Williamson-Hall Method Research Articles

Structural, vibrational and optical characterisations of Li2Ba3(P2O7)2:Cr3+ by solid-state reaction method

ABSTRACT Cr3+ doped Li2Ba3(P2O7)2 pyrophosphate nanopowder was successfully synthesised by solid-state reaction technique. The nanopowder was characterised by several techniques. X-ray diffraction analysis reveals orthorhombic crystal structureand average crystallite size values 34.21 and 28.41 nm are determined by Debye Scherrer’s formula and Williamson-Hall (W-H) method. The morphology displayed both SEM and HR-TEM images are irregular stone-like shapes. EDS analysis confirms the constituted elements. The SAED patterns of HR-TEM with well matched with XRD data. FT-IR and Raman spectra analysis confirmed incorporation of Cr3+ in the Li2Ba3(P2O7)2 pyrophosphate nanopowder. The EPR spectrum exhibited signal at g = 1.968 which is attributed to interaction between Cr3+ and Cr3+ exchange pair. The site symmetry of Cr3+ ions occupy a distorted octahedral. Photoluminescence spectrum exhibited bands correspond to ultraviolet, blue and green regions. The evaluated CCT of 6517 K indicates yellowish-green emission near cold light which reveals that the present prepared sample is useful for LEDs applications.

Evaluation of structural parameters of monoclinic nanocrystalline CuO and study of sunlight-driven photocatalytic dye degradation, antimicrobial and antioxidant potential

Highly pure, crystalline and spherical-shaped Copper oxide nanoparticles (NPs) have been synthesized via facile chemical coprecipitation. Various models including the Scherrer, Monshi-Scherrer, Williamson-Hall, Size-Strain Plot and Halder-Wagner method have been applied to study the crystal structure characteristics. The lattice parameters associated with the monoclinic crystal lattice of CuO NPs were estimated to be a = 4.69 Å, b = 3.41 Å, c = 5.14 Å and β = 99.87(degree), unit cell volume V = 81.35Å3 and cell density dx = 6.49 g/cm3. The photocatalytic dye degradation proficiency at 20 mg/l CuO concentration and 120 min sunlight exposure results the order of percentage dye degradation Malachite Green (88.4%) > Crystal Violet (70.8%) > Eosin Yellow (70.2%) > Methylene Blue (54.08%) dyes. The antimicrobial activity assessment was done against the broad-spectrum pathogenic microbes unveiled the exceptional microbial controlling capability of CuO NPs. Furthermore, the antioxidant activity test demonstrated the potential free radical scavenging activity of CuO NPs with an IC50 value of 47.733 µg/ml. Highlights Synthesis of pure and spherical shaped nanocrystalline CuO was done by using low cost and facile chemical coprecipitation method. XRD, FTIR, FESEM, EDX, UV-Vis, and Raman spectroscopic techniques were used for characterization purpose. The structural and crystallographic parameters of monoclinic crystal structure of CuO NPs were evaluated successfully. The photocatalytic performance of CuO NPs follow the percentage dye degradation order as MG (88.4%) > CV (70.8%) > EY (70.20%) > MB (54.08%) after 120 minutes of sunlight exposure. CuO NPs exhibit promising antifungal activity against COVID-19 associated Pulmonary Aspergillosis (CAPA) causing pathogenic fung. CuO NPs show potential DPPH free radical scavenging activity with an IC50 value of 47.733 µg/ml.

Planning Mechanical Behavior of A356 Alloy Wheels by Using Distinct Heat Treatments

The aim of this investigation concerns evaluating the mechanical strength and microhardness values of A356 alloy samples in distinctive heat treatments, including those commonly applied to automotive wheels. It is recognized that A356 and Al-Si-based alloys exhibit considerable versatility across numerous industrial applications. The mechanical behavior obtained is intimately associated with different operational parameters (e.g., cooling rates, solution treatment, quenching, and artificial aging). In this study, a group of samples are quenched at 30, 60 and 80 °C. Another set is quenched and subsequently aged at three different temperatures, i.e., 180, 200, and 220 °C for 5 h, and mechanical responses are compared. Microstructural characterization, X-ray diffraction (XRD) analysis, tensile testing, and microhardness measurements are carried out. Using the Rietveld data and based on the modified Williamson–Hall method, the microstrains, crystallite size, and dislocation densities are calculated. Based on this, the resulting mechanical strengths from distinctive quenching and aging are understood. It was found that there exists a “quasi-optimal range” of operational parameters involving different A356 alloy treatments, which vary depending on the manufacturing route. Considering A356 alloy wheels, the planning of the powder coat treatment before or after T6 treating provides better mechanical properties and ductility.

X-ray Diffraction Line Profile Analysis of Natural Calcite Minerals found in Southern Philippines by Williamson-Hall Method

This study employs the Williamson–Hall (W–H) models to examine the microstrains and crystallite sizes of CaCO3 occurring as calcite in limestone samples found in General Santos City and Sarangani Province, Southern Philippines. Using both the Uniform Deformation Model (UDM) and Uniform Stress Deformation (USDM) models, computations for average sizes were established to be identical, implying minimal strain influence. The consistency of resulting measurements extends to the microstrain, revealing uniform results for all samples. Correlation between crystallite sizes and microstrains in the calcite crystals was observed, where high-purity calcites exhibited larger crystallite sizes and microstrains. The crystallite sizes decrease with microstrains for calcites with higher Mg concentration, a finding that can be attributed to lattice distortion and the formation of defects. The release of stress forms these defects, thereby resulting in a reduction of microstrains. Moreover, the distinctly variable responses to strain exhibited by the samples could be influenced by either their anisotropic properties or other additional components. The W–H models, used jointly with UDM and USDM consistently predicted crystallite sizes, and thus offer valuable insights into the uniform stress responses of calcites. These promising results notwithstanding, USDM is shown to be especially relevant for anisotropic samples owing to the display deviations of crystallite sizes, a key feature of anisotropic natural calcites. The microscopic analysis is expected to provide additional understanding regarding the state of the limestone samples.

Silver-impregnated vanadium pentoxide nanofillers for reinforcement in titanium-based missile surfaces

An optimal content of silver doped vanadium pentoxide nanofillers (Ag-V2O5 NFs) was envisaged for reinforcement in Ti-based surfaces for boosting up the operational performance of high-supersonic and hypersonic missiles. Bar-shaped Ag-V2O5 NFs developed at 1, 3, and 5 % doping contents synthesized via microwave-assisted chemical solution technique were investigated for morphological, crystallographic, structural, and compositional properties by employing FESEM, XRD, Raman, and FTIR spectroscopy. Owing to their solubility differences, a blend of orthorhombic α- and β-phases were identified as spectral fingerprints specific to the developed Ag-embedded vanadium oxide crystalline structures. The Williamson-Hall method estimated the average crystallite size of α-Ag3-VO4 and β-Ag0.35-V2O5 phase NFs as 31.4 and 29.9 nm, respectively. The best results of the developed Ag-V2O5 NFs for the surface material transpired for the monoclinic metastable β-Ag0.333-V2O5 phase at optimal 3 % doping content with 13.7 nm average crystallite size, 0.35 % lattice strain, and 4.113 g/cm3 mass density.

A new spinel compound, Ba0.25Sr0.25Fe2.5O4, developed for use in gas sensing applications

In this article, nanoscale materials of the spinel type Ba0.25Sr0.25Fe2.5O4 have been successfully prepared using the solvothermal method, with sodium acetate as a protective agent and polyvinylpyrrolidone (PVP) to control the size and shape of the particles. The structural, morphological, and gas sensing characteristics of the sample have been thoroughly examined. It has been confirmed that the compound Ba0.25Sr0.25Fe2.5O4 exhibits a crystallite size of 32 nm, a fully cubic structure, and significant porosity, as established by the Williamson–Hall method. The electrical properties have revealed the semiconductor-type (n) behavior of our compound. The results of the ethanol, acetone, and H2S detection tests highlighted a particularly pronounced sensitivity of Ba0.25Sr0.25Fe2.5O4.Gas detection tests were conducted on the prepared compound by varying the concentrations of ethanol, acetone, and H2S gases (500 ppb, 1 ppm, 5 ppm, 10 ppm, 20 ppm, 40 ppm, 80 ppm, 100 ppm). The compound Ba0.25Sr0.25Fe2.5O4 demonstrated very good reactivity towards the three gases, even at very low concentrations, with respective optimal operating temperatures of 200 °C, 200 °C and 120 °C. Furthermore, the response and recovery time values for these three gases were found to be very short.

Study of the structure and properties of interstitial alloys TixMo1 – xCyNz

Developing the new materials with improved properties suggests study of the crystal structure and properties of multicomponent interstitial alloys. We present the results of studying the crystal structure and microhardness of TixMo1 – xCyNz interstitial alloys in massive samples with different ratios of concentrations of constituent elements. The samples obtained by self-propagating high-temperature synthesis were subjected to homogenizing annealing at 2600 K for 8 h and cooled together with the furnace. Data of neutron diffraction revealed that the alloys have a face-centered cubic crystal structure in which Ti and Mo atoms, as well as C and N, are intersubstituted and statistically located in the 4b positions and octahedral 4a positions, respectively. The Rietveld method was used to determine crystallite sizes, dislocation densities, and microstrain using X-ray diffraction patterns. The microhardness of the samples was determined by the Vickers method. It is shown that the crystallite sizes determined by the Williamson-Hall and Scherrer methods differ significantly, whereas the patterns of crystallite growth in size, as well as regularities of changes in the dislocation density and microstrains follow change in the concentration of the components in the composition. As the carbon content in the alloy increases, the crystallite sizes and microstrains decrease, and the dislocation density increases. It is revealed that the smaller the crystallite size and the higher the dislocation density, the more microhardness is displaced towards increasing the carbon content. With a change in the ratio of components in TixMo1 – xCyNz as the crystallite size and microstrains decrease and dislocation density increases, the microhardness of the alloy increases by 1.5 – 2 times compared to binary carbide and titanium nitride. The results obtained can be applied to the use of interstitial alloys in instrumental and high-temperature engineering.

Experimental and first-principle insight into Structural, optical and electrical properties and photocatalytic water purification application of Zn1-xMgxO

Environmental concern essentially demands solemn consideration of industrial waste-water containing organic dyes. To develop efficient photocatalysts for degradation of organic dyes in waste water, metal-oxide nanostructures are the promising candidate owing to their tunable physical properties. The present work emphasizes on the experimental and first-principle (DFT + U) studies to understand the impact of magnesium doping on the structural, optical and electrical properties, and photocatalytic degradation tendency of zinc oxide (ZnO) nano-ceramics. The ZnO lattice contraction endorsed by Mg-doping, has been examined mutually from the first principle calculations and Rietveld refinement investigations. The decrease in crystallite-size (93 to 88 nm) and enrichment in structural imperfections of Zn1-xMgxO nanostructures were analyzed with Williamson-Hall peak profile methods. The band gap broadening of ZnO with Mg doping was demonstrated by UV–visible spectroscopy (3.32 to 3.43 eV) which was further confirmed from DFT + U (3.39 to 3.55 eV) calculations. The increase in dielectric constant and reduction in ac conductivity has been observed due to Mg addition. The photocatalytic performance of Zn1-xMgxO nanostructures was evaluated under sunlight for Methylene-blue (MB) and Congo-red (CR) dyes. The performance has been optimally improved with 6 mol% Mg content leading to degradation of 86.2 % and 58.3 % of MB and CR dyes respectively in 160 min.

A comparative study in estimating of crystallite sizes of synthesized and natural hydroxyapatites using Scherrer Method, Williamson-Hall model, Size-Strain Plot and Halder-Wagner Method

In this study, an approach was made to create hydroxyapatite (HAp) crystals on nanoscale ranges from CaCO3 and H3PO4 utilizing a wet chemical process. Both fish and cow bones were used effectively for making bone powder as the natural sources of HAp. X-ray diffraction approach proved that powdered bone and HAp were in the crystalline phase. The determination of crystallite size in synthesized HAp crystals and bone powders was investigated using a range of techniques, including Linear Straight-Line Method (LSLM), Williamson-Hall Method (WHM), Size-Strain Plot (SSP), Halder-Wagner Method (HWM), and Sahadat-Scherrer Method (SSM). We also employed different Williamson-Hall models to quantify the stress and strain of the powdered materials for all diffraction peaks, including the Uniform Deformation Model (UDM), Uniform Stress Deformation Model (USDM), and Uniform Deformation Energy Density Model (UDEDM). Williamson-Hall is regarded as the best approach out of all of them since it was used to find the energy density, lattice stress, lattice strain, and crystallite size of the formed crystal. All the results from each model were compared to check the variation of analyzed data. The obtained results confirmed that there was an interrelation between the particle sizes of the Size Strain Plot and the Williamson-Hall method.

Microstructural, optical, and morphological investigations of SnO2 nanomaterials grown by microwave assisted sol gel method

Tin Oxide (SnO2) nanomaterials were grown using the microwave-assisted sol–gel method at different concentrations of tin precursor (namely 0.05, 0.1, 0.2, and 0.3 M). Stannous chloride is used as a Sn precursor. Liquid ammonia was used to maintain the pH in the range of 12–13. Synthesis was carried out in an aqueous medium using a Teflon container in a microwave oven for 1 hour. Precipitate was annealed in ambient air for 600oC. Structural, optical, and morphological investigations were done. XRD reveals the growth of the tetragonal phase of SnO2. The prominent presence of (110), (101), and (211) reflections was noticed at 26.6, 33.7, and 52 two-theta values. Tin oxide is transparent in the visible region of the electromagnetic spectrum. However, several attempts have been made to decrease the visible blindness of tin oxide. The band gap is a property of nanomaterials that can tailor their application in the optoelectronic field. Band gap and crystallite size show a prominent relationship in the nano-domain. Strain was not considered while calculating crystallite size using the Scherrer formula. In this investigation, we have measured the crystallite size and other structural features such as strain, stress, deformation energy, dislocation de\ sity, etc using the W-H plot method. All modified models of the W-H method have been utilized for this measurement. A comparative and comprehensive study of structural features was carried out using the Scherrer method, the Williamson–Hall method, and all its modified models. The crystallite size measured by the Scherrer method and various models of the W-H method shows a peak at 0.2 M concentration. Crystallite size plots of various modified W-H methods show similar trends, followed by the Scherrer plot. Strain calculated by Brag’s theory as well as all modified W-H depicts similar behaviour upon changing the concentration. Globular agglomerated morphology was revealed by scanning electron microscopy (SEM). The presence of tin (Sn) and oxygen (O) was confirmed by energy dispersive x-ray spectroscopy. The band gap was obtained using the Tauc theory, which portrays variation in the range of 3.4 to 3.6 eV.

Synthesis of nano-crystallite hydroxyapatites in different media and a comparative study for estimation of crystallite size using Scherrer method, Halder-Wagner method size-strain plot, and Williamson-Hall model

Hydroxyapatite (HAp) [Ca10(PO4)6(OH)2] is remarkably similar to the hard tissue of the human body and the uses of this material in various fields in addition to the medical sector are increasing day by day. In this research, mustered oil, soybean oil, as well as coconut oil were employed as liquid media for synthesizing nanocrystalline HAp using a wet chemical precipitation approach. The X-ray diffraction (XRD) study verified the crystalline phase of the HAp in all the indicated media and discovered similarities with the standard database. Several prominent models such as the Scherrer's Method (SM), Halder-Wagner Method (HWM), linear straight-line method (LSLM), Williamson-Hall Method (W-M), Monshi Scherrer Method (MSM), Size-Strain Plot Method (SSPM), Sahadat-Scherrer Method (S–S) were applied for the determination of crystallite size. The stress, strain, and energy density were also computed from the above models. All the models, without the Linear straight-line technique of Scherrer's equation, resulted in an appropriate value of crystallite size for synthesized products. The calculated crystallite sizes were 6.5 nm for HAp in master oil using Halder-Wagner Method, and 143 nm for HAp in coconut oil using the Scherrer equation which were the lowest and the largest, respectively.

Synthesis of pure and Cd-doped hydroxyapatite for the photo-catalytic degradation of Amoxicillin and Ciprofloxacin: Crystallographic characterization using XRD

Nanosized hydroxyapatite (HAp) is considered an elementary material for artificial bone tissue engineering and the applications are expanding and one of them is the photocatalytic degradation of environmentally hazardous pollutants. In this research, HAp nanoparticles, in pure form and doped with cadmium (Cd), were synthesized using a conventional wet-chemical precipitation method. Additionally, the synthesized samples such as pure and Cd-doped HAp were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and UV–Vis spectroscopy. Moreover, the XRD analysis allowed for a detailed estimation of the crystallite size, assisting in their tailoring of increased photocatalytic activity. The crystallite sizes of the nano-crystallite Hap were evaluated using the Scherrer Method (SM), Williamson-Hall Method (WHM), Size-Strain Plot (SSP), Halder-Wagner Method (HWM), and Sahadat-Scherrer Method (SSM). The models confirmed the formation of nano crystallite hydroxyapatite in pure and doped form. Cadmium doping in HAp showed great photocatalytic activity for example at 150 min, 31 % amoxicillin and 52 % ciprofloxacin were degraded upon 1.5 wt % Cd doping in HAp crystal. The research demonstrated that doping Cd in HAp crystal improved photocatalytic activity towards antibiotic solution (ciprofloxacin and amoxicillin) under all test circumstances.

Different solvents and organic modifiers for the control of crystallographic parameters in nano-crystallite hydroxyapatite for amplification of photocatalytic activity.

In this research, HAp nanocrystals were synthesized using conventional wet chemical precipitation methods using various organic modifiers, including urea, palmitic acid, and naphthalene. Ethanol and isopropyl alcohol (IPA) were used as solvents in this process. Different characterization techniques, namely X-ray diffraction (XRD), scanning electron microscopy (SEM), and UV-vis absorption spectroscopy, were employed to ascertain the formation of HAp nanocrystals. Numerous structural parameters, including lattice parameters, unit cell size, volume of the unit cell, specific surface area, degree of crystallinity, dislocation density, macrostrain, and crystallinity index, were assessed using XRD data. The linear straight-line method of Scherrer's equation, Monshi-Scherrer's method, the Williamson-Hall method, the size-strain plot method, the Halder-Wagner method, and Sahadat-Scherrer's model were applied to compute the crystallite size of the synthesized HAp samples. All the synthesized HAp has crystalline structures within the permissible range of 1-150 nm which were estimated from the XRD data using the mentioned models. However, the values for strain (from -3 × 10-4 to 6.4 × 10-3), strain (from -9.599 × 104 to 7 × 1010 N m-2), and energy density (from -11 × 1011 to 2 × 107 J m-3) were also calculated for the synthesized samples. In addition, the optical band gap energy of the synthesized HAp was computed (5.89 to 6.19 eV). The synthesis media have a control on the crystallographic planes, e.g. in the case of the ethanol medium, the (110) plane exhibited significant intensity (which could potentially serve as a driving force for enhancing photocatalytic activity). The use of 100% ethanol HAp yields the most favorable outcome regarding both the degradation percentage (91.79%) and degradation capacity (7%) for the Congo red dye.

Crystal structure modification of nano-hydroxyapatite using organic modifiers and hydrothermal technique.

Hydroxyapatite (HAp) synthesis was achieved through a hydrothermal method involving orthophosphoric acid and calcium hydroxide. Different organic modifiers such as urea, naphthalene, and palmitic acid were applied in the reaction system to modify the crystallite size along with the morphology of HAp. The synthesized HAp was validated via X-ray diffraction (XRD) data, Fourier Transform Infrared (FTIR) spectra, Field Emission Scanning Electron Microscopy (FESEM) image, and optical bandgap energy (<6 eV) was determined through UV-vis spectrophotometry. Apart from that, different techniques such as Scherrer's method, Halder-Wagner model, Williamson-Hall method, size-strain plot, as well as Sahadat-Scherrrer's models were applied for calculating the crystal domain size, and some models also incorporated energy density, strain, and stress. The synthesized HAp has a crystal structure that falls within the permissible range of <100 nm, as established by analyzing the XRD data using established models. Nevertheless, the values for strain (from -0.0006 to 0.0062), stress (from -30 902 to 36 940 N m-2), as well as energy density (from 4 × 10-14 to 113.72 J m-3) were likewise computed for the synthesized HAp. The texture co-efficient analysis reveals that doped HAp is grown in the (202) and (112) planes, palmitic acid_HAp in (002), (112), and (202) planes, while all the synthesized HAp (pure HAp, urea, naphthalene) is grown in the (002) and (112) planes. Rietveld refinement was also performed to estimate the quantative phase percentage from XRD data.

Synthesis of different types of nano-hydroxyapatites for efficient photocatalytic degradation of textile dye (Congo red): a crystallographic characterization.

The textile industry, a vital economic force in developing nations, faces significant challenges including the release of undesired dye effluents, posing potential health and environmental risks which need to be minimized with the aid of sustainable materials. This study focuses on the photocatalytic potential of hydroxyapatite together with different dopants like titanium-di-oxide (TiO2) and zinc oxide (ZnO). Here, we synthesized hydroxyapatite (HAp) using different calcium sources (calcium hydroxide, calcium carbonate) and phosphorous sources (phosphoric acid, diammonium hydrogen phosphate) precursors through a wet chemical precipitation technique. Pure and doped HAp were characterized via different technologies, which consist of X-ray diffraction (XRD), Fourier Transform Infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), as well as UV-vis spectroscopy. The effectiveness of the synthesized photocatalyst was evaluated by its interactivity with synthetic azo dyes (Congo red). The photodegradation of Ca(OH)2_HAp, CaCO3_HAp, ZnO-doped HAp as well as TiO2-doped HAp, were obtained as 89%, 91%, 86%, and 91%, respectively. Furthermore, at neutral pH, TiO2-doped HAp shows the highest degradation (86%), whereas ZnO-doped HAp possesses the lowest degradation (73%). Additionally, various XRD models (Monshi-Scherrer's, Williamson-Hall, and Halder-Wagner methods) were employed to study crystallite dimension.

A detailed investigation of rare earth lanthanum substitution effects on the structural, morphological, vibrational, optical, dielectric and magnetic properties of Co-Zn spinel ferrites.

In this work, Co0.5Zn0.5LaxFe2-xO4 (0.00 ≤ x ≤ 0.10) spinel ferrites were synthesized using the sol-gel auto-combustion method. X-ray diffraction (XRD) analysis and Rietveld refinement confirmed the presence of a cubic spinel structure. The crystallite size was estimated to be between 17.5nm and 26.5nm using Scherrer's method and 31.27 nm-54.52nm using the Williamson-Hall (W-H) method. Lattice constants determined from XRD and Rietveld refinement ranged from (8.440 to 8.433Å and 8.442 to 8.431Å), respectively. Scanning electron microscopy (SEM) revealed a non-uniform distribution of morphology with a decrease in particle size. The bandgap values decreased from 2.0eV to 1.68eV with increasing rare earth (La3+) doping concentration. Fourier-transform infrared (FT-IR) spectroscopy confirmed the presence of functional groups and M-O vibrations. The dielectric constant and dielectric loss exhibited similar behavior across all samples. The maximum tan δ value obtained at lower frequencies. Regarding magnetic behavior, there was a decrease in magnetization from 55.84 emu/g to 22.08 emu/g and an increase in coercivity from 25.63Oe to 33.88Oe with higher doping concentrations. Based on these results, these materials exhibit promising properties for applications in microwave and energy storage devices.

Investigating Fe-doped Ba0.67Ni0.33Mn1-xFexO3 (x = 0, 0.2) ceramics: insights into electrical and dielectric behaviors.

This study investigates the characteristics of the Ba0.67Ni0.33Mn1-xFexO3 perovskite compound, focusing on its structural and electrical aspects under varying Fe doping levels at the Mn-site (x = 0, 0.2). X-ray diffraction patterns confirm the material's consistent structure, with Fe3+ ions substituting Mn3+ ions while maintaining their identical ionic radius. Nano-crystallinity studies reveal single-phase crystallization in the orthorhombic structure with space group Imma. Samples are prepared through conventional solid-state sintering. The Williamson-Hall method calculates crystallite sizes, averaging 37 nm for x = 0 and 33 nm for x = 0.2. Electrical properties are examined using complex impedance spectroscopy at different temperatures and frequencies. Techniques such as energy dispersive X-ray spectroscopy (EDX) and scanning electron microscopy (SEM) assess chemical composition. Activation energy values increase from 0.138 eV for x = 0 to 0.171 eV for x = 0.2, leading to reduced dc conductivity across the investigated temperature range. Dielectric permittivity enhances proportionally with increasing Fe doping. Variations in impedance profiles reveal a relaxation phenomenon. A circuit model, Rg + (Rgb//CPEgb), elucidates impedance data. This study illuminates the interplay between Fe doping, activation energy, and electrical conductivity in Ba0.67Ni0.33Mn1-xFexO3 perovskite, offering insights applicable to electronic and energy-related devices. Perovskite-based nanomaterials have diverse environmental applications, including solar cells, light-emitting devices, transistors, sensors, and energy storage.

Magnetoelectric behaviour of Pb-free Na0.5Bi0.5TiO3-Ni0.5Co0.5Fe2O4 particulate novel ceramic composites

Magnetoelectric (ME) multiferroic composites are more promising candidates for low-power consumption devices, next-generation spintronic devices, and multistate memory devices since they exhibit significantly higher Magnetoelectric interaction over single-phase multiferroics. In this regard magnetic behaviour, dielectric, and magnetoelectric characteristics of a novel Pb-free (1-x) Na0.5Bi0.5TiO3-(x) Ni0.5Co0.5Fe2O4, (x = 0, 0.2, 0.4, 0.6, 0.8 & 1) particulate composites were explored. Solid-state synthesis was adopted to prepare the single-phase Na0.5Bi0.5TiO3 (NBT), Ni0.5Co0.5Fe2O4 (NCFO), and their composites. The presence of rhombohedral NBT and cubic inverse spinel NCFO in the composites were confirmed with X-ray diffraction (XRD) patterns. Microstrain (ε) induced in the prepared samples was estimated by using the Williamson-Hall (W-H) method. The piezoelectric NBT phase shows the tensile strain and the ferromagnetic NCFO shows the comprehensive strain. Among all the composites 0.8NBT-0.2NCFO shows a higher strain value of 0.012%, and the decrement in the strain values was observed upon increases in ferrite concentration. Backscattered scanning electron microscope (BS-SEM) images revealed the existence of highly dense uniformly distributed elements and Energy dispersive spectroscopy (EDS) confirmed the existing elements in the composites. UV–vis absorbance spectra disclosed a rise in energy gap values from 1.14 eV to 3.0 eV with increasing NBT percentage. Variations of dielectric permittivity and dielectric loss with respect to AC frequency were studied at room temperature (RT), and the 0.2NBT-0.8NCFO sample shows a high dielectric permittivity of 8500 at ∼100Hz. M − H (Magnetization-Magnetic field) hysteresis loops demonstrate the pure ferrite phase has a coercive field (Hc) = 578 Oe, remnant magnetization (Mr) = 21.43 emu/g and saturation magnetization (Ms) = 71.29 emu/g. The Ms and Mr values in the composites are enhanced with increasing ferrite percentage. Studies on ME behaviour of (1-x) NBT-(x) NCFO, (x = 0.2,0.4,0.6 & 0.8) show the coupling effect between both the phases at room temperature and the highest coupling coefficient value 3.16mV/Cm. Oe was observed for the 0.8NBT-0.2NCFO further the reasons and mechanisms are discussed.

Quantitative Determination of the Compositional Inhomogeneity in NMC Cathode Materials by Williamson-Hall Analysis

Over the past decades, the co-precipitation synthesis technique has been used, particularly for making LiNixMnyCozO2 (NMC) cathode materials for lithium-ion batteries (LIBs), due to better control of particle morphology and higher compositional homogeneity in the final NMC product compared to other methods. However, the co-precipitation method introduces complexity and consumes large amounts of energy and water, which can increase cost. This has led researchers to investigate solid-state NMC synthesis techniques in order to improve sustainability and reduce LIB cost [1-3]. Obtaining homogeneous mixing of transition metals at the atomic scale by solid-state methods remains a challenge. Since compositional homogeneity has a vital effect on the electrochemical performance of the NMCs, it is essential to quantitatively estimate the degree of inhomogeneity in cathode materials for the development of new synthesis methods.In the present study, a quantitative X-ray diffraction (XRD) analysis technique using the Williamson-Hall (WH) method is used to determine the degree of inhomogeneity in NMC precursors and NMC cathode materials. In this regard, single-phase rock salt (RS) precursors with varying degrees of transition metal homogeneity were prepared by combining NiO, MnO and CoO by grinding for different times, followed by heating under an Ar flow. Then, NMC cathode materials were made by heating the RS-precursors with lithium carbonate in air. EDS elemental maps showed that transition metal inhomogeneity existed in the RS-precursors and final NMCs and that this inhomogeneity is primarily associated with the Mn distribution (Figure 1(a)). Furthermore, the compositional inhomogeneity became reduced with increasing precursor grinding time.Using a WH analysis method, composition variation in the NMC precursor and in the final NMC product could be quantitatively determined from conventional XRD powder patterns. Utilizing this analysis, it was found that inhomogeneity in the precursor is translated into the final NMC, so that a similar trend in the degree of inhomogeneity was observed for both synthesized precursors and their NMC products (Figure 1(b) and (c)). Additionally, NMCs with high compositional homogeneity showed much better electrochemical performance compared to the samples with higher degree of inhomogeneity. We believe the proposed method is highly useful in the development of new cathode precursors and in predicting the performance of the NMC cathode materials by quantitatively determining their degree of compositional inhomogeneity.

Formation of PbS microstructured films by CBD method and study of structural properties

Microcrystalline lead sulfide (PbS) films were synthesized using the chemical deposition method. The films were deposited on pre-cleaned glass substrates and polished silicon wafers. Chemicals of high purity were utilized in the process. The morphology, composition, and structure of the films were characterized using scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and X-ray diffraction (XRD). The films exhibited a galena phase with a face-centered cubic structure belonging to the Fm-3m space group. The average grain size was determined using the WilliamsonHall method, revealing a homogenous structure. Raman spectroscopy further confirmed the structural integrity of the films. The obtained results contribute to the understanding of the synthesis and properties of microcrystalline PbS films.