X-ray photoelectron spectroscopic investigation of nanocrystalline calcium silicate hydrates synthesised by reactive milling

Black, Leon; Garbev, Krassimir; Beuchle, Gfinter; Stemmermann, Peter; Schild, Dieter

doi:10.1016/j.cemconres.2006.03.018

Cited by 88 publications

(67 citation statements)

References 41 publications

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“…Surface composition, as determined by XPS, has been shown to be applicable for the investigation of the bulk structure of calcium silicates [2][3][4][5] and calcium silicate hydrates [6][7][8][9][10]. Systematic changes in photoelectron spectra can be related to structural changes [11][12][13].…”

Section: Introductionmentioning

confidence: 99%

Surface carbonation of synthetic C-S-H samples: A comparison between fresh and aged C-S-H using X-ray photoelectron spectroscopy

Black

Garbev²,

Gee

2008

Cement and Concrete Research

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135

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This paper presents a continuation of studies into silicate anion structure using X-ray photoelectron spectroscopy (XPS). A series of C-S-H samples have been prepared mechanochemically, and then stored under ambient conditions for six months. Storage led to surface carbonation, the extent of which was dependent upon the calcium/silicon ratio of the fresh sample. Carbonation arose through decalcification of the C-S-H, leading to increased silicate polymerisation. The surfaces of the most calcium-rich phases (C/S = 1.33 and 1.50) underwent complete decalcification to yield silica (possibly containing some silanol groups) and calcium carbonate. Carbonation, and hence changes in silicate anion structure, was minimal for the C-S-H phases with C/S = 0.67 and 0.75.

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Section: Introductionmentioning

confidence: 99%

Surface carbonation of synthetic C-S-H samples: A comparison between fresh and aged C-S-H using X-ray photoelectron spectroscopy

Black

Garbev²,

Gee

2008

Cement and Concrete Research

Self Cite

135

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“…However, this was related to changes in calcium coordination number rather than the extent of polymerisation. We did not see a dependency upon C/S ratio when examining a series of mechanochemically synthesised C-S-H samples [34]. Thus we can infer changes in the strength of bonding upon hydrothermal treatment, but no significant changes in bonding dependent upon synthesis conditions.…”

Section: Xpsmentioning

confidence: 83%

“…As mentioned above, the energy separation between the Ca 2p 3/2 and Si 2p peaks has previously been used to assess the extent of silicate polymerisation [30,34,35,36], there being a decrease in energy separation with increasing polymerisation. This approach has the advantage of negating 12 errors due to charge correction, but does not allow comparisons between phases that are too dissimilar.…”

Section: Xpsmentioning

confidence: 99%

“…We have shown how XPS may be used to investigate the structures of crystalline calcium silicates [30] and calcium silicate hydrates [31][32][33][34], relating spectral features to structural changes. Binding energies and peak widths (in particular the silicon 2p and 2s lines) provide information as to the extent of silicate polymerisation and the degree of structural disorder.…”

Section: Xpsmentioning

confidence: 99%

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Structure, bonding and morphology of hydrothermally synthesised xonotlite

Black¹,

Garbev²,

Stumm³

2008

Advances in Applied Ceramics

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We have systematically investigated the role of synthesis conditions upon the structure and morphology of xonotlite. Starting with a mechanochemically-prepared, semi-crystalline phase with Ca:Si = 1, we have prepared a series of xonotlite samples hydrothermally, at temperatures between 200 and 250°C. Analysis in each case was by x-ray photoelectron spectroscopy (XPS), environmental scanning electron microscopy (ESEM) and x-ray diffraction (XRD). There was increased silicate polymerisation with both increased synthesis temperature and duration of synthesis. Concerning crystal morphology, there was an increase in crystal size with increasing temperature, but this led to some crystal damage. Longer hydrothermal treatment however led to more perfect crystal morphologies.

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“…Building on work in the field of mineralogy, x-ray photoelectron spectroscopy has been used to examine the earliest stages of cement hydration 22 and probe the silicate structure of fresh 23 and aged 24 C-S-H phases, and now in this issue for the first time hydrated aluminate phases formed upon the exposure of cement clinker to water vapour 25 . The extreme surface sensitivity of this technique has been employed to look at the earliest stages of both hydration and sample ageing.…”

Section: Innovative Analysis and Characterisationmentioning

confidence: 99%