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采用分析超速离心法测定氧化石墨烯纳米片的横向尺寸。

Determination of the lateral dimension of graphene oxide nanosheets using analytical ultracentrifugation.

机构信息

Institute of Particle Technology (LFG), Friedrich-Alexander University Erlangen-Nürnberg (FAU), Cauerstr. 4, 91058, Erlangen, Germany.

出版信息

Small. 2015 Feb 18;11(7):814-25. doi: 10.1002/smll.201401940. Epub 2014 Sep 8.

Abstract

In this paper, a method to determine the lateral dimensions of 2D nanosheets directly in suspension by analytical ultracentrifugation (AUC) is shown. The basis for this study is a well-characterized and stable dispersion of graphene oxide (GO) monolayers in water. A methodology is developed to correlate the sedimentation coefficient distribution measured by AUC with the lateral size distribution of the 2D GO nanosheets obtained from atomic force microscopy (AFM). A very high accuracy can be obtained by virtue of counting several thousand sheets, thereby minimizing any coating effects or statistical uncertainties. The AFM statistics are further used to fit the lateral size distribution obtained from the AUC to determine the unknown hydrodynamic sheet thickness or density. It is found that AUC can derive nanosheet diameter distributions with a relative error of the mean sheet diameter of just 0.25% as compared to the AFM analysis for 90 mass% of the particles in the distribution. The standard deviation of the size-dependent error for the total distribution is found to be 3.25%. Based on these considerations, an expression is given to calculate the cut size of 2D nanosheets in preparative centrifugation experiments.

摘要

本文展示了一种通过分析超速离心(AUC)直接确定悬浮液中二维纳米片横向尺寸的方法。本研究的基础是在水中具有良好特征和稳定分散的氧化石墨烯(GO)单层。开发了一种将 AUC 测量的沉降系数分布与原子力显微镜(AFM)获得的二维 GO 纳米片的横向尺寸分布相关联的方法。通过计数数千个薄片,可以获得非常高的精度,从而最小化任何涂层效应或统计不确定性。AFM 统计数据进一步用于拟合 AUC 获得的横向尺寸分布,以确定未知的流体动力片厚度或密度。结果发现,与 AFM 分析相比,AUC 可以获得纳米片直径分布,对于分布中 90%的颗粒,平均片直径的相对误差仅为 0.25%。对于总分布的尺寸相关误差的标准偏差,发现为 3.25%。基于这些考虑,给出了一个表达式来计算制备离心实验中二维纳米片的切割尺寸。

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