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Silica materials are popular in biomedical applications as composites and drug delivery platforms due to their low toxicity and biocompatibility. Mesoporous silica nanoparticles are attractive drug delivery systems based on their porous silica framework with high surface area. In the preparation of mesoporous silica frameworks, most commonly, MCM-41, the efficient removal of the template responsible for introducing porous networks, cetyltrimethyl ammonium bromide (CTAB), is a critical step due to the template’s high toxicity in the environment and human health. In this work, we present a new one-pot approach of introducing challenging antibiotics within a silica framework without the need of toxic templates, but instead using micelle formation by an antibacterial agent. We demonstrate that micelles formed by cetylpyridinium chloride (CPC), a known antibacterial agent, entrap antibiotics such as rifampicin and ciprofloxacin. Extensive NMR studies elucidate the precise localisation of the antibiotic within the CPC micelle. Ciprofloxacin is placed between the outer and palisade region while rifampicin is located further into the hydrophobic CPC micelle core. In both cases, the formation of the silica framework can be built around the CPC-antibiotic loaded micelles. The resulting silica nanoparticles show loading of both CPC and antibiotic agents, porosity and dual antibacterial release upon disruption of the micelle within the silica framework. The design not only provides a strategy of a therapeutic design to form porous frameworks but also highlights the potential of precise antibiotic dose and release in nanoparticle systems.
Electromagnetic stirring is known to promote material flow, reduce porosity, uniform elements distribution, and refine grain in laser beam welding (LBW), which enhances the applicability of LBW in various industries. In this study, a phase-field model of dendrite growth in AA5754 Al alloy electromagnetic stirring laser beam welding was established. The model considered the thermal electromagnetic Lorentz force resulting from the interaction between the electric field generated by the Seebeck effect and the magnetic field, as well as the temperature gradient and solidification rate of the solidification interface obtained from the computational fluid dynamics electromagnetic stirring LBW model. The variation rules of dendrite growth with different magnetic parameters and effects are analyzed. Comprehensively, the magnetic field promotes the solidification rate, thus promoting interfacial instability and a large magnetic flux density leads to a faster interface instability. The solidification rate as well as the temperature gradient affect the growth rate, and the accelerated growth caused by the so lidification rate with a high frequency and a large magnetic flux density effectively inhibits the slow growth caused by the temperature gradient. The thermal electromagnetic Lorentz force is the main factor for the branch increment at low frequencies, while both thermal electromagnetic Lorentz force and temperature gradient in crease the number of branches at high frequencies. The calculated average branch numbers considering various factors in the stable stage under different magnetic parameters were consistent with the results of the scanning electron microscope tests.
Two-dimensional covalent organic frameworks (COFs) based on phosphinine and thiophene building blocks have been synthesized with two different side groups. The materials are denoted as CPSF-MeO and CPSF-EtO where CxxF correspond to the covalent framework, whereas P and S are related to heteroatoms phosphorous and sulfur. MeO and EtO indicate the substituents, i.e. methoxy and ethoxy.
Their morphologies were studied by scanning electron microcopy and X-ray scattering. The absence of crystalline reflexes in the X-ray pattern reveal that both materials are amorphous and can be considered as glasses. Furthermore, N2 adsorption measurements indicate substantial Brunauer–Emmett–Teller (BET) surface area values pointing to the formation of three-dimensional pores by stacking of the aromatic 2D layer. An analysis of the porosity of both COFs showed a mean radius of the pores to be of ca. 4 nm, consistent with their chemical structure. The COFs form nanoparticles with a radius of around 100 nm. The thermal behavior of the COFs was further investigated by fast scanning calorimetry. These investigations showed that both COFs undergo a glass transition. The glass transition temperature of CPSF-EtO is found to be ca. 100 K higher than that for CPSF-MeO. This large difference in the glass transition is discussed to be due to a change in the interaction of the COF sheets induced by the longer ethoxy group. It might be assumed that for CPSF-EtO more individual COF sheets assemble to larger stacks than for CPSF-MeO. This agrees with the much larger surface area value found for CPSF-EtO compared to CPSF-MeO. To corroborate the results obtained be fast scanning calorimetry dielectric measurements were conducted which confirm the occurrence of a dynamic glass transition. The estimated temperature dependence of the relaxation rates of the dielectric relaxation and their absolute values agrees well with the data obtained by fast scanning calorimetry. Considering the fragility approach to the glass transition, it was further found that CPSF-MeO is a fragile glass former whereas CPSF-EtO behaves as a strong glass forming material. This difference in the fragility points also to distinct differences in the interaction between the 2D COF molecules in both materials.
The Na salt of chloroacetic acid is condensed in suspension. Furthermore,glycolic acid is condensed in bulk or in concentrated solution by means of SnCl2 or 4-toluene sulfonic acid (TSA) as catalysts. The temperatures are varied from 160 to 200°C and the time from 1 to 5 days. Low molar mass cyclic poly(glycolic acid) (PGA) is detected by means of matrix-assisted laser desorption ionization time-of-flight (MALDI TOF) mass spectrometry in most PGAs. A predominance of certain cycles having an even number of repeat units is observed suggesting a thermodynamically favored formation of extended-ring crystals. Extremely high melting temperatures (up to 237.5°C)and high melting enthalpies are found for polycondensations with TSA in 1,2-dichlorobenzene.
The present work demonstrates a sustainable approach of using relatively coarser iron ore particles for ironmaking. The motivation is to reduce the energy consumption in the milling of the iron ore by utilizing coarser iron ore particles (+0.05 mm) and to select a suitable binder for improving pellet properties. Iron ore fines in the range of 0.05–0.25 mm was selected and classified into three size ranges. Fluxed iron ore pellets were prepared using lime as a binder for the basicity of 0, 1, and 2. Reduction of these pellets with a packed bed of coal fines was performed in the temperature range of 900–1200 °C for a duration of 30–120 min. The direct reduction kinetics of the iron ore pellets were studied by employing diffusion and chemical reaction control models to the experimental data. The results show that pellets made with coarser iron ore particles have improved reduction behavior and kinetics. The reduction reaction is found to be a mixed control. The activation energy for the reduction reaction varies from 44.3 to 74.76 kJ mol−1 as iron ore particle size decreases from 0.25 to 0.05 mm and basicity increases from 0 to 2.
Glycolide was polymerized in bulk by means of four different ROPPOC catalysts: tin(II) 2-ethylhexanoate (SnOct2), dibutyltin bis(pentafluoro-phenoxide) (BuSnOPF),zinc biscaproate (ZnCap), and zinc bis(pentafluoro-phenyl sulfide) (ZnSPF). The temperature was varied between 110 and 180°C and the time between 3 h and 7 days. For the few polyglycolides (PGAs) that were soluble extremely high molecular masses were obtained. The MALDI TOF mass spectra had all a low signal-to-noise ration and displayed the peaks of cyclic PGAs with a“saw-tooth pattern ”indicating formation of extended-ring crystallites in the mass range below m/z 2500. The shape of DSC curves varied considerably with catalyst and reaction conditions, whereas the long-distance values measured by SAXS were small and varied little with the polymeriza-tion conditions.
AbstractThe sustainable and resource-efficient production of wind energy plants requires the use of modern high-strength fine-grain structural steels. This applies to both foundation and erection structures, like mobile or ship cranes. During the assembly of steel structures, unacceptable defects can occasionally be found in the weld area. In most cases, the economical solution would be local thermal gouging of the affected areas and re-welding. Due to the high shrinkage restraint of the joint groove in the overall structure, the superposition of global and local welding-induced stresses may lead to crack formation and component failure, particularly in interaction with the degradation of the microstructure and mechanical properties of high-strength steels during the repair process. However, manufacturers hardly have any information about these issues and there is a lack of recommendations and guidelines to take these safety-relevant aspects into account in adequate repair concepts. The aim of this research is to derive recommendations for repair concepts appropriate to the stresses and materials involved providing a basis for standards and guidelines to avoid cold cracking, damage and expensive reworking especially for high-strength steels. Part 1 of this study involves systematic investigations of influences of shrinkage restraint during repair welding of two high-strength steels S500MLO for offshore application and S960QL for mobile crane structures. The quantification of the shrinkage restraint of repair weld joints was achieved by means of experimental and numerical restraint intensity analysis. In welding experiments with self-restrained slot specimens, restraint intensity and introduction of hydrogen via the welding arc using anti spatter spray were varied systematically to analyse the effect on welding result, residual stresses and cold cracking. It could be shown that increasing restraint intensities result in significantly higher transverse residual stress levels. In the case of hydrogen introduction S500MLO showed no cold cracking independent of the restraint conditions. However, S960QL was found to be considerably cold cracking sensitive if hydrogen is introduced. With increasing restraint intensity length and number of cold cracks increases significantly. Part 2 [1] of this study is focussed on microstructure and residual stresses due to gouging and stress optimization via adequate heat control parameters in repair welding.
The emission of ultrafine particles from small desktop Fused Filament Fabrication (FFF) 3D printers has been frequently investigated in the past years. However, the vast majority of FFF emission and exposure studies have not considered the possible occurrence of particles below the typical detection limit of Condensation Particle Counters and could have systematically underestimated the total particle emission as well as the related exposure risks. Therefore, we comparatively measured particle number concentrations and size distributions of sub-4 nm particles with two commercially available diethylene glycol-based instruments – the TSI 3757 Nano Enhancer and the Airmodus A10 Particle Size Magnifier. Both instruments were evaluated for their suitability of measuring FFF-3D printing emissions in the sub-4 nm size range while operated as a particle counter or as a particle size spectrometer. For particle counting, both instruments match best when the Airmodus system was adjusted to a cut-off of 1.5 nm. For size spectroscopy, both instruments show limitations due to either the fast dynamics or rather low levels of particle emissions from FFF-3D printing in this range. The effects are discussed in detail in this article. The findings could be used to implement sub-4 nm particle measurement in future emission or exposure studies, but also for the development of standard test protocols for FFF-3D printing emissions.
Antibacterial photodynamic therapy (a‐PDT) has emerged as a promising non‐invasive therapeutic modality that utilizes the combination of a photosensitive agent, molecular oxygen, and excitation light to generate reactive oxygen species (ROS), demonstrating remarkable activity against multidrug‐resistant bacterial infections. However, the effective use of conventional photosensitizers is significantly limited by a number of their shortcomings, namely, poor water solubility and low selectivity. Herein, we present a novel biocompatible water‐soluble nanocomposite based on hydrophobic tetraphenylporphyrin (TPP) molecules and hydrophilic ternary AgInS2/ZnS quantum dots incorporated into a chitosan matrix as an improved photosensitizer for a‐PDT. We demonstrated that TPP molecules could be successfully transferred into chitosan solution while remaining primarily in the form of monomers, which are capable of singlet oxygen generation. We performed a detailed analysis of the Förster resonance energy transfer (FRET) between quantum dots and TPP molecules within the nanocomposite and proposed the mechanism of the singlet oxygen efficiency enhancement via FRET.
With 2,2-dibutyl-2-stanna-1,3-dithiolane (DSTL) and 2-stanna-1,3-dioxa-4,5,6,7-dibenzoxepane (SnBiPh) as catalysts ring-expansion polymerizations (REP) were performed either in 2 M solution using three different solvents and two different temperatures or in bulk at 140 and 120 ◦C. A kinetically controlled rapid REP up to weight average molecular masses (Mẃs) above 300 000 was followed by a slower degradation of the molecular masses at 140 ◦C, but not at 120 ◦C Furthermore, a low molecular mass cyclic poly(L-lactide) (cPLA) with a Mn around 16 000 was prepared by polymerization in dilute solution and used as starting material for ring-ring equilibration at 140 ◦C in 2 M solutions. Again, a decrease of the molecular mass was detectable, suggesting that the equilibrium Mn is below 5 000. The degradation of the molecular masses via RRE was surprisingly more effective in solid cyclic PLA than in solution, and a specific transesterification mechanism involving loops on the surface of crystallites is proposed. This degradation favored the formation of extended-ring crystallites, which were detectable by a “saw-tooth pattern” in their MALDI mass spectra.