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Title: Inference of the phase-to-mechanical property link via coupled X-ray spectrometry and indentation analysis: Application to cement-based materials

Abstract

A novel approach for the chemo-mechanical characterization of cement-based materials is presented, which combines the classical grid indentation technique with elemental mapping by scanning electron microscopy-energy dispersive X-ray spectrometry (SEM-EDS). It is illustrated through application to an oil-well cement system with siliceous filler. The characteristic X-rays of major elements (silicon, calcium and aluminum) are measured over the indentation region and mapped back on the indentation points. Measured intensities together with indentation hardness and modulus are considered in a clustering analysis within the framework of Finite Mixture Models with Gaussian component density function. The method is able to successfully isolate the calcium-silica-hydrate gel at the indentation scale from its mixtures with other products of cement hydration and anhydrous phases; thus providing a convenient means to link mechanical response to the calcium-to-silicon ratio quantified independently via X-ray wavelength dispersive spectroscopy. A discussion of uncertainty quantification of the estimated chemo-mechanical properties and phase volume fractions, as well as the effect of chemical observables on phase assessment is also included.

Authors:
;  [1];  [2];  [3];  [1]
  1. Department of Civil and Environmental Engineering, Massachusetts Institute of Technology, 77 Massachusetts Avenue, Cambridge, MA 02139-4307 (United States)
  2. Schlumberger Riboud Product Center, 1 Rue Henri Becquerel, Clamart 92140 (France)
  3. Schlumberger-Doll Research Center, 1 Hampshire St., Cambridge, MA 02139-1578 (United States)
Publication Date:
OSTI Identifier:
22395948
Resource Type:
Journal Article
Journal Name:
Cement and Concrete Research
Additional Journal Information:
Journal Volume: 67; Other Information: Copyright (c) 2014 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; Country of input: International Atomic Energy Agency (IAEA); Journal ID: ISSN 0008-8846
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; ALUMINIUM; CALCIUM; CEMENTS; DENSITY; GRIDS; HARDNESS; HYDRATION; MIXTURES; MULTIVARIATE ANALYSIS; SCANNING ELECTRON MICROSCOPY; SILICA; SILICON; SIMULATION; X RADIATION; X-RAY SPECTROSCOPY

Citation Formats

Krakowiak, Konrad J., Wilson, William, James, Simon, Musso, Simone, and Ulm, Franz-Josef. Inference of the phase-to-mechanical property link via coupled X-ray spectrometry and indentation analysis: Application to cement-based materials. United States: N. p., 2015. Web. doi:10.1016/J.CEMCONRES.2014.09.001.
Krakowiak, Konrad J., Wilson, William, James, Simon, Musso, Simone, & Ulm, Franz-Josef. Inference of the phase-to-mechanical property link via coupled X-ray spectrometry and indentation analysis: Application to cement-based materials. United States. https://doi.org/10.1016/J.CEMCONRES.2014.09.001
Krakowiak, Konrad J., Wilson, William, James, Simon, Musso, Simone, and Ulm, Franz-Josef. 2015. "Inference of the phase-to-mechanical property link via coupled X-ray spectrometry and indentation analysis: Application to cement-based materials". United States. https://doi.org/10.1016/J.CEMCONRES.2014.09.001.
@article{osti_22395948,
title = {Inference of the phase-to-mechanical property link via coupled X-ray spectrometry and indentation analysis: Application to cement-based materials},
author = {Krakowiak, Konrad J. and Wilson, William and James, Simon and Musso, Simone and Ulm, Franz-Josef},
abstractNote = {A novel approach for the chemo-mechanical characterization of cement-based materials is presented, which combines the classical grid indentation technique with elemental mapping by scanning electron microscopy-energy dispersive X-ray spectrometry (SEM-EDS). It is illustrated through application to an oil-well cement system with siliceous filler. The characteristic X-rays of major elements (silicon, calcium and aluminum) are measured over the indentation region and mapped back on the indentation points. Measured intensities together with indentation hardness and modulus are considered in a clustering analysis within the framework of Finite Mixture Models with Gaussian component density function. The method is able to successfully isolate the calcium-silica-hydrate gel at the indentation scale from its mixtures with other products of cement hydration and anhydrous phases; thus providing a convenient means to link mechanical response to the calcium-to-silicon ratio quantified independently via X-ray wavelength dispersive spectroscopy. A discussion of uncertainty quantification of the estimated chemo-mechanical properties and phase volume fractions, as well as the effect of chemical observables on phase assessment is also included.},
doi = {10.1016/J.CEMCONRES.2014.09.001},
url = {https://www.osti.gov/biblio/22395948}, journal = {Cement and Concrete Research},
issn = {0008-8846},
number = ,
volume = 67,
place = {United States},
year = {Thu Jan 15 00:00:00 EST 2015},
month = {Thu Jan 15 00:00:00 EST 2015}
}