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

Abstract

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 4more » °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.« less

Authors:
 [1];  [1];  [1];  [2];  [1]
+ Show Author Affiliations
  1. Univ. of Kentucky, Lexington, KY (United States)
  2. Argonne National Lab. (ANL), Argonne, IL (United States)
Publication Date:
Research Org.:
Argonne National Laboratory (ANL), Argonne, IL (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
OSTI Identifier:
1245149
Grant/Contract Number:  
AC02-06CH11357
Resource Type:
Accepted Manuscript
Journal Name:
Journal of Physical Chemistry. C
Additional Journal Information:
Journal Volume: 119; Journal Issue: 40; Journal ID: ISSN 1932-7447
Publisher:
American Chemical Society
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; 75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND SUPERFLUIDITY; self-assembly; thin films; mesophases; block copolymers; sol-gel

Citation Formats

Nagpure, Suraj, Das, Saikat, Garlapalli, Ravinder K., Strzalka, Joseph, and Rankin, Stephen E. In Situ GISAXS investigation of low-temperature aging in oriented surfactant-mesostructured titania thin films. United States: N. p., 2015. Web. doi:10.1021/acs.jpcc.5b06945.
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Nagpure, Suraj, Das, Saikat, Garlapalli, Ravinder K., Strzalka, Joseph, & Rankin, Stephen E. In Situ GISAXS investigation of low-temperature aging in oriented surfactant-mesostructured titania thin films. United States. https://doi.org/10.1021/acs.jpcc.5b06945
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Nagpure, Suraj, Das, Saikat, Garlapalli, Ravinder K., Strzalka, Joseph, and Rankin, Stephen E. Fri . "In Situ GISAXS investigation of low-temperature aging in oriented surfactant-mesostructured titania thin films". United States. https://doi.org/10.1021/acs.jpcc.5b06945. https://www.osti.gov/servlets/purl/1245149.
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@article{osti_1245149,
title = {In Situ GISAXS investigation of low-temperature aging in oriented surfactant-mesostructured titania thin films},
author = {Nagpure, Suraj and Das, Saikat and Garlapalli, Ravinder K. and Strzalka, Joseph and Rankin, Stephen E.},
abstractNote = {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.},
doi = {10.1021/acs.jpcc.5b06945},
journal = {Journal of Physical Chemistry. C},
number = 40,
volume = 119,
place = {United States},
year = {Fri Sep 11 00:00:00 EDT 2015},
month = {Fri Sep 11 00:00:00 EDT 2015}
}
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Time-Resolved Infrared Spectroscopy as an In Situ Tool To Study the Kinetics During Self-Assembly of Mesostructured Films
journal, June 2006

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Controlling the Processing of Mesoporous Titania Films by in Situ FTIR Spectroscopy: Getting Crystalline Micelles into the Mesopores
journal, June 2010

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In Situ Synchrotron Small-Angle X-ray Scattering/X-ray Diffraction Study of the Formation of SBA-15 Mesoporous Silica
journal, June 2004

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Phase transformation during cubic mesostructured silica film formation
journal, March 2002

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Synthesis of Surfactant-Templated Silica Films with Orthogonally Aligned Hexagonal Mesophase
journal, March 2005

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Humidity-controlled mesostructuration in CTAB-templated silica thin film processing. The existence of a modulable steady state
journal, November 2002

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Phase diagram for mesoporous CTAB–silica films prepared under dynamic conditions
journal, November 2002

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Sol–Gel Based Hydrophobic Antireflective Coatings on Organic Substrates: A Detailed Investigation of Ammonia Vapor Treatment (AVT)
journal, February 2014

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A comprehensive study of the reaction parameters involved in the synthesis of Silica thin films with well-ordered uni-directional mesopores
journal, July 2013

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Control over in-channel mesostructure orientation through AAM surface modification
journal, January 2013

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Mesoporous Structures Confined in Anodic Alumina Membranes
journal, April 2011

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Perspective on the Influence of Interactions Between Hard and Soft Templates and Precursors on Morphology of Hierarchically Structured Porous Materials
journal, September 2013

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Mesoporous Titania Thin Film with Highly Ordered and Fully Accessible Vertical Pores and Crystalline Walls
journal, May 2008

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Synthesis of mesoporous titania thin films with vertical pore channels and thick and crystalline walls
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Scherrer grain-size analysis adapted to grazing-incidence scattering with area detectors
journal, October 2009

In Situ FTIR Investigation of the Kinetics of Silica Polycondensation in Surfactant Templated, Mesostructured Thin Films
journal, August 2014

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Highly Oriented and Ordered Arrays from Block Copolymers via Solvent Evaporation
journal, February 2004

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Highly Ordered Self-Assembled Mesostructured Hafnia Thin Films:  An Example of Rewritable Mesostructure
journal, September 2006

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Rheological Study of Order-to-Disorder Transitions and Phase Behavior of Block Copolymer–Surfactant Complexes Containing Hydrogen-Bonded Small Molecule Additives
journal, November 2014

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Block Copolymer Self Assembly during Rapid Solvent Evaporation: Insights into Cylinder Growth and Stability
journal, December 2013

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Cylinder Orientation Mechanism in Block Copolymer Thin Films Upon Solvent Evaporation
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