Time-resolved GISAXS and cryo-microscopy characterization of block copolymer membrane formation

Debora S. Marques, Rachel Mika Dorin, Ulrich B. Wiesner, Detlef Matthias Smilgies, Ali Reza Behzad, Ulla Vainio, Klaus-Viktor Peinemann, Suzana Pereira Nunes

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50 Scopus citations


Time-resolved grazing-incidence small-angle X-ray scattering (GISAXS) and cryo-microscopy were used for the first time to understand the pore evolution by copolymer assembly, leading to the formation of isoporous membranes with exceptional porosity and regularity. The formation of copolymer micelle strings in solution (in DMF/DOX/THF and DMF/DOX) was confirmed by cryo field emission scanning electron microscopy (cryo-FESEM) with a distance of 72 nm between centers of micelles placed in different strings. SAXS measurement of block copolymer solutions in DMF/DOX indicated hexagonal assembly with micelle-to-micelle distance of 84-87 nm for 14-20 wt% copolymer solutions. GISAXS in-plane peaks were detected, revealing order close to hexagonal. The d-spacing corresponding to the first peak in this case was 100-130 nm (lattice constant 115-150 nm) for 17 wt% copolymer solutions evaporating up to 100 s. Time-resolved cryo-FESEM showed the formation of incipient pores on the film surface after 4 s copolymer solution casting with distances between void centers of 125 nm. © 2014 Elsevier Ltd. All rights reserved.
Original languageEnglish (US)
Pages (from-to)1327-1332
Number of pages6
Issue number6
StatePublished - Mar 2014

Bibliographical note

KAUST Repository Item: Exported on 2020-10-01
Acknowledgements: We thank Yibei Gu, Cornell Materials Science, for assistance with the GISAXS measurements at CHESS. CHESS is supported by the National Science Foundation. The authors at Cornell were supported by the National Institutes of Health and General Medical Sciences via NSF award DMR-0936384. SAXS measurements were carried out at the light source DORIS III at DESY, a member of the Helmholtz Association (HGF). We further thank the National Science Foundation (DMR-1104773) for financial support.

ASJC Scopus subject areas

  • Organic Chemistry
  • Polymers and Plastics


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