E.A. (2015). 2D and 3D Imaging of Li-Ion Battery Materials Using Synchrotron Radiation Sources. In: Zhang, Z., Zhang, S. (eds) Rechargeable Batteries. Green Energy and Technology. Springer, Cham. https://doi.org/10.1007/978-3-319-15458-9_14
Download citation
DOI: https://doi.org/10.1007/978-3-319-15458-9_14
Published:
Publisher Name: Springer, Cham
Print ISBN: 978-3-319-15457-2
Online ISBN: 978-3-319-15458-9
eBook Packages: EnergyEnergy (R0)