Microbeam analysis - Methods of specimen preparation for analysis of general powders using WDS and EDS

2019 ◽  
2002 ◽  
Vol 8 (I1) ◽  
pp. 20-20

Topic: Characterization of Non-Conductive or Charging Materials by Microbeam AnalysisThe goal of this topical conference is to present the state of the art for materials characterization of non-conductive or charging materials using microbeam analysis. Examples of charging materials include polymeric materials, ceramic materials, and photoresist materials in the microelectronic industry. Also, the characterization of biological specimens will be covered because they are prone to problems related to charging. These materials are of great technological importance and their characterization is still a great challenge because they charge when analyzed with an electron beam. The techniques of microbeam analysis that will be considered are: X-ray Microanalysis in the Electron Microprobe, Low Voltage Scanning Electron Microscopy, Environmental Scanning Electron Microscopy, Analytical Electron Microscopy with Field Emission Transmission Electron Microscopy, and Focused Ion Beam Milling for specimen preparation. World experts will present papers on these topics. Papers from this topical conference will be published in a special issue of Microscopy & Microanalysis.


2002 ◽  
Vol 8 (I1) ◽  
pp. 36-37
Author(s):  
Stanley L. Erlandsen

It is my pleasure to welcome you to Microscopy and Microanalysis 2002, jointly sponsored by the Microscopy Society of America, Microbeam Analysis Society, Microscopy Society of Canada/Société de Microscopie du Canada, and the International Metallographic Society. An excellent program with an outstanding list of invited speakers for symposia has been assembled by the Program Committee consisting of the Chair, Edgar Voelkl, and Co-Chairs, David Piston (MSA), Raynald Gauvin (MAS/MSC), and Allan Lockley (IMS). Highlights of Microscopy and Microanalysis 2002 include the world's largest display of microscopes and related technologies together with outstanding sessions on all aspects of microscopy and microanalysis. Symposia will be held on 3-D electron microscopy of macromolecules and cryo-electron microscopy of macromolecules, the quantitative aspects of X-ray microscopy, confocal microscopy, biomaterials, biological and materials specimen preparation. Special sessions will be held on holography, phase imaging, deep tissue imaging, (S)TEM instrumentation, developments in focused-ion beam instruments and imaging, metallographic specimen preparation from start to finish, and the changing role of atom probe microscopes in the nanotechnology era. Advances in immunolabeling, EELS, and detectors for X-ray microanalysis also will be presented. A special analytical electron microscopy session honoring the work of Elmar Zeitler is also scheduled. A pre-meetingworkshop “Future of Materials Characterization of Charging Materialsusing Microbeam Analysis” organized by Dr. Raynald Gauvin will be held at McGill University in Montreal on August 2–3. The Local Arrangements Committee, headed by Pierre Charest, has coordinated the scheduling of many local events to complement the meeting.


Author(s):  
R. W. Anderson ◽  
D. L. Senecal

A problem was presented to observe the packing densities of deposits of sub-micron corrosion product particles. The deposits were 5-100 mils thick and had formed on the inside surfaces of 3/8 inch diameter Zircaloy-2 heat exchanger tubes. The particles were iron oxides deposited from flowing water and consequently were only weakly bonded. Particular care was required during handling to preserve the original formations of the deposits. The specimen preparation method described below allowed direct observation of cross sections of the deposit layers by transmission electron microscopy.The specimens were short sections of the tubes (about 3 inches long) that were carefully cut from the systems. The insides of the tube sections were first coated with a thin layer of a fluid epoxy resin by dipping. This coating served to impregnate the deposit layer as well as to protect the layer if subsequent handling were required.


Author(s):  
L. Gandolfi ◽  
J. Reiffel

Calculations have been performed on the contrast obtainable, using the Scanning Transmission Electron Microscope, in the observation of thick specimens. Recent research indicates a revival of an earlier interest in the observation of thin specimens with the view of comparing the attainable contrast using both types of specimens.Potential for biological applications of scanning transmission electron microscopy has led to a proliferation of the literature concerning specimen preparation methods and the controversy over “to stain or not to stain” in combination with the use of the dark field operating mode and the same choice of technique using bright field mode of operation has not yet been resolved.


Author(s):  
M. Talianker ◽  
D.G. Brandon

A new specimen preparation technique for visualizing macromolecules by conventional transmission electron microscopy has been developed. In this technique the biopolymer-molecule is embedded in a thin monocrystalline gold foil. Such embedding can be performed in the following way: the biopolymer is deposited on an epitaxially-grown thin single-crystal gold film. The molecule is then occluded by further epitaxial growth. In such an epitaxial sandwich an occluded molecule is expected to behave as a crystal-lattice defect and give rise to contrast in the electron microscope.The resolution of the method should be limited only by the precision with which the epitaxially grown gold reflects the details of the molecular structure and, in favorable cases, can approach the lattice resolution limit.In order to estimate the strength of the contrast due to the void-effect arising from occlusion of the DNA-molecule in a gold crystal some calculations were performed.


Author(s):  
F. Thoma ◽  
TH. Koller

Under a variety of electron microscope specimen preparation techniques different forms of chromatin appearance can be distinguished: beads-on-a-string, a 100 Å nucleofilament, a 250 Å fiber and a compact 300 to 500 Å fiber.Using a standardized specimen preparation technique we wanted to find out whether there is any relation between these different forms of chromatin or not. We show that with increasing ionic strength a chromatin fiber consisting of a row of nucleo- somes progressively folds up into a solenoid-like structure with a diameter of about 300 Å.For the preparation of chromatin for electron microscopy the avoidance of stretching artifacts during adsorption to the carbon supports is of utmost importance. The samples are fixed with 0.1% glutaraldehyde at 4°C for at least 12 hrs. The material was usually examined between 24 and 48 hrs after the onset of fixation.


Author(s):  
H.J. Dudek

The chemical inhomogenities in modern materials such as fibers, phases and inclusions, often have diameters in the region of one micrometer. Using electron microbeam analysis for the determination of the element concentrations one has to know the smallest possible diameter of such regions for a given accuracy of the quantitative analysis.In th is paper the correction procedure for the quantitative electron microbeam analysis is extended to a spacial problem to determine the smallest possible measurements of a cylindrical particle P of high D (depth resolution) and diameter L (lateral resolution) embeded in a matrix M and which has to be analysed quantitative with the accuracy q. The mathematical accounts lead to the following form of the characteristic x-ray intens ity of the element i of a particle P embeded in the matrix M in relation to the intensity of a standard S


Author(s):  
Jayesh Bellare

Seeing is believing, but only after the sample preparation technique has received a systematic study and a full record is made of the treatment the sample gets.For microstructured liquids and suspensions, fast-freeze thermal fixation and cold-stage microscopy is perhaps the least artifact-laden technique. In the double-film specimen preparation technique, a layer of liquid sample is trapped between 100- and 400-mesh polymer (polyimide, PI) coated grids. Blotting against filter paper drains excess liquid and provides a thin specimen, which is fast-frozen by plunging into liquid nitrogen. This frozen sandwich (Fig. 1) is mounted in a cooling holder and viewed in TEM.Though extremely promising for visualization of liquid microstructures, this double-film technique suffers from a) ireproducibility and nonuniformity of sample thickness, b) low yield of imageable grid squares and c) nonuniform spatial distribution of particulates, which results in fewer being imaged.


Author(s):  
Tokio Nei ◽  
Haruo Yotsumoto ◽  
Yoichi Hasegawa ◽  
Yuji Nagasawa

In order to observe biological specimens in their native state, that is, still containing their water content, various methods of specimen preparation have been used, the principal two of which are the chamber method and the freeze method.Using its recently developed cold stage for installation in the pre-evacuation chamber of a scanning electron microscope, we have succeeded in directly observing a biological specimen in its frozen state without the need for such conventional specimen preparation techniques as drying and metallic vacuum evaporation. (Echlin, too, has reported on the observation of surface structures using the same freeze method.)In the experiment referred to herein, a small sliced specimen was place in the specimen holder. After it was rapidly frozen by freon cooled with liquid nitrogen, it was inserted into the cold stage of the specimen chamber.


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