National Institute of Chemistry, Hajdrihova 19, SI-1000 Ljubljana, Slovenia.
J Colloid Interface Sci. 2010 Jun 15;346(2):317-23. doi: 10.1016/j.jcis.2010.03.001. Epub 2010 Mar 6.
ZnO nanoparticles of different sizes, from 20 to 200 nm in length, and morphologies, nanorods and coral-like structures, were synthesized via a simple one-pot synthesis by refluxing an oversaturated solution of zinc acetylacetonate hydrate in 1-butanol and isobutanol. On the basis of (1)H and (13)C NMR experiments, the reactions in both alcohols were found to proceed via the alcoholytic C-C cleavage of the acetylacetonate ligand, followed by the hydrolytic formation of the reactive Zn-OH intermediate from the water molecules present in the precursor hydrate species and/or those released during the condensation cycle. The zinc acetylacetonate conversion into ZnO in isobutanol is significantly slower than in the case when 1-butanol was used as both the medium and the reagent. FE-SEM studies showed that in 1-butanol the growth of the rod-shaped particles occurs via the agglomeration of ZnO primary particles that are less than 10 nm in size. The morphology of the particles formed in the isobutanol is time dependent, with the final coral-like structures developing from initially formed bundle-like structures.
通过在 1-丁醇和异丁醇中回流锌乙酰丙酮水合物过饱和溶液的简单一锅合成法，合成了不同尺寸（长 20 至 200nm）和形貌（纳米棒和珊瑚状结构）的 ZnO 纳米粒子。根据 1H 和 13C NMR 实验，发现两种醇中的反应都是通过乙酰丙酮配体的醇解 C-C 断裂进行的，然后是来自前体水合物种中的水分子和/或在缩合循环中释放的水分子水解形成反应性 Zn-OH 中间体。与使用 1-丁醇作为介质和试剂的情况相比，异丁醇中锌乙酰丙酮转化为 ZnO 的速度明显较慢。FE-SEM 研究表明，在 1-丁醇中，棒状颗粒的生长是通过小于 10nm 尺寸的 ZnO 初级颗粒的团聚来实现的。在异丁醇中形成的颗粒的形态是时间依赖性的，最终的珊瑚状结构是由最初形成的束状结构发展而来的。
