Skip to main content

Old Technique for New Materials: Characterization of Solid State Hydrogen Storage Materials by Temperature Programmed Reaction

  • Tecle S. Rufael (a1) and Cabral M. Williams (a1)

The most common diagnostic tools in studying reversible solid-state hydrogen storage materials involve volumetric or gravimetric approaches. In this study, a mature gas solid analysis technique called Temperature Programmed Reaction (TPR) is presented as an alternative and complementary approach in investigating solid-state hydrogen storage materials. TPR is fast, simple and offers valuable information from a wide range of solid materials. This technique is routinely used to characterize the reduction behavior of metal oxide and sulfide catalysts. In a typical TPR experiment, a sample powder is heated at a constant rate under a non steady-state environment of constant pressure and flow of a hydrogen/inert gas mixture, while monitoring the rate of hydrogen absorption and desorption by a thermal conductivity detector. The principle behind TPR is the high thermal conductivity coefficient of hydrogen when compared to other gases. The detector is sensitive enough that a slight change in hydrogen concentration is reflected by significant changes in the thermal conductivity signal. Hydrogen storage materials exhibit fingerprint type TPR spectra, unique to their composition and structure. Specific rates of hydrogen intake, heats of absorption and desorption as well as extent of activation can be extracted from TPR curves. In addition, multiple absorption and desorption states can be identified from the number of absorption or desorption peaks. Material stability and potential structural or phase changes can also be inferred indirectly. The simplicity and the highly sensitive thermal conductivity measurement provide a number of advantages over the traditional volumetric or gravimetric methods. Metal hydride alloys of AB5-type are used to demonstrate the effectiveness of TPR technique in characterizing hydrogen storage materials.

Hide All
1. US Deparment of Energy, Hydrogen, Fuel Cells and Infrastructure Technologies Program, Multi-Year Research, Development and Demonstration Plan, June 3, 2003.
2. Zotin, F.M.Z., Tournayan, L., Varloud, J., Perrichon, V. and Frèty, R., Appl. Catal. A: General 98, 99 (1993)
3. Bedford, M., Purves, J.H., Self, V. A. and Sermon, P.A., Appl. Catal. 58, 147 (1990)
4. Kanervo, J., Kinetic Analysis of Temperature-Programmed Reactions, Ph.D. Thesis, Helsinki University of Technology, 2003.
5. Rufael, T. and Williams, C., presentation at HYPOTHESIS V conference, Porto Conte, Italy, 2003 (unpublished).
6. Arnoldy, P. and Moulijn, J. A., J. Catal. 93, 38 (1985)
7. Janssen, F.J.J.G., Jour. Thermal. Anal. 37, 1281 (1991)
8. Yperman, J., Franco, D., Mullens, J., Reggers, G., D’olieslaeger, M. and Van Poucke, L.C., in Composition, Geochemistry and Conversion of Oil Shales, edited by Snape, C. (Kluwer Academic Publishers, Dordrecht, 1995) pp. 449459.
9. Hurst, N.W., Gentry, S.J., Jones, A. and McNicol, B., Catal. Rev.-Sci. Eng. 24(20), 223 (1982).
10. Jones, A. and McNicol, B., Temperature-Programmed Reduction for Solid Materials Characterization, (Marcel Dekker, New York, 1986)
11. Hu, Y.H. and Ruckenstein, E., Ind. Eng. Chem. Res. 42, 5135 (2003)
12. Dillon, A., Jones, K.M., Bekkedahl, T.A., Kiang, C.H., Bethuune, D.S. and Heben, M.J., Nature 386, 377 (1997)
13. Advance Scientific Design, Inc. Instrument Manual (1997)
14. Kanervo, J. and Krause, O., J. Catal. 207, 57 (2001)
15. Rossi, N.L., Eckert, J., Eddaoudi, M., Vodak, D.T., Kim, J., O'Keeffe, M. and Yaghi, O. M., Science 300, 1127 (2003).
16. Labruyère, F., Lacroix, M., Schweich, D. and Breyesse, M., J. Catal. 167, 464 (1997).
Recommend this journal

Email your librarian or administrator to recommend adding this journal to your organisation's collection.

MRS Online Proceedings Library (OPL)
  • ISSN: -
  • EISSN: 1946-4274
  • URL: /core/journals/mrs-online-proceedings-library-archive
Please enter your name
Please enter a valid email address
Who would you like to send this to? *


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