Transmission
electron microscopy (TEM), CO pulse, and N2O pulse titration
were applied to measuring Ni particle sizes on
Ni/α-Al2O3 catalysts. It was clarified
for the first time that the N2O pulse titration could estimate
the size at titration temperature between 50 and 100 °C, which
was confirmed by TEM observation. This agreement in the Ni particle
sizes by N2O titration and TEM observation means that the
Ni surface was fully covered with the monolayer of oxygen formed by
N2O decomposition and the adsorption of N2 and
N2O on the catalysts was negligible. The Ni particle sizes
estimated from the CO pulse technique were larger than those measured
by the TEM observations. This is because the stoichiometry of CO to
Ni was assumed to be one despite the complicated adsorption states
of CO on Ni surface. On the contrary, the stoichiometry of oxygen
to Ni using N2O pulse titration was one, which indicates
that the stoichiometry measurements were not required for this method.
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