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Peer-reviewedCC BY 4.0The Journal of Physical Chemistry Letters

Combining Small-Angle X‑ray Scattering with Photoelectron Spectroscopy to Increase the Accuracy of Silica Shell Thickness Measurements on Inorganic Nanocrystals

  • Sarah-Luise Abram1
  • Anna Matiushkina1,2
  • David Cant3
  • Nicholas Engel4
  • Robin Schürmann4
  • Jörg Radnik5
  • Elina Andresen1
  • Carsten Prinz1
  • Christian Gollwitzer4
  • Alexander Gordon Shard3
  • Ute Resch-Genger1
5 affiliations
  1. 1Federal Institute for Material Research and Testing (BAM), Division 1.2 Biophotonics, Richard-Willstaetter Str. 11, 12489 Berlin, Germany
  2. 2Free University Berlin, Department of Biology, Chemistry, and Pharmacy, Arnimallee 22, 14195 Berlin, Germany
  3. 3National Physical Laboratory (NPL), Hampton Road, TW11 0LW Teddington, U.K.
  4. 4Physikalisch-Technische Bundesanstalt (PTB), Abbestr. 2-12, 10587 Berlin, Germany
  5. 5Federal Institute for Material Research and Testing (BAM), Division 6.1 Surface Analysis and Interfacial Chemistry, Unter den Eichen 44-46, 12203 Berlin, Germany
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Abstract

X-ray photoelectron spectroscopy (XPS) is widely used to measure the surface chemistry of nanomaterials, yet it can also provide structural information. The thickness of surface passivation shells can be determined with XPS and hard X-ray photoelectron spectroscopy (HAXPES), but accuracy depends upon knowledge of the density of core and shell materials. This property is typically sourced from literature data on bulk materials, which may not be correct for nanomaterials. We representatively refine shell thickness XPS and HAXPES measurements for silica shells on iron oxide and lanthanide nanoparticles, exploiting electron densities experimentally derived by small-angle X-ray scattering (SAXS) measurements of the core–shell nanoparticles in liquid mixtures with different densities. This results in improved agreement between XPS results and transmission electron microscopy (TEM) and SAXS shell thickness measurements. Thereby, HAXPES provided results in closer agreement with TEM and SAXS than XPS, likely due to a lower sensitivity to coating thickness variations.

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Cite

BibTeXRIS
BibTeX
@article{abram2026combining,
  title = {{Combining Small-Angle X‑ray Scattering with Photoelectron Spectroscopy to Increase the Accuracy of Silica Shell Thickness Measurements on Inorganic Nanocrystals}},
  author = {Sarah-Luise Abram and Anna Matiushkina and David Cant and Nicholas Engel and Robin Schürmann and Jörg Radnik and Elina Andresen and Carsten Prinz and Christian Gollwitzer and Alexander Gordon Shard and Ute Resch-Genger},
  journal = {The Journal of Physical Chemistry Letters},
  year = {2026},
  month = sep,
  doi = {10.1021/acs.jpclett.6c02495},
  url = {https://doi.org/10.1021/acs.jpclett.6c02495},
  note = {CC BY 4.0},
}
RIS
TY  - JOUR
TI  - Combining Small-Angle X‑ray Scattering with Photoelectron Spectroscopy to Increase the Accuracy of Silica Shell Thickness Measurements on Inorganic Nanocrystals
AU  - Sarah-Luise Abram
AU  - Anna Matiushkina
AU  - David Cant
AU  - Nicholas Engel
AU  - Robin Schürmann
AU  - Jörg Radnik
AU  - Elina Andresen
AU  - Carsten Prinz
AU  - Christian Gollwitzer
AU  - Alexander Gordon Shard
AU  - Ute Resch-Genger
PY  - 2026
DA  - 2026/09/02
JO  - The Journal of Physical Chemistry Letters
DO  - 10.1021/acs.jpclett.6c02495
UR  - https://doi.org/10.1021/acs.jpclett.6c02495
AB  - X-ray photoelectron spectroscopy (XPS) is widely used to measure the surface chemistry of nanomaterials, yet it can also provide structural information. The thickness of surface passivation shells can be determined with XPS and hard X-ray photoelectron spectroscopy (HAXPES), but accuracy depends upon knowledge of the density of core and shell materials. This property is typically sourced from literature data on bulk materials, which may not be correct for nanomaterials. We representatively refine shell thickness XPS and HAXPES measurements for silica shells on iron oxide and lanthanide nanoparticles, exploiting electron densities experimentally derived by small-angle X-ray scattering (SAXS) measurements of the core–shell nanoparticles in liquid mixtures with different densities. This results in improved agreement between XPS results and transmission electron microscopy (TEM) and SAXS shell thickness measurements. Thereby, HAXPES provided results in closer agreement with TEM and SAXS than XPS, likely due to a lower sensitivity to coating thickness variations.
SN  - 1948-7185
ER  -