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Updated: Sep 13, 2025

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Modulation excitation pair distribution function experiments in catalysis to increase phase sensitivity.

Fabio Manzoni1, Ansgar Meise2, Mirijam Zobel1

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Summary
This summary is machine-generated.

Modulation excitation pair distribution function (ME-PDF) analysis reveals hidden structural changes in heterogeneous catalysts. This technique enhances signal-to-noise, identifying metal-support interactions and dynamic surface oxidation in nickel catalysts.

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Area of Science:

  • Materials Science
  • Catalysis
  • Physical Chemistry

Background:

  • Heterogeneous catalysts undergo structural changes during operation.
  • Modulation excitation (ME) experiments with phase-sensitive detection (PSD) are powerful for studying dynamic processes.
  • Previous PSD applications focused on spectroscopy, not structural analysis.

Purpose of the Study:

  • To introduce the first application of phase-sensitive detection (PSD) of modulation excitation (ME) experiments to pair distribution function (PDF) analysis.
  • To investigate structural changes in alumina-supported nickel (Ni@alumina) catalysts under reaction conditions.
  • To enhance the detection of subtle structural changes in catalytic materials.

Main Methods:

  • In situ X-ray total scattering studies.
  • Modulation excitation (ME) experiments.
  • Phase-sensitive detection (PSD) applied to pair distribution function (PDF) analysis, termed ME-PDF.
  • Analysis of nickel catalysts under methanation and hydrogen dropout conditions.

Main Results:

  • ME-PDF analysis significantly improves the signal-to-noise ratio in phase-resolved PDF data.
  • Detected otherwise hidden structural changes in Ni@alumina catalysts.
  • Identified a metal-support interaction between Ni nanoparticles and the γ-Al2O3 support for catalysts prepared via deposition-precipitation.
  • Observed dynamic surface oxidation of Ni nanoparticles in an industrial catalyst during unstable hydrogen supply.

Conclusions:

  • ME-PDF is a powerful new tool for in situ structural analysis of heterogeneous catalysts.
  • The preparation method influences metal-support interactions in Ni@alumina catalysts.
  • Catalyst stability under varying conditions is crucial and can be monitored using ME-PDF.