Search Results (40)

The effects of sigma (σ) phase morphology and distribution on the corrosion behavior of superduplex stainless steel (SDSS) were investigated. The aim of this study was to establish the relationship among distinct σ-phase morphologies, chromium redistribution, and the resulting corrosion mechanisms using electrochemical and microstructural characterization techniques. Heat treatments at 700 °C and 800 °C produced distinct σ-phase morphologies and volume fractions. Microstructural characterization was performed using optical microscopy (OM) and scanning electron microscopy (SEM), and corrosion behavior was evaluated using open-circuit potential (OCP), cyclic polarization, and double-loop electrochemical potentiodynamic reactivation (DL-EPR). Statistical analysis of chromium (Cr) distribution was used to link microstructural evolution to corrosion susceptibility. Lamellar σ promotes selective attack between lamellae of σ and secondary austenite due to localized Cr depletion, whereas σ at grain boundaries causes sensitization and intergranular corrosion. Notably, the sample aged at 800 °C for 30 h did not exhibit pitting during cyclic polarization. However, it showed clear signs of sensitization and selective attack in the DL-EPR test, indicating that temperature-driven Cr partitioning increases Cr gradients around σ. These gradients, together with the morphology and fraction of σ, ultimately govern the transition between lamellar-selective corrosion and grain-boundary sensitization. Overall, the findings underscore the importance of combining microstructural and electrochemical assessments to accurately predict localized corrosion and sensitization in SDSS. Full article

A corrosion device was established to simulate the service environment of stainless steel heat exchanger tubes in a gas water heater. The pitting corrosion behaviors on the inner walls of 444, 445 and 316L stainless steel tubes were investigated in a tap water solution at 60 °C under different heating temperatures from 600 to 800 °C for 500 h by means of optical microscopy (OM), scanning electron microscopy (SEM) and X-ray diffraction (XRD) analyses. The increase in heating temperature significantly promotes the thickening of scale layers and the formation and growth of corrosion pits on the inner surfaces of the three stainless steel tubes. Under different heating temperature conditions, the maximum and average depths of corrosion pits decrease sequentially from 444 to 445 and then to 316L stainless steel. The scales have similar compositions for the three steel tubes, but the scale thickness is thinner on 316L stainless steel than on the other two steels. In addition, the double-loop electrochemical potentiokinetic reactivation (DL-EPR) test indicates that there is almost no sensitization for the outer walls of the three stainless steel tubes after being heated at 800 °C. Full article

Direct hydroxylation of benzene to phenol using hydrogen peroxide is a cornerstone of sustainable green chemistry. This paper presents the results of a stability study of an iron-containing mordenite catalyst in the liquid-phase hydroxylation of benzene to phenol with a 30% aqueous hydrogen peroxide solution. The study utilizes a combination of catalytic activity measurements, dynamic light scattering (DLS), and electron paramagnetic resonance (EPR) spectra. The system is initially shown to exhibit high phenol selectivity; however, over time, DLS measurements indicate aggregation of the catalyst particles with an increase in the average particle diameter from 1.8 to 2.6 μm and the formation of byproducts–dihydroxybenzenes. Iron is present predominantly as magnetite nanoparticles (Fe₃O₄) ~10 nm in diameter, stabilized on the outer surface of mordenite, with minor leaching (<10%) due to the formation of iron ion complexes with ascorbic acid as a result of the latter’s interaction with magnetite particles. Using a thermodynamic approach based on the Ulich formalism (first and second approximations), it is shown that the reaction of benzene hydroxylation H₂O₂ in the liquid phase is thermodynamically quite favorable (ΔG° = −(289–292) kJ·mol⁻¹ in the range of 293–343 K, K = 1044–1052). It is shown that ascorbic acid acts as a redox mediator (reducing Fe³⁺ to Fe²⁺) and a regulator of the catalytic medium activity. The stability of the catalytic system is examined in terms of the Lyapunov criterion: it is shown that the total Gibbs free energy (including the surface contribution) can be considered as a Lyapunov functional describing the evolution of the system toward a steady state. Ultrasonic (US) treatment of the catalytic system is shown to redisperse aggregated particles and restore its activity. It is established that the catalytic activity is due to nanosized Fe₃O₄ particles, which react with H₂O₂ to form hydroxyl radicals responsible for the selective hydroxylation of benzene to phenol. Full article

Potassium (K⁺) channel blockers are promising anticancer agents but suffer from off-target toxicities. We designed cross-linked poly-2-Hydroxyethyl methacrylate (HEMA)–pectin nanogels (HPN) to deliver two model blockers—dofetilide (Dof) and azimilide (Azi)—and evaluated their physicochemical properties, release behavior, and in vitro anticancer activity. HPN was synthesized by surfactant-assisted aqueous nanogel polymerization and comprehensively characterized (FTIR, DLS, TEM/SEM, XRD, BET). The particles were monodispersed with a mean diameter ~230 nm, compatible with tumor accumulation via the Enhanced Permeability and Retention (EPR) effect, and exhibited a microporous matrix suitable for controlled release. Drug loading was higher for Dof than for Azi, with DL% values of 82.30 ± 3.1% and 17.84 ± 2.9%, respectively. Release kinetics diverged: Azi-HPN followed primarily first-order diffusion with a rapid burst, whereas Dof-HPN showed mixed zero/first-order behavior. Cytotoxicity was assessed in A549 lung cancer and BEAS-2B bronchial epithelial cells. Both free and nano-formulated blockers were selectively toxic to A549 with minimal effects on BEAS-2B. Notably, a hormesis-like pattern (low-dose stimulation/high-dose inhibition in MTT) was evident for free Dof and Azi; encapsulation attenuated this effect for Dof but not for Azi. Co-administration with paclitaxel (Ptx) potentiated Dof-HPN cytotoxicity in A549 but did not enhance Azi-HPN, suggesting mechanism-dependent drug-drug interactions. Overall, HPN provides a biocompatible platform that improves K⁺ blocker delivery. Full article

Among the many nanomaterials studied for biomedical uses, silica and gold nanoparticles have gained significant attention because of their unique physical and chemical properties and their compatibility with living tissues. Mesoporous silica nanoparticles (MSNs) have great stability and a large surface area, while gold nanoparticles (AuNPs) display remarkable optical features. Both types of nanoparticles have been widely researched for their individual roles in drug delivery, imaging, biosensing, and therapy. When combined with gadolinium (Gd), a common contrast agent, these nanostructures provide improved imaging due to gadolinium’s strong paramagnetic properties. This study focuses on incorporating gold nanoparticles and gadolinium into a silica matrix to develop a theranostic system. Various analytical techniques were used to characterize the nanocomposites, including infrared spectroscopy (FTIR), ultraviolet-visible spectroscopy (UV-Vis), thermogravimetric analysis (TGA), nitrogen adsorption, scanning electron microscopy (SEM), dynamic light scattering (DLS), X-ray fluorescence (XRF), X-ray diffraction (XRD), vibrating sample magnetometry (VSM), and neutron activation analysis (NAA). Techniques like XRF mapping, XANES, nitrogen adsorption, SEM, and VSM were crucial in confirming the presence of gadolinium and gold within the silica network. VSM and EPR analyses confirmed the attenuation of the saturation magnetization for all nanocomposites. This validates their potential for biomedical applications in diagnostics. Moreover, activating gold nanoparticles in a nuclear reactor generated a promising radioisotope for cancer treatment. These results indicate the potential of using a theranostic nanoplatform that employs mesoporous silica as a carrier, gold nanoparticles for radioisotopes, and gadolinium for imaging purposes. Full article

Background/Objectives: Boron neutron capture therapy (BNCT) is a promising, less-invasive anticancer treatment. However, the development of effective boron-based agents (BNCT probes) remains a critical and challenging issue. Previously, we developed a styrene–maleic acid (SMA) copolymer conjugated with glucosamine, encapsulating boronic acid, which exhibited tumor-targeted distribution via the enhanced permeability and retention (EPR) effect. Building upon this approach, in this study, we designed and synthesized a series of SMA-based polymeric probes for BNCT and evaluated their biological activities, with a particular focus on tumor-targeting properties. Methods: Two SMA-based BNCT nanoprobes, SMA–glucosamine conjugated Borax (SG@B) and SMA-conjugated aminophenylboronic acid encapsulating tavaborole (S-APB@TB), were designed and synthesized. The boron content in the conjugates was quantified using inductively coupled plasma mass spectrometry (ICP-MS), while particle sizes were measured via dynamic light scattering (DLS). In vitro cytotoxicity was assessed using the MTT assay in mouse colon cancer C26 cells. The tissue distribution of the conjugates was analyzed in a mouse sarcoma S180 solid tumor model using ICP-MS. Results: Both SG@B and S-APB@TB formed nanoformulations with average particle sizes of 137 nm and 99 nm, respectively. The boron content of SG@B was 2%, whereas S-APB@TB exhibited a significantly higher boron content of 14.4%. Both conjugates demonstrated dose-dependent cytotoxicity against C26 cells, even in the absence of neutron irradiation. Notably, tissue distribution analysis following intravenous injection revealed higher boron concentrations in plasma and tumor tissues compared to most normal tissues, with S-APB@TB showing particularly favorable tumor accumulation. Conclusions: These findings highlight the tumor-targeting potential of SMA-based BNCT nanoprobes. Further investigations are warranted to advance their clinical development as BNCT agents. Full article

The nuclear industry uses 304L stainless steel to construct canisters for storing spent nuclear fuel. The spent nuclear fuel canisters require the lifetime prediction and robustness of their corrosion behavior over periods ranging from thousands to hundreds of thousands of years. Since nuclear power plants are predominantly located in coastal areas, where storage conditions are highly vulnerable to chloride environments, extensive research has been conducted to enhance the canisters’ stress corrosion cracking (SCC) resistance. The welded canisters inherently possess residual tensile stress, prompting the application of plastic deformation-based techniques to boost their SCC resistance, with peening being the most prevalent method. It is reported that UNSM increases the SCC resistance by plastic deformation through surface treatment. In this study, the commercial 304L stainless steel was subjected to UNSM treatment on base metal, heat affected zone (HAZ), and weld metal U-bend test specimens to induce compressive residual stresses up to a depth of 1 mm. The impact of peening treatment on SCC properties was explored through microstructural analysis, corrosion properties analysis, and compressive residual stress assessments. The U-bend specimens underwent SCC testing (in 42% MgCl₂ at 155 °C), microstructure examination using an optical microscope (OM) and a scanning electron microscope (SEM), electron backscatter diffraction (EBSD) analysis, and compressive residual stress measurements via the hole-drilling method. Corrosion behavior on the surface and cross-section was evaluated using anodic polarization tests, electrochemical impedance spectroscopy (EIS) measurements, double loop-electrochemical potentiokinetic reactivation (DL-EPR) tests, and ASTM A262 Pr. C tests. The compressive residual stress imparted by UNSM refined the outermost grains of the cross-section and enhanced the corrosion resistance of 304L stainless steel. Furthermore, it led to a longer crack initiation time, a reduced crack propagation rate, and improved SCC properties. Full article

Improper thermal cycles on duplex stainless steels can lead to the formation of detrimental phases or alter the proportion of ferrite and austenite phases, thus influencing the material’s mechanical properties and corrosion resistance. Therefore, this study aimed to evaluate the effect of aging (at 850 and 950 °C) and solubilization (at 1000 and 1150 °C) thermal treatments on microstructure, indentation hardness, elasticity modulus, and susceptibility to intergranular corrosion of UNS S32205 duplex stainless steel. The sigma phase (σ) formation in the aged samples, with hardness values between 8 and 10 GPa, was confirmed. Furthermore, the pieces treated from 1000 °C upwards showed that increased temperature favored the formation of more equiaxial grains and the ferrite fraction growth. The thermal treatments barely affected the elasticity modulus of austenite and ferrite grains, increasing the hardness of ferrite. The effect of sulfuric acid concentration in the intergranular corrosion was evaluated. Also, the deconvolution of the corrosion curves permits the determination of the influence of the different phases in the corrosion performance. These tests revealed sensitization only at the σ phase grain boundaries in the samples treated at 850 °C in electrolytes containing H₂SO₄ 2.5 mol/L and HCl 1 mol/L. Although the treatment at 950 °C led to the σ phase formation, its higher corrosion resistance was ascribed to the lower volumetric fraction of this phase, its morphology, and its increased Cr mobility compared to the 850 °C treatment. Therefore, it was shown that the σ characteristics and the sulfuric acid concentrations are determining factors in the UNS S32205 intergranular corrosion resistance. Full article

In a quest to vet UNS S32205 as a potential structural material to serve moderate-to-high temperature operations of NPP auxiliary components, the DL-EPR test was exploited. A bifronted scheme comprised of 650 and 850 °C discrete treatments intended to explore progressive eutectoid decomposition and degree-of-sensitization (DoS) scenarios was adopted. The nuance witnessed with yet another dual approach—the Cihal- and image processing (IP)-normalized signal landscape—was rationalized through its attribution to culprit microstructures. This was sought, inter alia, in the vicinity of grain boundaries and σ-phase inclusions by virtue of postmortem FESEM, STEM-EDX, HRTEM SAED and XRD ascertainment. Discernable reactivation-kinetics resurgence was believed to mark the onset of deleterious σ-phase dissolution. This only came into fruition with longer ageing times (8–17 h) at 650 °C and succumbed to prematurely (1 h), and at DC biases more cathodic than −0.25 VAg/AgCl with the 850 °C counterpart. Opportune corroboration was offered in i_r/i_a breakaway for the respective conditions, which was unveiled to be particularly pre-emptive (5 h) with IP- vs. Cihal-normalized peers (8 h) related to the 650 °C condition. Meanwhile, the 850 °C condition endured a similar surge after as little as 1 h of ageing across the board, which hints at concomitant sigma-phase culpability. Full article

The effect of tempering temperature on the microstructure and intergranular corrosion property of 2205 duplex stainless steel (DSS2205) was determined using a boiling acid intergranular corrosion test (boiling 65% nitric acid and 50% sulfuric acid–ferric sulfate), an optical microscope, a transmission electron microscope, and a double-loop electrochemical potentiokinetic reactivation (DL-EPR) test. The results show that the ferrite content of the DSS2205 is about 50% in a specimen close to a solid solution state (1050 °C for 1 h, then water-quenched) when tempered at 675 °C–725 °C for 1 h. As the tempering temperature rises to 750 °C–800 °C for 1 h, the ferrite content drops gradually from 49% to 35%. M₂₃C₆, FeCr (σ phase), and Cr₂N phases are precipitated when the specimen is tempered at 675°C–800 °C for 1 h. When the tempering temperature rises to 750 °C–800 °C for 1 h, the content and size of σ phase increase significantly. In the boiling acid intergranular corrosion test, when the specimen is tempered at 675 °C–725 °C for 1 h, the corrosion rate is higher than when it is tempered at 750 °C–800 °C for 1 h. In the DL-EPR test, when the specimen is tempered at 675 °C–800 °C for 1 h, the intergranular corrosion sensitivity rises gradually. External polarization is added during the DL-EPR test, and the test principle is different from that of the boiling acid intergranular corrosion test, resulting in a different sensitivity to intergranular corrosion compared to boiling acid intergranular corrosion. Full article

Austenitic stainless steels used in structural applications suffer from stress corrosion cracking due to residual stresses during welding. Much research is being conducted to prevent the stress corrosion cracking of austenitic steels by inducing compressive residual stresses. One method is ultrasonic shot peening (USP), which is used to apply compressive stress by modifying the mechanical properties of the material’s surface. In this study, 304L stainless steel was butt-welded by gas tungsten arc welding (GTAW) and subsequently subjected to compressive residual stress to a depth of 1 mm from the surface by a USP treatment. The influence of USP on microstructural changes in the base metal, the HAZ and weldment, and the corrosion properties was analyzed. A microstructural analysis was conducted using SEM-EDS, XRD, and EBSD methods alongside residual stress measurements. The surface and cross-sectional corrosion behavior was evaluated and analyzed using a potentiodynamic polarization test, electrochemical impedance spectroscopy (EIS) measurements, a double-loop electrochemical potentiokinetic reactivation (DL-EPR) test, and an ASTM A262 Pr. C test. The surface was deformed and roughened by the USP. The deformed areas formed crevices, and the inside of the crevices contained some cracks. The crevices and internal cracks caused pitting, which reduced the resistance of the passivation film. The cross-section was subjected to compressive residual stress to a depth of 1 mm from the surface, and the outermost area of the cross-section had fine grain refinement, forming a solid passivation film that improved the corrosion resistance. Full article

The accumulation of proteins in filter membranes limits the efficiency of filtering technologies for cleaning wastewater. Efforts are ongoing to coat commercial filters with different materials (such as titanium dioxide, TiO₂) to reduce the fouling of the membrane. Beyond monitoring the desired effect of the retention of biomolecules, it is necessary to understand what the biophysical changes are in water-soluble proteins caused by their interaction with the new coated filter membranes, an aspect that has received little attention so far. Using spin-label electron paramagnetic resonance (EPR), aided with native fluorescence spectroscopy and dynamic light scattering (DLS), here, we report the changes in the structure and dynamics of bovine serum albumin (BSA) exposed to TiO₂ (P25) nanoparticles or passing through commercial polyvinylidene fluoride (PVDF) membranes coated with the same nanoparticles. We have found that the filtering process and prolonged exposure to TiO₂ nanoparticles had significant effects on different regions of BSA, and denaturation of the protein was not observed, neither with the TiO₂ nanoparticles nor when passing through the TiO₂-coated filter membranes. Full article

A comparative investigation of amino acids (proline, cysteine, and alanine) as dosimetric materials using electron paramagnetic resonance (EPR) spectroscopy in the absorbed dosage range of 1–25 kGy is presented. There were no signals in the EPR spectra of the samples before irradiation. After irradiation, the complex spectra were recorded. These results showed that the investigated amino acids were sensitive to radiation. In the EPR spectrum of cysteine after irradiation, RS• radicals dominated. The effects of the microwave power on the saturation of the EPR signals showed the presence of at least three different types of free radicals in proline. It was also found out that the DL-proline and cysteine had stable free radicals after irradiation and represented a linear dosage response up to 10 kGy. On the other hand, the amino acid alanine has been accepted by the International Atomic Energy Agency as a transfer standard dosimetry system. In view of this, the obtained results of the proline and cysteine studies have been compared with those of the alanine studies. The results showed that the amino acids proline and cysteine could be used as alternative dosimetric materials in lieu of alanine in a dosage range of 1–10 kGy of an absorbed dose of γ-rays using EPR spectroscopy. Regarding the radiation sensitivity, the following order of decreased dosage responses was determined: alanine > DL-proline > cysteine > L-proline. Full article

This research concerns the investigation of the preparation of polymeric nanocarriers containing a flavonoid—naringenin, xanthohumol or isoxanthohumol—based on Pluronics by the thin-film formation method. The size of the formed micelles and their stability upon dilution were evaluated using Dynamic light scattering (DLS) analysis; the high values of the drug loading and the encapsulation efficiency confirmed that the proposed systems of flavonoids delivery consisting of Pluronic P123 and F127 nanomicelles could effectively distribute the drug into tumour tissues, which makes these nanocarriers ideal candidates for passive targeting of cancer cells by the enhanced permeation and retention (EPR) effect. The in vitro cytotoxicity of proposed flavonoids in the Pluronic formulations was investigated by the SRB assay with human colon cancer cells. We designed mixed polymeric micelles, which was a successful drug delivery system for the case of naringenin not being able to enhance the bioavailability and cytotoxic activity of xanthohumol and isoxanthohumol. Furthermore, it was observed that the higher amount of polymer in the formulation achieved better cytotoxic activity. Full article

A Ni-Cr-Mo-based C276 superalloy was cold rolled to 5–40% and annealed at 1050 °C for 30 min. The microstructure and grain boundary character distribution after cold rolling and annealing were characterized. Grain refinement and a certain amount of coincident-site lattice (CSL) boundaries were obtained through recrystallization. The fraction of CSL boundaries reached peak at the cold rolling of 15% and annealing at 1050 °C for 30 min, which was the critical condition for completed recrystallization. In addition, sensitization treatments and double-loop electrochemical potentiokinetic reaction (DL-EPR) tests were applied to the cold rolled and annealed samples. The samples with a high fraction of CSL boundaries showed higher intergranular corrosion resistance as compared to the ones with a low fraction of CSL boundaries. It implies that the intergranular corrosion resistance of C276 superalloy can be enhanced by optimizing the grain boundary structure through cold rolling and annealing. Full article