Search results for: Rietveld analysis

Authors: Kausar Harun, Ahmad Azmin Mohamad

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Zinc oxide (ZnO) has been extensively used in optoelectronic devices, with recent interest as photoanode material in dye-sensitize solar cell. Numerous methods employed to experimentally synthesized ZnO, while some are theoretically-modeled. Both approaches provide information on ZnO properties, but theoretical calculation proved to be more accurate and timely effective. Thus, integration between these two methods is essential to intimately resemble the properties of synthesized ZnO. In this study, experimentally-grown ZnO nanoparticles were prepared by sol-gel storage method with zinc acetate dihydrate and methanol as precursor and solvent. A 1 M sodium hydroxide (NaOH) solution was used as stabilizer. The optimum time to produce ZnO nanoparticles were recorded as 12 hours. Phase and structural analysis showed that single phase ZnO produced with wurtzite hexagonal structure. Further work on quantitative analysis was done via Rietveld-refinement method to obtain structural and crystallite parameter such as lattice dimensions, space group, and atomic coordination. The lattice dimensions were a=b=3.2498Å and c=5.2068Å which were later used as main input in first-principles calculations. By applying density-functional theory (DFT) embedded in CASTEP computer code, the structure of synthesized ZnO was built and optimized using several exchange-correlation functionals. The generalized-gradient approximation functional with Perdew-Burke-Ernzerhof and Hubbard U corrections (GGA-PBE+U) showed the structure with lowest energy and lattice deviations. In this study, emphasize also given to the modification of valence electron energy level to overcome the underestimation in DFT calculation. Both Zn and O valance energy were fixed at Ud=8.3 eV and Up=7.3 eV, respectively. Hence, the following electronic and optical properties of synthesized ZnO were calculated based on GGA-PBE+U functional within ultrasoft-pseudopotential method. In conclusion, the incorporation of Rietveld analysis into first-principles calculation was valid as the resulting properties were comparable with those reported in literature. The time taken to evaluate certain properties via physical testing was then eliminated as the simulation could be done through computational method.

Keywords: density functional theory, first-principles, Rietveld-refinement, ZnO nanoparticles

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Authors: Xiaopeng Shang, Xin YU, Jun CHANG

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Calcium barium sulphoaluminate (CBSA), derived from calcium sulphoaluminate(CSA), has excellent cementitious properties. In this study, the sintering system of CBSA with a theoretical stoichiometric Ca3BaAl6SO16 was investigated. Rietveld refinement was performed using TOPAS 4.2 software to quantitatively calculate the content of CBSA and the actual ionic site occupancy of Ba2+. The results indicate that the contents of Ca4-xBaxAl6SO16 increases with increasing sintering temperature in the 1200℃-1400℃ ranges. When sintered at 1400℃ for 180min, the content of CBSA reaches 88.4%. However, CBSA begins to decompose at 1440℃ and the content of which decreases. The replacement rate of Ba2+ was also enlarged by increasing sintering temperature and prolonged sintering time. Sintering at 1400℃ for 180min is considered as the optimum when replacement rate of Ba2+ and the content of CBSA were taken into account. Ca3.2Ba0.8Al6SO16 with a content of 88.4% was synthesized.

Keywords: calcium barium sulphoaluminate, sintering system, Ba2+ replacement rate, Rietveld refinement

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Authors: A. Chari, A. El Bouari, B. Orayech, A. Faik, J. M. Igartua

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The phosphate is a natural resource of great importance in Morocco. In order to exploit this wealth, synthesis and studies of new a material based phosphate, were carried out. The apatite structure present o lot of characteristics, One of the main characteristics is to allow large and various substitutions for both cations and anions. Beside their biological importance in hard tissue (bone and teeth), apatites have been extensively studied for their potential use as fluorescent lamp phosphors or laser host materials.The apatite have interesting possible application fields such as in medicine as materials of bone filling, coating of dental implants, agro chemicals as artificial fertilizers. The LiPb2Ca2(PO4)3 was synthesized by the solid-state method, its crystal structure was investigated by Rietveld analysis using XRPD data. This material crystallizes with a structure of lacunar apatite anion deficit. The LiPb2Ca2(PO4)3 is hexagonal apatite at room temperature, adopting the space group P63/m (ITA No. 176), Rietveld refinements showed that the site 4f is shared by three cations Ca, Pb and Li. While the 6h is occupied by the Pb and Li cations. The structure can be described as built up from the PO4 tetrahedra and the sixfold coordination cavities, which delimit hexagonal tunnels along the c-axis direction. These tunnels are linked by the cations occupying the 4 f sites. Raman and Infrared spectroscopy analyses were carried out. The observed frequencies were assigned and discussed on the basis of unit-cell group analysis and by comparison to other apatite-type materials.

Keywords: apatite, Lacunar, crystal structure, Rietveldmethod, LiPb2Ca2(PO4)3, Phase transition

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Authors: E. A. Asabina, V. I. Pet'kov, P. A. Mayorov, A. V. Markin, N. N. Smirnova, A. M. Kovalskii, A. A. Usenko

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The purpose of this work was to synthesize and investigate phase formation, structure and thermophysical properties of the phosphates M_0.5+xM'_xZr_2–x(PO₄)₃ (M – Cd, Sr, Pb; M' – Mg, Co, Mn). The compounds were synthesized by sol-gel method. The results showed formation of limited solid solutions of NZP/NASICON type. The crystal structures of triple phosphates of the compositions MMg_0.5Zr_1.5(PO₄)₃ were refined by the Rietveld method using XRD data. Heat capacity (8–660 K) of the phosphates Pb_0.5+xMg_xZr_2-x(PO₄)₃ (x = 0, 0.5) was measured, and reversible polymorphic transitions were found at temperatures, close to the room temperature. The results of Rietveld structure refinement showed the polymorphism caused by disordering of lead cations in the cavities of NZP/NASICON structure. Thermal expansion (298−1073 K) of the phosphates MMg_0.5Zr_1.5(PO₄)₃ was studied by XRD method, and the compounds were found to belong to middle and low-expanding materials. Thermal diffusivity (298–573 K) of the ceramic samples of phosphates slightly decreased with temperature increasing. As was demonstrated, the studied phosphates are characterized by the better thermophysical characteristics than widespread fire-resistant materials, such as zirconia and etc.

Keywords: NASICON, NZP, phosphate, structure, synthesis, thermophysical properties

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Authors: Karthika Chandran, Pulkit Prakash, Amitabh Das, Santhosh P. N.

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Rare earth orthoferrites (RFeO₃) exhibit interesting and useful magnetic properties like multiferroicity, magnetodielectric coupling, spin reorientation (SR) and exchange bias. B site doped RFeO₃ are attracting attention due to the complex and tuneable magnetic transitions. In this work, 45% Mn-doped HoFeO₃ polycrystalline sample (HoFe₀.₅₅Mn₀.₄₅O₃) was synthesized by a solid-state reaction method. The magnetic structure and transitions were studied by magnetization measurements and neutron powder diffraction methods. The neutron diffraction patterns were taken at 13 different temperatures from 7°K to 300°K (7°K and 25°K to 300°K in 25°K intervals). The Rietveld refinement was carried out by using a FULLPROF suite. The magnetic space groups and the irreducible representations were obtained by SARAh module. The room temperature neutron diffraction refinement results indicate that the sample crystallizes in an orthorhombic perovskite structure with Pnma space group with lattice parameters a = 5.6626(3) Ǻ, b = 7.5241(3) Ǻ and c = 5.2704(2) Ǻ. The temperature dependent magnetization (M-T) studies indicate the presence of two magnetic transitions in the system ( TN Fe/Mn~330°K and TSR Fe/Mn ~290°K). The inverse susceptibility vs. temperature curve shows a linear behavior above 330°K. The Curie-Weiss fit in this region gives negative Curie constant (-34.9°K) indicating the antiferromagnetic nature of the transition. The neutron diffraction refinement results indicate the presence of mixed magnetic phases Γ₄(AₓFᵧG

Keywords: neutron powder diffraction, rare earth orthoferrites, Rietveld analysis, spin reorientation

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Authors: Mohammed Mesrar, Hamza El Malki, Hamza Mesrar

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In this study, ceramics of (1-x)(Na0.5Bi0.5)TiO3 x(K0.5 Bi0.5)TiO3 were synthesized through a conventional calcination process (solid-state method) at 1000°C for 4 hours, with x(%) values ranging from 0.0 to 100. Room temperature XRD patterns confirmed the phase formation of the samples. The Rietveld refinement method was employed to verify the morphotropic phase boundary (MPB) at x(%)=16-20. We investigated the average crystallite size and lattice strain using Scherrer's formula and Williamson-Hall (W-H) analysis. SEM image analyses provided additional evidence of the impact of doping on structural growth under low temperatures. Relaxation time extracted from Z″(f) and M″(f) spectra for x(%) = 0.0, 12, 16, 20, and 30 followed the Arrhenius law, revealing the presence of three distinct relaxation mechanisms with varying activation energies. The shoulder response in M″(f) indirectly indicated the existence of highly polarizable entities in the samples, serving as a signature of polar nanoregions (PNRs) within the grains.In this study, ceramics of (1-x)(Na0.5Bi0.5)TiO3 x(K0.5 Bi0.5)TiO3 were synthesized through a conventional calcination process (solid-state method) at 1000°C for 4 hours, with x(%) values ranging from 0.0 to 100. Room temperature XRD patterns confirmed the phase formation of the samples. The Rietveld refinement method was employed to verify the morphotropic phase boundary (MPB) at x(%)=16-20. We investigated the average crystallite size and lattice strain using Scherrer's formula and Williamson-Hall (W-H) analysis. SEM image analyses provided additional evidence of the impact of doping on structural growth under low temperatures. Relaxation time extracted from Z″(f) and M″(f) spectra for x(%) = 0.0, 12, 16, 20, and 30 followed the Arrhenius law, revealing the presence of three distinct relaxation mechanisms with varying activation energies. The shoulder response in M″(f) indirectly indicated the existence of highly polarizable entities in the samples, serving as a signature of polar nanoregions (PNRs) within the grains.

Keywords: (1-x)(Na0.5Bi0.5)TiO3 x(K0.5 Bi0.5)TiO3, Rietveld refinement, Scanning electron microscopy (SEM), Williamson-Hall plots, charge density distribution, dielectric properties

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Authors: Oladejo S. O, Tomori W. B, Adebayo A. O

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The main objective of this research is to identify the geochemical and mineralogical characteristics potential of unexplored tailings around the gold deposit region using spatial statistics and map modeling. Some physicochemical parameters such as pH, redox potential, electrical conductivity, cation exchange capacity, total organic carbon, total organic matter, residual humidity, Cation exchange capacity, and particle size were determined from both the mine drains and tailing samples using standard methods. The physicochemical parameters of tailings ranges obtained were pH (6.0 – 7.3), Eh (−16 - 95 Mev), EC (49 - 156 µS/cm), RH (0.20-2.60%), CEC (3.64-6.45 cmol/kg), TOC (3.57-18.62%), TOM (6.15-22.93%). The geochemical oxide composition were identified using Proton Induced X-ray emission and the results indicated that SiO2>Al2O3>Fe2O3>TiO2>K2O>MgO>CaO>Na2O> P2O5>MnO>Cr2O3>SrO>K2O>P2O5. The major mineralogical components in the tailing samples were determined by quantitative X-ray diffraction techniques using the Rietveld method. Geostatistical relationships among the known points were determined using ArcGIS 10.2 software to interpolate mineral concentration with respect to the study area. The Rietveld method gave a general Quartz value of 73.73-92.76%, IImenite as 0.38-4.77%, Kaolinite group as 3.19-20.83%, Muscovite as 0.77-11.70% with a trace of other minerals. The high percentage of quartz is an indication of a sandy environment with a loose binding site.

Keywords: tailings, geochemical, mineralogy, spatial

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Authors: G. Çelik Gül, F. Kurtuluş

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Rare earths containing complex metal oxides have drawn much attention due to physical, chemical and optical properties which make them feasible in so many areas such as non-linear optical materials and ion exchanger. We have researched a systematic study to obtain rare earth containing zirconium molybdate compound, characterization, investigation of crystal system and calculation of unit cell parameters.  After a successful synthesis of Nd₂Zr₃(MoO₄)₉ which is a member of rare earth metal containing complex oxides family, X-ray diffraction (XRD), High Score Plus/Rietveld refinement analysis, and Fourier Transform Infrared Spectroscopy (FTIR) were completed to determine the crystal structure. Morphological properties and elemental composition were determined by scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) analysis. Thermal properties were observed via Thermogravimetric-differential thermal analysis (TG/DTA).

Keywords: Nd₂Zr₃(MoO₄)₉, powder x-ray diffraction, solid state synthesis, zirconium molybdates

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Authors: Suresh Palla, Kalpna Sharma, Gaurav Bhatnagar, S. K. Chaturvedi, B. N. Mohapatra

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Determining the content of free lime is especially important to judge reactivity of the raw materials and clinker quality. The free lime limit isn’t the same for all cements; it depends on several factors, especially the temperature reached during the cooking and the grain size distribution in cement after grinding. Estimation of free lime by conventional method is influenced by the presence of portlandite and misleads the actual free lime content in the clinker for quality check up conditions. To ensure the product quality according to the standard specifications in terms of within the quality limits or not, a reliable, precise, and very reproducible method to quantify the relative phase abundances in the Portland Cement clinker and Portland Cements is to use X-ray diffraction (XRD) in combination with the Rietveld method. In the present study, a methodology was proposed using XRD to validate the obtained results of free lime by conventional method. The XRD and TG/DTA results confirm the presence of portlandite in the clinker to take the decision on the obtained free lime results through conventional method.

Keywords: free lime, quantitative phase analysis, conventional method, x ray diffraction

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Authors: M. P. Joshi, F. Deganello, L. F. Liotta, V. La Parola, G. Pantaleo

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For the first time, commercial iron nitrate was replaced by rust wastes, as a source of Iron for the preparation of LaFeO₃ powders by solution combustion synthesis (SCS). A detailed comparison with a reference powder obtained by SCS, starting from a commercial iron nitrate, was also performed. Several techniques such as X-ray diffraction combined with Rietveld refinement, mass plasma atomic emission spectroscopy, nitrogen adsorption measurements, temperature programmed reduction, X-ray photoelectron spectroscopy, Fourier transform analysis and scanning electron microscopy were used for the characterization of the rust wastes as well as of the perovskite powders. The performance of this ecofriendly material was evaluated by testing the activity and selectivity in the propylene oxidation, in order to use it for the benefit of the environment. Characterization and performance results clearly evidenced limitations and peculiarities of this new approach.

Keywords: perovskite type catalysts, solution combustion synthesis, X-ray diffraction, rust wastes

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Authors: Nidhi Adhlakha, K. L. Yadav

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Three phase magnetoelectric (ME) composites (1-x)(0.7BiFeO3-0.3CoFe2O4)-xPbTiO3 (or equivalently written as (1-x)(0.7BFO-0.3CFO)-xPT) with x variations 0, 0.30, 0.35, 0.40, 0.45 and 1.0 were synthesized using hybrid processing route. The effects of PT addition on structural, multiferroic and optical properties have been subsequently investigated. A detailed Rietveld refinement analysis of X-ray diffraction patterns has been performed, which confirms the presence of structural phases of individual constituents in the composites. Field emission scanning electron microscopy (FESEM) images are taken for microstructural analysis and grain size determination. Transmission electron microscopy (TEM) analysis of 0.3CFO-0.7BFO reveals the average particle size to be lying in the window of 8-10 nm. The temperature dependent dielectric constant at various frequencies (1 kHz, 10 kHz, 50 kHz, 100 kHz and 500 kHz) has been studied and the dielectric study reveals that the increase of dielectric constant and decrease of average dielectric loss of composites with incorporation of PT content. The room temperature ferromagnetic behavior of composites is confirmed through the observation of Magnetization vs. Magnetic field (M-H) hysteresis loops. The variation of magnetization with temperature indicates the presence of spin glass behavior in composites. Magnetoelectric coupling is evidenced in the composites through the observation of the dependence of the dielectric constant on the magnetic field, and magnetodielectric response of 2.05 % is observed for 45 mol% addition of PT content. The fractional change of magnetic field induced dielectric constant can also be expressed as ∆ε_r~γM^2 and the value of γ is found to be ~1.08×10-2 (emu/g)-2 for composite with x=0.40. Fourier transformed infrared (FTIR) spectroscopy of samples is carried out to analyze various bonds formation in the composites.

Keywords: composite, X-ray diffraction, dielectric properties, optical properties

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Authors: Hakan Gungunes, Ismail A. Auwal, Abdulhadi Baykal, Sagar E. Shirsath

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Barium hexaferrite, BaFe₁₂O₁₉, substituted by Bi³⁺ and La³⁺ (BaBiₓLaₓFe₁₂₋₂ₓO₁₉ where 0.0 ≤ x ≤ 0.5) were prepared by solid state synthesis route. The effect of substituted Bi³⁺ and La³⁺ ions on the structure, morphology, magnetic and cation distributions of barium hexaferrite were investigated by X-ray powder diffractometry (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), Fourier transform infrared spectroscopy (FT-IR) and Mössbauer spectroscopy. XRD powder patterns were refined by the Rietveld analysis method which confirmed the formation of single phase magneto-plumbite structure and the substitution of La³⁺ and Bi³⁺ ions into the lattice of barium ferrite. These results show that both La³⁺ and Bi³⁺ ions completely enter into barium hexaferrite lattice without disturbing the hexagonal ferrite structure. The EDX spectra confirmed the presence of all the constituents in expected elemental percentage. From 57Fe Mössbauer spectroscopy data, the variation in line width, isomer shift, quadrupole splitting and hyperfine magnetic field values on Bi and La substitutions have been determined. Cation distribution in the presently investigated hexaferrite system was estimated using the relative area of Mössbauer spectroscopy.

Keywords: hexaferrite, mössbauer, cation distribution, solid state synthesis

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Authors: Essebti Dhahri

Abstract:

We present a new refrigerant La₀.₇Ca₀.₁₅Sr₀.₁₅Mn₁₋ₓGaₓO₃ (x = 0.0-0.1) manganites. These compounds were prepared by the sol-gel method. The refinement of the X-ray diffraction reveals that all samples crystallize in a rhombohedral structure (space group R3 ̅c). Detailed measurements of the magnetization as a function of temperature and magnetic applied field M (µ₀H, T) were carried out. From the M(µ₀H, T) curves, we have calculated the magnetic entropy change (ΔSM) according to the Maxwell relation. The temperature dependence of the magnetization M(T) reveals a decrease of M when increasing the x content. The magnetic entropy change (ΔSM) reaches a maximum value near room temperature. It was also found that this compound exhibits a large magnetocaloric effect MCE which increases when decreasing Ga concentration. So, the studied compounds could be considered potential materials for magnetic refrigeration application.

Keywords: magnetic measurements, Rietveld refinement, magnetic refrigeration, magnetocaloric effect

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Authors: A. Selmi, A. Bettaibi, H. Rahmouni, R. M’nassri, N. Chniba Boudjada, A. Chiekhrouhou, K. Khirouni

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Investigation of magnetic and magnetocaloric properties of Pr₀.₇Ca₀.₃Mn₀.₉M₀.₁O₃ perovskite manganites (M=Cr and Ni) has been carried out. Our compounds were prepared by the conventional solid-state reaction method at high temperatures. Rietveld refinement of X-ray diffraction pattern using FULLPROF method shows that all compounds adopt the orthorhombic structure with Pnma space group. The partial substitution of Mn-site drives the system from charge order state to ferromagnetic one with a Curie temperature T𝒸=150K, 118k and 116K for M=Cr and Ni, respectively. Magnetization measurements versus temperature in a magnetic applied field of 0.05T show that all our samples exhibit a paramagnetic–ferromagnetic transition with decreasing temperature. From M(H) isotherms, we have deduced the magnetic entropy change, which present maximum values of 2.37 J/kg.K and 2.94 J/kg.K, in a magnetic field change of 5T for M=Cr and Ni, respectively.

Keywords: manganites, magnetocaloric, magnetic, refrigeration

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Authors: Anastasiia Maklakova

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The perovskite type oxides formed in the Ln-Me-Me/-O systems (where Ln – rare-earth, Me – alkaline earth metal, Me/ - 3-d metal) have potential applications as gas sensors, catalysts or cathode materials for IT-SOFCs due to the high values of mixed electronic -ionic conductivity and high oxygen diffusivity. Complex oxides in the Sr-(Pr,Gd)-Co-O systems were prepared via the glycerol-nitrate technique The phase composition was determined using a Shimadzu XRD-7000 diffractometer at room temperature in air. Phase identification was performed using the ICDD database. The structure was refined by the full-profile Rietveld method using Fullprof 2008 software. Gradual substitution of strontium by Pr or Gd leads to the decrease of unit cell parameters and unit cell volume that can be explained by the size factor. An introduction of Pr or Gd into the strontium cobaltite increases the oxygen content in samples.

Keywords: phase equilibria, crystal structure, oxygen nonstoichiometry, solid oxide fuel cell

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Authors: Bhairi Lakshminarayana, Surajit Sarker, Ch. Subrahmanyam

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The present study reports the development of noble metal free nano catalysts for low-temperature CO oxidation and water gas shift reaction. Mn-substituted CeO2 solid solution catalysts were synthesized by co-precipitation, combustion and hydrothermal methods. The formation of solid solution was confirmed by XRD with Rietveld refinement and the percentage of carbon and nitrogen doping was ensured by CHNS analyzer. Raman spectroscopic confirmed the oxygen vacancies. The surface area, pore volume and pore size distribution confirmed by N2 physisorption analysis, whereas, UV-visible diffuse reflectance spectroscopy and XPS data confirmed the oxidation state of the Mn ion. The particle size and morphology (spherical shape) of the material was confirmed using FESEM and HRTEM analysis. Ce0.8Mn0.2O2-δ was calcined at 400 °C, 600 °C and 800 °C. Raman spectroscopy confirmed that the catalyst calcined at 400 °C has the best redox properties. The activity of the designed catalysts for CO oxidation (0.2 vol%), carried out with GHSV of 21,000 h-1 and it has been observed that co-precipitation favored the best active catalyst towards CO oxidation and water gas shift reaction, due to the high surface area, improved reducibility, oxygen mobility and highest quantity of surface oxygen species. The activation energy of low temperature CO oxidation on Ce0.8Mn0.2O2- δ (combustion) was 5.5 kcal.K-1.mole-1. The designed catalysts were tested for water gas shift reaction. The present study demonstrates that Mn ion substituted ceria at 400 °C calcination temperature prepared by co-precipitation method promise to revive a green sustainable energy production approach.

Keywords: Ce0.8Mn0.2O2-ð, CO oxidation, physicochemical characterization, water gas shift reaction (WGS)

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Authors: Wassima El Mofid, Svetlozar Ivanov, Andreas Bund

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The increasing requirements for high power and energy lithium ion batteries have led to the development of several classes of positive electrode materials. Among those one promising material is LiNixMnyCo1−x−yO2 due to its high reversible capacity and remarkable cycling performance. Further structural stabilization and improved electrochemical performance of this class of cathode materials can be achieved by cationic substitution to a transition metal such as Al, Mg, Cr, etc. The current study discusses a novel NMC type material obtained by simultaneous cationic substitution of the cobalt which is a toxic element, with aluminum and iron. A compound with the composition LiNi0.6Mn0.2Co0.15Al0.025Fe0.025O2 (NMCAF) was synthesized by the self-combustion method using sucrose as fuel. The material has a layered α-NaFeO2 type structure with a good hexagonal ordering. Rietveld refinement analysis of the XRD patterns revealed a very low cationic mixing compared to the non-substituted material LiNi0.6Mn0,2Co0.2O2 suggesting a structural stabilization. Galvanostatic cycling measurements indicate improved electrochemical performance after the metal substitution. An initial discharge capacity of about 190 mAh.g−1 at slow rate (C/20), and a good cycling stability even at moderately faster rates (C/5 and C) have been observed. The long term cycling displayed a capacity retention of about 90% after 10 cycles.

Keywords: cationic substitution, lithium ion batteries, positive electrode material, self-combustion synthesis method

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Authors: Bastola Narayan, Rajeev Ranjan

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The morphotropic phase boundary (MPB) in the magnetoelectric (1-x)BiFeO3-(x)PbTiO3 has remained a matter of controversy ever since its discovery in 1964. The nature of the phase stabilized (single phase tetragonal or coexistence of tetragonal and rhombohedral phases) is very sensitive to the slight changes in the synthesis conditions. It thus remained an enigma as to what is the essential physical factor which is controlled by the slight difference in the synthesis conditions that finally determines, whether the phase formed will be single phase or coexistence of phases. In this paper, we demonstrate that the nature of the phase stabilized in this system is uniquely dependent on the crystallite size. The system is shown to exhibit features of abnormal grain growth (AGG) during sintering with abrupt increase in the grain size from ~ 1 micron to ~ 10 microns. The 10 micron grains exhibit pure tetragonal phase while the 1 micron grains exhibit coexistence of rhombohedral and tetragonal ferroelectric phases. The Rietveld analysis of powder neutron diffraction shows a paramagnetic to antiferromagnetic order transition inducing with crystalline size reduction from 10 micron to 1 micron. Since tetragonal phase is known to have paramagnetic order and rhombohedral phase has antiferromagnetic order in room temperature, this further strengthens our argument of size induced structure transition.

Keywords: size driven MPB, size driven magnetic ordering, abnormal grain growth, phase formation in BF-PT system

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Authors: S. Khardazi, H. Zaitouni, A. Neqali, S. Lyubchyk, D. Mezzane, M. Amjoud, E. Choukri, S. Lyubchyk, Z. Kutnjak

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In the present paper, structural, dielectric, ferroelectric, and energy storage properties of pure perovskite lead-free BCZT, BTSn, and BTSn-BCZT ferroelectric ceramics have been investigated. Rietveld refinement of XRD data confirms the coexistence of the rhombohedral and orthorhombic phases at room temperature in the composite BCZT–BTSn ceramic. Remarkably, an improved recoverable energy density of 137.86 mJ/cm³ and a high energy storage efficiency of 86.19 % at 80°C under a moderate applied electric field of 30 kV/cm were achieved in the designed BCZT–BTSn ceramic. Besides, the sample exhibits excellent thermal stability of the energy storage efficiency (less than 3%) in the temperature range of 70 to 130 °C under 30 kV/cm. Such results make the pb-free BCZT–BTSn ferroelectric ceramic a very promising potential matrix for energy storage capacitor applications.

Keywords: sol-gel, ferroelectrics, lead-free, perovskites, energy storage

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Authors: Lamia L. G. Al-Mahamad, Benjamin R. Horrocks, Andrew Houlton

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Hydrogels based on metal coordination polymers of nucleosides and a range of metal ions (Au, Ag, Cu) have been prepared and characterized by atomic force microscopy (AFM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, ultraviolet-visible absorption spectroscopy, and powder X-ray diffraction. AFM images of the xerogels revealed the formation of extremely long polymer molecules (> 10 micrometers, the maximum scan range). This result is also consistent with TEM images which show a fibrous morphology. Oxidative doping of the Au-nucleoside fibres produces an electrically conductive nanowire. No sharp Bragg peaks were found at the at the X-ray diffraction pattern for metal ions hydrogels indicating that the samples were amorphous, but instead the data showed broad peaks in the range 20 < Q < 40 and correspond to distances d=2μ/Q. The data was analysed using a simplified Rietveld method by fitting a regression model to obtain the distance between atoms.

Keywords: hydrogel, metal ions, nanowire, nucleoside

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Authors: Sidi Mohamed Mesli, Mohamed Habchi, Mohamed Kotbi, Rafik Benallal, Abdelali Derouiche

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Fluoride glasses with a nominal composition of BaMnMF7 (M = FeV assuming isomorphous replacement) have been structurally modelled through the simultaneous simulation of their neutron diffraction patterns by a reverse Monte Carlo (RMC) model and by a Rietveld for disordered materials (RDM) method. Model is consistent with an expected network of interconnected [MF6] polyhedra. The RMC results are accompanied by artificial satellite peaks. To remedy this problem, we use an extension of the RMC algorithm, which introduces an energy penalty term in acceptance criteria. This method is called the Hybrid Reverse Monte Carlo (HRMC) method. The idea of this paper is to apply the (HRMC) method to the title glasses, in order to make a study of the phenomenon nature of order and disorder by displaying and discussing the partial pair distribution functions (PDFs) g(r). We suggest that this method can be used to describe average correlations between components of fluoride glass or similar system.

Keywords: fluoride glasses, RMC simulation, neutron scattering, hybrid RMC simulation, Lennard-Jones potential, partial pair distribution functions

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Authors: Prajna Paramita Mohapatra, Pamu Dobbidi

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Lithium ferrite (LiFe5O8) has potential applications as a component of microwave magnetic devices such as circulators and monolithic integrated circuits. For efficient device applications, spinel ferrites in the form of thin films are highly required. It is necessary to improve their magnetic and dielectric behavior by optimizing the processing parameters during deposition. The lithium ferrite thin films are deposited on Pt/Si substrate using the pulsed laser deposition technique (PLD). As controlling the film thickness is the easiest parameter to tailor the strain, we deposited the thin films having different film thicknesses (160 nm, 200 nm, 240 nm) at oxygen partial pressure of 0.001 mbar. The formation of single phase with spinel structure (space group - P4132) is confirmed by the XRD pattern and the Rietveld analysis. The optical bandgap is decreased with the increase in thickness. FESEM confirmed the formation of uniform grains having well separated grain boundaries. Further, the film growth and the roughness are analyzed by AFM. The root-mean-square (RMS) surface roughness is decreased from 13.52 nm (160 nm) to 9.34 nm (240 nm). The room temperature magnetization is measured with a maximum field of 10 kOe. The saturation magnetization is enhanced monotonically with an increase in thickness. The magnetic resonance linewidth is obtained in the range of 450 – 780 Oe. The dielectric response is measured in the frequency range of 104 – 106 Hz and in the temperature range of 303 – 473 K. With an increase in frequency, the dielectric constant and the loss tangent of all the samples decreased continuously, which is a typical behavior of conventional dielectric material. The real part of the dielectric constant and the dielectric loss is increased with an increase in thickness. The contribution of grain and grain boundaries is also analyzed by employing the equivalent circuit model. The highest dielectric constant is obtained for the film having a thickness of 240 nm at 104 Hz. The obtained results demonstrate that desired response can be obtained by tailoring the film thickness for the microwave magnetic devices.

Keywords: PLD, optical response, thin films, magnetic response, dielectric response

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Authors: Omneya Messallam, Sara S. Fouad

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The Modernist Movement initially flourished in France, Holland, Germany and the Soviet Union. Many architects and designers were inspired and followed its principles. Two of its most important architects (Gerrit Rietveld and Ludwig Mies van de Rohe) were introduced in this paper. Each did not follow the other’s principles and had their own particular rules; however, they shared the same features of the Modernist International Style, such as Anti-historicism, Abstraction, Technology, Function and Internationalism/ Universality. Key Modernist principles translated into high expectations, which sometimes did not meet the inhabitants’ aspirations of living comfortably; consequently, leading to a conflict and misunderstanding between the designer and their clients’ needs. Therefore, historical case studies (the Schroder and the Farnsworth houses) involving two Modernist pioneer architects have been chosen. This paper is an attempt to explore some of the influential factors affecting buildings design such as: needs, gender, and question concerning commonalities between both designers and their clients. The three aspects and two designers explored here have been chosen because they have been influenced the researchers to understand the impact of those factors on the design process, building’s performance, and the dweller’s satisfaction. This is a descriptive/ analytical research based on two historical comparative case studies that involve several steps such as: key evaluation questions (KEQs), observations, document analysis, etc. The methodology is based on data collation and finding validations. The research aims to state a manifest to regulate the relation between architects and their clients to reach the optimum building performance and functional interior design that suits their clients’ needs, reflects the architects’ character, and the school they belong to. At the end, through the investigation in this paper, the different needs between both the designers and the clients have been seen not only in the building itself but also it could convert the inhabitant’s life in various ways. Moreover, a successful relationship between the architect and their clients could play a significant role in the success of projects. In contrast, not every good design or celebrated building could end up with a successful relationship between the designer and their client or full-fill the inhabitant’s aspirations.

Keywords: architect’s character, building’s performance, commonalities, client’s character, gender, modernist movement, needs

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Authors: J. Plocek, P. Holec, S. Kubickova, B. Pacakova, I. Matulkova, A. Mantlikova, I. Němec, D. Niznansky, J. Vejpravova

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This article presents summary on preparation and characterization of zinc, copper, cadmium and cobalt chromite nano crystals, embedded in an amorphous silica matrix. The ZnCr2O4/SiO2, CuCr2O4/SiO2, CdCr2O4/SiO2 and CoCr2O4/SiO2 nano composites were prepared by a conventional sol-gel method under acid catalysis. Final heat treatment of the samples was carried out at temperatures in the range of 900–1200 °C to adjust the phase composition and the crystallite size, respectively. The resulting samples were characterized by Powder X-ray diffraction (PXRD), High Resolution Transmission Electron Microscopy (HRTEM), Raman/FTIR spectroscopy and magnetic measurements. Formation of the spinel phase was confirmed in all samples. The average size of the nano crystals was determined from the PXRD data and by direct particle size observation on HRTEM; both results were correlated. The mean particle size (reviewed by HRTEM) was in the range from ~ 4 to 46 nm. The results showed that the sol-gel method can be effectively used for preparation of the spinel chromite nano particles embedded in the silica matrix and the particle size is driven by the type of the cation A2+ in the spinel structure and the temperature of the final heat treatment. Magnetic properties of the nano crystals were found to be just moderately modified in comparison to the bulk phases.

Keywords: sol-gel method, nanocomposites, Rietveld refinement, Raman spectroscopy, Fourier transform infrared spectroscopy, magnetic properties, spinel, chromite

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Authors: P. Suchismita Behera, V. G. Sathe, A. K. Nigam, P. A. Bhobe

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Co-existence of long-range ferromagnetism and semi-conductivity with correlated behavior of structural, magnetic, optical and electrical properties in various sites doping at CdCr2Se4 makes it a most promising candidate for spin-based electronic applications and magnetic devices. It orders ferromagnetically below TC = 130 K with a direct band gap of ~ 1.5 eV. The magnetic ordering is believed to result from strong competition between the direct antiferromagnetic Cr-Cr spin couplings and the ferromagnetic Cr-Se-Cr exchange interactions. With an aim of understanding the influence of crystal structure on its magnetic properties without disturbing the magnetic site, we investigated four compositions with 3%, 5%, 7% and 10% of Sn-substitution at Cd-site. Partial substitution of Cd2+ (0.78Å) by small sized nonmagnetic ion, Sn4+ (0.55Å), is expected to bring about local lattice distortion as well as a change in electronic charge distribution. The structural disorder would affect the Cd/Sn – Se bonds thus affecting the Cr-Cr and Cr-Se-Cr bonds. Whereas, the charge imbalance created due to Sn4+ substitution at Cd2+ leads to the possibility of Cr mixed valence state. Our investigation of the local crystal structure using the EXAFS, Raman spectroscopy and magnetic properties using SQUID magnetometry of the Cd1-xSnxCr2Se4 series reflects this premise. All compositions maintain the Fd3m cubic symmetry with tetrahedral distribution of Sn at Cd-site, as confirmed by XRD analysis. Lattice parameters were determined from the Rietveld refinement technique of the XRD data and further confirmed from the EXAFS spectra recorded at Cr K-edge. Presence of five Raman-active phonon vibrational modes viz. (T2g (1), T2g (2), T2g (3), Eg, A1g) in the Raman spectra further confirms the crystal symmetry. Temperature dependence of the Raman data provides interesting insight to the spin– phonon coupling, known to dominate the magneto-capacitive properties in the parent compound. Below the magnetic ordering temperature, the longitudinal damping of Eg mode associated with Se-Cd/Sn-Se bending and T2g (2) mode associated to Cr-Se-Cr interaction, show interesting deviations with respect to increase in Sn substitution. Besides providing the estimate of TC, the magnetic measurements recorded as a function of field provide the values of total magnetic moment for all the studied compositions indicative of formation of multiple Cr valences.

Keywords: exchange interactions, EXAFS, ferromagnetism, Raman spectroscopy, spinel chalcogenides

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Authors: S. Alina Wang

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A Gibsonian approach is used to understand the existential dimensions of the human ecological niche. Then, this existential-Gibsonian framework is applied to rethinking Hacking’s historical analysis of multiple personality disorder. This research culminates in a generalized account of psychiatric illness from an enactivist lens. In conclusion, reflections on the implications of this account on approaches to psychiatric treatment are mentioned. J.J. Gibson’s theory of affordances centered on affordances of sensorimotor varieties, which guide basic behaviors relative to organisms’ vital needs and physiological capacities (1979). Later theorists, notably Neisser (1988) and Rietveld (2014), expanded on the theory of affordances to account for uniquely human activities relative to the emotional, intersubjective, cultural, and narrative aspects of the human ecological niche. This research shows that these affordances are structured by what Haugeland (1998) calls existential commitments, which draws on Heidegger’s notion of dasein (1927) and Merleau-Ponty’s account of existential freedom (1945). These commitments organize the existential affordances that fill an individual’s environment and guide their thoughts, emotions, and behaviors. This system of a priori existential commitments and a posteriori affordances is called existential enactivism. For humans, affordances do not only elicit motor responses and appear as objects with instrumental significance. Affordances also, and possibly primarily, determine so-called affective and cognitive activities and structure the wide range of kinds (e.g., instrumental, aesthetic, ethical) of significances of objects found in the world. Then existential enactivism is applied to understanding the psychiatric phenomenon of multiple personality disorder (precursor of the current diagnosis of dissociative identity disorder). A reinterpretation of Hacking’s (1998) insights into the history of this particular disorder and his generalizations on the constructed nature of most psychiatric illness is taken on. Enactivist approaches sensitive to existential phenomenology can provide a deeper understanding of these matters. Conceptualizing psychiatric illness as strictly a disorder in the head (whether parsed as a disorder of brain chemicals or meaning-making capacities encoded in psychological modules) is incomplete. Rather, psychiatric illness must also be understood as a disorder in the world, or in the interconnected networks of existential affordances that regulate one’s emotional, intersubjective, and narrative capacities. All of this suggests that an adequate account of psychiatric illness must involve (1) the affordances that are the sources of existential hindrance, (2) the existential commitments structuring these affordances, and (3) the conditions of these existential commitments. Approaches to treatment of psychiatric illness would be more effective by centering on the interruption of normalized behaviors corresponding to affordances targeted as sources of hindrance, the development of new existential commitments, and the practice of new behaviors that erect affordances relative to these reformed commitments.

Keywords: affordance, enaction, phenomenology, psychiatry, psychopathology

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Authors: Aurore Lechevallier, Mohend Chaouche, Jerome Soudier, Guillaume Renaudin

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The cement industry accounts for 8% of the global CO₂ emissions, and approximately 60% of these emissions are associated with the Portland cement clinker production from the decarbonization of limestone (CaCO3). Their impact on the greenhouse effect results in growing social awareness. Therefore, CO2 footprint becomes a product selection choice, and substituting Portland cement with a lower CO2-footprint alternative binder is sought. In this context, new hydraulic binders have been studied as a potential Ordinary Portland Cement substitute. Many of them are composed of iron oxides and aluminum oxides, present in the Ca₄Al₂-xFe₂+ₓO₁₀-like phase and forming Ca-LDH (i.e. AFM) as a hydration product. It has become essential to study the possible existence of Fe/Al AFM solid solutions to characterize the hydration process properly. Ca₂Al₂-xFex(OH)₆.X.nH₂O layered AFM samples intercalated with either nitrate or chloride X anions were synthesized based on the co-precipitation method under a nitrogen atmosphere to avoid the carbonation effect.AFM samples intercalated with carbonate anions were synthesized based on the anionic exchange process, using AFM-NO₃ as the source material. These three AFM samples were synthesized with varying Fe/Al molar ratios. The experimental conditions were optimized to make possible the formation of Al-AFM and Fe-AFM using the same parameters (namely pH value and salt concentration). Rietveld refinements were performed to demonstrate the existence of a solid solution between the two trivalent metallic end members. Spectroscopic analyses were used to confirm the intercalation of the targeted anion; secondary electron images were taken to analyze the AFM samples’ morphology, and energy dispersive X-ray spectroscopy (EDX) was carried out to determine the elemental composition of the AFM samples. Results of this study make it possible to quantify the Al/Fe ratio of the AFM phases precipitated in our hydraulic binder, thanks to the determined Vegard's law characteristic to the corresponding solid solutions

Keywords: AFm phase, iron-rich binder, low-carbon cement, solid solution

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Authors: Dimitra Das, Anuradha Mitra, Kalyan Kumar Chattopadhyay

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Organic polymers, constructed from light elements like carbon, hydrogen, nitrogen, oxygen, sulphur, and boron atoms, are the emergent class of non-toxic, metal-free, environmental benign advanced materials. Covalent triazine-based polymers with a functional triazine group are significant class of organic materials due to their remarkable stability arising out of strong covalent bonds. They can conventionally form hydrogen bonds, favour π–π contacts, and they were recently revealed to be involved in interesting anion–π interactions. The present work mainly focuses upon the development of a single-crystalline, highly cross-linked triazine-based nitrogen-rich organic polymer with nanodendritic morphology and significant thermal stability. The polymer has been synthesized through hydrothermal treatment of melamine and ethylene glycol resulting in cross-polymerization via condensation-polymerization reaction. The crystal structure of the polymer has been evaluated by employing Rietveld whole profile fitting method. The polymer has been found to be composed of monoclinic melamine having space group P21/a. A detailed insight into the chemical structure of the as synthesized polymer has been elucidated by Fourier Transform Infrared Spectroscopy (FTIR) and Raman spectroscopic analysis. X-Ray Photoelectron Spectroscopic (XPS) analysis has also been carried out for further understanding of the different types of linkages required to create the backbone of the polymer. The unique rod-like morphology of the triazine based polymer has been revealed from the images obtained from Field Emission Scanning Electron Microscopy (FESEM) and Transmission Electron Microscopy (TEM). Interestingly, this polymer has been found to selectively detect mercury (Hg²⁺) ions at an extremely low concentration through fluorescent quenching with detection limit as low as 0.03 ppb. The high toxicity of mercury ions (Hg²⁺) arise from its strong affinity towards the sulphur atoms of biological building blocks. Even a trace quantity of this metal is dangerous for human health. Furthermore, owing to its small ionic radius and high solvation energy, Hg²⁺ ions remain encapsulated by water molecules making its detection a challenging task. There are some existing reports on fluorescent-based heavy metal ion sensors using covalent organic frameworks (COFs) but reports on mercury sensing using triazine based polymers are rather undeveloped. Thus, the importance of ultra-trace detection of Hg²⁺ ions with high level of selectivity and sensitivity has contemporary significance. A plausible sensing phenomenon by the polymer has been proposed to understand the applicability of the material as a potential sensor. The impressive sensitivity of the polymer sample towards Hg²⁺ is the very first report in the field of highly crystalline triazine based polymers (without the introduction of any sulphur groups or functionalization) towards mercury ion detection through photoluminescence quenching technique. This crystalline metal-free organic polymer being cheap, non-toxic and scalable has current relevance and could be a promising candidate for Hg²⁺ ion sensing at commercial level.

Keywords: fluorescence quenching , mercury ion sensing, single-crystalline, triazine-based polymer

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Authors: Anna S. Tolkacheva, Sergey N. Shkerin, Kirill G. Zemlyanoi, Olga G. Reznitskikh, Pavel D. Khavlyuk

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Calcium oxovanadates with garnet related structure are multifunctional oxides in various fields like photoluminescence, microwave dielectrics, and magneto-dielectrics. For example, vanadate garnets are self-luminescent compounds. They attract attention as RE-free broadband excitation and emission phosphors and are candidate materials for UV-based white light-emitting diodes (WLEDs). Ca₅M₄(VO₄)₆ (M = Mg, Zn, Co, Ni, Mn) compounds are also considered promising for application in microwave devices as substrate materials. However, the relation between their structure, composition and physical/chemical properties remains unclear. Given the above-listed observations, goals of this study are to synthesise Ca₅M₄(VO₄)₆ (M = Mg, Zn, Ni) and to study their thermal and electrical properties. Solid solutions Ca₅Mg₄₋ₓMₓ(VO₄)₆ (0 ≤ x ≤ 4) where M is Zn and Ni have been synthesized by sol-gel method. The single-phase character of the final products was checked by powder X-ray diffraction on a Rigaku D/MAX-2200 X-ray diffractometer using Cu Kα radiation in the 2θ range from 15° to 70°. The dependence of thermal properties on chemical composition of solid solutions was studied using simultaneous thermal analyses (DSC and TG). Thermal analyses were conducted in a Netzch simultaneous analyser STA 449C Jupiter, in Ar atmosphere, in temperature range from 25 to 1100°C heat rate was 10 K·min⁻¹. Coefficients of thermal expansion (CTE) were obtained by dilatometry measurements in air up to 800°C using a Netzsch 402PC dilatometer; heat rate was 1 K·min⁻¹. Impedance spectra were obtained via the two-probe technique with an impedance meter Parstat 2273 in air up to 700°C with the variation of pH₂O from 0.04 to 3.35 kPa. Cation deficiency in Ca and Mg sublattice under the substitution of MgO with ZnO up to 1/6 was observed using Rietveld refinement of the crystal structure. Melting point was found to decrease with x changing from 0 to 4 in Ca₅Mg₄₋ₓMₓ(VO₄)₆ where M is Zn and Ni. It was observed that electrical conductivity does not depend on air humidity. The reported study was funded by the RFBR Grant No. 17–03–01280. Sample attestation was carried out in the Shared Access Centers at the IHTE UB RAS.

Keywords: garnet structure, electrical conductivity, thermal expansion, thermal properties

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Authors: Chidiebere C. Agoha, Armstong C. Awuzie, Chukwuebuka N. Onwubuariri, Joy O. Njoku

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Spatial analysis is a field of study that utilizes geographic or spatial information to understand and analyze patterns, relationships, and trends in data. It is characterized by the use of geographic or spatial information, which allows for the analysis of data in the context of its location and surroundings. It is different from non-spatial or aspatial techniques, which do not consider the geographic context and may not provide as complete of an understanding of the data. Spatial analysis is applied in a variety of fields, which includes urban planning, environmental science, geosciences, epidemiology, marketing, to gain insights and make decisions about complex spatial problems. This review paper explores definitions of spatial analysis from various sources, including examples of its application and different analysis techniques such as Buffer analysis, interpolation, and Kernel density analysis (multi-distance spatial cluster analysis). It also contrasts spatial analysis with non-spatial analysis.

Keywords: aspatial technique, buffer analysis, epidemiology, interpolation

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