Skip to main content

Advertisement

Log in

Confocal Raman microscopy study of the melamine distribution in polyester–melamine coil coating

  • Published:
Journal of Coatings Technology and Research Aims and scope Submit manuscript

Abstract

Hexamethoxymethylmelamine, a common crosslinker used in combination with polyester resins to prepare thermosetting coatings, can self-condense during curing and in theory build up regions with high crosslink density (melamine enrichment). This distribution may affect such properties as the “local” glass transition temperature and structural heterogeneity and thereby modify formability, stain resistance, and weatherability. The self-condensation regions have not previously been observed in detail so their distribution in the film is unclear. Confocal Raman microscopy (CRM) has been used to characterize the melamine distribution in three polyester–melamine paint systems: one clear and two pigmented coil coatings. Both the surface mapping and depth profiling features of CRM were used to perform a 3D analysis. The depth profiling of the clear coating was performed in a nondestructive way, but due to the opaque nature of the pigments, cross sections of the pigmented coatings were prepared in order to facilitate the analysis of the melamine distribution through the film thickness. Melamine-enriched zones were found on the surfaces of all three samples. They appeared to be approximately spherical with diameters of around 5 μm. It was also observed from the cross sections that the melamine-enriched zones appeared as “particles” distributed randomly through the coating. The Raman spectra collected at these regions show significantly higher triazine ring band intensity. All of these findings confirm the hypotheses constructed over the past 20–30 years.

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

Access this article

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

Instant access to the full article PDF.

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7
Fig. 8
Fig. 9
Fig. 10

Similar content being viewed by others

References

  1. Koral, Jerry N. and Petropulos, John C. 1996 Hexakis (MethoxyMethyl) Melamine: Its Chemistry and Utilization in Surface Coatings”, Journal of Paint Technology, 38, 600–609.

    Google Scholar 

  2. Calbo, Leonard J. 1980 Effect of Catalyst Structure on The Properties of Coatings Cross-linked with Hexa(MethoxyMethyl) Melamine. Journal of Coatings Technology, 52, 75–83.

    CAS  Google Scholar 

  3. Blank, Werner J. 1979 Reaction Mechanism of Melamine Resins”, Journal of Coatings Technology, 51, 61–70.

    CAS  Google Scholar 

  4. Gan, S, Solimeno, RD, Jones, FN, Hill, LW, “Recent Studies of the Curing of Polyester-Melamine Enamels. Possible Causes of Overbake Softening.” Water-Borne and Higher-Solids Coatings Symposium (1989)

  5. Jones, Frank N., Chu, G., and Samaraweera, U. 1994 “Recent Studies of Self-Condensation and Co-Condensation of Melamine-Formaldehyde Resins; Cure at Low Temperatures”, Progress in Organic Coatings, 24, 189–208. doi:10.1016/0033-0655(94)85014-3

    Article  CAS  Google Scholar 

  6. Hirayama, T. and Urban, Marek W. 1992 Distribution of Melamine in Melamine/Polyester Coatings; FT-IR Spectroscopic Studies, Progress in Organic Coatings, 20, 81–96. doi:10.1016/0033-0655(92)85006-H

    Article  CAS  Google Scholar 

  7. Hamada, T., Kanai, H., Koike, T., and Fuda, M. 1997 FTIR Study of Melamine Enrichment in The Surface Region of Polyester/Melamine Film, Progress in Organic Coatings, 30, 271–278. doi:10.1016/S0300-9440(97)00003-9

    Article  CAS  Google Scholar 

  8. Gammage, N. J. W., Hill, D. J. T., Lukey, C. A. and Pomer P. J. 2004 Distribution of Melamine in Polyester-Melamine Surface Coatings Cured Under Nonisothermal Conditions, Journal of Polymer Science, Part A: Polymer Chemistry, 42, 83–91. doi:10.1002/pola.11006

    Article  Google Scholar 

  9. Fleming, O. S., Kazarian, S. G., Bach, E. and Schollmeyer, E. 2005 Confocal Raman Study of Poly(Ethylene Terephthalate) Fibres Dyed in Supercritical Carbon Dioxide: Dye Diffusion and Polymer Morphology. Polymer, 46, 2943–2949. doi:10.1016/j.polymer.2005.02.067

    Article  CAS  Google Scholar 

  10. Schrof, W., Beck, E., Königer, R., Reich, W., and Schwalm, R. 1999 Depth Profiling of UV Cured Coatings Containing Photostabilizers by Confocal Raman Microscopy, Progress in Organic Coatings, 35, 197–204. doi:10.1016/S0300-9440(99)00026-0

    Article  CAS  Google Scholar 

  11. Dupuie, J. L., Weber, W. H., Scholl, D. J. and Gerlock, J. L. 1997 “Clearcoat Analysis in Isolated and Multi-Layer Paint Systems by Confocal Raman Microscopy”, Polymer Degradation and Stability, 57, 339–348. doi:10.1016/S0141-3910(97)00029-3

    Article  CAS  Google Scholar 

  12. Mura, C., Yarwood, J., Swart, R. and Hodge, D. 2000 “Raman Microscopy Studies of The Distribution of The Fungicide Fluorfolpet in Plasticized PVC Films, Polymer, 41, 8659–8671. doi:10.1016/S0032-3861(99)00446-2

    Article  CAS  Google Scholar 

  13. Schmidt, P., Fernandez, M. R., Pastor J. M. and Roda, J. 1997 “Study of the Conformations of Poly (ε-Caprolactam) and Poly (ε-Caprolactam)-Polybytadiene Block Copolymers by FTi.r. Spectroscopy with Photoacoustic Detection and by Micro-Raman Confocal Spectroscopy”, Polymer, 38, 2067–2075. doi:10.1016/S0032-3861(96)00766-5

    Article  CAS  Google Scholar 

  14. Everall, Neil J. 2000 “Modeling and Measuring the Effect of Refraction on the Depth Resolution of Confocal Raman Microscopy”, Applied Spectroscopy, 54, 773–782. doi:10.1366/0003702001950382

    Article  ADS  CAS  Google Scholar 

  15. Everall, Neil J. 2000 “Confocal Raman Microscopy: Why the Depth Resolution and Spatial Accuracy Can Be Much Worse than You Think”, Applied Spectroscopy, 54, 1515–1520. doi:10.1366/0003702001948439

    Article  ADS  CAS  Google Scholar 

  16. Zhang, WR, Lowe, C, Smith, R., “Depth Profiling of Coil Coating by Confocal Raman Microscopy.” Prog. Org. Coat. (2008), submitted

Download references

Acknowledgments

The authors thank Mr. James Maxted and Mr. James Smith (Becker Industrial Coatings, UK) for useful discussions and help, and acknowledge Becker Industrial Coatings for financial support.

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Wanrui Zhang.

Additional information

This paper was awarded Second Place in the 2008 FSCT Roon Awards competition held as part of the FutureCoat! conference sponsored by the Federation of Societies for Coatings Technology, in Chicago, IL, on October 14–16, 2008.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Zhang, W., Smith, R. & Lowe, C. Confocal Raman microscopy study of the melamine distribution in polyester–melamine coil coating. J Coat Technol Res 6, 315–328 (2009). https://doi.org/10.1007/s11998-008-9136-2

Download citation

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s11998-008-9136-2

Keywords

Navigation