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Published May 1, 2019 | Supplemental Material
Journal Article Open

Local Structure and Bonding of Carbon Nanothreads Probed by High-Resolution Transmission Electron Microscopy

Abstract

Carbon nanothreads are a new one-dimensional sp^3-bonded nanomaterial of CH stoichiometry synthesized from benzene at high pressure and room temperature by slow solid-state polymerization. The resulting threads assume crystalline packing hundreds of micrometers across. We show high-resolution electron microscopy (HREM) images of hexagonal arrays of well-aligned thread columns that traverse the 80–100 nm thickness of the prepared sample. Diffuse scattering in electron diffraction reveals that nanothreads are packed with axial and/or azimuthal disregistry between them. Layer lines in diffraction from annealed nanothreads provide the first evidence of translational order along their length, indicating that this solid-state reaction proceeds with some regularity. HREM also reveals bends and defects in nanothread crystals that can contribute to the broadening of their diffraction spots, and electron energy-loss spectroscopy confirms them to be primarily sp^3-hybridized, with less than 27% sp^2 carbon, most likely associated with partially saturated "degree-4" threads.

Additional Information

© 2019 American Chemical Society. Received: December 21, 2018; Published: April 5, 2019. We acknowledge the Energy Frontier Research in Extreme Environments (EFree) Center, an Energy Frontier Research Center funded by the Department of Energy (DOE) Office of Science (DE-SC0001057). We also acknowledge support from the Center for Nanothread Chemistry (CNC), funded by the National Science Foundation (CHE-1832471). Samples were synthesized at the Spallation Neutrons and Pressure (SNAP) beamline at the Spallation Neutron Source, a DOE Office of Science User Facility operated by Oak Ridge National Laboratory, and the High-Pressure Neutron Diffractometer (PLANET) beamline at the Japan Proton Accelerator Research Complex. TEM was performed at the Materials Characterization Laboratory (MCL) in the Materials Research Institute (MRI) at the Pennsylvania State University. We acknowledge Dr. Ke Wang for his advice and assistance in performing TEM for this work. The authors declare no competing financial interest.

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