Williamson-Hall Method Research Articles

The effect of strain induced phase transformation on the thermal expansion compatibility of plasma sprayed spinel coating on SOFC metallic interconnect – A study using in-situ high temperature X-ray diffraction

A new and novel approach has been adopted in this study to evaluate thermal mismatch induced by thermal expansion in substrate-coating contact pairs using in-situ high-temperature X-ray diffraction (HT-XRD). Atmospheric plasma sprayed (APS) Mn1.0Co1.9Fe0.1O4(MCF) coating on Crofer 22 APU steel interconnect was investigated. In-situ HT-XRD was performed individually for substrate and coating from 25 °C to 900 °C. Diffraction data were recorded for different temperatures to obtain lattice parameters and strain as a function of temperature. The coefficient of thermal expansion (CTE) of MCF coating was slightly higher than steel substrate and showed no significant thermal expansion mismatch till 700 °C. The increasing lattice strain measured by Scherrer and Williamson-Hall methods indicates strain-induced phase transformation of MCF coating with temperature, supporting the phase transformation-induced self-healing phenomenon of MCF coating. The merit of in-situ HT-XRD as a tool for optimizing operating temperature and measuring thermal mismatch of solid oxide fuel cell (SOFC) stacks has been discussed.

Investigation of Structural and Dielectric Behavior of Ba0.7Gd0.3MoxFe12-xO19 (Where x = 0.02) Hexaferrite Ceramics

Multiferroic ceramic composites of (Ba0.7Gd0.3MoxFe12-xO19 were prepared by using the solid-state reaction method with mol% fractions of x = 0.02, The preliminary structural studies carried out by X-ray diffraction at room temperature. It reveals that the samples have a hexagonal structure ferrite phase. The impurity phase of x-Fe2O3 appear at 32 ∼ 34 degree. Debye–Scherer and Williamson–Hall method were used to analysis for peak broadening Ba0.7Gd0.3MoxFe12-xO19 (where x = 0.02). Dielectric graphs show that curie temperature shifted towards the high temperature with increasing the frequency. the dielectric transitions at 200–300 °C.

Radio-frequency controlled crystalline phase transformation of MoS2 thin film fabricated by unique vapour-plasma mixing technique

Successful fabrication of molybdenum disulfide thin films on silicon substrates by a unique vapour-plasma mixing technique at a relatively low temperature of 300 °C is reported. This mixing technique involves simultaneous sputtering of a molybdenum target and thermal evaporation of sulphur flakes to form MoS2 molecules. Raman studies confirm the formation of MoS2 with characteristic E12g and A1g modes observed at ∼384 and ∼408 cm−1. The effects of radio frequency (RF) power on the physical properties of MoS2 film at a constant sulphur evaporation rate are investigated. The Raman and X-Ray photon spectroscopy reveal that a controlled crystalline phase transition between metallic tetragonal (1 T-MoS2) and semiconducting hexagonal (2H–MoS2) has been successfully achieved upon variation of the RF power. Furthermore in X-Ray diffraction analysis, Scherrer's, Williamson-Hall and Size-Strain Plot methods are used to extract relevant correlations between structural properties (viz. Crystallite sizes, strains) and the thin film growth controlling parameters.

Effect of thermal expansion on the high temperature wear resistance of Ni-20%Cr detonation spray coating on IN718 substrate

The temperature-dependent materials properties on the dry sliding wear resistance of the detonation sprayed Ni-20%Cr coating have been studied. In-situ high-temperature X-ray diffraction (HT-XRD) was used to investigate high-temperature properties such as stress relieving, recrystallization, and thermal expansion. The dry sliding wear test was performed by using a ball-on-disc tribometer by sliding velocities (0.1 m/s), varying loads (6 N and 10 N), and temperatures (25 °C and 850 °C) against alumina (Al2O3) ball. The phase evolution, thermal expansion, crystallite size, and lattice strain were determined by the Williamson-Hall method. Field emission scanning electron microscopy and a non-contact optical profilometer was used to characterize the wear scar and calculate the wear rate. The wear test results demonstrated that the as-deposited coatings coefficient of friction (CoF) and wear rate (ω) continuously decreased as the temperature increased. The primary wear mechanism changed from abrasive and surface fatigue to adhesive and oxidative wear. The impact of stress relieving, recrystallization, and forming a composite tribolayer (Cr2O3, NiO) at elevated temperatures reduced the friction and enhanced the wear resistance. The effect of stress relieving, recrystallization, thermal expansion, and oxidation on the wear resistance of the coating has been discussed with a suitable mechanism.

Deciphering the role of pristine and Ni ions substituted Co3O4 nanoparticles with altered structural, magnetic and dielectric traits towards elevated photosensing and photocatalytic activity

ABSTRACT Pure and nickel (Ni) doped cobalt oxide nanoparticles were employed by the co-precipitation method to present the structural, optical, and photocatalytic characteristics of NixCo3-xO4 nanoparticles (x = 0, 0.05, 0.1, and 0.3) for organic pollutant photodegradation. X-ray diffraction (XRD) was employed on NixCo3-xO4 samples with particle sizes ranging from 14 to 22 nm, confirming the occurrence of cubic phase. In addition, particle size was calculated by Debye Scherrer, Williamson-Hall (W-H) and Halder methods, respectively. The Fourier transform infrared (FTIR) analyses of all samples characterised the inherent lattice vibrations of spinel structures octahedral and tetrahedral sites, respectively. FESEM image depicts irregular-shaped clusters and EDX confirmed the presence of Ni, Co and O elements. The mesoporous nature of the pores and high BET specific surface area indicated the presence of several active sites, proving their viability as photocatalysts. UV-Vis spectrophotometer was utilised to measure the optical properties, which included recording absorption spectra and computing optical parameters. The photocatalytic activities of the pure Co3O4 and NixCo3-xO4 photocatalysts were studied by the degradation of a series of four dyes (Congo Red, Tartrazine, Rhodamine B, and Methylene Blue) solution under visible light irradiation. Compared to pure cobalt oxide, Ni-incorporated Co3O4 exhibits a substantially higher photocatalytic efficiency that increases with Ni doping concentration. The photocatalysts displayed superior recycling stability, retaining high performance after three cycles. The photosensing properties were investigated under UV light, and a considerable photocurrent enhancement was observed. As a result, it is illustrated that Ni-doped cobalt oxide NPs are a potential material for the fabrication of photosensitive devices.

Determining the Particle Size of Cu and Ni in Thin Cu/Ni Films using the Williamson-Hall Method

This research focuses on analyzing the particle size of a thin Cu/Ni layer produced through electroplating by varying the input voltage. The Williamson-Hall method is used to determine the particle size of the layer, and an X-ray diffractometer is used to characterize the layer. The study finds that the particle size of Cu and Ni layers with different applied voltages has different values due to various factors. The optimum voltage for the Ni layer is found to be 7.5 volts, and its overall particle size is 4.13 × 10^(-10) nm, while the particle size of Cu is 5.00 × 10^(-9) nm. The applied voltage affects the particle size produced, and the research identifies an optimum voltage at 7.5 volts.

Strain induced by temperature evolution of mesoporous ZnO nanopowders and its effect on structural, optical and electrical impedance properties

The structural and optical properties of ZnO nanopowder samples prepared by a novel green hydrothermal method have been studied. The prepared ZnO nanopowder samples were annealed (200, 250, 300, 400, 500 °C) and characterised through XRD (X-ray diffraction), FE-SEM (field emission scanning electron microscopy), BET (Brunauer–Emmett–Teller), FT-IR (Fourier transform infrared spectroscopy), UV–Vis (Ultraviolet–visible) spectroscopy, PL (Photoluminescence) spectroscopy and EIS (Electrochemical Impedance spectroscopy). The XRD Study revealed that the prepared samples were crystalline with ZnO hexagonal wurtzite structures. The crystallite sizes were determined using the Debye–Scherrer and Williamson–Hall methods and found to increase from 20.5037 to 25.9157 nm and 22.3261 to 31.4388 nm respectively with an increase in annealing temperature. The FE-SEM revealed that the prepared ZnO nanopowder samples were of spherical shape which corroborated the XRD results. The BET results showed that the prepared nanopowder samples were mesoporous with the average pore size varying between 15.125 and 25.583 nm and surface area varying between 15.337 and 23.959 m2/g. The presence of functional groups and chemical bonding were confirmed by the FTIR measurements. The energy band gaps were determined using the Kubelka-Munk function applied to UV–Vis spectra and found to be decreasing from 3.243 to 3.160 eV with an increase in annealing temperature. PL results revealed a clear dependence of the emission with annealing temperature which was caused by the decrease of free carrier concentration as the annealing temperature increased. EIS measurements indicated an increase in electrical resistance with an increase in annealing temperature with the sample annealed at 300 °C having the smallest resistance.

Morphological, structural, surface, thermal, chemical, and magnetic properties of Al-doped nanostructured copper ferrites

Aluminum-doped copper ferrite nanoparticles synthesized via thermal decomposition were analyzed for Al3+ substitution effects. Nanocrystalline doped copper ferrite with a crystallite size <9 nm was characterized using several advanced techniques, including X-ray diffractometry (XRD), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), and X-ray photoelectron spectroscopy (XPS). The degree of thermal decomposition used for doping copper ferrite at the nanoparticle level correlates well with the quantitative, dimensional, and structural characterizations. The Scherrer equation and Williamson–Hall method were employed to determine the general lattice strain and constants. Structural properties, such as the oxygen positional parameters, radii of the octahedral and tetrahedral sites, hopping lengths, bond lengths and angles, site bonds, and edge lengths, were determined using XRD patterns. The improved A–B super-exchange interaction was demonstrated by the discrepancy in the theoretically anticipated bond angles. The analysis of magnetic hysteresis (M − H) using a vibrating sample magnetometer (VSM) and XPS confirmed the improvement in the super-exchange interaction. XPS results suggest that Fe and Cu in the crystal lattice are in the form of FeIII and CuII, respectively. The investigation of the degree of inversion, state, and composition using XPS aids to understand the properties of the nanostructured copper ferrites. The saturation and remnant magnetization were determined from hysteresis loops at 1.8 T obtained using the VSM at room temperature. The noncollinear spin and efficient sublattice interactions are responsible for the decrease in Ms and Mr.

Zno nanoparticles: Synthesis and crystal structure study

(Zn(NO2)2.6H2O) and (NaOH) are used for synthesis ZnO nanostructures by one step reaction at 80℃ . X-ray diffraction (XRD) pattern referes polycrystalline nature with a hexagonal structure. Rietveld refinement (curried out by fullprof software) of XRD patterns a provide accurate values for the lattice parameter a=3.250353 0.00009 Å , c=5.207006 0.00020Å where c/a ratio is 1.601981. The average crystalline size was calculated by Debye-Scherrer method about 30 nm. The effects of strain in X- ray line broadening of ZnO nanoparticles (NPs) were investigated by Williamson-Hall method revealed that the peak broadening is not only due to reduced coherently diffracting domain size but also due to a significant strain distribution. The extracted particle size is about 31.5 nm and internal lattice strain value was found to be 6*10-4. The morphological and topographical studies were carried out by using scanning electron microscopy SEM, the average particle size is matched with that obtained by Debye-Scherrer and Williamson-Hall methods.

Effect of sintering additives on Y2O3 ceramic: Synthesis, structural, morphological, and optical properties investigations

Solid-state ceramic lasers have a wide range of applications in industrial, medical, and military applications. This research work presents the fabrication of vacuum sintered Y2O3 ceramics synthesized using co-precipitation method. The impact of sintering additives such as La2O3 and ZrO2 were examined on the structural and morphological traits of Y2O3. The development of pure cubic phases is revealed by X-ray diffraction studies. Williamson-Hall method is used to determine the crystallite size and micro-strain. The incorporation of La3+ and Zr4+ are confirmed through FTIR spectra. The optical characteristics are investigated through UV–VIS spectroscopy. The addition of La3+ and Zr4+ additives increases the densification of Y2O3 ceramic pellets and improves their sintering behavior. The effect of sintering additives on grain size and elemental composition were examined using scanning electron microscopy and energy dispersive spectroscopy.

X-ray diffraction analysis of SrTiO3 nanoparticles by Williamson-Hall, size-strain plot and FullProf method

Strontium Titanate (SrTiO3) nanoparticles were synthesized using solid state method. Rietveld refinement using FullProf tool of x-ray diffraction data revealed the cubic structure with Pm-3 m space symmetry is present in SrTiO3-NPs. Williamson-Hall analysis with size-strain plot were used to examine the impact of crystallite size and lattice strain on the physical phenomenon of SrTiO3 nanoparticles. Different models like uniform density model (UDM), uniform stress deformation model (USDM), uniform deformation energy density model (UDEDM), and the size-strain plot (SSP) were used to estimate the strain, stress, and energy density parameters using shape profile of the X-ray diffraction peaks. FESEM microscopy is used to investigate the surface morphology as well as the particle size of the crystalline material. The particle size is obtained to be 66 nm.

Influence of Pulse Laser Energy on Structural and Magnetic Properties of CoFe2O4 and CoLa0.01Fe1.99O4 Thin Films

Cobalt ferrite and CoLa0.01Fe1.99O4 thin film were prepared using the pulsed laser deposition method with varying pulse laser energy. XRD analysis was used to investigate the structure of ferrite thin films. The study was expanded to include morphology and magnetic properties. The prepared films showed a strong peak at (311), which belongs to the cubic spinel cobalt ferrite phase with the presence of some peaks belonging to α-Fe2O3 as hematite phase that depressed when doping with La ion, and the crystallization improvement significantly after intensity increases by increasing the pulsed laser energy from 500 to 650 mJ. The lattice constant of Cobalt ferrite thin films increased with the increase in the laser pulse energy while the crystallite size deduced from the Williamson Hall method showed decreases with the increases of pulse laser energy. The saturation, remnant magnetization, and coercivity of prepared films were studied according to increasing pule laser energy and Lanthanum doping.

Effect of pulsed magnetic field on retained austenite of quenched 8Cr4Mo4V steel under cryogenic condition

High-intensity pulsed magnetic field was applied to modify the microstructure and mechanical propertis of quenched 8Cr4Mo4V bearing steel under the cryogenic environment. The microstructual transformation in 8Cr4Mo4V bearing steel was investigated by X-ray diffraction (XRD), Vibrating sample magnetometer (VSM) and Electron Backscatter Diffraction (EBSD) and so on. The results revealed that individual deep cryogenic treatment (DCT) promote the transformation from retained austenite (RA) in quenched steel to martensite. However, this phase transformation will be inhibited by coupling high-intensity magnetic field with deep cryogenic treatment (MDCT). For instance, the relative reduction of RA content in DCT samples was 10 ± 2%, while that in MDCT samples was 3 ± 3%. Furthermore, the modified Williamson-Hall method was utilized to estimate the dislocation characteristics based on XRD profile analysis. It exhibited that the proportion of edge dislocation significantly decrease from 61.8% to 43.7% by DCT, while this type of dislocation remains almost unchanged after MDCT. Moreover, the microhardness of quenched 8Cr4Mo4V steel became more uniform after MDCT than that of DCT. It can be indicated that the martensite transformation is blocked and carbon cluster is dissolved under the condition of coupling pulsed magnetic field treatment.

Gamma radiation effect on the optical linear and nonlinear properties of PVA with trypan blue film

A film of polyvinyl alcohol (PVA) and trypan blue dye is prepared via the casting method. The characterization of the film is carried out using the microscope and Image J software, x-ray diffraction (XRD), UV–vis spectrophotometer and computational chemistry using density functional theory (DFT). The prepared film optical properties are studied under the irradiation with gamma radiation of doses that varied in the range 14.4–57.6 Gy. The crystallite size of the film is studied using the Scherrer method and the Williamson–Hall method. Numbers of linear and nonlinear (NLO) parameters of the prepared film are obtained via the measurement of its absorbance and transmittance spectra before and after irradiation with the gamma radiation.

A comparison of antibacterial activity in dark-UV light in perspective of surface and structural properties of spray pyrolysis grown Cu doped Cr2O3 thin films

Thin films of Cr2O3 and Cu doped Cr2O3 thin films were prepared using the spray pyrolysis technique with different Cu/Cr ratios. Precursor solution of 0.2 M was sprayed on a pre-heated (≈ 400 °C) soda lime glass substrate using air as the carrier gas. XRD analysis confirmed polycrystalline nature of the films with rhombohedral structure. Crystallite size and lattice strain have been estimated using Williamson-Hall method. These films were porous and presented a rough morphology and showed a strong signature on the presence of vibrational Cr-O bonding. The solid-liquid surface contact angle measurements revealed a large contact angle which is indicative of reduced surface energy. Vickers hardness measurement reveals that Cr2O3 thin film with 2% Cu/Cr ratio have high hardness value of 903 HV (0.2 kgf). The antibacterial activity of the films was investigated against two gram-positive (Bacillus Subtilus and Bacillus Meurellus) and two gram-negative bacteria (Escherichia Coli and Acetobacter Rhizopherensis). A comparison was established both under dark and UVA light in terms of structural properties of the films. Antibacterial activity was significantly enhanced with the increase in Cu/Cr ratio. Interestingly, the UVA light further facilitated to boost the antibacterial effect against both types of bacteria. A good correlation was found between the structural parameters and the zone of inhibition.

Influence of the A-site cation on structural, morphological, magnetic, optical and transport properties of R2CoMnO6(R = Nd, Y, Ho and Er) double perovskite oxides

The A-site substituted double perovskite oxides (DPOs) have in the recent decades gained much attention due to their various interesting properties and possible applications. For this reason, R2CoMnO6 (R = Nd, Y, Ho, and Er) DPOs have been synthesized using the auto-combustion sol-gel method. X-ray diffraction analysis suggests the crystal structure, i.e., monoclinic for all under-investigated DPOs at room temperature (RT), consisting of space group P2 1 /n which is confirmed by Rietveld refinement. Crystallite size is calculated using Scherrer and Williamson-Hall methods, and it was found that the crystallite size decreased with decreasing ionic radii from 55–29 nm on average. The micrographs were obtained by using a field-emission scanning electron microscope (FE-SEM), which reveals an almost homogeneous distribution of grains throughout the surface of all DPOs. All observed infrared and Raman active phonon modes have been assigned to vibrations of atoms and groups of atoms consistent with the prediction of group theory. The intermediate band gap values (1.34–1.63 eV) determined by the Tauc relations suggest the semiconducting nature of these DPOs which makes them promising materials for photovoltaic applications. Dc electrical resistivity and dielectric measurements also suggest semiconducting behaviour above ambient temperature, which is attributed to a small polaron hopping conduction mechanism. The Maxwell-Wagner type interfacial polarization has described the nature of the frequency-dependent dielectric constants in these DPOs. The dielectric (ac) study also suggests the small polaron hopping conduction mechanism in all samples, which supports our findings in resistivity measurements.

Strain effects on the optoelectronic performance of ultra-wide band gap polycrystalline β-Ga2O3 thin film grown on differently-oriented Silicon substrates for solar blind photodetector

β-Ga2O3 based photodetectors are being intensively researched as possible substitutes to conventional Silicon deep-UV PDs. However, high cost of single-crystalline Ga2O3 poses hindrance towards commercialization by semiconductor industry still monopolized by Si. An easier integration with existing technology can be achieved by growing Ga2O3 thin films on Si directly, but growth of lattice mismatched substrates is often tricky and complicated with various parameters such as interfacial energies, surface energies, etc. playing important roles. Thus, it becomes imperative to investigate the role of each of these on film growth and devices thereof. Herein, polycrystalline β-Ga2O3 thin films are grown on different orientations of Si namely (100), (110) and (111), offering varied surface energies for film growth even under identical conditions. Best growth is observed on Si (111) substrate, deduced by largest crystallite size and lowest strain using Williamson-Hall method. This leads to devices of Ga2O3 on Si (111) having improved performance compared to other orientations. To validate effect of strain on device performance, a well-known method of reducing strain further – introduction of seed layer – is utilized, leading to further enhancement. This implies that PD performance is highly dependent on orientation of substrate used as the strain induced ultimately affects film growth.

Crystallographic characterization of bio-waste material originated CaCO3, green-synthesized CaO and Ca(OH)2

Municipal inorganic waste material (eggshell), which was chosen as the source of calcium carbonate, was utilized to synthesize two industrially valuable inorganic compounds, calcium oxide and calcium hydroxide following a sustainable synthesis method. The crystallographic parameters such as lattice parameter, unit cell volume, crystallite size, microstrain, dislocation density, relative intensity, crystal growth preference, and crystallinity index of raw eggshell, calcium oxide, and calcium hydroxide were explored based on the X-ray diffraction. The polymorphic mole fraction of calcite, vaterite, and aragonite in natural eggshells was also estimated. Crystallite size was calculated with the assistance of the Scherrer equation along with Williamson–Hall Method, Monshi-Scherrer Method, and Liner straight-line method of Scherrer’s equation. A relationship among the crystal growth preference, dislocation density, and microstrain was established for the considering compounds. The raw eggshells and synthesized products were also characterized with the aid of Thermogravimetric Analysis (TGA), Differential Scanning Calorimetry (DSC), Fourier Transform Infrared (FTIR), and Scanning Electron Microscopy (SEM).

A double perovskite BaCaZrMnO6: synthesis, microstructural dielectric, transport and optical properties

In this communication, synthesis (solid-state reaction) and characterization of a double perovskite BaCaZrMnO6 are reported. The Williamson–Hall method is used to compute average crystallite and micro-lattice strain in the prepared sample after structural analysis with X-Pert High-Score software. The sample's microstructural characteristics were investigated using a scanning electron microscope (SEM), and compositional purity was determined using energy dispersive x-ray spectroscopy (EDX). The Raman spectrum displays all atomic modes of vibration, providing information on phase, polymorphic crystallinity, and molecular interaction, as well as confirming the presence of all constituent elements. The ultraviolet visible spectrum research gives good bandgap energy for several optoelectronic devices. The impedance parameters have been measured using an impedance analyzer in a wide range of frequencies (102–106 Hz) and temperatures from 25 °C to 500 °C. The dielectric versus temperature and frequency analysis validates the Maxwell–Wanger type of dielectric dispersion. The impedance spectroscopy investigation indicates that the sample exhibits a negative temperature coefficient of resistance (NTCR), whereas the modulus analysis verifies a non-Debye type of relaxation process. The results of the ac conductivity research confirm a thermally activated relaxation process. Nyquist plot analysis reveals the NTCR character, which is well supported by Cole–Cole plots. The resistance versus temperature analysis supports the NTC thermistor nature, but the polarization–electric field (P–E) loop analysis reveals the presence of ferroelectric character, making it a strong option for temperature sensors and ferroelectric-related devices.

Синтез и магнитные свойства цинк-теллуритных стекол, активированных наночастицами магнетита

An effect of activation with nanosized particles Fe3O4 on structural and magnetic properties of zinc-tellurite glasses 20·ZnO−(80−x)·TeO2−x·Fe3O4 (x = 0, 1, 3, 7), prepared with melt-quenching method, have been investigated. Some functional properties of the glasses were experimentally investigated with X-Ray diffraction, Energy dispersive and Raman spectroscopies, and SQUID magnetometry. The values of the average crystallite sizes calculated with Scherer and Williamson–Hall methods were comparable with the sizes of magnetically active clusters reconstructed from the results of processing of the magnetic field dependences of the values of specific magnetizations, indicating their effect on the change in the magnetic properties of activated glasses. A partial phase transformation of ferrimagnetic magnetite Fe3O4 into paramagnetic maghemite γ-Fe2O3, caused by the oxidation of Fe2+ cations into Fe3+, has been revealed.