采用草酸盐热分解还原法制备了粒径1μm的多孔结构FeNi合金粉,研究了草酸铁镍前驱体热分解过程.结果表明,FeNi合金为纯BCC相,前驱体在加热过程中在217.5和352.5℃脱水和热分解释放出CO和CO2气体,产生多孔结构;前驱体热分解活化能为148.59 k J/mol,热分解过程遵循随机成核和随后生长模型,指前因子为1.25×107,动力学方程为G(α)=[-ln(1-α)]0.44.
According to the principles of simultaneous equilibrium and mass equilibrium, the thermodynamics model of the precipitation-coordination equilibrium of Ni2+-C2H8N2- 2-2 4C O -H2O system was established, and calculation for the relationships between concentration of each substance in solution and parameters was carried out, including pH value, concentrations of ethylenediamine and oxalate by MATLAB program. The results show that Ni exists as Ni2+and [Ni(C2O4)n]2-2n mainly at pH〈1 and pH=1-6, respectively. When pH〉6, the complex between Ni2+and ethylenediamine is predominant. The precursor of Ni microfiber was prepared by an oxalate precipitation process using ethylenediamine as a coordination agent, and the role of ethylenediamine in the growth of the precursor fiber was discussed. The Ni microfiber can be obtained by a thermal decomposition-reduction process of the precursor in N2 and H2 mixed atmosphere. The diameters and aspect ratios of the obtained Ni microfibers are 0.2-1 μm and 20-30, respectively.