Time-resolved 3D characterisation of early-age microstructural development of Portland cement

Vigor, James E.; Bernal, Susan A.; Xiao, Xianghui; Provis, John L.

doi:10.1007/s10853-022-06952-z

Title: Time-resolved 3D characterisation of early-age microstructural development of Portland cement

Journal Article · 09 February 2022 · Journal of Materials Science

DOI: https://doi.org/10.1007/s10853-022-06952-z · OSTI ID:1844438

Vigor, James E.; Bernal, Susan A.; Xiao, Xianghui;

Abstract Time-resolved in-situ synchrotron X-ray microtomography reveals new levels of detail about the chemical and physical processes that take place as Portland cement hardens. The conversion of a fluid paste into a hardened product can be monitored on a sub-minute time-scale, and with sample movement/settlement corrections applied to enable individual particles to be tracked as they react, hydrate, and become interconnected into a single strong monolith. The growth of the strength-giving hydrate phases surrounding cement grains, and of the fluid-filled pore network that surrounds them, is able to be directly viewed at the level of individual cement particles through the application of this tracking protocol. When cement is brought into contact with water, a layer which differs in density from the bulk of the cement grains becomes observable on the grain surfaces during the induction period (during which time the heat evolution from the paste is relatively low). As hydration continues, reaction products grow both from particle surfaces into the initially fluid-filled region, and also into the space originally occupied by the cement particles, forming a density gradient within the microstructure. As the reaction accelerates and larger volumes of solid phases precipitate, the newly-formed solid structure percolates via interconnection of agglomerated low-density outer hydrates, which then densify as hydration continues. This eventually leads to solidification of the structure into a hardened porous matrix. Graphical abstract

View Journal Article

Cite

Export

Save

Research Organization:: Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS)

Sponsoring Organization:: Engineering and Physical Sciences Research Council (EPSRC); Nuclear Decommissioning Authority (NDA); USDOE; USDOE Office of Science (SC), Basic Energy Sciences (BES). Scientific User Facilities Division

Grant/Contract Number:: AC02-06CH11357

OSTI ID:: 1844438

Journal Information:: Journal of Materials Science, Journal Name: Journal of Materials Science Journal Issue: 8 Vol. 57; ISSN 0022-2461

Publisher:: Springer Science + Business MediaCopyright Statement

Country of Publication:: United States

Language:: English

References (53)

First Seconds in a Building’s Life-In Situ Synchrotron X-Ray Diffraction Study of Cement Hydration on the Millisecond Timescale Schlegel, Moritz-Caspar; Sarfraz, Adnan; Müller, Urs Angewandte Chemie International Edition, Vol. 51, Issue 20 https://doi.org/10.1002/anie.201200993	journal	April 2012
Influence of silica on the hydration of 3 CaO,SiO2 Stein, H. N.; Stevels, J. M. Journal of Applied Chemistry, Vol. 14, Issue 8 https://doi.org/10.1002/jctb.5010140805	journal	August 1964
In Situ Experiments with X ray Tomography: an Attractive Tool for Experimental Mechanics Buffiere, J. -Y.; Maire, E.; Adrien, J. Experimental Mechanics, Vol. 50, Issue 3 https://doi.org/10.1007/s11340-010-9333-7	journal	January 2010
Some general considerations of a membrane/osmosis model for portland cement hydration Birchall, J. D.; Howard, A. J.; Double, D. D. Cement and Concrete Research, Vol. 10, Issue 2 https://doi.org/10.1016/0008-8846(80)90071-X	journal	March 1980
Effect of alkalies on portland cement hydration II. Alkalies present in form of sulphates Odler, I.; Wonnemann, R. Cement and Concrete Research, Vol. 13, Issue 6 https://doi.org/10.1016/0008-8846(83)90078-9	journal	November 1983
A kinetic model for the hydration of tricalcium silicate Brown, Paul Wencil; Pommersheim, James; Frohnsdorff, Geoffrey Cement and Concrete Research, Vol. 15, Issue 1 https://doi.org/10.1016/0008-8846(85)90006-7	journal	January 1985
Percolation of phases in a three-dimensional cement paste microstructural model Bentz, Dale P.; Garboczi, Edward J. Cement and Concrete Research, Vol. 21, Issue 2-3 https://doi.org/10.1016/0008-8846(91)90014-9	journal	March 1991
Backscattered electron imaging of cementitious microstructures: understanding and quantification Scrivener, Karen L. Cement and Concrete Composites, Vol. 26, Issue 8 https://doi.org/10.1016/j.cemconcomp.2004.02.029	journal	November 2004
Visualization and quantification of pore structure of oil-well cement slurry in liquid-solid transition stage using high-resolution computed tomography Liu, Kaiqiang; Cheng, Xiaowei; Ma, Yong Cement and Concrete Composites, Vol. 111 https://doi.org/10.1016/j.cemconcomp.2020.103633	journal	August 2020
A colloidal interpretation of chemical aging of the C-S-H gel and its effects on the properties of cement paste Thomas, Jeffrey J.; Jennings, Hamlin M. Cement and Concrete Research, Vol. 36, Issue 1 https://doi.org/10.1016/j.cemconres.2004.10.022	journal	January 2006
X-ray microtomography: Application to microstructure analysis of a cementitious material during leaching process Burlion, Nicolas; Bernard, Dominique; Chen, Da Cement and Concrete Research, Vol. 36, Issue 2 https://doi.org/10.1016/j.cemconres.2005.04.008	journal	February 2006
The calcium silicate hydrates Richardson, I. G. Cement and Concrete Research, Vol. 38, Issue 2 https://doi.org/10.1016/j.cemconres.2007.11.005	journal	February 2008
Quantification of tortuosity in hardened cement pastes using synchrotron-based X-ray computed microtomography Promentilla, M. A. B.; Sugiyama, T.; Hitomi, T. Cement and Concrete Research, Vol. 39, Issue 6 https://doi.org/10.1016/j.cemconres.2009.03.005	journal	June 2009
Microstructural development of early age hydration shells around cement grains Gallucci, E.; Mathur, P.; Scrivener, K. Cement and Concrete Research, Vol. 40, Issue 1 https://doi.org/10.1016/j.cemconres.2009.09.015	journal	January 2010
Dissolution theory applied to the induction period in alite hydration Juilland, Patrick; Gallucci, Emmanuel; Flatt, Robert Cement and Concrete Research, Vol. 40, Issue 6 https://doi.org/10.1016/j.cemconres.2010.01.012	journal	June 2010
Mechanisms of cement hydration Bullard, Jeffrey W.; Jennings, Hamlin M.; Livingston, Richard A. Cement and Concrete Research, Vol. 41, Issue 12 https://doi.org/10.1016/j.cemconres.2010.09.011	journal	December 2011
X-ray microtomography shows pore structure and tortuosity in alkali-activated binders Provis, John L.; Myers, Rupert J.; White, Claire E. Cement and Concrete Research, Vol. 42, Issue 6 https://doi.org/10.1016/j.cemconres.2012.03.004	journal	June 2012
Dissolution rates during the early hydration of tricalcium silicate Bellmann, Frank; Sowoidnich, Thomas; Ludwig, Horst-Michael Cement and Concrete Research, Vol. 72 https://doi.org/10.1016/j.cemconres.2015.02.002	journal	June 2015
A new view on the kinetics of tricalcium silicate hydration Nicoleau, L.; Nonat, A. Cement and Concrete Research, Vol. 86 https://doi.org/10.1016/j.cemconres.2016.04.009	journal	August 2016
Direct three-dimensional observation of the microstructure and chemistry of C3S hydration Hu, Qinang; Aboustait, Mohammed; Kim, Taehwan Cement and Concrete Research, Vol. 88 https://doi.org/10.1016/j.cemconres.2016.07.006	journal	October 2016
Use of iodine for improving phase quantification using x-ray tomography Deboodt, Tyler; Wildenschild, Dorthe; Ideker, Jason H. Cement and Concrete Research, Vol. 116 https://doi.org/10.1016/j.cemconres.2018.11.004	journal	February 2019
Advances in understanding cement hydration mechanisms Scrivener, Karen; Ouzia, Alexandre; Juilland, Patrick Cement and Concrete Research, Vol. 124 https://doi.org/10.1016/j.cemconres.2019.105823	journal	October 2019
Multiscale X-ray tomography of cementitious materials: A review Brisard, Sébastien; Serdar, Marijana; Monteiro, Paulo J. M. Cement and Concrete Research, Vol. 128 https://doi.org/10.1016/j.cemconres.2019.105824	journal	February 2020
Automated correction for the movement of suspended particulate in microtomographic data Vigor, James E.; Bernal, Susan A.; Xiao, Xianghui Chemical Engineering Science, Vol. 223 https://doi.org/10.1016/j.ces.2020.115736	journal	September 2020
In situ synchrotron X-ray powder diffraction study of the early age hydration of cements blended with zeolitite and quartzite fines and water-reducing agent Snellings, R.; Mertens, G.; Adriaens, R. Applied Clay Science, Vol. 72 https://doi.org/10.1016/j.clay.2012.12.002	journal	February 2013
Multi-scale observations of structure and chemical composition changes of portland cement systems during hydration Moradian, Masoud; Hu, Qinang; Aboustait, Mohammed Construction and Building Materials, Vol. 212 https://doi.org/10.1016/j.conbuildmat.2019.04.013	journal	July 2019
Permeability prediction and pore structure feature of pervious concrete using brick as aggregate Debnath, Barnali; Sarkar, Partha Pratim Construction and Building Materials, Vol. 213 https://doi.org/10.1016/j.conbuildmat.2019.04.099	journal	July 2019
Comparison of thresholding techniques for quantifying portland cement hydrates using synchrotron microtomography Deboodt, Tyler; Wildenschild, Dorthe; Ideker, Jason H. Construction and Building Materials, Vol. 266 https://doi.org/10.1016/j.conbuildmat.2020.121109	journal	January 2021
Representative elementary volume analysis of hardened cement paste during hydration using X-ray Computed Tomography Fan, Meicen; Chen, Yue; Wan, Keshu Construction and Building Materials, Vol. 277 https://doi.org/10.1016/j.conbuildmat.2021.122268	journal	March 2021
Imaging and image-based fluid transport modeling at the pore scale in geological materials: A practical introduction to the current state-of-the-art Bultreys, Tom; De Boever, Wesley; Cnudde, Veerle Earth-Science Reviews, Vol. 155 https://doi.org/10.1016/j.earscirev.2016.02.001	journal	April 2016
A brief guide to synchrotron radiation-based microtomography in (structural) geology and rock mechanics Fusseis, F.; Xiao, X.; Schrank, C. Journal of Structural Geology, Vol. 65 https://doi.org/10.1016/j.jsg.2014.02.005	journal	August 2014
Evaluating the chloride diffusion coefficient of cement mortars based on the tortuosity of pore structurally-designed cement pastes Guo, Yiqun; Zhang, Tongsheng; Du, Junpeng Microporous and Mesoporous Materials, Vol. 317 https://doi.org/10.1016/j.micromeso.2021.111018	journal	April 2021
pytrax: A simple and efficient random walk implementation for calculating the directional tortuosity of images Tranter, T. G.; Kok, M. D. R.; Lam, M. SoftwareX, Vol. 10 https://doi.org/10.1016/j.softx.2019.100277	journal	July 2019
Calculation of the Compounds in Portland Cement Bogue, R. H. Industrial & Engineering Chemistry Analytical Edition, Vol. 1, Issue 4 https://doi.org/10.1021/ac50068a006	journal	October 1929
Understanding silicate hydration from quantitative analyses of hydrating tricalcium silicates Pustovgar, Elizaveta; Sangodkar, Rahul P.; Andreev, Andrey S. Nature Communications, Vol. 7, Issue 1 https://doi.org/10.1038/ncomms10952	journal	March 2016
The crucial effect of early-stage gelation on the mechanical properties of cement hydrates Ioannidou, Katerina; Kanduč, Matej; Li, Lunna Nature Communications, Vol. 7, Issue 1 https://doi.org/10.1038/ncomms12106	journal	July 2016
Fiji: an open-source platform for biological-image analysis Schindelin, Johannes; Arganda-Carreras, Ignacio; Frise, Erwin Nature Methods, Vol. 9, Issue 7 https://doi.org/10.1038/nmeth.2019	journal	June 2012
Simultaneous phase and amplitude extraction from a single defocused image of a homogeneous object Paganin, D.; Mayo, S. C.; Gureyev, T. E. Journal of Microscopy, Vol. 206, Issue 1 https://doi.org/10.1046/j.1365-2818.2002.01010.x	journal	April 2002
Beamline I11 at Diamond: A new instrument for high resolution powder diffraction Thompson, S. P.; Parker, J. E.; Potter, J. Review of Scientific Instruments, Vol. 80, Issue 7 https://doi.org/10.1063/1.3167217	journal	July 2009
Recent studies of cements and concretes by synchrotron radiation crystallographic and cognate methods Aranda, Miguel A. G. Crystallography Reviews, Vol. 22, Issue 3 https://doi.org/10.1080/0889311X.2015.1070260	journal	September 2015
Metamorphosis revealed: time-lapse three-dimensional imaging inside a living chrysalis Lowe, Tristan; Garwood, Russell J.; Simonsen, Thomas J. Journal of The Royal Society Interface, Vol. 10, Issue 84 https://doi.org/10.1098/rsif.2013.0304	journal	July 2013
Fast X-ray powder diffraction on I11 at Diamond Thompson, Stephen P.; Parker, Julia E.; Marchal, Julien Journal of Synchrotron Radiation, Vol. 18, Issue 4 https://doi.org/10.1107/S0909049511013641	journal	May 2011
TomoPy: a framework for the analysis of synchrotron tomographic data Gürsoy, Dogˇa; De Carlo, Francesco; Xiao, Xianghui Journal of Synchrotron Radiation, Vol. 21, Issue 5 https://doi.org/10.1107/S1600577514013939	journal	August 2014
Developments in synchrotron x-ray computed microtomography at the National Synchrotron Light Source Dowd, Betsy A.; Campbell, Graham H.; Marr, Robert B. SPIE's International Symposium on Optical Science, Engineering, and Instrumentation, SPIE Proceedings https://doi.org/10.1117/12.363725	conference	September 1999
X-ray tomography system, automation, and remote access at beamline 2-BM of the Advanced Photon Source De Carlo, Francesco; Xiao, Xianghui; Tieman, Brian SPIE Optics + Photonics, SPIE Proceedings https://doi.org/10.1117/12.681037	conference	August 2006
A high-level 3D visualization API for Java and ImageJ Schmid, Benjamin; Schindelin, Johannes; Cardona, Albert BMC Bioinformatics, Vol. 11, Issue 1 https://doi.org/10.1186/1471-2105-11-274	journal	May 2010
Stripe and ring artifact removal with combined wavelet—Fourier filtering Münch, Beat; Trtik, Pavel; Marone, Federica Optics Express, Vol. 17, Issue 10 https://doi.org/10.1364/OE.17.008567	journal	January 2009
In Vivo Time-Resolved Microtomography Reveals the Mechanics of the Blowfly Flight Motor Walker, Simon M.; Schwyn, Daniel A.; Mokso, Rajmund PLoS Biology, Vol. 12, Issue 3 https://doi.org/10.1371/journal.pbio.1001823	journal	March 2014
X-Ray Microtomography of an Astm C109 Mortar Exposed to Sulfate Attack Bentz, D. P.; Martys, Nicos. S.; Stutzman, P. MRS Proceedings, Vol. 370 https://doi.org/10.1557/PROC-370-77	journal	January 1994
A new model to calculate water permeability of cement-based materials from MIP results Aït-Mokhtar, A.; Amiri, O.; Dumargue, P. Advances in Cement Research, Vol. 14, Issue 2 https://doi.org/10.1680/adcr.2002.14.2.43	journal	April 2002
Tortuosity in Porous Media: A Critical Review Ghanbarian, Behzad; Hunt, Allen G.; Ewing, Robert P. Soil Science Society of America Journal, Vol. 77, Issue 5 https://doi.org/10.2136/sssaj2012.0435	journal	January 2013
Advances in dissolution understanding and their implications for cement hydration Juilland, Patrick; Nicoleau, Luc; Arvidson, Rolf S. RILEM Technical Letters, Vol. 2 https://doi.org/10.21809/rilemtechlett.2017.47	journal	September 2017
Micro-computed tomography: Introducing new dimensions to taxonomy Faulwetter, Sarah; Vasileiadou, Aikaterini; Kouratoras, Michail ZooKeys, Vol. 263 https://doi.org/10.3897/zookeys.263.4261	journal	February 2013

Similar Records

Strength development, hydration reaction and pore structure of autoclaved slag cement with added silica fume

Journal Article · 1996 · Cement and Concrete Research · OSTI ID:477170

Xi, Y; Siemer, D D; Scheetz, B E

Microstructural Features of a Mortar as Seen by Computed Microtomography

Journal Article · 2006 · Materials and Structures · OSTI ID:960168

Diamond, S; Landis, E

Microstructure of tricalcium silicate and Portland cement systems at middle periods of hydration-development of Hadley grains

Journal Article · 2007 · Cement and Concrete Research · OSTI ID:20871578

Kjellsen, K O; Lagerblad, B

Related Subjects

36 MATERIALS SCIENCE
cement
hydration
in-situ imaging
microstructure
microtomography
synchrotron
tomography

Title: Time-resolved 3D characterisation of early-age microstructural development of Portland cement

Citation Formats

References (53)

Similar Records

Related Subjects