Polycrystalline wafers of silicalite-1 etched by HF acid and viewed by SEM.pdfVIP

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Polycrystalline wafers of silicalite-1 etched by HF acid and viewed by SEM.pdf

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Polycrystalline wafers of silicalite-1 etched by HF acid and viewed by SEM.pdf

Short communication Polycrystalline wafers of silicalite-1 etched by HF acid and viewed by SEM L. Brabec*, M. Koc?ir???k J. Heyrovsky? Institute of Physical Chemistry, Academy of Sciences of the Czech Republic, Dolejs?kova 3, 182 23 Praha 8, Czech Republic Received 4 November 2003; received in revised form 6 January 2004; accepted 6 January 2004 Abstract HF etching of polycrystalline silicalite-1 wafers enables to visualize grain boundaries of non-calcined crystals by dissolution of a phase between individual crystals as well as to reveal resistant shells of calcined crystals by dissolution of a crystal bulk. # 2004 Elsevier B.V. All rights reserved. Keywords: HF etching; Grain boundaries visualization; Carbon residue 1. Introduction The number of studies dealing with etching of zeolite crystals seems to be very limited [1–4]. We have not found any work on etching of crystalline films of zeolites. Wloch [4] etched non-calcined crystals of ZSM-5 by HF in water–acetone solutions which represented a moderate etching agent as com- pared with HF acid. After such a treatment crystal edges remained sharp, no pits occurred and the crystal faces were smoothed by dissolution of a phase accompanying the crystal growth. During the process also a formation of a resistant thin TPAF layer was assumed. As concerns our non-calcined polycrystalline wafers, HF etching provided more information about wafer texture by visualizing grain boundaries of crys- tals. In calcined wafers a coating of crystals appeared, undoubtedly due to residual carbon species impreg- nating a material present at crystal boundaries. Our silicalite-1 wafers (Fig. 1) were prepared by hydrothermal synthesis on mercury support as was described by Kiyozumi et al. [5]. The synthesis tem- perature was usually 170 8C, the reaction time was 15–65 h. A colloidal solution with SiO2 species of ca. 25 nm size was used as a silica source. Composition of the reaction mixture was 10SiO2:NaOH:TPA- Br:800H2O. Removal of templat