Papers by Keyword: Rietveld Method

Abstract: The characterization of historic lime mortars is crucial for many cultural heritage conservation issues. In this work, the characterization of a historical lime mortar is described. Samples for chemical analysis were obtained after different milling times and using the RILEM acid digestion method on several replicates. Qualitative and quantitative determination of phases in the mortar and in the residues after acid attack and the potential presence of CaCO₃ polymorphs, were accomplished with X-ray powder diffraction. Results suggest that representativeness of the sample and the homogenisation, although not always achievable in conservation practice, are strongly affecting results.

Abstract: The present work reviews current practices in quantitative XRD analysis of anhydrous and hydrated Portland cement. While Part 1 of this two-part work reviews the conventional internal standard method and the reference intensity ratio (RIR) method, Part 2 reviews the more commonly used computer-based methods, which include the Rietveld method (with or without internal standard) and the G-factor method (with external standard). Further, some critical general aspects of the experimental procedures that affect the accuracy of the analysis are discussed.

Abstract: NiTe nanocrystals were prepared through facile and fast solid state reaction (mechanical alloying) of pure elemental tellurium and nickel powders in an argon atmosphere. The samples processed for 3 h, 5 h and 10 h were characterized by X-ray diffraction, transmission electron microscopy, magnetization and Raman spectroscopy. Hexagonal NiTe crystals with an average size of 30 nm can be obtained after only 3 h of processing time. Transmission electron microscopy images showed a broad crystalline size distribution in the agglomerated particles and selected area electron diffraction revealed its crystalline character. NiTe ferromagnetic behavior was confirmed and magnetic parameters were dependent on processing time. Raman spectra showed no unreacted Te or tellurium oxides, but it also showed that laser induced phases transitions (including Te re-crystallization) can be observed for modest laser power (<3 mW).

Abstract: This paper presents the synthesis, characterization and influence of oxidizing atmosphere in the calcinations and sintering processes on microstructural properties of mixed oxides of Cerium and Zinc, obtained by the polymeric precursor method, aiming at a subsequent catalytic application. The material was submitted to calcinations and sintering at 900 and 1050 °C. The samples were characterized by XRD analysis techniques, surface area by BET method and refined by the Rietveld method. The results of X-ray diffraction showed that interest phase was formed, indicating that the method for obtaining the phase is effective. The results of surface area for the system calcined in air were 85 m²/g and 65 m²/g for the system subjected to oxidizing atmosphere both at 900°C, in the same temperature. It was observed that the temperature increase leads to an increase in crystallite size. This fact is in line with other studies in the literature.

Abstract: Transition metal oxide-doped CCTO (CaCu₃Ti₄O₁₂) ceramics were prepared by a conventional solgel synthesis method and the effects of pure CCTO and CCTO doped with Mn, Fe, Co, Ni to the crystal structure, microstructures and dielectrical properties of samples were investigated. The phase composition and microstructure were studied by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). The XRD analysis reveals that all samples exhibited multiphases with the pseudo-perovskite cubic CCTO phase with space group Im-3 as the main phase in undoped and doped CCTO samples. Peaks of monoclinic CuO and peroveskite CaTiO₃ could also be seen in all samples which indicate that solid solution of CuO in CaTiO₃ lattice was incomplete.SEM results show that doping effectively enhanced densification. SEM micrographs also suggested that the morphologies of doped CCTO ceramics had showed a matrix consisting of large grains wherein the small grains were embedded between the larger grains. Dielectric properties of pure and doped CCTO were investigated in a broad frequency range of the dielectric constant reached a value as high as ε_r = 29.4 at room temperature for CCTO doped with Ni at frequency (1000 Hz). Besides the sintering conditions, the microstructure and the dielectric properties of the CCTO are strongly influenced by type of doping elements.

Abstract: The quantitative phase analyses of a slag have been successfully carried out by using both of the full-profile Rietveld and RIR methods from X-ray powder diffraction data. The qualitative phase analysis indicates that the slag contains mayenite (CaO)₁₂(Al₂O₃)₇, olivine Ca₂(SiO₄), gehlenite Ca₂Al (AlSiO₇), lemite Ca₂(SiO₄) and hibonite CaO(Al₂O₃)₆. The quantitative analysis from Rietveld refinement shows that the weight concentrations of mayenite, olivine, gehlenite, lemite and hibonite for the slag are 48.8(4) wt.%, 32.2(5) wt.%, 11.0(9) wt.%, 6.2(1.1) wt.% and 1.8 (1.2) wt.%, respectively. The quantitative phase analysis results obtained by Rietveld method are more precise then those by RIR method.

Abstract: During the process of leaching of roasted ore from fluidized-bed furnace a decrease of zinc (as ZnO) recovery was observed. Within the investigations a comprehensive structural analysis of samples from the process of roasting of zinc concentrates has been made. It has been found that one of the essential causes for zinc recovery decrease is a presence of (Zn,Fe)S sulphide in the ore, instead of pure zinc blende ZnS. Subsequently, (Zn,Fe)S iron blende is oxidized not to ZnO, but to a mixture where the main component is mixed (Zn,Fe)Fe₂O₄ oxide. Such oxide does not decompose into simple oxides during the process, which leads to a decrease of zinc recovery.

Abstract: Abstract. The structure and chemical order of a Heusler alloy of non-stoichiometric composition Ni-Mn-Ga were studied using constant-wavelength (1.538 Å) neutron diffraction at 363K and the diffraction pattern was refined using the FullProf software. At this temperature the structure is austenite (cubic) with Fm space group and lattice constant of a = 5.83913(4) [Å]. The chemical order is of critical importance in these alloys, as Mn becomes antiferromagnetic when the atoms are closer than the radius of the 3d shell. In the studied alloy the refinement of the site occupancy showed that the 4b (Ga site) contained as much as 22% Mn; that significantly alters the distances between the Mn atoms in the crystal and, as a result, also the exchange energy between some of the Mn atoms. Based on the refinement, the composition was determined to be Ni1.91Mn1.29Ga0.8

Abstract: The allotropic phase transformation of cobalt powder prepared by high-energy ball milling was investigated as a function of milling time. Measurement of crystallite size and micro-strain in the powder systems milled for different times were conducted by X-ray diffractometry. The X-ray diffraction (XRD) peaks were analyzed using the Pearson VII profile function in conjunction with Rietveld method. X-ray diffraction line broadening revealed that allotropic transformation between face-centred-cubic phase (fcc) and hexagonal close-packed phase (hcp) in cobalt is grain size dependent and also on the accumulation of structure defects. The results showed that the phase formation of cobalt depends on the mill intensity that influences of both the grain size and the accumulation of structure defects. However, this theory alone is not adequate to explain the effects in this work. It was found that the total surface energy (Ω) theory satisfactorily explains the phase transformation behavior of cobalt. The smaller value of surface energy (Ω) of the fcc crystal than the hcp phase when size decreases may alter the qualitative aspects of the phase formation.

Abstract: This aim of this work is to evaluate the influence of citric acid/metallic cation ratio of 3:1, 4:1 and 5:1 used in the TiO₂ synthesis by Pechini method in the structure, morphology and photocatalytic activity of methyl red dye. The prepared samples were characterized by X-ray Diffraction (XRD) using Rietveld refinement method, textural analyses, and photocatalytic activity. The results obtained by XRD technique confirm the efficiency of the Pechini method in the preparation of TiO₂ samples with nanosize particle. All samples present anatase phase and presence of rutile as secondary phase with content of 15.6, 10.5 and 18.3%. The isothermal adsorption showed that samples have mesopores characteristics and morphology with irregular shape agglomerates. The sample 4:1 presented better photocatalytic performance discoloring 70% of dye in 24h, indicating that the presence of 10.5% of rutile phase jointly with anatase phase improve the photocatalytic activity.