Search Results (1,225)

Thermoelectric (TE) materials represent a critical frontier in sustainable energy conversion technologies, providing direct thermal-to-electrical energy conversion with solid-state reliability. The optimizations of TE performance demand a nuanced comprehension of structure–property relationships across diverse length scales. This review summarizes established and emerging spectroscopic and microscopic techniques used to characterize inorganic and polymer TE materials, specifically poly(3,4-ethylenedioxythiophene): poly(styrenesulfonate) (PEDOT:PSS). For inorganic TE, ultraviolet–visible (UV–Vis) spectroscopy, energy-dispersive X-ray (EDX) spectroscopy, and X-ray photoelectron spectroscopy (XPS) are widely applied for electronic structure characterization. For phase analysis of inorganic TE materials, Raman spectroscopy (RS), electron energy loss spectroscopy (EELS), and nuclear magnetic resonance (NMR) spectroscopy are utilized. For analyzing the surface morphology and crystalline structure, chemical scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD) are commonly used. For polymer TE materials, ultraviolet−visible–near-infrared (UV−Vis−NIR) spectroscopy and ultraviolet photoelectron spectroscopy (UPS) are generally employed for determining electronic structure. For functional group analysis of polymer TE, attenuated total reflectance–Fourier-transform infrared (ATR−FTIR) spectroscopy and RS are broadly utilized. XPS is used for elemental composition analysis of polymer TE. For the surface morphology of polymer TE, atomic force microscopic (AFM) and SEM are applied. Grazing incidence wide-angle X-ray scattering (GIWAXS) and XRD are employed for analyzing the crystalline structures of polymer TE materials. These techniques elucidate electronic, structural, morphological, and chemical properties, aiding in optimizing TE properties like conductivity, thermal stability, and mechanical strength. This review also suggests future research directions, including in situ methods and machine learning-assisted multi-dimensional spectroscopy to enhance TE performance for applications in electronic devices, energy storage, and solar cells. Full article

Expansive soils present a significant geotechnical challenge due to their pronounced volume changes with moisture variations, leading to substantial infrastructure damage. This study investigates the efficacy of thermal stabilization in mitigating the swell potential and compressibility of a high-plasticity, kaolinite-rich clay from Al Ghat, Saudi Arabia. As well, the changes in basic properties including consistency limits, specific gravity, and compaction characteristics were studied and highlighted. Microstructural studies using X-ray diffraction (XRD), Scanning electron microscopy (SEM), and Energy-dispersive X-ray spectroscopic (EDX) were performed to trace the structural changes and interpret the achieved improvement. Soil specimens were subjected to heat treatment at levels of 200 °C, 400 °C, and 600 °C for two hours, after which their geotechnical and microstructural properties were comprehensively evaluated. The results demonstrate a direct correlation between increasing temperature and the reduction in expansive behavior. Treatment at 600 °C caused a substantial decrease in the plasticity index from 27.00 to 2.94. Correspondingly, oedometer tests showed that the free swell was reduced from 6% to nearly zero, and the swelling pressure was eliminated, dropping from 250 kPa to 0 kPa. XRD analysis confirmed kaolinite decomposition through dehydroxylation, producing metakaolin with diminished water absorption capacity. SEM further revealed significant particle aggregation and the formation of a coarser soil fabric. The findings confirm that heat treatment at temperatures of 400 °C and above is a highly effective method for permanently stabilizing kaolinitic expansive soils, rendering them suitable for construction applications. Full article

Background/Objectives: This study aimed to synthesize a novel, high-molecular-weight acyclic heterocyclic compound, compound 5, via a one-pot reaction between Trichloroisocyanuric acid (TCCA) and ethanolamine, and evaluate its anticancer, antioxidant, and antifungal activities. Methods: Its complex tetrameric structure, assembled through N-N linkages, was unequivocally confirmed by a full suite of spectroscopic techniques including IR, ¹H & ¹³C NMR, ²D-NMR, and high-resolution mass spectrometry (LC/Q-TOF/MS). The MTT assay was used to assess the anticancer activity of compound 5 against four different human cancer cell lines. Results: The findings indicate that human colon (HT29) and ovarian (OVCAR3) cancer cells were sensitive to the treatment, whereas brain (glioblastoma) (T98G) cancer cells were resistant. The most pronounced cytotoxic effect was observed in pancreatic (MiaPaCa2) cancer cells. Notably, compound 5 exhibited potent antifungal properties, achieving 100% inhibition of the pathogenic water mould Saprolegnia parasitica zoospores at 100 µM after 10 min. Molecular docking studies corroborated the biological data, revealing a high binding affinity for key cancer and fungal targets (Thymidylate Synthase and CYP51), providing a strong mechanistic basis for its observed activities. Conclusions: These findings establish compound 5 as a promising dual-action agent with significant potential as both a targeted anticancer lead and an eco-friendly antifungal for applications in aquaculture. Full article

Driven by environmental concerns and aligned with the principles of the circular economy, urban plastic waste—including packaging materials, disposable items, non-functional objects, and industrial scrap—is increasingly being collected, recycled, and marketed as a potential substitute for virgin polymers. However, the use of recycled polymers introduces uncertainties that can significantly affect both the durability and the further recyclability of the resulting products. This paper demonstrates how spectroscopic analysis in the mid-infrared (MIR) and near-infrared (NIR) regions can be applied well beyond the basic identification of the main polymeric component, typically performed during the sorting stage of recycling processes. A detailed interpretation of spectral data, based on well-established correlations between spectroscopic response and material structure, enables the classification of recycled polymers according to specific physicochemical properties, such as chemical composition, molecular architecture, and morphology. In this context, infrared spectroscopy not only provides a reliable comparison with the corresponding virgin polymer references but also proves particularly effective in assessing the homogeneity of recycled materials and the reproducibility of their properties—factors not inherently guaranteed due to the variability of input sources. As a case study, we present a robust protocol for determining the polypropylene content in recycled polyethylene samples. Full article

This study developed the RATS (Range-Aware Two-Stage) modeling approach to establish mechanistic foundations for feed ratio optimization in fluoroelastomers. Using ¹⁹F NMR spectroscopic analysis, the approach decomposes complex composition–property relationships into sequential processes: monomer feed ratios to NMR-derived structural features, and structural features to properties, enabling mechanistic pathway analysis through quantifiable structural intermediates. Using 52 industrial datasets, RATS achieved an average R² of 0.90 across four property predictions, representing a 0.14 improvement over direct modeling and a 28% reduction in prediction error. The approach identified 72 systematic transmission pathways, including promoting effects of PMVE-series structures (+0.220 influence strength) and inhibitory effects of VDF monomers (−0.219 influence strength), through quantified model parameter analysis. This methodology provides a practical analytical tool for mechanism-driven feed ratio optimization, facilitating the transition from empirical trial-and-error to systematic, data-guided fluoroelastomer formulation. Full article

This study systematically investigates the solvent-dependence of copper(II) extraction using di-2-ethylhexyl phosphoric acid (D2EHPA) across a range of polar and non-polar diluents, including chloroform, dichloromethane, carbon tetrachloride, cyclohexane, 1-octanol, and methyl isobutyl ketone (MIBK). Through analysis of extraction constants and distribution coefficients at varying pH levels, it was demonstrated that solvent polarity and dipole moment critically influenced the coordination geometry and extraction efficiency of the Cu(II)-D2EHPA complex. Notably, the highest extraction efficiencies were exhibited by 1-octanol and cyclohexane. A solvent-dependent structural transition was revealed by Ultraviolet–Visible (UV) spectroscopic evidence: tetrahedral coordination was dominated in polar media, while square planar geometries prevailed in non-polar environments. These findings establish a direct correlation between diluent properties and the extractant’s performance, offering a mechanistic framework for optimizing industrial-scale copper recovery processes. The insights gained highlight the importance of solvent selection in tailoring metal extraction systems for specific applications. Full article

This study investigates the structural and magnetic properties of CoFe₂O₄ nanoparticles prepared by five different synthesis methods: coprecipitation, ultrasound-assisted coprecipitation, coprecipitation coupled with mechanochemical treatment, microemulsion and microwave-assisted hydrothermal synthesis. The produced powders were additionally functionalized with starch to improve biocompatibility and colloidal stability. The starch-coating procedure itself by sonication in starch solution, as well as its result, affects the structural and magnetic properties of functionalized nanoparticles. The resulting changes of properties in the process of ligand addition depend significantly on the starting nanoparticles, or rather, on the method of their synthesis. The structural, magnetic and spectroscopic properties of the resulting materials were systematically investigated using X-ray diffraction (XRD), Raman spectroscopy, Mössbauer spectroscopy and magnetic measurements. Taken together, XRD, Raman and Mössbauer spectroscopy show that starch deposition reduces structural disorder and internal stress, resulting in nanoparticles with a more uniform size distribution. These changes, in turn, affect all magnetic properties—magnetization, coercivity and magnetic anisotropy. Magnetic responses are preserved what is desirable for future biomedical applications. This work emphasizes the importance of surface modification for tailoring the properties of magnetic nanoparticles while maintaining their desired functionality. Full article

Due to its multiple amino groups, triethylenetetramine (TETA) can be used as an effective formaldehyde scavenger contributing to the reduction in formaldehyde emission from plywood. This study aimed to evaluate the effect of small TETA loadings on the properties of urea-formaldehyde (UF) resin and the performance of the resulting plywood. Adhesive mixtures containing 0%, 0.5%, 1.0%, and 1.5% TETA were prepared and characterized in terms of pH, viscosity, solids content, and gel time. The incorporation of TETA significantly increased adhesive pH and gel time, while viscosity and solid content were not significantly affected. The analysis of formaldehyde content and spectroscopic and thermogravimetric analyses of the cured adhesives showed reduced formaldehyde content, changes in chemical structure, and enhanced thermal stability at lower temperatures but accelerated degradation at higher temperatures. Formaldehyde emission from plywood was reduced; however, bonding quality and mechanical performance decreased with higher TETA content. Nevertheless, the wet shear strength of all variants exceeded 1 N/mm². Adhesive formulation containing 0.5% TETA was selected as the optimal variant, providing environmental benefits while maintaining satisfactory plywood performance. Full article

In recent years, apatite-based materials have garnered significant interest, particularly for applications in tissue engineering. Apatite is most commonly employed as a coating for metallic implants, as a component in composite materials, and as scaffolds for bone and dental tissue regeneration. Among its various forms, hydroxyapatite (HAP) is the most widely used, owing to its natural occurrence in human and animal hard tissues. An emerging area of research involves the use of fluoride-substituted apatite, particularly fluorapatite (FAP), which can serve as a direct fluoride source at the implant site, potentially offering several biological and therapeutic advantages. However, substituting HAP with FAP may lead to unforeseen changes in material behavior due to the differing physicochemical properties of these two calcium phosphate phases. This study investigates the effects of replacing hydroxyapatite with fluorapatite in ceramic–polymer composite materials incorporating β-1,3-glucan as a bioactive polymeric binder. The β-1,3-glucan polysaccharide was selected for its proven biocompatibility, biodegradability, and ability to form stable hydrogels that promote cellular interactions. Nitrogen adsorption analysis revealed that FAP/glucan composites had a significantly lower specific surface area (0.5 m²/g) and total pore volume (0.002 cm³/g) compared to HAP/glucan composites (14.15 m²/g and 0.03 cm³/g, respectively), indicating enhanced ceramic–polymer interactions in fluoride-containing systems. Optical profilometry measurements showed statistically significant differences in profile parameters (e.g., Rp: 134 μm for HAP/glucan vs. 352 μm for FAP/glucan), although average roughness (Ra) remained similar (34.1 vs. 27.6 μm, respectively). Microscopic evaluation showed that FAP/glucan composites had smaller particle sizes (1 μm) than their HAP counterparts (2 μm), despite larger primary crystal sizes in FAP, as confirmed by TEM. XRD analysis indicated structural differences between the apatites, with FAP exhibiting a reduced unit cell volume (524.6 ų) compared to HAP (528.2 ų), due to substitution of hydroxyl groups with fluoride ions. Spectroscopic analyses (FTIR, Raman, ³¹P NMR) confirmed chemical shifts associated with fluorine incorporation and revealed distinct ceramic–polymer interfacial behaviors, including an upfield shift of PO₄³⁻ bands (964 cm⁻¹ in FAP vs. 961 cm⁻¹ in HAP) and OH vibration shifts (3537 cm⁻¹ in FAP vs. 3573 cm⁻¹ in HAP). The glucan polymer showed different hydrogen bonding patterns when combined with FAP versus HAP, as evidenced by shifts in polymer-specific bands at 888 cm⁻¹ and 1157 cm⁻¹, demonstrating that fluoride substitution significantly influences ceramic–polymer interactions in these bioactive composite systems. Full article

Silicon-doped C₆₀ fullerenes represent a distinctive class of heterofullerenes with tunable structural, electronic, and chemical properties arising from substitutional incorporation of Si atoms into the carbon cage. This review provides a comprehensive analysis of substitutional Si–C₆₀ systems and their endohedral and exohedral complexes, with emphasis on synthesis strategies, structural features, and theoretical investigations. Experimental methods, including laser vaporization and arc discharge of Si-containing graphite targets, have enabled the preparation of Si-doped fullerenes, although challenges remain in controlling the dopant number, position, and distribution. Computational studies, dominated by density functional theory and molecular dynamics simulations, elucidate the effects of Si substitution on cage geometry, HOMO–LUMO modulation, charge localization, aromaticity, and finite-temperature stability. Exohedral functionalization and endohedral encapsulation of Si-doped cages significantly enhance their potential for applications in sensing, catalysis, energy storage, and nanomedicine. Si incorporation consistently strengthens adsorption of small molecules, pharmaceuticals, biomolecules, and environmental pollutants, often transforming weak physisorption into strong chemisorption with pronounced electronic and spectroscopic changes. The synergistic insights from experimental and theoretical work establish Si-doped fullerenes as versatile, electronically responsive nanoplatforms, offering a balance between stability, tunability, and reactivity, and highlighting future opportunities for targeted synthesis and application-specific design. 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

Cyclodextrin-based nanosponges (CDNSs) are novel polymers composed of cross-linked cyclodextrin (CD) macrocyclic units, whose characteristics make them great candidates for drug delivery systems with adjustable properties for the drug release process. Examination of the molecular structure and dynamics of CDNSs is a necessary starting point in the first step toward their broad application. Spectroscopic methods are effective analytical tools for probing the structure–property relationships of polymer structures. Infrared (IR) and Raman spectroscopies provide insight into the behavior of hydrogen bond (H-bond) networks influencing the properties of CDNS polymeric networks. Scattering techniques such as inelastic neutron scattering (INS) and Brillouin light scattering (BLS) probe elastic properties, while small-angle neutron scattering (SANS) examines the structural inhomogeneities and water sorption abilities of CDNS materials. Complete evaluation is possible using nuclear magnetic resonance (NMR), which can provide data on CDNS network dynamics. This article summarizes the results of a wide examination of CDNSs with the use of spectroscopic methods and reveals the links between the microscopic behavior and macroscopic properties of CDNSs, enabling the customization of their properties for various biomedical purposes. Full article

Levoglucosenone (LGO) smoothly undergoes microwave-assisted hetero-Diels–Alder reactions with thiochalcones in THF solution at 60 °C. The studied reactions are completed after 10 min, and the expected tricyclic 2,3-dihydro-4H-thiopyran derivatives are formed in a highly regio- and moderately stereoselective manner via competitive exo- and endo-attacks of the 1-thiadiene moiety onto the activated C=C bond of dienophile LGO. Although eight isomers are possible, only the formation of exo,exo- (major) and exo,endo- (minor) cycloadducts was observed. In most cases, isomeric products were separated by preparative layer chromatography and identified by means of spectroscopic methods. Some of the cycloadducts were obtained as single crystalline solids, and X-ray analyses enabled unambiguous confirmation of their structures. In order to explain the observed selectivity of the studied hetero-Diels–Alder reactions, DFT studies were carried out to determine the thermodynamic and kinetic properties of all regio- and stereoisomers. The results of these calculations predict the preferred formation of the two experimentally observed isomers. In addition, remarkable details on the electronic structure of E-1,3-diphenylprop-2-en-1-thione and on involved and hypothetical transition states could be elucidated. Full article

This work describes the synthesis and characterization of novel organometallic polymeric frameworks derived from lactone-based poly(benzofuran-co-arylacetic acid) (PBAAA) ligands complexed with 3d transition metal salts (Co²⁺, Cu²⁺, Zn²⁺). Two distinct synthetic approaches were investigated: conventional solution-based methods and mechanochemical ball milling. A comprehensive spectroscopic evaluation was performed utilizing FTIR, XRD, UV-Vis, and XPS techniques to detail the structural characteristics of the synthesized materials. The thermal assessments were conducted using TGA and thermal conductivity, demonstrating that the chosen synthesis method has a significant impact on the crystallinity, coordination environment, and thermal transport characteristics of the resultant complexes. Remarkably, using the mechanosynthesis, the resulting organometallic polymer materials exhibited enhanced chain ordering and improved thermal conductivity, with a value of 0.32 W/mK, almost double that of the starting polymer. A correlation was identified among thermal conductivity, metal ionic radius, coordination number, and the synthesis method utilized. XPS analysis revealed the presence of multiple oxidation states and varied electronic environments, particularly in copper complexes. These had a direct effect on how they behaved when heated. These results show that mechanochemical synthesis is a useful and long-lasting method to make complex organometallic polymers with thermal properties that can be changed. Full article

The rehabilitation of underground infrastructure requires cement grouts that combine high injectability into micro-cracks with superior mechanical strength and durability. Conventional grouts, however, are limited by excessive yield stress and the formation of weak crystalline phases. This study investigated sodium polyacrylate (PAAS) as a multi-functional modifier to address these limitations. Through a multi-scale approach combining rheological measurements, spectroscopic analysis (FTIR, LF-NMR), diffraction (XRD), and electron microscopy (SEM), we elucidated the synergistic modification mechanisms of PAAS. The results demonstrated that PAAS operated via two pathways: (i) chemically, its carboxyl groups chelated Ca²⁺ ions, suppressing Ca(OH)₂ crystallization and refining C-S-H gel; (ii) physically, it provided electrostatic and steric dispersion, dismantling flocculated networks to reduce yield stress by 80.3% and enhance fluidity by 30.7%. This drastically improved injectability was complemented by micro-structural optimization, where PAAS eliminated percolation pores (>1 μm) and promoted a homogeneous, dense matrix. Consequently, the mechanical properties were significantly enhanced, with a 0.04% PAAS dosage maximizing compressive strength (15.56 MPa, +26.2%) and a 0.06% dosage elevating flexural strength (5.74 MPa, +29.3%). This work establishes that low-dosage PAAS modification enables a unique combination of high fluidity, strength, and durability by leveraging synergistic chemical and physical mechanisms, providing a tailored, cost-effective solution for advanced grouting applications. Full article