Faculty of Applied Sciences, Delft University of Technology, Mekelweg 15, 2629 JB Delft, The Netherlands.
Department of Physics and Astronomy, The University of Sheffield, Sheffield, S3 7RH, UK and Department of Mechanical Engineering, The University of Sheffield, Sheffield, S1 3DJ, UK.
Soft Matter. 2016 May 25;12(21):4709-14. doi: 10.1039/c5sm02772a.
Stöber silica particles are used in a diverse range of applications. Despite their widespread industrial and scientific uses, information on the internal structure of the particles is non-trivial to obtain and is not often reported. In this work we have used spin-echo small angle neutron scattering (SESANS) in conjunction with ultra small angle X-ray scattering (USAXS) and pycnometry to study an aqueous dispersion of Stöber particles. Our results are in agreement with models which propose that Stöber particles have a porous core, with a significant fraction of the pores inaccessible to solvent. For samples prepared from the same master sample in a range of H2O : D2O ratio solutions we were able to model the SESANS results for the solution series assuming monodisperse, smooth surfaced spheres of radius 83 nm with an internal open pore volume fraction of 32% and a closed pore fraction of 10%. Our results are consistent with USAXS measurements. The protocol developed and discussed here shows that the SESANS technique is a powerful way to investigate particles much larger than those studied using conventional small angle scattering methods.
Stöber 硅石颗粒在多种应用中得到了广泛应用。尽管它们在工业和科学上有着广泛的用途,但关于颗粒内部结构的信息很难获得,并且通常也不会被报道。在这项工作中,我们使用了自旋回波小角中子散射(SESANS)与超小角 X 射线散射(USAXS)和比重瓶法结合来研究 Stöber 颗粒的水基分散体。我们的结果与模型一致,该模型提出 Stöber 颗粒具有多孔核心,其中很大一部分孔对溶剂不可用。对于从同一母样在一系列 H2O:D2O 比溶液中制备的样品,我们能够模拟 SESANS 结果,对于溶液系列,我们假设为半径为 83nm 的单分散、表面光滑的球体,具有 32%的内部开放孔体积分数和 10%的封闭孔分数。我们的结果与 USAXS 测量结果一致。本文中所开发和讨论的方案表明,SESANS 技术是一种强大的方法,可以研究比使用传统小角散射方法研究的颗粒大得多的颗粒。