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

• Main Authors: Awais Ikram, M. Farhan Mehmood, Zoran Samardžija, Richard Stuart Sheridan, Muhammad Awais, Allan Walton, Saso Sturm, Spomenka Kobe, Kristina Žužek Rožman
• Format: Article
• Language: English
• Published: MDPI AG 2019-05-01
• Series: Materials
• Subjects: rare earth permanent magnets; HDDR Nd₂Fe₁₄B; recycling; spark plasma sintering; coercivity; doping DyF₃
• Online Access: https://www.mdpi.com/1996-1944/12/9/1498
• ISSN: 1996-1944

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 (H_Ci) 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 H_Ci peaked to 1407 kA/m with the thermal treatment at 750 °C for 1 h. The obtained H_Ci 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.