Controlled Synthesis of TiC Nanoparticles Using Solid Oxide Membrane Technology in Molten CaCl2

Abstract

Metal carbides (MCs), especially transition metal carbides have attracted a lot of attentions due to their unique properties, such as high strength and hardness, good chemical and thermal stability. In this paper, a new route was proposed for preparing TiC nanoparticles directly from TiO2/C precursor by using solid oxide membrane (SOM) technology in molten CaCl2. The TiO2/C pellet pressed under 8 MPa was used as the cathode, and a yttria-stabilized zirconia (YSZ) tube filled with carbon-saturated liquid tin was served as the anode. This process employs an inert SOM to separate the anodic reaction area from the molten electrolyte to control the electrolysis process. The electrochemical process was carried out in molten CaCl2 at 1000 °C and 4.0 V from 0.5 to 4 h. The characteristics of the phase composition and morphology of the electrolysis products were investigated. The product electrolyzed was examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM) with energy dispersive spectrometer (EDS). The results show that TiC nanoparticles can be obtained directly from TiO2/C mixture at 1000 °C, 4.0 V and for 4 h in molten CaCl2 and the current efficiency is calculated to be 74.1%. In conclusion, we suggest that the SOM process is a promising environmentally friendly and low energy costs electrochemical method for the facile and controllable electrodeoxidation of MOx/C precursors to micro/nanostructured MCs.