Skip to main content Accessibility help
×
Home

In situ analysis of LiFePO4 batteries: Signal extraction by multivariate analysis

  • Mark A. Rodriguez (a1), Mark H. Van Benthem (a1), David Ingersoll (a1), Sven C. Vogel (a2) and Helmut M. Reiche (a2)...

Abstract

The electrochemical reaction behavior of a commercial Li-ion battery (LiFePO4-based cathode, graphite-based anode) has been measured via in situ neutron diffraction. A multivariate analysis was successfully applied to the neutron diffraction data set facilitating in the determination of Li bearing phases participating in the electrochemical reaction in both the anode and cathode as a function of state-of-charge (SOC). The analysis resulted in quantified phase fraction values for LiFePO4 and FePO4 cathode compounds as well as the identification of staging behavior of Li6, Li12, Li24, and graphite phases in the anode. An additional Li-graphite phase has also been tentatively identified during electrochemical cycling as LiC48 at conditions of ∼5% to 15% SOC.

Copyright

References

Hide All
Andersson, A. S., Kalska, B., Haggstrom, L., and Thomas, J. O. (2000). “Lithium extraction/insertion in LiFePO4: An X-ray diffraction and Mossbauer spectroscopy study,” Solid State Ionics SSIOD3 130, 4152.10.1016/S0167-2738(00)00311-8
Arico, A. S., Bruce, P., Scrosati, B., Tarascon, J. -M., and Van Schalkwijk, W. (2005). “Nanostructural materials for advanced energy conversion and storage devices,” Nature Mater. NMAACR 4, 366377.10.1038/nmat1368
Billaud, D., McRae, E., and Herold, A. (1979). “Synthesis and electrical resistivity of lithium-pyrographite intercalation compounds (stages I, II, and III),” Mater. Res. Bull. MRBUAC 14, 857864.10.1016/0025-5408(79)90149-1
Conte, M., Prosini, P. P., and Passerini, S. (2004). “Overview of energy/hydrogen storage: State-of-the-art of the technologies and prospects for nanomaterials,” Mater. Sci. Eng., B MSBTEK 108, 28.10.1016/j.mseb.2003.10.107
Jollife, I. T. (2002). Principal Component Analysis, 2nd ed. (Springer-Verlag, New York).
Keenan, M. R. and Kotula, P. G. (2004). “Accounting for Poisson noise in the multivariate analysis of ToF-SIMS spectrum images,” Surf. Interface Anal. SIANDQ 36, 203212.10.1002/sia.1657
Larson, A. C. and Von Dreele, R. B. (2000). General Structure Analysis System (GSAS), LAUR Report No. 86-748, Los Alamos National Laboratory, Los Alamos, New Mexico.
Ravet, N., Chouinard, Y., Magnan, J. F., Besner, S., Gauthier, M., and Armand, M. (2001). “Electroactivity of natural and synthetic triphylite,” J. Power Sources JPSODZ 97–98, 503507.10.1016/S0378-7753(01)00727-3
Rodriguez, M. A., Keenan, M. R., and Nagasubramanian, G. (2007). “In situ X-ray diffraction analysis of (CFx)n batteries: Signal extraction by multivariate analysis,” J. Appl. Crystallogr. JACGAR 40, 10971104.10.1107/S0021889807042045
The Mathworks. (2008). MATLAB. VERSION 7.7.0.471 (The Mathworks Inc., Natick, MA).
Toby, B. H. (2001). “EXPGUI, a graphical user interface for GSAS,” J. Appl. Crystallogr. JACGAR 34, 210213.10.1107/S0021889801002242
Van Benthem, M. H. and Keenan, M. R. (2004). “Fast algorithm for the solution of large-scale non-negativity-constrained least squares problems,” J. Chemom. JOCHEU 18, 441450.10.1002/cem.889
Van Benthem, M. H., Keenan, M. R., and Haaland, D. M. (2002). “Application of equality constraints on variables during alternating least squares procedures,” J. Chemom. JOCHEU 16, 613622.10.1002/cem.761
Wenk, H. -R., Lutterotti, L., and Vogel, S. (2003). “Texture analysis with the new HIPPO TOF diffractometer,” Nucl. Instrum. Methods Phys. Res. A NIMAER 515, 575588.10.1016/j.nima.2003.05.001

Keywords

Metrics

Full text views

Total number of HTML views: 0
Total number of PDF views: 0 *
Loading metrics...

Abstract views

Total abstract views: 0 *
Loading metrics...

* Views captured on Cambridge Core between <date>. This data will be updated every 24 hours.

Usage data cannot currently be displayed