Structural Characterization of Ti-Silicalite-1: A Synchrotron Radiation X-Ray Powder Diffraction Study

Abstract We present high-resolution X-ray powder diffraction (XRPD) data collected at the BM16 beamline at ESRF on a set of dehydrated Ti-silicalite-1 (TS-1) samples 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 )=2093.0 x + V (0) [ V (0)=5335.8 A 3 ]. This work 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 measurements are performed under carefully controlled vacuum conditions a highly linear correlation between V and x is obtained without any need for sample pretreatment. Finally, the very high quality of our experimental data allows us to comment on the presence of some preferential framework T sites for Ti substitution. Such sites were recently proposed by two different groups on the basis of the results of molecular dynamics modeling.