In Situ Soft X-ray Spectromicroscopy of Early Tricalcium Silicate Hydration

Bae, Sungchul; Kanematsu, Manabu; Hernandez-Cruz, Daniel; Moon, Juhyuk; Kilcoyne, David; Monteiro, Paulo J. M.

doi:10.3390/ma9120976

Title: In Situ Soft X-ray Spectromicroscopy of Early Tricalcium Silicate Hydration

Journal Article · Thu Dec 01 00:00:00 EST 2016 · Materials

DOI:https://doi.org/10.3390/ma9120976· OSTI ID:1413704

Bae, Sungchul ^[1]; Kanematsu, Manabu ^[2]; Hernandez-Cruz, Daniel ^[3]; Moon, Juhyuk ^[4]; Kilcoyne, David ^[5]; Monteiro, Paulo J. M. ^[6]

Hanyang Univ., Seoul (Korea)
Tokyo Univ. of Science, Chiba (Japan)
Univ. Autonoma de Chiapas, Chiapas (Mexico)
National Univ. of Singapore (Singapore)
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
Univ. of California, Berkeley, CA (United States)

The understanding and control of early hydration of tricalcium silicate (C₃S) is of great importance to cement science and concrete technology. However, traditional characterization methods are incapable of providing morphological and spectroscopic information about in situ hydration at the nanoscale. Using soft X-ray spectromicroscopy, we report the changes in morphology and molecular structure of C₃S at an early stage of hydration. In situ C₃S hydration in a wet cell, beginning with induction (~1 h) and acceleration (~4 h) periods of up to ~8 h, was studied and compared with ex situ measurements in the deceleration period after 15 h of curing. Analysis of the near-edge X-ray absorption fine structure showed that the Ca binding energy and energy splitting of C₃S changed rapidly in the early age of hydration and exhibited values similar to calcium silicate hydrate (C–S–H). The formation of C–S–H nanoseeds in the C₃S solution and the development of a fibrillar C–S–H morphology on the C₃S surface were visualized. Following this, silicate polymerization accompanied by C–S–H precipitation produced chemical shifts in the peaks of the main Si K edge and in multiple scattering. However, the silicate polymerization process did not significantly affect the Ca binding energy of C–S–H.

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Research Organization:: Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: AC02-05CH11231

OSTI ID:: 1413704

Journal Information:: Materials, Vol. 9, Issue 12; ISSN 1996-1944

Publisher:: MDPICopyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 15 works

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36 MATERIALS SCIENCE
hydration
tricalcium silicate
C–S–H
kinetics
spectromicroscopy

Title: In Situ Soft X-ray Spectromicroscopy of Early Tricalcium Silicate Hydration

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References (35)

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