X-ray nanoscale profiling of layer-by-layer assembled metal/organophosphonate films

Joseph A. Libera, Richard W. Gurney, Son Binh T. Nguyen, Joseph T. Hupp, Chian Liu, Ray Conley, Michael J. Bedzyk*

*Corresponding author for this work

Research output: Contribution to journalArticlepeer-review

21 Scopus citations


The nanoscale structure of multilayer metal/phosphonate thin films prepared via a layer-by-layer assembly process was studied using specular X-ray reflectivity (XRR), X-ray fluorescence (XRF), and long-period X-ray standing wave (XSW) analysis. After the SiO 2 X-ray mirror surfaces were functionalized with a monolayer film terminated with phosphonate groups, the organic multilayer films were assembled by alternating immersions in (a) aqueous solutions containing Zr 4+, Hf 4+, or Y 3+ cations and then (b) organic solvent solutions of PO 3-R-PO 3, where R was a porphyrin or porphyrin-square spacer molecule. The different heavy metal cations provided X-ray fluorescence marker layers at different heights within the different multilayer assemblies. The XSW measurements used a 22 nm period Si/Mo multilayer mirror. The long-period XSW generated by the zeroth-order (total external reflection) through fourth-order Bragg diffraction conditions made it possible to examine the Fourier transforms of the fluorescent atom distributions over a much larger q z range in reciprocal space than previously achieved.

Original languageEnglish (US)
Pages (from-to)8022-8029
Number of pages8
Issue number19
StatePublished - Sep 14 2004

ASJC Scopus subject areas

  • Materials Science(all)
  • Condensed Matter Physics
  • Surfaces and Interfaces
  • Spectroscopy
  • Electrochemistry


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