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Title: Radiation damage in polymer films from grazing-incidence X-ray scattering measurements

Grazing-incidence X-ray scattering (GIXS) is widely used to analyze the crystallinity and nanoscale structure in thin polymer lms. 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: lms are exposed to patterns of x-ray radiation, and changes in polymer structure are revealed by immersing the lm 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, llm 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.
 [1] ;  [2] ;  [2] ;  [3] ;  [1]
  1. Department of Chemical and Biomolecular Engineering, University of Houston, Houston Texas 77204-4004
  2. Department of Electrical and Computer Engineering, University of Houston, Houston Texas 77204-4005
  3. X-Ray Science Division, Argonne National Laboratory, Argonne Illinois 60439
Publication Date:
OSTI Identifier:
DOE Contract Number:
Resource Type:
Journal Article
Resource Relation:
Journal Name: Journal of Polymer Science. Part B, Polymer Physics; Journal Volume: 54; Journal Issue: 11
Research Org:
Argonne National Laboratory (ANL)
Sponsoring Org:
National Science Foundation (NSF); USDOE Office of Science
Country of Publication:
United States