Helium Ion Microscopy with Secondary Ion Mass Spectrometry for Nanoscale Chemical Imaging and Analysis of Polyolefins

Olga S. Ovchinnikova; Nikolay Borodinov; Artem A. Trofimov; Steven T. King; Matthias Lorenz; William Lamberti; David Abmayr; Anton V. Ievlev

doi:10.1021/acsapm.1c00407

Helium Ion Microscopy with Secondary Ion Mass Spectrometry for Nanoscale Chemical Imaging and Analysis of Polyolefins

Olga S. Ovchinnikova, Nikolay Borodinov, Artem A. Trofimov, Steven T. King, Matthias Lorenz, William Lamberti, David Abmayr, Anton V. Ievlev

Functional Atomic Force Microscopy Group

Research output: Contribution to journal › Article › peer-review

1 Scopus citations

Abstract

To date, chemical imaging of polymers and polymer blends has been primarily accomplished using time-of-flight secondary ion mass spectrometry (ToF-SIMS) to directly visualize the distribution of components in a complex material with spatial resolution ranging from 100 nm to 5 μm. However, in many cases, this resolution falls far short of visualizing interfaces directly. To overcome these limitations, recent work has focused on developing a SIMS detection system based on a helium ion microscope (HIM) enabling chemical imaging with a demonstrated ∼14 nm spatial resolution. Here, we utilize HIM-SIMS for differentiation between the olefin-based polymers of polyethylene (PE) and polypropylene (PP). We illustrate both analyses for separating PE and PP using specific mass fragment ratios as well as demonstrate spatially resolved imaging of phase-separated domains within PE. Overall, we demonstrate the abilities of HIM-SIMS as a multimodal chemical technique for imaging and quantification of polyolefin interfaces, which could be more broadly applied to the analysis of more complex polymeric systems.

Original language	English
Pages (from-to)	3478-3484
Number of pages	7
Journal	ACS Applied Polymer Materials
Volume	3
Issue number	7
DOIs	https://doi.org/10.1021/acsapm.1c00407
State	Published - Jul 9 2021

Bibliographical note

Publisher Copyright:
© 2021 American Chemical Society.

Funding

The research was conducted at the Center for Nanophase Materials Sciences, which is a Department of Energy (DOE) Office of Science User Facility and using instrumentation within ORNL’s Materials Characterization Core provided by UT-Battelle, LLC under Contract No. DE-AC05-00OR22725 with the U.S. Department of Energy. A.A.T., W.L., and D.A. were supported by ExxonMobil Chemical Company. The authors are grateful to Dr. Dale K. Hensley at CNMS for performing gold coating of the samples and Dr. Alex Belianinov for useful discussion of the data. This manuscript has been authored by UT-Battelle, LLC, under Contract No. DE-AC0500OR22725 with the U.S. Department of Energy. The United States Government retains and the publisher, by accepting the article for publication, acknowledges that the United States Government retains a nonexclusive, paid-up, irrevocable, worldwide license to publish or reproduce the published form of this manuscript or allow others to do so, for the United States Government purposes. The Department of Energy will provide public access to these results of federally sponsored research in accordance with the DOE Public Access Plan ( http://energy.gov/downloads/doe-public-access-plan ).

Funders	Funder number
ExxonMobil Chemical Company
U.S. Department of Energy
Office of Science
UT-Battelle	DE-AC0500OR22725

Keywords

ToF-SIMS
helium ion microscope
polymer
polyolefins
secondary ion mass spectrometry

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10.1021/acsapm.1c00407

Cite this

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title = "Helium Ion Microscopy with Secondary Ion Mass Spectrometry for Nanoscale Chemical Imaging and Analysis of Polyolefins",

abstract = "To date, chemical imaging of polymers and polymer blends has been primarily accomplished using time-of-flight secondary ion mass spectrometry (ToF-SIMS) to directly visualize the distribution of components in a complex material with spatial resolution ranging from 100 nm to 5 μm. However, in many cases, this resolution falls far short of visualizing interfaces directly. To overcome these limitations, recent work has focused on developing a SIMS detection system based on a helium ion microscope (HIM) enabling chemical imaging with a demonstrated ∼14 nm spatial resolution. Here, we utilize HIM-SIMS for differentiation between the olefin-based polymers of polyethylene (PE) and polypropylene (PP). We illustrate both analyses for separating PE and PP using specific mass fragment ratios as well as demonstrate spatially resolved imaging of phase-separated domains within PE. Overall, we demonstrate the abilities of HIM-SIMS as a multimodal chemical technique for imaging and quantification of polyolefin interfaces, which could be more broadly applied to the analysis of more complex polymeric systems.",

keywords = "ToF-SIMS, helium ion microscope, polymer, polyolefins, secondary ion mass spectrometry",

author = "Ovchinnikova, {Olga S.} and Nikolay Borodinov and Trofimov, {Artem A.} and King, {Steven T.} and Matthias Lorenz and William Lamberti and David Abmayr and Ievlev, {Anton V.}",

note = "Publisher Copyright: {\textcopyright} 2021 American Chemical Society.",

year = "2021",

month = jul,

day = "9",

doi = "10.1021/acsapm.1c00407",

language = "English",

volume = "3",

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AU - Ovchinnikova, Olga S.

AU - Borodinov, Nikolay

AU - Trofimov, Artem A.

AU - King, Steven T.

AU - Lorenz, Matthias

AU - Lamberti, William

AU - Abmayr, David

AU - Ievlev, Anton V.

PY - 2021/7/9

Y1 - 2021/7/9

N2 - To date, chemical imaging of polymers and polymer blends has been primarily accomplished using time-of-flight secondary ion mass spectrometry (ToF-SIMS) to directly visualize the distribution of components in a complex material with spatial resolution ranging from 100 nm to 5 μm. However, in many cases, this resolution falls far short of visualizing interfaces directly. To overcome these limitations, recent work has focused on developing a SIMS detection system based on a helium ion microscope (HIM) enabling chemical imaging with a demonstrated ∼14 nm spatial resolution. Here, we utilize HIM-SIMS for differentiation between the olefin-based polymers of polyethylene (PE) and polypropylene (PP). We illustrate both analyses for separating PE and PP using specific mass fragment ratios as well as demonstrate spatially resolved imaging of phase-separated domains within PE. Overall, we demonstrate the abilities of HIM-SIMS as a multimodal chemical technique for imaging and quantification of polyolefin interfaces, which could be more broadly applied to the analysis of more complex polymeric systems.

AB - To date, chemical imaging of polymers and polymer blends has been primarily accomplished using time-of-flight secondary ion mass spectrometry (ToF-SIMS) to directly visualize the distribution of components in a complex material with spatial resolution ranging from 100 nm to 5 μm. However, in many cases, this resolution falls far short of visualizing interfaces directly. To overcome these limitations, recent work has focused on developing a SIMS detection system based on a helium ion microscope (HIM) enabling chemical imaging with a demonstrated ∼14 nm spatial resolution. Here, we utilize HIM-SIMS for differentiation between the olefin-based polymers of polyethylene (PE) and polypropylene (PP). We illustrate both analyses for separating PE and PP using specific mass fragment ratios as well as demonstrate spatially resolved imaging of phase-separated domains within PE. Overall, we demonstrate the abilities of HIM-SIMS as a multimodal chemical technique for imaging and quantification of polyolefin interfaces, which could be more broadly applied to the analysis of more complex polymeric systems.

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KW - helium ion microscope

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Helium Ion Microscopy with Secondary Ion Mass Spectrometry for Nanoscale Chemical Imaging and Analysis of Polyolefins

Abstract

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Keywords

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