A Scanning Transmission X-ray Microscopy Study of Cubic and Orthorhombic C₃A and Their Hydration Products in the Presence of Gypsum.

This paper shows the microstructural differences and phase characterization of pure phases and hydrated products of the cubic and orthorhombic (Na-doped) polymorphs of tricalcium aluminate (C₃A), which are commonly found in traditional Portland cements. Pure, anhydrous samples were characterized using scanning transmission X-ray microscopy (STXM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) and demonstrated differences in the chemical and mineralogical composition as well as the morphology on a micro/nano-scale. C₃A/gypsum blends with mass ratios of 0.2 and 1.9 were hydrated using a water/C₃A ratio of 1.2, and the products obtained after three days were assessed using STXM. The hydration process and subsequent formation of calcium sulfate in the C₃A/gypsum systems were identified through the changes in the LIII edge fine structure for Calcium. The results also show greater Ca LII binding energies between hydrated samples with different gypsum contents. Conversely, the hydrated samples from the cubic and orthorhombic C₃A at the same amount of gypsum exhibited strong morphological differences but similar chemical environments

A Scanning Transmission X-ray Microscopy Study of Cubic and Orthorhombic C3A and Their Hydration Products in the Presence of Gypsum

This paper shows the microstructural differences and phase characterization of pure phases and hydrated products of the cubic and orthorhombic (Na-doped) polymorphs of tricalcium aluminate (C3A), which are commonly found in traditional Portland cements. Pure, anhydrous samples were characterized using scanning transmission X-ray microscopy (STXM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) and demonstrated differences in the chemical and mineralogical composition as well as the morphology on a micro/nano-scale. C3A/gypsum blends with mass ratios of 0.2 and 1.9 were hydrated using a water/C3A ratio of 1.2, and the products obtained after three days were assessed using STXM. The hydration process and subsequent formation of calcium sulfate in the C3A/gypsum systems were identified through the changes in the LIII edge fine structure for Calcium. The results also show greater Ca LII binding energies between hydrated samples with different gypsum contents. Conversely, the hydrated samples from the cubic and orthorhombic C3A at the same amount of gypsum exhibited strong morphological differences but similar chemical environments

Incorporating carbon sequestration materials in civil infrastructure: A micro and nano-structural analysis

The Calera method for carbon sequestration promotes carbon mineralization through aqueous precipitation. This work reports a comprehensive analysis on a carbonate obtained by the Calera process to evaluate its suitability as a cement replacement for concrete applications. This work focuses on the analysis of two hydrated cement pastes made with a blend of Portland cement and Calera carbonates by various advanced analytical techniques. Scanning Electron Microscopy (SEM) equipped with Energy Dispersive Spectroscopy (EDS) was used to observe microstructures and determine elemental compositions. The synchrotron X-ray diffraction technique combined with Rietveld analysis were applied to identify constituent phases and refine crystal structures, crystallite sizes as well as relative phase abundances. Calcite and vaterite are observed in all samples while CSH II and portlandite are dominant in the cement pastes. Near-Edge X-ray Absorption Fine Structure (NEXAFS) spectrometry and Scanning Transmission X-ray Microscopy (STXM) experiments were conducted to investigate chemical speciation and morphological information of carbonate minerals with different absorption energies. STXM results confirmed heterogeneity of the samples, and also provided a nano-scale phase map across multiple particles. Differential Thermogravimetric (DTG) was used to observe heat transfer through structures and changes in mass upon heating. A compressive strength tests were performed on materials and shown comparable strength to Portland cement. © 2013 Elsevier Ltd. All rights reserved

A scanning transmission X-ray microscopy study of cubic and orthorhombic tricalcium aluminate and their hydration products in the presence of gypsum

This paper shows the microstructural differences and phase characterization of pure phases and hydrated products of the cubic and orthorhombic (Na-doped) polymorphs of tricalcium aluminate (C3A), which are commonly found in traditional Portland cements. Pure, anhydrous samples were characterized using scanning transmission X-ray microscopy (STXM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) and demonstrated differences in the chemical and mineralogical composition as well as the morphology on a micro/nano-scale. C3A/gypsum blends with mass ratios of 0.2 and 1.9 were hydrated using a water/C3A ratio of 1.2, and the products obtained after three days were assessed using STXM. The hydration process and subsequent formation of calcium sulfate in the C3A/gypsum systems were identified through the changes in the LIII edge fine structure for Calcium. The results also show greater Ca LII binding energies between hydrated samples with different gypsum contents. Conversely, the hydrated samples from the cubic and orthorhombic C3A at the same amount of gypsum exhibited strong morphological differences but similar chemical environments

Phase Changes of Monosulfoaluminate in NaCl Aqueous Solution.

Monosulfoaluminate (Ca₄Al₂(SO₄)(OH)12∙6H₂O) plays an important role in anion binding in Portland cement by exchanging its original interlayer ions (SO₄2- and OH-) with chloride ions. In this study, scanning transmission X-ray microscope (STXM), X-ray absorption near edge structure (XANES) spectroscopy, and X-ray diffraction (XRD) were used to investigate the phase change of monosulfoaluminate due to its interaction with chloride ions. Pure monosulfoaluminate was synthesized and its powder samples were suspended in 0, 0.1, 1, 3, and 5 M NaCl solutions for seven days. At low chloride concentrations, a partial dissolution of monosulfoaluminate formed ettringite, while, with increasing chloride content, the dissolution process was suppressed. As the NaCl concentration increased, the dominant mechanism of the phase change became ion exchange, resulting in direct phase transformation from monosulfoaluminate to Kuzel's salt or Friedel's salt. The phase assemblages of the NaCl-reacted samples were explored using thermodynamic calculations and least-square linear combination (LC) fitting of measured XANES spectra. A comprehensive description of the phase change and its dominant mechanism are discussed

A scanning transmission X-ray microscopy study of cubic and orthorhombic tricalcium aluminate and their hydration products in the presence of gypsum

This paper shows the microstructural differences and phase characterization of pure phases and hydrated products of the cubic and orthorhombic (Na-doped) polymorphs of tricalcium aluminate (C3A), which are commonly found in traditional Portland cements. Pure, anhydrous samples were characterized using scanning transmission X-ray microscopy (STXM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) and demonstrated differences in the chemical and mineralogical composition as well as the morphology on a micro/nano-scale. C3A/gypsum blends with mass ratios of 0.2 and 1.9 were hydrated using a water/C3A ratio of 1.2, and the products obtained after three days were assessed using STXM. The hydration process and subsequent formation of calcium sulfate in the C3A/gypsum systems were identified through the changes in the LIII edge fine structure for Calcium. The results also show greater Ca LII binding energies between hydrated samples with different gypsum contents. Conversely, the hydrated samples from the cubic and orthorhombic C3A at the same amount of gypsum exhibited strong morphological differences but similar chemical environments