Search Results (4,251)

Rare earth elements (REEs), as necessary elements in many industries, have driven increased demand for mineral exploitation. However, understanding the occurrence states of REEs is crucial for their extraction. Therefore, this work primarily investigated the differences in the occurrence states of REEs and the thermal decomposition behavior of carbonatite rare earth deposits in China using scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray powder diffraction, and X-ray photoelectron spectroscopy. The results showed that the bastnaesite concentrate from the M deposit in southwestern China (referred to herein as B-ore), contained REEs accounting for 53.59%, and was associated with small amounts of wulfenite, barite, and iron ore. In contrast, the contents of REEs in the raw ores of N deposit in northern China (referred to herein as R-ore) was relatively low (3.71%), but were also enriched in Fe. R-ore consisted of small particle, with 32.44% sized between 0.075 and 0.11 mm, and 26.38% below 0.075 mm. The contents of Fe, La, and Ce in these smaller particles were higher than those of larger particles. Fe might be substituted with Ce, La, and other REEs in magnetite crystals, forming isomorphic structures. This research was expected to provide assistance in the efficient extraction of REEs from carbonatite deposits. Full article

This paper focuses on the study of the arena wall decoration in the amphitheater at the archaeological site of Viminacium. The architectural characteristics of the amphitheater, along with the spectacle iconography, have made this finding one of the most interesting discoveries at Viminacium, as well as in a wider context. A multidisciplinary approach that included an iconographic and archaeological study, as well as Energy Dispersive X-ray Fluorescence (EDXRF), X-ray Powder Diffraction (XRD), and Raman and Fourier-transform Infrared (FTIR) spectroscopy analysis, was applied to determine the palette of the pigments used for the arena wall decoration and understand the iconography and its context in more detail. Among the commonly used earth pigments (yellow, red, brown, and green colors), copper-based pigments (green and blue Egyptian blue), and the most precious ones for the period—namely, cinnabar and lapis lazuli—were identified. The applied analytical techniques enabled a tentative suggestion of the origin of the raw materials of some of the pigments that were used, such as marine sediments or rocks from different destinations. Due to the fact that the Viminacium amphitheater constitutes a typical example of a provincial building reserved for public spectacles, the results of this study will significantly contribute to our understanding of the function of the amphitheaters in the Danubian region, as well as throughout the Roman world. Full article

A small, strongly schistose Ni-laterite occurrence at the Vermion ophiolite (40°26′ Ν, 22°10′ Ε), Northen Greece, along a strong shear zone, is characterized by relatively high Ni, Co and Mn contents, magnetite as the dominant mineral, garnet (grossularite), theophrastite [β-Ni(OH)₂], otwayite-like phase (ideally Ni₂CO₃(OH)₂.H₂O), (Ni, Co, Mn)-hydroxides, and Ni-phyllosilicates. New analytical data, including black-white and color back-scattered electron images (BSEIs), elemental mapping and scanning, and Raman Spectroscopy, alongside silicates and hydroxides revealed the presence of varying silica content (less than 1 to 29 wt.%) in theophrastite and in (Ni, Co, Mn ± Fe)-hydroxides, although the X-ray powder diffraction data correspond to those of pure hydroxides. The gradual stacking of fine fibrous otwayite-like crystals to the boundaries of successive thin layers and within layers themselves, results in porous mineral phases of varying density shifting towards more compact mineral with increasing residence time. The presented data suggest that a potential explanation of the presence of Si in theophrastite may be the precipitation of Si after initial Ni-hydroxyl-carbonate fine crystals deposition. A potential sequence of the stability of Ni-minerals at Vermion may be as follows: Hydroxyl-carbonates < [β-Ni(OH)₂] (theophrastite) < (Ni, Co, Mn)(OH)₂ < Ni-phyllosilicates; this may be a significant factor for Ni-exploration in Ni-larerite deposits. Full article

The dynamic response in propane atmospheres at different voltages was investigated for samples made from powders of the semiconductor oxide CoSb₂O₆ synthesized using the microwave-assisted colloidal method. Powders of the compound calcined at 700 °C were studied with X-ray diffraction, confirming the CoSb₂O₆ crystalline phase. The microstructural characteristics of the oxide were analyzed using scanning and transmission electron microscopy (SEM/TEM), revealing a high abundance of nanorods, nanoplates, and irregular nanoparticles. These nanoparticles have an average size of ~21 nm. Using UV-Vis, absorption bands associated with the electronic transitions of the CoSb₂O₆’s characteristic bonds were identified, which yielded a bandgap value of ~1.8 eV. Raman spectroscopy identified vibrational bands corresponding to the oxide’s Sb–O and Co–O bonds. Dynamic sensing tests at 300 °C confirmed the material’s p-type semiconductor behavior, showing an increase in resistance upon exposure to propane. Critically, these tests revealed that the sensor’s baseline resistance and overall response are tunable by the applied voltage (1–12 V), with the highest sensitivity observed at the lowest voltages. This establishes a clear relationship between the electrical operating parameters and the sensing performance. The samples exhibited good operational stability, capacity, and efficiency, along with short response and recovery times. Extra-dry air (1500 cm³/min) was used as the carrier gas to stabilize the films’ surfaces during propane detection. These findings lead us to conclude that the CoSb₂O₆ could serve as an excellent gas detector. Full article

Hydrothermal scheelite from three Romanian occurrences was analyzed in order to ascertain its structural, physical, vibrational, paragenetic, and crystal-chemical peculiarities as an important tool for characterizing the metallogenetic behavior and facilitating the ore-processing. All three occurrences, i.e., Ciclova and Oravița in Banat and Băița Bihor in the Bihor Mountains, are related to skarn deposits developed at the contact of Upper Cretaceous granodioritic bodies with Mesozoic calcareous deposits. Typical crystals show {001}, {111}, and {101} forms and are up to 15 mm across. The structure was successfully refined as tetragonal, space group I4₁/a, with R₁ = 0.0165 (Ciclova), 0.0204 (Oravița), and 0.0237 (Băița Bihor), respectively. The cell parameters refined for the same samples are a = 5.2459(10) Å and c = 11.3777(5) Å at Ciclova, a = 5.2380(2) Å and c = 11.3679(8) Å at Oravița, and a = 5.2409(2) Å and c = 11.3705(6) Å at Băița Bihor. The multiplicity of bands in both infrared absorption and Raman spectra is consistent with the S₄ punctual symmetry of the tungstate anion, agreeing with the structural data. In all cases, the analyzed scheelite is close to the CaWO₄ end-member. Cathodoluminescence peculiarities at the level of single crystals suggest that they crystallized in a slightly oxidizing to reducing environment from late hydrothermal solutions. Textural and paragenetic peculiarities suggest that scheelite from the three occurrences crystallized from epithermal, low-temperature, fluoride- and boron-bearing aqueous solutions. Full article

In this study, supramolecular inclusion complexes composed of komecosanol (Ko), a lipophilic compound derived from rice bran, and α-cyclodextrin (αCD) were prepared using a solvent-free three-dimensional (3D) ball milling method. Their physicochemical properties were examined using various techniques. Powder X-ray diffraction analysis of the ground mixture at a Ko/αCD ratio of 1/8 revealed the disappearance of diffraction peaks characteristic of Ko and the emergence of new peaks, indicating the formation of a distinct crystalline phase. Moreover, differential scanning calorimetry analysis showed the disappearance of the endothermic peaks corresponding to Ko, indicating molecular-level interactions with αCD. Near-infrared spectroscopy results suggested the formation of hydrogen bonds between the C–H groups of Ko and the O–H groups of αCD. Solid-state ¹³C CP/MAS NMR and T₁ relaxation time measurements indicated the formation of a pseudopolyrotaxane structure, while scanning electron microscopy images confirmed distinct morphological changes consistent with complex formation. These findings demonstrate that 3D ball milling facilitates the formation of Ko/αCD inclusion complexes with a supramolecular architecture, providing a novel approach to improve the formulation and bioavailability of poorly water-soluble lipophilic compounds. Full article

Porous CaCO₃ vaterite particles have been widely used as drug carriers for biomedical applications due to their high biocompatibility and low production costs. However, controlling the particle size and porosity of CaCO₃ nanoparticles with the desired crystalline phase is still challenging. In this study, we have systematically investigated the preparation of CaCO₃ nanoparticles under various conditions including precursor types/ratios/concentrations, additive concentrations (ethylene glycol), and temperatures. The materials were fully characterized by optical microscopy, scanning and transmission electron microscopy, infrared spectroscopy, powder X-ray diffraction, dynamic laser scattering, thermogravimetric analysis, and gas sorption. The impacts of the reaction parameters were rationalized and the mechanism for the formation of porous vaterite particles was suggested. It was possible to produce porous vaterite nanoparticles (200 nm) under the optimized conditions, which were further used as drug carrier to upload a model drug curcumin. The potential of using these vaterite particles for controlled drug release was demonstrated. Full article

Shape memory alloys (SMAs) are known for their exceptional mechanical properties, particularly their superior wear resistance compared to conventional alloys with similar surface hardness. Rare earth oxides are often used as additives to further improve these characteristics. This study investigates the effects of different CeO₂ (cerium dioxide) concentrations (0.01 wt.%, 0.1 wt.%, 0.5 wt.%, and 1.0 wt.%) on the properties of CuAlMnFe alloys produced via powder metallurgy (PM). Various analyses were performed, including scanning electron microscopy (SEM), Energy Dispersive Spectroscopy (EDS), X-ray diffraction (XRD), as well as hardness, wear, and corrosion tests. The increase in wear rate is closely related to the formation of precipitates from CeO₂ addition. Improvements in wear resistance and hardness are attributed to the effects of grain refinement and solid solution strengthening due to CeO₂. Specifically, the wear rate increased from 1.5 × 10⁻³ mm³/(Nm) to 3.4 × 10⁻³ mm³/(Nm) with higher CeO₂ content. Additionally, the friction coefficient of the CuAlMnFe alloy was reduced with CeO₂ addition, indicating enhanced frictional properties. The optimal CeO₂ concentration of 0.5% was found to improve grain uniformity, resulting in better wear resistance. Incorporating CeO₂ particles into CuAlMnFe alloy enhances hardness and reduces wear rate when used in appropriate amounts. Additionally, it exhibits superior corrosion resistance, as evidenced by a positive shift in corrosion potential in Tafel measurements in solutions and a decrease in corrosion current density. The C0.5 specimen showed the highest corrosion potential (E_corr, −588 V) and the lowest corrosion current density (i_corr, 6.17 μA/cm²) during electrochemical corrosion in 3.5 wt.% NaCl solution. Full article

Tribological performance is critical for the longevity and efficiency of machined components in industries such as aerospace, automotive, and biomedical. This study investigates whether electrical discharge machining recast layers can serve as a cost-effective and time-efficient alternative to conventional tungsten inert gas cladding coatings for enhancing surface properties. The samples were prepared using electrical discharge machining and tungsten inert gas cladding. For electrical discharge machining, various combinations of electrical and non-electrical parameters were applied using Taguchi’s L18 orthogonal array. Similarly, tungsten inert gas cladding coatings were prepared using a suitable combination of current, voltage, powder size, and speed. The samples were characterized using, scanning electron microscopy, optical microscopy, microhardness testing, tribological testing, energy-dispersive X-ray spectroscopy, X-ray diffraction analysis and profilometry. The electrical discharge machining recast layers exhibited superior tribological performance compared to tungsten inert gas cladding coatings. This improvement is attributed to the formation of carbides, such as TiC and Ti₆C_3.75. The coefficient of friction and specific wear rate were reduced by 11.11% and 1.57%, respectively, while microhardness increased by 10.93%. Abrasive wear was identified as the predominant wear mechanism. This study systematically compares electrical discharge machining recast layers with tungsten inert gas cladding coatings. The findings suggest that optimized electrical discharge machining recast layers can serve as effective coatings, offering cost and time savings. Full article

Bi₆Fe₂Ti₃O₁₈ (BFTO) ceramics were synthesized via a solid-state reaction route using stoichiometric amounts of Bi₂O₃, TiO₂, and Fe₂O₃ powders. A thermal analysis of the powder mixture was conducted to optimize the heat treatment parameters. Energy-dispersive X-ray spectroscopy (EDS) confirmed the conservation of the chemical composition following calcination. Final densification was achieved through hot pressing. The crystal structure of the sintered samples, examined via X-ray diffraction at room temperature, revealed a tetragonal symmetry for BFTO ceramics sintered at 850 °C. Electron backscatter diffraction (EBSD) provided detailed insight into the crystallographic orientation and microstructure. Broadband dielectric spectroscopy (BBDS) was employed to investigate the dielectric response of BFTO ceramics over a frequency range of 10 mHz to 10 MHz and a temperature range of −30 °C to +200 °C. The temperature dependence of the relative permittivity (ε_r) and dielectric loss tangent (tan δ) were measured within a frequency range of 100 kHz to 900 kHz and a temperature range of 25 °C to 570 °C. The impedance data obtained from the BBDS measurements were validated using the Kramers–Kronig test and modeled using the Kohlrausch–Williams–Watts (KWW) function. The stretching parameter (β) ranged from ~0.72 to 0.82 in the impedance formalism within the temperature range from 200 °C to 20 °C. Full article

The phase equilibria of the Si-C-Cu ternary system at 700 °C and 810 °C were experimentally investigated for the first time. Fifteen key alloys were prepared via powder metallurgy and analyzed using X-ray diffraction (XRD), scanning electron microscopy (SEM), and electron probe microanalysis (EPMA). Isothermal sections were constructed based on the identified equilibrium phases. At 700 °C, eight single-phase regions and six three-phase regions—(C)+(Cu)+hcp, (C)+hcp+γ-Cu₃₃Si₇, (C)+γ-Cu₃₃Si₇+SiC, γ-Cu₃₃Si₇+SiC+ε-Cu₁₅Si₄, SiC+ε-Cu₁₅Si₄+η-Cu₃Si(ht), and SiC+(Si)+η-Cu₃Si(ht)—were determined. At 810 °C, nine single-phase regions and seven three-phase regions were identified. The solubility of C and Si/Cu in the various phases was quantified and found to be significantly higher at 810 °C compared to 700 °C. Key differences include the presence of the bcc (β) and liquid phases at 810 °C. The results demonstrate that higher temperatures promote increased mutual solubility and reaction tendencies among Cu, C, and Si. Motivated by these findings, the influence of vacuum hot pressing parameters on SiC-fiber-reinforced Cu composites (SiC_f/Cu) was investigated. The optimal processing condition (1050 °C, 60 MPa, 90 min) yielded a high bending strength of 998.61 MPa, attributed to enhanced diffusion and interfacial bonding facilitated by the high-temperature phase equilibria. This work provides essential fundamental data for understanding interactions and guiding processing in SiC-reinforced Cu composites. Full article

This study reports on the magnetic properties of commercial cornflakes, which are primarily influenced by the iron content. An initial analysis of X-ray fluorescence on a brand of cornflakes evidenced the presence of a high concentration of Cl and up to 10.9 mg/100 g of Fe. After the extraction of iron from the cornflakes of two different brands, as iron filings, X-ray diffraction measurements indicate the presence of crystals of elemental iron, and no traces of other crystals of iron-derived compounds were found. The Fourier Transform Infrared analysis on the iron filings does not show any binding between iron and oxygen, which further discards the presence of iron oxides. The magnetic hysteresis loops of whole powdered cornflakes exhibit weak Langevin-like magnetizations, which principally correspond to the iron used as a fortification element. The diamagnetic behavior of the higher organic material content significantly attenuates this magnetic response. The hysteresis loops of the iron filings reached magnetic saturations 1% and 5% lower than those of a pure iron sample. Additionally, the indirect measurement of magnetic susceptibility of the iron filings by magneto-thermograms revealed only one Curie transition very close to 771 °C, which corresponds to pure elemental iron. Full article

Asphalt plant reclaimed powder is a common solid waste in road engineering. Reusing reclaimed powder as filler holds significant importance for environmental protection and resource conservation. The key factors affecting the feasibility of reclaimed powder reuse are its acidity/alkalinity and cleanliness. Traditional evaluation methods, such as the methylene blue test and plasticity index, can assess reclaimed powder properties to guide its recycling. However, these methods suffer from inefficiency, strong empirical dependence, and high variability. To address these limitations, this study proposes a rapid and precise evaluation method for reclaimed powder properties based on Fourier transform infrared spectroscopy (FTIR). To do so, five field-collected reclaimed powder samples and four artificial samples were evaluated. Scanning electron microscopy (SEM), X-ray fluorescence spectroscopy (XRF), and X-ray diffraction (XRD) were employed to characterize their microphase morphology, chemical composition, and crystal structure, respectively. Subsequently, FTIR was used to establish correlations between key acidity/alkalinity, cleanliness, and multiple characteristic peak intensities. Representative infrared characteristic peaks were selected, and a quantitative functional group index (Is) was proposed to simultaneously evaluate acidity/alkalinity and cleanliness. The results indicate that reclaimed powder primarily consists of tiny, crushed stone particles and dust, with significant variations in crystal structure and chemical composition, including calcium carbonate, silicon oxide, iron oxide, and aluminum oxide. Some samples also contained clay, which critically influenced the reclaimed powder properties. Since both filler acidity/alkalinity and cleanliness are affected by clay (silicon/carbon ratio determining acidity/alkalinity and aluminosilicate content affecting cleanliness), this study calculated four functional group indices based on FTIR absorption peaks, namely the Si-O-Si stretching vibration (1000 cm⁻¹) and the CO₃²⁻ asymmetric stretching vibration (1400 cm⁻¹). These indices were correlated with conventional testing results (XRF for acidity/alkalinity, methylene blue value, and pull-off strength for cleanliness). The results show that the Is index exhibited strong correlations (R² = 0.89 with XRF, R² = 0.80 with methylene blue value, and R² = 0.96 with pull-off strength), demonstrating its effectiveness in predicting both acidity/alkalinity and cleanliness. The developed method enhances reclaimed powder detection efficiency and facilitates high-value recycling in road engineering applications. Full article

Background: Precision medicine refers to the formulation of personalized drug regimens according to the individual characteristics of patients to achieve optimal efficacy and minimize adverse reactions. Additive manufacturing (AM), also known as three-dimensional (3D) printing, has emerged as an optimal solution for precision drug delivery, enabling customizable and the fabrication of multifunctional structures with precise control over morphology and release behavior in pharmaceutics. However, the influence of 3D printing parameters on the printed tablets, especially regarding in vitro and in vivo performance, remains poorly understood, limiting the optimization of manufacturing processes for controlled-release profiles. Objective: To establish the fabrication process of 3D-printed controlled-release tablets via comprehensively understanding the printing parameters using fused deposition modeling (FDM) combined with hot-melt extrusion (HME) technologies. HPMC-AS/HPC-EF was used as the drug delivery matrix and carbamazepine (CBZ) was used as a model drug to investigate the in vitro drug delivery performance of the printed tablets. Methodology: Thermogravimetric analysis (TGA) was employed to assess the thermal compatibility of CBZ with HPMC-AS/HPC-EF excipients up to 230 °C, surpassing typical processing temperatures (160–200 °C). The formation of stable amorphous solid dispersions (ASDs) was validated using differential scanning calorimetry (DSC), hot-stage polarized light microscopy (PLM), and powder X-ray diffraction (PXRD). A 15-group full factorial design was then used to evaluate the effects of the fan speed (20–100%), platform temperature (40–80 °C), and printing speed (20–100 mm/s) on the tablet properties. Response surface modeling (RSM) with inverse square-root transformation was applied to analyze the dissolution kinetics, specifically t_50% (time for 50% drug release) and Q_4h (drug released at 4 h). Results: TGA confirmed the thermal compatibility of CBZ with HPMC-AS/HPC-EF, enabling stable ASD formation validated by DSC, PLM, and PXRD. The full factorial design revealed that printing speed was the dominant parameter governing dissolution behavior, with high speeds accelerating release and low speeds prolonging release through porosity-modulated diffusion control. RSM quadratic models showed optimal fits for t_50% (R² = 0.9936) and Q_4h (R² = 0.9019), highlighting the predictability of release kinetics via process parameter tuning. This work demonstrates the adaptability of polymer composite AM for tailoring drug release profiles, balancing mechanical integrity, release kinetics, and manufacturing scalability to advance multifunctional 3D-printed drug delivery devices in pharmaceutics. Full article

In the rapidly evolving fields of materials science, catalysis, electronics, drug delivery, and environmental remediation, the development of effective substrates for molecular deposition has become increasingly crucial. Ordered mesoporous silica materials have garnered significant attention due to their unique structural properties and exceptional potential as substrates for molecular immobilization across these diverse applications. This study compares three mesoporous silica powders: MCM-41, SBA-15, and SBA-16. A multi-technique characterization approach was employed, utilizing low- and wide-angle X-ray diffraction (XRD), nitrogen physisorption, and transmission electron microscopy (TEM) to elucidate the structure–property relationships of these materials. XRD analysis confirmed the amorphous nature of silica frameworks and revealed distinct pore symmetries: a two-dimensional hexagonal (P6mm) structure for MCM-41 and SBA-15, and three-dimensional cubic (Im$\overline{3}$m) structure for SBA-16. Nitrogen sorption measurements demonstrated significant variations in textural properties, with MCM-41 exhibiting uniform cylindrical mesopores and the highest surface area, SBA-15 displaying hierarchical meso- and microporosity confirmed by NLDFT analysis, and SBA-16 showing a complex 3D interconnected cage-like structure with broad pore size distribution. TEM imaging provided direct visualization of particle morphology and internal pore architecture, enabling estimation of lattice parameters and identification of structural gradients within individual particles. The integration of these complementary techniques proved essential for comprehensive material characterization, particularly for MCM-41, where its small particle size (45–75 nm) contributed to apparent structural inconsistencies between XRD and sorption data. This integrated analytical approach provides valuable insights into the fundamental structure–property relationships governing ordered mesoporous silica materials and demonstrates the necessity of combined characterization strategies for accurate structural determination. Full article