ACCURATE MEASUREMENT OF THE THERMAL EXPANSION OF MFI ZEOLITE MEMBRANES BY INSITU HTXRPD

摘要

Template removal by calcination of MFI type membranes is often accompanied by crack formation. The thermal behavior of MFI type membranes, synthesized with and without masking, was studied to understand the mechanism. Masking prevents growth of zeolite in the interior of the support during membrane synthesis. Rietveld refinements of powder diffraction data collected in situ at high temperature allowed to accurately determine the change in thermal expansion of the MFI film and the porous α-alumina support. During heating, a relatively large contraction of the cell volume during template removal occurred in the zeolite powder and in the film of the membrane prepared with masking. The much smaller decrease in the non-masked sample indicates that this membrane is under stress during heating and as a consequence, cracks are formed. The stress imposed in the membrane prepared without masking may be due to the opposite thermal behavior of the substrate in combination with strong bonds between the membrane and the support.