Synthesis of titanosilicate ETS-4 utilizing organic precursors

B. Yilmaz, K. G. Shattuck, P. Q. Miraglia, J. Warzywoda, A. Sacco

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ETS-4, a titanosilicate molecular sieve, was grown from various synthesis mixtures utilizing organic titanium (titanium isopropoxide) and silicon (tetraethyl orthosilicate) sources. Syntheses were performed at three different temperatures (403, 448, and 473 K) for heat treatment durations up to 15 days, utilizing various mixing methodologies. ETS-4 was obtained at all three temperatures. Analyses of morphology and surface characteristics of the products were carried out by utilizing field emission scanning electron microscopy (FE-SEM) and atomic force microscopy (AFM). FE-SEM analyses have demonstrated two types of morphology: the rectangular prism crystals with minimal intergrowth and the highly intergrown particles in the form of cuboids. Growth spirals were detected on the (100) surface of the ETS-4 crystals with rectangular prism morphology and the average step height was measured to be 1.10±0.15 nm. Energy dispersive X-Ray spectroscopy (EDX) analyses had shown a correlation between the relative titanium content of the ETS-4 crystals and their morphological characteristics. Nucleation and growth rates for ETS-4 synthesis utilizing organic precursors were also investigated and found to be dependent on the synthesis mixture composition and the crystallization temperature. Effects of several synthesis parameters, such as the composition of the synthesis mixture, the crystallization temperature, and the degree of mixing of the synthesis mixture prior to crystallization on the product characteristics were studied. It was determined that product uniformity in terms of degree of intergrowth, relative titanium content, size, and morphology were all affected by these synthesis parameters.

Original languageEnglish
Pages (from-to)763-769
Number of pages7
JournalStudies in Surface Science and Catalysis
Volume154 A
StatePublished - 2004


  • Crystal growth
  • Crystallization kinetics
  • ETS-4
  • Hydrothermal synthesis
  • Titanosilicate
  • Zeo-type


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