Environmentally Friendly Approach for Nd2Fe14B Magnetic Phase Extraction by Selective Chemical Leaching: A Proof-of-Concept Study.

The green transition initiative has exposed the importance of effective recycling of Nd-Fe-B magnets for achieving sustainability and foreign independence. In this study, we considered strip-cast, hydrogenated, jet-milled Nd-Fe-B powder as a case study to explore the potential for selective chemical leaching of the Nd-rich phase, aiming to extract the Nd2Fe14B matrix phase. Diluted citric and nitric acids at concentrations of 0.01, 0.1, and 1 M were considered potential leaching mediums, and the leaching time was 15 min. Microstructural investigation, magnetic characterization, and elemental compositional analysis were performed to investigate leaching efficiency and selectivity. Based on SEM analysis, Nd/Fe ratio monitoring via ICP-MS, and the high moment/mass value at 160 emu/g for the sample leached with 1 M citric acid, 1 M citric acid proved highly selective toward the Nd-rich phase. Exposure to nitric acid resulted in a structurally damaged Nd2Fe14B matrix phase and severely diminished moment/mass value at 96.2 emu/g, thus making the nitric acid unsuitable for selective leaching. The presence of hydrogen introduced into the material via the hydrogen decrepitation process did not notably influence the leaching dynamics. The proposed leaching process based on mild organic acids is environmentally friendly and can be scaled up and adopted for reprocessing industrial scrap or end-of-life Nd-Fe-B magnets to obtain single-phase Nd-Fe-B powders that can be used for novel magnet-making.

Presence of polyethylene terephthalate (PET) fibers in hyporheic zone alters colonization patterns and seasonal dynamics of biofilm metabolic functioning.

Worldwide, the production of plastics is increasing, and plastic pollution in aquatic environments is a major global concern. Under natural conditions, plastic weathers to smaller pieces called microplastics (MP), which come in various shapes, with fibers often being the most common in freshwater sediments. The hyporheic zone, an ecotone between surface and groundwater, is important for the transport and fate of all MP particles. The main metabolic pathways in rivers take place in the hyporheic zone and are driven by a diverse microbial community. The objective of this study was to investigate in situ whether the presence of PET fibers in riverbed sediments affects patterns of colonization and the seasonal dynamics of microbial metabolic activities in the hyporheic zone. The effects of the presence of PET on microbial metabolism were evaluated in situ over a month (colonization study) and over a year (seasonal study) by measuring total protein content (TPC), and microbial respiration as respiratory electron transport system activity (ETSA) and by community-level physiological profiling (CLPP). Additionally, PET fibers were examined under a scanning electron microscope (SEM), and isotopic analysis (δ13C) of PET was performed after one year of exposure to field conditions. The findings demonstrated that during colonization and biofilm formation, and also over the seasons, the date had a large and significant impact on biofilm growth and activity, while PET presence slightly suppressed microbial biomass (TPC) and respiratory activity (ETSA). Overall microbial activity was repressed in the presence of PET fibers but there was a higher capacity for the utilization of complex synthetic polymer substrates (i.e., Tween 40) which have previously been linked to polluted environments. SEM micrographs showed diverse microbial communities adhering to PET fibers but little surface deterioration. Similarly, isotopic analysis suggested little deterioration of PET fibers after one year of in situ conditions. The study indicated that PET fibers present in riverbed sediments could have impacts on the metabolic functioning in rivers and thus affect their self-cleaning ability.

Direct Recycling of Nd-Fe-B Magnets Based on the Recovery of Nd2 Fe14 B Grains by Acid-free Electrochemical Etching.

Recycling of end-of-life Nd-Fe-B magnets is an important strategy for reducing the environmental dangers associated with rare-earth mining and overcoming the supply risks associated with the rare-earth elements. In this study, a novel concept for recycling of sintered Nd-Fe-B magnets by directly recovering the matrix Nd2 Fe14 B grains is presented. The procedure is based on the anodic etching of sintered Nd-Fe-B magnets in a nonaqueous dimethylformamide (DMF)/0.3 mol L-1 FeCl2 bath. Selective recovery of Nd2 Fe14 B grains was realized within the applied current density <5 mA cm-2 based on the etching priority of phases: metallic Nd > intergranular NdFe4 B4 > matrix Nd2 Fe14 B. The total energy consumption of the proposed recycling route is estimated to be 2.99 kWh kg-1 , which is comparable to the state-of-the-art methods. However, the proposed recycling route is currently the only procedure that enables repeated recycling of sintered Nd-Fe-B magnets in a closed-loop system.

Coercivity Increase of the Recycled HDDR Nd-Fe-B Powders Doped with DyF3 and Processed via Spark Plasma Sintering & the Effect of Thermal Treatments.

The magnetic properties of the recycled hydrogenation disproportionation desorption recombination (HDDR) Nd-Fe-B powder, doped with a low weight fraction of DyF3 nanoparticles, were investigated. Spark plasma sintering (SPS) was used to consolidate the recycled Nd-Fe-B powder blends containing 1, 2, and 5 wt.% of DyF3 grounded powder. Different post-SPS sintering thermal treatment conditions (600, 750, and 900 °C), for a varying amount of time, were studied in view of optimizing the magnetic properties and developing characteristic core-shell microstructure in the HDDR powder. As received, recycled HDDR powder has coercivity (HCi) of 830 kA/m, and as optimally as SPS magnets reach 1160 kA/m, after the thermal treatment. With only 1-2 wt.% blended DyF3, the HCi peaked to 1407 kA/m with the thermal treatment at 750 °C for 1 h. The obtained HCi values of the blend magnet is ~69.5% higher than the starting recycled HDDR powder and 17.5% higher than the SPS processed magnet annealed at 750 °C for 1 h. Prolonging the thermal treatment time to 6 h and temperature conditions above 900 °C was detrimental to the magnetic properties. About ~2 wt.% DyF3 dopant was suitable to develop a uniform core-shell microstructure in the HDDR Nd-Fe-B powder. The Nd-rich phase in the HDDR powder has a slightly different and fluorine rich composition i.e., Nd-O-F2 than in the one reported in sintered magnets (Nd-O-F). The composition of reaction zone-phases after the thermal treatment and Dy diffusion was DyF4, which is more abundant in 5 wt.% doped samples. Further doping above 2 wt.% DyF3 is ineffective in augmenting the coercivity of the recycled HDDR powder, due to the decomposition of the shell structure and formation of non-ferromagnetic rare earth-based complex intermetallic compounds. The DyF3 doping is a very effective single step route in a controlled coercivity improvement of the recycled HDDR Nd-Fe-B powder from the end of life magnetic products.

Quantitative Microanalysis of (1-x)Pb(Mg(1/3)Nb(2/3))O3×xPbTiO3 (PMNT) Ferroelectric Ceramics.

Optimized quantitative electron-probe microanalysis was applied for compositional characterization of a ferroelectric ceramic single crystal that was made from the complex perovskite-type solid-solution (1-x)Pb(Mg(1/3)Nb(2/3))O3×xPbTiO3 (PMNT). Cation concentrations were determined with high accuracy and ultimate relative experimental uncertainty of ≤±1%, showing that the average chemical composition of the crystal corresponds to Pb(Mg(1/3)Nb(2/3))(0.67)Ti(0.33)O3 (i.e., x=0.33), which is close to the morphotropic phase boundary composition. Over the PMNT single crystal slight compositional heterogeneity was measured for concentrations of the perovskite B-site cations Ti4+, Mg2+, and Nb5+, with variations up to ±2.3%, whereas the Pb concentration remained uniform within a variation below ±0.5%.

Gel-sol synthesis of rutile nanoparticles.

Titanium dioxide (TiO(2)) rutile nanoparticles were synthesized at temperatures below 100 °C using a gel-sol process that provides control of the final particles' characteristics, such as the nanoparticle size, morphology, crystal structure and crystallinity. The synthesized rutile nanoparticles were analyzed using X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results show that the gel-sol process allows control over the final nanoparticle characteristics with the proper choice of reaction parameters. The most profound influence on the nanoparticles' properties is achieved by the type and concentration of the acid used in the reaction mixture. The gel-sol synthesis resulted in anisotropic rutile nanoparticles that are 60-160 nm long, depending on the reaction parameters, and have an aspect ratio of about 5. A reaction mechanism is presented, explaining the influence of various reaction parameters on the characteristics of the TiO(2) nanoparticles.

Molecular ultrastructure of the urothelial surface: insights from a combination of various microscopic techniques.

The urothelium forms the blood-urine barrier, which depends on the complex organization of transmembrane proteins, uroplakins, in the apical plasma membrane of umbrella cells. Uroplakins compose 16 nm intramembrane particles, which are assembled into urothelial plaques. Here we present an integrated survey on the molecular ultrastructure of urothelial plaques in normal umbrella cells with advanced microscopic techniques. We analyzed the ultrastructure and performed measurements of urothelial plaques in the normal mouse urothelium. We used field emission scanning electron microscopy (FESEM), atomic force microscopy (AFM), transmission electron microscopy (TEM) on immunolabeled ultrathin sections (immuno-TEM), and freeze-fracture replicas (FRIL). We performed immunolabeling of uroplakins for scanning electron microscopy (immuno-FESEM). All microscopic techniques revealed a variability of urothelial plaque diameters ranging from 332 to 1179 nm. All immunolabeling techniques confirmed the presence of uroplakins in urothelial plaques. FRIL showed the association of uroplakins with 16 nm intramembrane particles and their organization into plaques. Using different microscopic techniques and applied qualitative and quantitative evaluation, new insights into the urothelial apical surface molecular ultrastructure have emerged and may hopefully provide a timely impulse for many ongoing studies. The combination of various microscopic techniques used in this study shows how these techniques complement one another. The described advantages and disadvantages of each technique should be considered for future studies of molecular and structural membrane specializations in other cells and tissues.