Ultra-Low kV EDS – A New Approach to Improved Spatial Resolution, Surface Sensitivity, and Light Element Compositional Imaging and Analysis in the SEM

Burgess, Simon; Sagar, James; Holland, J.; Li, Xiaobing; Bauer, Frank

doi:10.1017/s1551929517000013

Cited by 33 publications

(13 citation statements)

References 11 publications

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“…Since low-voltage EDS is useful to achieve high-resolution chemical mapping and to obtain efficient chemical spectra in low ionization energy ranges, its demand is increasing in the fields of surface analysis and light element analysis (Burgess et al, 2017). In this study, we confirmed that the electron source is very important for signal acquisition.…”

Section: Comparison Of Eds Data For Oxygensupporting

confidence: 67%

Development of SEM and STEM-in-SEM grid holders for EDS analysis and their applications to apatite phases

Kwon

Kim

Kim³

et al. 2019

J Anal Sci Technol

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Background: With the application of the scanning transmission electron microscopy (STEM) detector, transmitted electron images similar to transmission electron microscopy (TEM) can be obtained from scanning electron microscopy (SEM), which is referred to STEM-in-SEM imaging. Compared to TEM-energy dispersive spectroscopy (EDS), SEM-EDS is expected to be more efficient and reliable for chemical analysis of TEM specimens due to the larger sample space in SEM and the higher takeoff angle of the SEM-EDS detector. Unfortunately, this advantage is not well applied to TEM specimens in practice, mainly because of fault signals generated from the commercial grid holders used in SEM and STEM-in-SEM. This study is designed to solve this problem by modifying the commercial holders and to test them through EDS analysis of apatite phases. Findings: We first changed the way of assembling parts of the commercial multi-grid holder for SEM. This new assembly was capable of producing a thinner upper cover part, resulting in the reduction of the EDS fault signals generated from the holder. Furthermore, the thin upper part allowed us to get images in shorter working distances, that is, at higher magnifications. This design concept was also applied to the commercial single-grid holder for STEM-in-SEM, producing a new multi-grid holder to be used for loading multiple samples. Conclusion: We confirmed that the new holders produced reliable chemical data from apatite phases. In case of oxygen analysis, despite of low electron brightness from the tungsten source, 5 kV provided more stable acquisition and signal yields than 15 kV. We expect that these modified holders facilitate more efficient EDS analysis for multiple samples under the same analytical conditions in SEM and STEM-in-SEM.

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Section: Comparison Of Eds Data For Oxygensupporting

confidence: 67%

Development of SEM and STEM-in-SEM grid holders for EDS analysis and their applications to apatite phases

Kwon

Kim

Kim³

et al. 2019

J Anal Sci Technol

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“…SEM microscopy reveals that the secondary phase consists of particle and needle-like structures that emerge in both the grain boundaries and grain interiors ( Figure 4(a)). Low voltage EDS [14] (3 kV accelerating voltage) confirms that these structures are Cu-rich (Figure 4(b)). STEM was performed on a FIBed foil of SPS700 after being sequentially heat treated at T HT = 450, 500, and 550°C for 2 h at each temperature.…”

Section: Resultsmentioning

confidence: 74%

Entropic phase transformation in nanocrystalline high entropy oxides

Dupuy

Wang

Schoenung

2018

Materials Research Letters

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High entropy oxide (HEO) materials display a reversible entropy-driven phase transformation that gives rise to a phase state consisting of the entropic single-phase and controllable volume fractions of a secondary phase, which we call the 'phase spectrum'. Consolidated HEO samples were prepared with grain sizes spanning several orders of magnitude and were heat treated to demonstrate the dramatic effect that grain size has on controlling the phase spectrum behavior. The volume fraction and morphology of the secondary phase, determined here to be a Cu-rich multicomponent tenorite phase, and the corresponding heat treatment conditions were significantly influenced by the grain size. IMPACT STATEMENTNanocrystalline high entropy oxides (HEOs) exhibit a wider phase transformation temperature window, as well as changes to the concentration and morphology of the secondary phase, a Cu-rich multicomponent tenorite phase. ARTICLE HISTORY

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“…The behavior is different for cathodoluminescence. The throughput count rate is about the same for all shaping times (see figure [8][9]. Note that because of variations in the filament brightness, the curves are plotted as a function of iodine count rate.…”

Section: Process Timementioning

confidence: 97%

“…In the middle of 2000s came silicon drift detectors, which work at higher temperature and higher count rates [1][2][3]. During the last 20 years, silicon drift detectors were improved [4][5]: increase of sensor active area [6], new geometries decreasing detector -specimen distance [7][8] and new materials for the window or windowless detectors [4,[9][10] allowed to improve the spatial resolution and the detection of low energy X-rays. EDX detectors are made from silicon, a material in which X-ray photons but also visible light can create electron-hole pairs, which are further collected to give the useful signal.…”

Section: Introductionmentioning

confidence: 99%

Study on the Use of Silicon Drift Detector to Get Information on Light Emitted by Luminescent Materials

Béranger¹

2019

AJPA

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Energy dispersive X-Ray detectors are among the most common tools installed on scanning electron microscopes and, as they are sensitive to light, they can be used to get panchromatic cathodoluminescence information. This article presents practical considerations about the parameters to choose to obtain a good cathodoluminescence signal on a silicon drift detector. Probe current is the most important but other parameters of electron microscope and energy dispersive X-Ray detector are also explored. Filament brightness, if not fixed, influences the number of electrons incident on the sample and modifies cathodoluminescence response. Beam voltage and working distance must be adapted to the sample and to the electron microscope geometry. Acquisition and shaping times are important parameters for spectrum quality: the high sensitivity of silicon drift detector to light allows the use of low acquisition times and high shaping times. As cathodoluminescent materials are mostly high band gap materials, charge effects can influence their response and the size of the acquisition area must be carefully chosen. The influence of all these parameters is studied through two scintillating materials. Some examples of application are described to show the potential of this method. They include localization of luminescent particles, a demonstration of the effect of strong electron beam on a needle of material and the characterization of light emitted by a structural defect in a scintillator material.

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Ultra-Low kV EDS – A New Approach to Improved Spatial Resolution, Surface Sensitivity, and Light Element Compositional Imaging and Analysis in the SEM

Cited by 33 publications

References 11 publications

Development of SEM and STEM-in-SEM grid holders for EDS analysis and their applications to apatite phases

Development of SEM and STEM-in-SEM grid holders for EDS analysis and their applications to apatite phases

Entropic phase transformation in nanocrystalline high entropy oxides

Study on the Use of Silicon Drift Detector to Get Information on Light Emitted by Luminescent Materials

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