Hostname: page-component-78c5997874-fbnjt Total loading time: 0 Render date: 2024-11-10T10:16:40.208Z Has data issue: false hasContentIssue false
  • English
  • Français

Monitoring of FES2 reactions using high-temperature XRD coupled with gas chromatography

Published online by Cambridge University Press:  03 May 2019

K.-A. M. Stirrup ,
M. A. Rodriguez ,
E. N. Coker ,
J. J. M. Griego  and
T. M. Anderson
K.-A. M. Stirrup
Affiliation:
Sandia National Laboratories, Albuquerque, New Mexico 87185-1411
M. A. Rodriguez*
Affiliation:
Sandia National Laboratories, Albuquerque, New Mexico 87185-1411
E. N. Coker
Affiliation:
Sandia National Laboratories, Albuquerque, New Mexico 87185-1411
J. J. M. Griego
Affiliation:
Sandia National Laboratories, Albuquerque, New Mexico 87185-1411
T. M. Anderson
Affiliation:
Sandia National Laboratories, Albuquerque, New Mexico 87185-1411
*
a)Author to whom correspondence should be addressed. Electronic mail: marodri@sandia.gov
Get access Rights & Permissions [Opens in a new window]

Abstract

High-temperature X-ray diffraction with concurrent gas chromatography (GC) was employed in the study of iron disulfide (FeS2) cathode pellets disassembled from thermal batteries. When FeS2 cathode materials were analyzed in an air environment, reaction of the KCl and LiCl salt phases led to the formation of Li2(SO4) and KFe2S3 phases beginning at ~230 °C. These phases subsequently reacted to generate various forms of potassium iron sulfates in the 280–500 °C range, with the final products resulting in a β-Fe2O3 phase and K2(SO4). Independent simultaneous thermal analysis coupled with mass spectroscopy (MS) augmented the diffraction results and supported the overall picture of FeS2 decomposition. Both gas analysis measurements (i.e. GC and MS) from the independent experiments confirmed the formation of SO2 off-gas species during the breakdown of the FeS2. In contrast, characterization of the same cathode material under inert conditions showed the persistence of the initial FeS2 phase throughout the entire temperature range of analysis.

Keywords

high-temperature XRDgas chromatographypyrite FeS2
Type
Technical Article
Information
Powder Diffraction , Volume 34 , Issue 2 , June 2019 , pp. 90 - 96
Copyright
Copyright © International Centre for Diffraction Data 2019 

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Danno, T., Nakatsuka, D., Kusano, Y., Asaoka, H., Nakanishi, M., Fujii, T., Ikeda, Y., and Takada, J. (2013). “Crystal structure of β-Fe2O3 and topotactic phase transformation to α-Fe2O3,” Cryst. Growth Des. 13, 770–774.Google Scholar
Eneroth, E. (2007). “Combined magnetic and structural investigation of nano crystalline iron oxides: the interplay between crystal size and phase composition during FeS2 oxidation,” J. Magn. Magn. Mater. 308, 250–268.Google Scholar
Guidotti, R. A., and Masset, P. (2006). “Thermally activated (‘thermal’) battery technology Part I: an overview,” J. Power Sources 161, 1443–1449.Google Scholar
Hu, Z., Zhu, Z., Cheng, F., Zhang, K., Wang, J., Chen, C., and Chen, J. (2015). “Pyrite FeS2 for high-rate and long-life rechargeable sodium batteries,” Energy Environ. Sci. 8, 1309–1316.Google Scholar
Rodriguez, M. A., Coker, E. N., Griego, J. J. M., Mowry, C. D., Pimentel, A. S., and Anderson, T. M. (2016). “Monitoring of CoS2 reactions using high-temperature XRD coupled with gas chromatography (GC),” Powder Diffr. 31, 90–96.Google Scholar
Tuček, J., Machala, L., Ono, S., Namai, A., Yoshikiyo, M., Imoto, K., Tokoro, H., Ohkishi, S., and Zboril, R. (2015). “Zeta-Fe2O3—A new stable polymorph in iron(III) oxide family,” Nat. Sci. Rep. 5, 15091–1–11.Google Scholar
Yasuda, K., Nohira, T., Ogata, Y. H., and Ito, Y. (2005). “Electrochemical window of molten LiCl–KCl–CaCl2 and the Ag+/Ag reference electrode,” Electrochim. Acta 51, 561–565.Google Scholar