Search Results (2,101)

Lignin used in this work was isolated from sapele (Entandrophragma cylindricum) wood through a hybrid pulping process using soda/ethanol as pulping liquor and denoted soda-oxyethylated lignin (SOL). SOL was mixed with a polyethylene glycol (PEG)–glycerol mixture (80/20 v/v) as liquefying solvent with 98% wt. sulfur acid as catalyst, and the mixture was taken to boil at 140 °C for 2, 2.5, and 3 h. Three bio-polyols LBP1, LBP2, and LBP3 were obtained, and each of them exhibited a high proportion of -OH groups. Lignin-based polyurethane foams (LBPUFs) were prepared using the bio-polyols obtained with a toluene diisocyanate (TDI) prepolymer by the one-shot method. Gel permeation chromatography (GPC), Fourier transform infrared spectroscopy (FTIR), and carbon-13 nuclear magnetic resonance spectroscopy (¹³C NMR) were used characterize lignin in order to determine viscosity, yield, and composition and to characterize their structure. The PEG-400–glycerol mixture was found to react with the lignin bio-polyols’ phenolic -OHs. The bio-polyols’ viscosity was found to increase as the liquefaction temperature increased, while simultaneously their molecular weights decreased. All the NCO groups were eliminated from the samples, which had high thermal stability as the liquefaction temperature increased, leading to a decrease in cell size, density, and crystallinity and an improvement in mechanical performance. Based on these properties, especially the presence of some aromatic rings in the bio-polyols, the foams produced can be useful in automotive applications and for floor carpets. Full article

Potassium bromide (KBr) thin films were deposited by resistive thermal evaporation at substrate temperatures ranging from 50 °C to 250 °C to systematically elucidate the temperature-dependent evolution of their physical properties. Structural, morphological, and optical characteristics were examined by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), and Fourier transform infrared spectroscopy (FTIR). The results reveal a complex, non-monotonic response to temperature rather than a simple linear trend. As the substrate temperature increases, growth evolves from a mixed polycrystalline texture to a pronounced (200) preferred orientation. Morphological analysis shows that the film surface is smoothest at 150 °C, while the microstructure becomes densest at 200 °C. These structural variations directly modulate the optical constants: the refractive index attains its highest values in the 150–200 °C window, approaching that of bulk KBr. Cryogenic temperature (6 K) FTIR measurements further demonstrate that suppression of multi-phonon absorption markedly enhances the infrared transmittance of the films. Taken together, the data indicate that 150–200 °C constitutes an optimal process window for fabricating KBr films that combine superior crystallinity, low defect density, and high packing density. This study elucidates the temperature-driven structure–property coupling and offers valuable guidance for optimizing high-performance infrared and cryogenic optical components. Full article

This study presents the development of Cu-doped NiMo/TiO₂ photoelectrocatalysts for simultaneous green hydrogen production and pharmaceutical pollutant removal under simulated solar irradiation. The catalysts were synthesized via wet impregnation (15 wt.% total metal loading with 0.6 wt.% Cu) and thermally treated at 400 °C and 900 °C to investigate structural transformations and catalytic performance. Comprehensive characterization (XRD, BET, SEM, XPS) revealed phase transitions, enhanced crystallinity, and redistribution of redox states upon Cu incorporation, particularly the formation of NiTiO₃ and an increase in oxygen vacancies. Crystallite sizes for anatase, rutile, and brookite ranged from 21 to 47 nm at NiMoCu400, while NiMoCu900 exhibited only the rutile phase with 55 nm crystallites. BET analysis showed a surface area of 44.4 m²·g⁻¹ for NiMoCu400, and electrochemical measurements confirmed its higher electrochemically active surface area (ECSA, 2.4 cm²), indicating enhanced surface accessibility. In contrast, NiMoCu900 exhibited a much lower BET surface area (1.4 m²·g⁻¹) and ECSA (1.4 cm²), consistent with its inferior photoelectrocatalytic performance. Compared to previously reported binary NiMo/TiO₂ systems, the ternary NiMoCu/TiO₂ catalysts demonstrated significantly improved hydrogen production activity and more efficient photoelectrochemical degradation of paracetamol. Specifically, NiMoCu400 showed an anodic peak current of 0.24 mA·cm⁻² for paracetamol oxidation, representing a 60% increase over NiMo400 and a cathodic current of −0.46 mA·cm⁻² at −0.1 V vs. RHE under illumination, nearly six times higher than the undoped counterpart (–0.08 mA·cm⁻²). Mott–Schottky analysis further revealed that NiMoCu400 retained n-type behavior, while NiMoCu900 exhibited an unusual inversion to p-type, likely due to Cu migration and rutile-phase-induced realignment of donor states. Despite its higher photosensitivity, NiMoCu900 showed negligible photocurrent, confirming that structural preservation and surface redox activity are critical for photoelectrochemical performance. This work provides mechanistic insight into Cu-mediated photoelectrocatalysis and identifies NiMoCu/TiO₂ as a promising bifunctional platform for integrated solar-driven water treatment and sustainable hydrogen production. Full article

Steel pickling sludge serves as a valuable iron source for synthesizing Fe-based catalysts in heterogeneous advanced oxidation processes (AOPs). Here, MoS₂@CoFe₂O₄ catalyst derived from steel pickling sludge was prepared via a facile solvothermal approach and utilized to activate peroxymonosulfate (PMS) for tetracycline hydrochloride (TCH) degradation. Comprehensive characterization using scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and X-ray diffraction (XRD) confirmed the supported microstructure, composition, and crystalline structure of the catalyst. Key operational parameters—including catalyst dosage, PMS concentration, and initial pH—were systematically optimized, achieving 81% degradation efficiency within 30 min. Quenching tests and EPR analysis revealed ∙SO₄^‒ as the primary oxidative species, while the catalyst maintained high stability and reusability across cycles. TCH degradation primarily occurs through hydroxylation, decarbonylation, ring-opening, and oxidation reactions. This study presents a cost-effective strategy for transforming steel pickling sludge into a high-performance Fe-based catalyst, demonstrating its potential for practical AOP applications. Full article

Background/Objectives: Magnetic nanoparticles, particularly iron oxide-based materials, such as magnetite (Fe₃O₄), have gained significant attention as contrast agents in medical imaging This study aimsto syntheze and characterize Fe₃O₄-based core–shell nanostructures, including Fe₃O₄@TiO₂ and Fe₃O₄@SiO₂, and to evaluate their potential as tunable contrast agents for diagnostic imaging. Methods: Fe₃O₄, Fe₃O₄@TiO₂, and Fe₃O₄@SiO₂ nanoparticles were synthesized via co-precipitation at varying temperatures from iron salt precursors. Fourier transform infrared spectroscopy (FTIR) was used to confirm the presence of Fe–O bonds, while X-ray diffraction (XRD) was employed to determine the crystalline phases and estimate average crystallite sizes. Morphological analysis and particle size distribution were assessed by scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDX) and transmission electron microscopy (TEM). Magnetic properties were investigated using vibrating sample magnetometry (VSM). Results: FTIR spectra exhibited characteristic Fe–O vibrations at 543 cm⁻¹ and 555 cm⁻¹, indicating the formation of magnetite. XRD patterns confirmed a dominant cubic magnetite phase, with the presence of rutile TiO₂ and stishovite SiO₂ in the coated samples. The average crystallite sizes ranged from 24 to 95 nm. SEM and TEM analyses revealed particle sizes between 5 and 150 nm with well-defined core–shell morphologies. VSM measurements showed saturation magnetization (Ms) values ranging from 40 to 70 emu/g, depending on the synthesis temperature and shell composition. The highest Ms value was obtained for uncoated Fe₃O₄ synthesized at 94 °C. Conclusions: The synthesized Fe₃O₄-based core–shell nanomaterials exhibit desirable structural, morphological, and magnetic properties for use as contrast agents. Their tunable magnetic response and nanoscale dimensions make them promising candidates for advanced diagnostic imaging applications. Full article

As the most unstable crystalline form of calcium carbonate, vaterite is rarely found in nature due to being highly prone to phase transitions. However, its high specific surface area, excellent biocompatibility, and high solubility properties have led to a research boom and the following breakthroughs in the last two decades: (1) From primitive calculations and spectroscopic analyses to modern multidimensional research methods combining calculations and experiments, the crystal structure of vaterite has turned from early identifications in orthorhombic and hexagonal crystal systems to a complex polymorphic structure within the monoclinic crystal system. (2) The formation process of vaterite not only conforms to the classical crystal growth theory but also encompasses the nanoparticle aggregation theory, which incorporates the concepts of oriented nanoparticle assembly and mesoscale transformation. (3) Regardless of the conditions, the formation of vaterite depends on an excess of CO₃²⁻ relative to Ca²⁺, and its stability duration relates to preservation conditions. (4) Vaterite demonstrates significant value in biomedical applications—including bone repair scaffolds, targeted drug carriers, and antibacterial coating materials—leveraging its porous structure, high specific surface area, and exceptional biocompatibility. While it also shows utility in environmental pollutant adsorption and general coating technologies, the current research remains predominantly concentrated on its medical applications. Currently, the rapid transformation of vaterite presents the primary limitation for its industrial application. Future research should prioritize investigating its formation kinetics and stability. Full article

A scalable synthesis of two-dimensional titanium nitride chloride (TiNCl) via flash Joule heating (FJH) using titanium tetrachloride (TiCl₄) precursor has been developed. This single-step method overcomes traditional synthesis challenges, including high energy consumption, multi-step procedures, and hazardous reagent requirements. The structural and chemical properties of the synthesized TiNCl were characterized through multiple analytical techniques. X-ray diffraction (XRD) patterns confirmed the presence of TiNCl phase, while Raman spectroscopy data showed no detectable oxide impurities. Fourier transform infrared spectroscopy (FTIR) analysis revealed characteristic Ti–N stretching vibrations, further confirming successful titanium nitride synthesis. Transmission electron microscopy (TEM) imaging revealed thin, plate-like nanostructures with high electron transparency. These analyses confirmed the formation of highly crystalline TiNCl flakes with nanoscale dimensions and minimal structural defects. The material exhibits excellent structural integrity and phase purity, demonstrating potential for applications in photocatalysis, electronics, and energy storage. This work establishes FJH as a sustainable and scalable approach for producing MXenes with controlled properties, facilitating their integration into emerging technologies. Unlike conventional methods, FJH enables rapid, energy-efficient synthesis while maintaining material quality, providing a viable route for industrial-scale production of two-dimensional materials. Full article

In this study, we report the synthesis of Te and Ag₂Te micron-sized rods (MRs) via a controlled hot-injection-based quenching process, enabling the control of rod morphology and enhanced crystallinity. Structural analysis confirmed that the synthesized Te MRs exhibit a trigonal phase, growing along the (110) direction, while Ag₂Te MRs undergo a phase transformation into a monoclinic structure upon Ag doping. A simple and scalable photodetector (PD) was fabricated by drop-casting Te and Ag₂Te MRs onto PET plastic films, followed by the application of Ag paste electrodes. The PD demonstrated room-light-induced photocurrent responses, which increased significantly upon mechanical bending due to the formation of additional conductive pathways between MRs. The Ag₂Te-based bending sensor exhibited a fivefold enhancement in photocurrent compared to its Te counterpart and maintained high stability over 1000 bending cycles. These results highlight the potential of Te and Ag₂Te MRs for use in flexible and wearable motion-sensing technologies, offering a simple yet effective approach for integrating 1D telluride nanostructures into scalable optoelectronic applications. Full article

This study explores using polyvinylidene fluoride (PVDF) membranes modified with multi-walled carbon nanotubes (MWCNTs) to treat simulated and industrial brine from coal power stations. The MWCNTs were acid-treated and characterized using Fourier Transform Infrared Spectroscopy (FTIR), Raman, and nitrogen sorption at 77 K, Thermogravimetric analysis (TGA), and Transmission electron microscopy (TEM). The desired membranes were obtained by casting from a solution of N-Methyl-2-pyrrolidone, PVDF, various weight percentages of MWCNTs, and a small amount of polyvinylpyrrolidone. The acid treatment of the MWCNTs introduced oxygen moieties on the surface, and increased pore volume and surface area while maintaining crystallinity and structural integrity remain preserved. The maximum rejection rate achieved was 41.82% with 1 wt.% of acid-treated MWCNTs in the PVDF membrane. Acid-treated MWCNTs loaded membranes had an improved rejection rate, which was 5× higher than membranes without MWCNTs. Full article

Polylactic acid (PLA) is a renewable biopolymer that has attracted considerable interest due to its ability to replace petroleum-based synthetic polymers, thereby offering a more sustainable alternative to global environmental concerns. This study focused on evaluating the effect of catalyst concentration and reaction time on the efficiency of PLA synthesis via the Ring-Opening Polymerization (ROP) technique. The process involved a lactic acid esterification stage (using 88% lactic acid) to obtain lactide, employing 40% and 60% (v/v) sulfuric acid concentrations, followed by polymerization at various reaction times (10, 15, 20, and 30 min). Analysis of variance (ANOVA) results revealed that the 40% catalyst concentration had a statistically significant effect on polymer yield (p = 0.032), whereas reaction time showed no statistical significance (p = 0.196), although the highest yields were recorded at 10 and 15 min. Fourier Transform Infrared Spectroscopy (FTIR) confirmed the presence of the characteristic functional groups of PLA, and Differential Scanning Calorimetry (DSC) revealed a semi-crystalline structure with a high melting temperature, indicating good thermal stability. These results validate the viability of PLA as a functional and sustainable biopolymer. Full article

A review of the literature on polymorphic transformations by milling on pharmaceutical materials was carried out. The available information on 18 pharmaceutical materials was compiled. In particular, when data are available, the starting and final crystalline forms, their enantiotropic or monotropic relationship, the glass transition temperature of the compound and its melting temperature, the experimental observation of a transient or partial amorphization of compounds, and the transformation kinetics make it possible to suggest a two-step transformation mechanism. First, an amorphization occurs under milling of the starting polymorphic form. Secondly, a recrystallization of the amorphous form occurs towards the final form. The observed transformation kinetics are due to the fact that the recrystallization of the amorphous material towards the final form depends on the accidental formation of a cluster of this form during milling. Moreover, the observation of the transient amorphous form depends on the relative position of the glass transition temperature of the material with respect to the milling temperature. This mechanism seems to be independent of the enantiotropic or monotropic character of the polymorphic forms involved in the transformation. Full article

The color of flowers in Osmanthus fragrans is regulated by carotenoid metabolism. The orange-red variety, Dangui, is believed to have evolved from the yellow variety, Jingui, through a natural bud mutation. This study uses the Jingui cultivar ‘Jinqiu Gui’ (JQG) and its bud mutation cultivar ‘Huolian Jindan’ (HLJD) as materials, combining genome resequencing, ultrastructural observation, targeted metabolomics, and transcriptomic analysis to elucidate the molecular and cellular mechanisms underlying flower color variation. Phylogenetic analysis confirms that HLJD is a natural bud mutation of JQG. Ultrastructural observations reveal that during petal development, chromoplasts are transformed from proplastids. In HLJD petals, starch granules degrade more slowly and exhibit abnormal morphology, resulting in chromoplasts displaying crystalline, tubular, and fibrous composite structures, in contrast to the typical spherical plastoglobuli found in JQG. Targeted metabolomics identified 34 carotenoids, showing significant increases in the levels of ε-carotene, γ-carotene, α-carotene, and β-carotene in HLJD petals compared to JQG, with these levels continuing to accumulate throughout the flowering process, while the levels of the cleavage products α-ionone and β-ionone decrease. Transcriptomic analysis indicates that carotenoid metabolic pathway genes do not correlate directly with the phenotype; however, 49 candidate genes significantly associated with pigment accumulation were identified. Among these, the expression of genes such as glycoside hydrolases (LYG036752, etc.), sucrose synthase (LYG010191), and glucose-1-phosphate adenylyltransferase (LYG003610) are downregulated in HLJD. This study proposes for the first time the pathway of “starch degradation delay → chromoplast structural abnormalities → carotenoid cleavage inhibition” for deepening flower color, providing a new theoretical model for the metabolic regulation of carotenoids in non-photosynthetic tissues of plants. This research not only identifies key target genes (such as glycoside hydrolases) for the color breeding of O. fragrans but also establishes a theoretical foundation for the color enhancement of other ornamental plants. Full article

The role and performance of desert sand in alkali-activated mortar remain insufficiently understood. To address this knowledge gap, this study systematically investigates the fluidity, mechanical properties, and microscopic morphology of alkali-activated mortar with varying desert sand substitution rates (DSRR, 0–100%). The key findings reveal that a low DSRR (10–20%) enhances mortar fluidity and reduces drying shrinkage, though at the cost of reduced compressive strength. At 40% DSRR, the mortar exhibits elevated porosity (12.3%) and diminished compressive strength (63 MPa). Notably, complete substitution (100% DSRR) yields a well-structured matrix with optimized pore distribution, characterized by abundant gel micropores, and achieves a compressive strength of 76 MPa. These results demonstrate that desert sand can fully replace river sand in alkali-activated mortar formulations without compromising performance. Microstructural analysis confirms that desert sand actively participates in the alkali activation process. Specifically, the increased Ca²⁺ content facilitates the transformation of amorphous gels into crystalline phases. It also found that desert sand could make the fly ash more soluble, affecting the alkali activation reaction. Full article

Herein, electrospun nanofibers composed of polyaniline (PANI), polyethylene oxide (PEO), and Luffa cylindrica (LC) cellulose, reinforced with titanium dioxide (TiO₂) nanoparticles, were synthesized via electrospinning to investigate the effect of TiO₂ nanoparticles on PANI/PEO/LC nanocomposites and the effect of conductivity on nanofiber morphology. Cellulose extracted from luffa was added to the PANI/PEO copolymer solution, and two different ratios of TiO₂ were mixed into the PANI/PEO/LC biocomposite. The morphological, vibrational, and thermal characteristics of biocomposites were systematically investigated using scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). As anticipated, the presence of TiO₂ enhanced the electrical conductivity of biocomposites, while the addition of Luffa cellulose further improved the conductivity of the cellulose-based nanofibers. FTIR analysis confirmed chemical interactions between Luffa cellulose and PANI/PEO matrix, as evidenced by the broadening of the hydroxyl (OH) absorption band at 3500–3200 cm⁻¹. Additionally, the emergence of characteristic peaks within the 400–1000 cm⁻¹ range in the PANI/PEO/LC/TiO₂ spectra signified Ti–O–Ti and Ti–O–C vibrations, confirming the incorporation of TiO₂ into the biocomposite. SEM images of the biocomposites reveal that the thickness of nanofibers decreases by adding Luffa to PANI/PEO nanofibers because of the nanofibers branching. In addition, when blending TiO₂ nanoparticles with the PANI/PEO/LC biocomposite, this increment continued and obtained thinner and smother nanofibers. Furthermore, the incorporation of cellulose slightly improved the crystallinity of the nanofibers, while TiO₂ contributed to the enhanced crystallinity of the biocomposite according to the XRD and DCS results. Similarly, the TGA results supported the DSC results regarding the increasing thermal stability of the biocomposite nanofibers with TiO₂ nanoparticles. These findings demonstrate the potential of PANI/PEO/LC/TiO₂ nanofibers for advanced applications requiring conductive and structurally optimized biomaterials, e.g., for use in humidity or volatile organic compound (VOC) sensors, especially where flexibility and environmental sustainability are required. Full article

In this work, we report a green synthesis of zinc oxide (ZnO) nanoparticles using aqueous and ethanolic extracts of Tradescantia spathacea (purple maguey) as bioreducing and stabilizing agents, which are plant extracts not previously employed for metal oxide nanoparticle synthesis. This method provides an efficient, eco-friendly, and reproducible route to obtain ZnO nanoparticles, while minimizing environmental impact compared to conventional chemical approaches. The extracts were prepared following a standardized protocol, and their phytochemical profiles, including total phenolics, flavonoids, and antioxidant capacity, were quantified via UV-Vis spectroscopy to confirm their reducing potential. ZnO nanoparticles were synthesized using zinc acetate dihydrate as a precursor, with variations in pH and precursor concentration in both aqueous and ethanolic media. UV-Vis spectroscopy confirmed nanoparticle formation, while X-ray diffraction (XRD) revealed a hexagonal wurtzite structure with preferential (101) orientation and lattice parameters a = b = 3.244 Å, c = 5.197 Å. Scanning electron microscopy (SEM) showed agglomerated morphologies, and Fourier transform infrared spectroscopy (FTIR) confirmed the presence of phytochemicals such as quercetin, kaempferol, saponins, and terpenes, along with Zn–O bonding, indicating surface functionalization. Zeta potential measurements showed improved dispersion under alkaline conditions, particularly with ethanolic extracts. This study presents a sustainable synthesis strategy with tunable parameters, highlighting the critical influence of precursor concentration and solvent environment on ZnO nanoparticle formation. Notably, aqueous extracts promote ZnO synthesis at low precursor concentrations, while alkaline conditions are essential when using ethanolic extracts. Compared to other green synthesis methods, this strategy offers control and reproducibility and employs a non-toxic, underexplored plant source rich in phytochemicals, potentially enhancing the crystallinity, surface functionality, and application potential of the resulting ZnO nanoparticles. These materials show promise for applications in photocatalysis, in antimicrobial coatings, in UV-blocking formulations, and as functional additives in optoelectronic and environmental remediation technologies. Full article