以MgCl2·6H2O、H3BO3和H2C2O4·2H2O为原料,利用草酸盐法制备出长度为4.0~8.0μm,直径为0.6~1.5μm,长径比约为10,形貌良好的硼酸镁晶须。采用XRD、SEM及TG-DTA等分析手段,研究了烧结温度、烧结时间、n(B)/n(Mg)、n(HzC204)/n(Mg)对硼酸镁晶须的生长过程和质量的影响,探讨了其最佳制备条件。结果显示,硼酸镁晶须的最佳制备条件为:烧结温度为800℃,烧结时间为4.0h,n(B)/n(Mg)=1.2,n(H2C2O4)/n(Mg)=1.2。根据XRD和TGDTA分析,MgC2O4前驱体对硼酸镁晶须的形成和生长有较大的促进作用,分解产物不引入其它杂质,使得制备的晶须纯度较高。晶须的生长机理为S-L-S机理。
With MgCl2 · 6H2O, HaBO3 and H2C2O4 · 2H2O as raw materials, magnesium borate whiskers were synthesized by oxalate method. The lengths of the whiskers varied from 4. 0 μm to 8. 0μm, the diameters varied from 0.6 μm to 1.5 tam, and the aspect ratio was about 10. The produced samples were characterized by XRD, SEM, and TG-DTA. The effects of reaetion temperature, reaction time, n(B)/n(Mg), and n(H2C2O4)/n(Mg) on the whisker growth process and product quality were explored. The best preparation conditions were obtained. It was found that the best prepared parameters of reaction temperature, reaction time, n (B)/n (Mg), and n ( Hz C4 04 ) / n(Mg) were 800 ℃ ,4. 0 h,1.2 and 1.2, respectively. According to the XRD and TG-DTA analysis, MgC2O4 precur- sor greatly promotes the formation and growth of Mg2 132 O2 whiskers, its decomposition products do not introduce im- purities,making the whiskers more purity. The whisker growth process is solid-liquid-solid (S-L-S) mechanism.