Environmental high-voltage S/TEM combined with a quadrupole mass spectrometer for concurrent <i>in situ</i> structural characterization and detection of product gas molecules associated with chemical reactions

Muto, Shunsuke; Arai, Shigeo; Higuchi, Tetsuo; Orita, Koji; Ohta, Shozo; Tanaka, Hiromochi; Suganuma, Takuya; Ibe, Masaya; Hirata, Hirohito

doi:10.1093/jmicro/dfy141

Cited by 9 publications

(16 citation statements)

References 8 publications

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“…Muto et al . [61] installed a quadrupole mass spectrometer (QMAS) (JEOL; JMS-1500GC) in the ‘big’ E-HVEM and obtained mass spectra during catalytic reactions of palladium (Pd) and rhodium (Rh) nanoparticles on ZrO 2 flakes in accordance with the in-situ high-resolution observations in the atmosphere of nitrogen monoxide (NO) gas.…”

Section: Various Kinds Of Application Resultsmentioning

confidence: 99%

Progress in environmental high-voltage transmission electron microscopy for nanomaterials

Tanaka

Fujita

Takahashi

et al. 2020

Phil. Trans. R. Soc. A.

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A new environmental high-voltage transmission electron microscope (E-HVEM) was developed by Nagoya University in collaboration with JEOL Ltd. An open-type environmental cell was employed to enable in-situ observations of chemical reactions on catalyst particles as well as mechanical deformation in gaseous conditions. One of the reasons for success was the application of high-voltage transmission electron microscopy to environmental (in-situ) observations in the gas atmosphere because of high transmission of electrons through gas layers and thick samples. Knock-on damages to samples by high-energy electrons were carefully considered. In this paper, we describe the detailed design of the E-HVEM, recent developments and various applications. This article is part of a discussion meeting issue ‘Dynamic in situ microscopy relating structure and function'.

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Section: Various Kinds Of Application Resultsmentioning

confidence: 99%

Progress in environmental high-voltage transmission electron microscopy for nanomaterials

Tanaka

Fujita

Takahashi

et al. 2020

Phil. Trans. R. Soc. A.

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“…By labeling with Au NPs or fluorescent quantum dots and binding them to features of interest, the spatial position, density, and arrangement of these electron-dense labels can provide significant insights into the corresponding positions and functions of the targeted intracellular structures , and resolving the dynamic structures of proteins and living cells . Similarly, a recent study reported the connection of mass spectrometry to ETEM (Figure g), realizing the real-time detection of gas species from oxidation of CNTs . Such design may open more opportunities to the deeper investigation into reactions such as alcohol oxidation and the Fischer–Tropsch process, and the combination of mass spectrometry (and even NMR, high-performance liquid chromatography) with liquid-phase EM can be expected.…”

Section: Discussionmentioning

confidence: 99%

“…448 The pressure inside the gas cell can even reach ambient pressure, which is much higher than that in ETEM, and thus the reaction condition in the gas cell can be closer to that in practical applications. Both techniques can be combined with heating functions, and even connected to a mass spectrometer 450 to enable the simultaneous detection of gas products during chemical reactions, correlating nanomaterials' structures with their catalytic performance. Aside from real-space imaging, electron diffraction patterns can also be recorded in situ to track the fast-speed structural and compositional change of NPs during reactions.…”

Section: Othermentioning

confidence: 99%

Electron Microscopy Studies of Soft Nanomaterials

et al. 2023

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This review highlights recent efforts on applying electron microscopy (EM) to soft (including biological) nanomaterials. We will show how developments of both the hardware and software of EM have enabled new insights into the formation, assembly, and functioning (e.g., energy conversion and storage, phonon/photon modulation) of these materials by providing shape, size, phase, structural, and chemical information at the nanometer or higher spatial resolution. Specifically, we first discuss standard real-space two-dimensional imaging and analytical techniques which are offered conveniently by microscopes without special holders or advanced beam technology. The discussion is then extended to recent advancements, including visualizing three-dimensional morphology of soft nanomaterials using electron tomography and its variations, identifying local structure and strain by electron diffraction, and recording motions and transformation by in situ EM. On these advancements, we cover state-of-the-art technologies designed for overcoming the technical barriers for EM to characterize soft materials as well as representative application examples. The even more recent integration of machine learning and its impacts on EM are also discussed in detail. With our perspectives of future opportunities offered at the end, we expect this review to inspire and stimulate more efforts in developing and utilizing EM-based characterization methods for soft nanomaterials at the atomic to nanometer length scales in academic research and industrial applications.

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“…Muto et al employed an ETEM equipped with a quadrupole mass spectrometer (QMS) to detect product gas species during the chemical reactions occurring in the TEM column, which allows operando characterization of the catalytic reactions. In this work, they demonstrated the direct correlation between the detected gas species and atomic structural evolutions of catalysts during the redox reactions under reactive conditions.…”

Section: In Situ Tem On Catalytic Gas Reactionmentioning

confidence: 99%

Section: In Situ Tem On Catalytic Gas Reactionmentioning

confidence: 99%

In Situ Transmission Electron Microscopy on Energy‐Related Catalysis

Hwang

Chen

Zhou

et al. 2019

Advanced Energy Materials

106

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Energy‐related catalytic reactions have been extensively investigated in past years in order to efficiently utilize clean and environmentally benign energy sources. In these systems, the catalysts and the catalyst/active medium interfaces play a crucial role in determining their performance. Thus, understanding the physical and chemical properties of catalysts during reactions is of importance to provide fundamental insights for designing the devices. Transmission electron microscopy can provide tremendous information regarding materials' morphology, microstructure, and chemical properties at nanoscales. With in situ electron microscopy, dynamic processes of catalytic reactions in both gas and liquid environments have been investigated in real time. In this paper, the recent research progress of in situ and operando electron microscopy techniques are introduced with the representative works in energy‐related reactions, including electrochemical catalysis in liquid media and heterogeneous catalysis in gas media. The uniqueness of the specific electron microscopy methods and scientific merits of each work are highlighted. Finally, outlooks on emerging research opportunities are discussed.

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Environmental high-voltage S/TEM combined with a quadrupole mass spectrometer for concurrent in situ structural characterization and detection of product gas molecules associated with chemical reactions

Cited by 9 publications

References 8 publications

Progress in environmental high-voltage transmission electron microscopy for nanomaterials

Progress in environmental high-voltage transmission electron microscopy for nanomaterials

Electron Microscopy Studies of Soft Nanomaterials

In Situ Transmission Electron Microscopy on Energy‐Related Catalysis

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