Reactivity of Heated Kaolinite from a Combination of Solid State NMR and Chemical Methods

  • Cristina Ruiz-Santaquiteria
  • Jørgen SkibstedEmail author
Conference paper
Part of the RILEM Bookseries book series (RILEM, volume 10)


The effect of the heat-treatment temperature for kaolinite on the types of formed aluminum and silicon sites after dehydroxylation and the relation of these sites to the reactivity of the heated materials are investigated in this work. Kaolinite has been heated to temperatures in the range 500 – 1100 °C in intervals of 50 °C. The reactivity for each sample has been tested in acid media using HF (1 vol.%) and the residues have been stored and dried for further analysis. The heat-treated samples and their corresponding residues are analyzed by solid-state 29Si and 27Al MAS NMR, where comparison of the spectra for the heated clay and the residue provide information about the structurally reactive sites. The chemical methods indicate that kaolinite reaches its maximum reactivity at ~800 °C. The reactivity decreases at higher temperatures as a consequence of the formation of spinel-type and mullite phases, as deduced by 27Al NMR and by the evolution with temperature of the Si/Al ratio for the dissolved phase, determined by ICP analysis. Comparison of normalized 29Si and 27Al NMR spectra for the heated samples and their residues provides the basis for a clear differentiation between different silicon and aluminum environments present in the samples. The 27Al NMR spectra suggest the presence of different tetrahedral aluminum sites and that these sites are correlated with different silicon environments, suggesting that Q3 and Q4 silicon sites coexist in metakaolin.


Heated Sample Mullite Phase Kaolinite Sample Silicon Site Amorphous Silica Phase 
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.



The Danish Council for Strategic Research is acknowledged for financial support to the LowE-CEM project.


  1. 1.
    Ramachandran, V.S., Paroli, R.M., Beaudoin, J.J, Delgado, A.H.: Handbook of Thermal Analysis of Construction Materials, 1st edn. Noyes publications (2002)Google Scholar
  2. 2.
    Meinhold, R.H., MacKenzie, K.J.D., Brown, I.W.M.: Thermal reactions of kaolinite studied by solid state 27Al and 29Si NMR. J. Mater. Sci. Lett. 4, 163–166 (1985)CrossRefGoogle Scholar
  3. 3.
    Rocha, J., Klinowski, J.: 29Si and 27Al magic-angle-spinning NMR studies of the thermal transformation of kaolinite. Phys. Chem. Miner. 17, 179–186 (1990)CrossRefGoogle Scholar
  4. 4.
    Sanz, J., Madani, A., Serratosa, J.M., Moya, J.S., Aza, S.: Aluminum-27 and Silicon-29 magic-angle spinning nuclear magnetic resonance study of the kaolinite-mullite transformations. J. Am. Ceram. Soc. 71, 418–421 (1988)CrossRefGoogle Scholar
  5. 5.
    Engelhardt, G., Michel, D.: High-Resolution Solid-State NMR of Silicates and Zeolites. Wiley, New York (1987)Google Scholar

Copyright information

© RILEM 2015

Authors and Affiliations

  1. 1.Instrument Centre for Solid-State NMR Spectroscopy, Department of Chemistry and Interdisciplinary Nanoscience Center (iNANO)Aarhus UniversityAarhus CDenmark

Personalised recommendations