The Surface Characterization of Nanosized Powders: Relevance of the FTIR Surface Spectrometry

  • Marie-Isabelle Baraton
Part of the NATO ASI Series book series (ASHT, volume 50)


Even though the study of the bulk properties of crystalline solids is facilitated by the periodicity existing in the lattice, the control of the surface properties and of the interface behavior still represents a challenge to scientists. Techniques to investigate the specific structure and composition of the first atomic layers are very often derived from bulk analysis methods. As a consequence, the minimum depth that can be analyzed, although adequate for traditional materials, may be too large for nanosized materials in which crystal sizes can be smaller than the depth resolution of the characterization technique. Fourier transform infrared (FTIR) spectrometry, widely used for bulk analyses, is, however, a powerful tool to characterize the very first atomic layer provided specific setups are attached to the spectrometer. Several examples will be discussed in the following showing the specific nature of the surface and the relevance of the FTIR spectrometry for obtaining detailed information on the chemical species and the atoms constituting the first atomic layer as well as the coordination number of the surface atoms. Moreover, because of the important role played by the nanomaterial surface in many industrial applications, the surface modifications are a key issue to tailor the surface properties. To this end, FTIR surface spectrometry is also a performant technique to follow the modification of the surface chemical species and to study in situ the selectivity and the behavior of the modifications under various treatments.


Surface Enhance Raman Spectroscopy Atomic Layer Aluminum Nitride Surface Species Aluminum Atom 
These keywords were added by machine and not by the authors. This process is experimental and the keywords may be updated as the learning algorithm improves.


Unable to display preview. Download preview PDF.

Unable to display preview. Download preview PDF.


  1. 1.
    Alvarez, J. and Asensio, M.C. (1990) Electronic structure and composition of surfaces, in Spectroscopic characterization of heterogeneous catalysis (Part A), J.L.G. Fierro Ed, Elsevier, Amsterdam, pp. A79 - A160.CrossRefGoogle Scholar
  2. 2.
    Morterra, C. and Magnacca, G. (1996) A case study: surface chemistry and surface structure of catalytic aluminas, as studied by vibrational spectroscopy of adsorbed species, Catalysis Today 27, 497–532.CrossRefGoogle Scholar
  3. 3.
    Rheis, K. (1995) Nanostructures in industrial materials, Thin Solid Films 264, 135–140.CrossRefGoogle Scholar
  4. 4.
    Veprek, S. (1997) Electronic and mechanical properties of nanocrystalline composites when approaching molecular size, Thin Solid Films 297, 145–153.CrossRefGoogle Scholar
  5. 5.
    Busca, G. (1996) The use of vibrational spectroscopies in studies of heterogeneous catalysis by metal oxides: an introduction, Catalysis Today 27, 323–352.CrossRefGoogle Scholar
  6. 6.
    Fierro, J.L.G. (1990) Surface spectroscopic techniques, in Spectroscopic characterization of heterogeneous catalysis (Part A), J.L.G. Fierro Ed, Elsevier, Amsterdam, pp. Al-A78.Google Scholar
  7. 7.
    Prutton, M. (1994) Introduction to surface physics, Oxford University Press, Oxford (UK).Google Scholar
  8. 8.
    Boehm, 11.-P. and Knözinger, H. (1983) Nature and estimation of functional groups on solid surfaces, in Catalysis V.4, J.R.A. Anderson and M. Boudart Eds, Springer Verlag, Berlin, pp. 39–207.CrossRefGoogle Scholar
  9. 9.
    Conesa, J.C., Esteban, P., Dexpert, H. and Bazin, D. (1990) Characterization of catalyst structures by extended X-ray absorption spectroscopy, in Spectroscopic characterization of heterogeneous catalysis (Part A), J.L.G. Fierro Ed, Elsevier, Amsterdam, pp. A225 - A297.CrossRefGoogle Scholar
  10. 10.
    Yu, E.T. (1996) Nanoscale characterization of semiconductor materials and devices using scanning probe techniques, Materials Science and Engineering R17, 147–206.Google Scholar
  11. 11.
    Knözinger, H. (1996) In situ Raman spectroscopy. A powerful tool for studies in selective catalytic oxidation, Catalysis Today 32, 71–80.CrossRefGoogle Scholar
  12. 12.
    Griffiths, P.R. and de Haseth, J.A. (1986) Fourier transform infrared spectrometry, John Wiley & Sons, New-York.Google Scholar
  13. 13.
    Hair, M.L. (1967) Infrared spectroscopy in surface chemistry, M. Dekker, New-York.Google Scholar
  14. 14.
    Basu, P., Ballinger, T.H. and Yates, J.T. Jr (1988) Wide temperature range IR spectroscopy cell for studies of adsorption and desorption on high area solids, Rev. Sci. Instruments 59, 1321–1327.CrossRefGoogle Scholar
  15. 15.
    Baraton, M.-I. (1994) Infrared and Raman characterization of nanophase ceramic materials, High Temperature and Chemical Processes 3, 545–554.Google Scholar
  16. 16.
    Brimmer, P.J., Griffiths, P.R. and Harrick, N.J. (1986) Angular dependence of diffuse reflectance infrared spectra. Part I: FTIR spectrogoniometer, Applied Spectroscopy 40, 258–265.CrossRefGoogle Scholar
  17. 17.
    Hollins, P. (1992) The influence of surface defects on the infrared spectra of adsorbed species, Surface Science Reports 16, 51–94.CrossRefGoogle Scholar
  18. 18.
    Baraton, M.-I., Chen, X. and Gonsalves, K.E. (1996) Application of Fourier transform infrared spectroscopy to nanostructured materials surface characterization, in Nanotechnology-Molecularly designed materials, G.M. Chow and K.E. Gonsalves Eds, ACS Symposium Series 622, Washington DC, pp. 312–333.CrossRefGoogle Scholar
  19. 19.
    Knözinger, H. (1976) Specific poisoning and characterization of catalytically active oxide surfaces, Advances in Catalysis 25, 184–261.CrossRefGoogle Scholar
  20. 20.
    Lavalley, J.C. (1996) Infrared spectrometric studies of the surface basicity of metal oxides and zeolites using adsorbed probe molecules, Catalysis Today 27, 377–401.CrossRefGoogle Scholar
  21. 21.
    Morrow, B.A. (1990) Surface groups on oxides, in Spectroscopic characterization of heterogeneous catalysis (Part A), J.L.G. Fierro Ed, Elsevier, Amsterdam, pp. A161 - A224.CrossRefGoogle Scholar
  22. 22.
    Davydov, A.A. (1984) Infrared spectroscopy of adsorbed species on the surface of transition metal oxides, John Wiley & Sons, New-York.Google Scholar
  23. 23.
    Baraton, M.-I., Chang, W. and Kear, B.H. (1996) Surface chemical species investigation by FT-IR spectrometry and surface modification of a nanosized SiCN powder synthesized via chemical vapor condensation, J. Physical Chemistry 100, 16647–16652.CrossRefGoogle Scholar
  24. 24.
    Ramis, G., Busca, G., Lorenzelli, V., Baraton, M.-I., Merle-Mejean, T. and Quintard, P. (1989) FT-IR characterization of high surface area silicon nitride and carbide, in Surfaces and Interfaces of ceramic materials, L.-C. Dufour et al. Eds, Kluwer Academic Publishers, Dordrecht, 173–184.CrossRefGoogle Scholar
  25. 25.
    Baraton, M.-I., Chen, X. and Gonsalves, K.E. (1996) FTIR analysis of the surface of nanostructured aluminum nitride powder prepared via chemical synthesis, J. Materials Chemistry 6, 1407–1412.CrossRefGoogle Scholar
  26. 26.
    Baraton, M.-I., Chen, X. and Gonsalves, K.E. (1997) FT-IR characterization of the acidic and basic sites on a nanostructured aluminum nitride surface, Proceedings MRS Fall Meeting 1996 Symposium S, MRS Ed, Pittsburgh, in press.Google Scholar
  27. 27.
    Whitesides, G.M. and Laibinis, P.E. (1990) Wet chemical approaches to the characterization of organic surfaces: self-assembled monolayers, wetting, and the physical-organic chemistry of the solid-liquid interface, Langmuir 6, 87–96.CrossRefGoogle Scholar
  28. 28.
    Baraton, M.-I., Chancel, F. and Merhari, L. (1997) In situ determination of the grafting sites on nanosized ceramic powders by FT-IR spectrometry, Nanostructured Materials 9, 319–322.CrossRefGoogle Scholar
  29. 29.
    Baraton, M.-I., Carlson, G. and Gonsalves, K.E. (1997) DRIFTS characterization of a nanostructured gallium nitride powder and its interactions with organic molecules, Materials Science & Engineering B, in press.Google Scholar

Copyright information

© Springer Science+Business Media Dordrecht 1998

Authors and Affiliations

  • Marie-Isabelle Baraton
    • 1
  1. 1.Faculty of Sciences, LMCTS - ESA 6015 CNRSUniversity of LimogesLimogesFrance

Personalised recommendations