Preparation and characterization of polyhedral oligomeric silsesquioxane (POSS) using domestic microwave oven

• Published in: Journal of non-crystalline solids 2015-11, Vol.428, p.82-89
• Main Authors: Penso, Igor, Cechinatto, Eduardo A., Machado, Giovanna, Luvison, Caroline, Wanke, Cesar H., Bianchi, Otávio, Soares, Márcio R.F.
• Format: Article
• Language: English
• Subjects: Condensation; Dielectrics; Domestic; Heating; Hydrolysis; Microwave; Microwaves; Nanomaterials; Ovens; Polyhedral oligomeric silsesquioxane; POSS; Synthesis
• ISSN: 0022-3093; 1873-4812
• DOI: 10.1016/j.jnoncrysol.2015.08.020

This paper reports the preparation and characterization of polyhedral oligomeric silsesquioxane (POSS) using a domestic microwave oven. The hybrid nanomaterials were synthesized using the hydrolytic condensation of vinyltriethoxysilane (VTES) and a VTES/tetraethyl orthosilicate (TEOS) mixture. The samples were characterized by FTIR, 1H-NMR, 29Si-NMR, GPC, SEM, TEM, WAXD and TGA. The dielectric heating of the VTES and VTES/TEOS systems enabled the production of POSS with increased yield, showing rates 47 and 59 times faster than conventional heating, respectively. The POSS VTES samples prepared by dielectric and conventional heating showed very similar chemical characteristics. However, for the POSS obtained with the addition of TEOS the same behavior was not observed, because of the selective effect occasioned by microwave-assisted synthesis. The morphological shape of the hybrid clusters is dependent on the synthesis method and the precursor type. The simple approach used in this work represents an alternative to obtaining nanomaterials more efficiently. •The combinations of TEOS and VOTES resulted in the random POSS structure.•The microwave-assisted synthesis shows superior reaction rate.•The POSS obtained with VTES by the conventional and microwave methods has similar chemical characteristics.