在298.15K下采用现代微量热技术监测了微乳液法原位合成MnMoO4·H2O纳米棒过程中能量变化的微量热曲线.该曲线显示,反应开始瞬时放热,有一个尖锐的放热峰,在随后的过程中分别出现一个强的吸热峰和放热峰.通过x射线粉末衍射仪(XRD)、场发射扫描电子显微镜(FESEM)和透射电子显微镜(TEM)等对MnMoO4·H2O纳米棒的结构、形貌及尺寸进行了表征.结合微乳液的特性和量热曲线,讨论了MnMoO4·H2O纳米棒生长过程中的形貌演变和热动力学信息.整个生长过程包含微乳液的碰撞凝聚、反应成核、结晶和生长过程.经计算,反应成核过程、晶化过程及晶体二次生长过程的速率常数分别为6.35×10^-3 ,7.18×10^-4和9.16×10^-5S-1.生长速率小于成核速率,这有利于纳米材料的形成.
A novel method utilizing in situ microcalorimetry to monitor the instantaneous information of MnMoO4 · H2O nanorods growth process in microemulsion was reported. We presented the microcalorimetric heat flow(MCHF) curve which traced the energy evolution of MnMoO4· H2O nanorods growth process. The MCHF curve revealed that an exothermic peak appeared firstly, and then followed by an endothermic peak and a second exothermic peak. Combined with the performance of microemulsion and the MCHF curve, we discussed the morphology evolution and the thermokinetic information of MnMoO4 · H2O nanorods growth process. The whole process contained the collision and coalescence-exchange of drops, reaction, nucleation, crystal crystallization and the secondary growth. The rate constant of the reaction and nucleation, crystal crystallization, and the secondary growth were found to be 6.35 ×10^-3, 7.18 × 10^-4, and 9.16 × 10^-5 s-1, respectively. The growth rate was less than the nucleation rate and it was helpful for the formation of nanoparticles, which further proved microemulsion as soft template for the controlled synthesis of nanomaterials had a scientific significance.