Synthesis, crystal structure and thermal decomposition of Zr6O4(OH)4(CH3CH2COO)12

The present study reports on a novel zirconium oxo-hydroxypropionate complex, obtained by the reaction of zirconium acetylacetonate with propionic acid, used as an oxide precursor for applications in Zr based thin films deposition. The molecular structure of the zirconium precursor has been determined by X-ray diffraction on single crystals and was demonstrated to be [Zr6O4(OH)4(CH3CH2COO)12]2, in good agreement with the formula calculated from the thermogravimetric analysis. The zirconium complex precursor is a three dimensional channel-type polymer. The thermal decomposition of the zirconium precursor has been studied by simultaneous differential thermal analysis-thermogravimetry-mass spectrometry (DTA-TG-MS) both in air and argon atmosphere at a heating rate of 10 °C/min. The infrared spectroscopy (FT-IR) has confirmed the molecular structure as determined from the X-ray diffraction on single crystals. The aging of the precursor solution was investigated by NMR relaxometry measurements. The X-ray diffraction on the precursor powder at different temperatures was also performed to investigate the nature of the intermediate decomposition products.