Solid-State Energy-Dispersion Spectrometer for Electron-Microprobe X-ray Analysis

Fitzgerald, R. W.; Keil, K.; Heinrich, Kurt F. J.

doi:10.1126/science.159.3814.528

Cited by 138 publications

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“…On February 2, 1968, Fitzgerald, Keil and Heinrich [1] described, in a seminal paper in Science, a solidstate Si(Li) energy dispersive spectrometer (EDS) for electron probe microanalysis (EPMA) with an initial resolution of 600 eV. This tool, for the first time, allowed energy dispersion of X-rays of ~ 3-30 keV and separation of characteristic X-ray peaks of elements adjacent in the Periodic Chart with atomic numbers 20 and higher in complex X-ray spectra.…”

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“…3 shows a composite of pure element K and L X-ray spectra obtained with the original solid-state Si(Li) energy dispersive spectrometer (EDS) with a resolution of 600 eV of [1], mounted in an existing X-ray port in an ARL EPMA. By comparison to the performance of modern solid-state EDS devices, the performance of the spectrometer by [1] seems archaic, but it was an exciting and seminal step forward in the detection of x-rays in a host of analytical devices, including the EPMA. Figure 1 (upper left).…”

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“…This talk and paper is dedicated to my friend, Ray Fitzgerald ( Fig. 1), who really was the brains behind our 1968 Science paper [1]. Image ca.…”

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The Beginnings of EDS in EPMA

Keil

2018

Microsc Microanal

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On February 2, 1968, Fitzgerald, Keil and Heinrich [1] described, in a seminal paper in Science, a solidstate Si(Li) energy dispersive spectrometer (EDS) for electron probe microanalysis (EPMA) with an initial resolution of 600 eV. This tool, for the first time, allowed energy dispersion of X-rays of ~ 3-30 keV and separation of characteristic X-ray peaks of elements adjacent in the Periodic Chart with atomic numbers 20 and higher in complex X-ray spectra. This spectrometer ushered in a new era not only in EPMA, but also in SEM, ATEM, XRD and XRF.Theirs was not the first attempt in using energy dispersive spectroscopy to detect X-Rays. Earlier attempts were mostly made using the rather limited energy resolution of ~1.3-1.8 keV for CuKα radiation of gas-filled proportional counters [2]. For example, Dolby [3] used a flow-proportional counter to obtain signals for the K-bands of boron, carbon, nitrogen, and oxygen; Duncumb [4] built an electron microscope microanalyzer (EMMA) that combined a TEM with an EPMA and featured a gasfilled proportional counter to detect X-rays; and, similarly, Birks and Batt [5] also used gas-filled proportional counters in conjunction with a 400 channel pulse height analyzer in an EPMA. However, while these results were discouraging, [5] made a visionary statement: "The possible applications of EDS to X-ray spectro-chemical analyses are unlimited." Finally, Bowman et al. [6] used what they refer to as a "high-resolution" solid-state semiconductor Si(Li) detector for the detection of X-rays in an XRF apparatus with a resolution of 1.1 keV, still insufficient to resolve the Kα X-ray lines of neighboring elements in the Periodic Chart. However, [6] noted that such devices had a great future in all fields where X-rays were to be detected and, specifically, pointed to the EPMA, noting that "the semiconductor X-ray spectrometer would be an excellent device for analysis of this radiation."What inspired [1] to develop their solid-state Si(Li) EDS for EPMA? Fitzgerald (Fig. 1) attended a talk at Stanford University in 1965 on the use of a solid-state ionization chamber used in conjunction with a multichannel analyzer for energy dispersive analysis. That prompted him to work with F.J. Walter and R.C. Trammel of ORTEC to develop an EDS (Fig. 2) that had sufficient energy resolution of 600 eV in the X-ray range to be of practical analytical use. The spectrometer consisted of a nitrogen-cooled lithium-drifted silicon diode, a low-noise preamplifier (ORTEC 116), a linear amplifier (ORTEC 440), a 1024 multi-channel analyzer (Nuclear Data 2200), and a read-out device such as a high-speed printer. The detector was mounted inside a separate vacuum chamber, isolated from the main vacuum chamber of the ARL EPMA by a 0.125 mm Be window. Fig. 3 shows a composite of pure element K and L X-ray spectra obtained with the original solid-state Si(Li) energy dispersive spectrometer (EDS) with a resolution of 600 eV of [1], mounted in an existing X-ray port in an ARL EPMA. By comparison to the performance of modern...

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The Beginnings of EDS in EPMA

Keil

2018

Microsc Microanal

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“…The Si(Li) energy-dispersive spectroscopy (EDS) X-ray detector was the industry standard from the inception of its use on electron microscopes [1]. Since then silicon drift detectors (SDDs) have been introduced [2], and these are currently the X-ray detector of choice across most fields and industries.…”

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Improvements in SDD Efficiency – From X-ray Counts to Data

Nylese¹,

Rafaelsen²

2017

Micros. Today

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Continuing advancements in window materials, detector modules, and electronics are leading to higher count rates, better light-element sensitivity, and improved energy-resolution stability over a wide range of count rates. In this article we will briefly review how the different parts of the EDS system interact, from X-rays leaving the sample to the production of useful data and where recent changes have taken place. We then apply the gains offered by this new technology to three samples to illustrate the benefits that can be reaped.

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“…Within another 5 years, other commercial electron microprobes were developed, and an electron-beam rastering capability was also developed to provide compositional distribution imaging, and soon thereafter, a commercial SEM. Another major development came in 1968, with the introduction of a solid-state Si(Li) or lithium-drifted silicon detector [2,3] for rapid qualitative analysis. And within a few more years, the development of thin windows for X-ray detectors extended the method to low-energy Xrays and light-element analysis.…”

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Historical and Current Importance of Electron Probe Microanalysis in Space Sciences, A Retro- and Forward-looking Perspective

Jolliff

Carpenter

2017

Microsc Microanal

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Electron Probe Microanalysis (EPMA) is today a mature analytical method used heavily in the investigation of meteoritic and planetary materials. EPMA is commonly the main analytical tool used to classify new meteorites by providing definitive information about mineral assemblage and quantitative mineral compositional data needed to specify a parent body or discern a grouping. EPMA is the main method used to provide detailed petrographic context for the materials that make up planetary suites such as lunar rocks and martian meteorites. Since the early days of Apollo sample investigations, EPMA has undergone numerous advances, leading to the diverse array of capabilities of modern instruments. In this paper, we provide a perspective on that progression of capabilities.

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Solid-State Energy-Dispersion Spectrometer for Electron-Microprobe X-ray Analysis

Cited by 138 publications

References 3 publications

The Beginnings of EDS in EPMA

The Beginnings of EDS in EPMA

Improvements in SDD Efficiency – From X-ray Counts to Data

Historical and Current Importance of Electron Probe Microanalysis in Space Sciences, A Retro- and Forward-looking Perspective

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