X-ray Diffraction Studies Research Articles

Intramolecular Charge Transfer and Stimuli-Responsive Emission in Cholesterol-Appended Phenothiazine-Cyanostyryl-Based Donor-Acceptor Systems.

Organic fluorescent molecules have received considerable attention owing to their various optoelectronic applications. Herein, we report the design and synthesis of two cholesterol-functionalized cyanostyrene-phenothiazine-based D-π-A systems that are emissive in both the solution and solid states. The newly synthesized cholesterol-appended phenothiazine-cyanostyrene diads PTCS-1 and PTCS-2 vary in the N-alkylation of phenothiazine, respectively, with─octyl and─hexyl chains. Both molecules are highly fluorescent and show reasonably good quantum yields in nonpolar solvents because of twisted intramolecular charge transfer (TICT). The molecules exhibit aggregation-induced emission in the solid state. Due to the presence of flexible alkyl chains in the phenothiazine and cholesterol moieties, PTCS-1 and PTCS-2 show mechanochromic luminescence switching in response to external shear stress and emission recovery under methanol vapor. Powder X-ray diffraction studies prove that the emission switching on the applied stimuli in both PTCS-1 and PTCS-2 is attributed to the reversible transformation between the crystalline and amorphous states. Time-dependent density functional theory (TD-DFT) studies are carried out to gain insight into the ICT interactions. TD-DFT analysis at the TD-M06-2X/def2-TZVP level further revealed that in both molecules, the lowest unoccupied molecular orbital (LUMO) + 2, LUMO, highest occupied molecular orbital (HOMO), and HOMO - 1 orbitals are responsible for the charge transfer interactions. These ICT interactions are identified as π-π* type interactions.

Work hardening and X-ray diffraction studies on ASS 304 at high temperatures

Abstract One of the most common characteristics of metallic alloys is work hardening, which is most beneficial as it is the primary reason for the alloys’ tenacity to withstand loading even in the presence of internal flaws or geometrical errors. Thus, the work hardening coefficient gives the maximum amount of homogeneous plastic deformation in tensile straining. Thus, complex-forming operations are facilitated by a high coefficient without experiencing premature failure. Naturally, work hardening has a significant impact on the mechanical energy required to shape a material by plastic deformation, such as rolling, forming, etc. The quantity of energy that the material stores during plastic deformation is also managed by work hardening. As a result, it significantly influences how the metal behaves when it is subsequently softened during annealing. Finally, the hardening capacity and durability of the work hardened state are significant practical challenges because many high-volume stretch formed components are directly used. Typically, the current study begins, at homologous temperatures above 0.4 times melting point, with a description of work hardening at 700, 800, and 900°C temperatures in three different orientations with respect to rolling direction R 0, R 45, and R 90 and 10−1−10−3 s−1 strain rates, where thermally triggered processes exhibit a prominent role in work hardening. Three stages of behavior were identified by analyzing the tensile work hardening of ASS 304 steel. Dynamic strain aging is the cause of the anomalous fluctuation in the work hardening rate that is seen in hot working temperatures. X-ray diffraction examination is conducted to introspect any phase changes occurring in hot working regions improving plasticity of ASS 304.

Interactions of Brominated Flame Retardants with Membrane Models of Dehalogenating Bacteria: Langmuir Monolayer and Grazing Incidence X-ray Diffraction Studies.

Brominated flame retardants (BFRs) are small organic molecules containing several bromine substituents added to plastics to limit their flammability. BFRs can constitute up to 30% of the weight of some plastics, which is why they are produced in large quantities. Along with plastic waste and microplastic particles, BFRs end up in the soil and can easily leach causing contamination. As polyhalogenated molecules, multiple BFRs were classified as persistent organic pollutants (POPs), meaning that their biodegradation in the soils is especially challenging. However, some anaerobic bacteria as Dehaloccocoides can dehalogenate BFRs, which is important in the bioremediation of contaminated soils. BFRs are hydrophobic, can accumulate in plasma membranes, and disturb their function. On the other hand, limited membrane accumulation is necessary for BFR dehalogenation. To study the BFR-membrane interaction, we created membrane models of soil dehalogenating bacteria and tested their interactions with seven legacy and novel BFRs most common in soils. Phospholipid Langmuir monolayers with appropriate composition were used as membrane models. These membranes were doped in the selected BFRs, and the incorporation of BFR molecules into the phospholipid matrix and also the effects of BFR presence on membrane physical properties and morphology were studied. It turned out that the seven BFRs differed significantly in their membrane affinity. For some, the incorporation was very limited, and others incorporated effectively and could affect membrane properties, while one of the tested molecules induced the formation of bilayer domains in the membranes. Thus, Langmuir monolayers can be effectively used for pretesting BFR membrane activity.

Discovery of a New Polymorph of 5-Methoxy-1H-Indole-2-Carboxylic Acid: Characterization by X-Ray Diffraction, Infrared Spectroscopy, and DFT Calculations

This study presents a new 5-methoxy-1H-indole-2-carboxylic acid (MI2CA) polymorph investigated by single-crystal X-ray diffraction, infrared spectroscopy, and density functional theory (ωB97X-D) calculations employing two basis sets (6-31++G(d,p) and aug-cc-pVTZ). The compound crystallizes in the monoclinic system, space group P21/c (a = 4.0305(2) Å, b = 13.0346(6) Å, c = 17.2042(9) Å, β = 91.871(5)°, Z = 4). In the crystalline structure, the formation of cyclic dimers via double hydrogen bonds O−H⋯O between MI2CA molecules was observed. Interactions between the NH groups of the indole rings and the adjacent methoxy groups, as well as C–H⋯O contacts, significantly influence the spatial arrangement of molecules. The results from DFT calculations, including dimeric and trimeric structures, agree well with the experimental structural and spectroscopic data. Analysis of the infrared spectra confirms the conclusions drawn from X-ray diffraction studies and reveals differences between the IR spectra of the newly obtained polymorph and that reported earlier in the literature. This comprehensive study sheds some light on the MI2CA polymorphism and is important for a potential pharmacological applications of this compound.

A tetrahedral neptunium(V) complex.

Neptunium is an actinide element sourced from anthropogenic production, and, unlike naturally abundant uranium, its coordination chemistry is not well developed in all accessible oxidation states. High-valent neptunium generally requires stabilization from at least one metal-ligand multiple bond, and departing from this structural motif poses a considerable challenge. Here we report a tetrahedral molecular neptunium(V) complex ([Np5+(NPC)4][B(ArF5)4], 1-Np) (NPC = [NPtBu(pyrr)2]-; tBu = C(CH3)3; pyrr = pyrrolidinyl (N(C2H4)2); B(ArF5)4 = tetrakis(2,3,4,5,6-pentafluourophenyl)borate). Single-crystal X-ray diffraction, solution-state spectroscopy and density functional theory studies of 1-Np and the product of its proton-coupled electron transfer (PCET) reaction, 2-Np, demonstrate the unique bonding that stabilizes this reactive ion and establishes the thermochemical and kinetic parameters of PCET in a condensed-phase transuranic complex. The isolation of this four-coordinate, neptunium(V) complex reveals a fundamental reaction pathway in transuranic chemistry.

Thermoelectric and photovoltaic properties of 12-BaBi2S4

In this report, we have investigated the structure and properties of the 12-BaBi2S4. A single crystal X-ray diffraction study shows that the 12-BaBi2S4 crystallizes in the hexagonal crystal system (space group = P63/m) with refined lattice parameters of a = b = 25.2687(10) Å, c = 4.1859(2) Å, and formula unit = Z = 12 at room temperature. The structure contains fifteen crystallographic independent sites, including three Ba, four Bi, and eight types of S atoms. A phase pure polycrystalline sample of 12-BaBi2S4 was synthesized by heating stoichiometric amounts of BaCO3 and Bi2O3 under a CS2 atmosphere. The phase pure sample is found to be a semiconductor with a direct bandgap of 1.3(1) eV. The polycrystalline 12-BaBi2S4 exhibits ultra-low thermal conductivity values, varying from 0.47 Wm−1K−1 at 323 K to 0.43 Wm−1K−1 at 773 K. The sample shows high values of the Seebeck coefficient (S = −300 μV/K to −210 μV/K) in the 323 K–773 K range with poor electrical conductivity values. The negative sign of the S implies that the sample is a n-type semiconductor. DFT studies of the 12-BaBi2S4 also predict semiconducting properties. We have explored the 12-BaBi2S4 sample for photovoltaic (PV) applications by fabricating a liquid junction solar cell, TiO2/CdS/12-BaBi2S4/Sn2−/S2−/MWCNTs@Ni, which delivered an efficiency enhanced by ∼12 % to the control cell based on sole CdS as the photo-sensitizer. Theoretical electronic structure calculations suggest the semiconducting nature of the 12-BaBi2S4 in agreement with the optical absorption and electrical resistivity studies.

1,2,3-Triazole-containing azamacrocycles from chiral triazolopeptoids: synthesis and solid-state studies.

Two new chiral 1,2,3-triazole-containing macrocyclic oligoamides (i.e.: triazolopeptoid 4 and 5) were obtained through solid-phase synthesis of linear precursors followed by high dilution macrocyclization reaction. Theoretical (DFT) and spectroscopic (NMR) studies revealed the intricate interplay between the Na-chiral side chains and their conformational attitudes. BH3-mediated reduction of the tertiary amide groups of known 1-3 and newly synthesized 4 gave novel azamacrocycles 6-9. Detection of borane complexes of azamacrocycles 6 and 9 (i.e.: 10 and 11), corroborated by X-ray diffraction studies, demonstrated the peculiar properties of 1,2,3-triazole-containing macrorings.

Deep eutectic solvent-assisted synthesis of transition metal oxide and its integration into polymer matrix for supercapacitor

Transition metal oxide-based materials continue to attract interest in energy and environmental applications due to their unique characteristics. However, their integration with polymers needs to be explored to achieve enhanced capacitance values. To address this issue, two step strategy is utilized wherein the first step involves preparation of a pristine transition metal oxide (Co3O4) by a deep eutectic solvent (DES) consisting of choline chloride and hydrogen donor ethyelene glycol in the ratio of 2:1. In the second step the environmentally friendly high energy ball milling is utilized with strong mechanical forces producing desired poly-3-dodecyl thiophene (P3DDT)-wrapped cobalt oxide (Co3O4). The structural and morphological properties of the prepared Co3O4 and its composite (P3DDT-Co3O4) are determined by aid of X-ray diffraction (XRD) studies, Field emission scanning electron microscope (FESEM), and X-ray photoelectron spectroscopy (XPS). The synthesized Co3O4 exhibited petal-like morphology, whereas in P3DDT-Co3O4 the polymer appears to be completely wrapped on transition metal oxide. The electrochemical characteristics of electrodes were studied. The P3DDT-Co3O4 exhibited higher specific capacitance (294F/g) than pristine Co3O4 (174F/g) at a current density of 1 A/g and its retention capacity increased (96%) and then decreased (93%) over 5000 cycles in a three-electrode cell assembly. The lowest capacitance (136F/g) was obtained for P3DDT. Experimental results demonstrate that the design is suitable for upgrading favorably active electrochemical spots in Co3O4 during the incorporation of P3DDT by the ball-milling procedure, showing outstanding performance in energy-storage applications.

Mercaptoethanol-assisted synthesis of sulfonic acid-functionalized polysiloxanes as inorganic fillers in composite membranes for energy-storage applications

Developing proton-exchange membranes (PEMs) for energy applications is necessary for fulfilling the increasing energy demand without environmental effects. In this study, we prepared composite membranes containing mercaptoethanol-assisted sulfonic acid-functionalized polysiloxanes (MASFPs) and perfluorinated sulfonic acid (PFSA). The MASFP-containing composite membrane (i.e., CMASFP-2) exhibited better membrane properties than the composite membrane prepared without mercaptoethanol (CMASFP-1) and the reference Nafion 212 membrane. Wide-angle X-ray diffraction (XRD) studies revealed a broad peak at 2θ = 17.4° and 39°, indicating that the composite membranes are semicrystalline. Scanning electron microscopy (SEM) analysis revealed that the prepared composite membranes had good morphology, whereas energy-dispersive X-ray spectroscopy analysis revealed that it had siloxane and more sulfonic acid than the pristine PFSA membrane. Thermogravimetric and mechanical strength analyses revealed that incorporating sulfonic acid-functionalized siloxanes improved the thermal stability and mechanical strain of the membrane. The prepared CMASFP-2 membrane had a high ionic conductivity of 0.106 mS cm−1 and an ion-exchange capacity of 1.09 meq·g−1. CMASFP-2 also exhibited lower hydrogen gas permeability than the Nafion 212 and PFSA membranes, demonstrating that it can be used for energy applications.

Structural, optical and photoluminescence characteristics of apatite type lanthanide silicates

This article reports the solid state synthesis of apatite type rare earth-transition metal silicates Nd4MnSi3O13 and Sm4MnSi3O13. These oxyapatite type lanthanide silicates were characterized through structural, micro structural, optical and photoluminescence properties. The indexed X-ray diffraction patterns and Raman analysis confirm that both the samples crystallize in single phase hexagonal symmetry with space group P63/m. Transmission electron microscopy images along with electron diffraction pattern indicate the good crystalline nature of both the samples which further support the results obtained from X-ray diffraction study. The optical band gap energies are found to be 4.1 eV and 3.9 eV for Nd4MnSi3O13 and Sm4MnSi3O13 respectively. The wide optical band gap values of these semiconductor silicates make enable them for fundamental and technological applications. The luminescent properties and CIE coordinates showed the green-yellow emission of these synthesized silicates which further indicate that these compounds may have uses in solid state lighting because of the tunable luminescence.

Effect of hetero-valence ions on structural and electrical properties of La2Ni(Mn0.5Ti0.5)O6 ceramics

The study of powder X-ray diffraction of La2Ni(Mn0.5Ti0.5)O6 (0.5LNMT) confirms a multi-phasic composition. The monoclinic P21/n phase content dominates. Occurrence of minor rhombohedral R3‾c phase and precipitates of MnO2 and La2MnO4 were detected. The morphology was analyzed using a SEM test and ceramics showed a porous structure and variation in the grain size below 4 μm. Dielectric permittivity of marked magnitude varies from ∼30 to ∼100 000 when temperature increases. Dielectric loss coefficient frequency dependence exhibits well-defined dielectric relaxation peaks, which were found to obey the Arrhenius law with the activation energy of 0.29 eV, below the presumed phase transition. Two sets of relaxation peaks in the imaginary part of electric modulus spectra relate to relaxations of different activation energies of 0.28 eV and 0.38 eV. An optical gap magnitude of 0.8 eV was determined from the diffuse reflectance spectrum in the Vis-NIR range. It compares with the band gap estimated from the X-ray photoelectron spectroscopy test. We also compare the influence of doping ions on the crystal lattice of the surface and the bulk ceramics. Electrical conductivity relaxation processes were attributed to the electron hopping mechanism between multi-valence Mnk+ and Nin+ ions’ states, which were determined from XPS analysis. The dc resistivity shows thermally generated dependence. Activation energy Edc magnitude varies between 0.27 and 0.37 eV which indicates the occurrence of defects and structural disorder. Such disorder correlates to the variable range hopping of small polarons involved in electrical conductivity. The density of states near Fermi energy was estimated N(EF) = 2.1 × 1025 eV−1 m−3. The 0.5LNMT application prospects were discussed.

Electrolytic Performance of Sodium Alginate-Poly Vinyl Alcohol Matrix with Ammonium Bromide for Proton Conduction: Applications in Electrochemical Systems

Polymer blend electrolytes based on poly(vinyl alcohol) (PVA) and sodium alginate (NaAlg) were prepared using the solution casting method. These electrolytes were doped with varying amounts of ammonium bromide (NH4Br). The compatibility of NH4Br with PVA:NaAlg polymers was examined through X-ray diffraction (XRD) and Fourier-transform infrared (FTIR) studies. The FTIR assessment confirmed the formation of a complex between PVA:NaAlg and the added salt, as evidenced by modifications and reductions in the intensity of FTIR bands related to functional groups. The conductivity and dielectric behavior of the samples were analyzed using AC impedance spectroscopy. The sample with 20wt.% of added salt exhibited a higher ionic conductivity of 1.661×10-5 Scm-1. Activation energy and relaxation time were estimated, and dielectric studies revealed a non-Debye nature. The conduction mechanism was best described by the correlated overlapping large polaron tunneling model (OLPT). The highest conducting sample was found to be suitable for electrochemical devices, as demonstrated by transference number (TNM), cyclic volumetric (CV), and linear sweep voltammetry (LSV) analyses. This high-conductivity sample can be employed in electrochemical devices such as EDLC. The cyclic voltammetry (CV) curve exhibited a nearly rectangular shape with non-faradaic peaks. GCD(Galvanostatic charge-discharge) analysis yielded specific capacitance, power density, and energy density values of 125.01 Fg-1, 1037 WKg-1, and 14.06 WhKg-1 respectively. These results indicate that polymer electrolytes show great promise as electrolytes in proton-conducting electrochemical devices.

Lithium(I), Cesium(I), Barium(II) and Cadmium (II) [2-(2,6-dichlorophenylamino)phenyl]acetate (diclofenac) complexes and coordination polymers

Two new lithium complexes and three coordination polymers with cesium, barium, and cadmium having deprotonated diclofenac acid (HDFA) ligand are reported. All these non-ionic complexes or the coordination polymers were characterized by single crystal X-ray diffraction, IR and thermal studies. The lithium-diclofenac complexes, [Li(DFA)(H2O)3] and [Li(DFA)(H2O)2(DMF)] were respectively obtained from reaction carried out in aqueous ethanol or dimethylformamide as solvent. Each formed hydrogen bonded 2D-sheets, which were further assembled into 3D-layers by involving edge-on Cl-π interactions. The respective average particle sizes determined by dynamic light scattering of the respective lithium complexes were 648.3 nm and 588.8 nm. The average particle size of the tri-aquated complex dissolved in water was decreased upon addition of dimethylformamide. The cesium coordination polymer [Cs(DFA)(μ-H2O)2]n had two-dimensional sheets formed through dative bonds. The hydrophobic parts of the sheets were projecting outward and two alternative sheets were inter-linked by edge-on chlorine-π interactions (3.391 Å) to provide 3-D supramolecular layered structure. One dimensional barium coordination polymer [Ba(DFA)2(H2O)4]n and a cadmium coordination polymer [{Cd(DMF)4}2+{Cd(DFA)4}2−]n having linear-chain structure were reported. The linear chain of the cadmium coordination polymer was comprised of the coordinatively linked assembly of complex cation [Cd(DMF)4]2+ with anion [Cd(DFA)4]2− located at alternative positions by side-on carboxylate bridges.

Strategic Ni integration to study its impact on the photoluminescence and photocatalytic performances of SnO2 nanorod architecture

The sol-gel process was utilized to fabricate SnO2 nanoparticles, both in their pure form and with the addition of Ni dopants. The nanoparticles obtained were further examined to ascertain the characteristics associated with their structure, alterations in band gap, and photocatalytic performance. The insertion of nickel ions into tin sites hinders the formation of grain growth in tin oxide. The variation in the valence states and ionic radius of Sn4+ and Ni2+ ions, as revealed by X-ray diffraction (XRD) study, accounts for this disparity. FTIR measurements indicate the existence of stretching vibrations of metal-oxygen bonds that include Ni ions in the doped samples. The photoluminescence (PL) analysis reveals that the introduction of nickel doping alters the band structure of SnO2, leading to the creation of additional defect states, such as oxygen vacancies inside the crystal lattice. A study was undertaken to investigate the photocatalytic (PC) activity of SnO2 in the presence of Ni dopants. The results revealed a noticeable improvement in the efficiency of photodegradation. The degradation of Congo red (CR) dye using Ni-SnO2 nanocrystals achieves an efficiency of 94.88 % within a duration of 180 minutes. An analysis has been conducted on the impact of dye content, photocatalyst dosage, and pH on the degradation efficiency. As per the study, lower dose of Ni-SnO2 has shown better degradation efficiency in comparison to other studies. The improved performance of Ni-SnO2 can be ascribed to two main factors: the inhibition of carrier recombination due to the inclusion of defective states, and the production of hydroxyl radicals (OH•). The stability and reusability of these photocatalysts have been noted in their efficient application for environmental remediation.

Square-planar nickel/copper(II) complexes of (E)-2-(((2-ethylphenyl)imino) (phenyl) methyl)phenol: Supramolecular analysis, keto-enol tautomerism, polymorphism and antibacterial activities

A new Schiff base proligand, (E)-2-(((2-ethylphenyl)imino)(phenyl)methyl)phenol (HL), was synthesized from 2-hydroxybenzophenone and 2-ethylaniline and its coordination chemistry with nickel(II) and copper(II) acetate explored. In solution, the proligand HL undergoes ketoimine -enolimine tautomerism which settles exclusively into an enolimine form in the solid-state. Interestingly, while a single crystalline habit was obtained for the nickel complex 1 (block-shaped single crystals), the copper species 2 was found to solidify in two detectable polymorphs: block-shaped crystals (2a, monoclinic space group P21/c) and rhombic crystals (2b, triclinic space group P-1). Single-crystal X-ray diffraction studies reveal that the N,O Schiff base ligand chelates the divalent metal ions with square-planar geometry in the isostructural 1 and 2a and in a distorted square-planar geometry with a dihedral chelate-plane angle of 27.9° in 2b. The copper complex 2 exhibits significant antibacterial activity against the E. coli and medium activity against S. aureus bacteria. The physical properties of the complexes were further probed using thermal techniques, while their electronic structure was investigated by electrochemistry and electronic absorption spectroscopy.

Novel cobalt-incorporated two dimensional covalent organic frameworks for supercapacitor applications

Covalent-organic frameworks (COFs), are a promising new class of crystalline porous organic materials with confined structures either in 2D or 3D domains. The current study focuses on using a solvothermal approach consisting of sealed pyrex tubes to synthesize two-dimensional TBP-COF and TBP-COF that have been doped with cobalt (Co) (TBP-Co@COF). The results of the experimentally acquired X-ray diffraction study were compared with those from simulations, and it was discovered that both are in good agreement. A thorough theoretical analysis of the layer packing in AA stacking (P1) and AB stacking (P1) modes using the Materials Studio revealed that AA stacking is more stable than the AB stacking (P1) structure. The formation of imine linkage and incorporation of Co into the COF are indicated by the result of XPS. Unaggregated dispersion of Co particles can be seen on the square and rectangular sheets of TBP-COF in TEM and SEM images. Both materials are fabricated as electrode materials and evaluated for their supercapacitor applications. The TBP-Co@COF shows an enhanced specific capacitance (CSp) of 975F/g compared to the TBP-COF (827F/g) at 2 mV/s scan rate. TBP-Co@COF exhibit an energy density (ED) of 69 Wh/kg even at a high power density (PD) of 75000 W/kg and also retains 79 % of its initial capacitance up to 2000 cycles. TBP-COF and TBP-Co@COF were fabricated for an asymmetric supercapacitor device (ASD) and found to exhibit a CSp of 191F/g at a scan rate of 2 mV/s.

Self-powered photodetector based on 1D TiO2-3D CdS mixed dimensional heterostructure fabricated at low temperature

Solution processed photodetectors have garnered great attention in applications such as, machine vision perception, neuromorphic computing and opto-electronic memory storage. Though, such photodetectors offer several advantages such as ease of fabrication, high scalability, low thermal budget and low-cost processing, multi-modal functionality etc. however, they suffer from the major drawback of inferior device performance −as low responsivity and slow rise time, particularly due to the intrinsic poor crystallinity of the photoactive material. In this work, we demonstrate a solution processed photodetector with impressive performance at comparatively low processing temperatures (<150 °C) based on the mixed dimensional heterostructure configuration of 1D TiO2 nanorods and 3D CdS nanoflowers. TiO2 nanorods have been synthesized by hydrothermal technique, whereas their CdS sensitization is done by chemical bath deposition. Low cost carbon paste is used as electrode instead of conventional non-economic noble metal electrodes. X-ray diffraction studies validated excellent crystallinity of the photoactive material even under low temperature processing condition. The type-II Heterojunction (TiO2 and CdS) configuration photodetector shows efficient response at zero bias, thus yielding a self-powered device. The detector shows response in UV and visible region, with excellent responsivity of 110 mA/W (5 V), 563 µA/W (0 V) and a quicker rise time of 81 ms. Albeit the simple fabrication scheme and low processing temperatures, the detector exhibited promising figures-of-merit, which aids in fabrication of novel solution processed photodetectors.

Influence of pH on Growth, Structural, Thermal, Linear and Nonlinear Optical Properties of L-Asparagine Monohydrate Single Crystal

This report present investigation on influence of pH on growth, structural, thermal, linear and nonlinear optical properties of L-asparagine monohydrate (LAM) single crystal for first time. Single crystals of LAM were grown at different pH by solution growth method by allowing slow evaporation of solvent. Crystal grown at pH 6.4 grows slowly as compare to other crystals grown at other pH values. The slight variation in lattice parameters of grown crystals has been confirmed by powder X-ray diffraction study. FT-IR study confirms the presence of functional groups of LAM in all grown crystals. Influence of pH on optical quality of crystals has been discussed. The crystal grown at pH 5.4 has maximum optical transparency and shows 2 and 20 % more transmission than crystals grown at pH 4.4 and 6.4, respectively. Other optical parameters like cutoff wavelength (λmax), band gap (Eg), linear refractive index (n), reflectance, extinction coefficient (k), electrical susceptibility (χ), optical conductivity(σop), electrical conductivity (σel) and Urbach energy (Eu) of all crystals have been evaluated from transmission data. The LAM crystal grown at pH 6.4 show high values of third order nonlinear optical parameters,as compare to other grown crystals, that attest its suitability for applications like higher harmonic generation, optical switching, optical limiting and other photonic applications over other grown crystals. Thermal stability of the grown crystals has been attested by TG-DTA study.

Investigation of structural, morphological, dielectric, optical, and ferroelectric-energy storage properties of [(1-x) BCT-(x) BZT] electroceramics

Extensive research and advancements have been progressed by the vast potential of eco-friendly dielectric capacitors in high-level electronic elements and high-performance pulsed power systems thus far. Ferroelectric ceramic materials exhibiting relaxor properties and significant dielectric constants are prime candidates for attaining exceptional energy storage capabilities. Herein, a lead-free (1-x) Ba0.9Ca0.1TiO3–xBaZr0.15Ti0.85O3 (abbreviated as (1-x) BCT-xBZT) solid solution system has been synthesized via the conventional solid-state reaction technique, with varying levels of BZT doping. The X-ray diffraction study confirmed pure perovskite structure formation in the prepared ceramics, and the coexistence of orthorhombic (O) (space group- Amm2) and tetragonal (T) (space group-P4mm) phases has been detected through the Rietveld refinement technique at room temperature. Rietveld refinement data and associated analysis highlight the gradual shift of crystal symmetry from Amm2 to P4mm as the x content increases. Replacing BZT in Ca-modified BaTiO3 has led to significant enhancements in microstructural properties and an increase in the width of the optical band gap. This, in turn, enhances energy storage capabilities compared to pure BCT. Incorporating BZT into BCT has led to the evolution of relaxor ceramics, a crucial development for achieving elevated levels of recoverable energy storage density. In this study, the solid solution comprising 0.6BCT-0.4BZT exhibits distinct traits, including a diffuse phase transition, high breakdown strength, shallow dielectric loss (tanδ <0.007), and significantly high dielectric constant. Due to enhanced electrical characteristics, the 0.6BCT-0.4BZT possesses very high saturation polarization of ∼48 μCcm−2, a total energy density of 1.71 J/cm3, and a recoverable energy density of 1.1 J/cm3. In addition, the optimized ceramics demonstrate concurrent achievement of high-frequency stability (10–250 Hz), fatigue resistance (up to 104 cycles), and favorable temperature stability (20–160°C). This study showcased a potential material candidate suitable for energy storage devices functioning within low to medium-electric fields.

Enhancing the energy storage performance of titanium dioxide electrode material by green doping of Nd2O3 nanoparticles for electrochemical supercapacitors

Doping of sesquioxide alloy onto TiO2 nanomaterials was carried out in a novel green chemistry method using Corallo carpus epigaeus to fabricate the electrodes for pseudocapacitors. The conducted X-ray diffraction studies demonstrated the tetragonal phase of TiO2 and hexagonal phase of Nd2O3 nanomaterials. Morphological analysis revealed the irregular shape of TiO2 materials, each exceeding 100 nm in size, while Nd2O3 materials exhibited a spherical shape within the range of 10-20 nm. Electrochemical investigations unveiled a quasi-rectangular shape in cyclic voltammetric studies and a triangular shape in galvanostatic reactions, suggesting superior electrochemical performance of the electrodes. The doped electrodes exhibited a higher specific capacitance value (785.71 F/g) compared to pure TiO2 (707.14 F/g) at a current density of 1 A/g. These findings affirm the suitability of doped electrode materials for applications in electrical energy storage.