New Prospects for Particle Characterization Using Analytical Centrifugation with Sector‐Shaped Centerpieces
New Prospects for Particle Characterization Using Analytical Centrifugation with Sector‐Shaped Centerpieces
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DOI：
10.1002/ppsc.202000108
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发表时间：
2020-06
影响因子：
2.7
通讯作者：
M. Uttinger;S. Boldt;S. Wawra;Tobias D. Freiwald;C. Damm;J. Walter;D. Lerche;W. Peukert
中科院分区：
文献类型：
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作者：
M. Uttinger;S. Boldt;S. Wawra;Tobias D. Freiwald;C. Damm;J. Walter;D. Lerche;W. Peukert
分析离心（AC）最近显示出巨大的潜力，用于准确测定粒度分布。成熟的LUMiSizer（R）采用全新设计进行定制，可实现更高的转子速度、更好的隔热性和测量单元组装。后者能够对扇形中心件中的纳米颗粒（NP）进行沉降分析。AC实验的测量窗口由Peclet（Pe）数评估。结果表明，在低Pe数（0.7 < Pe < 30），沉降，扩散可以准确地和同时分析从一个实验中的沉降边界。此外，沉降性能可以可靠地确定高达4000的Pe数。通过在升高的温度下测量聚苯乙烯颗粒来验证整个沉降分析的热特性。此外，通过确定SiO2 NPs在中间Pe数下的沉降性能，与分析超离心实验的结果非常一致，证明了该设置的性能。最后，第一次，通过AC的Au纳米粒子的核-壳性质的准确分析。通过结合在低Pe数下的沉降和扩散性质的分析，确定了稳定剂十六烷基三甲基溴化铵的壳厚度以及Au NPs的核直径分布。
Analytical centrifugation (AC) has recently shown great potential for the accurate determination of particle size distributions. The well‐established LUMiSizer(R) is customized by a new design allowing for higher rotor speeds, improved thermal insulation, and measurement cell assembly. The latter enables sedimentation analysis of nanoparticles (NPs) in sector‐shaped centerpieces. The measurement window of AC experiments is assessed by the Peclet (Pe) number. It is shown that at low Pe numbers (0.7 < Pe < 30), sedimentation, and diffusion can be accurately and simultaneously analyzed from the sedimentation boundaries within one experiment. Moreover, sedimentation properties can be reliably determined up to Pe numbers of 4000. The thermal characteristic throughout the sedimentation analysis is validated by measuring polystyrene particles at elevated temperatures. Moreover, the performance of the setup is demonstrated by determining the sedimentation properties of SiO2 NPs at intermediate Pe numbers in excellent agreement with results from analytical ultracentrifugation experiments. Finally, for the first time, an accurate analysis of the core–shell properties of Au NPs via AC is presented. By combining the analysis of sedimentation and diffusional properties at low Pe numbers, the shell thickness of the stabilizer cetyltrimethylammonium bromide alongside the core diameter distribution of the Au NPs is determined.