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Solvent vapor annealing of block copolymer thin films: removal of processing history

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Abstract

The ordering processes of PS-b-P2VP block copolymer thin films with different processing histories were studied during solvent vapor annealing by in situ grazing incidence small-angle X-ray scattering (GISAXS). We compared cylinder-forming PS-b-P2VP thin films with 34 kg/mol molecular weight that were prepared in three different ways: spin coating, spin coating and subsequent solvent vapor annealing where the solvent vapor was removed instantaneously, and spin coating and subsequent solvent vapor annealing where the solvent vapor was removed slowly. Block copolymer thin films retained the morphology resulting from the different “processing histories” at smaller swelling ratios. This processing history was erased when the samples reached a higher swelling ratio (~1.4). After the solvent was slowly removed from the swollen film, the surface morphology was characterized by ex situ AFM. All samples showed the same morphology after solvent annealing regardless of the initial morphology, indicating the morphology of solvent annealed samples is determined by the polymer concentration in the swollen film and the solvent vapor removal rate, but not the processing history.

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Acknowledgments

This work was supported by the U.S. Department of Energy BES under contract BES-DE-FG02-96ER45612. X.G. acknowledges ALS Doctoral Fellowship program for providing partial financial support. I.G. acknowledges the support by the ALS Postdoctoral Fellowship program. A.H. was supported by a DOE Early Career Research Program grant. GISAXS measurements were performed at Beamline 7.3.3 at the Advanced Light Source, Lawrence Berkeley National Laboratory, which is supported by the Office of Science, Office of Basic Energy Sciences, of the U.S. Department of Energy under contract No. DE-AC02-05ch11231.

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Authors and Affiliations

  1. Polymer Science and Engineering Department, University of Massachusetts at Amherst, 120 Governors Drive, Amherst, MA, 01003, USA

    Xiaodan Gu, Ilja Gunkel & Thomas P. Russell

  2. Advanced Light Source, Lawrence Berkeley National Laboratory, 1 Cyclotron Road, Berkeley, CA, 94720, USA

    Ilja Gunkel & Alexander Hexemer

  3. Materials Science Division, Lawrence Berkeley National Laboratory, 1 Cyclotron Road, Berkeley, CA, 94720, USA

    Ilja Gunkel & Thomas P. Russell

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  1. Xiaodan Gu
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  2. Ilja Gunkel
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  3. Alexander Hexemer
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  4. Thomas P. Russell
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Correspondence to Thomas P. Russell.

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Gu, X., Gunkel, I., Hexemer, A. et al. Solvent vapor annealing of block copolymer thin films: removal of processing history. Colloid Polym Sci 292, 1795–1802 (2014). https://doi.org/10.1007/s00396-014-3286-9

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  • DOI: https://doi.org/10.1007/s00396-014-3286-9

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