S. Ram et al., FORMATION OF ND2FE14B HYDRIDE BY MILLING OF ANHYDRIDE PARTICLES IN TOLUENE IN A CLOSED REACTOR, Bulletin of Materials Science, 20(8), 1997, pp. 1049-1058
When milling micrometer thin Nd2Fe14B platelets, of an average 1-2 mm
diameter, in toluene in a closed reactor, part of the toluene decompos
es at the surface of the platelets and yields nascent hydrogen and car
bon/low hydrocarbons. The hydrogen diffuses into the Nd,Fe,,B platelet
s and the carbon forms a thin surface passivation layer of the platele
ts, forming the stable Nd2Fe14BHx, x less than or equal to 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. A
n N-2 gas atmosphere, if used during the heating, facilitates the H-de
sorption process with the modified kinetic parameters. For example, th
e enthalpy of the H-desorption Delta H and the related activation ener
gy E-a have the measured values Delta H=153J/g and E-a = 58.2 kJ/mol i
n argon and Delta H = 256 J/g and E-a = 41.6 kJ/mol in N-2. It is argu
ed that N-2 gas has a fast reaction with the H atoms desorbing off the
thin sample platelets and forms NH3 gas with an instantaneous decreas
e 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 N-2 gas.