Search Results (322)

In response to growing interest in green additives derived from natural raw materials or post-production waste of natural origin, epoxy compositions containing the additive in the form of waste wood flour and microcellulose were prepared. The research involved the chemical modification of the additive through a two-stage silanization process using 3-aminopropyltriethoxysilane. Followed by filler’s characterization using Fourier Transformed Infrared Spectroscopy (FT-IR) to analyze the modification in chemical structure, Wide Angle X-Ray Diffraction (WAXD) to detect differences in crystal structure, and Scanning Electron Microscopy (SEM) to observe morphological changes. Next, waste oak flour (WF) and microcrystalline cellulose (MCC) were used in unmodified and silanized form (sil-WF and sil-MCC, respectively) to prepare epoxy composites, followed by testing their influence on the mechanical (hardness, tensile strength, flexural strength, compressive strength, and impact strength), thermal, and morphological characteristics of epoxy composites based on Epidian 6. Comparing the effect of modification on the properties of the analyzed additives, it was found that silanization had a larger impact on increasing the interaction of the waste wood flour with the epoxy matrix than silanization of MCC due to a lesser tendency of the sil-WF than the sil-MCC to agglomerate. An enhanced interaction of sil-WF with the polymer resulted in improved mechanical properties. Composite EP/sil-WF (cured epoxy composite based on low-molecular-weight epoxy resin Epidian 6 filled with 5 wt.% of silanized wood flour) was characterized by improved flexural (61.97 MPa) and compressive properties (69.1 MPa) compared to both EP/WF (cured epoxy composite based on low-molecular-weight epoxy resin Epidian 6 filled with 5 wt.% of unmodified wood flour) (42.39 MPa and 61.0 MPa) and the unfilled reference composition (54.55 MPa and 67.4 MPa, respectively). Moreover, compositions containing a cellulosic additive were characterized by better impact properties than the reference composition. Full article

La-doped ZnO nanoclusters confined within mesoporous SBA-15 were synthesized using an impregnation–calcination method and evaluated for their visible-light-driven photocatalytic degradation of Rhodamine B (RhB). Small-angle X-ray diffraction (XRD) and transmission electron microscopy (TEM) confirmed the preservation of the 2D hexagonal mesostructure of SBA-15 post-loading. In contrast, wide-angle XRD and Fourier-transform infrared spectroscopy (FT-IR) analyses revealed that the incorporated ZnO existed predominantly as highly dispersed amorphous or ultrafine clusters within the mesopores. N₂ adsorption–desorption measurements exhibited Type IV isotherms with H1 hysteresis loops. Compared to pristine SBA-15, the specific surface area and pore volume of the composites decreased from 729.35 m² g⁻¹ to 521.32 m² g⁻¹ and from 1.09 cm³ g⁻¹ to 0.85 cm³ g⁻¹, respectively, accompanied by an apparent increase in the average pore diameter from 5.99 nm to 6.55 nm, attributed to non-uniform pore occupation. Under visible-light irradiation, the photocatalytic performance was highly dependent on the La doping level. Notably, the 5% La-ZnO/SBA-15 sample exhibited superior activity, achieving over 99% RhB removal within 40 min and demonstrating the highest apparent rate constant (k = 0.1152 min⁻¹), surpassing both undoped ZnO/SBA-15 (k = 0.0467 min⁻¹) and other doping levels. Reusability tests over four consecutive cycles showed a consistent degradation efficiency exceeding 93%, with only a ~7 percentage-point decline, indicating excellent structural stability and recyclability. Radical scavenging experiments identified h⁺, ·OH, and ·O₂⁻ as the primary reactive species. Furthermore, photoluminescence (PL) quenching observed at the optimal 5% La doping level suggested suppressed radiative recombination and enhanced charge carrier separation. Collectively, these results underscore the synergistic effect of La doping and mesoporous confinement in achieving fast, efficient, and recyclable photocatalytic degradation of organic pollutants. Full article

This paper presents a study of the thermal and rheological properties of isosorbide, showing that its degradation temperature (around 100 °C) is much lower than values previously proposed in the literature. Furthermore, remarkable calorimetric and viscoelastic behaviors, with features usually observed in semi-crystalline systems are presented. The onset of the melting is measured at 45 °C, while a glass transition occurs at −45 °C, followed by cold crystallization. Wide-angle X-ray diffraction confirmed the coexistence of crystalline domains and an amorphous fraction, which behaves as a molecular glass, with an estimated crystallinity of approximately 70%. Thermogravimetric analyses conducted under both air and nitrogen and at multiple heating rates, in line with ICTAC recommendations, established the robustness of the 100 °C degradation onset. These findings provide new structure–property relationships for isosorbide and open up new avenues for further research and development in this area. Full article

Two heteroaromatic hybrid compounds were synthesized and characterized using various analytical techniques. The results indicate that the benzimidazole/oxadiazole (BZ/OZ) metal derivative exhibits a tridentate coordination mode, where the carbonyl, imidazole and oxadiazole groups participate in coordination with the metal, in a ratio of 2:1 of the ligand to the metal. The antibacterial activities of the organic ligand and its metal complex were determined by in vitro tests against both Gram-positive bacterial strains and Gram-negative bacterial strains using the broth microdilution method. The metal complex showed greater antibacterial activities compared to the precursor ligand against all evaluated microorganisms. The results obtained through in silico predictions revealed significant toxicological differences among the analyzed molecules, suggesting special attention in the use of the ligand due to its possible carcinogenicity in mice and a need for structural modifications in the complex to reduce its carcinogenicity and toxicity. Furthermore, a biophysical study of the interaction of the BZ/OZ derivatives with different model membranes was explored through differential scanning calorimetry (DSC), simultaneous small- and wide-angle X-ray diffraction (SAXD and WAXD) and infrared spectroscopy (FT-IR). The results indicate that the compounds influenced membrane properties without significantly altering the lamellar organization. The findings suggest potential applications in understanding lipid interactions, elucidating toxicology and developing antibacterial agents. Full article

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

In this work, bare copper oxide-based catalysts were synthesized and evaluated for their dual (photo)catalytic activity in two model reactions: hydrogen generation via formic acid decomposition (FAD) and the photocatalytic hydroxylation of benzene to phenol. Catalysts were prepared from copper nitrate and copper acetate precursors and calcined for either 10 min or 2 h. Their structural and surface properties were characterized by wide-angle X-ray diffraction (WAXD), Raman spectroscopy, and BET surface area analysis. FAD was conducted under mild thermal conditions and monitored via ¹H NMR spectroscopy. At the same time, benzene hydroxylation was performed under UV irradiation and analyzed by gas chromatography (GC) and high-performance liquid chromatography (HPLC). All synthesized catalysts outperformed commercial CuO in the selective oxidation of benzene. The nitrate-derived sample calcined for 10 min (NCuO 10 min) achieved the best performance, with a phenol yield of ~10% and a selectivity of up to 19%, attributed to improved surface properties and the presence of Cu(I) domains, as indicated by Raman spectroscopy. For FAD, complete conversion of formic acid was achieved at low temperatures, with selective H₂ and CO₂ evolution and complete suppression of CO, even under short reaction times and low catalyst loadings. These results demonstrate the potential of nitrate-derived CuO catalysts as versatile, dual-function materials for sustainable applications in selective aromatic oxidation and low-temperature hydrogen generation, without the need for noble metals or harsh conditions. Full article

Geopolymers represent an innovative and environmentally sustainable alternative to traditional construction materials, offering significant potential for reducing anthropogenic CO₂ emissions. Among these, phosphoric acid-activated metakaolin-based systems have attracted increasing attention for their chemical and thermal resilience. In this study, we present a comprehensive structural and mechanical evaluation of metakaolin-based geopolymers synthesized across a wide range of Al/P molar ratios (0.8–4.0). Six formulations were systematically prepared and analyzed using X-ray powder diffraction (XRPD), small-angle X-ray scattering (SAXS), Fourier-transform infrared spectroscopy (FTIR), solid-state nuclear magnetic resonance (ssNMR), and complementary mechanical testing. The novelty of this work lies in the integrated mapping of composition–structure–property relationships across the broad Al/P spectrum under controlled synthesis, combined with the rare application of SAXS to reveal composition-dependent nanoscale domains (~18–50 nm). We identify a stoichiometric window at Al/P ≈ 1.5, where complete acid consumption leads to a structurally homogeneous AlVI–O–P network, yielding the highest compressive strength. In contrast, acid-rich systems exhibit divergent flexural and compressive behaviors, with enhanced flexural strength linked to hydrated silica domains arising from metakaolin dealumination, quantitatively tracked by ²⁹Si MAS NMR. XRPD further reveals the formation of uncommon Si–P crystalline phases (SiP₂O₇, Si₅P₆O₂₅) under low-temperature curing in acid-rich compositions. Together, these findings provide new insights into the nanoscale structuring, phase evolution, and stoichiometric control of silica–alumino–phosphate geopolymers, highlighting strategies for optimizing their performance in demanding thermal and chemical environments. Full article

Cobalt-based alloys such as Stellite 6 are widely applied in demanding conditions because of their good resistance to wear, erosion, and corrosion, but further improvements in erosion resistance are still required. This work analyzes the effect of adding titanium and tungsten on the structure and properties of Stellite 6 coatings produced by laser cladding, aiming to enhance their erosion resistance. Penetrant tests confirmed that the additions did not reduce coating quality, and macroscopic observations showed that appropriate process parameters allowed for defect-free coatings with strong bonding to the substrate. Microstructural studies carried out by SEM/EDS (Scanning Electron Microscopy/ Energy Dispersive Spectroscopy) and XRD (X-ray Diffraction) revealed that the reference Stellite 6 coating consisted of a cobalt-based austenitic matrix with interdendritic chromium carbides, while Ti and W additions led to the in situ formation of primary and eutectic (Ti,W)C carbides. Transmission electron microscopy showed a gradient in tungsten concentration inside the primary carbides, with progressive tungsten dissolution into the TiC lattice. Although different powder compositions had only a moderate effect on hardness, erosion tests demonstrated that the coatings with Ti and W exhibited clearly improved resistance. In particular, the in situ carbides enhanced erosion resistance at 30° impingement angles, while also maintaining high resistance under 90° impact. These findings confirm that modifying Stellite 6 with Ti and W during laser cladding is an effective way to improve its durability in erosive conditions. Full article

The results of strain-induced crystallization (SIC) studies on natural rubber compounds containing different amounts of carbon black and silica are reported. Two-dimensional wide-angle X-ray diffraction (2D WAXD) experiments were performed to quantify the degree of SIC at ambient and enlarged temperatures. The influence of temperature and filler system on the degree of crystallinity of natural rubber was investigated, since the estimated temperatures in truck tire treads are in the range 60–80 °C. Interestingly, the degree of crystallinity for silica-filled natural rubber compounds was commonly at least similar or higher compared to carbon black-filled compounds with identical filler mass fraction. In addition, it was demonstrated that the temperature dependence of natural rubber compounds containing silica and carbon black is also similar. In both cases the SIC disappeared slightly above 100 °C. Hence, it was concluded that the SIC behavior is most likely not the decisive factor for the different abrasion resistance of silica- and carbon black-reinforced natural rubber compounds for truck tire treads. This is an important insight considering the rising demand for sustainable rubber compounds for truck tire treads with low CO₂ emissions as well as reduced abrasion. 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

Background/Objectives: Hot-melt extrusion (HME) has become a key technology in pharmaceutical formulation, particularly for enhancing the solubility of poorly soluble Active Pharmaceutical Ingredients (APIs). While horizontal HME is widely adopted, vertical HME remains underexplored despite its potential benefits in footprint reduction, feeding efficiency, temperature control, and integration into continuous manufacturing. This study investigates vertical HME as an innovative approach in order to optimize drug polymer interactions and generate stable amorphous dispersions with controlled release behavior. Methods: Extrusion trials were conducted using a vertical hot-melt extruder developed by Rondol Industrie (Nancy, France). Acetylsalicylic acid (ASA) supplied by Seqens (Écully, France) was used as a model API and processed with Soluplus^® and Kollidon^® 12 PF (BASF, Ludwigshafen, Germany). Various process parameters (temperature, screw speed, screw profile) were explored. The extrudates were characterized by powder X-ray diffraction (PXRD) and small-angle X-ray scattering (SAXS) to evaluate crystallinity and microstructure. In vitro dissolution tests were performed under sink conditions using USP Apparatus II to assess drug release profiles. Results: Vertical HME enabled the formation of homogeneous amorphous solid dispersions. PXRD confirmed the absence of residual crystallinity, and SAXS revealed nanostructural changes in the polymer matrix influenced by drug loading and thermal input. In vitro dissolution demonstrated enhanced drug release rates compared to crystalline ASA, with good reproducibility. Conclusions: Vertical HME provides a compact, cleanable, and modular platform that supports the development of stable amorphous dispersions with controlled release. It represents a robust and versatile solution for pharmaceutical innovation, with strong potential for cost-efficient continuous manufacturing and industrial-scale adoption. Full article

This study investigates the hydrogen permeability of injection-molded polyamide 6 (PA6) nanocomposites reinforced with organo-modified montmorillonite (OMMT) at varying concentrations (1, 2.5, 5, and 10 wt. %) for potential use as Type IV composite-overwrapped pressure vessel (COPV) liners. While previous work examined their mechanical properties, this study focuses on their crystallinity, morphology, and gas barrier performance. The precise inorganic content was determined using thermal gravimetry analysis (TGA), while differential scanning calorimetry (DSC), wide-angle X-ray diffraction (WAXD), and scanning electron microscopy (SEM) were used to characterize the structural and morphological changes induced by varying filler content. The results showed that generally higher OMMT concentrations promoted γ-phase formation but also led to increased agglomeration and reduced crystallinity. The PA6/OMMT-1 wt. % sample stood out with higher crystallinity, well-dispersed clay, and low hydrogen permeability. In contrast, the PA6/OMMT-2.5 and -5 wt. % samples showed increased permeability, which corresponded to WAXD and SEM evidence of agglomeration and DSC results indicating a lower degree of crystallinity. PA6/OMMT-10 wt. % showed the most-reduced hydrogen permeability compared to all other samples. This improvement, however, is attributed to a tortuous path effect created by the high filler loading rather than optimal crystallinity or dispersion. SEM images revealed significant OMMT agglomeration, and DSC analysis confirmed reduced crystallinity, indicating that despite the excellent barrier performance, the compromised microstructure may negatively impact mechanical reliability, showing PA6/OMMT-1 wt. % to be the most balanced candidate combining both mechanical integrity and hydrogen impermeability for Type IV COPV liners. Full article

This study systematically investigates the impact of hydrolytic degradation on the crystallization kinetics and morphology of poly(butylene succinate-co-adipate) (PBSA). Gel Permeation Chromatography (GPC) confirmed extensive chain scission, significantly reducing the polymer’s weight-average molecular weight (M_w from ~103,000 to ~16,000 g/mol) and broadening its polydispersity index (PDI from ~2 to 7 after 64 days). Differential scanning calorimetry (DSC) analysis revealed that hydrolytic degradation dramatically accelerated crystallization rates, reducing crystallization time roughly 10-fold (e.g., from ~3000 s to ~300 s), and crystallinity increased from 34% to 63%. Multiple melting peaks suggested the presence of lamellae with varying thicknesses, consistent with the Gibbs–Thomson equation. Isothermal crystallization kinetics were evaluated using the Avrami equation (with n ≈ 3), reciprocal half-time of crystallization, and a novel inflection point slope method, all confirming accelerated crystallization; for instance, the slope increased from 0.00517 to 0.05203. Polarized optical microscopy (POM) revealed evolving spherulite morphologies, including hexagonal and flower-like dendritic spherulites with diamond-shape ends, while wide-angle X-ray diffraction (WAXD) showed a crystallization range shift to higher temperatures (e.g., from 72–61 °C to 82–71 °C) and a 14% increase in crystallite diameter, aligning with increased melting point and lamellar thickness and overall increased crystallinity. Full article

Polypropylene (PP), with its good physical, thermal, and mechanical properties and excellent processing capabilities, has become one of the most used synthetic polymers. It is known that the overall properties of semicrystalline polymers, including PP, are governed by morphology, which is influenced by the crystallization behavior of the polymer under specific conditions. The most important industrial PP remains the isotactic one, and it has been studied extensively for its polymorphic characteristics and crystallization behavior for over half a century. Due to its regular chain structure, isotactic polypropylene (iPP) belongs to the group of polymers with a high tendency for crystallization. The rapid quenching of molten iPP fails to produce a completely amorphous polymer but leads to an intermediate crystalline order. On the other hand, slow cooling yields a material with high crystalline content. The processing conditions that occur in practice and industry are between these two extremes and, in some cases, are even very close. Therefore, the study of limits in processability and the impact of extreme preparation conditions on morphology, structure, thermal, and mechanical properties fills a gap in the current understanding of how the processing conditions of iPP can be used to design the desired properties for specific applications and is in the focus of this research. The first set of samples (Q samples) was obtained by rapid quenching, while the second was prepared by very slow cooling from the melt to room temperature (SC samples). Testing of samples was performed by optical microscopy (OM), scanning electron microscopy (SEM), wide-angle X-ray diffraction (WAXD), Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), dynamic dielectric spectroscopy (DDS), and mechanical measurements. Characterization revealed that slowly cooled samples exhibited a significantly higher degree of crystallinity and larger crystallites (χ ≥ 55% and L₍₁₁₀₎ ≈ 20 nm), compared to quenched samples (χ < 30%, L₍₁₁₀₎ ≤ 3 nm). Mechanical testing showed a drastic contrast: quenched samples exhibited elongation at break > 500%, while slowly cooled samples broke below 15%, reflecting their brittle behavior. For the first time, DDS is applied to investigate molecular mobility differences between processing-dependent structural forms, specifically the mesomorphic (smectic) and α-monoclinic forms. In slowly cooled samples, α relaxation exhibited both enhanced intensity and an upward temperature shift, indicating stronger structural constraints due to a much higher crystalline phase content and significantly larger crystallite size, respectively. These findings provide novel insights into the structure–property–processing relationship, which is crucial for industrial applications. Full article

This study investigated the effects of electron beam radiation on the room-temperature and high-temperature mechanical properties of two ethylene-vinyl acetate (EVA) copolymers, designated EVA 206 and EVA 212. These copolymers had varying vinyl acetate (VA) contents (6 wt.% and 12 wt.%), with the same melt flow index of 2.0 g/10 min. Samples were irradiated at doses ranging from 60 to 180 kGy. The impact of electron beam irradiation on the creep, frequency sweep, and stress–strain behaviors of the ethylene-vinyl acetate copolymers was evaluated using a dynamical mechanical analyzer (DMA). Crystallinity was measured using differential scanning calorimetry (DSC) and wide-angle X-ray diffraction (WAXD). Creep compliance was quantitatively analyzed using four-parameter and six-parameter models. While crosslinking had minimal influence on the room-temperature properties, it significantly affected the behavior at 150 °C. With increasing irradiation dose, creep compliance decreased, while the shear modulus, viscosity, and shear stress at a strain of 0.03 increased, indicating enhanced resistance to deformation. Crosslink density also increased with irradiation dose. EVA 212 with a higher vinyl acetate content exhibited a higher resistance to creep and better high-temperature mechanical properties across all measurements. Full article