Dieckmann Yvonne, Cölfen Helmut, Hofmann Heinrich, Petri-Fink Alke
Laboratory of Powder Technology, Ecole Polytechnique Fédérale de Lausanne, Lausanne, Switzerland.
Anal Chem. 2009 May 15;81(10):3889-95. doi: 10.1021/ac900043y.
We performed particle size and particle size distribution measurements for L-cysteine-stabilized ZnS/Mn nanoparticles in the size region below 10 nm. For this we applied transmission electron microscopy (TEM), analytical ultracentrifugation (AUC), dynamic light scattering (DLS), and asymmetric flow field flow fractionation (aF-FFF) measurements, and we calculated particle sizes with the help of X-ray diffraction (XRD) patterns and the shift of the band gap absorption in the UV-vis spectrum. The different methods are explained, and their limitations are discussed, with the conclusion that only a combination of different techniques can yield a realistic and complete picture about the size distribution of the sample. From these methods TEM, AUC, DLS, and aF-FFF measure the actual particle size distribution either in dispersion or after drying of the sample, whereas the particle size obtained from XRD patterns and with the help of the band gap widening corresponds to the average size of the crystal domains within the particles. We obtained particle size distributions with their maximum between 3 and 7 nm and a mean crystallite size of 3.5-4 nm.
我们对尺寸小于10 nm的L-半胱氨酸稳定的ZnS/Mn纳米颗粒进行了粒径和粒径分布测量。为此,我们采用了透射电子显微镜(TEM)、分析超速离心法(AUC)、动态光散射(DLS)和不对称流场流分馏法(aF-FFF)测量,并借助X射线衍射(XRD)图谱和紫外-可见光谱中带隙吸收的位移计算粒径。文中对不同方法进行了解释,并讨论了其局限性,得出的结论是只有不同技术的组合才能得出关于样品粒径分布的真实完整情况。在这些方法中,TEM、AUC、DLS和aF-FFF测量的是样品分散状态或干燥后的实际粒径分布,而通过XRD图谱并借助带隙变宽获得的粒径对应于颗粒内晶畴的平均尺寸。我们获得了最大粒径在3至7 nm之间的粒径分布,平均微晶尺寸为3.5 - 4 nm。