Morphological and surface analysis of titanosilicate ETS-4 synthesized hydrothermally with organic precursors

Peter Q. Miraglia, Bilge Yilmaz, Juliusz Warzywoda, Stephane Bazzana, Albert Sacco

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23 Scopus citations

Abstract

Morphological and surface analysis was performed on titanosilicate ETS-4 crystals using atomic force microscopy (AFM) and field emission scanning electron microscopy. Crystals were synthesized hydrothermally at 175 °C in Teflon-lined stainless steel autoclaves using organic precursors. Rectangular and plate shaped crystals were formed with the largest crystals being 2×20×5 μm and 2×10×10 μm, respectively. EDX analysis revealed a disparity between the Si/Ti ratio in crystals characterized by different morphologies (2.5 for rectangular vs. 2.8 for plates). Growth occurred on the slowest growing and the largest crystal via a layer mechanism. Spiral hillocks were found on {100} surfaces of rectangular shaped crystals and on the largest faces of intergrown plate crystallites. Steps on these surfaces were observed to emanate from spiral hillocks and had a step height of 1.10±0.15 nm. The crystallographic d-spacing of the (200) plane, as measured by powder X-ray diffraction, correlated with the AFM measured step height.

Original languageEnglish
Pages (from-to)71-76
Number of pages6
JournalMicroporous and Mesoporous Materials
Volume69
Issue number1-2
DOIs
StatePublished - Apr 8 2004

Keywords

  • Atomic force microscopy
  • ETS-4
  • Step height
  • Surface structure
  • Titanosilicate

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