This work presents a detailed study of hydrogen decrepitation (HD) to obtain mono-crystalline Nd-Fe-B powder. The effect of decrepitation temperature has been investigated to optimize both particle size and shape. Differential scanning calorimetry was applied to analyze the hydrogenation kinetics of Nd2Fe14B and Nd-rich phases in the range of 25 to 300 degrees C. Thermogravimetry and X-ray diffraction allowed determining the hydrogen ab-sorption of the whole alloy and the matrix phase, respectively. While scanning electron microscopy (SEM) was used to visualize particle shape and size, dynamic image analysis was applied to evaluate quantitatively these properties. The high monocrystallinity of the powder was confirmed by electron backscattering diffraction. The partial pressure of hydrogen required to initiate the hydrogenation reactions decreases when the temperature increases. The hydrogen absorbed by the whole alloy and, in particular, by the Nd2Fe14B phase decreases with temperature. Below 150 degrees C, the hydrogen absorbed by the Nd2Fe14B phase produces a significant transgranular cracking that is undesirable for particle shape. At 300 degrees C, the fast and limited absorption of hydrogen by the Nd-rich phase causes insufficient intergranular fracture and, hence, polycrystallinity. Between 150 and 300 degrees C, the controlled fragmentation resulted in monocrystalline particles with a more equiaxial shape, which is a suitable precursor to develop anisotropic ultrafine powders by the hy-drogenation, disproportionation, desorption, recombination (HDDR) process.(c) 2023 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).

Gas atomized Nd-Fe-B powders of several compositions were separated in different size fractions by sieving. These fractions were annealed between 1100 degrees C and 1150 degrees C for 24 and 96 h. The oxygen content of the powders was measured before and after annealing for the different size fractions. The oxygen concentration of the powders depends strongly on the particle size and increases significantly during annealing, particularly in the case of small particle sizes. The effect of particle size on the microstructural changes was analyzed in detail, particularly on grain growth, using high resolution scanning electron microscopy and transmission electron microscopy. Electron back scattering diffraction was used to measure grain size. When the particle size rises, the degree of sintering decreases and the higher solid/vapor surface area reduces the mobility of grain boundaries. Oxidation also reduces grain growth rate and its effect is more evident for particles sizes below 45-63 mu m and high Nd concentrations. Nb addition leads to the formation of intra- and intergranular precipitates. The size of these Nb-Fe-containing precipitates increases with the particle size for equivalent annealing conditions. At 1150 degrees C, Nb loses its effect as an inhibitor of grain growth in the particle size fractions larger than 45-63 mu m.

Nd-Fe-B powders of different compositions were produced by gas atomization. These powders were annealed between 1000 and 1150 degrees C for several times to study the microstructural evolution. Differential scanning calorimetry was used to determine the thermal transitions on the as-atomized powders and after slow solidification. The microstructure was studied by high resolution scanning electron microscopy at each stage. Electron back scattering diffraction was used to measure grain size and confirm that gas atomized powders are isotropic. It was observed the formation of necks between the particles, densification, and grain growth due to liquid phase sintering. Grain growth and densification occur in parallel by a dissolution-reprecipitation mechanism. The effect of Nd content and Nb addition on the microstructural changes was analyzed in detail, particularly on grain growth. The degree of sintering increases with Nd content, as this element enhances the formation of the liquid phase. Nb addition leads to the formation of precipitates that delay densification and grain growth at 1000 degrees C, but promote abnormal grain growth at 1100 degrees C.

We report on the magnetic properties of NdFeB powders produced by gas atomization, which is a powder manufacturing technology scarcely used in the past to produce such alloys. Using this technique, we have produced several ternary NdFeB alloys with Nd contents between 26.9 wt.% and 28.5 wt.%. The as-atomized powders were split into different size fractions by sieving. Subsequently, we measured the magnetic properties as a function of temperature, between 10 and 400 K, and particle size. The magnetic behavior depends strongly on the microstructure of the material, which in turn is determined by the particle size. It is reported a slope anomaly in the curve of magnetization as a function of temperature at around 150 K due to a spin-reorientation transition. Since gas-atomized powders are isotropic, this magnetic transition produces an increment of the magnetization below this temperature.