Improved small-angle x-ray scattering of nanoparticle self-assembly using a cell with a flat liquid surface

  • Jiayang Hu
  • Evan W. C. Spotte-Smith
  • Brady Pan
  • Irving P. HermanEmail author
Research Paper


One important way of forming nanostructures entails the assembly of nanoparticle (NP) monolayers at a liquid surface. Probing this assembly of 11.8-nm-diameter iron oxide NPs by small-angle x-ray scattering (SAXS) is studied using cells with walls at angles designed to significantly reduce the size of the meniscus. This enables the collection of much larger signals in the SAXS images of ordered arrays of NPs at liquid/gas interfaces, as is needed for kinetics studies and x-ray exposure minimization, along with the observation of extremely high degrees of order. Meniscus flattening and improved signal collection are demonstrated for the assembly of ordered arrays of iron oxide NP monolayers at a diethylene glycol surface.


Nanoparticle self-assembly SAXS GISAXS Liquid surface Meniscus Nanoparticle monolayers 



This research used the CMS 11-BM beamline and other resources of the National Synchrotron Light Source II (NSLS-II) and resources of the Center for Functional Nanomaterials, which are U.S. Department of Energy (DOE) Office of Science user facilities operated for the DOE Office of Science by Brookhaven National Laboratory (BNL) under Contract No. DE-SC0012704. We thank Drs. Masafumi Fukuto, Ruipeng Li, and Kevin Yager at the BNL NSLS-II CMS 11-BM beamline for their assistance, and Dr. Oleg Gang, Jason Cardarelli (IGERT program of the National Science Foundation (DGE-1069240)) and Roy Garcia.

Funding information

Support was provided by the National Science Foundation (CBET-1603043).

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.


  1. Adamson AW (1967) Physical chemistry of surfaces. Wiley-Interscience, New YorkGoogle Scholar
  2. Boal AK, Ilhan F, DeRouchey JE, Thurn-Albrecht T, Russell TP, Rotello VM (2000) Self-assembly of nanoparticles into structured spherical and network aggregates. Nature 404:746–748CrossRefGoogle Scholar
  3. Böker A, He J, Emrick T, Russell TP (2007) Self-assembly of nanoparticles at interfaces. Soft Matter 3:1231–1248CrossRefGoogle Scholar
  4. Brennen CE (2006) An internet book on fluid dynamics. Accessed 12 April 2018
  5. Grzelczak M, Vermant J, Furst EM, Liz-Marzan LM (2010) Directed self-assembly of nanoparticles. ACS Nano 4:3591–3605CrossRefGoogle Scholar
  6. Henke BL, Gullikson EM, Davis JC (1993) Filter transmission. Lawrence Berkeley national laboratory. Accessed 30 Mar 2018
  7. Hyeon T, Lee SS, Park J, Chung Y, Na HB (2001) Synthesis of highly crystalline and monodisperse maghemite nanocrystallites without a size-selection process. J Am Chem Soc 123:12798–12801CrossRefGoogle Scholar
  8. Josten E, Wetterskog E, Glavic A, Boesecke P, Feoktystov A, Brauweiler-Reuters E, Rücker U, Salazar-Alvarez G, Brückel T, Bergström L (2017) Superlattice growth and rearrangement during evaporation-induced nanoparticle self-assembly. Sci Rep 7:2802CrossRefGoogle Scholar
  9. Lu C, Akey AJ, Herman IP (2012) Synchrotron x-ray modification of nanoparticle superlattice formation. Appl Phys Lett 101:133109CrossRefGoogle Scholar
  10. Luo G, Malkova S, Yoon J, Schultz DG, Lin B, Meron M, Benjamin I, Vanýsek P, Schlossman ML (2006) Ion distributions near a liquid-liquid interface. Science 311:216–218CrossRefGoogle Scholar
  11. Narayanan S, Wang J, Lin XM (2004) Dynamical self-assembly of nanocrystal superlattices during colloidal droplet evaporation by in situ small angle x-ray scattering. Phys Rev Lett 93:135503CrossRefGoogle Scholar
  12. Pershan PS, Schlossman M (2012) Liquid surfaces and interfaces: synchrotron x-ray methods. Cambridge University Press, New YorkCrossRefGoogle Scholar
  13. Weidman MC, Smilgies DM, Tisdale WA (2016) Kinetics of the self-assembly of nanocrystal superlattices measured by real-time in situ x-ray scattering. Nat Mater 15:775–781CrossRefGoogle Scholar
  14. Williamson GK, Hall WH (1953) X-ray line broadening from filed aluminium and wolfram. Acta Metall 1:22–31CrossRefGoogle Scholar
  15. Zhang Z, Mitrinovic DM, Williams SM, Huang Z, Schlossman ML (1999) X-ray scattering from monolayers of F(CF2)10(CH2)2OH at the water–(hexane solution) and water–vapor interfaces. J Chem Phys 110:7421–7432CrossRefGoogle Scholar
  16. Zhang D, Lu C, Hu J, Lee SW, Ye F, Herman IP (2015) Small angle x-ray scattering of iron oxide nanoparticle monolayers formed on a liquid surface. J Phys Chem C 119:10727–10733CrossRefGoogle Scholar
  17. Zhang D, Hu J, Kennedy KM, Herman IP (2016) Forming nanoparticle monolayers at liquid–air interfaces by using miscible liquids. Langmuir 32:8467–8472CrossRefGoogle Scholar

Copyright information

© Springer Nature B.V. 2019

Authors and Affiliations

  • Jiayang Hu
    • 1
  • Evan W. C. Spotte-Smith
    • 1
  • Brady Pan
    • 1
  • Irving P. Herman
    • 1
    Email author
  1. 1.Department of Applied Physics and Applied MathematicsColumbia UniversityNew YorkUSA

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