skip to main content
OSTI.GOV title logo U.S. Department of Energy
Office of Scientific and Technical Information

Title: Three-dimensional characterization of hardened paste of hydrated tricalcium silicate by serial block-face scanning electron microscopy

Abstract

With the application of a three-dimensional (3D) characterization technique, serial block-face scanning electron microscopy (SBFSEM), the 3D microstructure of a hydrated cement monomineral, tricalcium silicate (C 3S), was measured with nanoscale resolution. The 3D morphologies of anhydrous particles, hydrated products, and capillary pores were visualized. Closed and open pores were discovered inside an anhydrous particle. The size and distribution of both the anhydrous C 3S particles and their capillary pores were analyzed quantitatively and the porosity was determined to be 9%. The distribution of pores was found to be in a good agreement with the inner and outer product model of Hu et. al., with an inner shell distance of 860 nm. Here, considering the spatial resolution of the instrument and the volume of sample measured, most pores in this experiment could be characterized as capillary pores.

Authors:
 [1]; ORCiD logo [2];  [1];  [3];  [1];  [1];  [1]
  1. Tongji Univ., Shanghai (China)
  2. Tongji Univ., Shanghai (China); Univ. College London, London (United Kingdom); Brookhaven National Lab. (BNL), Upton, NY (United States)
  3. Tongji Univ., Shanghai (China); Univ. College London, London (United Kingdom)
Publication Date:
Research Org.:
Brookhaven National Lab. (BNL), Upton, NY (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)
OSTI Identifier:
1525403
Report Number(s):
BNL-211767-2019-JAAM
Journal ID: ISSN 1996-1944
Grant/Contract Number:  
SC0012704
Resource Type:
Journal Article: Accepted Manuscript
Journal Name:
Materials
Additional Journal Information:
Journal Volume: 12; Journal Issue: 12; Journal ID: ISSN 1996-1944
Publisher:
MDPI
Country of Publication:
United States
Language:
English
Subject:
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND SUPERFLUIDITY; tricalcium silicate (C3S); hydration; 3D microstructure; serial block-face scanning electron microscopy (SBFSEM)

Citation Formats

Zhao, Yongjuan, Robinson, Ian, Liu, Xianping, Chen, Bo, Yang, Fei, Zhang, Yongming, and Wang, Peiming. Three-dimensional characterization of hardened paste of hydrated tricalcium silicate by serial block-face scanning electron microscopy. United States: N. p., 2019. Web. doi:10.3390/ma12121882.
Zhao, Yongjuan, Robinson, Ian, Liu, Xianping, Chen, Bo, Yang, Fei, Zhang, Yongming, & Wang, Peiming. Three-dimensional characterization of hardened paste of hydrated tricalcium silicate by serial block-face scanning electron microscopy. United States. doi:10.3390/ma12121882.
Zhao, Yongjuan, Robinson, Ian, Liu, Xianping, Chen, Bo, Yang, Fei, Zhang, Yongming, and Wang, Peiming. Wed . "Three-dimensional characterization of hardened paste of hydrated tricalcium silicate by serial block-face scanning electron microscopy". United States. doi:10.3390/ma12121882. https://www.osti.gov/servlets/purl/1525403.
@article{osti_1525403,
title = {Three-dimensional characterization of hardened paste of hydrated tricalcium silicate by serial block-face scanning electron microscopy},
author = {Zhao, Yongjuan and Robinson, Ian and Liu, Xianping and Chen, Bo and Yang, Fei and Zhang, Yongming and Wang, Peiming},
abstractNote = {With the application of a three-dimensional (3D) characterization technique, serial block-face scanning electron microscopy (SBFSEM), the 3D microstructure of a hydrated cement monomineral, tricalcium silicate (C3S), was measured with nanoscale resolution. The 3D morphologies of anhydrous particles, hydrated products, and capillary pores were visualized. Closed and open pores were discovered inside an anhydrous particle. The size and distribution of both the anhydrous C3S particles and their capillary pores were analyzed quantitatively and the porosity was determined to be 9%. The distribution of pores was found to be in a good agreement with the inner and outer product model of Hu et. al., with an inner shell distance of 860 nm. Here, considering the spatial resolution of the instrument and the volume of sample measured, most pores in this experiment could be characterized as capillary pores.},
doi = {10.3390/ma12121882},
journal = {Materials},
issn = {1996-1944},
number = 12,
volume = 12,
place = {United States},
year = {2019},
month = {6}
}

Journal Article:
Free Publicly Available Full Text
Publisher's Version of Record

Citation Metrics:
Cited by: 1 work
Citation information provided by
Web of Science

Save / Share:

Works referenced in this record:

Direct measurements of 3d structure, chemistry and mass density during the induction period of C3s hydration
journal, November 2016


The hydration of tricalcium silicate: RILEM committee 68-MMH, Task Group 3
journal, November 1984

  • Taylor, H. F. W.; Barret, P.; Brown, P. W.
  • Materials and Structures, Vol. 17, Issue 6
  • DOI: 10.1007/BF02473986

Mechanisms of cement hydration
journal, December 2011


Recent advances in the field of cement hydration and microstructure analysis
journal, July 2011


Hydration of cementitious materials, present and future
journal, July 2011


Estimation of the degree of hydration of blended cement pastes by a scanning electron microscope point-counting procedure
journal, October 2004


Analysis of cement pastes and mortars by a combination of backscatter-based SEM image analysis and calculations based on the Powers model
journal, November 2004


Early hydration and setting of Portland cement monitored by IR, SEM and Vicat techniques
journal, May 2009


TEM Studies of Cement Hydration
journal, January 1986


Characterisation of cement hydrate phases by TEM, NMR and Raman spectroscopy
journal, October 2010


Study on the hydration product of cement in early age using TEM
journal, April 2012

  • Han, Song; Yan, PeiYu; Liu, RengGuang
  • Science China Technological Sciences, Vol. 55, Issue 8
  • DOI: 10.1007/s11431-012-4860-3

Atomic force and lateral force microscopy (AFM and LFM) examinations of cement and cement hydration products
journal, February 2013


Application of X-ray computed tomography to characterise the early hydration of calcium aluminate cement
journal, January 2003


Direct three-dimensional observation of the microstructure and chemistry of C3S hydration
journal, October 2016


In situ tomographic investigation on the early hydration behaviors of cementing systems
journal, April 2012


Three-dimensional imaging of cement microstructure evolution during hydration
journal, July 2005


In Situ Bragg Coherent Diffraction Imaging Study of a Cement Phase Microcrystal during Hydration
journal, May 2015

  • Liu, Xianping; Aranda, Miguel A. G.; Chen, Bo
  • Crystal Growth & Design, Vol. 15, Issue 7
  • DOI: 10.1021/cg5013389

A new approach in quantitative in-situ XRD of cement pastes: Correlation of heat flow curves with early hydration reactions
journal, January 2011


NMR, XRD, IR and synchrotron NEXAFS spectroscopic studies of OPC and OPC/slag cement paste hydrates
journal, April 2011

  • Mendes, Alessandra; Gates, Will P.; Sanjayan, Jay G.
  • Materials and Structures, Vol. 44, Issue 10
  • DOI: 10.1617/s11527-011-9737-6

Quantitative study of Portland cement hydration by X-ray diffraction/Rietveld analysis and independent methods
journal, September 2004


A combined QXRD/TG method to quantify the phase composition of hydrated Portland cements
journal, June 2013


Quantification of hydrated cement products of blended cements in low and medium strength concrete using TG and DTA technique
journal, December 2003


Specific Surface of Hardened Portland Cement Paste as Determined by Small-Angle X-Ray Scattering
journal, May 1974


Analysis of C–S–H gel and cement paste by small-angle neutron scattering
journal, March 2007


Examining microstructural evolution of Portland cements by in-situ synchrotron micro-tomography
journal, December 2014

  • Parisatto, Matteo; Dalconi, Maria Chiara; Valentini, Luca
  • Journal of Materials Science, Vol. 50, Issue 4
  • DOI: 10.1007/s10853-014-8743-9

Mercury porosimetry of cement-based materials and associated correction factors
journal, December 1993


Recurrent Lumbar Disc Herniation: Results of Revision Surgery and Assessment of Factors that May Affect the Outcome. A Non-Concurrent Prospective Study
journal, January 2015

  • Ibrahim, Mohammed; Arockiaraj, Justin; Amritanand, Rohit
  • Asian Spine Journal, Vol. 9, Issue 5
  • DOI: 10.4184/asj.2015.9.5.728

Serial Block-Face Scanning Electron Microscopy to Reconstruct Three-Dimensional Tissue Nanostructure
journal, October 2004


Ultramicrotomy in the ESEM, a versatile method for materials and life sciences
journal, January 2009


Quantitative characterization of porosity and determination of elastic modulus for sintered micro-silver joints
journal, November 2015


Three-Dimensional Structure Analysis and Percolation Properties of a Barrier Marine Coating
journal, January 2013

  • Chen, Bo; Guizar-Sicairos, Manuel; Xiong, Gang
  • Scientific Reports, Vol. 3, Issue 1
  • DOI: 10.1038/srep01177

Investigation of dealloying by ultra-high-resolution nanotomography: Ultra-high-resolution nanotomography
journal, November 2012

  • Hashimoto, T.; Curioni, M.; Zhou, X.
  • Surface and Interface Analysis, Vol. 45, Issue 10
  • DOI: 10.1002/sia.5176

3D microstructure reconstruction of casting aluminum alloy based on serial block-face scanning electron microscopy
journal, March 2019


Three-dimensional imaging and analysis of the internal structure of SAPO-34 zeolite crystals
journal, January 2018


New developments in electron microscopy for serial image acquisition of neuronal profiles
journal, January 2015


Exploring the third dimension: Volume electron microscopy comes of age
journal, June 2014


Investigation of Three-Dimensional Microstructure of Tricalcium Silicate (C3S) by Electron Microscopy
journal, June 2018

  • Yang, Fei; Liu, Xianping; Zhao, Yongjuan
  • Materials, Vol. 11, Issue 7
  • DOI: 10.3390/ma11071110

Accuracy in Rietveld quantitative phase analysis of Portland cements
journal, September 2003


X-ray computed tomography for pore-related characterization and simulation of cement mortar matrix
journal, March 2017


A critical comparison of 3D experiments and simulations of tricalcium silicate hydration
journal, November 2017

  • Bullard, Jeffrey W.; Hagedorn, John; Ley, M. Tyler
  • Journal of the American Ceramic Society, Vol. 101, Issue 4
  • DOI: 10.1111/jace.15323