Search Results (138)

In this work, we report a novel mechanochemical synthesis method for the synthesis of quinoxaline derivatives—a spiral gas–solid two-phase flow approach, which enables the efficient preparation of quinoxaline compounds. Compared to conventional synthetic methods, this approach eliminates the need for heating or solvents while significantly reducing reaction time. The structures of the synthesized compounds were characterized using nuclear magnetic resonance (NMR), Fourier-transform infrared spectroscopy (FT-IR), ultraviolet-visible (UV–Vis) absorption spectroscopy, powder X-ray diffraction (XRD), differential scanning calorimetry (DSC), and high-performance liquid chromatography (HPLC). Using the synthesis of 2,3-diphenylquinoxaline (1) as a model reaction, the synthetic process was investigated with UV–Vis spectroscopy. The results demonstrate that when the total feed amount was 2 g with a carrier gas pressure of 0.8 MPa, the reaction completed within 2 min, achieving a yield of 93%. Furthermore, kinetic analysis of the reaction mechanism was performed by monitoring the UV–Vis spectra of the products at different time intervals. The results indicate that the synthesis of 1 follows the A4 kinetic model, which describes a two-dimensional diffusion-controlled product growth process following decelerated nucleation. 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

The recycling of plastics collected from household waste to produce post-consumer recycled (PCR) materials is a critical step of sustainable waste management. However, the processing of PCR materials presents unique challenges, particularly in the context of seasonal input stream fluctuations and resulting PCR material composition variations. Within this paper, the influence of batch-to-batch fluctuations on the processing stability and product properties of high-density polyethylene (HDPE) PCR from the German municipal waste system is analysed. It examines how variations in batch composition affect key parameters such as processing data (injection pressure, torque), mechanical properties (tensile strength, E-modulus, impact strength), and product quality (gel formation, part dimensions, part weight). Therefore, six consecutive household HDPE PCR material batches are analysed regarding their composition, contaminations, and rheological characteristics through ashing, differential scanning calorimetry, high-temperature gel permeation chromatography, and high-pressure capillary rheometry. The batches are then processed using blown- and cast-film extrusion as well as injection moulding, and the resulting process stability and product quality are analysed. The results show a strong correlation between thermal properties, such as crystallisation enthalpy, molecular weight, polypropylene (PP) content, varying batch viscosities, and changes in processing data as well as the resulting product properties. Full article

Carbon dioxide (CO₂) clathrate hydrate is gaining attention as a promising material for cold thermal energy storage (CTES) due to its high energy storage capacity and low environmental footprint. It shows strong potential in building applications, where space cooling accounts for nearly 40% of total energy use and over 85% of electricity demand in developed countries. CO₂ hydrates are also being explored for use in refrigeration, cold chain logistics, supercomputing, biomedical cooling, and defense systems. With the growing number of applications in mind, this review focuses on the thermal behavior of CO₂ hydrates and their environmental impact. It highlights recent efforts to reduce formation pressure and temperature using chemical promoters and surfactants. This paper also reviews key experimental techniques used to study hydrate properties, including Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), high-pressure differential scanning calorimetry (HP-DSC), and the T-history method. In lifecycle comparisons, CO₂ hydrate systems show better energy efficiency and lower carbon emissions than traditional ice or other phase-change materials (PCMs). This review also discusses current commercialization challenges such as high energy input during formation and promoter toxicity. Finally, practical strategies to move CO₂ hydrate-based CTES from lab-scale studies to real-world cooling and temperature control applications are discussed. Full article

The porosity of hair fibers can be modified by chemical and physical damage, influencing their response to cosmetic treatments. To investigate the effect of commonly applied hair care protocols on textured hair, virgin and once-bleached tresses were subjected to multiple cycles of washing, blow-drying while combing, and styling with a hot flat iron, simulating a consumer routine spanning one to six months. Porosity-related properties were evaluated using swelling test, fluorescence, atomic force, and scanning electron microscopies, high-pressure differential scanning calorimetry, and tensile testing. Both chemical and physical processes induced significant changes in the hair’s water permeability, surface topography, and appearance, alongside a reduction in mechanical and thermal properties, indicating substantial structural alterations compared to virgin hair. Increased porosity compared to virgin hair possibly reduced the heat conductivity of bleached hair, leading to less pronounced effects of heat exposure. These findings underscore the damaging potential of routine practices for textured hair and emphasize the need for targeted cosmetic solutions to protect and repair these fibers as part of consumers’ hair care regimens. Full article

3,4-Dinitrofurazanfuroxan (DNTF) is characterized by its high energy, high detonation velocity, strong explosive power, and small critical diameter for detonation. However, its practical application is limited by poor thermal stability and mechanical properties. In this study, the polymeric desensitizer fluororubber (F2603) was introduced as a binder to enhance the overall performance of DNTF. Molecular dynamics (MD) simulations were used to investigate the thermal stability (trigger bond length and cohesive energy density (CED)) and mechanical properties, including elastic coefficient (C_ij), tensile modulus (E), bulk modulus (K), shear modulus (G), Cauchy pressure (C₁₂–C₄₄), and Poisson’s ratio, for both pure DNTF (1 1 1) and DNTF (1 1 1)/F2603 composite systems at varying temperatures. The thermal stability was further experimentally investigated using differential scanning calorimetry (DSC) technique. The results demonstrated that the addition of F2603 leads to a shorter trigger bond length, higher CED, and a 7.2 kJ·mol⁻¹ increase in activation energy (Ea), indicating improved thermal stability. Additionally, mechanical property simulations indicated that F2603 decreased the E, K, and G of DNTF while increasing the K/G ratio, suggesting enhanced mechanical toughness. These studies have important implications for the formulation design and practical application of DNTF and its composites. Full article

The aim of this work is to study the effect of high-temperature compaction (HTC) upon the polymorphism and the mechanical behavior of an additively manufactured (AM) carbon fiber-reinforced polyamide (PA6). Different pressure and temperature levels during HTC were tested to determine the overall effect on the mechanical behavior and material crystalline composition. Treated, carbon fiber-reinforced PA6 samples were analyzed using differential scanning calorimetry, X-ray diffraction, thermogravimetric analysis, scanning electron microscopy, and three-point bending testing. When considered with respect to as-printed samples, an HTC temperature of 190 °C combined with 80 psi pressure resulted in an increased flexural modulus and strength of 47% and 58%, respectively. This increase was attributed to the decrease in AM-induced cracking, voids (both inside and between the beads), and crystalline solid-state transition in the PA6. The effect of pressure and temperature on the crystalline structure was discussed in terms of an increased degree of crystallinity and the amount of α-phase. Therefore, HTC can help overcome some limitations of traditional annealing, which can result in recrystallization-induced cracking which can lead to material embrittlement. The proposed HTC method demonstrates the potential in improving the mechanical behavior of AM thermoplastic composites. Full article

In the present investigation, high stability Vitreloy Zr₄₄Ti₁₁Cu₁₀Ni₁₀Be₂₅ bulk metallic glass has been subjected to severe shear deformation by high-pressure torsion for 0.1 revolutions under an applied pressure of 4 and 8 GPa. The fully glassy nature of the as-cast glass has been confirmed by X-ray powder diffraction and differential scanning calorimetry. Deformation-induced surface features on an internal plane of the deformed disk-shaped specimens were studied in detail at the macroscopic level by optical reconstruction method and at microscopic scales by white-light optical profilometry. Shear and compressive strain components were measured based on surface changes and it was determined that compressive strain gradient with 0.2–0.4 strain change builds up toward the disk edge, while only part of the nominal shear deformation occurs in the disk interior. The effect of strain localization in the Vitreloy bulk metallic glasses has been quantified by a surface distortion model based on simple shear. The model was then validated experimentally by the reconstructed z-profiles. Full article

High-pressure treatment was utilized in this study to produce high-quality, reduced-sodium pork gels with desirable texture and sensory properties, addressing the challenge of maintaining quality in low-sodium meat products to meet health-conscious consumer demands. High-pressure treatment applied within the range of 150–200 MPa significantly reduced cooking loss while maintaining moisture content and provided an ideal network structure for reduced-sodium pork gels. High-pressure treatment at up to 100–200 MPa, in combination with added sodium chloride and sodium polyphosphate, was evaluated for its effects on gel texture, with results indicating that high-pressure treatment significantly improved breaking stress (increased by 10.01% under 150 MPa and 14.66% under 200 MPa), modulus of elasticity (increased by 14.77% under 150 MPa and 24.17% under 200 MPa), and hardness (increased by 11.12% under 150 MPa and 11.45% under 200 MPa). Rheological characteristic measurements revealed that gel strength was highest at 150 MPa (G′ = 443,000 Pa; G″ = 66,300 Pa and $tan\delta$ = 0.15), which showed higher G′ and G″ values and similar $tan\delta$ compared to the 0.1 MPa, 2% NaCl + 0.5% SPP condition (G′ = 334,000 Pa; G″ = 49,200 Pa; $tan\delta$ = 0.148). Protein analysis by sodium dodecyl sulfate–polyacrylamide gel electrophoresis showed a reduction in the $\alpha$-actinin band with increased pressure, which suggested protein interactions were enhanced. Differential scanning calorimetry analysis indicated that protein denaturation occurred more readily at higher pressures (0.071 J/g at 0.1 MPa, 0.057 J/g at 150 MPa, and 0.039 J/g at 200 MPa). These findings underscore the value of treatment under high pressure at 150 MPa developing reduced-sodium meat products with desirable texture and flavor characteristics. Full article

Celecoxib (CEL), a nonsteroidal anti-inflammation drug (NSAID), is categorized as a Class II drug (low solubility, high permeability) in the Biopharmaceutics Classification System (BCS). The aim of this study is to develop a novel formulation of CEL nanosuspensions in the form of dried powder for tableting or capsuling. In this study, CEL was formulated into nanosuspensions to improve its solubility. CEL nanosuspensions were prepared using the precipitation method followed by high-pressure homogenization. Drying of the nanosuspensions was performed by spray drying and freeze drying. We examined the impact of various formulation and processing parameters on the nanoparticles. The CEL nanoparticles were characterized by particle size analysis, differential scanning calorimetry (DSC), powder X-Ray diffraction (PXRD), attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), and dissolution tests. The choice of solvent, stabilizer, and surfactant appeared to have significant impacts on the crystallization and particle size and, consequently, the solubility of the CEL nanoparticles. CEL chemical stability was maintained throughout both drying processes. Both spray-dried and freeze-dried CEL nanosuspensions showed rapid dissolution profiles compared to raw CEL due to the nanosized particle dispersion with the presence of a lag phase. The freeze-dried nanosuspension showed a slight delay in the first 20 min compared to the spray-dried nanosuspension, after which dissolution progressed with a lag phase that represents aggregation. Full article

This technical paper delves into the creation and application of an enhanced mathematical model for semi crystalline thermoplastics based on the Pressure-Volume-Temperature (PVT) Two Domain Tait Equation. The model is designed to incorporate the impact of the cooling rate on the specific volume of the material. This is achieved by utilizing Flash differential scanning calorimetry (fDSC) measurements, thereby ensuring a direct correlation to the actual behavior of the material in reality. The practical application of the model in the context of injection molding simulation was also considered. This was done by integrating the mathematical model into the Moldflow software via the Solver API. The paper underscores the discontinuity issue inherent in the traditional Tait equation with cooling rates and proposes a solution that guarantees a correct transition from the liquid to the solid phase, even at high cooling rates and pressures. The results demonstrated a realistic PVT curve across a wide range of cooling rates and high pressures. The model was put to the test using a 3D tetrahedron meshed calculation model in the injection molding simulation. This study marks a significant step forward in the simulation of injection molding processes, as it successfully bridges the gap between real material properties and simplified simulation, paving the way for more accurate and efficient simulations in the future. Full article

With the continuous advancement of industrial technology, higher demands have been placed on the properties of gear oils, such as oxidation stability and shear resistance. Herein, the oxidation stability of high-viscosity metallocene poly-$\alpha$-olefins (mPAOs) was improved by chemical modification via aromatic amine alkylation. The modified mPAO base oils were synthesized separately with diphenylamine (mPAO-DPA) and N-phenyl-$\alpha$-naphthylamine (mPAO-NPA), and their applicability in industrial gear oil formulations was evaluated. The composition and physicochemical properties of the obtained samples were assessed using ¹H NMR spectroscopy, Fourier transform infrared spectroscopy, gel permeation chromatography, and the American Society for Testing and Materials standards (ASTM D445, ASTM D2270, ASTM D92, etc.) confirming the successful completion of the alkylation reaction. The oxidation stability of the samples was also evaluated using pressurized differential scanning calorimetry. The initial oxidation temperature of mPAO-NPA (230 °C) was 53 °C higher than that of mPAO, and the oxidation induction period of mPAO-DPA was nearly twice that of mPAO-NPA. Thermogravimetric analysis in air revealed the increased thermal decomposition temperature and improved thermal stability of modified mPAO. ISO VG 320 industrial gear oils were formulated using mPAO alkylated with N-phenyl-$\alpha$-naphthylamine(Lub-2) and commercially purchased PAO100 (Lub-1) as base oil components. The antioxidant performance of two industrial gear oils was evaluated through oven oxidation and rotating oxygen bomb tests. The oxidation induction period of Lub-2 was 30% higher than that of Lub-1, with the latter having a lower acid number and a smaller increase in viscosity at 40 °C. Finally, the friction performance of the samples was assessed on a four-ball friction tester, revealing the synergistic effect of the mPAO-NPA base oil with the HiTEC 3339 additive, forming a more stable oil film with a smaller wear scar diameter. Full article

This paper reports the vapor pressure and enthalpy of vaporization for a promising phase change material (PCM) guanidinium methanesulfonate ([Gdm][OMs]), which is a typical guanidinium organomonosulfonate that displays a lamellar crystalline architecture. [Gdm][OMs] was purified by recrystallization. The elemental analysis and infrared spectrum of [Gdm][OMs] confirmed the purity and composition. Differential scanning calorimetry (DSC) also confirmed its high purity and showed a sharp and symmetrical endothermic melting peak with a melting point (T_m) of 207.6 °C and a specific latent heat of fusion of 183.0 J g⁻¹. Thermogravimetric analysis (TGA) reveals its thermal stability over a wide temperature range, and yet three thermal events at higher temperatures of 351 °C, 447 °C, and 649 °C were associated with vaporization or decomposition. The vapor pressure was measured using the isothermogravimetric method from 220 °C to 300 °C. The Antoine equation was used to describe the temperature dependence of its vapor pressure, and the substance-dependent Antoine constants were obtained by non-linear regression. The enthalpy of vaporization (Δ_vapH) was derived from the linear regression of the slopes associated with the linear temperature dependence of the rate of weight loss per unit area of vaporization. Hence, the temperature dependence of vapor pressures ln P_vap (Pa) = 10.99 − 344.58/(T (K) − 493.64) over the temperature range from 493.15 K to 573.15 K and the enthalpy of vaporization Δ_vapH = 157.10 ± 20.10 kJ mol⁻¹ at the arithmetic mean temperature of 240 °C were obtained from isothermogravimetric measurements using the Antoine equation and the Clausius–Clapeyron equation, respectively. The flammability test indicates that [Gdm][OMs] is non-flammable. Hence, [Gdm][OMs] enjoys very low volatility, high enthalpy of vaporization, and non-flammability in addition to its known advantages. This work thus offers data support, methodologies, and insights for the application of [Gdm][OMs] and other organic salts as PCMs in thermal energy storage and beyond. Full article

In order to gain insight into the influence of grain size on precipitation thermodynamics, bulk materials of coarse-grained (CG), ultrafine-grained (UFG) (with or without dislocations), and nanocrystalline (NC) 7075 Al alloy have been fabricated by solid solution treatment, equal-channel angular pressing (ECAP), or high-pressure torsion (HPT) processes. The precipitation behavior and the corresponding thermal phenomenon were studied by transmission electron microscopy (TEM) and differential scanning calorimetry (DSC) heating. The results indicated that there are significant differences in precipitation thermodynamics among the four bulk materials. In the CG and UFG materials without dislocations, homogeneous nucleation is the primary precipitation mechanism. However, the nucleation of the GP zones is suppressed at lower temperatures due to a reduction in the number of residual vacancies and the supersaturation in the UFG interiors. This is attributed to the absorption of vacancies and solute atoms by a greater volume of grain boundaries. It can be observed that the greater the excess of vacancies remaining in grain interiors, the lower the temperature at which nucleation of GP zones occurs. Defect-assisted heterogeneous nucleation was identified as the predominant precipitation mechanism in the UFG materials with dislocations and the NC materials. These defects encompass dislocations, lattice distortions, and grain boundaries. The decomposition processes of solid solutions were found to be almost complete at a lower temperature. The presence of dislocations, lattice distortions, and grain boundaries enables solute atoms to diffuse at a much faster rate, significantly enhancing the precipitation rate and reducing the nucleation and formation energies of various precipitate phases. Full article

The aim of this study was to develop cholic-acid-stabilized itraconazole nanosuspensions (ITZ-Nanos) with the objective of enhancing drug dissolution and oral absorption. A laboratory-scale microprecipitation–high-pressure homogenization method was employed for the preparation of the ITZ-Nanos, while dynamic light scattering, transmission electron microscope analysis, X-ray diffraction, differential scanning calorimetry, and high-performance liquid chromatography analysis were utilized to evaluate their physicochemical properties. The absorption and bioavailability of the ITZ-Nanos were assessed using Caco-2 cells and rats, with Sporanox^® pellets as a comparison. Prior to lyophilization, the particle size of the ITZ-Nanos measured approximately 225.7 nm. Both X-ray diffraction and differential scanning calorimetry confirmed that the ITZ remained crystalline within the nanocrystals. Compared to the pellets, the ITZ-Nanos exhibited significantly higher levels of supersaturation dissolution and demonstrated enhanced drug uptake by the Caco-2 cells. The AUC(0–t) value for the ITZ-Nanos in rats was 1.33-fold higher than that observed for the pellets. These findings suggest that cholic acid holds promise as a stabilizer for ITZ nanocrystals, as well as potentially other nanocrystals. Full article