Parameters affecting the accuracy of nanoparticle shape and size measurement in 3D

Hayashida, Misa; Cui, Kai; Homeniuk, Darren; Phengchat, Rinyaporn; Blackburn, Arthur M.; Malac, Marek

doi:10.1016/j.micron.2019.102680

Cited by 13 publications

(6 citation statements)

References 24 publications

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“…Therefore, t was only measured from the right side of the sample marked by red shading in Figure 2c. All steps, such as thresholding, cross- 8 Although the Simultaneous Iterative Reconstruction Technique (SIRT) is frequently used to increase contrast and visual presentation of electron tomography reconstructions, FBP is preferable when extracting sample shape from reconstructed images by thresholding (Hayashida & Malac, 2016;Hayashida et al, 2019Hayashida et al, , 2021. 9…”

Section: Image Processing For Thickness Measurementmentioning

confidence: 99%

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High-Energy Electron Scattering in Thick Samples Evaluated by Bright-Field Transmission Electron Microscopy, Energy-Filtering Transmission Electron Microscopy, and Electron Tomography

Hayashida

Malac

2022

Microsc Microanal

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Energy-filtering transmission electron microscopy (TEM) and bright-field TEM can be used to extract local sample thickness $t$ and to generate two-dimensional sample thickness maps. Electron tomography can be used to accurately verify the local $t$ . The relations of log-ratio of zero-loss filtered energy-filtering TEM beam intensity ( $I_{{\rm ZLP}}$ ) and unfiltered beam intensity ( $I_{\rm u}$ ) versus sample thickness $t$ were measured for five values of collection angle in a microscope equipped with an energy filter. Furthermore, log-ratio of the incident (primary) beam intensity ( $I_{\rm p}$ ) and the transmitted beam $I_{{\rm tr}}$ versus $t$ in bright-field TEM was measured utilizing a camera before the energy filter. The measurements were performed on a multilayer sample containing eight materials and thickness $t$ up to 800 nm. Local thickness $t$ was verified by electron tomography. The following results are reported: • The maximum thickness $t_{{\rm max}}$ yielding a linear relation of log-ratio, $\ln ( {I_{\rm u}}/{I_{{\rm ZLP}}})$ and $\ln ( {I_{\rm p}}/{I_{{\rm tr}}} )$ , versus $t$ . • Inelastic mean free path ( $\lambda _{{\rm in}}$ ) for five values of collection angle. • Total mean free path ( $\lambda _{{\rm total}}$ ) of electrons excluded by an angle-limiting aperture. • $\lambda _{{\rm in}}$ and $\lambda _{{\rm total}}$ are evaluated for the eight materials with atomic number from $\approx$ 10 to 79. The results can be utilized as a guide for upper limit of $t$ evaluation in energy-filtering TEM and bright-field TEM and for optimizing electron tomography experiments.

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Section: Image Processing For Thickness Measurementmentioning

confidence: 99%

“… 8 Although the Simultaneous Iterative Reconstruction Technique (SIRT) is frequently used to increase contrast and visual presentation of electron tomography reconstructions, FBP is preferable when extracting sample shape from reconstructed images by thresholding (Hayashida & Malac, 2016; Hayashida et al, 2019, 2021). …”

mentioning

confidence: 99%

High-Energy Electron Scattering in Thick Samples Evaluated by Bright-Field Transmission Electron Microscopy, Energy-Filtering Transmission Electron Microscopy, and Electron Tomography

Hayashida

Malac

2022

Microsc Microanal

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“…It should be noted that the particle size refers to the maximum Feret diameter, as the nanoparticles are nonspherical. [51] The dynamic light scattering method allows to determine the hydrodynamic diameter of nanoparticles. It can be assumed that the hydrodynamic diameter of particles can be comparable with the maximum Feret diameter for nonspherical nanoparticles.…”

Section: The Characteristics Of Molybdenum Oxide Nanoparticlesmentioning

confidence: 99%

Plasma‐assisted synthesis and deposition of molybdenum oxide nanoparticles on polyethylene terephthalate for photocatalytic degradation of rhodamine B

Sirotkin

Khlyustova

Титов

et al. 2020

Plasma Processes & Polymers

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In this study, an atmospheric pressure glow discharge initiated between the metal molybdenum anode and the liquid cathode is applied to produce molybdenum oxide nanoparticles, which are deposited on a polyethylene terephthalate substrate. The presence of nanoparticles in the liquid solution is confirmed by ultraviolet‐vis absorbance spectroscopy and the dynamic light scattering method. The obtained composites are characterized by methods of scanning electron microscopy, infrared spectroscopy, and X‐ray photoelectron spectroscopy. The efficiency of the obtained composite as a photocatalyst is investigated. The composite demonstrates a high photocatalytic performance, ~100% dye removal in 30 min during five cycles of use.

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“…nanoparticles or pores in different materials. [19][20][21][22][23][24] While high-angle annular dark-field (HAADF) imaging 25 clearly distinguishes Pt grains from the carbon matrix, sequential image acquisition at tilt angles from 5 -90° to + 90° paves the way for a 3D reconstruction. 25 Thereby, we receive information about the shape, size and spatial distribution of Pt grains within the Pt-C nano-pillars.…”

mentioning

confidence: 99%

“…The 3D printing of nanoobjects via FEBID has undergone significant progress in the past few years, which has opened up new possibilities for various applications such as plasmonics, nanomagnetics, gas sensors, or nanoprobe concepts . For studying the shapes, sizes, and distribution of, e.g., nanoparticles or pores in different materials, electron tomography in a scanning transmission electron microscope is often used. − While high-angle annular dark-field (HAADF) imaging clearly distinguishes Pt grains from the C matrix, sequential image acquisition at tilt angles from −90° to +90° paves the way for 3D reconstruction . The combination of Z-sensitive imaging and sample tilting makes it possible to receive the shape, size, and spatial distribution of Pt grains within the Pt–C nanopillars.…”

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confidence: 99%

Analyzing the Nanogranularity of Focused-Electron-Beam-Induced-Deposited Materials by Electron Tomography

Trummer

Winkler

Plank

et al. 2019

ACS Appl. Nano Mater.

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Nanogranular material systems are promising for a variety of applications in research and development. Their physical properties are often determined by grain sizes, shapes, mutual distances and by the chemistry of the embedding matrix With focused electron beam induced deposition arbitrarily shaped nanocomposite materials can be designed, where metallic, nanogranular structures are embedded in a carbonaceous matrix. Using "post-growth" electron beam curing, these materials can be tuned for improved electric transport or mechanical behavior.Such an optimization necessitates a thorough understanding and characterization of the internal changes in chemistry and morphology, which is where conventional projection based imaging techniques fall short. Here, we apply scanning transmission electron tomography to get a comprehensive picture of the distribution and morphology degree of embedded Pt nanograins after initial fabrication, and we demonstrate the impact of electron beam curing, which leads to condensed regions of interconnected metal nanograins.

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Parameters affecting the accuracy of nanoparticle shape and size measurement in 3D

Cited by 13 publications

References 24 publications

High-Energy Electron Scattering in Thick Samples Evaluated by Bright-Field Transmission Electron Microscopy, Energy-Filtering Transmission Electron Microscopy, and Electron Tomography

High-Energy Electron Scattering in Thick Samples Evaluated by Bright-Field Transmission Electron Microscopy, Energy-Filtering Transmission Electron Microscopy, and Electron Tomography

Plasma‐assisted synthesis and deposition of molybdenum oxide nanoparticles on polyethylene terephthalate for photocatalytic degradation of rhodamine B

Analyzing the Nanogranularity of Focused-Electron-Beam-Induced-Deposited Materials by Electron Tomography

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