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Monitoring hydration in lime-metakaolin composites using electrochemical impedance spectroscopy and nuclear magnetic resonance spectroscopy†

Published online by Cambridge University Press:  27 February 2018

G. L. Pesce ,
C. R. Bowen ,
J. Rocha ,
M. Sardo ,
G. C. Allen ,
P. J. Walker ,
G. Denuault ,
M. Serrapede  and
R. J. Ball
G. L. Pesce
Affiliation:
Department of Architecture and Civil Engineering, University of Bath, Bath UK
C. R. Bowen
Affiliation:
Department of Mechanical Engineering, University of Bath, Bath, UK
J. Rocha
Affiliation:
Department of Chemistry, CICECO, University of Aveiro, Aveiro, Portugal
M. Sardo
Affiliation:
Department of Chemistry, CICECO, University of Aveiro, Aveiro, Portugal
G. C. Allen
Affiliation:
Interface Analysis Centre, University of Bristol, Bristol, UK
P. J. Walker
Affiliation:
Department of Architecture and Civil Engineering, University of Bath, Bath UK
G. Denuault
Affiliation:
Department of Chemistry, University of Southampton, Southampton, UK
M. Serrapede
Affiliation:
Department of Chemistry, University of Southampton, Southampton, UK
R. J. Ball*
Affiliation:
Department of Architecture and Civil Engineering, University of Bath, Bath UK
*
*E-mail: R.J.Ball@bath.ac.uk
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Abstract

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This paper describes a study of the hydraulic reactions between metakaolin (MK) and air lime using electrochemical impedance spectroscopy (EIS) and nuclear magnetic resonance spectroscopy (NMR). Tests were carried out at 20, 25 and 30°C on lime-MK pastes with 10:1 w/w ratio. Tests over 28 days allowed identification of relevant changes in the EIS signals and characterization of pastes using thermal analysis (TGA/DSC), scanning electron microscopy (SEM), mercury intrusion porosimetry (MIP) and uni-axial compressive tests. Tests over shorter periods of time (up to 42 h) allowed more detailed studies of the hydraulic phases formed at the very beginning of the reactions.

Results of thermal analyses demonstrate formation of hydraulic compounds such as CSH, C4AH13 and C3ASH6 and show their evolution over time. MIP analysis demonstrates changes in pore size distribution related to the formation and trasformation of hydraulic phases. Variations of impedance response with time are shown to be associated with reaction kinetics. Changes in the NMR signal within the first 42 h of reaction are shown to be associated with the dissolution of calcium hydroxide in the pore solution. Overall, this paper demonstrates the importance of NMR in the study of hydraulic reactions in lime based materials and the ability of EIS to detect the formation of hydraulic compounds and the end of the calcium hydroxide dissolution process.

Keywords

limemetakaolinimpedance spectroscopynuclear magnetic resonance spectroscopy
Type
Research Article
Information
Clay Minerals , Volume 49 , Issue 3 , June 2014 , pp. 341 - 358
Creative Commons
Creative Common License - CCCreative Common License - BY
Copyright © The Mineralogical Society of Great Britain and Ireland 2014 This is an Open Access article, distributed under the terms of the Creative Commons Attribution license. (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted re-use, distribution, and reproduction in any medium, provided the original work is properly cited.
Copyright
Copyright © The Mineralogical Society of Great Britain and Ireland 2014

Footnotes

†

Invited lecture given at the Cement and Concrete 2013 Conference in Portsmouth, September 2013

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