Skip to main content
SpringerLink
Log in

Calibration of micro-thermal analysis for the detection of glass transition temperatures and melting points

Repeatability and reproducibility

  • Regular Papers
  • Theory/Instrumentation
  • Published:
Journal of Thermal Analysis and Calorimetry Aims and scope Submit manuscript

Abstract

Micro-thermal analysis (μTATM) is a technique in which thermal analysis is performed on surfaces of test specimens on a small (ca. 2×2 μm) scale. Like any thermal analysis technique, interpretation of results benefits from accurate temperature information and knowledge of the precision of the resultant measurement. However, temperature calibration for such methods is more challenging than with its macro relatives since the calibrant comes into direct contact with the AFM sensor. This paper describes suitable calibration procedures for different types of transitions namely for first order transitions (melting points) and for glass transition temperatures using organic chemicals and polymers.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Similar content being viewed by others

References

  1. D. M. Price, M. Reading, A. Caswell, A. Hammiche and H. M. Pollock, Microscopy Anal., 65 (1998) 17.

    Google Scholar 

  2. D. Q. M. Craig, R. G. Royall, M. Reading, D. M. Price, T. J. Lever and J. Furry, Proc. 26th N. Am. Therm. Anal. Soc., 1998, p. 610.

  3. M. R. Reading, D. L. Hourston, M. Song, G. M. Pollock and A. Hammiche, Amer. Lab., 13 (1998).

  4. A. Hammiche, D. J. Hourston, H. M. Pollock, M. Reading and M. Song, J. Vac. Sci. Technol. B, 14 (1996) 1486.

    Article  CAS  Google Scholar 

  5. I. Woodward, S. Ebbens, J. Zhang, S. Luk, N. Patel and C. J. Roberts, Packaging Technol. Sci., 17 (2004) 129.

    Article  CAS  Google Scholar 

  6. J. Reussner and W. Pirgov, KGK Kautsch. Gummi Kunstst., 57 (2004) 516.

    CAS  Google Scholar 

  7. G. van Assche, A. Ghanem, O. Lhost and B. van Mele, Polymer, 46 (2005) 7132.

    Article  Google Scholar 

  8. G. van Assche and B. van Mele, Polymer, 43 (2002) 4605.

    Article  Google Scholar 

  9. M. S. Tillman, T. Takatoya, B. S. Hayes and J. C. Seferis, J. Therm. Anal. Cal., 62 (2000) 599.

    Article  CAS  Google Scholar 

  10. H. Fischer, Macromolecules, 35 (2002) 3592.

    Article  CAS  Google Scholar 

  11. J. Zhang, C. J. Roberts, K. M. Shakesheff, M. C. Davies and S. J. B. Tendler, Macromolecules, 36 (2003) 1215.

    Article  CAS  Google Scholar 

  12. I. Moon, R. Androsh, W. Chen and B. Wunderlich, J. Therm. Anal. Cal., 59 (2000) 187.

    Article  CAS  Google Scholar 

  13. M. C. Perkins, C. J. Roberts, D. Briggs, M. C. Davies, A. Friedmann, C. Hart and G. Bell, Appl. Surf. Sci., 243 (2005) 158.

    Article  CAS  Google Scholar 

  14. D. S. Fryer, P. F. Nealey and J. J. de Pablo, Macromolecules, 33 (2000) 6439.

    Article  CAS  Google Scholar 

  15. P. F. Nealey, R. E. Cohen and A. S. Argon, Macromolecules, 27 (1994) 4193.

    Article  CAS  Google Scholar 

  16. H. Breuer and G. Rehage, Kolloid-Z. 216/217 (1967) 159.

    Article  CAS  Google Scholar 

  17. D. W. van Krevelen and P. J. Hoftyzer, Properties of Polymer; Elsevier Scientific Publishing Company, Amsterdam 1976.

    Google Scholar 

  18. C. G. Slough, TA Instruments, Analytical Note TA 277: Characteristics of Tg Detection Using Micro-Thermomechanical Analysis, 1999.

  19. D. M. Price, M. Reading, A. Hammiche and H. M. Pollock, Int. J. Pharm., 192 (1999) 85.

    Article  CAS  Google Scholar 

  20. P. G. Royall, D. Q. M. Craig and D. B. Grandy, Thermochim. Acta, 380 (2001) 165.

    Article  CAS  Google Scholar 

  21. A. Hammiche, L. Bozec, M. Conroy, H. M. Pollock, G. Mills, J. M. R. Weaver, D. M. Price, M. Reading, D. J. Hourston and M. Song, J. Vac. Sci. Technol., B18 (2000) 1322.

    Google Scholar 

  22. J. R. Murphy, C. S. Andrews and D. Q. M. Craig, Pharm. Res., 20 (2003) 500.

    Article  CAS  Google Scholar 

  23. R. L. Blaine, C. G. Slough and D. M. Price, Micro-thermal analysis calibration, repeatability and reproducibility, Proc. 27th Conference of the North American Thermal Analysis Society. Savannah, GA, USA 1999, p. 691.

  24. J. Brandrup, E. H. Immergut, E. A. Grulke, A. Abe and D. R. Bloch, Polymer Handbook (4th Ed.), 2005 John Wiley and Sons.

  25. Y. Ding, A. Kisliuk and A. P. Sokolov, Macromolecules, 37 (2004) 161.

    Article  CAS  Google Scholar 

  26. L. H. Sperling, Introduction to Polymer Physics, John Wiley and Sons, New York 1992.

    Google Scholar 

Download references

Author information

Authors and Affiliations

  1. TNO Science and Industry, Materials Performance, P.O. Box 6235, 5600, HE Eindhoven, The Netherlands

    H. Fischer

Authors
  1. H. Fischer
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to H. Fischer.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Fischer, H. Calibration of micro-thermal analysis for the detection of glass transition temperatures and melting points. J Therm Anal Calorim 92, 625–630 (2008). https://doi.org/10.1007/s10973-007-8554-1

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10973-007-8554-1

Keywords

Search

Navigation