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采用多波长分析超速离心法测定胶体二氧化硅上银斑的产率、质量和结构。

Determination of the yield, mass and structure of silver patches on colloidal silica using multiwavelength analytical ultracentrifugation.

机构信息

Institute of Particle Technology, Friedrich-Alexander University Erlangen-Nürnberg, Cauerstrasse 4, Erlangen 91058, Germany.

Applied Mathematics 2, Friedrich-Alexander University Erlangen-Nürnberg, Cauerstrasse 11, Erlangen 91058, Germany.

出版信息

J Colloid Interface Sci. 2022 Feb;607(Pt 1):698-710. doi: 10.1016/j.jcis.2021.08.161. Epub 2021 Aug 27.

Abstract

Anisotropic nanoparticles offer considerable promise for applications but also present significant challenges in terms of their characterization. Recent developments in the electroless deposition of silver patches directly onto colloidal silica particles have opened up a simple and scalable synthesis method for patchy particles with tunable optical properties. Due to the reliance on patch nucleation and growth, however, the resulting coatings are distributed in coverage and thickness and some core particles remain uncoated. To support process optimization, new methods are required to rapidly determine patch yield, thickness and coverage. Here we present a novel approach based on multiwavelength analytical ultracentrifugation (MWL-AUC) which permits simultaneous hydrodynamic and spectroscopic characterization. The patchy particle colloids are produced in a continuous flow mixing process that makes use of a KM-type micromixer. By varying the process flow rate or metal precursor concentration we show how the silver to silica mass ratio distribution derived from the AUC-measured sedimentation coefficient distribution can be influenced. Moreover, through reasoned assumptions we arrive at an estimation of the patch yield that is close to that determined by arduous analysis of scanning electron microscopy (SEM) images. Finally, combining MWL-AUC, electrodynamic simulations and SEM image analysis we establish a procedure to estimate the patch thickness and coverage.

摘要

各向异性纳米粒子在应用方面具有很大的潜力,但在其特性表征方面也存在重大挑战。最近,通过无电沉积方法将银补丁直接沉积在胶体硅粒子上的技术发展,为具有可调光学性质的补丁粒子提供了一种简单且可扩展的合成方法。然而,由于依赖于补丁成核和生长,因此得到的涂层在覆盖率和厚度上分布不均,一些核心粒子仍然未被覆盖。为了支持工艺优化,需要新的方法来快速确定补丁的产率、厚度和覆盖率。在这里,我们提出了一种基于多波长分析超速离心(MWL-AUC)的新方法,该方法允许同时进行流体动力学和光谱学表征。在连续流混合过程中制备了具有补丁的胶体粒子,该过程利用了 KM 型微混合器。通过改变过程流速或金属前体浓度,我们展示了如何影响 AUC 测量的沉降系数分布中衍生的银与硅的质量比分布。此外,通过合理的假设,我们得到了一个接近通过扫描电子显微镜(SEM)图像进行艰苦分析确定的补丁产率的估计值。最后,结合 MWL-AUC、电动模拟和 SEM 图像分析,我们建立了一种估计补丁厚度和覆盖率的方法。

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