Search Results (158)

Calcium phosphates, including hydroxyapatite, are widely used biomaterials in bone tissue regeneration due to their bioactivity, osteoconductivity, and similarity to the mineral phase of bone. In this study, various apatite calcium phosphate powders were synthesized using three precipitation methods, with controlled pH conditions and reagent ratios, to assess the effect of the synthesis method on their physicochemical and biological properties. Elemental composition (Ca/P ratio), FT-IR spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM) coupled with EDS, and particle size measurements were used to determine the structure, morphology, and stoichiometry of the obtained powders. The results indicated that the synthesis method and pH significantly affect the phase composition of the material, particle size, and Ca/P ratio, which directly influence their solubility and bioactivity. Microbiological tests, NF-κB transcription factor activation, metabolic activity, and cell compatibility of mouse L929 fibroblasts and human hFOB 1.19 osteoblasts showed good biological tolerance of the obtained powders and no cytotoxic effects. The results confirm that a properly selected synthesis method allows for the control of material properties, which is crucial for applications in bone tissue engineering. The materials show potential for use as bioactive components in bone-related biomaterials. Full article

The synthesis, characterization, and equilibrium studies of complexes of selected lanthanide ions Eu(III), Gd(III), and Tb(III) with the ligand 1,3-bis(3-bromo-5-chlorosalicylideneamino)-2-propanol (H₃L) are reported. It was found that in the solid state, the complexes with the formulas [Eu(H₃L)₂(NO₃)₃], [Gd(H₃L)₂(NO₃)₃], and [Tb(H₃L)₂(NO₃)₃] are formed. In solution, complexes with stoichiometries of Ln(III):H₃L 1:1 and 1:2 were obtained. The ligand H₃L was isolated in crystalline form, and its molecular structure and conformation were determined by single-crystal X-ray diffraction analysis. The compounds were further characterized by elemental analysis, infrared spectroscopy, ¹H NMR, ¹³C NMR techniques, and mass spectrometry (ESI), confirming the formation of the Schiff base group. Stability constants of the complexes in solution were determined using potentiometric titration, providing insights into the metal-ligand binding equilibria. In addition, the spectroscopic properties of the ligand and its lanthanide(III) ion complexes were investigated by UV-Vis spectroscopy, which confirmed ligand-to-metal charge transfer interactions, as well as by luminescence measurements. The luminescence studies revealed inefficient energy transfer in [Eu(H₃L)₂(NO₃)₃] complexes, while no transfer was observed in [Tb(H₃L)₂(NO₃)₃] systems at any pH value. This behavior is attributed to the large energy gap between the ligand triplet state and the lowest resonant levels of the studied lanthanide ions. Full article

Carmustine (BCNU) is a powerful alkylating agent primarily used in the chemotherapeutic treatment of malignant brain tumors. However, its clinical application faces significant constraints due to its lipophilicity, low thermal stability, and rapid degradation in physiological environments. To tackle these challenges, our research aimed at the development and detailed characterization of α-cyclodextrin (α-CD) inclusion complexes (ICs) with BCNU employing three different synthesis techniques: co-grinding, cryomilling, and co-precipitation. The selected synthetic methods displayed variations dependent on the technique used, affecting the efficiency, inclusion ratios, and drug-loading capacities, with co-precipitation achieving the most favorable complexation parameters. Structural elucidation through ¹H NMR chemical shifts analysis indicated that only partial inclusion of BCNU occurred within α-CD in ICs produced via co-grinding, while cryomilling and co-precipitation allowed for complete inclusion. Multimodal spectroscopic analyses (FT-IR, UV-Vis, ¹³C CP MAS NMR, and ESI-MS) further substantiated the effective encapsulation of BCNU within α-CD, and systematic solubility assessments via Job’s continuous variation and the Benesi-Hildebrand method revealed a 1:1 host-guest stoichiometry. The ICs obtained were evaluated for BCNU release in vitro at pH levels of 4, 5, 6.5, and 7.4. The mechanism of BCNU drug release was determined to be Fickian diffusion, with the highest cumulative release noted in the acidic microenvironment. These findings collectively validate the effectiveness of α-CD as a functional excipient for the modulation of BCNU’s physicochemical properties through non-covalent complexation. This strategy shows potential for increasing the stability and solubility of BCNU, which may enhance its therapeutic effectiveness in the treatment of brain tumors. Full article

This study reports the successful synthesis of pure cobalt-substituted calcium molybdate powders (Co-doped CaMoO₄) through a co-precipitation method conducted at room temperature, without the use of surfactants or hazardous organic solvents. The formation of solid solutions with x values ranging from 0.00 to 0.08 was confirmed by X-ray diffraction, Rietveld refinement, and Raman spectroscopy analyses. Elemental analysis using energy-dispersive X-ray spectroscopy showed a strong correlation between the experimental and nominal stoichiometries. The synthesized molybdate powders consist of micrometer-sized particles exhibiting diverse morphologies, including microspheres, flower-like architectures, and dumbbell-shaped particles. These agglomerates are composed of primary particles smaller than 43 nm. The specific surface area increased from 3.59 m²/g for the undoped CaMoO₄ to 10.74 m²/g for the 6% Co-doped CaMoO₄. These nanostructured powders represent promising host materials for 4f ions, making them potential candidates for solid-state lighting applications. Full article

This study presents the synthesis and physicochemical characterization of coordination compounds formed between chrysin, a natural flavonoid, and transition metal ions: Mn(II), Co(II), and Zn(II). The complexes were obtained under mildly basic conditions and analyzed using elemental analysis, thermogravimetric analysis (TGA), silver-assisted laser desorption/ionization mass spectrometry (SALDI-MS), FT-IR spectroscopy, and ¹H NMR. The spectroscopic data confirm that chrysin coordinates as a bidentate ligand through the 5-hydroxyl and 4-carbonyl groups, with structural differences depending on the metal ion involved. The mass spectrometry results revealed distinct stoichiometries: 1:2 metal-to-ligand ratios for Mn(II) and Co(II), and 1:1 for Zn(II), with additional hydroxide coordination. Biological assays demonstrated that Co(II) and Mn(II) complexes exhibit enhanced antibacterial and anti-biofilm activity compared to free chrysin, particularly against drug-resistant Staphylococcus epidermidis, whereas the Zn(II) complex showed negligible biological activity. Full article

Lanthanide-based metal–organic frameworks (Ln-MOFs) represent a key material in various optical applications. Thus, they offer the possibility of fine-tuning their functional properties by adjusting the composition, stoichiometry, and ligand nature. This work reports for the first time the environmentally friendly one-pot synthesis of Eu-Tb-doped yttrium-1,3,5-benzenetricarboxylate MOF, i.e., Y-BTC: Eu (10%), Tb (10%), under mild conditions of temperature and pressure. Structural and morphological investigations were conducted through ATR-IR, XRD, and FE-SEM characterization. The doping percentage was analyzed by EDX spectroscopy. The luminescence properties confirm the down-shifting behavior of the MOF, paving the way for using this Eu-Tb-doped Y-BTC system in photovoltaic technology. Full article

In this study, BiBaO₃ perovskite was successfully synthesized via the sol–gel method and thoroughly characterized to evaluate its structural, microstructural, dielectric, electrical, and magnetic properties. X-ray diffraction (XRD) confirmed the formation of a single-phase perovskite structure with high crystallinity. Scanning electron microscopy (SEM) coupled with energy-dispersive X-ray spectroscopy (EDX) revealed a uniform grain morphology and elemental composition consistent with the intended stoichiometry. Dielectric measurements exhibited strong frequency-dependent behavior, suggesting potential for capacitive applications. The electrical conductivity displayed thermally activated behavior, indicative of semiconducting characteristics. Magnetic measurements showed weak ferromagnetic behavior at room temperature, an unusual observation for undoped BaBiO₃-based systems. This magnetism may stem from subtle structural distortions or compositional variations introduced during synthesis. Comparison with previously reported studies underscores the significant influence of the synthesis route and microstructural features on the multifunctional properties of BiBaO₃. Overall, the results highlight the promise of sol–gel-derived BiBaO₃ as a candidate for multifunctional electronic and magnetic applications. Full article

A common route for the synthesis of molybdenum nitrides is through the temperature-programmed reaction of molybdenum oxides with NH₃, or ammonolysis. In this work, the role of precursor phase, gas phase chemistry (impact of H₂O), and temperature profile on the reaction outcome (700 °C) was examined, which resulted in varying amounts of MoO₂, H₂MoO₅, and the nitride phases—cubic γ (nominally Mo₂N) and hexagonal δ (nominally MoN). The phase fraction of the δ phase increased with precursor in the sequence MoO₂ > MoO₃ > H₂MoO₅. Steam in the reaction gas also favored the production of δ over γ, but with too much steam, MoO₂ was obtained in the product. Synthesis conditions for obtaining nearly phase-pure δ were identified: MoO₂ as the precursor, 2% H₂O in the gas stream, and a moderate heating rate (3 °C/min). In situ X-ray diffraction provided insights into the reaction pathway. Extensive physico-chemical analysis of the δ phase, including synchrotron X-ray and neutron diffraction, electron microscopy, thermogravimetric analysis, X-ray photoelectron spectroscopy, and prompt gamma activation analysis, revealed its stoichiometry to be MoO_0.108(8)N_0.892(8)H_0.012(5), indicating non-trivial oxygen incorporation. The presence of N/O ordering and an impurity phase Mo₅N₆ were also revealed, detectable only by neutron diffraction. Notably, a computationally predicted MoON phase (doi: 10.1103/PhysRevLett.123.236402), of interest due to its potential to display a metal-insulator transition, did not appear under any reaction condition examined. Full article

Starch was plasticized with epoxidized soybean oil (ESO) modified by reaction with cinnamic acid (CA), and films were prepared using solvent casting from water/ethanol solutions. They exhibited good hydrophobicity, reduced water sensitivity, and showed the same transparency as glycerol-plasticized counterparts, but with less flexibility. Interestingly, modified ESO enhanced gelatinization and hindered retrogradation of the biopolymer. ESO was reacted with CA without the use of catalysts to obtain a β-hydroxyester; in order to optimize the synthesis process, different reaction conditions were explored, varying the stoichiometry and the heating cycles. Products were fully characterized by Fourier transform infrared (FTIR) spectroscopy, ¹H and ¹³C nuclear magnetic resonance (NMR), and the different reactions following the opening of the oxirane ring were discussed. The properties of the novel starch-based films prepared with modified ESO highlight their use in food packaging, disposable devices, and agricultural mulching films. Full article

We report on the arc melt syntheses of HoB₂ and Nb-substituted HoB₂ polycrystalline ingots and their magnetocaloric and microstructural properties. XRD data and microstructural analysis reveal that a nominal 10% Nb addition during synthesis results in changes to unit cell parameters and grain morphology. Interpretation of the refined cell parameters using Vegard’s law shows that Nb substitutes into HoB₂ with stoichiometry Ho_0.93Nb_0.07B₂. Arc-melted products are polycrystalline bulk samples containing minor phases such as Ho₂O₃, Ho, and HoB₄. Nb substitution results in a smaller grain size (~sub-micron) and a higher Curie temperature, T_C, compared to HoB₂. With a 10 T applied field, the maximum magnetic entropy, ΔS_M, for HoB₂ and for Ho_0.93Nb_0.07B₂, is 46.8 Jkg⁻¹K⁻¹ and 38.2 Jkg⁻¹K⁻¹ at 18 K and 21 K, respectively. Both samples show second-order phase transitions. Despite high totals of minor phases (e.g., ~10 wt.% and ~25 wt.%), the calculated relative cooling powers are greater than 1300 Jkg⁻¹ and 600 Jkg⁻¹ at 10 T and 5 T, respectively. The magnetocaloric properties of both samples are consistent with Holmium boride compounds prepared via alternative methods. Full article

Pulsed laser ablation in liquids is one of the most versatile and widespread techniques for the easy synthesis of different types of nanoparticles with controllable properties. A huge amount of energy compressed into one pulse that is directed onto a solid target leads to the ejection of materials into surrounding liquid. However, the precision of the focus of laser irradiation can play a crucial role in the synthesis of nanomaterials and, hence, significantly affect their physico-chemical properties. In this paper, we investigated the influence of the focus position of the laser spot on the optical properties of single- and double-element composite silicon/gold nanoparticles, as well as on their structure and chemical composition. Deepening of the focus to 0.5 mm inside the bulk material led to better chemical stability of the colloidal solutions and increased the particle and mass concentrations of the generated nanoparticles. This larger amount of materials led to a stronger absorbance, and resulted in slightly better photoluminescence excitation efficiencies for all nanostructures. Silicon-based nanoparticles had a remarkable photoluminescence peak at ~430 nm upon xenon lamp excitation, which was the most pronounced for pure silicon nanoparticles synthesized at the F+0.5 focus position. This position also led to the best laser-induced heating (~0.85 °C/min) of the colloidal solutions. All nanocomposites revealed amorphous silicon structures with some Si(111) and Au(111), suggesting the formation of gold silicide with different stoichiometries. The observed findings can help in choosing appropriate experimental conditions to achieve the best performance of laser-synthesized colloidal solutions of composite silicon/gold nanostructures. Full article

Optimal product synthesis in bioelectrochemical systems (BESs) requires a comprehensive understanding of the relationship between external voltage and microbial yield. While most studies assume constant growth yields or rely on empirical estimates, this study presents a novel thermodynamic model, linking anodic oxidation and cathodic carbon dioxide (${CO}_2$) reduction to methane (${CH}_4$) by growing microbial biofilm. Through integrating theoretical Gibbs free energy calculations, the model predicts electron and proton transfers for autotrophic methanogen and anode-respiring bacteria (ARB) growth, accounting for varying applied voltages and substrate concentrations. The findings identify an optimal applied cathodic potential of −0.3 V vs. the standard hydrogen electrode (SHE) for maximizing ${CH}_4$ production under standard conditions (pH 7, 25 °C, 1 atm) regardless of ohmic losses. The model bridges the stoichiometry of anodic and cathodic biofilms, addressing research gaps in simulating anodic and cathodic biofilm growth simultaneously. Additionally, sensitivity analyses reveal that lower substrate concentrations require more negative voltages than standard condition to stimulate microbial growth. The model was validated using experimental data, demonstrating reasonable predictions of biomass growth and ${CH}_4$ yield under different operating voltages in a multi substrate system. The results show that higher voltage inputs increase biomass yield while reducing ${CH}_4$ output due to non-optimal voltage. This validated model provides a tool for optimizing BES performance to enhance ${CH}_4$ recovery and biofilm stability. These insights contribute to finding optimum voltage for the highest ${CH}_4$ production for energy efficient ${CO}_2$ reduction for scaling up BES technology. Full article

The glycine nitrate procedure (GNP) is a method that proved to be the easiest and most effective method for controlling the composition and morphology during the synthesis of Co_0.9R_0.1MoO₄ (R = Ho, Yb, Gd). This method of the combustion process achieves control of stoichiometry, homogeneity, and purity. Metal nitrates and glycine were mixed in the appropriate stoichiometric ratios to produce Co_0.9R_0.1MoO₄ (R = Ho, Yb, Gd). The samples obtained by the mentioned method were further subjected to different characterization methods such as differential thermal analyses (DTA), X-ray diffraction (XRD), Fourier transform infrared spectrum (FTIR), spectroscopy, field emission scanning electron microscopy (FESEM), and nitrogen adsorption method. A high level of anisotropy of the shape and size of particles in the form of agglomerates was found. Also, there are noticeable differences in the microstructure and plate crystals. The color of the synthesized sample changes from darker to lighter shades after thermal treatments. There are pronounced changes in the dominant wavelength (nm) and color purity between the initial sample and the sample after heating (1100 °C) due to the concentration of Co. Full article

The prerequisite for rapid and steady development of TMDC-based optoelectronic devices is high efficiency in materials preparation, which relies on a mature synthesis technique and optimized production conditions. Visualization based on numerical simulation, which illustrates the impact of growth parameters on deposited products, is helpful to understand formation mechanisms and modify growth conditions. In this work, we construct two models with two different substrate placements, where the substrate is parallel or perpendicular to gas flow direction. The simulation results show more velocity distribution uniformity across a wider range from −1.4 cm to 1.4 cm for vertically placed (VP) compared to horizontally placed (HP) substrates. The calculated average velocities of 0.048, 0.053, 0.078, 0.137, and 0.391 cm/s along five different positions on the VP substrate are greater than the values of 0.027, 0.026, 0.025, 0.023, and 0.036 cm/s on the HP substrate. Comparing the precursor concentration distributions on both substrates, it is observed that the S molar concentration gradient on both substrates is negligible and the uniform Mo molar concentrations from z = −1.4 cm to 2.0 cm on the VP substrate ensure minimal change in the S/Mo ratio, which contributes to forming single-morphology domains. Furthermore, increasing the distance between the precursor inlets and the VP substrate decreases the amount of molecules on the substrate surface, achieving near-stoichiometry and promoting monolayer deposition. This is verified by the experimental result, which showed gentle morphological transformation on the VP substrate from a truncated triangle to a hexagon, and then back to a truncated triangle. By contrast, the multi-morphology and thickness of MoS₂ on the HP substrate result from the complex Mo concentration along the flow direction. Moreover, PL intensities of the MoS₂ domains deposited on the VP substrate are enhanced by 11.9-fold compared to the average intensity on the HP substrate. This result indicates the MoS₂ grown on the VP substrate has less intrinsic defects than that grown on the HP substrate. The combination of numerical simulation with experimental methods facilitates the visualization of invisible growth conditions, which provides effective guidance for using simulation results for other TMDC materials. Full article

Based on their various and outstanding properties, binary nitrides are used as (synthesis) materials in industry and research. Hence, their comprehensive characterization by analytical methods is of particular interest. Since Nuclear Magnetic Resonance (NMR) spectroscopy is very sensitive to the symmetry of the electronic density distribution, it is a suitable tool for the investigation of rock-salt structure types and, especially, for those with known stoichiometry issues. Here, we report on magic-angle spinning NMR spectra of the nuclides ⁸⁹Y ($I={\displaystyle \raisebox{1ex}{$1$}\!\left/ \!\raisebox{-1ex}{$2$}\right.}$), ¹³⁹La ($I={\displaystyle \raisebox{1ex}{$7$}\!\left/ \!\raisebox{-1ex}{$2$}\right.}$) and ¹⁴N ($I=1$) in polycrystalline samples of YN, LaN and LuN. Due to the high symmetry of their crystal structures, the spectra of all nuclides do not exhibit anisotropic effects of significant magnitude. The resulting isotropic chemical shift values are ${\delta }_{iso}$(⁸⁹Y) = 516 ppm for YN, ${\delta }_{iso}$(¹³⁹La) $=1294$ ppm for LaN, and ${\delta }_{iso}$(¹⁴N) = 457 ppm (YN), 788 ppm (LaN) and 384 ppm (LuN). The newly determined ${\delta }_{iso}$(¹⁴N) values for these three binary nitrides fit well into the previously reported linear correlation between nitrogen distance to the nearest cation and isotropic chemical shift, leading to a better correlation coefficient and reduced error margins for the fit parameters. Full article