C. Lamberti et al., Structural characterization of Ti-silicalite-1: A synchrotron radiation X-ray powder diffraction study, J CATALYSIS, 183(2), 1999, pp. 222-231
We present high-resolution X-ray powder diffraction (XRPD) data collected a
t the BM16 beamline at ESRF on a set of dehydrated Ti-silicalite-l (TS-1) s
amples having Ti content (molar ratio) x = [Ti]/([Ti] + [Si]) in the range
0-0.022. The cell volume values resulting from Rietveld refinements of the
powder diffraction data exhibit very good linear correlation (r = 0.99994)
with Ti content: V(x) = 2093.0x + V(0) [V(0) = 5335.8 Angstrom(3)]. This wo
rk represents a continuation of the important characterization work of the
EniRicerche group [J. Catal. 137, 497 (1992)] performed on TS-1 previously
treated with ammonium acetate, calcined, and measured in atmosphere (i.e.,
under partially hydrous conditions). Our results indicate that when XRPD me
asurements are performed under carefully controlled vacuum conditions a hig
hly linear correlation between V and x is obtained without any need for sam
ple pretreatment, Finally, the very high quality of our experimental data a
llows us to comment on the presence of some preferential framework T sites
for Ti substitution. Such sites were recently proposed by two different gro
ups on the basis of the results of molecular dynamics modeling. (C) 1999 Ac
ademic Press.