In Situ GISAXS investigation of low-temperature aging in oriented surfactant-mesostructured titania thin films

Nagpure, Suraj; Das, Saikat; Garlapalli, Ravinder K.; Strzalka, Joseph; Rankin, Stephen E.

doi:10.1021/acs.jpcc.5b06945

In Situ GISAXS investigation of low-temperature aging in oriented surfactant-mesostructured titania thin films

Journal Article · Fri Sep 11 00:00:00 EDT 2015 · Journal of Physical Chemistry. C

DOI:https://doi.org/10.1021/acs.jpcc.5b06945· OSTI ID:1245149

Nagpure, Suraj ^[1]; Das, Saikat ^[1]; Garlapalli, Ravinder K. ^[1]; Strzalka, Joseph ^[2]; Rankin, Stephen E. ^[1]

Univ. of Kentucky, Lexington, KY (United States)
Argonne National Lab. (ANL), Argonne, IL (United States)

In this study, the mechanism of forming orthogonally oriented hexagonal close packed (o-HCP) mesostructures during aging of surfactant-templated titania thin films is elucidated using in situ grazing incidence small-angle x-ray scattering (GISAXS) in a controlled-environment chamber. To promote orthogonal orientation, glass slides are modified with crosslinked Pluronic P123, to provide surfaces chemically neutral towards both blocks of mesophase template P123. At 4 °C and 80% RH, the o-HCP mesophase emerges in thin (~60 nm) films by a direct disorder-to-order transition, with no intermediate ordered mesophase. The Pluronic/titania o-HCP GISAXS intensity emerges only after ~10-12 minutes, much slower than previously reported for smallmolecule surfactants. The Avrami model applied to the data suggests 2D growth with nucleation at the start of the process with a half-life of 39.7 minutes for the aging time just after the induction period of 7 minutes followed by a period consistent with 1D growth kinetics. Surprisingly, films that are thicker (~250 nm) or cast on unmodified slides form o-HCP mesophase domains, but by a different mechanism (2D growth with continuous nucleation) with faster and less complete orthogonal alignment. Thus, the o-HCP mesophase is favored not only 2 by modifying the substrate, but also by aging at 4 °C, which is below the lower consolute temperature (LCST) of the poly(propylene oxide) block of P123. Consistent with this, in situ GISAXS shows that films aged at room temperature (above the LCST of the PPO block) have randomly oriented HCP mesostructure.

View Accepted Manuscript (DOE)

Research Organization:: Argonne National Lab. (ANL), Argonne, IL (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)

Grant/Contract Number:: AC02-06CH11357

OSTI ID:: 1245149

Journal Information:: Journal of Physical Chemistry. C, Journal Name: Journal of Physical Chemistry. C Journal Issue: 40 Vol. 119; ISSN 1932-7447

Publisher:: American Chemical SocietyCopyright Statement

Country of Publication:: United States

Language:: English

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