Simulation-guided analysis of resonant soft X-ray scattering for determining the microstructure of triblock copolymers

Resonant soft X-ray scattering (RSoXS) probes structure with chemical sensitivity that is useful for determining the morphology of multiblock copolymers. However, the hyperspectral scattering data produced by this technique can be challenging to interpret. Here, we use computational scattering simul...

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Bibliographic Details
Published inMolecular systems design & engineering Vol. 7; no. 11; pp. 1449 - 1458
Main Authors Reynolds, Veronica G, Callan, Devon H, Saurabh, Kumar, Murphy, Elizabeth A, Albanese, Kaitlin R, Chen, Yan-Qiao, Wu, Claire, Gann, Eliot, Hawker, Craig J, Ganapathysubramanian, Baskar, Bates, Christopher M, Chabinyc, Michael L
Format Journal Article
LanguageEnglish
Published Cambridge Royal Society of Chemistry 31.10.2022
Royal Society of Chemistry (RSC)
Subjects
Block copolymers
Electron density
Microstructure
Simulation
Soft x rays
Terpolymers
X-ray scattering
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Summary:Resonant soft X-ray scattering (RSoXS) probes structure with chemical sensitivity that is useful for determining the morphology of multiblock copolymers. However, the hyperspectral scattering data produced by this technique can be challenging to interpret. Here, we use computational scattering simulations to extract the microstructure of a model triblock copolymer from the energy-dependent scattering from RSoXS. An ABC triblock terpolymer formed from poly(4-methylcaprolactone) (P4MCL), poly(2,2,2-trifluoroethylacrylate) (PTFEA), and poly (dodecylacrylate) (PDDA), P4MCL- block -PTFEA- block -PDDA, was synthesized as the model triblock system. Through quantitative evaluation of simulated scattering data from a physics-informed set of candidate structure models against experimental RSoXS data, we find the best agreement with hexagonally packed core-shell cylinders. This result is also consistent with electron-density reconstruction from hard X-ray scattering data evaluated against electron-density maps generated with the same model set. These results demonstrate the utility of simulation-guided scattering analysis to study complex microstructures that are challenging to image by microscopy. Resonant soft X-ray scattering (RSoXS) probes structure with chemical sensitivity that is useful for determining the morphology of multiblock copolymers.
Bibliography:https://doi.org/10.1039/d2me00096b
Electronic supplementary information (ESI) available: Reagent information, synthetic methods, molecular characterization, automated flash chromatography method, optical microscopy of thin film samples for NEXAFS spectroscopy, refractive index calculation of mixtures, complex refractive indices and pairwise contrast functions of P4MCL, PTFEA, and PDDA, geometric derivations for structure models, radially-averaged RSoXS data, description of data reduction and peak fitting, complete set of scattering pattern simulations, relative root-mean-squared error calculation, discussion on the expected impact of varying cylinder orientation distributions. See DOI
USDOE
SC0012704
ISSN:2058-9689
2058-9689
DOI:10.1039/d2me00096b