采用喷雾干燥法制得空心球状结构偏钨酸铵,通过固定床气固反应,以CO/H2为还原碳化气氛在700~900℃下制备了介孔结构空心球状碳化钨(WC).经XRD,SEM及EDS测试表明,WC粉末样品在保持了单相WC的前提下,样品存在一个微量缺碳的原子比例,其W/C〉1,且在高氢环境中WC球体表面有部分纳米颗粒依附于片状碳化钨基体上.将制备得到的WC粉末样品制成微电极,采用电化学测试技术研究了WC在硫酸介质中对甲醇的电催化氧化反应.结果表明,缺碳的介孔结构空心球状WC催化剂对甲醇氧化有着良好的电催化活性,并对动力学参数进行了研究,结果显示其反应的表观活化能为105.06kJ/mol,且其在微电极中的氧化行为受扩散控制.
The precursors ammonium metatungstate (AMT) microspheres were prepared by using an airflow spray drying method. Tungsten carbide (WC) samples were prepared by gas-solid reaction in the atmosphere of CO/H2 in 700~900 ℃. XRD,SEM and EDS results showed that the samples were pure WC,with a ratio of W/C1. SEM images show that the structure of WC is hollow microsphere with nanoparticles around the surface. The WC was applied to a catalytic electrode for methanol electro-oxidation reaction by a PME (powder microelectrode) method. The results showed that the lower carbide content meso-WC-PME exhibited catalytic activity and stability in the methanol electro-oxidation,with the activation energy being 105.06 kJ/mol. The electrode reaction was controlled by liquid diffusion.