Shanmugaml Sathish, Muthu Kesavan, Subramanian Balakumar
J Nanosci Nanotechnol. 2016 Jan;16(1):418-25. doi: 10.1166/jnn.2016.10645.
We have investigated the formation mechanism of ZnO microspheres in polyol medium. The synthesis conditions have been varied with respect to temperature, medium and Zn-precursor concentration. The X-ray diffraction (XRD) and Raman spectroscopy result shows that the prepared ZnO nanoparticles are hexagonal wurtzite crystal structure and quite crystalline in nature. High resolution transmission electron microscopy (HRTEM) image indicates that the microsphere consists of aggregated nanoparticles in the range of 6 nm to 15 nm. The samples prepared in ethylene glycol medium shows a characteristic ether bond vibration mode in FTIR and it is additionally confirmed by NMR analysis. Initially, the nanoparticles are self-assembled into loosely packed microsphere and then the particles are densely packed by ether bonds formed between the glycol molecules adsorbed on adjacent particles which then grow as perfect microspheres. The sample prepared in EG medium at 150 °C did not show much aggregation. This study proposes the possible mechanism for the formation of ZnO microsphere.
我们研究了多元醇介质中ZnO微球的形成机理。合成条件在温度、介质和锌前驱体浓度方面有所变化。X射线衍射(XRD)和拉曼光谱结果表明,制备的ZnO纳米颗粒为六方纤锌矿晶体结构,本质上结晶度良好。高分辨率透射电子显微镜(HRTEM)图像表明,微球由6纳米至15纳米范围内的聚集纳米颗粒组成。在乙二醇介质中制备的样品在傅里叶变换红外光谱(FTIR)中显示出特征性的醚键振动模式,核磁共振(NMR)分析进一步证实了这一点。最初,纳米颗粒自组装成松散堆积的微球,然后通过吸附在相邻颗粒上的二醇分子之间形成的醚键使颗粒紧密堆积,进而生长为完美的微球。在150℃下于乙二醇介质中制备的样品没有表现出太多聚集现象。本研究提出了ZnO微球形成的可能机理。