Powder Diffraction Research Articles

AMINO-GRAFTED MESOPOROUS SILICA NANOPARTICLES: ASSESSMENT OF NEUROMODULATORY, MEMBRANOTROPIC AND ANTIOXIDANT PROPERTIES IN CORTEX NERVE TERMINALS

Aim. In biomedical applications, silica nanoparticles are promising for controlled drug delivery. Also, from an environmental point of view, silica accounts for the most significant part of the mass of air pollution, particularly matter components, especially during sand dust storms. Methods. Amino-grafted mesoporous silica nanoparticles (MSN-NH2) were synthesized by means of co-condensation of tetraethoxysilane and 3-aminopropyltriethoxysilane and characterized using TEM, IR-spectroscopy, and powder X-ray diffraction. Neuromodulatory and related properties of MSN-NH2 were evaluated using rat cortex nerve terminals (synaptosomes). Results. MSN-NH2 did not influence the extracellular synaptosomal level of excitatory neurotransmitter L-[14C]glutamate and so did not cause excitotoxicity. In fluorescence measurements, MSN-NH2 depolarised the synaptosomal membrane and demonstrated weak antioxidant properties, decreasing the spontaneous generation of reactive oxygen species, whereas MSN-NH2 did not alter H2O2 in nerve terminals. The model of Cd2+/Pb2+/Hg2+-induced excitotoxicity was used to assess the capability of MSN-NH2 to adsorb xenobiotic heavy metals. MSN-NH2 did not modulate the Cd2+/Pb2+/Hg2+-induced increase in the extracellular synaptosomal level of L-[14C]glutamate. Conclusion. MSN-NH2 did not demonstrate excitotoxic signs, had weak antioxidant properties, and was biocompatible. MSN-NH2 did not mitigate the excitotoxic effects of xenobiotic heavy metals and did not adsorb these metals in biological systems.

Temperature-Dependent Formation of Carbon Nanodomains in Silicon Oxycarbide Glass-A Reactive Force Field MD Study.

Novel anode materials for lithium-ion batteries (LIBs) are constantly being explored to further improve battery performance. In this work, ReaxFF molecular dynamics (MD) simulations are performed to model the early stages in the synthesis of nanostructured silicon carbide (SiC), which is one such promising material. The focus lies on its precursor, silicon oxycarbide glass of composition (Si5O8C16) x (17 mol% Si, 28 mol% O, and 54 mol% C), in the following referred to as SiOC. The structure of the amorphous material is characterized via NPT MD simulations at temperatures ranging from 300 to 1000 K. To this end, a graph theoretical approach is employed to quantify the formation of segregated carbon nanodomains in the solid. Three algorithms for detecting nearest neighbors in the amorphous solid, a crucial prerequisite for the assembly of an atomic connectivity graph, are compared. It is shown that the temperature-dependent carbon aggregation follows an exponential trend, largely independent of the neighbor detection method. Also, the effects of variations in elemental composition are explored. Furthermore, the calculated powder X-ray diffraction patterns of the equilibrated silicon oxycarbide glasses are in good agreement with experimental measurements.

Ni9Sn2S2: An n-type metal-rich 2D sulfide with a metal-to-metal transition

Using spark plasma sintering, a ceramic sample of Ni9Sn2S2 sulfide was densified by starting from a powder synthesized in an evacuated ampoule. The powder x-ray diffraction refinements confirm the formation of the I4/mmm tetragonal Ni9Sn2S2 phase [a = b = 3.6809(2) Å and c = 25.5410(7) Å]. Transmission electron microscopy—imaging and coupled EDX—also reveals the formation of a secondary Ni6SnS2 phase and intergrowth defects in the layer stacking between the Ni9Sn2S2 and Ni6SnS2 phases. More importantly, the structural study demonstrates that Ni9Sn2S2 can be described as the n = 2 term of the generic series of compounds, namely, [Ni3S2][Ni3Sn]n. The Ni3Sn block is of the Cu3Au cubic form. The measurements of the physical properties show metallic behavior, with ρ300K = 0.135 mΩ cm, a residual resistivity ratio RRR = 2.2, and a Seebeck coefficient S300K = −23.5 μV K−1, indicating an n-type feature, the absolute value of which increases with T, as expected for a metal, to reach S650K = −30 μV K−1. This compound also exhibits a large thermal conductivity, κ300K = 8.0 W K−1 m−1, dominated by the electronic part. Interestingly, the small magnetic susceptibility with Pauli-like values shows two transitions at 200 and 125 K, with the first one coinciding to the metal-to-metal transition and to the change of slope in the S(T) curve, suggesting the occurrence of a charge density wave below 200 K. This is discussed in light of the recent developments in topological metals like Ni3In.

Electric polarization induced by low magnetic field in the W-type hexaferrite BaCoFe17O27 single crystal

Recently, the noncollinear magnetic structure with varying Co/Zn ratios was reported in the W-type hexaferrites using neutron powder diffraction. It is believed that these noncollinear spin orderings may stimulate magnetoelectric (ME) effect in the W-type hexaferrite. Herein, we present distinct evidence of ME response through systematic investigation on the magnetic and ferroelectric properties in BaCoFe17O27. Magnetization exhibits two different anomalies at TC1 ∼ 350 K and TC2 ∼ 150 K, indicating the formation of long-range longitudinal spin configurations and the spin reorientation transition, respectively. We have found that the low field-driven electric polarization has been observed under the ME poling condition of E ⊥ (H ⊥ c, and c). Spin current mechanism is mainly considered as the physics origin in its ME response, corresponding to the other hexaferrites as reported early. In addition, the weak electric polarization observed with E(⊥c)//H(⊥c) suggests that the p–d hybridization mechanism should also be contributed to the ME response in this compound. Therefore, BaCoFe17O27 presents an intrinsic magnetoelectric effect and provides a thought for people to seek and study the more single-phase ME compounds from the viewpoint of foundational and applications.

Development of a compact near-infrared lamp furnace for synchrotron powder diffraction and its application for in situ high-temperature observation of ferrite magnets

Development of a compact near-infrared lamp furnace for synchrotron powder diffraction and its application for <i>in situ</i> high-temperature observation of ferrite magnets

Synthesis and properties of 12442-family superconductor

We report a synthesis of two members of recently discovered high-temperature superconductors of 12442 family, with formula MCa2Fe4As4F2 (M=Rb,K) and transition temperatures of 32.7 and 34.6K, respectively. Quality of the samples was assessed using X-ray powder diffraction, superconducting transitions were identified through transport and magnetic experiments. The temperature dependence of the upper critical field and vortex activation energy was investigated under magnetic fields up to 19T. Two distinct thermally activated flux flow regimes were observed in both systems. Field dependences of activation energy U0(H) indicate a change in the properties of vortex matter in these regimes and distinctly different dissipation mechanisms, reminiscent of cuprate HTSC.

Surface Decoration of Cellulose With Trifluoromethylphenyl Substituted Thiourea: A Robust Hydrogen-Bonding Catalyst in Conjunction With L-Proline for the Asymmetric Direct Mannich Reaction.

Cellulose is one of the most abundant biopolymers in nature. Despite being the subject of research in various fields, it is not as famous as chitosan in catalyst design. Herein, a novel thiourea-functionalized cellulose (CTU-6) was synthesized as a robust hydrogen bonding catalyst with the degree of substitution (DS) of 0.84. CTU-6 was characterized using Fourier transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM), x-ray powder diffraction (XRD), proton nuclear magnetic resonance spectroscopy (1HNMR), solid-state cross-polarization magic angle spinning carbon-13 nuclear magnetic resonance (CP/MAS 13C-NMR), thermal gravimetric analysis (TGA) and elementel analysis. CTU-6 catalyzed the direct asymmetric Mannich reaction between acetone, aniline, and various aromatic aldehydes in cooperation with L-proline. The reaction exhibited excellent enantioselectivity, achieving up to 98% enantiomeric excess (ee) at room temperature. Incorporating trifluoromethylphenyl-substituted thiourea into the cellulose framework leverages its ability to form hydrogen bonds, thereby enabling precise control over the asymmetric induction. This study highlights the potential of cellulose-based catalysts in advancing asymmetric synthesis and their versatility in various organic reactions in cooperation with small chiral ligands. This synergy not only facilitates the efficient catalytic process but also improves the stereochemical outcomes of the reactions. This method underscores the importance of utilizing renewable and versatile cellulose materials in combination with chiral auxiliaries to achieve high levels of enantioselectivity.

Development and in vitro tuning of empagliflozin-containing dissolvable microneedle patch for enhanced transdermal delivery.

This painless method allows drugs to penetrate the outer skin layer, offering several advantages over alternative administration routes, including ease of use and the ability to bypass enterohepatic circulation. Among transdermal drug delivery systems (TDDS), microneedle patches (MNPs) are emerging as an innovative approach for minimally invasive drug delivery, enhancing the skin permeation of substances ranging from macro to micro sizes. This study explores dissolvable microneedle patches (dMNPs) as a novel method to improve the systemic delivery of empagliflozin, an SGLT-2 inhibitor, commonly used to manage type 2 diabetes mellitus (T2DM). However, its oral administration poses challenges due to rapid absorption, variable bioavailability, and a moderate half-life that necessitates frequent dosing. The microneedle patches were manufactured using a mold-based solvent casting technique, utilizing a polymer-drug combination that dissolves upon skin application. The development of the dMNPs involved polyvinylpyrrolidone and polyvinyl alcohol. Characterization of the formulated dMNPs included scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), powder X-ray diffraction (PXRD), dissolution testing, tensile strength analysis, percentage elongation measurement, mechanical strength assessment, and skin irritation studies. The optimized dMNP formulation (MP6) exhibited notable characteristics such as sharp, uniform, pyramid-shaped needles, stability at elevated temperatures, crystalline structures of the drug and polymers, controlled weight loss upon heating, effective drug dissolution, optimal tensile strength, penetration depth, moisture content, elongation capability, and a favorable release rate. In vitro release demonstrated the enhanced properties of the dissolvable microneedle patches, with zero-order kinetics identified as the most suitable model for MP6 based on regression coefficient analysis. Overall, the characterization studies, in vitro skin irritation evaluation, confirmed the stability and biocompatibility of the optimized dMNPs, making them suitable for transdermal application.

Synthesis Strategy Toward Minimizing Adventitious Oxygen Contents in the Mechanochemically Made Semiconductor Kesterite Cu2ZnSnS4 Nanopowders.

A multipronged approach to the refined mechanochemical synthesis of the semiconductor kesterite Cu2ZnSnS4 with minimal quantities of adventitious oxygen as well as to optimizing handling procedures from that angle is described. Three precursor systems are used to provide a pool of freshly made cubic prekesterite nanopowders with no semiconductor properties and the thermally annealed at 500 °C tetragonal kesterite nanopowders of the semiconductor. Based on the previously reported high propensity of such nanopowders to long-term deteriorating oxidation in ambient air, suitable modifications of all crucial synthesis steps are implemented, which are directed toward excluding or limiting the materials' exposure to air. The nanopowders are comprehensively characterized by powder XRD, FT-IR/Raman/UV-Vis spectroscopies, solid-state 65Cu/119Sn MAS NMR, TGA/DTA-QMS analysis, SEM, BET/BJH specific surface area, and helium density determinations, and, significantly, are directly analyzed for oxygen and hydrogen contents. The important finding is that following the anaerobic procedures and realistically minimizing the materials' exposure to air in certain manipulation steps results in the preparation of better oxidation-resistant nanopowders with a dramatic relative decrease in their oxygen content than previously reported. The adherence to the strict synthesis conditions that limit contact of the no-oxygen-containing kesterite nanopowders with ambient air is emphasized.

Systematic Investigations of the Solid Solution Zr(V1-xAlx)2 Adopting the Laves Phase Structures.

Laves phases are an interesting field of research when it comes to structural chemistry and physical properties. Investigations of the ternary system Zr-V-Al showed, in contrast to the system Hf-V-Al, that no superstructures can be observed within the solid solution Zr(V1-xAlx)2. High values of x form aluminum rich phases that adopt the hexagonal MgZn2 type structure while low values of x lead to vanadium rich phases that adopt the cubic MgCu2 type. All samples were investigated by powder X-ray diffraction experiments. Single crystal studies indicated that no superstructure formation is present in the investigated samples. 27Al MAS NMR investigations confirmed these findings. For ZrAl2, quantum-chemical calculations helped with the analysis of the 27Al NMR spectrum of the binary endmember of the solid solution. Some of the prepared samples were investigated with respect to their magnetic properties. The investigated compounds show Pauli-paramagnetism, in Zr(V0.875Al0.125)2 in addition superconductivity with a critical temperature of TC = 4.17(1) K was observed. Investigations of compositions that do not belong to the Laves phase regime clearly indicate that the MgZn2 type structure is still the dominant phase. Regardless of the starting composition chosen, the hexagonal Laves phase was mostly present.

Effect of Co-Solvents, Modified Starch and Physical Parameters on the Solubility and Release Rate of Cryptotanshinone from Alcohologels.

(1) Background: The aim of the work was to investigate the influence of selected physico-chemical factors on the solubility and release rate of CT (cryptotanshinone) in alcohologels. (2) Methods: The alcohologels of methylcellulose (MC), hydroksyethylcellulose (HEC), polyacrylic acid (PA) and polyacrylic acid crosspolymer (PACP) with CT were prepared and/or doped with native potato starch (SN) and modified citrate starches (SM2.5 and SM10). The analytical methods included evaluation of CT release profiles, Fourier transform infrared spectroscopy (ATR-FTIR), differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD) and electrospray ionization mass spectrometry (ESI-MS), and scanning electron microscope (SEM) images were performed. (3) Results: The release and decomposition kinetics of CT in relation to the phosphate buffer solution (PBS) and methanol were observed. The amount of cryptotanshinone (CT) released into PBS was significantly lower (2.5%) compared to its release into methanol, where 22.5% of the CT was released into the model medium. The addition of SM2.5 to the alcohologel significantly increased the CT content to 70% in the alcohologel preparation containing NaOH (40%), and this enhanced stability was maintained for up to two months. The ATR-FTIR exhibited interactions between PA and 2-amino-2-methyl-1,3-propanediol (AMPD) as well as between PA and NaOH in case of the alcohologels. Moreover, it indicated the interaction between CT and NaOH. PXRD diffractograms confirmed the FTIR study. (4) Conclusions: The study observed the influence of a number of factors on the solubility and release rate of CT, as: alkalizers and their concentration, SM2.5 addition. The transition of CT in the presence of NaOH to the tanshinone V sodium (T-V sodium) form was suspected.

Investigating a Seemingly Simple Imine-Linked Covalent Organic Framework Structure.

The structures of covalent organic frameworks (COFs) are typically determined through modeling based on powder X-ray diffraction. However, the intrinsically limited crystallinity of COFs often results in structural determinations of low fidelity. Here, we present real-space imaging of an extensively studied two-dimensional imine-based COF. Contrary to the conventional understanding that this COF features uniform hexagonal pores, our observations reveal the presence of two distinct sets of pores with differences in shape and size. Motivated by this finding, we conducted reciprocal-space characterizations, complemented by solid-state nuclear magnetic resonance spectroscopy and density functional theory calculations, to reevaluate this seemingly simple structure. The collective results allow for the establishment of a new structural model for this landmark COF and its derivatives, differing from the conventional model in both intra- and interlayer configurations. Furthermore, we identified various previously unrecognized defective structures through real-space imaging, which have significant implications for COF applications in separation and catalysis. Our study demonstrates the complexity and heterogeneity of COF structures, while also highlighting the imperative for structural reevaluation using advanced characterization techniques.

Ketoconazole-Fumaric Acid Pharmaceutical Cocrystal: From Formulation Design for Bioavailability Improvement to Biocompatibility Testing and Antifungal Efficacy Evaluation.

Development of cocrystals through crystal engineering is a viable strategy to formulate poorly water-soluble active pharmaceutical ingredients as stable crystalline solid forms with enhanced bioavailability. This study presents a controlled cocrystallization process by cooling for the 1:1 cocrystal of Ketoconazole, an antifungal class II drug with the Fumaric acid coformer. This was successfully set up following the meta-stable zone width determination in acetone-water 4:6 (V/V) and pure ethanol. Considering the optimal crystallization data, laboratory scale-up processes were carried out at 1 g batch size, efficiently delivering the cocrystal in high yields up to 90% pure and single phase as revealed by powder X-ray diffraction. Biological assays in vitro showed improved viability and oxidative damage of the cocrystal over Ketoconazole on human dermal fibroblasts and hepatocarcinoma cells; in vivo, on Wistar rats, the cocrystal increased oral Ketoconazole bioavailability with transient minor biochemical transaminases increases and without histological liver alterations. Locally on Balb C mice, it induced no epicutaneuous sensitization. A molecular docking study conducted on sterol 14α-demethylase (CYP51) enzyme from the pathogenic yeast Candida albicans revealed that the cocrystal interacts more efficiently with the enzyme compared to Ketoconazole, indicating that the coformer enhances the binding affinity of the active ingredient.

Co(II)-doped Cu(II)-Orotate coordination polymer composite: exploring their potential in photocatalytic and luminescence sensing applications

We synthesized a copper-based coordination polymer (Cu-CP), further enhanced by cobalt doping to create a Co@Cu-CP-2 composite, which demonstrates remarkable photocatalytic activity under visible light. Characterizations of Cu-CP and Co@Cu-CP-2 were conducted using powder X-ray diffraction (PXRD), FT-IR spectroscopy, SEM-EDAX, and elemental mapping analyses. The Co@Cu-CP-2 composite proved to be an exceptional multi-functional luminescent sensor, showcasing high sensitivity toward Ni2+ ions (93.00%), dichloromethane (DCM) (91.02%), and triethylamine (TEA) (87.35%). Additionally, we explored the recyclability and photocatalytic efficiency of Co@Cu-CP-2 in the degradation of various organic dyes under sunlight irradiation. The composite exhibited outstanding performance, achieving 86% degradation of Rose Bengal (RB), 80% for Crystal Red (CR), and 74.12% for Rhodamine 6 G (Rh-6G) in aqueous solutions.

Supramolecular Assembly, Solvent-Induced, and Mechanochromic Luminescence of Au(I) Quinoline-8-thiolates.

AuCl(PMe3) and AuCl(PEt3) were used to react with quinoline-8-thiolate (8-QNS) to give three Au(I) complexes, i.e., [8-QNS(AuPMe3)2]ClO4 (1), [(8-QNS)2Ag(AuPMe3)2]ClO4 (2), and [8-QNS(AuPEt3)2]ClO4 (3), which have been structurally determined by X-ray diffraction to show various intra- and intermolecular metal···metal contacts (i.e., metal = Au(I) or Ag(I)). All complexes displayed solid-state luminescence at 535-568 nm, which is most likely attributed to an intraligand transition of 8-QNS and/or a S → Au(I) charge-transfer transition, possibly modified by Au(I)···Au(I) interactions. Notably, complex 1·CH2Cl2 exhibited remarkable mechanochromic luminescence from 535 to 601 nm upon grinding. While immersed in various solvents for the ground powder samples of complex 1·CH2Cl2, the luminescence at 601 nm mostly reverted to the original luminescence. Powder X-ray diffraction measurements indicated that complex 1·CH2Cl2 underwent structural transformation from a crystalline to an amorphous phase upon grinding, and it can be restored to the original crystalline phase upon immersion in various solvents. Additionally, the reversible experiments of complex 1·CH2Cl2 for the grinding and immersion actions were performed for up to five cycles. Moreover, the time-dependent luminescence spectra for the crystalline samples of complex 1·CH2Cl2 were measured, and they showed a significant luminescence change from 535 to 590 nm within 2 days.

Uncoordinated Carboxyl Groups as Proton Sources in Polyoxometalate-Based Metal-Organic Frameworks Enhance Proton Conduction.

To select appropriate organic ligands is an effective strategy to enhance the proton conductivities of polyoxometalate-based metal-organic frameworks (POMOFs). Two new Dawson-type POMOFs, named CUST-961 and CUST-962, have been designed and synthesized via combining Htzbc selected by hard and soft acid and base theory and density functional theory calculation, transition metal ions, alkali metal ions (Na+ and K+), and Dawson-type polyoxometalates ([P2W18]6-) under the hydrothermal method. Their stabilities under different temperatures and relative humidities (RHs) have been investigated through powder X-ray diffraction and thermogravimetric analysis. Both CUST-961 and CUST-962 exhibited excellent aqueous and thermal stabilities. The alternating current (AC) impedance spectrum tests revealed that the proton conductivity of CUST-961 could reach 1.4 × 10-4 S cm-1 at 95 °C and 98% RH, which is about 3 times that of CUST-962. The different proton conductivities between the two compounds are due to the fact that CUST-961 possesses more uncoordinated carboxylic acid groups, as confirmed by attenuated total reflection infrared spectroscopy and 1H solid-state nuclear magnetic resonance spectroscopy, which can not only act as the proton source but also establish a richer hydrogen bonding network to enhance proton conduction. This work provides a new strategy and insight for the design and preparation of polyoxometalate-based proton conductive materials.

Phase Evolution of Li-Rich Layered Li-Mn-Ni-(Al)-O Cathode Materials upon Heat Treatments in Air

The phase evolution of Li-rich Li-Mn-Ni-(Al)-O cathode materials upon heat treatments in the air at 900 °C was studied by X-ray and neutron powder diffraction. In addition, the structures of Li1.26Mn0.61−xAlx Ni0.15O2, x = 0.0, 0.05, and 0.10, were refined from neutron powder diffraction data. For two-phase mixtures containing a monoclinic Li2MnO3 type phase M and a rhombohedral LiMn0.5Ni0.5O2 type phase R, the structures, compositions, and phase fractions change with heat treatment time. This is realized by the substitution mechanism 3Ni2+ ↔ 2Li+ + 1Mn4+, which enables cation transport between the phases. A whole-powder pattern fitting analysis of size and strain broadening shows that strain broadening dominates. The X-ray domain size increases with heat treatment time and is larger than the sizes of the domains of M and R observed by electron microscopy. For heat-treated samples, the domain size is smaller for R than for M and decreases with increasing Al doping.

Intrinsic electronic phase separation and competition between G -type, C -type, and CE -type charge and orbital ordering modes in Hg1−xNaxMn3Mn4O12

The novel series of hole-doped quadruple manganite perovskites Hg1−xNaxMn3Mn4O12 (HNMO) has been synthesized and its charge and orbital order behavior investigated through high-resolution synchrotron powder x-ray diffraction techniques. Through careful Rietveld refinements of structural models via symmetry-motivated approaches, we show that the ground state of HNMO compositions adopts a polar G-type charge and orbital ordered state, which is rare in manganite perovskites, and is robust as a sole phase up to a critical doping level. Upon this critical doping, coincident with that in which colossal magnetoresistance (CMR) is maximal in canonical manganite perovskites, electronic phase separation occurs between G-type and orbital order with charge disorder-type states. The latter state has recently been identified in Ca1−xNaxMn3Mn4O12 perovskites, and proposed to be the competing insulating state from which CMR phenomena emerge. We show that the mechanism for the formation of the G-type state is due to charge transfer processes which may occur through a coupling of distortions involving structural and charge and orbital degrees of freedom, ultimately driving the polar ground state through an improper-like ferroelectric polarization mechanism. These results will act as an important recipe for designing novel ferroelectric-active materials, in addition to expanding the richness of charge and orbital ordered states in manganite perovskites. Published by the American Physical Society 2024

Electrical properties of chelating copolymers and their metal complexes: binary chelating copolymers of styrene with organic acids

BackgroundThe emulsion polymerization of vinyl monomers has been extensively researched, but copolymerization with crotonic acid or cinnamic acid is relatively uncommon. These acids are capable of coordinating with other metal ions. Our previous research has focused on synthesizing and characterizing copolymers of butyl acrylate (BuA)/vinyl acetate (VAc) and styrene-BuA using emulsion techniques, specifically for paint applications. The current work aimed to synthesize and characterize three binary chelating copolymers of styrene with maleic, cinnamic, and crotonic acids. In addition, the prepared chelating copolymers were treated with water and soluble salts of copper and iron for complex formation. Additionally, the characterization and electrical properties of these copolymers were investigated.ResultsThis article reports the synthesis of three binary copolymers of styrene with cinnamic, crotonic, and maleic acids via an emulsion polymerization process using a redox initiation system of potassium persulfate/glucose in the presence of sodium dodecyl benzene sulfonate as an emulsifier. The prepared emulsions of the copolymers were precipitated and purified using Soxhlet extraction in a mixture of n-hexane and toluene. Spectroscopic measurements, including Fourier transform infrared (FTIR), proton nuclear magnetic resonance (1H-NMR), and powder X-ray diffraction (PXRD), in addition to thermal analysis methods like thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) were employed to characterize the copolymers that were synthesized. The metal complexes of the chelating copolymers were prepared by treatment with soluble metal salts of Co(II), Cu(II), and Fe(III), purified, and characterized via IR, PXRD, TGA, and DSC. The semiconducting properties of the chelating polymers and their metal complexes were demonstrated through conductivity measurements taken at room temperature. The conductivity values ranged from 10−3 to 10−6 Ω−1 cm−1.ConclusionThe research underscores the significance of the electrical characteristics of chelating copolymers and their metal complexes, particularly focusing on styrene-based binary chelating copolymers, in driving advancements in technology, science, and economic development.

Enhanced Photoluminescence of Europium-Doped TiO2 Nanoparticles Using a Single-Source Precursor Strategy.

TiO2:Eu3+ nanoparticles with varying europium concentrations were successfully synthesized via a one-pot sol-gel approach using a molecular heterometallic single-source precursor (SSP) Eu-Ti. For comparison, nanomaterials with similar europium levels were also produced by impregnating europium salts onto the same TiO2 substrate. All the nanomaterials were thoroughly characterized using Eu elemental analysis, powder X-ray diffraction (XRD), scanning (SEM), transmission (TEM), scanning transmission electron microscopy (STEM), Brunauer-Emmett-Teller (BET) analysis, thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and photoluminescence (PL). This low-temperature synthesis yielded crystalline powders, and calcination at 400 °C was performed to remove surface organic impurities, enabling a precise comparison of the final nanomaterials. While both preparation methods produced materials with similarly dispersed and localized dopants on the TiO2 surface, photoluminescence studies revealed that the SSP-derived nanomaterials exhibited significantly superior electro-optical properties. This enhanced efficiency is attributed to the co-hydrolysis of both reactants, which facilitates an optimized interface between the crystalline TiO2 core and the dopant-rich amorphous surface, thereby enabling far more effective charge transfer than that achieved by impregnation.