Ultrasoft-X-ray emission spectroscopy using a newly designed wavelength-dispersive spectrometer attached to a transmission electron microscope

Terauchi, Masami; Takahashi, Hiroki; Handa, Nobuo; Murano, T.; Koike, Masato; Kawachi, Tetsuya; Imazono, Takashi; Koeda, M.; Nagano, T.; Sasai, Hiroyuki; Oue, Y.; Yonezawa, Z.; Kuramoto, Satoshi

doi:10.1093/jmicro/dfr076

Cited by 61 publications

(24 citation statements)

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“…5,6 Therefore, the SXES will give very valuable information of bonding state while energy dispersive spectroscopy (EDS) can give unresolvable peaks or cannot detect signals in this energy range.…”

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confidence: 99%

Direct observation and analysis of yolk-shell materials using low-voltage high-resolution scanning electron microscopy: Nanometal-particles encapsulated in metal-oxide, carbon, and polymer

et al. 2014

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Nanometal particles show characteristic features in chemical and physical properties depending on their sizes and shapes. For keeping and further enhancing their features, the particles should be protected from coalescence or degradation. One approach is to encapsulate the nanometal particles inside pores with chemically inert or functional materials, such as carbon, polymer, and metal oxides, which contain mesopores to allow permeation of only chemicals not the nanometal particles. Recently developed low-voltage high-resolution scanning electron microscopy was applied to the study of structural, chemical, and electron state of both nanometal particles and encapsulating materials in yolk-shell materials of Au@C, Ru/Pt@C, Au@TiO2, and Pt@Polymer. Progresses in the following categories were shown for the yolk-shell materials: (i) resolution of topographic image contrast by secondary electrons, of atomic-number contrast by back-scattered electrons, and of elemental mapping by X-ray energy dispersive spectroscopy; (ii) sample preparation for observing internal structures; and (iii) X-ray spectroscopy such as soft X-ray emission spectroscopy. Transmission electron microscopy was also used for characterization of Au@C.

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confidence: 99%

Direct observation and analysis of yolk-shell materials using low-voltage high-resolution scanning electron microscopy: Nanometal-particles encapsulated in metal-oxide, carbon, and polymer

et al. 2014

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“…In our case we often select the energy range to allow Li-K (54 eV) X-rays to be observed using the 50XL reflection diffraction grating. Typically the 50XL grating has an operational energy range of 48 -180 eV [8]. However, in our system we can observe X-rays as low as 44 eV, which allows direct observation of the Mg L-line (49 eV) and up to 195 eV at the high end.…”

Section: Sxes Alignment and Calibrationmentioning

confidence: 95%

Soft X-ray and cathodoluminescence measurement, optimisation and analysis at liquid nitrogen temperatures

MacRae

Wilson

Torpy

et al. 2018

IOP Conf. Ser.: Mater. Sci. Eng.

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Abstract. Advances in field emission gun electron microprobes have led to significant gains in the beam power density and when analysis at high resolution is required then low voltages are often selected. The resulting beam power can lead to damage and this can be minimised by cooling the sample down to cryogenic temperatures allowing sub-micrometre imaging using a variety of spectrometers. Recent advances in soft X-ray emission spectrometers (SXES) offer a spectral tool to measure both chemistry and bonding and when combined with spectral cathodoluminescence the complementary techniques enable new knowledge to be gained from both mineral and materials. Magnesium and aluminium metals have been examined at both room and liquid nitrogen temperatures by SXES and the L-emission Fermi-edge has been observed to sharpen at the lower temperatures directly confirming thermal broadening of the X-ray spectra. Gains in emission intensity and resolution have been observed in cathodoluminescence for liquid nitrogen cooled quartz grains compared to ambient temperature quartz. This has enabled subtle growth features at quartz to quartz-cement boundaries to be imaged for the first time. IntroductionField emission gun equipped electron probe microanalysers (FEG-EPMA) offer high beam power density at a range of accelerating voltages, with excellent beam stability over days of operation. However, with high beam current densities the onset of specimen damage occurs faster [1]. It has been observed that destruction of the specimen and defect transformation is time dependent, and provided spectral measurements can be performed quickly enough, "undamaged" hyperspectral maps can be collected. To slow the onset of beam damage we have integrated a liquid nitrogen (LN) cold stage into a modern FEG-EPMA. The LN cold stage has been optimised for stage mapping, offering an advantage over normal cold stages in that large area maps up to several mm

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“…Their principal features are compared in Table 2. Table 3 Elemental range of analyzing crystals (9,20,22,23,70,71) WDS uses the Bragg reflection of X-ray emission dispersed from the lattice planes of an analyzing curved crystal (2d sin θ = nλ). Crystals with different lattice spacings (0.4-10 nm) ( Table 3) are used usually to analyze the whole wavelength range from below 0.1 nm (U Lα ≈ 0.091 nm) to above 11 nm (Be α ≈ 11.3 nm).…”

Section: X-ray Emission Spectrometry In the Transmission Electron Micmentioning

confidence: 99%

“…At the low-energy end of this spectrometer, Li Kα emission spectra with a peak at 54.1 eV were obtained with an energy resolution of 0.2 eV. (70,71) The spot irradiated by the electron beam on the specimen acts as an entrance slit, while the analyzing crystal and the exit slit are mounted on a Rowland circle. The lattice planes of the crystal are bent so that their radius is 2R and the crystal surface is ground to a radius R. Focusing allows a better separation of narrow characteristic lines and a solid angle of collection of nearly 10 −3 -10 −2 sr.…”

Section: X-ray Emission Spectrometry In the Transmission Electron Micmentioning

confidence: 99%

Electron Microscopy, Nanoscopy, and Scanning Micro‐ and NanoanalysisUpdate based on the original article by Vladimir Oleshko, Renaat Gijbels and Severin Amelinckx,Encyclopedia of Analytical Chemistry, © 2000, John Wiley & Sons, Ltd

Oleshko

Gijbels

Amelinckx

2013

Encyclopedia of Analytical Chemistry

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The article considers the history and stages of development of electron microscopy (EM) and scanning microanalysis, including theoretical aspects of electron beam–solid interactions, instrumentation, methodology of particular techniques and image analysis, sample preparation, and some typical applications as well. Major classes of EM techniques, i.e. stationary beam (transmission) and scanning beam EM methods, analytical electron microscopy (AEM), in situ EM, holography, and tomography are overviewed. In AEM, several imaging, diffraction, and analytical modes are integrated in a design to provide analytical synergism having obvious advantages over any single instrument. The subject of EM is to determine the morphology, crystallinity, defect structure, phase and elemental compositions, and electronic properties of a material using the focused electron beam and signals generated in the course of its interaction with the specimen. Various electron–specimen interactions generate a great deal of structural and analytical information in the form of emitted electrons and/or photons and internally produced signals, such as elastically and inelastically scattered electrons, Auger electrons (AEs), X‐rays, and cathodoluminescence (CL), which can be analyzed in different operating modes. Imaging of solid materials is essentially due to elastic scattering (diffraction) of electrons by the periodic arrangement of atoms in crystals (diffraction contrast) and/or interference of several diffracted and transmitted beams (phase contrast). High‐resolution imaging in scanning transmission mode is possible by using incoherently scattered electrons (Z‐contrast). Inelastic interactions form the basis for all chemical analytical techniques (energy‐dispersive (EDS) and wavelength‐dispersive (WDS) X‐ray spectroscopy, electron energy‐loss spectroscopy (EELS) energy‐filtering transmission electron microscopy (EFTEM), AE‐, and CL‐spectroscopy). The introduction of aberration‐corrected and monochromatic electron optics during the last decade opened a new era of nanoscopy and nanoanalysis at sub‐0.1 nm lateral resolution and sub‐electronvolt energy resolution levels with improved signal‐to‐noise ratio (SNR). Basic data characterizing the current state‐of‐the‐art and trends in development of electron nanoscopy and nanoanalysis are presented.

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Ultrasoft-X-ray emission spectroscopy using a newly designed wavelength-dispersive spectrometer attached to a transmission electron microscope

Cited by 61 publications

References 24 publications

Direct observation and analysis of yolk-shell materials using low-voltage high-resolution scanning electron microscopy: Nanometal-particles encapsulated in metal-oxide, carbon, and polymer

Direct observation and analysis of yolk-shell materials using low-voltage high-resolution scanning electron microscopy: Nanometal-particles encapsulated in metal-oxide, carbon, and polymer

Soft X-ray and cathodoluminescence measurement, optimisation and analysis at liquid nitrogen temperatures

Electron Microscopy, Nanoscopy, and Scanning Micro‐ and NanoanalysisUpdate based on the original article by Vladimir Oleshko, Renaat Gijbels and Severin Amelinckx,Encyclopedia of Analytical Chemistry, © 2000, John Wiley & Sons, Ltd

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