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Nanoscale Cathodoluminescence Thermometry with a Lanthanide-Doped Heavy-Metal Oxide in Transmission Electron Microscopy

  • Won-Woo Park
    Won-Woo Park
    Department of Chemistry, College of Natural Sciences, Ulsan National Institute of Science and Technology (UNIST), Ulsan 44919, Republic of Korea
    More by Won-Woo Park
  • Pavel K. Olshin
    Pavel K. Olshin
    Department of Chemistry, College of Natural Sciences, Ulsan National Institute of Science and Technology (UNIST), Ulsan 44919, Republic of Korea
  • Ye-Jin Kim
    Ye-Jin Kim
    Department of Chemistry, College of Natural Sciences, Ulsan National Institute of Science and Technology (UNIST), Ulsan 44919, Republic of Korea
    More by Ye-Jin Kim
  • Hak-Won Nho
    Hak-Won Nho
    Department of Chemistry, College of Natural Sciences, Ulsan National Institute of Science and Technology (UNIST), Ulsan 44919, Republic of Korea
    More by Hak-Won Nho
  • Daria V. Mamonova
    Daria V. Mamonova
    St. Petersburg State University, St. Petersburg 199034, Russia
  • Ilya E. Kolesnikov
    Ilya E. Kolesnikov
    St. Petersburg State University, St. Petersburg 199034, Russia
  • Vassily A. Medvedev
    Vassily A. Medvedev
    St. Petersburg State University, St. Petersburg 199034, Russia
  • , and 
  • Oh-Hoon Kwon*
    Oh-Hoon Kwon
    Department of Chemistry, College of Natural Sciences, Ulsan National Institute of Science and Technology (UNIST), Ulsan 44919, Republic of Korea
    *Email for O.-H.K.: [email protected]
    More by Oh-Hoon Kwon
Cite this: ACS Nano 2024, 18, 6, 4911–4921
Publication Date (Web):January 30, 2024
https://doi.org/10.1021/acsnano.3c10020
Copyright © 2024 American Chemical Society

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    Abstract

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    When navigated by the available energy of a system, often provided in the form of heat, physical processes or chemical reactions fleet on a free-energy landscape, thus changing the structure. In in situ transmission electron microscopy (TEM), where material structures are measured and manipulated inside the microscope while being subjected to external stimuli such as electrical fields, laser irradiation, or mechanical stress, it is necessary to precisely determine the local temperature of the specimen to provide a comprehensive understanding of material behavior and to establish the relationship among energy, structure, and properties at the nanoscale. Here, we propose using cathodoluminescence (CL) spectroscopy in TEM for in situ measurement of the local temperature. Gadolinium oxide particles doped with emissive europium ions present an opportunity to utilize them as a temperature probe in CL measurements via a ratiometric approach. We show the thermometric performance of the probe and demonstrate a precision of ±5 K in the temperature range from 113 to 323 K with the spatial resolution limited by the size of the particles, which surpasses other methods for temperature determination. With the CL-based thermometry, we further demonstrate measuring local temperature under laser irradiation.

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    The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acsnano.3c10020.

    • Normalized cathodoluminescence (CL) spectra of Gd2O3:Eu3+ recorded at different temperatures, model relaxation kinetics and ratiometric approach on the intensities of 5D bands of Eu3+, modified model relaxation kinetics and relation of the CL intensities of the 5D1 and 5D0 bands to temperature, comparison between cathodoluminescence and photoluminescence spectra, normalized CL spectra of Gd2O3:Eu3+ recorded at different electron-dose rates at 113 K, temperature-dependent CLIR of the 5D27F1 to 5D17F1 transitions measured at an electron-dose rate of 0.2 e nm–2 s–1, difference in the temperature (ΔT) determined via CL-TEM nanothermometry and the reading of the temperature-controlled specimen holder at different temperatures shown in Figure 6b and the inset of Figure 6c, temperature-dependent CLIR of the 5D1–F1 to 5D0–F1 transitions obtained at an electron-dose rates of 10 and 200 e nm–2 s–1, and TEM image and CL-intensity map of a single Gd2O3:Eu3+ particle (PDF)

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