Self-supporting silicalite-1 layers were grown on mercury surface from clear solutions at temperatures 140-180 oC. Large silicalite-1 crystals were synthesized using TPABr as template. Layer morphology and thickness were characterized by SEM. Phase purity of silicalite-1 and orientation of crystals were determined by XRD. Layers with the thickness > 40 .mu.m were found to be highly compact. Wet HF etching of as-synthesized polycrystalline silicalite-1 layers caused formation of deep sharp slits at grain boundaries and thus it visualized them. Contrary to this result etching of calcined layers led to a kind of a negative image represented by preserved thin shells at crystal boundaries which were found to be impregnated by carbon residues formed during template removal. Results of etching experiments give a strong indication of the existence of a thin amorphous silica interface between neighbouring crystals. The etching patterns were somewhat different for large silicalite-1 crystals.
Libor Brabec (2004) studied this question.