Early hydration and microstructure formation of Portland cement paste studied by oscillation rheology, isothermal calorimetry, 1H NMR relaxometry, conductance and SAXS

Research output: Contribution to journalArticleResearchpeer review

Authors

  • A. Bogner
  • J. Link
  • M. Baum
  • M. Mahlbacher
  • T. Gil-Diaz
  • J. Lützenkirchen
  • T. Sowoidnich
  • F. Heberling
  • T. Schäfer
  • H.-M. Ludwig
  • F. Dehn
  • H.S. Müller
  • M. Haist

External Research Organisations

  • Karlsruhe Institute of Technology (KIT)
  • Friedrich Schiller University Jena
  • Bauhaus-Universität Weimar
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Details

Original languageEnglish
Article number105977
JournalCement and concrete research
Volume130
Early online date24 Jan 2020
Publication statusPublished - Apr 2020

Abstract

An open question in predicting the rheological properties of cement suspensions has been whether changes of rheology during hydration are merely a result of shifts in the electrostatic interaction patterns of the particles over time, or whether and to which extent steric bridging by hydration products occurs. The latter could explain phenomena such as thixotropy. In this context, parallel investigations using both rheological tests and isothermal calorimetry, 1H NMR relaxometry, conductance and small-angle X-ray scattering (SAXS) measurments were carried out. It could be shown that as early as approx. 2.5 h after water addition at approx. 30 °C, small amounts of Calcium Silicate Hydrate (C-S-H) form which may contribute to a bridging of the cement particles. This phase is followed by rapid C-S-H formation, leading to a non-linear increase in paste stiffness. This phase ends with percolation, i.e. the paste stiffness increases dramatically, simultaneously with the formation of gel pore like structures, which could be observed using NMR.

Keywords

    Hydration, Microstructure, Opus Fluidum Futurum, Rheology, Small-angle X-ray scattering

ASJC Scopus subject areas

Cite this

Early hydration and microstructure formation of Portland cement paste studied by oscillation rheology, isothermal calorimetry, 1H NMR relaxometry, conductance and SAXS. / Bogner, A.; Link, J.; Baum, M. et al.
In: Cement and concrete research, Vol. 130, 105977, 04.2020.

Research output: Contribution to journalArticleResearchpeer review

Bogner, A, Link, J, Baum, M, Mahlbacher, M, Gil-Diaz, T, Lützenkirchen, J, Sowoidnich, T, Heberling, F, Schäfer, T, Ludwig, H-M, Dehn, F, Müller, HS & Haist, M 2020, 'Early hydration and microstructure formation of Portland cement paste studied by oscillation rheology, isothermal calorimetry, 1H NMR relaxometry, conductance and SAXS', Cement and concrete research, vol. 130, 105977. https://doi.org/10.1016/j.cemconres.2020.105977
Bogner, A., Link, J., Baum, M., Mahlbacher, M., Gil-Diaz, T., Lützenkirchen, J., Sowoidnich, T., Heberling, F., Schäfer, T., Ludwig, H.-M., Dehn, F., Müller, H. S., & Haist, M. (2020). Early hydration and microstructure formation of Portland cement paste studied by oscillation rheology, isothermal calorimetry, 1H NMR relaxometry, conductance and SAXS. Cement and concrete research, 130, Article 105977. https://doi.org/10.1016/j.cemconres.2020.105977
Bogner A, Link J, Baum M, Mahlbacher M, Gil-Diaz T, Lützenkirchen J et al. Early hydration and microstructure formation of Portland cement paste studied by oscillation rheology, isothermal calorimetry, 1H NMR relaxometry, conductance and SAXS. Cement and concrete research. 2020 Apr;130:105977. Epub 2020 Jan 24. doi: 10.1016/j.cemconres.2020.105977
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title = "Early hydration and microstructure formation of Portland cement paste studied by oscillation rheology, isothermal calorimetry, 1H NMR relaxometry, conductance and SAXS",
abstract = "An open question in predicting the rheological properties of cement suspensions has been whether changes of rheology during hydration are merely a result of shifts in the electrostatic interaction patterns of the particles over time, or whether and to which extent steric bridging by hydration products occurs. The latter could explain phenomena such as thixotropy. In this context, parallel investigations using both rheological tests and isothermal calorimetry, 1H NMR relaxometry, conductance and small-angle X-ray scattering (SAXS) measurments were carried out. It could be shown that as early as approx. 2.5 h after water addition at approx. 30 °C, small amounts of Calcium Silicate Hydrate (C-S-H) form which may contribute to a bridging of the cement particles. This phase is followed by rapid C-S-H formation, leading to a non-linear increase in paste stiffness. This phase ends with percolation, i.e. the paste stiffness increases dramatically, simultaneously with the formation of gel pore like structures, which could be observed using NMR.",
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note = "Funding Information: The funding of Deutsche Forschungsgemeinschaft provided to Michael Haist, Thorsten Sch{\"a}fer and Michael Ludwig under the grants HA 7917/3-1 , SCHA 1854/4-1 and LU 1652/32-1 is gratefully acknowledged. Harald M{\"u}ller gratefully acknowledges the funding of 1 Deutsche Forschungsgemeinschaft for the SAXS instrument under the grant INST 121384/71-1 FUGG . Harald M{\"u}ller and Michael Haist gratefully acknowledge the funding of the Helmholtz Association within the Programme EMR for support in the SAXS measurements. The authors further thank Wittekind Hugo Miesbach S{\"o}hne KG for providing the cement.",
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AU - Bogner, A.

AU - Link, J.

AU - Baum, M.

AU - Mahlbacher, M.

AU - Gil-Diaz, T.

AU - Lützenkirchen, J.

AU - Sowoidnich, T.

AU - Heberling, F.

AU - Schäfer, T.

AU - Ludwig, H.-M.

AU - Dehn, F.

AU - Müller, H.S.

AU - Haist, M.

N1 - Funding Information: The funding of Deutsche Forschungsgemeinschaft provided to Michael Haist, Thorsten Schäfer and Michael Ludwig under the grants HA 7917/3-1 , SCHA 1854/4-1 and LU 1652/32-1 is gratefully acknowledged. Harald Müller gratefully acknowledges the funding of 1 Deutsche Forschungsgemeinschaft for the SAXS instrument under the grant INST 121384/71-1 FUGG . Harald Müller and Michael Haist gratefully acknowledge the funding of the Helmholtz Association within the Programme EMR for support in the SAXS measurements. The authors further thank Wittekind Hugo Miesbach Söhne KG for providing the cement.

PY - 2020/4

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N2 - An open question in predicting the rheological properties of cement suspensions has been whether changes of rheology during hydration are merely a result of shifts in the electrostatic interaction patterns of the particles over time, or whether and to which extent steric bridging by hydration products occurs. The latter could explain phenomena such as thixotropy. In this context, parallel investigations using both rheological tests and isothermal calorimetry, 1H NMR relaxometry, conductance and small-angle X-ray scattering (SAXS) measurments were carried out. It could be shown that as early as approx. 2.5 h after water addition at approx. 30 °C, small amounts of Calcium Silicate Hydrate (C-S-H) form which may contribute to a bridging of the cement particles. This phase is followed by rapid C-S-H formation, leading to a non-linear increase in paste stiffness. This phase ends with percolation, i.e. the paste stiffness increases dramatically, simultaneously with the formation of gel pore like structures, which could be observed using NMR.

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KW - Microstructure

KW - Opus Fluidum Futurum

KW - Rheology

KW - Small-angle X-ray scattering

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JO - Cement and concrete research

JF - Cement and concrete research

SN - 0008-8846

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ER -

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