Towards scanning nanostructure X-ray microscopy

Anton Kovyakh; Soham Banerjee; Chia-Hao Liu; Christopher J Wright; Yuguang C Li; Thomas E Mallouk; Robert Feidenhans'l; Simon J L Billinge

doi:10.1107/S1600576723005927

Towards scanning nanostructure X-ray microscopy

J Appl Crystallogr. 2023 Jul 28;56(Pt 4):1221-1228. doi: 10.1107/S1600576723005927. eCollection 2023 Aug 1.

Authors

Anton Kovyakh¹, Soham Banerjee², Chia-Hao Liu², Christopher J Wright², Yuguang C Li³, Thomas E Mallouk⁴, Robert Feidenhans'l^{1

5}, Simon J L Billinge^{2

6}

Affiliations

¹ Niels Bohr Institute, University of Copenhagen, Universitetsparken 5, DK-2100 Copenhagen, Denmark.
² Department of Applied Physics and Applied Mathematics, Columbia University, New York, NY 10027, USA.
³ Department of Chemistry, University at Buffalo, The State University of New York, Buffalo, New York, NY 14260, USA.
⁴ Department of Chemistry, The University of Pennsylvania, Philadelphia, PA, USA.
⁵ European XFEL, D-22869 Schenefeld, Germany.
⁶ Condensed Matter Physics and Materials Science Department, Brookhaven National Laboratory, Upton, NY 11973, USA.

Abstract

This article demonstrates spatial mapping of the local and nanoscale structure of thin film objects using spatially resolved pair distribution function (PDF) analysis of synchrotron X-ray diffraction data. This is exemplified in a lab-on-chip combinatorial array of sample spots containing catalytically interesting nanoparticles deposited from liquid precursors using an ink-jet liquid-handling system. A software implementation is presented of the whole protocol, including an approach for automated data acquisition and analysis using the atomic PDF method. The protocol software can handle semi-automated data reduction, normalization and modeling, with user-defined recipes generating a comprehensive collection of metadata and analysis results. By slicing the collection using included functions, it is possible to build images of different contrast features chosen by the user, giving insights into different aspects of the local structure.

Keywords: atomic pair distribution function; nanoparticles; spatial mapping; thin films.

Grants and funding

PDF methodology developments were funded by the US Department of Energy (DOE) Office of Science by Brookhaven National Laboratory under contract No. DE-SC0012704. AK acknowledges funding by the Innovation Fund Denmark (Green Chemistry for Advanced Materials 4107-00008B-GCAM). Sample preparation was supported by the Office of Basic Energy Sciences, Division of Chemical Sciences, Geosciences, and Energy Bioscience, Department of Energy under contract No. SC-0019781. X-ray PDF measurements were conducted on beamline 28-ID-2 of the National Synchrotron Light Source II, a US DOE Office of Science User Facility operated for the DOE Office of Science by Brookhaven National Laboratory under contract No. DE-SC0012704.