Spark plasma sintering as an effective texturing tool for reprocessing recycled HDDR Nd-Fe-B magnets with lossless coercivity

The low-pressure hot-deformation methodology was applied to reprocess the nanocrystalline hydrogenation–disproportionation–desorption–recombination (HDDR) Nd-Fe-B powders from end-of-life (EOL) permanent magnets’ waste to determine the mechanism of texture development and the resultant improvement in remanence (and BH$_{max}$) in the recycled material. Both the hot-pressed and hot-deformed magnets produced via spark plasma sintering (SPS) were compared in terms of their magnetic properties with respect to forging pressures. Also, a comparison was established with the microstructure to cite the effectiveness of texture development at low deformation rates and pressures which is pivotal for retaining high coercivity. The hot-pressed magnets maintain the high coercivity (better than 100%) of the original recycled powder due to the control of SPS conditions. The hot deformation pressure was varied from 100–150 MPa at 750 °C processing temperature to identify the optimal texture development in the sintered HDDR Nd-Fe-B magnets. The effect of post-hot-deformation thermal treatment was also investigated, which helped in boosting the overall magnetic properties and better than the recycled feedstock. This low-pressure hot deformation process improved the remanence of the hot-pressed magnet by 11% over the starting recycled powder. The M$_r$/M$_S$ ratio which was 0.5 for the hot-pressed magnets increased to 0.64 for the magnets hot-deformed at 150 MPa. Also, a 55% reduction in height of the sample was achieved with the c-axis texture, indicating approximately 23% higher remanence over the isotropic hot-pressed magnets. After hot deformation, the intrinsic coercivity (H$_{Ci}$) of 960 kA/m and the remanence (B$_r$) value of 1.01 T at 150 MPa is indicative that the controlled SPS reprocessing technique can prevent microstructure related losses in the magnetic properties of the recycled materials. This route also suggests that the scrap Nd-Fe-B magnets can be treated with recoverable magnetic properties subsequently via HDDR technique and controlled hot deformation with a follow-up annealing

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

Long-term oxidization and phase transition of InN nanotextures

The long-term (6 months) oxidization of hcp-InN (wurtzite, InN-w) nanostructures (crystalline/amorphous) synthesized on Si [100] substrates is analyzed. The densely packed layers of InN-w nanostructures (5-40 nm) are shown to be oxidized by atmospheric oxygen via the formation of an intermediate amorphous In-Ox-Ny (indium oxynitride) phase to a final bi-phase hcp-InN/bcc-In2O3 nanotexture. High-resolution transmission electron microscopy, energy-dispersive X-ray spectroscopy, electron energy loss spectroscopy and selected area electron diffraction are used to identify amorphous In-Ox-Ny oxynitride phase. When the oxidized area exceeds the critical size of 5 nm, the amorphous In-Ox-Ny phase eventually undergoes phase transition via a slow chemical reaction of atomic oxygen with the indium atoms, forming a single bcc In2O3 phase

Processability and Separability of Commercial Anti-Corrosion Coatings Produced by In Situ Hydrogen-Processing of Magnetic Scrap (HPMS) Recycling of NdFeB

The recycling of NdFeB magnets is necessary to ensure a reliable and ethical supply of rare earth elements as critical raw materials. This has been recognized internationally, prompting the implementation of large-scale legislative measured aimed at its resolution; for example, an ambitious recycling quote has been established in the Critical Raw Materials Act Successful recycling in sufficient quantities is challenged by product designs that do not allow the extraction and recycling of these high-performance permanent magnets without excessive effort and cost. This is particularly true for smaller motors using NdFeB magnets. Therefore, methods of recycling such arrangements with little or no dismantling are being researched. They are tested for the hydrogen-processing of magnetic scrap (HPMS) method, a short-loop mechanical recycling process. As contamination of the recycled material with residues of anti-corrosion coatings, adhesives, etc., may lead to downcycling, the separability of such residues from bulk magnets and magnet powder is explored. It is found that the hydrogen permeability, expansion volume, and the chosen coating affect the viable preparation and separation methods as recyclability-relevant design features

Long-term oxidization and phase transition of InN nanotextures

<p>Abstract</p> <p>The long-term (6 months) oxidization of hcp-InN (wurtzite, InN-w) nanostructures (crystalline/amorphous) synthesized on Si [100] substrates is analyzed. The densely packed layers of InN-w nanostructures (5-40 nm) are shown to be oxidized by atmospheric oxygen via the formation of an intermediate amorphous In-O_<it>x</it>-N_{<it>y </it>}(indium oxynitride) phase to a final bi-phase hcp-InN/bcc-In₂O₃nanotexture. High-resolution transmission electron microscopy, energy-dispersive X-ray spectroscopy, electron energy loss spectroscopy and selected area electron diffraction are used to identify amorphous In-O_<it>x</it>-N_{<it>y </it>}oxynitride phase. When the oxidized area exceeds the critical size of 5 nm, the amorphous In-O_<it>x</it>-N_{<it>y </it>}phase eventually undergoes phase transition via a slow chemical reaction of atomic oxygen with the indium atoms, forming a single bcc In₂O₃phase.</p