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Title: In situ GISAXS study of a Si-containing block copolymer under solvent vapor annealing: Effects of molecular weight and solvent vapor composition

Journal Article · · Polymer
ORCiD logo [1];  [2];  [1]
  1. Massachusetts Inst. of Technology (MIT), Cambridge, MA (United States)
  2. Brookhaven National Lab. (BNL), Upton, NY (United States)

The room-temperature solvent vapor annealing of polystyrene-b-polydimethylsiloxane (PS-b-PDMS) block copolymer films was studied in situ by grazing incidence small-angle X-ray scattering. Films of cylinder-forming PS-b-PDMS with molecular weight 16 kg/mol and 12.2 kg/mol, annealed under vapors of toluene:heptane with varying composition, exhibited swelling-ratio-dependent evolution of microdomain spacing and orientation. In a vapor made from a toluene:heptane 5:1 volumetric ratio liquid mixture, or from pure toluene, cylindrical microdomains reoriented from majority out-of-plane to in-plane during annealing, while drying led to shrinkage along the film normal and a large distortion of the hexagonal lattice of in-plane cylinders. As a result, annealing under vapor from a toluene:heptane 1:5 volumetric ratio liquid produced a non-bulk lamellar structure in the 16 kg/mol PS-b-PDMS.

Research Organization:
Brookhaven National Lab. (BNL), Upton, NY (United States). Center for Functional Nanomaterials (CFN)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
Grant/Contract Number:
SC00112704; SC0012704; DMR1419807
OSTI ID:
1337655
Alternate ID(s):
OSTI ID: 1359790
Report Number(s):
BNL-113318-2016-JA; R&D Project: 32452; KC0403020
Journal Information:
Polymer, Vol. 101, Issue C; ISSN 0032-3861
Publisher:
ElsevierCopyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 9 works
Citation information provided by
Web of Science

References (46)

Composite mesostructures by nano-confinement journal October 2004
Reversible Morphology Control in Block Copolymer Films via Solvent Vapor Processing: An in Situ GISAXS Study journal May 2010
Widely Tunable Morphologies in Block Copolymer Thin Films Through Solvent Vapor Annealing Using Mixtures of Selective Solvents journal April 2015
Thin Film Morphologies of Bulk-Gyroid Polystyrene- block -polydimethylsiloxane under Solvent Vapor Annealing journal August 2014
Solvent-Vapor-Induced Tunability of Self-Assembled Block Copolymer Patterns journal June 2009
A Top Coat with Solvent Annealing Enables Perpendicular Orientation of Sub-10 nm Microdomains in Si-Containing Block Copolymer Thin Films journal September 2014
Solvent Vapor Annealing of Block Polymer Thin Films journal June 2013
An In Situ Grazing Incidence X-Ray Scattering Study of Block Copolymer Thin Films During Solvent Vapor Annealing journal November 2013
Magnetic field alignment of block copolymers and polymer nanocomposites: Scalable microstructure control in functional soft materials journal October 2011
Directed Assembly of Block Copolymer Blends into Nonregular Device-Oriented Structures journal June 2005
3D TEM Tomography of Templated Bilayer Films of Block Copolymers journal October 2014
Perpendicular Block Copolymer Microdomains in High Aspect Ratio Templates journal September 2015
Self-assembly of block copolymer thin films journal June 2010
High-Aspect-Ratio Perpendicular Orientation of PS- b -PDMS Thin Films under Solvent Annealing journal October 2012
The Full Phase Behavior for Block Copolymers in Solvents of Varying Selectivity journal June 2002
Phase Behavior of Block Copolymers in a Neutral Solvent journal February 2003
Phase Behavior of a Block Copolymer in Solvents of Varying Selectivity journal August 2000
Morphology Control in Block Copolymer Films Using Mixed Solvent Vapors journal August 2012
Morphology-Controlled Kinetics of Solvent Uptake by Block Copolymer Films in Nonselective Solvent Vapors journal August 2014
Effect of dilution on a block copolymer in the complex phase window journal December 1998
An in situ GISAXS study of selective solvent vapor annealing in thin block copolymer films: Symmetry breaking of in-plane sphere order upon deswelling journal October 2015
Structural Rearrangements in a Lamellar Diblock Copolymer Thin Film during Treatment with Saturated Solvent Vapor journal January 2010
In Situ GISAXS Study on Solvent Vapour Induced Orientation Switching in PS- b -P4VP Block Copolymer Thin Films journal November 2010
Rapid fabrication of hierarchically structured supramolecular nanocomposite thin films in one minute journal June 2014
In Situ Characterization of the Self-Assembly of a Polystyrene–Polydimethylsiloxane Block Copolymer during Solvent Vapor Annealing journal November 2015
Cylinder Orientation Mechanism in Block Copolymer Thin Films Upon Solvent Evaporation journal September 2010
Structural Analysis of Block Copolymer Thin Films with Grazing Incidence Small-Angle X-ray Scattering journal May 2005
Inner Structure of Thin Films of Lamellar Poly(styrene- b -butadiene) Diblock Copolymers As Revealed by Grazing-Incidence Small-Angle Scattering journal January 2007
A SAXS/WAXS/GISAXS Beamline with Multilayer Monochromator journal October 2010
Depth-Dependent Structural Changes in PS- b -P2VP Thin Films Induced by Annealing journal August 2014
Lamellar Diblock Copolymer Thin Films during Solvent Vapor Annealing Studied by GISAXS: Different Behavior of Parallel and Perpendicular Lamellae journal August 2014
Controlling Domain Spacing and Grain Size in Cylindrical Block Copolymer Thin Films by Means of Thermal and Solvent Vapor Annealing journal April 2016
Solvent vapor annealing of block copolymer thin films: removal of processing history journal June 2014
Block Copolymer Self Assembly during Rapid Solvent Evaporation: Insights into Cylinder Growth and Stability journal December 2013
Toward an equilibrium structure in lamellar diblock copolymer thin films using solvent vapor annealing – An in-situ time-resolved GISAXS study journal August 2016
Structural Transitions in Asymmetric Poly(styrene)- block -Poly(lactide) Thin Films Induced by Solvent Vapor Exposure journal July 2014
Coexistence curves of polystyrene/ poly(dimethylsiloxane) blends journal January 1995
Sub-5 nm Domains in Ordered Poly(cyclohexylethylene)- block -poly(methyl methacrylate) Block Polymers for Lithography journal February 2014
Universal pattern transfer methods for metal nanostructures by block copolymer lithography journal August 2015
Eliminating the Trade-Off between the Throughput and Pattern Quality of Sub-15 nm Directed Self-Assembly via Warm Solvent Annealing journal November 2014
Simulation methods for solvent vapor annealing of block copolymer thin films journal January 2015
Topcoat-Assisted Perpendicular and Straightly Parallel Coexisting Orientations of Block Copolymer Films journal April 2015
Progress in control of microdomain orientation in block copolymers – Efficiencies of various external fields journal June 2008
Highly Oriented and Ordered Arrays from Block Copolymers via Solvent Evaporation journal February 2004
Block Copolymer Thermodynamics: Theory and Experiment journal October 1990
Failure of the dilution approximation in block copolymer solutions journal November 1995

Cited By (2)

In Situ Tracking of Composition and Morphology of a Diblock Copolymer Film with GISAXS during Exchange of Solvent Vapors at Elevated Temperatures journal March 2018
UV-solvent annealing of PDMS-majority and PS-majority PS- b -PDMS block copolymer films journal October 2016