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Title: Orientation mapping of semicrystalline polymers using scanning electron nanobeam diffraction

Abstract

Here, we demonstrate a scanning electron nanobeam diffraction technique that can be used for mapping the size and distribution of nanoscale crystalline regions in a polymer blend. In addition, it can map the relative orientation of crystallites and the degree of crystallinity of the material. The model polymer blend is a 50:50 w/w mixture of semicrystalline poly(3-hexylthiophene-2,5-diyl) (P3HT) and amorphous polystyrene (PS). The technique uses a scanning electron beam to raster across the sample and acquires a diffraction image at each probe position. Through image alignment and filtering, the diffraction image dataset enables mapping of the crystalline regions within the scanned area and construction of an orientation map.

Authors:
 [1];  [2];  [3];  [3];  [4];  [5];  [1]
  1. University of California, Berkeley, CA (United States); Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States). National Center for Electron Microscopy
  2. University of California, Berkeley, CA (United States); Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)
  3. Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States). National Center for Electron Microscopy
  4. Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)
  5. University of California, Berkeley, CA (United States); Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States). Materials Sciences Division and Joint Center for Energy Storage Research (JCESR)
Publication Date:
Research Org.:
Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES). Materials Sciences & Engineering Division; USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22). Materials Sciences & Engineering Division
OSTI Identifier:
1474961
Alternate Identifier(s):
OSTI ID: 1351660
Grant/Contract Number:  
AC02-05CH11231
Resource Type:
Accepted Manuscript
Journal Name:
Micron
Additional Journal Information:
Journal Volume: 88; Journal Issue: C; Related Information: © 2016 Elsevier Ltd.; Journal ID: ISSN 0968-4328
Publisher:
Elsevier
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; 77 NANOSCIENCE AND NANOTECHNOLOGY; TEM; STEM; spatially resolved; diffraction; crystal orientation; P3HT; polymers; locally resolved structure

Citation Formats

Panova, Ouliana, Chen, X. Chelsea, Bustillo, Karen C., Ophus, Colin, Bhatt, Mahesh P., Balsara, Nitash, and Minor, Andrew M. Orientation mapping of semicrystalline polymers using scanning electron nanobeam diffraction. United States: N. p., 2016. Web. doi:10.1016/j.micron.2016.05.008.
Panova, Ouliana, Chen, X. Chelsea, Bustillo, Karen C., Ophus, Colin, Bhatt, Mahesh P., Balsara, Nitash, & Minor, Andrew M. Orientation mapping of semicrystalline polymers using scanning electron nanobeam diffraction. United States. https://doi.org/10.1016/j.micron.2016.05.008
Panova, Ouliana, Chen, X. Chelsea, Bustillo, Karen C., Ophus, Colin, Bhatt, Mahesh P., Balsara, Nitash, and Minor, Andrew M. Fri . "Orientation mapping of semicrystalline polymers using scanning electron nanobeam diffraction". United States. https://doi.org/10.1016/j.micron.2016.05.008. https://www.osti.gov/servlets/purl/1474961.
@article{osti_1474961,
title = {Orientation mapping of semicrystalline polymers using scanning electron nanobeam diffraction},
author = {Panova, Ouliana and Chen, X. Chelsea and Bustillo, Karen C. and Ophus, Colin and Bhatt, Mahesh P. and Balsara, Nitash and Minor, Andrew M.},
abstractNote = {Here, we demonstrate a scanning electron nanobeam diffraction technique that can be used for mapping the size and distribution of nanoscale crystalline regions in a polymer blend. In addition, it can map the relative orientation of crystallites and the degree of crystallinity of the material. The model polymer blend is a 50:50 w/w mixture of semicrystalline poly(3-hexylthiophene-2,5-diyl) (P3HT) and amorphous polystyrene (PS). The technique uses a scanning electron beam to raster across the sample and acquires a diffraction image at each probe position. Through image alignment and filtering, the diffraction image dataset enables mapping of the crystalline regions within the scanned area and construction of an orientation map.},
doi = {10.1016/j.micron.2016.05.008},
journal = {Micron},
number = C,
volume = 88,
place = {United States},
year = {Fri May 27 00:00:00 EDT 2016},
month = {Fri May 27 00:00:00 EDT 2016}
}

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Cited by: 43 works
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Works referenced in this record:

Effect of Copolymer Composition on Electronic Conductivity of Electrochemically Oxidized Poly(3-hexylthiophene)- b -poly(ethylene oxide) Block Copolymers
journal, July 2015


Unique structural features and electrical properties of electrospun conjugated polymer poly(3-hexylthiophene) (P3HT) fibers
journal, December 2010


Control of the nanoscale crystallinity and phase separation in polymer solar cells
journal, March 2008

  • Chu, Chih-Wei; Yang, Hoichang; Hou, Wei-Jen
  • Applied Physics Letters, Vol. 92, Issue 10
  • DOI: 10.1063/1.2891884

Charge Transport in Organic Semiconductors
journal, July 2007

  • Coropceanu, Veaceslav; Cornil, Jerome; da Silva Filho, Demetrio A.
  • ChemInform, Vol. 38, Issue 29
  • DOI: 10.1002/chin.200729266

Packing Structure of Poly(3-hexylthiophene) Crystal: Ab Initio and Molecular Dynamics Studies
journal, May 2010

  • Dag, Sefa; Wang, Lin-Wang
  • The Journal of Physical Chemistry B, Vol. 114, Issue 18
  • DOI: 10.1021/jp1008219

A Strategy for Revealing the Packing in Semicrystalline π-Conjugated Polymers: Crystal Structure of Bulk Poly-3-hexyl-thiophene (P3HT)
journal, October 2012

  • Dudenko, Dmytro; Kiersnowski, Adam; Shu, Jie
  • Angewandte Chemie International Edition, Vol. 51, Issue 44
  • DOI: 10.1002/anie.201205075

The chemical and structural origin of efficient p-type doping in P3HT
journal, May 2013


Control of radiation damage in the TEM
journal, April 2013


Delocalized radiation damage in polymers
journal, January 2012


Diffraction contrast imaging using virtual apertures
journal, August 2015


Robust polythiophene nanowires cross-linked with functional fullerenes
journal, January 2014

  • Hammer, Brenton A. G.; Reyes-Martinez, Marcos A.; Bokel, Felicia A.
  • J. Mater. Chem. C, Vol. 2, Issue 45
  • DOI: 10.1039/C4TC01898B

Quantitative analysis of image contrast in electron micrographs of beam-sensitive crystals
journal, January 1985


Effect of Thickness-Dependent Microstructure on the Out-of-Plane Hole Mobility in Poly(3-Hexylthiophene) Films
journal, September 2012

  • Huang, Bingyuan; Glynos, Emmanouil; Frieberg, Bradley
  • ACS Applied Materials & Interfaces, Vol. 4, Issue 10
  • DOI: 10.1021/am3011252

X-ray structural and crystallinity studies of low and high molecular weight poly(3-hexylthiophene)
journal, March 2008

  • Joshi, S.; Grigorian, S.; Pietsch, U.
  • physica status solidi (a), Vol. 205, Issue 3
  • DOI: 10.1002/pssa.200723423

The Effect of Solution Processing on the Power Conversion Efficiency of P3HT-based Organic Solar Cells
journal, January 2014


Gelation of a Solution of Poly(3-hexylthiophene) Greatly Retards Its Crystallization Rate in the Subsequently Cast Film
journal, December 2014

  • Kao, Kuei-Yu; Lo, Shen-Chuan; Chen, Hsin-Lung
  • The Journal of Physical Chemistry B, Vol. 118, Issue 49
  • DOI: 10.1021/jp508775b

Structural Model of Regioregular Poly(3-hexylthiophene) Obtained by Electron Diffraction Analysis
journal, June 2010

  • Kayunkid, Navaphun; Uttiya, Sureeporn; Brinkmann, Martin
  • Macromolecules, Vol. 43, Issue 11, p. 4961-4967
  • DOI: 10.1021/ma100551m

Highly oriented crystals at the buried interface in polythiophene thin-film transistors
journal, February 2006

  • Joseph Kline, R.; McGehee, Michael D.; Toney, Michael F.
  • Nature Materials, Vol. 5, Issue 3
  • DOI: 10.1038/nmat1590

Advances in the Transmission Electron Microscopy of Polymers
journal, July 2010


X-ray scattering from oriented poly(3-alkylthiophenes)
journal, July 1992


Crystalline–crystalline poly(3-hexylthiophene)–polyethylene diblock copolymers: Solidification from the melt
journal, August 2008


The future of organic photovoltaics
journal, January 2015

  • Mazzio, Katherine A.; Luscombe, Christine K.
  • Chemical Society Reviews, Vol. 44, Issue 1
  • DOI: 10.1039/C4CS00227J

Relation between Microstructure and Charge Transport in Polymers of Different Regioregularity
journal, September 2011

  • McMahon, David P.; Cheung, David L.; Goris, Ludwig
  • The Journal of Physical Chemistry C, Vol. 115, Issue 39
  • DOI: 10.1021/jp207026s

Ordering of Poly(3-hexylthiophene) Nanocrystallites on the Basis of Substrate Surface Energy
journal, September 2009

  • Meredig, Bryce; Salleo, Alberto; Gee, Richard
  • ACS Nano, Vol. 3, Issue 10
  • DOI: 10.1021/nn800707z

Comparative study: The effects of solvent on the morphology, optical and structural features of regioregular poly(3-hexylthiophene):fullerene thin films
journal, May 2010


Strain mapping at nanometer resolution using advanced nano-beam electron diffraction
journal, June 2015

  • Ozdol, V. B.; Gammer, C.; Jin, X. G.
  • Applied Physics Letters, Vol. 106, Issue 25
  • DOI: 10.1063/1.4922994

Multi-phase microstructures drive exciton dissociation in neat semicrystalline polymeric semiconductors
journal, January 2015

  • Paquin, Francis; Rivnay, Jonathan; Salleo, Alberto
  • Journal of Materials Chemistry C, Vol. 3, Issue 41
  • DOI: 10.1039/C5TC02043C

The crystal structure of poly(2,6-naphthalenebenzobisthiazole)
journal, July 2005


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
  • DOI: 10.1063/1.3488459

X-ray structural studies of poly(3-alkylthiophenes): an example of an inverse comb
journal, August 1992

  • Prosa, T. J.; Winokur, M. J.; Moulton, Jeff
  • Macromolecules, Vol. 25, Issue 17
  • DOI: 10.1021/ma00043a019

Enthalpy of fusion of poly(3-hexylthiophene) by differential scanning calorimetry
journal, September 2014

  • Remy, Roddel; Weiss, Emily Daniels; Nguyen, Ngoc A.
  • Journal of Polymer Science Part B: Polymer Physics, Vol. 52, Issue 22
  • DOI: 10.1002/polb.23584

Dark field imaging of semicrystalline polymers by scanning transmission electron microscopy
journal, January 1981

  • Sherman, Edward S.; Wade Adams, W.; Thomas, Edwin L.
  • Journal of Materials Science, Vol. 16, Issue 1
  • DOI: 10.1007/BF00552052

The influence of fast secondary electrons on the aromatic structure of polystyrene
journal, May 2000


Remarkable Order of a High-Performance Polymer
journal, May 2013

  • Takacs, Christopher J.; Treat, Neil D.; Krämer, Stephan
  • Nano Letters, Vol. 13, Issue 6
  • DOI: 10.1021/nl4005805

Mapping Orientational Order in a Bulk Heterojunction Solar Cell with Polarization-Dependent Photoconductive Atomic Force Microscopy
journal, July 2014

  • Takacs, Christopher J.; Collins, Samuel D.; Love, John A.
  • ACS Nano, Vol. 8, Issue 8
  • DOI: 10.1021/nn502277d

Three-Dimensional Structure of P3HT Assemblies in Organic Solvents Revealed by Cryo-TEM
journal, March 2014

  • Wirix, Maarten J. M.; Bomans, Paul H. H.; Friedrich, Heiner
  • Nano Letters, Vol. 14, Issue 4
  • DOI: 10.1021/nl5001967

Single Crystals of Polythiophene with Different Molecular Conformations Obtained by Tetrahydrofuran Vapor Annealing and Controlling Solvent Evaporation
journal, May 2010

  • Xiao, Xinli; Wang, Zongbao; Hu, Zhijun
  • The Journal of Physical Chemistry B, Vol. 114, Issue 22
  • DOI: 10.1021/jp911525d

Molecular Dynamics of Regioregular Poly(3-hexylthiophene) Investigated by NMR Relaxation and an Interpretation of Temperature Dependent Optical Absorption
journal, January 2010

  • Yazawa, Koji; Inoue, Yoshio; Shimizu, Tadashi
  • The Journal of Physical Chemistry B, Vol. 114, Issue 3
  • DOI: 10.1021/jp910590d

Works referencing / citing this record:

Metal-organic framework crystal-glass composites
journal, June 2019


Nanoscale mosaicity revealed in peptide microcrystals by scanning electron nanodiffraction
journal, January 2019

  • Gallagher-Jones, Marcus; Ophus, Colin; Bustillo, Karen C.
  • Communications Biology, Vol. 2, Issue 1
  • DOI: 10.1038/s42003-018-0263-8