Zirconium nano building blocks based on the 3-butynoic acid ligand: Synthesis and thermomechanical studies of the resulting inorganic-organic hybrid material

A new zirconium nano building block (ZrNBB) was prepared by the reaction of Zirconium tetrapropoxide with 3‐butynoic acid in an alkoxide/acid at a 1 : 3 or 1 : 6 molar ratio. The complex was characterized by FTIR, 1H‐NMR and 13C‐NMR spectroscopy, thermogravimetric analysis, differential scanning calorimetry, energy‐dispersive X‐ray analysis, and elementary analysis. A spontaneous alkyne‐to‐allene isomerization process was observed for ZrNBB. A bulk sample was also prepared and analyzed via dynamical mechanical spectroscopy in compression mode. The zirconium complex was then embedded in a polymeric matrix by radical copolymerization with vinyl trimethoxysilane. The inorganic–organic hybrid material was chemically and thermally stable. The shear storage modulus and loss modulus were measured to determine the mechanical properties of the material. The preliminary results are presented. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012