Search Results (128)

Ammonium paratungstate (APT) was synthesized from scheelite ore concentrates from the Brejuí Mine in Currais Novos, Rio Grande do Norte, Northeast Brazil. The process involved acid leaching to obtain tungstic acid (H₂WO₄), followed by its conversion to APT. A 2³ factorial design evaluated the influence of temperature, HCl concentration, and reaction time on the leaching efficiency, revealing temperature and acid concentration as significant variables. Tungsten extraction reached 98.6% under moderate time and temperature conditions. The resulting H₂WO₄ phase exhibited a lamellar and porous morphology, facilitating its rapid dissolution and crystallization into APT at 60 °C. The produced nanometric APT exhibited high purity, a mixed rod-like/cubic morphology, and thermal stability above 600 °C. This work adds value to the Brazilian tungsten deposits by supporting more efficient and sustainable extraction routes for obtaining APT. Full article

In this study, bulk metallic glasses (BMGs) of Zr₅₆Cu₂₃Al₁₀Ni_11-xTa_x (x = 0, 0.5, 1, 1.5, 2, and 2.5 at.%) were prepared by copper mold suction-casting. The glass-forming ability, mechanical properties, crystallization kinetics, and corrosion resistance of the as-obtained amorphous alloys were all investigated. Experimental results showed enhanced forming ability of amorphous alloys in the presence of small amounts of Ta element. By adding appropriate amounts of Ta, the supercooled liquid region of bulk metallic glass increased from 64 K to 73 K. The critical diameter of the alloy rod at x = 1, 1.5 rose from 5 mm to 6 mm. The addition of Ta also reduced the sensitivity coefficients of the amorphous alloys to the heating rate during crystallization, while other quantities, like Eg, Ex, and Ep, all incremented. Thus, the addition of Ta declined the temperature sensitivity of amorphous alloy systems. This also increased the energy barrier required for atom rearrangement, nucleation and growth, as well as greatly enhancing the stability of the systems. At 2% Ta content, the plastic strain of the amorphous alloy exceeded 2.6%, and yield strength reached 1900 MPa. In sum, the mechanical properties of the amorphous alloys after the addition of Ta element obviously improved when compared to the original alloy. As Ta content raised, the corrosion current densities of BMGs in different corrosion solutions gradually decreased, while the corrosion potential gradually increased. Full article

MnCo₂O₄ and CoMn₂O₄ were successfully synthesized on a stainless-steel substrate using the hydrothermal method. The structural and morphological characteristics of the spinel samples were investigated using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The electronic and vibrational properties were studied through X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FTIR). Electrochemical properties were also evaluated using a three-electrode system associated with an electrochemical workstation. The studies revealed that the inversion of Mn and Co cation distribution between the spinel structure sites not only modifies the crystal structure and morphology but also alters specific functional properties. MnCo₂O₄ crystallized in a cubic spinel phase, exhibiting spherical particles, pronounced microstrain, and stronger metal–oxygen bonding. In contrast, CoMn₂O₄ adopted a tetragonal spinel structure with rod-like crystallites, lower microstrain, and more flexible bonding environments. Electrochemical impedance spectroscopy further revealed distinct charge-transfer dynamics, indicating differences in surface redox activity. This comparative analysis elucidates how cation site occupancy governs the performance of the synthesized spinel oxides and underscores their potential as efficient catalysts or catalyst supports for redox and energy-related applications. Full article

Ti₄₈Zr₂₇Cu₆Nb₅Be₁₄ amorphous composites were prepared by copper mold suction casting to obtain as-cast specimens. Subsequently, the as-cast specimens were held at 900 °C for different durations (5, 10, 20, 30, and 40 min) and then water quenched to cool, yielding treated specimens. Room-temperature compression tests were conducted to characterize the mechanical properties of the materials before and after the treatment. X-ray diffraction (XRD), optical microscopy (OM), and scanning electron microscopy (SEM) were used to detect and observe the microstructure of the specimens (before and after treatment) as well as the morphology of the side surface of compressed fractured specimens. Results show that the as-cast specimens are amorphous matrix composites, with dendrites (identified as β-Ti) predominantly distributed in the amorphous matrix. When the treatment duration increased from 5 to 40 min, two key phenomena were observed. The dendrites gradually disappeared and evolved into curved crystals first; subsequently, the curved crystals transformed into elongated crystals. Finally, the elongated crystals evolved into short and thick rod-like crystals, which further transformed into near-spherical crystals or spherical crystals. Furthermore, as the treatment duration prolonged, the average equivalent size of the crystals increased continuously, reaching 23.1 μm. Additionally, the plasticity of the specimens first increased, reached a maximum value of 16.2% when held for 30 min, and then decreased. Full article

Cordycepin (3′-deoxyadenosine, 3′-dA), the flagship nucleoside antibiotic from Cordyceps militaris, exerts potent anti-inflammatory, antimicrobial, and antitumor activity but is rapidly inactivated by human adenosine deaminase (ADA). While prodrugs, ADA inhibitors, and nanocarriers have been pursued to prolong its half-life, the influence of solid form on delivery performance remains unexplored. Here, three polymorphs—anhydrate-I (flake-like), anhydrate-II (rod-like), and a previously unreported monohydrate (fibrillar)—were prepared, characterized (PXRD, TG-DSC, FTIR), and subjected to equilibrium solubility, slurry-conversion, and humidity-sorption mapping. The monohydrate dehydrates at 144 °C and sequentially transforms to anhydrate-I → anhydrate-II (ΔH = −127.5 J g⁻¹), establishing a monotropic relationship between the two anhydrous forms. Solubility displays a bell-shaped profile versus water activity: the monohydrate is stable above aw 0.8, whereas anhydrate-II predominates below aw 0.2. In model immediate-release tablets, anhydrate-II achieves complete dissolution within 10 min, whereas the monohydrate sustains release for 30 min. Hygroscopicity tests show the monohydrate absorbs <6% water up to 75% RH without structural change, whereas anhydrate-I converts to the monohydrate above 63% RH. The quantitative humidity–crystal form–performance correlations provide a rational platform for crystal form selection and the design of stable, efficacious cordycepin solid dosage forms. Full article

This study investigates the Fe₂₂Ni₁₆Co₁₉Mn₁₂Cr₁₆P₁₅ alloy designed to enhance glass-forming ability. The alloy was synthesized by arc melting and examined using infrared thermography, differential scanning calorimetry (DSC), scanning electron microscopy with energy-dispersive spectroscopy (SEM/EDS), and X-ray diffraction (XRD). Thermographic measurements revealed a temperature arrest at ~1007 K associated with eutectic crystallization, accompanied by contraction visible as a flattened ingot surface. DSC confirmed the dominant eutectic transformation (−170.7 J/g). Compared with the previously studied Fe₂₂Ni₁₆Co₁₉Mn₁₂Cr₁₆P₁₅ alloy, this composition showed a simplified transformation sequence and a larger eutectic fraction. DSC of melt-spun ribbons demonstrated a three-step crystallization (659 K, 699 K, 735–773 K, completion ~820 K) with a total enthalpy of 180.4 J/g. The broad crystallization interval (ΔTc ≈ 161 K) indicates enhanced thermal stability compared with simpler Ni–P or Fe–Ni–P–C alloys. SEM/EDS observations revealed eutectic colonies with predominantly rod-like morphology and chemical partitioning in inter-colony regions, favoring precipitation of transition metal phosphides. XRD confirmed four crystalline phases (Fe–Ni, CrCoP, Ni₃P, MnNiP) in ingots, while ribbons exhibited a fully amorphous structure. These findings demonstrate that Fe₂₂Ni₁₆Co₁₉Mn₁₂Cr₁₆P₁₅ possesses good glass-forming ability but forms multiple phosphides under slower cooling. Precise cooling control is thus essential for tailoring its amorphous or crystalline state. Full article

Fly ash from coal-fired power plants is a promising precursor for zeolite synthesis due to its aluminosilicate-rich composition. However, its direct utilization is often limited by impurities and a low silicon-to-aluminum ratio (SAR). This study demonstrates the conversion of Class C fly ash from the Soma thermal power plant (Turkey) into FAU- and CHA-type zeolites through optimized acid leaching and hydrothermal synthesis. Acid treatment increased the SAR from 1.33 to 2.85 and effectively reduced calcium-, sulfur-, and iron-bearing impurities. The SAR enhancement by acid leaching was found to be reproducible among Class C fly ashes, whereas Class F materials exhibited a limited response due to their acid-resistant framework. Subsequent optimization of alkaline fusion-assisted synthesis enabled selective crystallization of FAU and CHA, while GIS and MER appeared under prolonged crystallization or higher alkalinity. SEM revealed distinct morphologies, with MER forming rod-shaped clusters, and CHA exhibiting disc-like aggregates. Water sorption analysis showed superior uptake for metastable FAU (~23 wt%) and CHA (~18 wt%) compared to stable GIS and MER (~12–13 wt%). Overall, this study establishes a scalable and sustainable route for producing high-performance zeolites from industrial fly ash waste, offering significant potential for adsorption-based applications in dehumidification, heat pumps, and gas separation. Full article

This study reports the discovery and structural characterization of a novel polymorph, designated as Form III, of Alclometasone dipropionate, a corticosteroid commonly used in the treatment of inflammatory dermatoses. Form III was obtained by modifying the crystallization conditions reported in prior art and was thoroughly characterized using Powder X-ray Diffraction (PXRD), Fourier Transform Infrared (FT-IR) spectroscopy, melting-point determination, Differential Scanning Calorimetry (DSC), Thermogravimetric Analysis (TGA), including its first derivative (DTG), optical microscopy, and Scanning Electron Microscopy (SEM). In parallel, pure Form II, previously observed only in mixtures with Form I, was successfully isolated and characterized using the same analytical techniques. Both forms were compared in terms of structural, thermal, and morphological properties. PXRD analysis revealed that Form III crystallizes in a triclinic system; FT-IR spectroscopy revealed unique vibrational signatures, and microscopy showed rod-like crystal morphology. The discovery of Form III expands the current understanding of the solid-state landscape of Alclometasone dipropionate and opens opportunities for the identification of new industrial purification methods for the compound. Full article

Magnesium whitlockite (Mg-WH) has emerged as a promising biomaterial for bone regeneration due to its compositional similarity to natural bone minerals. This study aimed to systematically modify a dissolution–precipitation synthesis method to produce Mg-WH granules with tailored morphologies and controlled phase compositions for possible use in bone regeneration applications. Three distinct precursor granules were prepared by mixing varying amounts of ammonium dihydrogen phosphate and magnesium hydrogen phosphate with calcium sulfate. The precursors were then transformed into biphasic and single-phase Mg-WH granules by means of immersion in magnesium- and phosphate-containing solutions under controlled conditions. The X-ray diffraction results demonstrated that biphasic materials containing Mg-WH and either calcium-deficient hydroxyapatite (CDHA) or dicalcium phosphate anhydrous (DCPA) formed after 24 h of synthesis, depending on the synthesis conditions. Prolonging the reaction time to 48 h resulted in complete transformation into single-phase Mg-WH granules. Fourier-transform infrared spectroscopy confirmed the presence of functional groups characteristic of Mg-WH, CDHA, and DCPA in the intermediate products. The spectra also indicated the absence of precursor phases and the progressive elimination of secondary phases as the reaction time increased. Scanning electron microscopy analyses revealed notable morphological transformations from the raw granules to the product granules, with the latter exhibiting interlocked spherical and rod-like particles composed of fine Mg-WH rhombohedral crystals. N₂ adsorption–desorption analyses exposed significant differences in the surface properties of the synthesized granules. By varying precursor, reaction solution compositions, and reaction times, the study elucidated the phase evolution mechanisms and demonstrated their impact on the structural, morphological, and surface properties of Mg-WH granules. Full article

This study investigated the impact of zinc oxide’s (ZnO’s) morphology on the piezoelectric performance of polyvinylidene fluoride (PVDF) composites for flexible sensors. Rod-like (NR) and sheet-like (NS) ZnO nanoparticles were synthesized via hydrothermal methods and incorporated into PVDF through direct ink writing (DIW). The structural analyses confirmed the successful formation of wurtzite ZnO and enhanced β-phase content in the PVDF/ZnO composites. At a degree of 15 wt% loading, the ZnO-NS nanoparticles achieved the highest β-phase fraction (81.3%) in PVDF due to their high specific surface area, facilitating dipole alignment and strain-induced crystallization. The optimized PVDF/ZnO-NS-15 sensor demonstrated superior piezoelectric outputs (4.75 V, 140 mV/N sensitivity) under a 27 N force, outperforming its ZnO-NR counterparts (3.84 V, 100 mV/N). The cyclic tests revealed exceptional durability (<5% signal attenuation after 1000 impacts) and a rapid response (<100 ms). The application trials validated their real-time motion-monitoring capabilities, including finger joint flexion detection. This work highlights the morphology-dependent interfacial polarization as a critical factor for high-performance flexible sensors, offering a scalable DIW-based strategy for wearable electronics. Full article

High-melting point 1,3-diacylglycerols not only provide health benefits, but are also suitable for manufacture of foods containing various specialty fats. It is difficult to prepare such high-melting point diacylglycerols, as the activities of specific enzymes will severely reduce at their melting points. In the present study, a combined technique was developed to prepare 1,3-dipalmitoylglycerol (1,3-DPG) and 1,3-distearoylglycerol (1,3-DSG) using selective esterification, molecular distillation, and solvent fractionation. Lipozyme TL IM was suitable for use as the optimal enzyme to maintain relatively high activity levels at esterification temperatures of 73–75 °C. 1,3-DAG/(DAG + TAG) was selected as the most important index to monitor the esterification and to evaluate the synthesized fats. The obtained 1,3-DPG and 1,3-DSG showed high purities, at more than 83%, and possessed hard attributes at room temperature. Both 1,3-DPG and 1,3-DSG exhibited fat crystals with β′ and β crystals. Needle-like and rod-like crystals were observed at 5–25 °C for 1,3-DPG, and closely packed feather-like crystals were found at 5–20 °C for 1,3-DSG, indicating their multiple abilities in modifying the crystallization stabilization of the fat matrix during food processing. Full article

Self-assembly of amphiphilic molecules is an important phenomenon attracting a broad range of research. In this work, we study the self-assembly of KTOF₄ sphere–rod amphiphilic molecules in mixed water–dioxane solvents. The molecules are of a T-shaped geometry, comprised of a hydrophilic spherical Keggin-type cluster attached by a flexible bridge to the center of a hydrophobic rod-like oligodialkylfluorene (OF), which consists of four OF units. Transmission electron microscopy (TEM) uncovers self-assembled spherical structures of KTOF₄ in dilute solutions. These spheres are filled with smectic-like layers of KTOF₄ separated by layers of the solution. There are two types of layer packings: (i) concentric spheres and (ii) flat layers. The concentric spheres form when the dioxane volume fraction in the solution is 35–50 vol%. The flat layers are formed when the dioxane volume fraction is either below (20 and 30 vol%.) or above (55 and 60 vol%.) the indicated range. The layered structures show no in-plane orientational order and thus resemble thermotropic smectic A liquid crystals and their lyotropic analogs. The layered packings reveal edge and screw dislocations. Evaporation of the solvent produces a bulk birefringent liquid crystal phase with textures resembling the ones of uniaxial nematic liquid crystals. These findings demonstrate that sphere–rod molecules produce a variety of self-assembled structures that are controlled by the solvent properties. Full article

The crystal structures of rod-like molecules with nitro-biphenyl or nitro-phenyl end groups and attached n-alkyl units with terminal acid or ester groups are determined by single crystal analysis and their arrangements are compared. The molecules are linked by head-to-tail arrangements and form strings. They point in a single or two different directions and are placed side by side to create the crystal structure. Some of the space groups of the structures can only be determined by a statistical routine because strongly disordered structures prevent the use of extinction methods, since many extinction violations occur for monoclinic and orthorhombic unit cells. An agreement between experimental and calculated X-ray reflection intensities serves as proof of the correctness of the method as well as a test of the existence of an inversion center. The single crystals are grown in solution with ethanol, isopropanol, DMAc, and toluene as solvents. Cocrystals are formed in DMAc solutions by the dissolved acid compounds. The two-molecule asymmetric unit of the acid compound is reduced to a one-molecule asymmetric unit with one DMAc included which forms a hydrogen bond with the acid group of the biphenyl molecule. These changes alter the hydrogen bonding scheme along a string. Some structural similarities as the head-to-tail arrangement in the strings are maintained between the terminal acid and ester compounds despite disordered ester groups in the compounds and the ester molecules themselves at ambient temperature. Full article

In this study, the crystallization behavior, microstructure, and mechanical and physical properties of CaO-Al₂O₃-SiO₂ (CAS)-based glass-ceramics prepared from eggshell waste, zeolite, and pumice were investigated using X-ray diffraction (XRD), differential thermal analysis (DTA), scanning electron microscopy (SEM), a nanoindentation tester, and the Archimedes method. XRD analysis revealed that anorthite and wollastonite crystalline phases precipitated in the glass-ceramic samples after sintering at temperatures of 1000 °C and 1100 °C. However, diffraction peaks belonging to the wollastonite phase disappeared after sintering at 1200 °C, while peaks representing the pseudowollastonite phase were detected together with anorthite in the samples. SEM images showed that the crystals become coarser as the sintering temperature increased, with the crystal morphology transitioning from needle-like to rod-like. The crystallization activation energy (E_a) and Avrami parameter (n), both kinetic parameters, were calculated from DTA curves plotted at different heating rates using the Kissinger, Ozawa, and Matusita approaches. The results indicated that the crystallization activation energy of the CASZ glass ranged from 406 to 428 kJ mol⁻¹, while that of the CASP glass varied from 356 to 378 kJ mol⁻¹, depending on the method used. Additionally, the Avrami constant (n) was calculated to be 3.33 for CASZ and 2.89 for CASP. The hardness and bulk density of the glass-ceramic samples were significantly affected by the porosity present in the structure, with the highest hardness and bulk density values achieved for the CASZ glass-ceramic sample at the initial sintering temperature of 1000 °C. Full article

The present work was the preliminary study of phase diagrams and miscibilities of low-temperature metallomesogen (MOM) model structures based on rod-like palladium (Pd) alkyl/alkoxy-azobenzene metal complexes and their mixtures with commercial liquid crystal materials for potential application. The initial results indicated the accessible temperature range and mesgenic miscibility between parent ligand, MOMs and commercial liquid crystal mixtures. The eutectic ligand/MOM composition with other MOMs and commercial nematic liquid crystal materials exhibited complete mesogenic miscibility and wide low-temperature mesogenic stability for eventual utilization in commercial liquid crystal devices. Full article