Dolotko, O.

Ehrenberg, H.

Knapp, M.

Mühlbauer, M.J.

Senyshyn, A.

English

Mühlbauer, M. J.

KITopen

KIT – University of the State of Baden-Wuerttemberg and National Research Center of the Helmholtz Association In opernando neutron diffraction and tomography on Li-ion cells  H.Ehrenberg1,2, O. Dolotko3, M.J. Mühlbauer1,3, A. Senyshyn3, M. Knapp1 Effect of fatigue on crystal structure of electrode materials 1Institute for Applied Materials (IAM), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, D-76344 Eggenstein-Leopoldshafen, Germany 2Helmholtz-Institute Ulm for Electrochemical Energy Storage (HIU), P.O. Box 3640, D-76021 Karlsruhe, Germany 3Heinz Maier-Leibnitz Zentrum (MLZ), Technische Universität München, Lichtenbergstr. 1, 85748 Garching, Germany Contact: Prof. Dr. Helmut Ehrenberg e-mail: helmut.ehrenberg@kit.edu This work was supported by Deutsche Forschungsgemeinschaft, Research Collaborative Center 595 “Electrical Fatigue in Functional Materials”. O. Dolotko, A. Senyshyn, M. J. Mühlbauer, K. Nikolowski, F. Scheiba, H. Ehrenberg, J. Electrochem. Soc. 159(12) (2012) A2082-A2088 Two batches of Li-ion cells were cycled (CCCV, 1C) 200, 400, 600, 800 and 1000 times at  25 ˚C and 50 ˚C 0 200 400 600 800 10006080100  25°C 50°CLi ammount in anode, %Number of cyclesAmmount of intercalated into anode Li in batteries, cycled at 25 and 50°C15 % 26 %0 200 400 600 800 10000102030 LiC12 (cycling at 25°C) LiC6  (cycling at 25°C LiC12 (cycling at 50°C) LiC6  (cycling at 50°C)Phase fraction, wt.%Number of cycles0 200 400 600 800 10001900200021002200230024002500260021.9 %   25°C 50°CCapacity, mAhNumber of cycles12.8 %Capacity loss 21,9% discharged charged Active lithium loss  (20,8 %) 0 200 400 600 800 10003035404550556065707580859095100Li occupation, %Number of cyclesBattery cycled at 25°C2040608010020 40 60 80 100 120 140-505 observed calculated difference Bragg position7)6)5)2)Angle 2, degs.Normalised intensity, %1)"fresh" Li-ion battery(discharged to 3.40V)=1.5482(1) Å  (a)2040608010020 40 60 80 100 120 140-505 observed calculated difference Bragg position7)6)5) 4)3)Angle 2, degs.Normalised intensity, %1)"fresh" Li-ion battery(charged to 4.20V)=1.5482(1) A  (b)High-resolution monochromatic neutron powder diffraction In operando experiment carried out at the instrument SPODI (FRM-II) at =1.5482 Å in Debye-Scherrer geometry using a multidetector array. Neutron powder diffraction patterns from Li-ion cell of 18650-type vs. state-of-charge Expected pattern 1st order  Observed 1st order Observed 2nd order LiC12 C Carbon framework from neighbouring graphene layers under increasing sine-wave modulation period A. Senyshyn, O. Dolotko, M. J. Mühlbauer, K. Nikolowski, H. Fuess, H. Ehrenberg, J. Electrochem. Soc. 160(5) (2013) A3198-A3205 A. Senyshyn, M.J. Mühlbauer, O. Dolotko, M. Hofmann, T. Pirling, H. Ehrenberg, J. Power Sources 245 (2014) 678-683 Spatially-resolved neutron powder diffraction on 18650-type cell Exp. layout and corrections 2D diffraction data Intensity evolution Peak position Lithium concentration Experimental parameters for the in-situ measurements at STRESS-SPEC (FRM-II): =1.64 Å, gauge volume: 2x2x20 mm3 Discharge capacity  vs. cycling Li occupation in LixCoO2 vs. cycling at 25˚C LiC6/LiC12 phase fraction vs. cycling Li concentration inside the anode vs. c cling Typical NPD dataset  and Rietveld r finement ANTARES (FRM-II), FOV 100x100 mm2, ~100 µm pixel resolution Radon  transformation Absorption  to a chosen color scheme A. Senyshyn, M.J. Mühlbauer, K. Nikolowski, T. Pirling, H. Ehrenberg, J. Power Sources 203 (2012) 126-129. Energy: 100-130 keV ~40 µm pixel resolution Neutron tomography X-ray tomography 

In operando neutron diffraction and tomography on Li-ion cells

https://publikationen.bibliothek.kit.edu/220097898/3816680

In operando neutron diffraction and tomography on Li-ion cells

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