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A Continuous-flow Photocatalytic Reactor for the Precisely Controlled Deposition of Metallic Nanoparticles

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Spectro-Microscopy of Individual Pt-Rh Core-Shell Nanoparticles during Competing Oxidation and Alloying.

Jagrati Dwivedi¹, Lydia J Bachmann^1,2, Arno Jeromin¹

¹Centre for X-ray and Nano Science (CXNS), Deutsches Elektronen-Synchrotron (DESY), Hamburg 22603, Germany.

|July 30, 2025

Summary

Rhodium (Rh) behavior on platinum (Pt) core-shell nanoparticles was investigated. Rh oxidized more on Pt cores than on supports, alloying with Pt and sintering on the support at high temperatures.

Keywords:

AFM Pt–Rh core–shell nanoparticles SEM−EBSD XPEEM correlative approach facet-dependent oxidation–reduction in situ spectro-microscopy

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Preparation of Nanoparticles for ToF-SIMS and XPS Analysis

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Preparation of Nanoparticles for ToF-SIMS and XPS Analysis

Preparation of Nanoparticles for ToF-SIMS and XPS Analysis

Published on: September 13, 2020

Area of Science:

Surface Science
Catalysis
Materials Science

Background:

Understanding nanoparticle surface chemistry is crucial for catalyst design.
The behavior of bimetallic nanoparticles under reaction conditions is complex.
Platinum-Rhodium (Pt-Rh) nanoparticles are important in catalysis.

Purpose of the Study:

To investigate the surface chemical composition and behavior of supported single Pt-Rh core-shell nanoparticles.
To understand Rh behavior in oxidizing and reducing gas environments.
To distinguish Rh oxidation-reduction, dewetting-sintering, and alloying-segregation.

Main Methods:

Combined *in situ* X-ray photoemission electron microscopy (XPEEM) with *ex situ* scanning electron microscopy (SEM), atomic force microscopy (AFM), and scanning Auger microscopy (SAM).
Utilized high spatial resolution spectro-microscopy.
Employed electron backscatter diffraction (EBSD) for nanoparticle facet analysis.

Main Results:

A >20% higher Rh 3d$_{5/2}$ oxide to metal photoemission intensity ratio was observed for Rh on Pt cores compared to Rh on strontium titanate (STO) support.
At elevated temperatures, Rh diffused into the Pt particle, alloying with the Pt surface.
Rh/RhO_x nanoparticles on the STO support sintered under oxidizing conditions.
Rh oxidation was most advanced on small nanoparticles with low coordination top facets.

Conclusions:

Alloying of Rh into the Pt surface competes with Rh oxidation.
Rh nanoparticles on STO support undergo sintering under oxidizing conditions.
Nanoparticle facet structure influences the extent of Rh oxidation, highlighting the utility of correlative microscopy.