Analysis Of X-ray Diffraction Data Research Articles

Electrical resistivity and magnetoresistance of Sr3Fe2+xMo1–xO9–3x/2 (x = 0.45, 0.60, and 1.00) prepared by the solid-state reaction

In this paper, we focus on understanding the behavior of the temperature dependence of electrical resistivity (ρ) and magnetoresistance (MR) in Sr3Fe2+xMo1–xO9–3x/2 perovskites with x = 0.45, 0.60, and 1.00. Three polycrystalline materials were synthesized using conventional solid-state reaction techniques. Rietveld analysis of room-temperature X-ray diffraction data reveals that all three compositions crystallize in tetragonal symmetry; where x = 0.45 and 0.60 undergo an I4/mcm space group, while x = 1.00 adopts a P4/mmm space group. Electrical resistivity measurements carried out at magnetic fields (0 and 1 T) reveal the presence of a transition from the ferromagnetic phase to the paramagnetic phase in the vicinity of the TMI. The metal-insulator transition temperature (TMI) decreases with increasing Fe content and rises slightly with changing magnetic field from 0 to 1 T. The magnetoresistance (MR) of the SrFeO3–δ sample (x = 1.00) has a large value of about 63.6%, indicating that it can be exploited for certain devices. A variety of theoretical models are used to study the behavior of electrical resistivity in various temperature ranges, showing excellent agreement with experimental results.

Structural, optical, and electrical characteristics of anatase Titanium dioxide tailored by doping of Nitrogen and Copper ions

Pure anatase TiO2 nanoparticles and its mono–doped and co–doped derivatives [i.e. (TiN0.007O1.993); (Ti0.998Cu0.002O2); (Ti0.998Cu0.002N0.007O1.993)] were prepared by sol–gel auto–combustion technique. Further, the effects of copper (Cu) and nitrogen (N) dopants have been investigated on structural, optical and dielectric properties of nanostructured TiO2 using X–ray diffraction (XRD), Raman spectroscopy, ultraviolet–visible (UV–Vis) spectroscopy and dielectric spectroscopy measurement respectively. The Rietveld refinement analysis of XRD data and Raman spectra revealed that all the synthesized samples have pure anatase phase having tetragonal structure with space group of I41/amd. The pure anatase phase of doped samples illustrate the substitution of Cu ions at Ti4+ sites and N ions at O2– sites in the TiO2 host lattice. The crystallite size of TiO2 and its derivatives has been observed in the range of 11–14 nm. The band gap of TiO2 reduced from 3.2 to 1.9 eV with mono–doping and co–doping of the N and Cu in TiO2 lattice as confirmed by UV–Vis spectroscopy. This red–shift might be occur due to the possible formation of N–2p and Cu–3d localized levels (mono–doping case), and the creation of isolated intermediate states (co–doping case). The dielectric spectroscopy was carried out to investigate the electrical properties in details and explained in terms of structural and intrinsic ionic behaviour of different dopants. The detected band gap energies in N/Cu mono–doped and co–doped anatase TiO2 fall within the visible spectrum, rendering them suitable for harnessing solar energy in photocatalysis and photovoltaic applications.

Sol-Gel Multilayered Niobium (Vanadium)-Doped TiO2 for CO Sensing and Photocatalytic Degradation of Methylene Blue.

Multilayered TiO2 films doped either with Niobium or Vanadium (1.2 at. %) were deposited by the sol-gel dip coating method on c-Si and glass substrates. The films on glass substrates were tested for CO sensing and photocatalytic degradation of methylene blue. X-ray diffraction data analysis showed that all the TiO2:Nb(V) films were nanocrystalline in the anatase phase, with a uniform and compact microstructure and a homogeneous superficial structure of small grains with diameters in the range of 13-19 nm. For the electrical characterization, the TiO2:Nb(V) films were incorporated in Metal-Insulator-Semiconductor (MIS) structures. The specific resistivity is of the order of 104 Ωcm and its value decreases with increasing the electrical field, which testifies to the injection of electrons into these layers. From the analysis of the current-voltage curves taken at different temperature- and frequency-dependent capacitance-voltage and conductance-voltage characteristics, the density and parameters of deep levels in these TiO2 films are evaluated and the electron charge transport mechanism is established. It was shown that the current in these TiO2:Nb(V)-Si MIS structures is mainly carried out by inter-trap tunneling via deep levels energetically distributed in the TiO2 bandgap. Testing these sol-gel TiO2:Nb(V) layers for gas sensing and photocatalytic capabilities proved that they could serve such purposes. In particular, the results of the V-doped sol-gel TiO2 film confirm its CO detection capability, which is rarely reported in the literature. For the photodegradation of methylene blue, the Nb-doped TiO2 samples were superior, with nearly double the photocatalytic efficiency of undoped TiO2.

Investigation of structural, electrical, and magnetic variations of Ni-Zn-Co ferrites by substituting rare earth Ho3+ for high-frequency applications

The investigation of structural, magnetic, and electrical properties of Ni0.6Zn0.3Co0.1HoxFe2−xO4 (NZCHF, 0 ≤ x ≤ 0.2) ferrites, synthesized through the sol–gel autocombustion method, has been undertaken. The refined x-ray diffraction (XRD) analysis was performed for XRD data analysis using Fullprof Suite software and it confirmed a single-phase cubic spinel structure, with the determination of crystallite size, refinement parameters and lattice constants. The bulk density of the samples consistently remained lower than the x-ray density, with densities increasing proportionally to the enhancement of Ho concentration. FTIR analysis corroborated the presence of metal-oxygen bonds within the ferrite possessing a spinel cubic structure. 57Fe Mossbauer spectroscopy showed that the hyperfine magnetic field of tetrahedral (A) and octahedral (B) sites decreased with the substitution of Ho3+ ions that preferentially occupy the B site. The impedance analyzer and vibrating sample magnetometer (VSM) were utilized to measure the real and imaginary parts of the complex permeability and magnetic properties of the samples, respectively. Complex impedance plots were scrutinized to discern the contributions of grain and grain boundary resistances, providing insights into the electrical behavior of the ferrite samples. Furthermore, the introduction of Ho concentration led to alterations in other key properties of the ferrites, including coercivity (H c ), retentivity (M r ), anisotropy constant (K), and magnetic moment (μ B ).The impact of the rare-earth content on the magnetic features of the prepared NiZnCo ferrite microspheres was investigated by analyzing magnetic-hysteresis (M-H) loops, which showed soft ferrimagnetism. Concurrently, the dielectric constant and dielectric loss tangent of the studied samples exhibited a decrease with the rise in Ho3+ concentration. The expected reduction in tan loss in the prepared samples is attributed to the increase in ac resistivity associated with the higher Ho3+ content.

Pharmacological Effect of In Vitro Antioxidant Property and Green Synthesis of Silver Nanoparticles (AgNPs) Utilizing Murraya koenigii Antibacterial Application

ABSTRACT Background: Nonessential heavy metals pose a significant threat to human health due to their toxicity. Mercury, in particular, is identified as a hazardous metal. The study aims to detect mercury using colorimetric analysis with Murraya koenigii, emphasizing the eco-friendliness of the method. Aims and Objectives: The primary objective is to detect mercury using a colorimetric analysis method employing Murraya koenigii. Additionally, the study aims to investigate the eco-friendliness of this detection method. Materials and Methods: Colorimetric analysis was conducted using Murraya koenigii to detect mercury. Ultraviolet-visible (UV-vis) spectroscopy was employed to detect the formation of silver nanoparticles (AgNPs), with a characteristic surface plasmon resonance (SPR) band observed. X-ray diffraction (XRD) data analysis was performed to determine the crystalline nature and size of AgNPs. Scanning electron microscopy (SEM) was utilized to visualize the morphology of AgNPs. Fourier transform infrared (FTIR) spectroscopy was employed to identify functional groups involved in reducing silver ions. Antibacterial properties of synthesized AgNPs were tested against various microorganisms, including Escherichia coli, Staphylococcus aureus, Streptococcus mutans, and Enterococcus faecalis. Results: Mercury was successfully detected using colorimetric analysis with Murraya koenigii. Formation of AgNPs was confirmed by UV-vis spectroscopy, with a characteristic SPR band at 418 nm. AgNPs were found to be crystalline with an average size of 5.20 nm, as determined by XRD analysis. SEM images revealed spherical and polycrystalline AgNPs. FTIR spectra indicated the involvement of the -OH group of compounds in the extract in reducing silver ions. Synthesized AgNPs exhibited antibacterial properties against various microorganisms. Conclusion: A sustainable and eco-friendly method for synthesizing AgNPs using Murraya koenigii extract was successfully developed. This method not only detected mercury but also demonstrated antibacterial properties against various microorganisms. The study underscores the health implications of nonessential heavy metals, emphasizing the importance of eco-friendly detection and mitigation methods.

Spectroscopic properties and photoluminescence of the Li2B4O7:Mn,Sm glass

The Li2B4O7:Mn,Sm glass containing 1.0 mol.% MnO2 and Sm2O3 were researched by X-ray diffraction (XRD), electron paramagnetic resonance (EPR), and optical spectroscopy methods. The studied glass of high optical quality was obtained by high temperature melting technique. Parameters of the local structure (interatomic distances and coordination numbers) of Li2B4O7:Mn,Sm glass were derived from XRD data analysis. The EPR and optical spectroscopy (absorption, luminescence excitation, emission, decay kinetics) show the presence of Mn2+(3d5) and Mn3+(3d4) impurity ions in the Li2B4O7:Mn,Sm glass. By EPR spectroscopy in the studied glass were identified three types of Mn2+ centres: single Mn2+ (1) centres in the strongly distorted sites (ratio of rhombic and axial constants, |E/D| ≤ 1/3), single Mn2+ (2) centres in the sites with almost cubic symmetry (D ≅ 0, E ≅ 0) as well as Mn2+ pairs and small clusters coupled by magnetic dipolar and exchange interaction, respectively. The Mn2+ EPR spectra parameters in the Li2B4O7:Mn,Sm glass have been determined at T = 295 K. Optical absorption spectrum of the Li2B4O7:Mn,Sm glass contains a very broad intense band peaked at 467 nm belonging to the 5Eg(D) → 5T2g(D) transition of Mn3+ ions and several weak narrow lines corresponding to the 6H5/2 → 6P3/2, 6H5/2 → 6F9/2, 6F7/2, 6F5/2 transitions of Sm3+ (4f5, 6H5/2) ions. Emission spectrum of the Li2B4O7:Mn,Sm glass exhibits a broad band corresponding to the 4T1g(G) → 6A1g(S) transition of Mn2+ ions and three characteristic bands in the yellow-orange-red range belonging to the 4G5/2 → 6H5/2, 6H7/2, 6H9/2 transitions of Sm3+ ions. Photoluminescence spectra (excitation and emission) and decay kinetics of the Mn2+ and Sm3+ ions in the Li2B4O7:Mn,Sm glass are interpreted in comparison with corresponding results for Li2B4O7:Mn and Li2B4O7:Sm glasses. Energy transfer processes Sm3+→Mn2+, Mn3+, and Mn2+→Mn3+ in the studied glass are considered.

Raman spectroscopic evaluation of structural-phase state of titanium and zirconium pseudo-single crystals deformed in Bridgman anvils

A complex study of the microstructure of titanium and zirconium pseudo-single crystals subjected to severe plastic deformation in Bridgman anvils under a pressure of 8 GPa at a temperature of 80 K has been carried out. Raman spectra of the samples deformed to different degrees show a two-phase α + ω state, which indicates the realization of the pressure-induced transition during deformation process with the retention of the ω-phase in the structure of both metals after the load removal. The quantitative ratio of α- and ω- phases in the structure of deformed metals and its change with increasing degree of deformation has been analyzed.Correlation of Raman spectroscopy results with experimental data of X-ray diffraction analysis, electron microscopic analysis, as well as literature data of calorimetry and calculated thermodynamic data by DFT method on kinetics of the reverse ω → α transformation demonstrates the efficiency of Raman spectroscopy method for estimation of the phase composition of pure metals, which experienced phase transition under loading.

Characterization of dielectric and piezoelectric responses in 0.76(Na0.5Bi0.5)TiO3-0.06BaTiO3-0.18(K0.5Bi0.5)TiO3 ceramics synthesized by the solid-state method

In this research, the authors explore the structural, dielectric, electrical insulating, electromechanical, and piezoelectric characteristics of ceramics that have been modified using BaTiO3 and (K0.5Bi0.5)TiO3.as key components. Specifically, they explore the composition (1-x-y)(Na0.5Bi0.5)TiO3-xBaTiO3-y(K0.5 Bi0.5)TiO3, where x (mol.%) varies between 0, 6, and NBT, and y (mol.%) varies between 0, 18, and KBT. These ceramics were fabricated using a solid-state synthesis technique. The optimized calcination temperature for achieving a pure perovskite phase was determined to be 1000 °C for a duration of 4 hours. The research involves a comprehensive analysis of the composition, microstructure, electrical insulating, and electromechanical characteristics of the ceramics. Rietveld analysis of X-ray diffraction (XRD) data was employed to accurately ascertain the morphotropic phase boundary (MPB) within this material. In this paper, we discuss the impact of crystallite size on the shifts in Raman band frequencies. Sintering at 1100 °C for 4 hours was found to enhance densification, with scanning electron microscopy (SEM) images illustrating a nearly uniform distribution of compact grains. Electrical insulating assessments demonstrate that each of the ceramics displays a scattered phase transition around the temperature Tm, with a diffusivity ranging from 1.4 to 1.8, and a shift of Tm towards elevated temperatures. Exceptional piezoelectric properties were observed at the morphotropic phase boundary (MPB), including a d33 value of 149 pC/N and electromechanical coupling factors kp of 0.297. These findings are attributed to the coexistence of rhombohedral and tetragonal phases, as well as precise grain size control. This research presents a novel approach to enhancing lead-free ferroelectric materials based on the composition 0.76(Na0.5Bi0.5)TiO3-0.06BaTiO3-0.18(K0.5Bi0.5)TiO3.

Synthesis, characterization and optical tuning of Sm3+ doped NaZnPO4 phosphors for white LED technology

This study presents a comprehensive investigation into the synthesis, structural-spectroscopic characterization, and optical properties analysis of Sm3-activated NaZnPO4 phosphors with varied Sm3+-doping percentiles, aimed at developing tunable luminescent materials for white-light-emitting diode (WLED) applications. The polycrystalline samples NaZn(1-x) Smx3+ PO4 (x = 0.00, 0.05, 0.10 and 0.15) phosphors were synthesized via a solid-state reaction method. X-ray diffraction data analysis confirms single phase monoclinic lattice with space group P 1 21/c 1 for all compositions. The Rietveld procedure also confirms the single phase and monoclinic structure of synthesized phosphors. Fourier-transform infrared) spectroscopy confirms compositional homogeneity. FE-SEM micrographs show irregularly stacked microstructures and morphology for all compositions irrespective of Sm3+ doping percentage. While EDS and Elemental mapping confirm uniform incorporation of Sm3+ ions in phosphors lattice. Diffuse Reflectance Spectra studies show Sm3+ doping resulted in redshift and band gap narrowing. In Photoluminescence spectroscopies, excitation and emission spectra reveal that distinctive photoluminescence spectra with notable emission peaks at 402 nm (6H5/2 → 4F5/2) and 599 nm (4G5/2 → 6H5/2). CIE chromaticity coordinates demonstrated varied color purity and coordinates for different doping levels, with promising orange-red emissions and increased luminosity. The observed optical properties suggest the potential suitability of Sm3+-activated NaZnPO4 phosphors as promising candidates for enhancing WLED efficiency and color quality.

Origin of linear magnetoresistance in Bi2Te3 topological insulator: Role of surface state and defects

Connection between topological surface states (TSS) and large linear magnetoresistance (LMR) is established in tetradymite Bi2Te3 through tuning of native defects. Thorough analysis of temperature dependent synchrotron X-ray diffraction data quantifies 0-D, 1-D and 2-D defect concentrations. Plausible variation of antisite defects is explained via carrier concentration data. Resistivity data divulge contribution of mixed bulk and surface states in the synthesized samples. High Fermi velocity (∼106 ms−1) and low Fermi energy (∼14 meV) of carriers are obtained. Lower defect concentration sample emerges with high magnetoresistance (MR) and higher mobility. Weak antilocalization (WAL) effect, signature of TSS, is revealed from MR. Large (80%), non-saturating LMR along with ultrahigh mobility (∼1 m2V−1s−1) in Bi2Te3 supports the presence of TSS. Magnetoconductance data are fitted with Hikami-Larkin-Nagaoka equation, obtaining further insight on WAL effect. In addition, extracted parameters like disorder correlation length and coherence length explicate the role of defect density on LMR.

Exploitation of mangliculous marine fungi, Amarenographium solium, for the green synthesis of silver nanoparticles and their activity against multiple drug-resistant bacteria

Abstract The green synthesis pathway for silver nanoparticles (AgNPs) used in bacterial treatment is regarded as crucial because of its cost-effectiveness, nontoxicity, and eco-friendliness. During the present work, the mangliculous marine fungi Amarenographium solium isolated from the Arabian Gulf Coast of Saudi Arabia were utilized for the synthesis of AgNP, through the bio-reduction of aqueous silver nitrate (AgNO3) solution. The success in AgNP synthesis was visually identified by the development of dark brown color in the cell-free filtrate and was further confirmed by ultraviolet–visible spectroscopy, which showed a peak at 425 nm. The AgNPs produced were further characterized using X-ray diffraction data analysis that proved the bioreduction of silver to 20 nm, and transmission electron microscopy revealed the formation of well-dispersed spherical nanoparticles with an average mean size of 12 nm. The optimization reaction parameters of temperature, pH, and metal salt concentration were carried out and resulted in a combination of 30°C, 7 and 1.5 mM, respectively, for rapid and maximum yield production. The antibacterial activity of the produced nanoparticles was evaluated using the two-fold microdilution method and showed a minimum inhibitory concentration of 9.375 μg/mL of AgNP against multiple drug-resistant bacterial strains.

Effect of La, Zr Doping on the Structural and Electrical Conduction Behaviour of BiFeO<sub>3</sub>-BaTiO<sub>3</sub> Ceramics

<p>This study presents a comprehensive investigation of the crystal structure and DC conduction mechanism of [(Ba<sub>0.7-x</sub> La<sub>x</sub>) Bi<sub>0.3</sub>][(Ti<sub>0.5</sub> Zr<sub>0.2</sub>) Fe<sub>0.3</sub>]O<sub>3</sub> with x = 0.00, 0.01, 0.03, 0.05 employing X-ray diffraction (XRD) and electrical conductivity measurements. Various compositions were synthesized through the solid-state ceramic route. XRD was used to investigate phase formation. Analysis of XRD data suggested a structural transition from cubic to tetragonal for x ≥ 0.01. The average crystallite size first increases for x = 0.01 and then decreases for x ≥ 0.03. The temperature-dependent electrical conductivity measurements were investigated over a wide temperature range which revealed distinct conductivity mechanisms governing the material's transport properties. The activation energy (E<sub>a</sub>) has been estimated from temperature-dependent DC conductivity. Overall, this study provides valuable insights into the correlation between crystal structure and electrical properties in [(Ba<sub>0.7-x</sub> La<sub>x</sub>) Bi<sub>0.3</sub>][(Ti<sub>0.5</sub> Zr<sub>0.2</sub>) Fe<sub>0.3</sub>]O<sub>3</sub>, offering significant implications for its potential applications in electronic and optoelectronic devices requiring tailored conductivity characteristics.</p>

Structure, soft magnetic properties of Fe-based magnetic composites and its practical application

A multi-stage technique for applying insulating coatings to metal powder particles has been developed in order to create a new class of Fe-based soft magnetic materials with improved characteristics. The density value calculated from the data of X-ray diffraction analysis is approximately 3 % higher than the experimentally measured values, which are 7.4–7.45 g/cm3. The low porosity of the composites is confirmed by the SEM and EDX results. The proposed method of encapsulation of iron powder with an oxide layer is a highly economical method for applying coatings of various chemical compositions to metal powders, and can be widely used in practice to obtain electrical materials. Comprehensive studies of the properties of the obtained samples of powder composite materials based on ABC100.30 iron, the particles of which are encapsulated with phosphorus oxide, have been carried out. It has been established that in a field of 1.5 T, the losses at a frequency of 1 kHz decrease 10 times with an increase in the thickness to 30 nm. The synthesized materials are recommended for use in the development of various types of high-frequency electric motors, generators, chokes, magnetic circuits and electrodes for high-frequency welding and other applications.

Waste to wealth: Facile activation of red mud waste and insights into industrial reactive dye removal from wastewater

Reactive dyes, widely applied in the textile industry for their vibrant colors, excellent fastness, and ease of application. Their presence poses multifaceted threats to aquatic ecosystems and health risks, including skin irritation, allergic reactions, respiratory problems, and increased cancer risk. In response to these challenges, this study explores the potential of acid-activated red mud, an industrial solid waste by-product from the aluminum industry, as an economical adsorbent for the removal of commercial reactive dyes from industrial wastewater. The robustness of the employed Box-Behnken design is evidenced by the high determination coefficient (0.997) and correlation coefficient (0.994) values. The optimum acid activation condition was determined to be 385 K activation temperature, 91 min activation time, and 2.5 N HCl acid concentration, resulting in a 99.24 ± 0.04 % removal efficiency for reactive dyes. Analysis of X-ray Diffraction and X-ray Fluorescence data revealed that the activation process significantly increased the composition of Al and Fe compounds. This enhancement was achieved by eliminating compounds that block active sites and improves the overall surface area from 37.35 m2/g to 173.81 m2/g. Detailed morphological analysis, conducted through high-resolution transmission electron microscopy and scanning electron microscopy, reveals profound transformation in the surface structure. The study primarily focuses on removing four commercial reactive dyes: Reactive Blue 2 (RBL-2), Reactive Black 5 (RBK-5), Reactive Red 24 (RR-24), and Reactive Yellow 15 (RY-15). These dyes demonstrate maximum adsorption capacities of 118.24 mg/g, 121.02 mg/g, 129.19 mg/g, and 142.64 mg/g, respectively. In order to comprehend the interactions between dye molecules and the adsorbent, a first principle based model was employed to simulate the adsorption kinetics.

Structure and Electrochemical Characterization of Nd0.5Ba0.5Zr0.8Fe0.2O3+δ Cobalt-Free Cathode Material for Intermediate-Temperature Solid Oxide Fuel Cells: An Experimental Investigation

Compared to other energy-generating technologies and energy conversion devices, intermediate-temperature solid oxide fuel cells (IT-SOFCs) have gained significant attention from energy experts due to its high energy density, moderate operating temperature (600 – 800 ℃), low emissions, and reliability. Enhancing the performance of IT-SOFCs requires suitable and excellent cathode materials. Thus, a perovskite-type Nd0.5Ba0.5Zr0.8Fe0.2O3+δ (NBZFO) material was synthesised via traditional solid-state reaction technique and analysed as a potential cathode material for IT-SOFCs. Analysis of x-ray diffraction data (XRD) revealed a single-phase perovskite material that crystallises in cubic space group (pm-3m). The thermal and electrochemical properties were analysed with the aid of thermogravimetric analysis (TGA) and electrochemical impedance spectroscopy (EIS). NBZFO has an electrical conductivity in air of 80 S/cm at 400 ℃, and a polarization resistance (PR) of 0.106 Ω∙cm2 at 800 ℃. TGA analysis reveals a slight loss in weight of about 0.58%, thereby suggesting a highly stable cathode material for IT-SOFC. Electrochemical investigation shows that NBZFO has good electronic and ionic conductivity and excellent oxygen stichometry. Further studies are required to understand the effects of varying B-site composition of the cathode material.

Resilience of the Aurivillius structure upon La and Cr doping in a Bi5Ti3FeO15 multiferroic.

Combining the experimental techniques of high-resolution X-ray diffraction, magnetometry, specific heat measurement, and X-ray photoelectron, Raman and dielectric spectroscopy techniques, we have studied the influence of La and Cr doping on the crystal structure and magnetism of the room temperature Aurivillius multiferroic Bi5Ti3FeO15 by investigating the physical properties of (Bi4La)Ti3FeO15 and Bi5Ti3 (Fe0.5Cr0.5)O15. The parent (Bi5Ti3FeO15) and the doped ((Bi4La)Ti3FeO15 and Bi5Ti3(Fe0.5Cr0.5)O15) compounds crystallize in the A21am space group, which is confirmed through our analysis of high-resolution synchrotron X-ray diffraction data obtained on phase-pure polycrystalline powders. We determined the oxidation states of the metal atoms in the studied compounds as Fe3+, Ti4+, Cr3+, and La3+ through the analysis of X-ray photoelectron spectroscopy data. The magnetic susceptibilities of the three compounds are marked by the absence of a long-range ordered ground state, but dominated by superparamagnetic clusters with dominant antiferromagnetic interactions. This signature of short-range magnetism is also seen in specific heat as a low temperature enhancement which is suppressed upon the application of external magnetic fields up to 8 T. Our dielectric spectroscopy experiments showed that the three studied compounds display similar features in the dielectric constant measured as a function of frequency. However, upon doping La at the Bi site, the width of the ferroelectric hysteresis loop increases for (Bi4La)Ti3FeO15 compared to that of the parent compound Bi5Ti3FeO15, and with Cr doping, Bi5Ti3(Fe0.5Cr0.5)O15 becomes a leaky dielectric. The resilience of the Aurivillius crystal structure towards doping of La at the Bi site and Cr at the Fe site is clearly seen in the bulk properties of magnetic susceptibility, specific heat and the average crystal structure. The relevance of changes in the local structure is evident from our Raman spectroscopy and X-ray pair distribution function studies.

Deriving kinetic insights from mechanochemically synthesized compounds using multivariate analysis (MCR-ALS) of powder X-ray diffraction data

Application of MCR-ALS method on PXRD data from ex situ and in situ experiments, to study the kinetics of the co-crystallization of theophylline and malonic acid via mechanochemistry.

Selective adsorption of fluorinated super greenhouse gases within a metal-organic framework with dynamic corrugated ultramicropores.

Perfluorocompound (PFC) gases play vital roles in microelectronics processing. Requirements for ultra-high purities traditionally necessitate use of virgin sources and thereby hinder the capture, purification, and reuse of these costly gases. Most importantly, gaseous PFCs are incredibly potent greenhouse gases with atmospheric lifetimes on the order of 103-104 years, and thus any environmental emissions have an outsized and prolonged impact on our climate. The development of sorbents that can capture PFC gases from industrial waste streams has lagged substantially behind the progress made over the last decade in capturing CO2 from both point emission sources and directly from air. Herein, we show that the metal-organic framework Zn(fba) (fba2- = 4,4'-(hexafluoroisopropylidene)bis-benzoate) displays an equilibrium selectivity for CF4 adsorption over N2 that surpasses those of all water-stable sorbents that have been reported for this separation. Selective adsorption of both CHF3 and CH4 over N2 is also evident, demonstrating a general preference for tetrahedral C1 gases. This selectivity is enabled by adsorption within narrow corrugated channels lined with ligand-based aryl rings, a site within this material that has not previously been realized as being accessible to guests. Analyses of adsorption kinetics and X-ray diffraction data are used to characterize sorption and diffusion of small adsorbates within these channels and strongly implicate rotation of the linker aryl rings as a gate that modulates transport of the C1 gases through a crystallite. Multi-component breakthrough measurements demonstrate that Zn(fba) is able to resolve mixtures of CF4 and N2 under flow-through conditions. Taken together, this work illuminates the dynamic structure of Zn(fba), and also points toward general design principles that can enable large CF4 selectivities in sorbents with more favorable kinetic profiles.

Synthesis, crystal structure and investigation of ion-exchange possibility for sodium tellurate NaTeO3(OH).

A new sodium tellurate has been hydrothermally synthesized and comprehensively analysed using spectroscopic and thermogravimetric techniques, resulting in the determination of its composition as NaTeO3(OH). The analysis of synchrotron X-ray and neutron diffraction data indicates that NaTeO3(OH) has a crystal structure similar to that of the previously reported tellurate, KTeO3(OH), with the space group P21/a (No. 14). NaTeO3(OH) consists of zigzag one-dimensional chains built by edge-sharing TeO6 octahedra, running parallel to the c-axis and connected to sodium and hydrogen atoms. The hydrogen atoms covalently bond to the terminal oxygen atoms on the one-dimensional chain and also form hydrogen bonds with other terminal oxygen atoms on nearby chains. The structure has been confirmed by optimization using the pseudopotential method and performing Bond Valence Sum (BVS) analysis. Although Li+ ions in LiTeO3(OH) can be exchanged reversibly with H+ ions, no ion exchange behaviour is observed in NaTeO3(OH). The difference is attributed to the size of the alkali ions and their crystal structure.

Insights into non-covalent interactions in dicopper(II,II) complexes bearing a naphthyridine scaffold: anion-dictated electrochemistry.

A family of bis(μ-hydroxido)dicopper(II,II) complexes bearing a naphthyridine-based scaffold has been synthesized and characterized. Cyclic voltammetry reveals that the nature of the anions present in the complexes plays a pivotal role in their electrochemical properties. X-ray diffraction, spectroscopic and electrochemical analysis data support the formation of intimate ion pairs by non-covalent interactions driving to a ca. 270 mV difference for the potential required to monooxidize the CuIICuII species.