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Keywords = parametric Rietveld refinement

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20 pages, 6900 KB  
Article
Luminescent Properties of (Ca7ZrAl6O18-Ca3Al2O6-CaZrO3):Eu3+ Composite Ceramics and Tracing in the Hydration Process
by Dominika Madej and Andrzej Kruk
Molecules 2023, 28(23), 7799; https://doi.org/10.3390/molecules28237799 - 27 Nov 2023
Cited by 3 | Viewed by 1713
Abstract
In this work, solid-state reaction sintering was used to fabricate Ca7ZrAl6O18-Ca3Al2O6-CaZrO3:Eu3+ ternary composite ceramics and cements. The structural, microstructural, and spectroscopic properties of the ceramics with different Eu [...] Read more.
In this work, solid-state reaction sintering was used to fabricate Ca7ZrAl6O18-Ca3Al2O6-CaZrO3:Eu3+ ternary composite ceramics and cements. The structural, microstructural, and spectroscopic properties of the ceramics with different Eu2O3 content were characterized by X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS), and spectrofluorimetry, respectively. The XRD patterns analyzed with Rietveld refinement confirm the presence of the orthorhombic phase of Ca7ZrAl6O18 and the cubic phase of Ca3Al2O6 in all the samples, indicating that doping of Eu3+ slightly changes the crystalline structure of both aluminate phosphors. EDS analysis revealed that the Eu doping element was strongly concentrated to the two phases, i.e., Ca7ZrAl6O18 and Ca3Al2O6, with the Eu concentrations of 8.45 wt.% and 8.26 wt.%, respectively. The luminescent properties of the ceramics doped with different Eu3+ ion concentrations were investigated by excitation and emission spectroscopy at room temperature. These results were compiled using a laser with an optical parametric oscillator (OPO) system. The obtained spectra indicated changes in the luminescence intensity and shape occurring with phase composition and Eu2O3 concentration. The emission spectra of the ceramics exhibit a strong dependence on the excitation wavelength in the range from 210 to 300 nm, and invariably, five peaks were assigned to the 5D07FJ (J = 0, 1, 2, 3, 4) transitions of Eu3+. The luminescence spectroscopy was then used to trace the early and long-term hydration behavior of cements. Thus, luminescence spectroscopy may provide a new tool for non-destructive testing of cement-based structures. Full article
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16 pages, 4491 KB  
Article
In-Situ Investigation of the Oxidation Behaviour of Chemical Vapour Deposited Zr(C,N) Hard Coatings Using Synchrotron X-ray Diffraction
by Florian Frank, Michael Tkadletz, Christian Saringer, Andreas Stark, Norbert Schell, Marco Deluca, Christoph Czettl and Nina Schalk
Coatings 2021, 11(3), 264; https://doi.org/10.3390/coatings11030264 - 24 Feb 2021
Cited by 10 | Viewed by 3922
Abstract
The oxidation behaviour of chemical vapour deposited ZrN, ZrC and ZrCN coatings was investigated using in-situ synchrotron X-ray diffraction (XRD). To obtain a precise analysis of the temperature–dependent phase evolution during oxidation, coating powders were annealed in air between 100 °C and 1000 [...] Read more.
The oxidation behaviour of chemical vapour deposited ZrN, ZrC and ZrCN coatings was investigated using in-situ synchrotron X-ray diffraction (XRD). To obtain a precise analysis of the temperature–dependent phase evolution during oxidation, coating powders were annealed in air between 100 °C and 1000 °C. Simultaneously, 2D XRD patterns were recorded in ~2 °C increments, which were subsequently evaluated using parametric Rietveld refinement. The results were correlated with differential scanning calorimetry and thermogravimetric analysis measurements, to further illuminate the oxidation mechanism of each coating system. ZrCN exhibited the highest oxidation onset temperature, followed by ZrC and ZrN. Furthermore, ZrCN was completely oxidised at a temperature of ~720 °C, which was ~50–70 °C higher than for ZrN and ZrC. The in-situ experiments revealed a similar oxidation sequence for all three samples: first, tetragonal and/or cubic (c/t)–ZrO2 is formed, which subsequently transforms into the more stable monoclinic (m)–ZrO2 phase. ZrCN and ZrC showed a higher c/t–ZrO2 fraction than the ZrN sample at 1000 °C. Furthermore, ex-situ Raman and XRD investigations of the oxidised samples revealed the ongoing c/t–ZrO2 → m–ZrO2 phase transformation during cooling. Full article
(This article belongs to the Special Issue Chemical Vapor Deposition (CVD) Coatings)
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