Single Atom Catalyst Detection

Detecting single atom catalysts via the difference pair distribution function method

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Challenges

  • Randomly dispersed single atom sites

    It is extremely challenging to detect the presence of single atom sites when they are dispersed randomly within a support material.

  • Distinguishing from nanoparticles

    Few methods can provide quantitative validation of local coordination environments or distinguish single atom sites from small nanoparticles.

Example: Pd single-atom catalysts in covalent organic frameworks

Pd single-atom catalyst complexes are installed into a covalent organic framework. Cyclopalladation red-shifts the absorption edge, enabling photocatalytic activity under NIR light (810 nm). Pd facilitates charge transfer and suppresses recombination for photocatalytic hydrogen peroxide production.

Pd single-atom catalyst in covalent organic framework

Rodríguez-Camargo et al. Nat. Synth (2025) 4, 710–719.

License: CC BY 4.0

Result

Transmission electron microscopy supports COF crystallinity while STEM–EDX elemental mapping analysis shows Pd & Cl uniformly distributed. XPS suggests Pd(II) ions in complexes.

Remaining questions

  • What is the nature of the binding configuration?

  • Are there any Pd nanoparticles formed?

X-ray diffraction and difference pair distribution function analysis of Pd single-atom catalysts

Rodríguez-Camargo et al. Nat. Synth (2025) 4, 710-719

License: CC BY 4.0

X-ray diffraction and difference pair distribution function analysis results:

  • Diffraction indicates contraction along the in-plane and stacking directions with complexes loaded.
  • Difference PDF analysis:
    • Verifies the presence and identity of Pd complexes formed
    • Proves that nanoparticle formation is insignificant
    • Indicates that conformational changes accompany complexation explaining the contracted structural state.

Signal sensitivity

  • Signal-to-noise of instrument and sample preparation are key factors to success
  • Requires synchrotron radiation. Sensitivity generally not achieved with laboratory diffractometers (even with 24h measurement).
  • Signal extraction is non-trivial and requires data processing by experienced personnel.
Difference PDF signal extraction for single atom catalyst detection

Kappel et al. Mater. Today Chem. (2025) 47, 102776

License: CC BY 4.0

Problems with standard analysis method

  • Localized complexes and single-atom catalysts are non-periodic and therefore do not diffract sharp signals.

  • The isolation of signals in reciprocal space is non-trivial.

Benefits of our method

  • PDF directly probes localized catalytic sites

    Provides more intuitive means for signal extraction and directly probes structuring of local sites.

  • High-sensitivity candidate model testing

    Allows for convenient testing of candidate models with high sensitivity, distinguishing single atoms from nanoparticles.

  • Synchrotron-grade signal quality

    Signal extraction is non-trivial and requires data processing by experienced personnel—our service handles this end-to-end.

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