Energy-Dispersive X-ray Spectrometry Performance on Multiple Transmission Electron Microscope Platforms

Author(s):  
James Demarest ◽  
Chris Deeb ◽  
Thomas Murray ◽  
Hong-Ying Zhai

Abstract Energy-dispersive X-ray spectrometry (EDS) is a key analytical tool aiding root cause determination in the failure analysis (FA) process. This paper looks at a number of analytical TEM microscopes currently in use in various facilities: microscope A, a STEM operated at 200kV; microscope B, a 300kV TEM; and microscopes C and D, both 200kV TEMs. EDS counts per unit time from multiple microscope platforms were examined. Microscope D demonstrated two orders of magnitude higher counts per unit time than the other three microscopes. Microscope D represents the state-of-the-art EDS analytical TEM configuration and has achieved this through a novel windowless EDS configuration which significantly increases the detector area (by about a factor of three) that receives X-rays generated from the sample.

Author(s):  
D.W. Dempster ◽  
W.A.P. Nicholson ◽  
H.Y. Elder ◽  
D.A.S. Smith ◽  
R.P. Ferrier

The use of an energy dispersive X-ray microanalytical system (EDX) attached to a conventional transmission electron microscope (TEM) allows images of good morphological resolution from ultra-thin specimens and spectra of all detectable elements to be obtained simultaneously at radiation doses which are low compared to wavelength dispersive detectors. For reasons of detection efficiency the solid angle subtended from the specimen to the detector is maximised (∼0.l sterad) in our system, a LINK SYSTEMS 290 with a 30mm2Si(Li) crystal fitted to a JEOL JEM lOOC. However, with this type of system the recorded spectrum has contributions not only from the small areas which can be probed but also from scattered electrons, and X-rays originating in the surrounding specimen, the specimen support system and the microscope environment of the specimen. The problem is particularly acute in projects, such as the present, where it is necessary to detect and determine the ratios of elements (Ca and P) in small quantities in close proximity to relatively massive concentrations of the same elements.Modifications to our system have been described (Nicholson et al., 1977a;Biddlecombe et al., 1977) which greatly improve the peak/background ratios for quantitative analysis and eliminate all of the specific peaks of non-specimen origin. For ease of maintenance the JEOL 100C is fitted with thin foil condenser apertures (10μm thick molybdenum) as standard. At the accelerating voltage used in this study (80 keV) a considerable number of electrons are transmitted by these apertures and with the electron probe placed adjacent to fully mineralized bone the scattered electrons were responsible for generation of sizeable Ca and P signals. We have replaced the standard foils with thick (0.25 mm) molybdenum apertures.


Author(s):  
C. M. Helmick ◽  
J. F. Bailey ◽  
S. S. Ristow

Since not all research facilities have access to a transmission electron microscope (TEM) / x-ray microanalysis system, a study was conducted to determine if a scanning electron microscope (SEM) equipped with an energy dispersive x-ray microanalyer would detect and quantify an immunogold labeled virus on a TEM thin sectioned sample. The objectives of the study were to first, demonstrate that a particular region (serous cardiac gland) of a thin sectioned fish esophageal tissue sample could be detected on a SEM. Secondly, we sought to demonstrate that the quantities of colloidal gold x-rays emitted were in association with the viral infected esophageal tissue at 1 and 24 hours post infection.Tissue and Immunogold labeling. Juvenile rainbow trout (Oncorhychus mykiss) were challenged in vivo at 105 pfu with Hagerman infectious hematopoietic necrosis virus (IHNV) or mocked infected with phosphate buffered saline (PBS). Fish were killed and fixed in 6% paraformaldehyde and 0.5% glutaraldehyde in 0.1 M PBS at 1 and 24 hours post infection and stored at 4°C.


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.


Author(s):  
Michael E. Rock ◽  
Vern Kennedy ◽  
Bhaskar Deodhar ◽  
Thomas G. Stoebe

Cellophane is a composite polymer material, made up of regenerated cellulose (usually derived from wood pulp) which has been chemically transformed into "viscose", then formed into a (1 mil thickness) transparent sheet through an extrusion process. Although primarily produced for the food industry, cellophane's use as a separator material in the silver-zinc secondary battery system has proved to be another important market. We examined 14 samples from five producers of cellophane, which are being evaluated as the separator material for a silver/zinc alkaline battery system in an autonomous underwater target vehicle. Our intent was to identify structural and/or chemical differences between samples which could be related to the functional differences seen in the lifetimes of these various battery separators. The unused cellophane samples were examined by transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDS). Cellophane samples were cross sectioned (125-150 nm) using a diamond knife on a RMC MT-6000 ultramicrotome. Sections were examined in a Philips 430-T TEM at 200 kV. Analysis included morphological characterization, and EDS (for chemical composition). EDS was performed using an EDAX windowless detector.


Author(s):  
Y. Sato ◽  
T. Hashimoto ◽  
M. Ichihashi ◽  
Y. Ueki ◽  
K. Hirose ◽  
...  

Analytical TEMs have two variations in x-ray detector geometry, high and low angle take off. The high take off angle is advantageous for accuracy of quantitative analysis, because the x rays are less absorbed when they go through the sample. The low take off angle geometry enables better sensitivity because of larger detector solid angle.Hitachi HF-2000 cold field emission TEM has two versions; high angle take off and low angle take off. The former allows an energy dispersive x-ray detector above the objective lens. The latter allows the detector beside the objective lens. The x-ray take off angle is 68° for the high take off angle with the specimen held at right angles to the beam, and 22° for the low angle take off. The solid angle is 0.037 sr for the high angle take off, and 0.12 sr for the low angle take off, using a 30 mm2 detector.


1995 ◽  
Vol 73 (6) ◽  
pp. 954-957 ◽  
Author(s):  
M. Marcia West ◽  
Derrick T. Flannigan ◽  
John N.A. Lott

The mature seeds of some angiosperms contain perisperm tissue derived from remains of the nucellus tissue of the ovule. In our transmission electron microscopy studies, the perisperm tissues of the seeds of Yucca brevifolia, Coffea arabica, Beta vulgaris, Piper nigrum, and Zostera capricorni contained naturally electron-dense globoids. Energy dispersive X-ray analysis of globoids from the perisperm tissues of these seeds revealed varying levels of phosphorus, potassium, magnesium, and calcium, results that are consistent with the presence of the mineral nutrient store called phytate. Phosphorus, potassium, magnesium, calcium, and other mineral nutrients, likely stored as phytate, have routinely been located in globoids of endosperm, female gametophyte, and embryo tissues of seeds. Key words: perisperm, globoids, mineral nutrient reserves, phosphorus, seeds, energy dispersive X-ray analysis.


2022 ◽  
Vol 905 ◽  
pp. 192-197
Author(s):  
Lin Lin Cai ◽  
Xiao Qing Jiang

A new composite of graphene/MoS2 is synthesized by co-exfoliation of graphite and MoS2 in isopropanol (IPA) using the organic salt potassium sodium tartrate as the assistant. The composite is characterized by transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and Raman spectra. The results of TEM, XPS, and Raman spectra all illustrate that the graphene/MoS2 composite has been synthesized successfully. Furthermore, the composite is modified on glassy carbon electrode to fabricate a sensor to detect dopamine (DA). The sensor shows two linear detection ranges for DA. One is 1-45 μM and the other is 45-120 μΜ. The detection limit of the sensor (S/N=3) is 0.76 μM.


2021 ◽  
pp. 104063872110575
Author(s):  
Bianca R. Pfisterer ◽  
Anthony L. Ashley ◽  
Robert L. Donnell ◽  
John R. Dunlap ◽  
Kim M. Newkirk

Two rock hyraxes ( Procavia capensis), from the Chattanooga Zoo, were submitted separately for autopsy at the University of Tennessee Veterinary Medical Center. The first was a 4-y-old intact female that died without premonitory signs and the second was a 10-y-old intact male that was euthanized because of severe renal disease. Microscopically, the lungs of both hyraxes had multifocal-to-coalescing, <1-mm diameter aggregates of epithelioid macrophages separated by streams of fibrous tissue. Macrophages contained intracytoplasmic, clear, acicular, birefringent crystals. Transmission electron microscopy and energy-dispersive x-ray spectroscopy findings on the lung samples were consistent with silica crystal deposition. The hyraxes had been housed together on commercially sourced play sand composed of 99–99.5% quartz, a crystalline silica polymorph. The microscopic findings, transmission electron microscopy, and energy-dispersive x-ray spectroscopy of the intrahistiocytic crystals, in addition to the history of exposure to crystalline silica, were consistent with pulmonary silicosis. Pulmonary silicosis has not been reported previously in rock hyraxes, to our knowledge.


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