Radiation damage in polymer films from grazing-incidence X-ray scattering measurements
Abstract
Grazing-incidence X-ray scattering (GIXS) is widely used to analyze the crystallinity and nanoscale structure in thin polymer films. However, ionizing radiation will generate free radicals that initiate cross-linking and/or chain scission, and structural damage will impact the ordering kinetics, thermodynamics, and crystallinity in many polymers. We report a simple methodology to screen for beam damage that is based on lithographic principles: films are exposed to patterns of x-ray radiation, and changes in polymer structure are revealed by immersing the film in a solvent that dissolves the shortest chains. The experiments are implemented with high throughput using the standard beam line instrumentation and a typical GIXS configuration. The extent of damage (at a fixed radiation dose) depends on a range of intrinsic material properties and experimental variables, including the polymer chemistry and molecular weight, exposure environment, film thickness, and angle of incidence. The solubility switch for common polymers is detected within 10-60 sec at ambient temperature, and we verified that this first indication of damage corresponds with the onset of network formation in glassy polystyrene and a loss of crystallinity in polyalkylthiophenes. Therefore, grazing-incidence x-ray patterning offers an efficient approach to determine the appropriate data acquisition times for any GIXS experiment.
- Authors:
-
- Univ. of Houston, Houston TX (United States). Dept. of Chemical and Biomolecular Engineering
- Univ. of Houston, Houston TX (United States). Dept. of of Electrical and Computer Engineering
- Argonne National Lab. (ANL), Argonne, IL (United States). X-Ray Science Division
- Publication Date:
- Research Org.:
- Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS)
- Sponsoring Org.:
- National Science Foundation (NSF); USDOE Office of Science (SC)
- OSTI Identifier:
- 1267165
- Alternate Identifier(s):
- OSTI ID: 1400955
- Grant/Contract Number:
- AC02-06CH11357; CBET-1236606; DMR-1151468
- Resource Type:
- Accepted Manuscript
- Journal Name:
- Journal of Polymer Science. Part B, Polymer Physics
- Additional Journal Information:
- Journal Volume: 54; Journal Issue: 11; Journal ID: ISSN 0887-6266
- Publisher:
- Wiley
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 36 MATERIALS SCIENCE; beam damage; grazing incidence; radiation crosslinking; WAXS; irradiation; SAXS; crosslinking; block copolymers; conjugated polymers; x-ray
Citation Formats
Vaselabadi, Saeed Ahmadi, Shakarisaz, David, Ruchhoeft, Paul, Strzalka, Joseph, and Stein, Gila E. Radiation damage in polymer films from grazing-incidence X-ray scattering measurements. United States: N. p., 2016.
Web. doi:10.1002/polb.24006.
Vaselabadi, Saeed Ahmadi, Shakarisaz, David, Ruchhoeft, Paul, Strzalka, Joseph, & Stein, Gila E. Radiation damage in polymer films from grazing-incidence X-ray scattering measurements. United States. doi:10.1002/polb.24006.
Vaselabadi, Saeed Ahmadi, Shakarisaz, David, Ruchhoeft, Paul, Strzalka, Joseph, and Stein, Gila E. Tue .
"Radiation damage in polymer films from grazing-incidence X-ray scattering measurements". United States. doi:10.1002/polb.24006. https://www.osti.gov/servlets/purl/1267165.
@article{osti_1267165,
title = {Radiation damage in polymer films from grazing-incidence X-ray scattering measurements},
author = {Vaselabadi, Saeed Ahmadi and Shakarisaz, David and Ruchhoeft, Paul and Strzalka, Joseph and Stein, Gila E.},
abstractNote = {Grazing-incidence X-ray scattering (GIXS) is widely used to analyze the crystallinity and nanoscale structure in thin polymer films. However, ionizing radiation will generate free radicals that initiate cross-linking and/or chain scission, and structural damage will impact the ordering kinetics, thermodynamics, and crystallinity in many polymers. We report a simple methodology to screen for beam damage that is based on lithographic principles: films are exposed to patterns of x-ray radiation, and changes in polymer structure are revealed by immersing the film in a solvent that dissolves the shortest chains. The experiments are implemented with high throughput using the standard beam line instrumentation and a typical GIXS configuration. The extent of damage (at a fixed radiation dose) depends on a range of intrinsic material properties and experimental variables, including the polymer chemistry and molecular weight, exposure environment, film thickness, and angle of incidence. The solubility switch for common polymers is detected within 10-60 sec at ambient temperature, and we verified that this first indication of damage corresponds with the onset of network formation in glassy polystyrene and a loss of crystallinity in polyalkylthiophenes. Therefore, grazing-incidence x-ray patterning offers an efficient approach to determine the appropriate data acquisition times for any GIXS experiment.},
doi = {10.1002/polb.24006},
journal = {Journal of Polymer Science. Part B, Polymer Physics},
number = 11,
volume = 54,
place = {United States},
year = {2016},
month = {2}
}
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Works referenced in this record:
Quantification of Thin Film Crystallographic Orientation Using X-ray Diffraction with an Area Detector
journal, June 2010
- Baker, Jessy L.; Jimison, Leslie H.; Mannsfeld, Stefan
- Langmuir, Vol. 26, Issue 11
Layering Transitions in Thin Films of Spherical-Domain Block Copolymers
journal, April 2007
- Stein, Gila E.; Kramer, Edward J.; Li, Xuefa
- Macromolecules, Vol. 40, Issue 7
Molecular rearrangements in ultra high molecular weight polyethylene after irradiation and long-term storage in air
journal, April 1999
- Premnath, V.; Bellare, A.; Merrill, E. W.
- Polymer, Vol. 40, Issue 9
Properties of crosslinked polyolefin-based materials
journal, January 1995
- Chodak, I.
- Progress in Polymer Science, Vol. 20, Issue 6
Characterization of the effects of soft X-ray irradiation on polymers
journal, January 2002
- Coffey, T.; Urquhart, S. G.; Ade, H.
- Journal of Electron Spectroscopy and Related Phenomena, Vol. 122, Issue 1
Statistical Mechanics of Swelling of Network Structures
journal, January 1950
- Flory, Paul J.
- The Journal of Chemical Physics, Vol. 18, Issue 1
Grazing incidence wide angle x-ray scattering at the wiggler beamline BW4 of HASYLAB
journal, October 2010
- Perlich, J.; Rubeck, J.; Botta, S.
- Review of Scientific Instruments, Vol. 81, Issue 10
Fabrication of Advanced Functional Devices Combining Soft Chemistry with X-ray Lithography in One Step
journal, September 2009
- Falcaro, Paolo; Malfatti, Luca; Vaccari, Lisa
- Advanced Materials, Vol. 21, Issue 48
Effect of Photovoltaic Polymer/Fullerene Blend Composition Ratio on Microstructure Evolution during Film Solidification Investigated in Real Time by X-ray Diffraction
journal, May 2011
- Sanyal, Monamie; Schmidt-Hansberg, Benjamin; Klein, Michael F. G.
- Macromolecules, Vol. 44, Issue 10
Morphology and microphase separation of star copolymers
journal, October 2014
- Park, Jicheol; Jang, Sangshin; Kon Kim, Jin
- Journal of Polymer Science Part B: Polymer Physics, Vol. 53, Issue 1
Thermal degradation of crosslinked high density polyethylene
journal, February 1999
- Han, Seong Ok; Lee, Dong Won; Han, Oc Hee
- Polymer Degradation and Stability, Vol. 63, Issue 2
The dedicated high-resolution grazing-incidence X-ray scattering beamline 8-ID-E at the Advanced Photon Source
journal, June 2012
- Jiang, Zhang; Li, Xuefa; Strzalka, Joseph
- Journal of Synchrotron Radiation, Vol. 19, Issue 4
Proximity X-ray Lithography Using Self-Assembled Alkylsiloxane Films: Resolution and Pattern Transfer
journal, January 2001
- Yang, Xiao M.; Peters, Richard D.; Kim, Tae K.
- Langmuir, Vol. 17, Issue 1
Radiation-induced crystallinity changes in linear polyethylene: Influence of aging
journal, February 1983
- Bhateja, S. K.
- Journal of Applied Polymer Science, Vol. 28, Issue 2
Molecular Order in High-Efficiency Polymer/Fullerene Bulk Heterojunction Solar Cells
journal, September 2011
- Hammond, Matthew R.; Kline, R. Joseph; Herzing, Andrew A.
- ACS Nano, Vol. 5, Issue 10
Morphology and Charge Transport in Conjugated Polymers
journal, January 2006
- Kline, R. J.; McGehee, M. D.
- Journal of Macromolecular Science, Part C: Polymer Reviews, Vol. 46, Issue 1
Spin-Cast Bulk Heterojunction Solar Cells: A Dynamical Investigation
journal, February 2013
- Chou, Kang Wei; Yan, Buyi; Li, Ruipeng
- Advanced Materials, Vol. 25, Issue 13
Widely Tunable Morphologies in Block Copolymer Thin Films Through Solvent Vapor Annealing Using Mixtures of Selective Solvents
journal, April 2015
- Chavis, Michelle A.; Smilgies, Detlef-M.; Wiesner, Ulrich B.
- Advanced Functional Materials, Vol. 25, Issue 20
La théorie générale des couches minces
journal, January 1950
- Abelès, Florin
- Journal de Physique et le Radium, Vol. 11, Issue 7
The Active Layer Morphology of Organic Solar Cells Probed with Grazing Incidence Scattering Techniques
journal, February 2014
- Müller-Buschbaum, Peter
- Advanced Materials, Vol. 26, Issue 46
A saddle field ion source of spherical configuration for etching and thinning applications
journal, October 1974
- Franks, J.; Ghander, A. M.
- Vacuum, Vol. 24, Issue 10
Advanced grazing-incidence techniques for modern soft-matter materials analysis
journal, January 2015
- Hexemer, Alexander; Müller-Buschbaum, Peter
- IUCrJ, Vol. 2, Issue 1
Quantitative Determination of Organic Semiconductor Microstructure from the Molecular to Device Scale
journal, June 2012
- Rivnay, Jonathan; Mannsfeld, Stefan C. B.; Miller, Chad E.
- Chemical Reviews, Vol. 112, Issue 10
Nanoimprint-Induced Molecular Orientation in Semiconducting Polymer Nanostructures
journal, August 2011
- Hlaing, Htay; Lu, Xinhui; Hofmann, Tommy
- ACS Nano, Vol. 5, Issue 9
Stepwise Swelling of a Thin Film of Lamellae-Forming Poly(styrene- b -butadiene) in Cyclohexane Vapor
journal, June 2012
- Di, Zhenyu; Posselt, Dorthe; Smilgies, Detlef-M.
- Macromolecules, Vol. 45, Issue 12
Equilibrium Swelling of Polystyrene Networks by Linear Polystyrene
journal, January 2003
- Russ, Thomas; Brenn, Rüdiger; Geoghegan, Mark
- Macromolecules, Vol. 36, Issue 1
Polystyrene negative resist for high-resolution electron beam lithography
journal, January 2011
- Ma, Siqi; Con, Celal; Yavuz, Mustafa
- Nanoscale Research Letters, Vol. 6, Issue 1
Fabrication of 5–7 nm wide etched lines in silicon using 100 keV electron‐beam lithography and polymethylmethacrylate resist
journal, March 1993
- Chen, Wei; Ahmed, Haroon
- Applied Physics Letters, Vol. 62, Issue 13
Probing surface and interface morphology with Grazing Incidence Small Angle X-Ray Scattering
journal, August 2009
- Renaud, Gilles; Lazzari, Rémi; Leroy, Frédéric
- Surface Science Reports, Vol. 64, Issue 8
Radiation-induced crystallinity changes in linear polyethylene
journal, April 1983
- Bhateja, S. K.; Andrews, E. H.; Young, R. J.
- Journal of Polymer Science: Polymer Physics Edition, Vol. 21, Issue 4
Swelling of Zwitterionic Polymer Films Characterized by Spectroscopic Ellipsometry
journal, December 2001
- Tang, Y.; Lu, J. R.; Lewis, A. L.
- Macromolecules, Vol. 34, Issue 25
Conversion of mass spectrometers for fast-atom bombardment using easily constructed components
journal, March 1983
- Hogg, A. M.
- International Journal of Mass Spectrometry and Ion Physics, Vol. 49, Issue 1
Structural Analysis of Block Copolymer Thin Films with Grazing Incidence Small-Angle X-ray Scattering
journal, May 2005
- Lee, Byeongdu; Park, Insun; Yoon, Jinhwan
- Macromolecules, Vol. 38, Issue 10
X-ray lithography from 500 to 30 nm: X-ray nanolithography
journal, May 1993
- Smith, Henry I.; Schattenburg, M. L.
- IBM Journal of Research and Development, Vol. 37, Issue 3
Molecular Characterization of Organic Electronic Films
journal, August 2010
- DeLongchamp, Dean M.; Kline, R. Joseph; Fischer, Daniel A.
- Advanced Materials, Vol. 23, Issue 3
GIXSGUI : a MATLAB toolbox for grazing-incidence X-ray scattering data visualization and reduction, and indexing of buried three-dimensional periodic nanostructured films
journal, April 2015
- Jiang, Zhang
- Journal of Applied Crystallography, Vol. 48, Issue 3
Charge transport in polymeric transistors
journal, March 2007
- Salleo, Alberto
- Materials Today, Vol. 10, Issue 3
1.14 Energy distribution of the ions produced by saddle field ion sources
journal, January 1977
- Khorossany, M.; Fitch, Rk
- Vacuum, Vol. 27, Issue 3
Extendibility of synchrotron radiation lithography to the sub-100 nm region
journal, November 1996
- Deguchi, Kimiyoshi
- Journal of Vacuum Science & Technology B: Microelectronics and Nanometer Structures, Vol. 14, Issue 6
Direct Patterning of Conductive Polymer Domains for Photovoltaic Devices
journal, July 2012
- Moungthai, Suchanun; Mahadevapuram, Nikhila; Ruchhoeft, Paul
- ACS Applied Materials & Interfaces, Vol. 4, Issue 8
Grazing incident small angle x-ray scattering: A metrology to probe nanopatterned surfaces
journal, January 2009
- Hofmann, T.; Dobisz, E.; Ocko, B. M.
- Journal of Vacuum Science & Technology B: Microelectronics and Nanometer Structures, Vol. 27, Issue 6
Scherrer grain-size analysis adapted to grazing-incidence scattering with area detectors
journal, October 2009
- Smilgies, Detlef-M.
- Journal of Applied Crystallography, Vol. 42, Issue 6
Radiation Induced Crystallinity Changes in Linear Polyethylenes: Long Term Aging Effects
journal, September 1989
- Bhateja, S. K.; Andrews, E. H.; Yarbrough, S. M.
- Polymer Journal, Vol. 21, Issue 9
X‐ray Scattering from Films of Semiconducting Polymers
journal, August 2008
- Chabinyc, Michael L.
- Polymer Reviews, Vol. 48, Issue 3
Near neighbor averaging: A technique for improving image uniformity in aperture array lithography
journal, January 2009
- Nasrullah, A.; Smith, D.; Sherlock, T.
- Journal of Vacuum Science & Technology B: Microelectronics and Nanometer Structures, Vol. 27, Issue 6
Probing Self-Assembly of Cylindrical Morphology Block Copolymer Using in Situ and ex Situ Grazing Incidence Small-Angle X-ray Scattering: The Attractive Case of Graphoepitaxy
journal, October 2014
- Maret, Mireille; Tiron, Raluca; Chevalier, Xavier
- Macromolecules, Vol. 47, Issue 20
Electron-Beam Surface-Patterned Poly(ethylene glycol) Microhydrogels
journal, July 2003
- Krsko, P.; Sukhishvili, S.; Mansfield, M.
- Langmuir, Vol. 19, Issue 14
Crystallinity changes and melting behavior of the uniaxially oriented iPP exposed to high doses of gamma radiation
journal, February 2005
- Stojanović, Z.; Kačarević-Popović, Z.; Galović, S.
- Polymer Degradation and Stability, Vol. 87, Issue 2
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Determining order-to-disorder transitions in block copolymer thin films using a self-referencing fluorescent probe
journal, January 2020
- Qiang, Zhe; Li, Lingqiao; Torkelson, John M.
- Molecular Systems Design & Engineering, Vol. 5, Issue 1
Swelling responses of surface-attached bottlebrush polymer networks
journal, January 2018
- Mah, Adeline Huizhen; Mei, Hao; Basu, Prithvi
- Soft Matter, Vol. 14, Issue 32
Visualizing percolation and ion transport in hybrid solid electrolytes for Li–metal batteries
journal, January 2019
- Zaman, Wahid; Hortance, Nicholas; Dixit, Marm B.
- Journal of Materials Chemistry A, Vol. 7, Issue 41
Visualizing percolation and ion transport in hybrid solid electrolytes for Li–metal batteries
journal, January 2019
- Zaman, Wahid; Hortance, Nicholas; Dixit, Marm B.
- Journal of Materials Chemistry A, Vol. 7, Issue 41