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In this study, the effect of vanadium addition on the structural and magnetic properties of cobalt ferrite (Co 1− x V x Fe 2 O 4 ; where x  = 0, 0.05, 0.10, 0.15, 0.20, and 0.25) prepared by a novel sol–gel autocombustion method was investigated. The formation of cubic spinel structure (space group Fd3m ) was confirmed by X-ray diffraction in combination of Rietveld structure refinement analysis and transform infrared spectroscopic spectrum (FT-IR) analyses. Also, phase and elemental analyses confirmed that an inevitable secondary phase of hematite along with the spinel phase appears by addition of vanadium; therefore, a nanocomposite was formed in the sample containing vanadium. However, the SEM observations in combination of the results obtained by Rietveld structure refinement analysis showed that the presence of vanadium can affect the size of synthesized cobalt ferrite. VSM measurements showed that saturation magnetization and coercivity values are strongly dependent on the vanadium content and particle size, so that the maximum value of coercivity was obtained equal to ~916 Oe for Co 0.85 V 0.15 Fe 2 O 4 . Highlights Effect of vanadium ions addition on the magnetic properties of cobalt ferrite. Effect of adding these ions on morphology and agglomeration of the nanoparticles. The evolution of structural properties by using the Rietveld method.

Cellulose is often described as a mixture of crystalline and amorphous material. A large part of the general understanding of the chemical, biochemical and physical properties of cellulosic materials is thought to depend on the consequences of the ratio of these components. For example, amorphous materials are said to be more reactive and have less tensile strength but comprehensive understanding and definitive analysis remain elusive. Ball milling has been used for decades to increase the ratio of amorphous material. The present work used 13 techniques to follow the changes in cotton fibers (nearly pure cellulose) after ball milling for 15, 45 and 120 min. X-ray diffraction results were analyzed with the Rietveld method; DNP (dynamic nuclear polarization) natural abundance 2D NMR studies in the next paper in this issue assisted with the interpretation of the 1D analyses in the present work. A conventional NMR model’s paracrystalline and inaccessible crystallite surfaces were not needed in the model used for the DNP studies. Sum frequency generation (SFG) spectroscopy also showed profound changes as the cellulose was decrystallized. Optical microscopy and field emission-scanning electron microscopy results showed the changes in particle size; molecular weight and carbonyl group analyses by gel permeation chromatography confirmed chemical changes. Specific surface areas and pore sizes increased. Fourier transform infrared (FTIR) and Raman spectroscopy also indicated progressive changes; some proposed indicators of crystallinity for FTIR were not in good agreement with our results. Thermogravimetric analysis results indicated progressive increase in initial moisture content and some loss in stability. Although understanding of structural changes as cellulose is amorphized by ball milling is increased by this work, continued effort is needed to improve agreement between the synchrotron and laboratory X-ray methods used herein and to provide physical interpretation of the SFG results.

Neodymium Ferrite Oxide (Nd1.2FeO3) has been successfully synthesized using solid state reaction by varying annealing time. Structural crystallographic characteristics were obtained by X-ray diffraction. The results of X-ray diffraction analysis showed the samples had been identified composed of NdFeO3 and Nd2O3 phase, with peak dominant correspond to hkl (121), FWHM value of 0.22° and estimated crystal size of 393 nm. Analysis using Rietveld methods obtained Nd1.2FeO3 oxide material has a crystal structure is orthorhombic with space-group of PNMA. The results are comparable as was reported elsewhere that the oxide material is useful for gas sensor application.

The synthetic anhydrous crystalline CaCO 3 polymorphs—vaterite, aragonite and calcite—were tested using dilatometry and nanoindentation. Microstructural changes in the samples before and after measurements were observed under scanning electron microscope and their phase composition quantified with X-ray powder diffraction with the Rietveld method. The thermal expansion coefficients of vaterite and the hardness and elastic modulus of synthetic aragonite are reported for the first time. The physical and nanomechanical properties were measured under similar conditions for each CaCO 3 polymorph. Aragonite, calcite and vaterite showed volumetric thermal expansion coefficient at 303 K of 49.2(8), 48.6(2) and 44.1(3) 10 −6  K −1 , respectively. The elastic modulus increased from 5(4), 16(7) to 31(8) GPa for aragonite, calcite and vaterite, respectively. Average hardness was found lower than values from the literature, ranging from 0.3 to 1.3 GPa. The results are considered of interest for the design of CaCO 3 -based materials for applications.

Ce 2 [Zr 1− x (Mg 1/3 Sb 2/3 ) x ] 3 (MoO 4 ) 9 (0.02 ⩽ x ⩽ 0.10) ceramics were prepared by the traditional solid-state method. A single phase, belonging to the space group of R 3 ¯ c , was detected by using X-ray diffraction at the sintering temperatures ranging from 700 to 850 °C. The microstructures of samples were examined by applying scanning electron microscopy (SEM). The crystal structure refinement of these samples was investigated in detail by performing the Rietveld refinement method. The intrinsic properties were calculated and explored via far-infrared reflectivity spectroscopy. The correlations between the chemical bond parameters and microwave dielectric properties were calculated and analyzed by Phillips-van Vechten-Levine (P-V-L) theory. Ce 2 [Zr 0.94 (Mg 1/3 Sb 2/3 ) 0.06 ] 3 (MoO 4 ) 9 ceramics with excellent dielectric properties were sintered at 725 °C for 6 h ( ε r = 10.37, Q × f = 71,748 GHz, and τ f = −13.6 ppm/°C, ε r is the dielectric constant, Q × f is the quality factor, and τ f is the temperature coefficient of resonant frequency).

Bismuth ferrite (BiFeO 3 or BFO), is an extremely promising multiferroic material having broad range of applications. In the present study, we investigated the optimization of annealing temperature for the preparation of pure phase bismuth ferrite using quantitative Rietveld analysis of XRD patterns. The rhombohedral structure was confirmed by X-ray diffraction with R3c space group as a primary phase (pure BFO) along with a cubic secondary phase (Bi 25 FeO 40 ) having space group I23 . The quantitative analysis of refine data shows the decrease in the values of fitting parameters in case of double refinement and hence convergence towards the best fitting. Also, with the increase in annealing temperature, very nominal decrease in phase percentage of secondary phase was observed. At annealing temperature of 780 °C, the intensity of (110) planes suddenly becomes more in comparison to (104) planes. The average crystallite size of samples was calculated using Scherrer formula, W–H plot method, and Rietveld method, and lattice strain was derived from the W–H plot method. Overall, the crystallite size increases with the increase in annealing temperature. It has been also observed that the strain, lattice parameters, unit cell volume, and effective bond lengths decrease with the increase in annealing temperature, but no significant change was observed in bond angles with the variation in annealing temperature.

Mechanical amorphization of three chitosan samples with high, medium, and low molecular weight was studied. It is shown that there are no significant differences between the course of amorphization process in a planetary ball mill of chitosan with different molecular weights, and the maximum degree of amorphization was achieved in 600 s of high intensity mechanical action. Specific energy consumption was 28 kJ/g, being comparable to power consumption for amorphization of cellulose determined previously (29 kJ/g) and 5–7-fold higher than that for amorphization of starch (4–6 kJ/g). Different techniques for determining the crystallinity index (CrI) of chitosan (analysis of the X-ray diffraction (XRD) data, the peak height method, the amorphous standard method, peak deconvolution, and full-profile Rietveld analysis) were compared. The peak height method is characterized by a broader working range but provides deviated CrI values. The peak deconvolution method (with the amorphous Voigt function) makes it possible to calculate the crystallinity index of chitosan with greater accuracy, but the analysis becomes more difficult with samples subjected to mechanical processing. In order to refine the structure and calculation of CrI by the Rietveld method, an attempt to optimize the structure file by the density functional theory (DFT) method was performed. The averaged profile of amorphous chitosan approximated by an eighth-order Fourier model improved the correctness of the description of the amorphous contribution for XRD data processing. The proposed equation may be used as a universal standard model of amorphous chitosan to determine the crystallinity index both for the amorphous standard method and for peak deconvolution of XRD patterns for arbitrary chitosan samples.

X-ray diffraction (XRD) analysis, as one of the most powerful methods, has been widely used to identify and quantify minerals in earth science. How to improve the precision of mineral quantitative analysis is still a hot topic. To date, several quantitative methods have been proposed for different purposes and accompanied by diverse software. In this study, three quantitative mineral analysis methods, including the reference intensity ratio (RIR), Rietveld, and full pattern summation (FPS) methods, are compared and evaluated to systematically investigate their accuracy and applicability. The results show that the analytical accuracy of these methods is basically consistent for mixtures free from clay minerals. However, there are significant differences in accuracy for clay-mineral-containing samples. In comparison, it seems that the FPS method has wide applicability, which is more appropriate for sediments. The Rietveld method has been shown to be capable of quantifying complicated non-clay samples with a high analytical accuracy; nevertheless, most conventional Rietveld software fails to accurately quantify phases with a disordered or unknown structure. The RIR method represents a handy approach but with lower analytical accuracy. Overall, the present results are expected to provide a potentially important reference for the quantitative analysis of minerals in sediments.

Dense microwave dielectric ceramics of Ce 2 [Zr 1 − x (Al 1/2 Ta 1/2 ) x ] 3 (MoO 4 ) 9 (CZMAT) ( x = 0.02–0.10) were prepared by the conventional solid-state route. The effects of (Al 1/2 Ta 1/2 ) 4+ on their microstructures, sintering behaviors, and microwave dielectric properties were systematically investigated. On the basis of the X-ray diffraction (XRD) results, all the samples were matched well with Pr 2 Zr 3 (MoO 4 ) 9 structures, which belonged to the space group R 3 ¯ c . The lattice parameters were obtained using the Rietveld refinement method. The correlations between the chemical bond parameters and microwave dielectric properties were calculated and analyzed by using the Phillips—Van Vechten—Levine (P—V—L) theory. Excellent dielectric properties of Ce 2 [Zr 0.94 (Al 1/2 Ta 1/2 ) 0.06 ] 3 (MoO 4 ) 9 with a relative permittivity ( ε r ) of 10.46, quality factor ( Q × f ) of 83,796 GHz, and temperature coefficient of resonant frequency ( τ f ) of −11.50 ppm/°C were achieved at 850 °C.

This research has comprehended the crystallographic characterization of two naturally occurring calcium carbonates phases e.g. aragonite and calcite in Pila globosa (P. globosa) and eggshells respectively. The tools employed to confirm the phases of aragonite and calcite were X-ray diffractoion (XRD) and Fourier Transform Infrared (FT-IR) spectroscopy. Several important crystallographic parameters like crystallite size, lattice parameters, dislocation density, crystallinity index, microstrain, volume of the unit cell, relative intensity of a certain plane, preference growth, and specific surface area were taken into account while assessing the desired aragonite and calcite phases. A number of well-known models e.g. Straight-line model of the Scherrer model, the Monshi-Scherrer model, the Williamson-Hall model, the Sahadat-Scherrer model, and the three-peak model aided the estimation of crystallite size. In all the cases, the observed crystallite size of calcite was larger than that of aragonite. The percentage of calcite and aragonite in eggshell and P. globosa were assessed by Rietveld refinement method. Observed results revealed that 97.4% calcite and 2.6% aragonite phases are present in eggshell while in P. globosa these percentages exist inversely, i.e. 93.2% aragonite and 6.8% calcite phases.