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Melting of indium by temperature-modulated differential scanning calorimetry

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Abstract

The melting and crystallization of a sharply melting standard has been explored for the calibration of temperature-modulated differential scanning calorimetry, TMDSC. Modulated temperature and heat flow have been followed during melting and crystallization of indium. It is observed that indium does not supercool as long as crystal nuclei remain in the sample when analyzing quasi-isothermally with a small modulation amplitude. For standard differential scanning calorimetry, DSC, the melting and crystallization temperatures of indium are sufficiently different not to permit its use for calibration on cooling, unless special analysis modes are applied. For TMDSC with an underlying heating rate of 0.2 K min−1 and a modulation amplitude of 0.5–1.5 K at periods of 30–90 s, the extrapolated onsets of melting and freezing were within 0.1 K of the known melting temperature of indium. Further work is needed to separate the effects originating from loss of steady state between sample and sensor on the one hand and from supercooling on the other.

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Authors and Affiliations

  1. Department of Chemistry, The University of Tennessee, 37996-1600, Knoxville, TN

    K. Ishikiriyama, A. Boller & B. Wunderlich

  2. Chemical and Analytical Sciences Division, Oak Ridge National Laboratory, 37831-6197, Oak Ridge, TN, USA

    K. Ishikiriyama, A. Boller & B. Wunderlich

Authors
  1. K. Ishikiriyama
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  2. A. Boller
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  3. B. Wunderlich
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Additional information

On leave from Toray Research Center, Inc., Otsu, Shiga 520, Japan.

This work was supported by the Division of Materials Research, National Science Foundation, Polymers Program, Grant # DMR 90-00520 and the Division of Materials Sciences, Office of Basic Energy Sciences, U.S. Department of Energy at Oak Ridge National Laboratory, managed by Lockheed Martin Energy Research Corp. for the U.S. Department of Energy, under contract number DEACOS-960R22464. Support for instrumentation came from TA Instruments, Inc. and Mettler-Toledo Inc. Research support was also given by ICI Paints.

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Ishikiriyama, K., Boller, A. & Wunderlich, B. Melting of indium by temperature-modulated differential scanning calorimetry. Journal of Thermal Analysis 50, 547–558 (1997). https://doi.org/10.1007/BF01979027

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  • DOI: https://doi.org/10.1007/BF01979027

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