Abstract
A novel microthermogravimetric apparatus to study the kinetics of metal sulphur reactions and transport properties of transition metal sulphides has been described. The main feature of this arrangement includes the application of the carrier gas for sulphur vapour transportation and the protection of the balance chamber from sulphur attack. As a consequence, the helix balance could have been replaced by an automatic electronic microbalance and the accuracy of the mass change measurements increased more than two orders of magnitude, up to 10–7 g. The application of two liquid sulphur reservoirs created very stable, strictly defined reaction conditions, and enabled to make rapid changes of sulphur partial pressure in the reaction chamber. It has been demonstrated that all these innovations make it possible to study not only the kinetics of very slow sulphidation processes but also to determine deviations from stoichiometry and defect mobility in transition metal sulphides.
Article PDF
Similar content being viewed by others
References
D. B. Meadowcroft and H. J. Manning, Corrosion Resistant Materials for Coal Gasification Systems, Applied Science, London 1993.
P. Kofstad, High-temperature Corrosion, Elsevier, Amsterdam 1988, p. 425.
S. Mrowec, Oxid. Met., 44 (1995) 177.
S. Mrowec and K. Przybylski, High Temp. Mater. Processes, 6 (1984) 1.
S. Mrowec and J. Janowski, Similarities and Differences in defect dependent properties of Transition Metal Sulphides and Oxides, in: Selected Topics in High-Temperature Chemistry, Ed. by O. Johannesen and A. G. Andersen, Elsevier, Amsterdam 1989, p. 55.
S. Mrowec, Defects and Diffusion in Solids, Elsevier, Amsterdam 1980, p. 174.
S. Mrowec and T. Werber, Gas Corrosion of Metals, National Bureau of Standards and National Science Foundation, Washington, D. C. 1978, p. 444.
S. Mrowec and T. Werber, Modern Scaling Resistant Materials, National Bureau of Standards and National Science Foundation, Washington D. C. 1982, p. 195.
M. Danielewski, S. Mrowec and A. Wojtowicz, Oxid. Met., 35 (1991) 223.
O. Neeunhoffer and K. Hauffe, Z. anorg. allg. Chem., 262 (1950) 300.
K. Hauffe and A. Rahmel, Z. physik. Chem., 199 (1952) 152.
P. Geld and A. Krasowskaya, J. Phys. Chem., 34 (1962) 1721.
B. Lichter and C. Wagner, J.Electrochem. Soc., 807 (1960) 168.
L. Czerski, S. Mrowec and T. Werber, J. Electrochem. Soc., 109 (1962) 273.
S. Mrowec, A. Stoklosa and M. Danielewski, Oxid. Met., 11 (1977) 355.
M. Danielewski and S. Mrowec, J. Thermal Anal., 29 (1984) 1025.
B. S. Lee and R. A. Rapp, J. Electrochem. Soc., 131 (1984) 2988.
M. F. Chen and D. L. Douglass, Oxid. Met., 32 (1989) 185.
R. Rusiecki, A. Wojtowicz, S. Mrowec and K. Przybylski, Solid State Ionics, 21 (1986) 273.
Z. Zurek, J. Thermal Anal., 39 (1993) 15.
W. Znamirowski, F. Gesmundo, S. Mrowec, M. Danielewski, K. Godlewski and F. Viani, Oxid. Met., 35 (1991) 175.
G. Simkovich, Werkstoffe und Korrosion, 21 (1970) 973.
T. Norby, Hydrogen Defects in Inorganic Solids, in: Selected Topics in High-Temperature Chemistry, Ed. by O. Johannesen and A. G. Andersen, Elsevier, Amsterdam 1989, p. 101.
T. Norby and P. Kofstad, J. Amer. Ceram. Soc., 67 (1984) 786.
M. Wakihara, T. Uhida and M. Taniguchi, Mater. Res. Bull., 11 (1976) 973.
F. A. Elrefaie and W. W. Smeltzer, Oxid. Met., 16 (1981) 267.
J. Larpin and M. Perez, Oxid. Met., 21 (1984) 279.
M. Danielewski, Oxid. Met., 25 (1986) 51.
S. Mrowec and K. Przybylski, Oxid. Met., 23 (1985) 107.
M. Danielewski and S. Mrowec, Solid State Ionics, 17 (1985) 29.
H. Rau, J. Phys. Chem. Solids, 39 (1978) 3339.
S. Mrowec, M. Danielewski and H. J. Grabke, J. Mater. Sci., 25 (1990) 837.
P. Papaiacovou, K. Hennesen and H. J. Grabke, Solid State Communications, 73 (1990) 105.
J. Gilewicz-Wolter, M. Danielewski and S. Mrowec, Physical Rev. B, 56 (1997) 8695.
S. Mrowec, M. Danielewski and J. Gilewicz-Wolter, Solid State Ionics, 117 (1999) 65.
H. Le Brusq and J. P. Delmaire, Rev. Int. Hautes Temp. Refact., 11 (1974) 193.
J. Rasneur and D. Carton, C. R. Acad. Sci. Paris, Ser. II, 290 (1980) 405.
M. Danielewski and S. Mrowec, Solid State Ionics, 17 (1985) 319.
P. Kofstad, Non-stoichiometry, Diffusion and Electrical Conductivity in Binary Metal Oxides, Wiley, New York 1972.
S. Mrowec, An Introduction to the Theory of Metal Oxidation, National Bureau of Standards and National Science Foundation, Washington D. C. 1982, p. 172.
S. Mrowec, Reactivity of Solids, 5 (1988) 241.
S. Mrowec and K. Hashimoto, J. Mater. Sci., 30 (1995) 4801.
J. B. Wagner, in: Mass Transport in Oxides, NBS Special Publ., 269 (1969) 65.
P. E. Child, L. W. Laub and J. B. Wagner, Proc. Brit. Ceram. Soc., Mass Transport in Non-Metallic Solids, 19 (1971) 29.
P. E. Child and J. B. Wagner, Heterogeneous Kinetics at Elevated Temperatures, Plenum Press, New York 1970, p. 269.
Author information
Authors and Affiliations
Rights and permissions
About this article
Cite this article
Grzesik, Z., Mrowec, S., Walec, T. et al. New Microthermogravimetric Apparatus. Kinetics of metal sulphidation and transport properties of transition metal sulphides. Journal of Thermal Analysis and Calorimetry 59, 985–997 (2000). https://doi.org/10.1023/A:1010199030780
Issue Date:
DOI: https://doi.org/10.1023/A:1010199030780