rietveld quantitative phase analysis
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2021 ◽  
Author(s):  
Zein K. Heiba ◽  
Mohamed Bakr Mohamed ◽  
Noura M. Farag ◽  
Ali Badawi

Abstract (1-x)NiCo2O4/xPbS (0≤x≤0.2) nanocomposite samples were synthesized using the hydrothermal and thermolysis procedures. The different phases developed in the obtained nanocomposite samples were accurately determined using the x-ray diffraction technique equipped with a line-detector. The percentage of the formed phases (NiCo2O4 (NCO), PbS, PbSO4), structural and microstructure parameters were determined using Rietveld quantitative phase analysis. The transmission electron microscope (TEM) images and Rietveld analysis reveal almost isotropic particle size in the nano range with a very narrow size distribution. The obtained phase percentages of PbS and PbSO4 are smaller than nominated values (x) suggesting dissolving of some Pb and S ions in NCO which then confirmed by the analysis of Fourier-transform infrared (FTIR) spectra of nanocomposite samples. The absorption spectra are modified upon doping NCO with PbS. The optical band gaps of the nanocomposites increase as the amount of PbS is increased. The effect of alloying on extinction coefficient, refractive index, dielectric constant, optical conductivity, the intensity, and emitted color from the photoluminescence of the nanocomposite samples are also studied. The refractive index values of NCO and NCO-PbS nanocomposite samples exhibit normal dispersions. The photoluminescent measurements reveal that NCO-PbS nanocomposites could emit a violet color. The improvement in the values of the non-linear optical (NLO) parameters of pristine NCO at high frequencies or the nanocomposite samples at low frequencies, nominated them to be used in NLO photonic applications.



2020 ◽  
Vol 1010 ◽  
pp. 262-267
Author(s):  
Tinesha Selvaraj ◽  
Johar Banjuraizah ◽  
Shing Fhan Khor

The aim of this study is to understand the compaction characteristics of as received granulated 8 mol% yttria-stabilized zirconia (8YSZ). The samples were compacted at different loads and sintered at 1550 °C with the heating rate of 5°C/min for 5 hours. The densification, morphology analysis and crystal structure of the sintered were compared. The densification of granulated 8YSZ achieved 67% as increasing pressing load (0.1 tonne to 0.4 tonne). Rietveld quantitative phase analysis demonstrates that the tetragonal-ZrO2 phase reduces in granulated 8YSZ. The amount of cubic-ZrO2 phase dramatically dropped for both granulated as the pressing load increased. From the morphology analysis, granulated sample found to be porous observed on the surface as compaction load applied. Compaction load has no significant effect on the densification of granule sintered 8YSZ in the current study. The maximum densification was only reached 67% by using granulated 8YSZ powder with 0.4 tonne pressing load.



Author(s):  
L. León-Reina ◽  
A. Cuesta ◽  
M. García-Maté ◽  
G. Álvarez-Pinazo ◽  
I. Santacruz ◽  
...  


2018 ◽  
Vol 280 ◽  
pp. 58-64
Author(s):  
Tinesha Selvaraj ◽  
Johar Banjuraizah ◽  
S.F. Khor ◽  
M.N. Mohd Zainol

A facile strategy was proposed to incorporate the dopant Fe into 8YSZ-based material, which can be potentially applied as solid electrode materials for Solid Oxide Fuel Cells (SOFC). In this study, 8YSZ powder was investigated in terms of densification, conductivity and thecrystal structure as a solid electrolytes. Therefore, varying mol% of Fe included 1, 2, and 3 were prepared for investigation. The crystalline structure of the pristine and Fe doped samples were characterized by X-ray diffraction (XRD) and the phase contents were evaluated by using the Rietveld method. Rietveld quantitative phase analysis demonstrates that the monoclinic-ZrO2phase increases (12.8 wt% to 39.7 wt%) as the concentration of Fe increases, while the amount of tetragonal-ZrO2phase drop (40.4 wt% to 11.9 wt%) dramatically. Sintering activity was applied to improve incorporation of the 8YSZ powder and the dopant Fe where the relative density increases from 77% to 92%. Sample YSZ-2Fe has been fitted with CPE equivalent circuit and achieved 6.251 x 10-6S/cm at 300 °C in air. However, it was found that conductivity levels decreased as the mol% of Fe increased. In short, sample YSZ-2Fe ceramic demonstrated good results in terms of densification (92.09%), cubic ZrO2phase (22 wt%) and conductivity 6.251 x 10-6S/cm.



2014 ◽  
Vol 30 (1) ◽  
pp. 25-35 ◽  
Author(s):  
Ana Cuesta ◽  
Gema Álvarez-Pinazo ◽  
Marta García-Maté ◽  
Isabel Santacruz ◽  
Miguel A. G. Aranda ◽  
...  

Building materials are very complex samples of worldwide importance; hence quantitative knowledge of their mineralogical composition is necessary to predict performances. Rietveld quantitative phase analysis (RQPA) allows a direct measurement of the crystalline phase contents of cements. We highlight in this paper the use of laboratory X-ray powder diffraction (LXRPD) employing high-energy radiation, molybdenum (Mo), for attaining the RQPA of cements. Firstly, we evaluate the accuracy of RQPA employing a commercial calcium sulfoaluminate clinker with gypsum. In addition to MoKα1 and MoKα1,2 radiations, Cu and synchrotron patterns are also analyzed for the sake of comparison. Secondly, the assessment of the accuracy of RQPA results obtained using different radiations (synchrotron, Mo, and Cu) and geometries (reflection and transmission) is performed by analyzing two well-known commercial samples. As expected, for LXRPD data, accuracy in the RQPA results improves as the irradiated volume increases. Finally, three very complex aged hydrated cements have been analyzed using MoKα1-LXRPD and Synchrotron-XRPD. The main overall outcome of this work is the benefit for RQPA of using strictly monochromatic MoKα1 radiation. Best laboratory results arise from MoKα1 data as the effective tested volume is much increased but peak overlapping is not swelled.





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