Electron-Excited Energy Dispersive X-Ray Spectrometry at High Speed and at High Resolution: Silicon Drift Detectors and Microcalorimeters

2006 ◽  
Vol 12 (6) ◽  
pp. 527-537 ◽  
Author(s):  
Dale E. Newbury

Two recent developments in X-ray spectrometer technology provide dramatic improvements in analytical capabilities that impact the frontiers of electron microscopy. Silicon drift detectors (SDD) use the same physics as silicon (lithium) energy dispersive spectrometers [Si(Li) EDS] but differ in design: only 10% of the thickness of the Si(Li) EDS with an anode area below 0.1 mm2 and a complex rear surface electrode pattern that creates a lateral internal charge collection field. The SDD equals or betters the Si(Li) EDS in most measures of performance. For output versus input count rate, the SDD exceeds the Si(Li) EDS by a factor of 5 to 10 for the same resolution. This high throughput can benefit analytical measurements that are count limited, such as X-ray mapping and trace measurements. The microcalorimeter EDS determines the X-ray energy by measuring the temperature rise in a metal absorber. Operating at 100 mK, the microcalorimeter EDS achieves resolution of 2–5 eV over a photon energy range of 200 eV to 10 keV in energy dispersive operation, eliminating most peak interference situations and providing high peak-to-background to detect low fluorescence yield peaks. Chemical bonding effects on low energy (<2 keV) peak shapes can be measured.

Author(s):  
Marc H. Peeters ◽  
Max T. Otten

Over the past decades, the combination of energy-dispersive analysis of X-rays and scanning electron microscopy has proved to be a powerful tool for fast and reliable elemental characterization of a large variety of specimens. The technique has evolved rapidly from a purely qualitative characterization method to a reliable quantitative way of analysis. In the last 5 years, an increasing need for automation is observed, whereby energy-dispersive analysers control the beam and stage movement of the scanning electron microscope in order to collect digital X-ray images and perform unattended point analysis over multiple locations.The Philips High-speed Analysis of X-rays system (PHAX-Scan) makes use of the high performance dual-processor structure of the EDAX PV9900 analyser and the databus structure of the Philips series 500 scanning electron microscope to provide a highly automated, user-friendly and extremely fast microanalysis system. The software that runs on the hardware described above was specifically designed to provide the ultimate attainable speed on the system.


1970 ◽  
Vol 24 (6) ◽  
pp. 557-566 ◽  
Author(s):  
R. S. Frankel ◽  
D. W. Aitken

A review is given of recent developments in energy-dispersive x-ray emission spectroscopy, with the aim of providing both an introductory and usefully practical look at this innovative field. The review begins with the first principles of x-ray production and observation, including a brief comparison of the performance capabilities of different types of detectors, but then specializes to a major extent in solid state x-ray spectrometers, which have led to the most significant new developments and applications. Evidence is presented which suggests that we are nearing an asymptotic limit in the attainment of ever better resolution with these types of systems. Applications that have been made possible by significant improvements in system resolution are discussed, but in the context of the need for a realistic appraisal of over-all system requirements. The great advantages offered by the marriage of silicon x-ray spectrometers to scanning electron microscopes and electron microprobe analyzers are reviewed and illustrated.


2011 ◽  
Vol 17 (S2) ◽  
pp. 892-893 ◽  
Author(s):  
R Terborg ◽  
J Berlin ◽  
T Salge

Extended abstract of a paper presented at Microscopy and Microanalysis 2011 in Nashville, Tennessee, USA, August 7–August 11, 2011.


1979 ◽  
Vol 23 ◽  
pp. 81-86
Author(s):  
Ronald A. Vane ◽  
William D. Stewart ◽  
Mike Barker

AbstractEnergy dispersive X-ray fluorescence (EDXRF) spectrometry has been applied to the high speed analysis of uranium ore for the purpose of grading and sorting truckloads of ore at the mine. The system is able to analyze uranium ore in less than 60 seconds with uranium levels ranging from < 0.005% to > 5% U3O8. Precision at the 2σ level for 200 ppm ore is better than 10% relative. Good agreement is obtained with wet chemical results in a large variety of rock matrices.


1978 ◽  
Vol 22 ◽  
pp. 395-400
Author(s):  
Bradner D. Wheeler ◽  
Nancy Jacobus

Recent developments in analytical techniques and software have allowed the accurate quantitative determinations of both the major and minor elements in stainless steels by energy dispersive x-ray fluorescence. The successful analysis of 300 and 400 series stainless steel is reported utilizing this technique. The analysis of this type of material represents one of the most severe tests of the method due to numerous peak overlaps and interelement effects such as absorption and enhancement.Sixteen standards of ASTM 300 series and ten 400 series were prepared by polishing on a 220 grit aluminum oxide belt and subsequently washing the surface in absolute methanol. Analyses were performed with an EG&G ORTEC 6110 Tube Excited Fluorescence Analyzer utilizing a dual anode (Rh/W) x-ray tube. Peak deconvolutions and interelement corrections were made with a 16K PDP-11/05 computer utilizing the program FLINT (1). Utilization of spectral deconvolutions and interelement corrections yields a relative accuracy of approximately IX of the concentrations of the major elements.


1961 ◽  
Vol 5 ◽  
pp. 86-93 ◽  
Author(s):  
G.W. Goetze ◽  
A. Taylor

AbstractExperiments on the application of X-ray image intensifiers of the Fluorex type and of transmission-type secondary electron image intensifies (Astracon tubes) to the direct observation and recording of X-ray diffraction patterns have proved highly successful. Further improvements can be obtained by combining a Fluorex tube directly with an Astracon tube. By this means, the useful signal strength is so improved that movies at standard frame speed can be made which record the changing Laue pattern from a rotating crystal. It is shown how still further improvements are possible if the optical coupling in the system is improved by incorporating a fiber-optics window at the input of the Fluorex-Astracon tube. It is further indicated how a fiber-optics adapter can be used as an analog computer to convert the X-ray diffraction pattern from a single crystal into an exact representation of the reciprocal lattice which can be viewed directly.


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