M. Polisset et J. Fraissard, H-1-NMR STUDY OF HYDROGEN ADSORPTION ON PD-NAY - INFLUENCE OF METAL-PARTICLE SIZE, Colloids and surfaces. A, Physicochemical and engineering aspects, 72, 1993, pp. 197-206
Small palladium particles on NaY zeolite have been studied by H-1 NMR
using hydrogen as a probe. Several species may be identified: hydrides
(alpha and beta) and chemisorbed and physisorbed hydrogen. The ranges
where the two hydrides exist are demonstrated by this method. NMR spe
ctra show two signals depending on the hydrogen concentration. The fir
st, detected at low concentration, is attributable to the alpha-hydrid
e and the chemisorbed hydrogen. Its resonance shift varies from -100 t
o 0 ppm (vs TMS). The variation is linear up to a coverage theta almos
t-equal-to 1. Beyond this value the second signal appears and increase
s at the expense of the previous one. It corresponds to the beta-hydri
de; its chemical shift is positive (+26 ppm) and it is almost insensit
ive to the hydrogen concentration and the metal dispersion. These resu
lts show also that the Pd-H(alpha) concentration depends on the covera
ge of the surface and that it is possible to produce a monolayer of hy
drogen on the metal just before formation of the beta-hydride.