Search Results (310)

An anion exchange-assisted technique was used for the synthesis of platinum-decorated SnO₂ supports, providing nanocatalysts with enhanced activity for the reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP). In this study, a series of SnO₂ supports, namely SnA (synthesized almost at room temperature), SnB (hydrothermally treated at 180 °C), and SnC (annealed at 600 °C), are systematically investigated, all loaded with 1 mol% Pt from H₂PtCl₆ under identical mild conditions. The chloride ions from the SnCl₄ precursors were efficiently removed via a strong-base anion exchange reaction, resulting in highly dispersed, crystalline ~5 nm cassiterite SnO₂ particles. All Pt/SnO₂ composites displayed mesoporous structures with type IVa isotherms and H₂-type hysteresis, with SP1a (Pt on SnA) exhibiting the largest surface area (122.6 m²/g) and the smallest pores (~3.5 nm). STEM-HAADF imaging revealed well-dispersed PtOx domains (~0.85 nm), while XPS confirmed the dominant Pt⁴⁺ and Pt²⁺ species, with ~25% Pt⁰ likely resulting from photoreduction and/or interactions with Sn–OH surface groups. Raman spectroscopy revealed three new bands (260–360 cm⁻¹) that were clearly visible in the sample with 10 mol% Pt and were due to the vibrational modes of the PtOx species and Pt-Cl bonds introduced due the addition and hydrolysis of H₂PtCl₆ precursor. TGA/DSC analysis revealed the highest mass loss for SP1a (~7.3%), confirming the strong hydration of the PtOx domains. Despite the predominance of oxidized PtOx species, SP1a exhibited the highest catalytic activity (k_app = 1.27 × 10⁻² s⁻¹) and retained 84.5% activity for the reduction of 4-NP to 4-AP after 10 cycles. This chloride-free low-temperature synthesis route offers a promising and generalizable strategy for the preparation of noble metal-based nanocatalysts on oxide supports with high catalytic activity and reusability. Full article

Currently, numerous conventional airport runways suffer from cracking distresses and cannot meet their structural and functional requirements. To address the urgent demand for rapid and durable maintenance of airport runways, this study investigates the material optimization and curing behavior of cold-mix epoxy asphalt (CEA) for non-disruptive overlays. Eight commercial CEAs were examined through tensile and overlay tests to evaluate their strength, toughness, and reflective cracking resistance. Two high-performing formulations (CEA 1 and CEA 8) were selected for further curing characterization using differential scanning calorimetry (DSC) tests, and the non-isothermal curing kinetics were analyzed with different contents of Component C. The results reveal that CEA 1 and CEA 8 were selected as promising formulations with superior toughness and reflective cracking resistance across a wide temperature range. DSC-based curing kinetic analysis shows that the curing reactions follow an autocatalytic mechanism, and activation energy decreases with conversion, confirming a self-accelerating process of CEA. The addition of Component C effectively modified the curing behavior, and CEA 8 with 30% Component C reduced curing time by 60%, enabling traffic reopening within half a day. The curing times were accurately predicted for each type of CEA using curing kinetic models based on autocatalytic and iso-conversional approaches. These findings will provide theoretical and practical guidance for high-performance airport runway overlays, supporting rapid repair, extended service life, and environmental sustainability. Full article

In this study, the possibility of using cement bypass dust as a cement additive was investigated. The utilization of cement bypass dust remains a major problem in cement production, as huge amounts of it are stored in landfills. In this study, a hydrothermal treatment is proposed to modify the properties of this dust and to expand its use. Hydrothermal treatment with pure bypass dust and quartz was carried out to achieve a CaO/SiO₂ ratio of 1 to 2. Samples were synthesized at 200 °C for 2, 4, 8, and 24 h. To examine the influence of the hydrothermal treatment on cement properties, a sample with a CaO/SiO₂ ratio of 1, hydrothermally treated for 8 h, was selected. This study employed XRD, XRF, DSC-TG, and isothermal calorimetry. Most of the target synthesis products, e.g., tobermorite and calcium silicate hydrates, formed after 8 h of sample synthesis, during which quartz was added to bypass dust and a CaO/SiO₂ ratio of 1 was achieved. An examination of the composition of the liquid medium following hydrothermal processing showed that almost all chlorine passed into the liquid medium, while some K₂O remained in the solid synthesis product. The synthesized additive is an effective catalyst for the hydration of Portland cement. After a 28-day curing period, specimens incorporating modified bypass dust replacing up to 10% of the Portland cement by weight demonstrated compressive strengths comparable to, or surpassing, those of specimens composed exclusively of Portland cement. Full article

Moroccan oil shale ash (MOSA) represents an underutilized industrial by-product, particularly in the Rif region, where its high mineral content has often led to its neglect in value-added applications. This study highlights the successful conversion of MOSA into amorphous mesoporous silica (AS-Si) using a sol–gel process assisted by polyethylene glycol (PEG-6000) as a soft template. The resulting AS-Si material was extensively characterized to confirm its potential for environmental remediation. FTIR analysis revealed characteristic vibrational bands corresponding to Si–OH and Si–O–Si bonds, while XRD confirmed its amorphous nature with a broad diffraction peak at 2θ ≈ 22.5°. SEM imaging revealed a highly porous, sponge-like morphology composed of aggregated nanoscale particles, consistent with the nitrogen adsorption–desorption isotherm. The material exhibited a specific surface area of 68 m²/g, a maximum in the pore size distribution at a pore diameter of 2.4 nm, and a cumulative pore volume of 0.11 cm³/g for pores up to 78 nm. DLS analysis indicated an average hydrodynamic diameter of 779 nm with moderate polydispersity (PDI = 0.48), while a zeta potential of –34.10 mV confirmed good colloidal stability. Furthermore, thermogravimetric analysis (TGA) and DSC suggested the thermal stability of our amorphous silica. The adsorption performance of AS-Si was evaluated using methylene blue (MB) and ciprofloxacin (Cipro) as model pollutants. Kinetic data were best fitted by the pseudo-second-order model, while isotherm studies favored the Langmuir model, suggesting monolayer adsorption. AS-Si could be used four times for the removal of MB and Cipro. These results collectively demonstrate that AS-Si is a promising, low-cost, and sustainable adsorbent derived from Moroccan oil shale ash for the effective removal of organic contaminants from aqueous media. Full article

This research work focused on the development of an adsorbent biocomposite material based on polyhydroxybutyrate (PHB) and cellulose acetate derived from sugarcane (Saccharum officinarum) fibre, through cellulose acetylation. The resulting material represents both an accessible and effective alternative for the treatment and remediation of water contaminated with heavy metals, such as Ni (II). The biocomposite was prepared by blending cellulose acetate (CA) with the biopolymer PHB using the solvent-casting method. The resulting biocomposite exhibited a point of zero charge (pHpzc) of 5.6. The material was characterised by FTIR, TGA-DSC, and SEM analyses. The results revealed that the interaction between Ni (II) ions and the biocomposite is favoured by the presence of functional groups, such as –OH, C=O, and N–H, which act as active adsorption sites on the material’s surface, enabling efficient interaction with the metal ions. Adsorption kinetics studies revealed that the biocomposite achieved an optimal adsorption capacity of 5.042 mg/g at pH 6 and an initial Ni (II) concentration of 35 mg/L, corresponding to a removal efficiency of 86.44%. Finally, an analysis of the kinetic and isotherm models indicated that the experimental data best fit the pseudo-second-order kinetic model and the Freundlich isotherm. Full article

In this work, a finite element modelling methodology is presented for the prediction of the bending behaviour of a glass fibre-reinforced elastomer composite with embedded shape memory alloy (SMA) wire actuators. Three configurations of a multi-layered composite with differences in structural stiffness and thickness are experimentally and numerically analysed. The bending experiments are realised by Joule heating of the SMA, resulting in deflection angles of up to 58 deg. It is shown that a local degradation in the structural stiffness in the form of a hinge significantly increases the amount of deflection. Modelling is fully elaborated in the finite element software ANSYS, based on material characterisation experiments of the composite and SMA materials. The thermomechanical material behaviour of the SMA is modelled via the Souza–Auricchio model, based on differential scanning calorimetry (DSC) and isothermal tensile experiments. The methodology allows for the consideration of an initial pre-stretch for straight-line positioned SMA wires and an evaluation of their phase transformation state during activation. The results show a good agreement of the bending angle for all configurations at the activation temperature of 120 °C reached in the experiments. The presented methodology enables an efficient design and evaluation process for soft robot structures with embedded SMA actuator wires. 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

The present work aims to determine the levels of contaminant oils in biodiesel obtained from the residual oil of the industrial processing of Nile tilapia via Quasi-Isothermal Thermogravimetry (TGA-qISO) and Differential Scanning Calorimetry (DSC). For this purpose, mixtures of tilapia oil (OT) and biodiesel (BD) were prepared in the mass proportions of OT/BD (5:95 m/m), OT/BD (10:90 m/m), OT/BD (15:85 m/m), OT/BD (20:80 m/m), OT/BD (25:75 m/m) and OT/BD (30:70 m/m). These mixtures were used to construct the calibration curve of the TGA-qISO and DSC techniques. To evaluate the efficiency of these techniques, three samples were prepared at concentrations of 7.01 OT%, 16.66 OT% and 27.05 OT%. The data obtained show that the biodiesel/oil mixtures presented two stages of mass loss, the first between 100 and 200 °C, which was attributed to the decomposition of the biodiesel, and from 250 °C, to the decomposition of the oil. In the DSC curves of the mixtures, it was observed that as the concentration of tilapia oil in the mixtures increases, there is a decrease in the intensity of the peaks and a shift to a higher temperature range. Statistical tools show that the TGA-qISO measurements presented analytical curves with a correlation coefficient (r) of 0.9999, while in the DSC analyses, r of −0.9727 and −0.9903 were obtained. Analysis of variance (ANOVA) confirmed that there is no significant difference between the measurements performed by TGA-qISO and DSC. This result shows that both techniques can be used to determine the oil adulteration in biodiesel samples. Full article

In the pursuit of environmental sustainability, reduced emissions, and alignment with circular economy principles, bio-epoxy resin nanocomposites have emerged as a promising alternative to traditional petroleum-based resins. This study investigates the development of novel bio-epoxy nanocomposites incorporating iron-oxide nanoparticles (Fe₂O₃, MnP) as multifunctional fillers at loadings of 0.5 wt.% and 3.0 wt.%. MnP nanoparticles were synthesized and subsequently functionalized with citric acid (MnP-CA) to enhance their surface properties. Comprehensive characterization of MnP and MnP-CA was performed using X-ray diffraction (XRD) to determine the crystalline structure, attenuated total reflection Fourier-transform infrared spectroscopy (ATR-FTIR), thermogravimetric analysis (TGA), and zeta potential measurements to confirm surface functionalization. The bio-epoxy resins matrix (bio-EP), optimized for compatibility with MnP and MnP-CA, was thoroughly analyzed in terms of chemical structure, thermal stability, curing behavior, dynamic–mechanical properties, and surface characteristics. Non-isothermal differential scanning calorimetry (DSC) was employed to evaluate the curing kinetics of both the neat (bio-EP) and the MnP/MnP-CA-reinforced composites, offering insights into the influence of nanoparticle functionalization on the resin system. Surface zeta potential measurements further elucidated the effect of filler content on the surface charge and hydrophilicity. Magnetic characterization revealed superparamagnetic behavior in all MnP- and MnP-CA-reinforced (bio-EP) composites. This research provides a foundational framework for the design of green bio-epoxy nanocomposites, demonstrating their potential as environmentally friendly materials and representing an emerging class of sustainable alternatives. The results underscore the viability of bio-epoxy systems as a transformative solution for advancing sustainable resin technologies across eco-conscious industries. Full article

Thermokinetic characterization of amorphous carbamazepine was performed utilizing non-isothermal differential scanning calorimetry (DSC) and thermogravimetry (TGA). Structural relaxation of the amorphous matrix was described in terms of the Tool–Narayanaswamy–Moynihan model with the following parameters: Δh* ≈ 200–300 kJ·mol⁻¹, β = 0.57, x = 0.44. The crystallization of the amorphous phase was modeled using complex Šesták–Berggren kinetics, which incorporates temperature-dependent activation energy and degree of autocatalysis. The activation energy of the crystal growth was determined to be >320 kJ·mol⁻¹ at the glass transition temperature (T_g). Owing to such a high value, the amorphous carbamazepine is stable at T_g, allowing for extensive processing of the amorphous phase (e.g., self-healing of the quench-induced mechanical defects or internal stress). A discussion was conducted regarding the converse relation between the activation energies of relaxation and crystal growth, which is possibly responsible for the absence of sub-T_g crystal growth modes. The high-temperature thermal decomposition of carbamazepine proceeds via multistep kinetics, identically in both an inert and an oxidizing atmosphere. A complex reaction mechanism, consisting of a series of consecutive and competing reactions, was proposed to explain the second decomposition step, which exhibited a temporary mass increase. Whereas a negligible degree of carbamazepine degradation was predicted for the temperature characteristic of the pharmaceutical hot-melt extrusion (~150 °C), the degradation risk during the pharmaceutical 3D printing was calculated to be considerably higher (1–2% mass loss at temperatures 190–200 °C). Full article

Background/Objectives: The increasing prevalence of multidrug-resistant bacteria presents a major global health challenge, prompting a search for innovative antimicrobial strategies. This study aimed to develop and evaluate a novel nanobiostructure combining alumina nanoparticles (NPs) with the antimicrobial peptide lunatin-1 (Lun-1), forming peptide-functionalized nanofilaments. The main objective was to investigate how the site of peptide functionalization (C-terminal vs. N-terminal) affects membrane interactions and antibacterial activity. Methods: NP–peptide conjugates were synthesized via covalent bonding between lun-1 and alumina NP and characterized using transmission electron microscopy (TEM), X-ray diffraction (XRD), zeta potential analysis, dynamic light scattering (DLS), Fourier-transform infrared (FTIR), and solid-state ¹³C NMR. Antibacterial activities were assessed against different Gram-positive and Gram-negative strains. Biophysical analyses, including circular dichroism (CD), isothermal titration calorimetry (ITC), differential scanning calorimetry (DSC), and solid-state ²H NMR, were employed to evaluate peptide–membrane interactions in the presence of membrane-mimetic vesicles composed of POPC:POPG (3:1) and DMPC:DMPG (3:1). Results: Characterization confirmed the successful formation of NP–peptide nanofilaments. Functionalization at the N-terminal significantly influenced both antibacterial activity and peptide conformation compared to C-terminal attachment. Biophysical data demonstrated stronger membrane interaction and greater membrane disruption when lun-1 was conjugated at the N-terminal. Conclusions: The site of peptide conjugation plays a crucial role in modulating the biological and biophysical properties of NP–lunatin-1 conjugates. C-terminal attachment of lunatin-1 retains both membrane interaction and antibacterial efficacy, making it a promising strategy for the design of peptide-based nanotherapeutics targeting resistant pathogens. Full article

Straw biomass is a renewable but problematic fuel due to its high alkali and chlorine content, which can cause slagging and corrosion during combustion. To mitigate these issues, this study investigates the influence of aluminosilicate additives on the thermal behavior and combustion characteristics of straw biomass. Laboratory-scale testing is carried out using thermogravimetric analysis under atmospheric air, showing the TG, DTG, and DSC profiles of samples (kaolinite, halloysite, straw biomass, and straw biomass with 4 wt.% of halloysite). Additionally, the main combustion parameters, like the ignition temperature, the maximum peak temperature, the burnout temperature, and some combustion indexes, are presented. The results show the effect of a heating rate in the range of 5–20 °C/min. Moreover, in this study, two non-isothermal model methods (Kissinger and Ozawa) are used to estimate energy activation. While halloysite slightly affects the combustion indexes and marginally reduces energy activation, its overall influence does not significantly alter combustion efficiency. These findings support the potential and safe use of halloysite for the biomass combustion process. Full article

Welding of maraging steels leads to a microstructural gradient from base material (BM) to weld metal (WM). During post-weld heat treatment (PWHT) the precipitation and reverted austenite (γ_r) reactions will occur defining the mechanical properties. These reactions are affected by the microstructure and local chemical composition of each zone in the “as welded” (AW) condition. This effect has not been clearly described yet nor the evolution of the microstructure. The objective of this work was to analyse the phase transformations at the different zones of the welded joint during the PWHT to explain the microstructure obtained at each zone. Samples of C250 maraging steel were butt-welded by GTAW-P (Gas Tungsten Arc Welding—Pulsed) process without filler material. The AW condition showed an inhomogeneous microhardness profile, associated with a partial precipitation hardening in the subcritical heat affected zone (SC-HAZ) followed by a softening in the intercritical (IC-HAZ) and recrystallized heat affected zone (R-HAZ). A loop-shaped phase was observed between low temperature IC-HAZ and SC-HAZ, associated with γ_r, as well as microsegregation at the weld metal (WM). The microstructural evolution during PWHT (480 °C) was evaluated on samples treated to different times (1–360 min). Microhardness profile along the welded joint was mostly homogeneous after 5 min of PWHT due to precipitation reaction. The microhardness in the WM was lower than in the rest of the joint due to the depletion of Ni, Ti and Mo in the martensite matrix related with the γ_r formation. The isothermal kinetics of precipitation reaction at 480 °C was studied using Differential Scanning Calorimetry (DSC), obtaining a JMAK expression. The average microhardness for each weld zone was proposed for monitoring the precipitation during PWHT, showing a different behaviour for the WM. γ_r in the WM was also quantified and modelled, while in the IC-HAZ tends to increase with PWHT time, affecting the microhardness. Full article

Nowadays, nitrate ions and azo dyes are a significant source of water pollution due to their high toxicity, persistence, and potential to be carcinogenic. Both contaminants are the result of anthropogenic sources, such as sewage or industrial wastewater discharge; the first one results also as a consequence of the intensive use of fertilizers. In this work we report the use of a new quaternized pentablock copolymer (PTBr) for the removal of nitrate ions and methyl orange (MO) dye from water by adsorption processes. Morphological, chemical, and thermal properties of the pentablock copolymer were investigated, respectively, by scanning electron microscopy (SEM), Attenuated Total Reflectance Infrared Spectroscopy (ATR-FTIR) (FT-IR), and X-ray photoelectron spectroscopy (XPS), thermal gravimetric analysis (TGA), and differential scanning calorimetry (DSC) analyses. Anionic removal ability and adsorption rate in water solutions containing either a single contaminant species or a mix of the two contaminants were studied by UV–VIS absorbance spectroscopy as a function of time and initial concentration. The presence of imidazole groups confers on PTBr a positive charge and a hydrophilic character that are responsible for an effective removal of anions from water. PTBr film reports an adsorption efficiency of 10.15 mg/g for nitrate removal and this value is in line with others reported in the literature. In the case of the simultaneous presence of nitrate and MO, it is found that nitrate ions removal is slightly affected by the presence of the dye, since both contaminants compete for electrostatic interaction with imidazole groups. On the contrary, the dye removal does not show significant change with or without the presence of nitrate ions, probably due to other kinds of interaction that it can establish with the polymer surface (π-π interaction). The adsorption process and the related mechanisms are described using kinetic and isothermal models. Despite a certain reduction in the adsorption efficiency for one of the investigated contaminants, the results confirm the possibility of using the quaternized pentablock copolymer for the co-adsorption of both inorganic and organic anions. Full article

This study investigates the impact of various nucleating agents on the crystallization behavior, thermal stability, and mechanical properties of poly(3-hydroxybutyrate-co-3-hydroxyhexanoate) (P3HBHHx) with 6 mol% 3-hydroxyhexanoate (3HHx) units. Nucleating agents, including boron nitride (BN), poly(3-hydroxybutyrate) (PHB), talc, ultrafine cellulose (UFC), and an organic potassium salt (LAK), were incorporated to enhance the crystallization performance. Differential scanning calorimetry (DSC) revealed that BN and PHB significantly increased the crystallization temperature and reduced the crystallization time by half, with BN exhibiting the highest nucleation efficiency. Isothermal kinetics modeled using the Avrami and Lauritzen–Hoffman theories confirmed faster crystallization and reduced nucleation barriers in nucleated samples. Polarized optical microscopy (POM) revealed that the nucleating agents altered the spherulite morphology and increased the growth rates. Under fast cooling, only BN induced crystallization, confirming its superior nucleation activity. Thermogravimetric analysis (TGA) indicated minimal changes in thermal stability, while mechanical testing showed a slight reduction in stiffness without compromising the tensile strength. Overall, BN emerged as the most effective nucleating agent for enhancing the P3HBHHx crystallization kinetics, providing a promising strategy for improving processing efficiency and reducing the cycle times in industrial applications. Full article