Ba Jianhua, Feldhoff Armin, Fattakhova Rohlfing Dina, Wark Michael, Antonietti Markus, Niederberger Markus
Max Planck Institute of Colloids and Interfaces, Research Campus Golm, Potsdam, Germany.
Small. 2007 Feb;3(2):310-7. doi: 10.1002/smll.200600425.
The crystallization pathway of indium tin oxide nanoparticles during solvothermal synthesis in benzyl alcohol was investigated. The synthesis was stopped after different reaction times in the range of 1-24 h, and the structural and morphological characteristics of the products were analyzed by powder X-ray diffraction, electron microscopy, and UV/Vis spectroscopy. Interestingly, the crystallization mechanism does not proceed along a simple nucleation and growth pathway, but involves a two-step process. In the first 12 h an intermediate phase is formed, which consists of nanocrystallites 3-6 nm in size stabilized by an organic matrix. In this organic-inorganic network the nanoparticles are aligned into superstructures, but without any crystallographic orientation. After 12 h the intermediate phase is abruptly transformed into indium tin oxide nanoparticles with the bixbyite structure and with crystallite sizes of about 10-12 nm. This step is accompanied by the disappearance of the organic phase and the loss of the superstructure.
研究了苄醇溶剂热合成过程中氧化铟锡纳米颗粒的结晶途径。在1 - 24小时的不同反应时间后停止合成，并通过粉末X射线衍射、电子显微镜和紫外/可见光谱对产物的结构和形态特征进行了分析。有趣的是，结晶机制并非沿着简单的成核和生长途径进行，而是涉及一个两步过程。在前12小时形成了一个中间相，它由尺寸为3 - 6纳米的纳米微晶组成，由有机基质稳定。在这个有机 - 无机网络中，纳米颗粒排列成超结构，但没有任何晶体学取向。12小时后，中间相突然转变为具有方铁锰矿结构、微晶尺寸约为10 - 12纳米的氧化铟锡纳米颗粒。这一步伴随着有机相的消失和超结构的丧失。
