The First Results of the Low Voltage Cold-FE SEM/STEM System Equipped With EELS

Yamazawa, Yu; Okada, Satoshi; Yasenjiang, Zulihuma; Sunaoshi, Takeshi; Kaji, Kazutoshi

doi:10.1017/s1431927616001100

Cited by 17 publications

(10 citation statements)

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“…Despite the stark differences between these types of instruments, recent years have seen increased adaptation of transmission-based techniques for use in SEMs, including scanning-transmission electron microscopy (STEM) imaging, low-energy nanodiffraction [3], transmission Kikuchi diffraction [4], and even electron energy loss spectroscopy (EELS) [5]. Since SEMs are often more financially and logistically accessible for smaller laboratories, development of crossover techniques enables a wider range of researchers to collect information obtainable only via transmission experiments.…”

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confidence: 99%

Quantitative SEM-EDS Analysis of Semi-Transparent Samples

Boona

2021

Micros. Today

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Section: Introductionmentioning

confidence: 99%

Quantitative SEM-EDS Analysis of Semi-Transparent Samples

Boona

2021

Micros. Today

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“…The high resolution imaging is complemented by two analytical systems: electron energy loss spectrometry (EELS) and energy dispersive spectrometry (EDS). Examples of low voltage EELS were previously presented to validate the possibility of low voltage EELS [1,2]. Figure 3 shows an example of high resolution x-ray EDS microanalysis.…”

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confidence: 96%

“…Examples of low voltage EELS were previously presented to validate the possibility of low voltage EELS [1,2]. Figure 3 shows an example of high resolution x-ray EDS microanalysis.…”

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Low Accelerating Voltage Scanning Transmitted Electron Microscope: Imaging, Diffraction, X-ray Microanalysis, and Electron Energy-Loss Spectroscopy at the Nanoscale

2017

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For developing new technologies, it is important to characterize materials at the nanoscale. To achieve high resolution, a field emission scanning electron microscope (FE-SEM) with low voltage scanning transmitted electron microscope mode (STEM) was developed. The HITACHI SU-9000 provides low accelerating voltage, deceleration mode, and energy-filtering of the electron signals (secondary and backscattered electrons), low voltage STEM bight-field (BF) and dark-field (DF) imaging capability are possible on these instruments to allow the characterization of materials at the nanoscale with various types of contrasts. Furthermore, the instrument has diffraction analysis, electron energy loss spectrometry (EELS), and energy dispersive spectrometry (EDS) systems, which allow crystallographic and chemical characterization at the nanoscale materials. Figure 1 shows an example of high resolution imaging of an AA 2099 Al-Li alloy in BF and DF imaging modes at low voltage (30 kV). One of the advantages of the low accelerating voltage used is the increase of the contrast observed, which is very important when the characterized phases containing lithium and the difference in mass density is very small. Another problem with Li alloy is the electron probe damage, which is minimized when using low accelerating voltage by reducing the electron dose. The high resolution imaging is complemented by two analytical systems: electron energy loss spectrometry (EELS) and energy dispersive spectrometry (EDS). Examples of low voltage EELS were previously presented to validate the possibility of low voltage EELS [1,2]. Figure 3 shows an example of high resolution x-ray EDS microanalysis. A line scan across a T1 precipitate in an AA 2099 Al-Li alloy was recorded. The spatial resolution on the DF micrograph is between 2.0 and 2.5 nm and around 3.0 nm on the x-ray line scan. The low concentration of Zn in the T1 (Al2CuLi) was clearly observed. Furthermore, the decrease of Al concentration in the T1 phase versus the Al matrix was also observed. We are currently working to acquire EELS and EDS data simultaneously to clearly observe the complete composition of each Al-Li alloy phase as the low concentration Zn cannot be detected with EELS [5] and Li is difficult to detect with EDS.These examples show the high resolution imaging and analysis possibility of low voltage STEM of instrument like SU-9000 for characterization of nanoscale materials and also minimizing the electron probe damage by reducing the dose used.

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“…Examples of low voltage EELS were previously presented to validate the possibility of low voltage EELS [3,4]. This instrument have three sensors for energy-filtering imaging.…”

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The Joy of Nanoscale Imaging and Spectroscopy in a Low Accelerating Voltage Scanning Transmitted Electron Microscope

et al. 2018

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For developing new technologies, it is important to characterize materials at the nanoscale. To achieve high resolution, a field emission scanning electron microscope (FE-SEM) with low voltage scanning transmitted electron microscope mode (STEM) was recently developed. The HITACHI SU-9000 provides low accelerating voltage, deceleration mode, and energy-filtering of the electron signals (secondary and backscattered electrons), low voltage STEM bight-field (BF) and dark-field (DF) imaging capability are possible on this instrument to allow the characterization of materials at the nanoscale with various types of contrasts. Furthermore, the instrument has diffraction analysis, electron energy loss spectrometry (EELS), and energy dispersive spectrometry (EDS) systems, which allow crystallographic and chemical characterization of materials nanostructures.Low accelerating voltage (30 kV) lattice imaging was demonstrated by Joy on a multi wall carbon nanotube in BF mode [1]. A later study has explained the method and gave other materials examples [2]. Figure 1 shows a lattice image of a rutile TiO2 specimen. The Fourier transform of the lattice fringes indicates a distance of 0.34 nm for the dark grain and 0.35 nm for the bright grain. The lattice is not present for all grains as the condition for lattice visibility depends on the defocus and the lattice spacing. For a specific defocus value, only a range of lattice spacing value is visible, which explain why the two grains have similar lattice spacing.The high resolution imaging is complemented by two analytical systems: electron energy loss spectrometry (EELS) and energy dispersive spectrometry (EDS). Examples of low voltage EELS were previously presented to validate the possibility of low voltage EELS [3,4]. This instrument have three sensors for energy-filtering imaging. Using the same conditions as used in Figure 1, an energy-filtered lattice image was obtained as shown in Figure 2. Energy filtering improves the contrast of the bright-field image. In Figure 2, the micrograph was formed using electrons with the energy loss of the surface plasmon ( Fig.2A) and the volume plasmon (Fig.2B). The surface plasmon micrograph shows a bright contrast at the edge of the specimen while the volume plasmon micrograph shows a better contrast across the full range of thickness of the specimen. We are presently developing simultaneous acquisition of EELS and EDS spectra to correctly characterize the specimen composition by combining these two complementary techniques.These examples show the high resolution imaging and analysis possibilities of low voltage STEM obtained with an instrument like the SU-9000 for characterizing materials at the nanoscale, while at the same time minimizing the electron probe damage by reducing the dose used.

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The First Results of the Low Voltage Cold-FE SEM/STEM System Equipped With EELS

Cited by 17 publications

References 4 publications

Quantitative SEM-EDS Analysis of Semi-Transparent Samples

Quantitative SEM-EDS Analysis of Semi-Transparent Samples

Low Accelerating Voltage Scanning Transmitted Electron Microscope: Imaging, Diffraction, X-ray Microanalysis, and Electron Energy-Loss Spectroscopy at the Nanoscale

The Joy of Nanoscale Imaging and Spectroscopy in a Low Accelerating Voltage Scanning Transmitted Electron Microscope

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