Formation of Nd2Fe14B hydride by milling of anhydride particles in toluene in a closed reactor

When milling micrometer thin Nd₂Fe₁₄B platelets, of an average 1–2 mm diameter, in toluene in a closed reactor, part of the toluene decomposes at the surface of the platelets and yields nascent hydrogen and carbon/low hydrocarbons. The hydrogen diffuses into the Nd₂Fe₁₄B platelets and the carbon forms a thin surface passivation layer of the platelets, forming the stable Nd₂Fe₁₄BH _x ,x ≤ 5, hydride at room temperature. On heating in a calorimeter, the hydrogen desorbs off the sample with a well-defined endotherm between 370 and 425 K. An N₂ gas atmosphere, if used during the heating, facilitates the H-desorption process with the modified kinetic parameters. For example, the enthalpy of the H-desorption ΔH and the related activation energyE _a have the measured values ΔH = 153 J/g andE _a = 58·2 kJ/mol in argon and ΔH = 256 J/g andE _a = 41·6 kJ/mol in N₂. It is argued that N₂ gas has a fast reaction with the H atoms desorbing off the thin sample platelets and forms NH₃ gas with an instantaneous decrease of the total external gas pressure at the sample. This supports the fast desorption of H atoms in the sample with the modified desorption kinetics in N₂ gas.