Rietveld Method Research Articles

Paramagnetism found in Mn-doped CuO nanofibers at room temperature explained by XPS , XAS and Rietveld method

CuO and 3 % Mn-doped CuO nanofibers were synthesized employing the electrospinning method. X-ray diffraction (XRD) verified a monoclinic phase with a C 2/c space group. An electronic density analysis, obtained using Fullprof software, was projected on the (110) and (001) planes for both materials, showing modifications in the Cu positions. This fact generated vacancies involved in the paramagnetism formation in the Mn-doped CuO nanofibers, in contrast to the mixed magnetic phase composed by both ferromagnetic and paramagnetic behaviors found in the undoped CuO. The vacancy amount was quantified by X-ray absorption spectroscopy (XAS) applying CASTEP software. In addition, an analysis from Cu 2p XPS peaks supports the predicted Cu-Cu rearrangement by the Fullprof software study, while the presence of Cu1+ confirms the substitution of Mn for Cu in the doped sample.

Characterization and potential toxicity of asbestiform erionite from Gawler Downs, New Zealand

Abstract Erionite is the name for a zeolite mineral series originating from diagenesis or hydrothermal alteration of volcanic rocks. The particular erionite “species” is based on the dominant extra-framework cation, erionite-Ca, erionite-K, or erionite Na. Irrespective of the species, erionite can display a fibrous/asbestiform morphology and has been linked with cases of malignant mesothelioma, a disease typically associated with asbestos exposure. Characterization of new discoveries of erionite is therefore important to assess any potential exposure hazards. This study describes a new asbestiform erionite from vesicles within the Upper Cretaceous Mt. Somers Volcanics Group (MSVG), Canterbury, New Zealand. The erionite is within the Hinds River Dacite, the youngest unit within the MSVG at Gawler Downs, ~100 km west of Christchurch, in the foothills of the Southern Alps. A multi-analytical approach was taken to analyze the sample which included micro-Raman spectroscopy, thermogravimetric analysis, electron microscopy, electron microprobe analysis, and X-ray powder diffraction with the Rietveld method. Results confirmed the mineral as fibrous erionite-K. The chemical composition of the mineral is unique due to the presence of higher levels of Mg. While Fe was also identified, this was due to smectite flakes occurring on the surface of the erionite fibers. According to the World Health Organization (WHO) respirable mineral fiber definition, where length ≥5 μm, width ≤3 μm, and aspect ratio (L/w) ≥3:1, the Gawler Downs erionite fibers are respirable, while the fibers themselves exceed respirable thickness. In addition to morphology, a value for the potential toxicity model was computed to be 2.28 for the Gawler Downs erionite. This is similar to those of other carcinogenic erionites from Karain, Turkey (2.33), and Nevada, U.S.A. (2.28). Taken together, results indicate Gawler Downs erionite represents an environmental hazard. Nevertheless, further investigation is required to determine potential environmental exposure pathways by which erionite may become airborne and assess the actual environmental risk in the Gawler Downs area.

Impact of mechanical activation and mechanochemical activation on microstructural changes, leaching rate and leachability of natural chalcopyrite

The influence of mechanical activation (MA) and mechanochemical activation (MCA) with Fe and Fe2O3 on the microstructural changes, leachability and leaching rate of natural chalcopyrite was investigated and compared. MCA pretreatments were carried out by chalcopyrite co-milling with Fe and Fe2O3 for 20 and 50 min. The XRD analysis indicated that even after 50 min MA and MCA, constituent phases of chalcopyrite, Fe and Fe2O3 could be detectable beside the newly formed bornite. Regarding the peak broadening and peak intensity reduction, MCA generally intensified the microstructural changes of chalcopyrite in comparison with MA. The microstructural study performed by the Rietveld method also proved that all microstructural parameters changed in favor of reactivity, such that the amorphization degree and microstrain were increased to 96 % and 0.164 (%), respectively, while crystallite size was reduced to 14.6 nm after 50 min MCA of chalcopyrite with Fe2O3. It could be concluded from the leaching tests that MCA along with Fe and Fe2O3 addition could promote the leachability and leaching rate of chalcopyrite, as compared to MA and nonactivated chalcopyrite. Although both the MCA of chalcopyrite with Fe and Fe2O3 could enhance copper extractions in the 1 M sulfuric acid leaching tests at 80 °C, Fe addition was slightly more effective than Fe2O3. The results obtained from the kinetic study also revealed that the leaching mechanism of nonactivated chalcopyrite, mechanically activated chalcopyrite and mechanochemically activated chalcopyrite with Fe2O3 changed from diffusion control to chemical control due to MCA with Fe. Finally, the combination of kinetic and microstructural studies proved that all microstructural parameters, except for the microstrain parameters of chalcopyrite MCA with Fe2O3, could be effective in chalcopyrite reactivity promotion.

Exploring the Diversity and Dehydration Performance of New Mixed Tutton Salts (K2V1−xM’x(SO4)2(H2O)6, Where M’ = Co, Ni, Cu, and Zn) as Thermochemical Heat Storage Materials

Tutton salts form an isomorphic crystallographic family that has been intensively investigated in recent decades due to their attractive thermal and optical properties. In this work, we report four mixed Tutton crystals (obtained by the slow solvent evaporation method) with novel chemical compositions based on K2V1−xM’x(SO4)2(H2O)6, where M’ represents Co, Ni, Cu, and Zn, aiming at thermochemical energy storage applications. Their structural and thermal properties were correlated with theoretical studies. The crystal structures were solved by powder X-ray diffraction using the Rietveld method with similar compounds. All of the samples crystallized in monoclinic symmetry with the P21/a-space group. A detailed study of the intermolecular interactions based on Hirshfeld surfaces and 2D fingerprint mappings showed that the main interactions arise from hydrogen bonds (H∙∙∙O/O∙∙∙H) and dipole–ion (K∙∙∙O/O∙∙∙K). On the other hand, free space percentages in the unit cells determined by electron density isosurfaces presented low values ranging from 0.53 (V–Ni) to 0.81% (V–Cu). The thermochemical findings from thermogravimetry, a differential thermal analysis, and differential scanning calorimetry indicate that K2V0.47Ni0.53(SO4)2(H2O)6 salt is the most promising among mixed salts (K2V1−xM’x(SO4)2(H2O)6) for heat storage potential, achieving a low dehydration temperature (≈85 °C), high dehydration enthalpy (≈360 kJ/mol), and high energy storage density (≈1.84 GJ/m3).

Synchrotron Micro-X-ray Diffraction in Transmission Geometry: A New Approach to Study Polychrome Stratigraphies in Cultural Heritage

In cultural heritage, paint stratigraphies are complex systems typically consisting of various paint layers with fine crystalline phases mixed with coarse pigment and filler grains. This complexity poses significant challenges for X-ray diffraction (XRD) analysis. In this work, we employed synchrotron radiation micro-X-ray diffraction in transmission geometry (SR-µTXRD) with linear mapping to develop a novel approach for studying the crystalline phases (pigments and fillers) in mock-up paint stratigraphies. A targeted approach was followed for qualitative, quantitative, and microstructural analysis, combining signals from micrometric crystallites and coarse single crystals as well as from randomly oriented and iso-oriented crystalline phases. This allows for identifying, localizing, and quantifying these phases even in low fractions and distinguishes the same phases across different layers with varying grain sizes or spatial orientations. Critical analysis of 2D XRD patterns, coupled with full-profile fitting performed by the Rietveld method, provides insights into material preparation (e.g., grinding), painting technique (e.g., color palette, use of fillers, brushing), and crystallo-chemical modifications over time. This analytical approach, integrating spatially resolved investigation with high-quality phase characterization, enhances the potential of specific XRD methodologies for a 2D investigation of multi-phase materials in cultural heritage, even without dedicated micro-mapping techniques.

Tailoring the structural and optical properties of lead-free Na0.5(Bi1-xSmx)0.5TiO3 multifunctional ceramics by Sm-doping

In this study, the effects of Sm3+-content on the structural and optical properties of the Na0.5(Bi1-xSmx)0.5TiO3 multifunctional lead-free system were investigated using x-ray diffraction (XRD), ultraviolet-visible (UV-Vis), Raman spectroscopy and photoluminescence (PL) spectroscopy. The Na0.5(Bi1-xSmx)0.5TiO3 (x = 0.000, 0.005, 0.010, 0.015, and 0.020) ceramics were synthesized by the solid-state reaction method with subsequent annealing. The Rietveld method was used to refine the XRD data. The results of these refinements indicated that pure NBT (Na0.5Bi0.5TiO3) and the Sm3+-doped samples showed the coexistence of the rhombohedral (R3c) and tetragonal (P4bm) phases in different fractions, which depend on the Sm3+-content. The UV-Vis data revealed that the optical band gap of the Na0.5(Bi1-xSmx)0.5TiO3 samples monotonically decreases with increasing Sm3+-content, providing evidence of replacement of Bi3+- by Sm3+-ions. Furthermore, Raman spectroscopy confirmed that substitution of Bi3+- by Sm3+-ions leads to a shortening of the Na/Bi-O bond length. It was demonstrated that this behavior is responsible for the increase in the local symmetry of the TiO6 octahedron and the consequent decrease in the ratio between both rhombohedral and tetragonal phases, as observed by the XRD data. The findings from the PL data revealed typical emissions corresponding to transitions between the 4G5/2 → 6Hj (j = 5/2, 7/2, 9/2, 11/2, 13/2) states of the Sm3+-ion. Additionally, the presence of non-radiative recombination processes was found to depend on both laser pumping power and Sm3+-content.

Investigating the microstructure and mechanical properties of Al–Ag-Sc ultra-fine grain alloy processed by accumulative rolling bonding method

The aim of the present study is to investigate the effect of accumulative roll bonding (ARB) and precipitation hardening on the microstructure development and there of mechanical properties of ultrafine grained Al–Ag-Sc alloy. For this purpose, the samples were heated to a temperature of 600 °C for 24 h, and then they were quenched in water. In order to carry out the two-stage precipitation hardening process, the samples were placed in the furnace at a temperature of 350 °C for 5000 s in the first stage, which was followed by quenching in water. In the second stage, they were heated to 250 °C for 5000 s following by water quenching too. Following, the samples were subjected to the ARB for up to 8 cycles. Scanning Electron Microscope (SEM) equipped with Electron Backscatter Diffraction (EBSD) and energy dispersive spectroscopy (EDS) techniques, and X-Ray Diffraction (XRD) was used to verify the microstructure and phase analysis of the prepared samples. Also, tensile and microhardness tests were conducted to confirm the mechanical properties, and pin-on-disk tests were done to check wear behavior. Microstructural parameters such as crystallite size, microstrain, and density of dislocations in rolled sheets were estimated using the Rietveld method. The Results have shown that applying various cycles of the ARB process leads to the development of ultra/nano grain structure. In that sense, performing 8-cycle of the ARB transformed the low angle grain boundaries (LAGBs) of the 4-cycle ARB condition to high angle grain boundaries (HAGBs). Results showed that there is proper welding between different layers, except for the layers created in the last cycle. Similarly, the obtained size of the crystallites demonstrates that the samples become finer when ARB cycles are increased. The results of the mechanical tests indicated that after 8 cycles, there is approximately 3.5-fold and 2.5-fold increase in the tensile strength and hardness compared to the original (annealed) sample, respectively. While the elongation decreased slowly and reached 1.5% in the 8th cycle. A fractography of the fracture surface of the original sample included deep and coaxial dimples, indicating a ductile fracture. Analysis of wear surface degradation showed that scratch wear occurred for all samples.

Fabrication, structure, and physical properties of three-B-site perovskite Ba(Zr1–2xTixCex)O3

In this study, three-B-site perovskite Ba(Zr1–2xTixCex)O3 (x=0–0.2) materials with the co-substitution of Ti4+ and Ce4+ at the Zr-site of barium zirconate (BaZrO3) were successfully prepared. The analyses of XRD & Rietveld method, SEM, and TEM indicated that the substituted ions Ti4+ and Ce4+ entered the BaZrO3 lattice to form a single-phase solid solution, showing a conventional primitive cubic perovskite structure (Pm-3 m space group), and its lattice parameters gradually increased from 0.4192 nm to 0.4206 nm with x value. The sample with x=0.1 exhibited relatively optimal structural uniformity and densification, as well as comprehensive physical properties. The sample Ba(Zr0.8Ti0.1Ce0.1)O3 showed a minimum mean grain size of 1.50 μm. And due to the combined effect of solid solution formation and grain refinement, it displayed an apparent porosity of 1.42 % with a cold modulus of rupture (CMOR) of 123.8 MPa, and a thermal conductivity at ambient temperature of 2.197 W/mK. Furthermore, this three-B-site perovskite Ba(Zr1–2xTixCex)O3 exhibits excellent high-temperature stability. This study demonstrates the promising application of the dense, high-strength, and low-thermal conductivity Ba(Zr0.8Ti0.1Ce0.1)O3 perovskite material in the field of advanced refractory ceramics.

Microwave-assisted hydrothermal synthesis of carbonated apatite with calcium and phosphate resources derived from green mussel shell and bovine bone wastes

Resources recovery of calcium and phosphates from respective green mussel shells and bovine bones by calcination and chemically extracting are viable precursors for carbonate-rich apatite biomedical material applications. Because of their high osteoconductivity, carbonate-rich apatite bioceramics are being studied intensively for synthetic bone transplants. In the study, powder processing routes of calcination and following chemical dissolution in MgCl2 and H2SO4 were each for recovering calcium of mussel shells and phosphate of bovine bones yielding a crystal-forming solution feedstock for use in microwave-irradiated synthesis. FTIR spectra and XRD patterns validated the crystallinity and phase identification for as-synthesized powders. As a result, the presence of CO3, PO43-, and OH- bands in carbonate-calcium phosphate complexes were present in FTIR spectra. According to the XRD Rietveld method, the as-synthesized powder product contained brushite, carbonated hydroxyapatite (CHA), calcite, and gypsum. The recoverable CHA crystallites' size was 40 nm. This present study demonstrated that microwave irradiation synthesis of CHA powder with calcium and phosphates derived from mussel shells and bovine bones is the potential to yield a large amount of CHA for bioceramics and would aid in the design of a powder processing step for preparing the CHA powder precursor in biomedical applications.

Crystal Structure Parameter Analysis of Reduced Graphene Oxide (rGO) from Coconut Shell Charcoal

In this research, reduced graphene oxide (rGO) material from coconut shell charcoal was synthesized using the modified Hummer method. The reduction process of Graphene Oxide (GO) to rGO uses the reducing agent L-Ascorbic Acid (LAA) and is assisted by microwave radiation. The samples obtained were then characterized using XRD to analyze the crystal structure parameters of the rGO samples obtained. Based on the XRD results, the data obtained was then analyzed using the Scherrer and modified Scherrer equations to determine the crystal size in the sample. In addition, the Williamson-Hall equation is also used to analyze crystal size and lattice strain. This article also analyzes XRD data using the Rietveld method using Rietica software. The output from the Rietica software obtained lattice parameter values a ≠ b ≠ c and angle α = β = γ = 90° which indicates an orthorhombic crystal lattice structure. In the refinement process, Rietica's software affects the suitability parameters in the form of R and GOF indicator values. The sample obtained was also measured for the electrical conductivity value of the rGO sample using an LCR meter.

Study of the identity of the polymorphic form of API – dapagliflosin derivative and of its permanency structure under the influence of the tableting process

The aim. To investigate the polymorphic structure of the API – Dapagliflozin propanediol monohydrate and to reveal the absence of an effect of the tabletting process on the polymorphic structure of the API in model compositions of tablets. Materials and methods. Model mixtures of API - dapagliflozin propanediol monohydrate and excipients were studied. The research used the method of designing pharmaco-technological parameters of solid dosage forms, the method of quantum-chemical modelling of the mechanical properties of polymorphic modifications of APIs, the modelling of shear deformation, the nanoindentation method, the Rietveld method for calculating X-ray patterns, X-ray structural analysis of API and selected model compositions of tablets. Results. The polymorphic structure of API - dapagliflozin propanediol monohydrate and its polymorphic structure in selected model compositions of tablets produced by the pressing method were studied and analyzed. An X-ray structural study was carried out, and the qualitative and phase composition of samples and polymorphic modifications of API and model series of tablets were determined. According to the results of the X-ray structural analysis, it was established that there is no polymorphic transition and that the polymorphic structure of API is invariant under the influence of pressing pressure, which ensures the quality of the tablet form. Conclusions. The design of an experimental study was determined based on the application of the QbD concept, design of experiments – DoE, for designing and ensuring a high-quality technological process – tabletting of API - Dapagliflozin propanediol monohydrate and excipients. To manage a critical technological parameter - the stability of the polymorphic structure of the API, which guarantees the quality of the tablet form, its bioavailability and bioequivalence, it is necessary to use a set of methods for studying structural changes and polymorphic modifications of the API during the tableting process. According to the results of the X-ray structural study of API and selected model compositions of tablets, it was established that during the process of tabletting under pressure, the structure of the polymorphic modification of dapagliflozin propanediol monohydrate does not change, and no polymorphic transition is observed

Obtaining of disordered highly ionic conductive Ag7+x(P1−xSix)S6 single crystalline materials

For the first time, bulk single crystals of the Ag7+x(P1−xSix)S6 solid solution were obtained via directional crystallization from the melt. The crystal structure of the Ag7+x(P1−xSix)S6 solid solution was determined by the Rietveld method. It was demonstrated that Ag7+x(P1−xSix)S6 solid solutions crystallize in two crystal systems—cubic and orthorhombic, and different SG: P213, F-43m and Pna21. The grown crystals were studied by SEM and EDS methods. The electrical parameters of Ag7+x(P1−xSix)S6 were studied in wide frequency and temperature ranges. Established that Ag7+x(P1−xSix)S6 solid solutions exhibit an increase in ionic conductivity compared to the initial compounds. Among the studied solid solutions, the Ag7.25P0.75Si0.25S6 sample demonstrated the highest conductivity with values reaching σion = 2.9 × 10−2 S/cm. The lowest activation energy value (Ea(ion) = 0.2 eV) is also observed for the given composition of solid solutions. The mechanism of ion transport is considered within the context of limiting distances and position occupancy.

Production of dense forsterite with ultra low dielectric loss using ZrO2 additive

Forsterite was synthesized with MgCO3 and SiO2 powders using a solid-state method at 1200–1300°C. The ceramic specimen with the highest forsterite phase content was sintered with the ZrO2 sintering aid at mass fractions of 0.5, 1.0, and 1.5 wt% at 1400°C for 4 h. The dielectric constant and loss tangent were also measured via the waveguide method at 8–12 GHz. The formation of enstatite and cristobalite was minimized through precise synthesis temperature control. Phase measurement by the Rietveld method showed that specimen F28 contained more than 99.8% forsterite. It was found that ZrO2 reduced the pore volume percent and increased the density even at low mass fractions. A liquid phase on the grain boundaries was demonstrated. The solid ceramic specimen F28-15Z showed a dielectric constant of 6.5 and high quality factor of 189000.

Ternary intermetallic compounds R23Ru7In4 (R[dbnd]Ce, Pr): Synthesis, crystal structure and physical properties

Two novel ternary intermetallic compounds Ce23Ru7In4 and Pr23Ru7In4 were synthesized by arc melting of components and subsequent annealing at 600 °C. Both compounds crystallize in a hexagonal cell, with structure type Pr23Ir7Mg4, space group P63mc (№ 186), Pearson symbol hP68, Z = 2, the cell parameters: a = 9.861(5) Å, c = 22.520(12) Å (Ce); a = 9.9260(7) Å, c = 22.4109(2) Å (Pr). The structure of Ce23Ru7In4 was determined by single-crystal X-ray diffraction and the structure of Pr23Ru7In4 was determined by the Rietveld method using powder X-ray diffraction pattern. Compound Ce23Ru7+xIn4-x exist in the homogeneity range 0 ≤ x ≤ 3. An essential feature of compound Ce23Ru7In4 is the presence of abnormally short distances Ce–Ru (2.637 Å, 2.735 Å). The compound Pr23Ru7In4 melts incongruently and compound Ce23Ru7In4 melts congruently at temperatures 756 and 683°С respectively. The Pr23Ru7In4 compound is characterized by the presence of a magnetic transition at 12 K. The observed magnetic transition is most likely indicative of a transition to the spin glass state.

Polar orientation and extension in a novel crystallographic model for PbTiO3-based perovskites explaining the experimental ferroelectric thermal anomalies

PbTiO3-based ferroelectric solid-solution ceramics have been widely used for electromechanical devices. However, it is still challenging to separate and control the contributions to the electromechanical functionalities, mainly as a function of temperature, where thermal anomalies and phase transitions can be observed. This study investigates the ultrasonic velocity and attenuation and the dielectric, ferroelectric and structural features of Pb0.55Ca0.45TiO3 ceramics from low temperatures (10 or 115 K) up to room temperature as an example of A-site isovalent substitution in PbTiO3. Such a combination of information makes possible the phenomenological deconvolution of the effects of ferroelectric domain wall pinning and structural features on spontaneous electric polarization. The room-temperature symmetry was determined as Pna21. The results show that this model refined by the Rietveld method for synchrotron X-ray diffraction patterns from 115 K to room temperature can explain the polarization extension features of these materials during heating. This study shows a correlation between structural thermal anomalies and low-temperature electric polarization in PbTiO3-based ferroelectric ceramics.

Effects of pore structure and chloride binding capacity on chloride diffusion in limestone cement paste

The limestone powder has been a preferred admixture in cement-based materials due to its abundant availability and potential to reduce carbon emission. The purpose of this study is to clarify the key influencing factors for chloride diffusion in cement paste as limestone is added. The pore structure, chloride binding capacity and chloride diffusivity of cement paste with different limestone addition and fineness were measured. The deconvolution of physically and chemically bound chloride was achieved by combining X-ray diffraction, energy dispersive spectroscopy and the Rietveld method. The results show that the addition of fine limestone increases the number of 50–100 nm pores while the coarse limestone leads to more pores in the size range of 100–1000 nm. As the limestone content increases, less chloride is bound by physical adsorption while more Friedel’s salt is formed. The effective chloride diffusivity is almost unaffected when less than 10 % fine limestone is added because of increased pore tortuosity. The changes of chloride binding capacity and chloride diffusivity are equally important for the chloride diffusion when 20 % fine limestone is added. On the other hand, the reduction of chloride resistance of cement paste containing coarse limestone is mainly due to the increase of the chloride diffusivity.

Synthesis and in-depth structure determination of a novel metastable high-pressure CrTe3 phase

This study reports the synthesis and crystal structure determination of a novel CrTe3 phase using various experimental and theoretical methods. The average stoichiometry and local phase separation of this quenched high-pressure phase were characterized by ex situ synchrotron powder X-ray diffraction and total scattering. Several structural models were obtained using simulated annealing, but all suffered from an imperfect Rietveld refinement, especially at higher diffraction angles. Finally, a novel stoichiometrically correct crystal structure model was proposed on the basis of electron diffraction data and refined against powder diffraction data using the Rietveld method. Scanning electron microscopy–energy-dispersive X-ray spectrometry (EDX) measurements verified the targeted 1:3 (Cr:Te) average stoichiometry for the starting compound and for the quenched high-pressure phase within experimental errors. Scanning transmission electron microscopy (STEM)–EDX was used to examine minute variations of the Cr-to-Te ratio at the nanoscale. Precession electron diffraction (PED) experiments were applied for the nanoscale structure analysis of the quenched high-pressure phase. The proposed monoclinic model from PED experiments provided an improved fit to the X-ray patterns, especially after introducing atomic anisotropic displacement parameters and partial occupancy of Cr atoms. Atomic resolution STEM and simulations were conducted to identify variations in the Cr-atom site-occupancy factor. No significant variations were observed experimentally for several zone axes. The magnetic properties of the novel CrTe3 phase were investigated through temperature- and field-dependent magnetization measurements. In order to understand these properties, auxiliary theoretical investigations have been performed by first-principles electronic structure calculations and Monte Carlo simulations. The obtained results allow the observed magnetization behavior to be interpreted as the consequence of competition between the applied magnetic field and the Cr–Cr exchange interactions, leading to a decrease of the magnetization towards T = 0 K typical for antiferromagnetic systems, as well as a field-induced enhanced magnetization around the critical temperature due to the high magnetic susceptibility in this region.

Batch Sintering of FeO·OH and Fe2O3 Blends: Chemical and Metallurgical Characterization

A sample of goethite iron ore sinter feed (G_SF) was employed as a raw material in a sintering bed. This sample partially replaced hematite sinter feed (H_SF), which is currently used as raw material in a sintering plant in the state of Minas Gerais, Brazil. This substitution did not adversely affect the chemical and metallurgical proprieties of the sinter mix product, provided that the utilization of G_SF was kept below 30% in weight. Despite the higher proportion of fines in G_SF, the presence of argillaceous minerals in the sample led to an improvement in the granulation index (GI) of the sinter mix product. The GI value increased from 68.4 to 82.7% for the experiments conducted without the presence of goethite ore and with 40% of goethite ore in the sintering mix, respectively. Consequently, the qualities of both the process and the produced sinter product were not compromised. The raw materials and the various sinters produced were characterized through X-ray fluorescence (XRF) and X-ray diffraction (XRD), as well as thermal gravimetric analysis (TGA). The XRD results were used to perform a quantitative assessment of the mineral phase using the Rietveld method (RM). This technique allowed for the determination of goethite content in the studied sample, which was 35.5%. Finally, the incorporation of G_SF in the sintering bed led to a 20% reduction in the cost of raw materials.

Improving the optical and dielectric characteristics of PVA/PVP/PEG/ZnWO4/CdS blends

This work aims to create novel nanocomposite blended polymers by incorporating (1−x)ZnWO4-xCdS into poly (vinyl alcohol) (PVA)/polyvinyl pyrrolidone (PVP)/polyethylene glycol (PEG) blend to employ these nanocomposites in various optoelectronic applications. This study focused on investigating the structural, optical and electrical features of PVA/PVP/PEG/(1−x)ZnMn2O4-xCdS blends. The x-ray diffraction and scanning electron microscope techniques were used to explore the structure and morphology of the formed samples. The structure and percentages of ZnWO4 and CdS in different fillers were performed using Rietveld method. The doped blends exhibited significant absorption of UVA and UVB types. The greatest amounts of absorption were observed when the filler contained 25 % CdS. The direct and indirect optical band gaps of the doped blend became 5.02 and (1.88, 2.37) eV as the amount of CdS became 25 % in the filler sample. The refractive index, optical dielectric constant, optical conductivity, and nonlinear optical parameters are affected by the amount of CdS in the fillers. The fluorescence spectra for the blends affected by the excitation wavelength and amount of CdS in the filler. The maximum energy density of the doped blend was reached when the amount of CdS in the filler reached 25 %. The purities of emitted color in the undoped blend are 83 % and 74 % under excitation wavelengths of 317 nm and 380 nm. The purity of the blend experienced a slight change when loaded with filler samples. As the ZnWO4 doping of the PVA/PVP/PEG blended polymer rose, its electrical dielectric constant and ac conductivity first enhanced and then irregularly declined as the filler's CdS content rose. Incorporating (1−x)ZnWO4-xCdS into the nanocomposite enhanced their optical and electrical properties, making them a potential material for flexible optoelectronic and energy storage uses.

Determine elastic parameters and nanocrystalline size of spinel ferrites MFe2O4 (M = Co, Fe, Mn, Zn) through X-ray diffraction and infrared spectrum: Comparative approach

MFe2O4 (M = Co, Fe, Mn, Zn) nanoparticles were successfully synthesized by coprecipitation. Analyzing the X-ray diffraction by the Rietveld method confirmed the spinel ferrite structure of the samples. Rietveld refinement results show that Co, Mn and Zn occupy both the tetrahedral and octahedral sites. Variation in elastic parameters was determined by Fourier transform infrared spectroscopy, and cation distribution was deduced from X-ray diffraction. X-ray diffraction peak expansion was analyzed by employing a variety of calculating methods such as modified Scherrer, Williamson–Hall, size–strain, and Halder–Wagner to determine the crystallite size and elastic parameters of the cubic-structured MFe2O4 nanoparticles, including intrinsic strain, stress, and energy density. Comparison of the results obtained from these different methods revealed that they are ideally suited to each other. Moreover, the transmission electron microscopy image confirmed that the average size of MFe2O4 (M = Co, Fe, Mn, Zn) nanoparticles ranges from 10 to 14 nm, consistent with the dimensions obtained from the preceding methods.