Sk. Purnell et al., GENESIS AND GROWTH OF PT PARTICLES ON MGO - CHARACTERIZATION BY X-RAY-ABSORPTION SPECTROSCOPY AND INFRARED-SPECTROSCOPY, Journal of physical chemistry, 98(4), 1994, pp. 1205-1212
Samples prepared by the reaction of [Pt(C3H5)(2)] With MgO powder were
treated in H-2 at temperatures in the range 25-150 degrees C and char
acterized by X-ray absorption spectroscopy and infrared spectroscopy.
As the temperature of treatment in H-2 was increased, the infrared spe
ctra indicated the disappearance of bands attributed to the allyl liga
nds, and the sample became gray, the color characteristic of a support
ed metal. Adsorption of CO was characterized by a single infrared peak
in the nu(CO) region at 2070 cm(-1), consistent with that observed fo
r CO chemisorbed on metallic Pt, The Fourier transforms of the EXAFS f
unctions measured near the Pt L(III) absorption edge for each sample c
onfirm the presence of metallic Pt, showing peaks at approximately 2.7
, 3.8, 4.7, and 5.6 Angstrom, consistent with the first, second, third
, and fourth nearest neighbors in bulk fee Pt. The EXAFS results indic
ate that the particle size increased from approximately 8 Angstrom aft
er treatment in H-2 at room temperature, to about 9 Angstrom after a s
imilar treatment at 50 degrees C, to about 10 Angstrom after treatment
at 150 degrees C. The metal-support interface was characterized by tw
o metal-support oxygen contributions, one at 2.18 Angstrom and one in
the range 2.7-2.9 Angstrom. The total Pt-O coordination number decreas
ed monotonically as the treatment temperature in H-2 increased. This r
esult confirms that the fraction of Pt atoms in contact with the suppo
rt decreased as the particle size increased.