Issue 5, 2020

Interaction of nanoparticle properties and X-ray analytical techniques

Abstract

In this work, Pt–Ti core–shell nanoparticles (NP) of 2 nm to 3 nm size and 30 000 u ± 1500 u as specified single particle mass, deposited on flat silicon substrates by means of a mass-selected cluster beam source, were used for the investigation of the modification of the X-ray Standing Wave (XSW) field intensity with increasing NP surface coverage. The focus of the investigation is on the determination of the range of validity of the undisturbed flat surface approach of the XSW intensity in dependence of the actual coverage rate of the surface. Therefore, the nanoparticles were characterized using reference-free grazing incidence X-ray fluorescence analysis (GIXRF) employing radiometrically calibrated instrumentation. In addition, near-edge X-ray absorption fine structure (NEXAFS) measurements were performed to investigate the binding state of titanium in the core–shell nanoparticles which was found to be amorphous TiO2. The combination of GIXRF measurements and of the calculated XSW field intensities allows for quantification of the core–shell nanoparticle surface coverage. For six different samples, the peak surface coverage could be determined to vary from 7% to 130% of a complete monolayer-equivalent coverage. A result of the current investigation is that core–shell nanoparticles modify the intensity distribution of the XSW field with increasing surface coverage. This experimental result is in line with calculated XSW field intensity distributions at different surface coverages using an effective density approach.

Graphical abstract: Interaction of nanoparticle properties and X-ray analytical techniques

Article information

Article type
Paper
Submitted
10 Feb 2020
Accepted
16 Apr 2020
First published
17 Apr 2020

J. Anal. At. Spectrom., 2020,35, 1022-1033

Interaction of nanoparticle properties and X-ray analytical techniques

R. Unterumsberger, P. Hönicke, Y. Kayser, B. Pollakowski-Herrmann, S. Gholhaki, Q. Guo, R. E. Palmer and B. Beckhoff, J. Anal. At. Spectrom., 2020, 35, 1022 DOI: 10.1039/D0JA00049C

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