Synthesis of nanosized zirconium carbide from preceramic polymers by the facile one-pot reaction

摘要

A novel preceramic polymer, polyzirconoxanesal (PZS), was synthesized efficiently by one-pot protocol. The PZS polymer was characterized by the techniques of Fourier transform infrared spectra (FTIR), nuclear magnetic resonance (~1H-NMR and ~(13)C-NMR) and gel permeation chromatography (GPC). The precursor exhibited excellent solubility and rheology for the processing of ceramic matrix fiber composites. Pyrolytic conversion of the preceramic polymer was studied by means of thermogravimetric analysis (TGA), X-ray diffraction (XRD), scanning electron microscope (SEM) and element analysis. It is suggested that the polymer decomposed completely at 600℃and nanosized ZrC is formed at 1300℃ for 2 hr in argon atmosphere with a yield of 68.5%. To the best of our knowledge, this is the lowest temperature reported in the literatures for preparing ZrC ceramics from preceramic polymers. The obtained ZrC particles exhibit spherical morphology with size ranged in 20-100 nm.