In Situ Tracking of Composition and Morphology of a Diblock Copolymer Film with GISAXS during Exchange of Solvent Vapors at Elevated Temperatures

Anatoly V. Berezkin, Florian Jung, Dorthe Posselt, Detlef-M. Smilgies, Christine M. Papadakis

Publikation: Bidrag til tidsskriftTidsskriftartikelForskningpeer review

Resumé

Solvothermal vapor annealing at elevated temperature is applied to a thin film from a cylinder‐forming polystyrene‐block‐poly(dimethyl siloxane) (PS‐b‐PDMS) diblock copolymer. At this, the film is swollen in the vapor of n‐heptane (highly selective for PDMS). This vapor is stepwise replaced by the vapor of toluene (weakly selective for PS). The morphologies are investigated using in situ, real‐time grazing‐incidence small‐angle X‐ray scattering (GISAXS). The initial cylindrical morphology is transformed into, among others, the lamellar one. This novel type of experiments allows probing a trajectory in the state diagram of the PS‐b‐PDMS/n‐heptane/toluene mixture. To corroborate the morphologies, they are generated by molecular simulations, and the 2D GISAXS maps are calculated using the distorted‐wave Born approximation. To relate the morphologies to the solvent distribution in the two types of nanodomains, the latter is estimated from the intensities of the Bragg reflections in the 2D GISAXS maps along with the swelling ratio of the film. Comparison with the results from a similar experiment carried out at room temperature results in the same sequence of morphologies; however, at elevated temperature, more well‐ordered structures are obtained. This new approach proves to be efficient to achieve a block copolymer thin film having a desired morphology and orientation.
OriginalsprogEngelsk
Artikelnummer1706226
TidsskriftAdvanced Functional Materials
Vol/bind28
Udgave nummer19
Antal sider15
ISSN1616-301X
DOI
StatusUdgivet - 2018

Citer dette

@article{73bc2f4654334911833b140cbde95371,
title = "In Situ Tracking of Composition and Morphology of a Diblock Copolymer Film with GISAXS during Exchange of Solvent Vapors at Elevated Temperatures",
abstract = "Solvothermal vapor annealing at elevated temperature is applied to a thin film from a cylinder‐forming polystyrene‐block‐poly(dimethyl siloxane) (PS‐b‐PDMS) diblock copolymer. At this, the film is swollen in the vapor of n‐heptane (highly selective for PDMS). This vapor is stepwise replaced by the vapor of toluene (weakly selective for PS). The morphologies are investigated using in situ, real‐time grazing‐incidence small‐angle X‐ray scattering (GISAXS). The initial cylindrical morphology is transformed into, among others, the lamellar one. This novel type of experiments allows probing a trajectory in the state diagram of the PS‐b‐PDMS/n‐heptane/toluene mixture. To corroborate the morphologies, they are generated by molecular simulations, and the 2D GISAXS maps are calculated using the distorted‐wave Born approximation. To relate the morphologies to the solvent distribution in the two types of nanodomains, the latter is estimated from the intensities of the Bragg reflections in the 2D GISAXS maps along with the swelling ratio of the film. Comparison with the results from a similar experiment carried out at room temperature results in the same sequence of morphologies; however, at elevated temperature, more well‐ordered structures are obtained. This new approach proves to be efficient to achieve a block copolymer thin film having a desired morphology and orientation.",
author = "Berezkin, {Anatoly V.} and Florian Jung and Dorthe Posselt and Detlef-M. Smilgies and Papadakis, {Christine M.}",
year = "2018",
doi = "10.1002/adfm.201706226",
language = "English",
volume = "28",
journal = "Advanced Functional Materials",
issn = "1616-301X",
publisher = "Wiley - V C H Verlag GmbH & Co. KGaA",
number = "19",

}

In Situ Tracking of Composition and Morphology of a Diblock Copolymer Film with GISAXS during Exchange of Solvent Vapors at Elevated Temperatures. / Berezkin, Anatoly V.; Jung, Florian; Posselt, Dorthe; Smilgies, Detlef-M.; Papadakis, Christine M.

I: Advanced Functional Materials, Bind 28, Nr. 19, 1706226, 2018.

Publikation: Bidrag til tidsskriftTidsskriftartikelForskningpeer review

TY - JOUR

T1 - In Situ Tracking of Composition and Morphology of a Diblock Copolymer Film with GISAXS during Exchange of Solvent Vapors at Elevated Temperatures

AU - Berezkin, Anatoly V.

AU - Jung, Florian

AU - Posselt, Dorthe

AU - Smilgies, Detlef-M.

AU - Papadakis, Christine M.

PY - 2018

Y1 - 2018

N2 - Solvothermal vapor annealing at elevated temperature is applied to a thin film from a cylinder‐forming polystyrene‐block‐poly(dimethyl siloxane) (PS‐b‐PDMS) diblock copolymer. At this, the film is swollen in the vapor of n‐heptane (highly selective for PDMS). This vapor is stepwise replaced by the vapor of toluene (weakly selective for PS). The morphologies are investigated using in situ, real‐time grazing‐incidence small‐angle X‐ray scattering (GISAXS). The initial cylindrical morphology is transformed into, among others, the lamellar one. This novel type of experiments allows probing a trajectory in the state diagram of the PS‐b‐PDMS/n‐heptane/toluene mixture. To corroborate the morphologies, they are generated by molecular simulations, and the 2D GISAXS maps are calculated using the distorted‐wave Born approximation. To relate the morphologies to the solvent distribution in the two types of nanodomains, the latter is estimated from the intensities of the Bragg reflections in the 2D GISAXS maps along with the swelling ratio of the film. Comparison with the results from a similar experiment carried out at room temperature results in the same sequence of morphologies; however, at elevated temperature, more well‐ordered structures are obtained. This new approach proves to be efficient to achieve a block copolymer thin film having a desired morphology and orientation.

AB - Solvothermal vapor annealing at elevated temperature is applied to a thin film from a cylinder‐forming polystyrene‐block‐poly(dimethyl siloxane) (PS‐b‐PDMS) diblock copolymer. At this, the film is swollen in the vapor of n‐heptane (highly selective for PDMS). This vapor is stepwise replaced by the vapor of toluene (weakly selective for PS). The morphologies are investigated using in situ, real‐time grazing‐incidence small‐angle X‐ray scattering (GISAXS). The initial cylindrical morphology is transformed into, among others, the lamellar one. This novel type of experiments allows probing a trajectory in the state diagram of the PS‐b‐PDMS/n‐heptane/toluene mixture. To corroborate the morphologies, they are generated by molecular simulations, and the 2D GISAXS maps are calculated using the distorted‐wave Born approximation. To relate the morphologies to the solvent distribution in the two types of nanodomains, the latter is estimated from the intensities of the Bragg reflections in the 2D GISAXS maps along with the swelling ratio of the film. Comparison with the results from a similar experiment carried out at room temperature results in the same sequence of morphologies; however, at elevated temperature, more well‐ordered structures are obtained. This new approach proves to be efficient to achieve a block copolymer thin film having a desired morphology and orientation.

U2 - 10.1002/adfm.201706226

DO - 10.1002/adfm.201706226

M3 - Journal article

VL - 28

JO - Advanced Functional Materials

JF - Advanced Functional Materials

SN - 1616-301X

IS - 19

M1 - 1706226

ER -