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.