Equipment for Beam Scanning and Step Scanning in Electron-Probe Analysis

1961 ◽  
Vol 5 ◽  
pp. 538-553 ◽  
Author(s):  
David B. Wittry ◽  
Ray Fitzgerald

AbstractA versatile beam-scanning system has been developed for use with the Electron Microprobe X-ray Analyzer manufactured by Applied Research Laboratories, Inc. It provides for the display of X-ray intensities from any of three spectrometers, three nondispersive detectors (either counters or scintiallation counters), as well as the current collected by the target or the current backscattered by the target. The electrostatic deflection system does not interfere with the use of the optical-viewing system and provides a maximum scanning area of only slightly less than field of view of the optical-viewing system.A stepping motor, controlled from the readout console, has also been developed which permits automatic point-by-point analysis of a specimen with minimum operator attention. In the use of this attachement, measurements may be made for fixed time, fixed charge, or fixed counts (integrated intensity) at each point. As a result, the step-scanning motor facilitates accurate measurement of one-dimensional concentration fluctuations and is particularly useful for phase identification and studies of diffusion and segregation.

1968 ◽  
Vol 39 (12) ◽  
pp. 1804-1806 ◽  
Author(s):  
Richard N. Kniseley ◽  
Francis C. Laabs ◽  
Dean Van Zuuk

Author(s):  
J. C. Russ ◽  
T. Taguchi ◽  
P. M. Peters ◽  
E. Chatfield ◽  
J. C. Russ ◽  
...  

Conventional SAD patterns as obtained in the TEM present difficulties for identification of materials such as asbestiform minerals, although diffraction data is considered to be an important method for making this purpose. The preferred orientation of the fibers and the spotty patterns that are obtained do not readily lend themselves to measurement of the integrated intensity values for each d-spacing, and even the d-spacings may be hard to determine precisely because the true center location for the broken rings requires estimation. We have implemented an automatic method for diffraction pattern measurement to overcome these problems. It automatically locates the center of patterns with high precision, measures the radius of each ring of spots in the pattern, and integrates the density of spots in that ring. The resulting spectrum of intensity vs. radius is then used just as a conventional X-ray diffractometer scan would be, to locate peaks and produce a list of d,I values suitable for search/match comparison to known or expected phases.


Author(s):  
C.M. Sung ◽  
K.J. Ostreicher ◽  
M.L. Huckabee ◽  
S.T. Buljan

A series of binary oxides and SiC whisker reinforced composites both having a matrix composed of an α-(Al, R)2O3 solid solution (R: rare earth) have been studied by analytical electron microscopy (AEM). The mechanical properties of the composites as well as crystal structure, composition, and defects of both second phases and the matrix were investigated. The formation of various second phases, e.g. garnet, β-Alumina, or perovskite structures in the binary Al2O3-R2O3 and the ternary Al2O3-R2O3-SiC(w) systems are discussed.Sections of the materials having thicknesses of 100 μm - 300 μm were first diamond core drilled. The discs were then polished and dimpled. The final step was ion milling with Ar+ until breakthrough occurred. Samples prepared in this manner were then analyzed using the Philips EM400T AEM. The low-Z energy dispersive X-ray spectroscopy (EDXS) data were obtained and correlated with convergent beam electron diffraction (CBED) patterns to identify phase compositions and structures. The following EDXS parameters were maintained in the analyzed areas: accelerating voltage of 120 keV, sample tilt of 12° and 20% dead time.


Author(s):  
Zenji Horita ◽  
Ryuzo Nishimachi ◽  
Takeshi Sano ◽  
Minoru Nemoto

Absorption correction is often required in quantitative x-ray microanalysis of thin specimens using the analytical electron microscope. For such correction, it is convenient to use the extrapolation method[l] because the thickness, density and mass absorption coefficient are not necessary in the method. The characteristic x-ray intensities measured for the analysis are only requirement for the absorption correction. However, to achieve extrapolation, it is imperative to obtain data points more than two at different thicknesses in the identical composition. Thus, the method encounters difficulty in analyzing a region equivalent to beam size or the specimen with uniform thickness. The purpose of this study is to modify the method so that extrapolation becomes feasible in such limited conditions. Applicability of the new form is examined by using a standard sample and then it is applied to quantification of phases in a Ni-Al-W ternary alloy.The earlier equation for the extrapolation method was formulated based on the facts that the magnitude of x-ray absorption increases with increasing thickness and that the intensity of a characteristic x-ray exhibiting negligible absorption in the specimen is used as a measure of thickness.


Author(s):  
John J. Donovan ◽  
Donald A. Snyder ◽  
Mark L. Rivers

We present a simple expression for the quantitative treatment of interference corrections in x-ray analysis. WDS electron probe analysis of standard reference materials illustrate the success of the technique.For the analytical line of wavelength λ of any element A which lies near or on any characteristic line of another element B, the observed x-ray counts at We use to denote x-ray counts excited by element i in matrix j (u=unknown; s=analytical standard; ŝ=interference standard) at the wavelength of the analytical line of A, λA (Fig. 1). Quantitative analysis of A requires an accurate estimate of These counts can be estimated from the ZAF calculated concentration of B in the unknown C,Bu measured counts at λA in an interference standard of known concentration of B (and containing no A), and ZAF correction parameters for the matrices of both the unknown and the interference standard at It can be shown that:


Author(s):  
Judith M. Brock ◽  
Max T. Otten

A knowledge of the distribution of chemical elements in a specimen is often highly useful. In materials science specimens features such as grain boundaries and precipitates generally force a certain order on mental distribution, so that a single profile away from the boundary or precipitate gives a full description of all relevant data. No such simplicity can be assumed in life science specimens, where elements can occur various combinations and in different concentrations in tissue. In the latter case a two-dimensional elemental-distribution image is required to describe the material adequately. X-ray mapping provides such of the distribution of elements.The big disadvantage of x-ray mapping hitherto has been one requirement: the transmission electron microscope must have the scanning function. In cases where the STEM functionality – to record scanning images using a variety of STEM detectors – is not used, but only x-ray mapping is intended, a significant investment must still be made in the scanning system: electronics that drive the beam, detectors for generating the scanning images, and monitors for displaying and recording the images.


Nanomaterials ◽  
2020 ◽  
Vol 10 (6) ◽  
pp. 1023 ◽  
Author(s):  
Ashish Chhaganlal Gandhi ◽  
Chia-Liang Cheng ◽  
Sheng Yun Wu

We report the synthesis of room temperature (RT) stabilized γ–Bi2O3 nanoparticles (NPs) at the expense of metallic Bi NPs through annealing in an ambient atmosphere. RT stability of the metastable γ–Bi2O3 NPs is confirmed using synchrotron radiation powder X-ray diffraction and Raman spectroscopy. γ–Bi2O3 NPs exhibited a strong red-band emission peaking at ~701 nm, covering 81% integrated intensity of photoluminescence spectra. Our findings suggest that the RT stabilization and enhanced red-band emission of γ‒Bi2O3 is mediated by excess oxygen ion vacancies generated at the octahedral O(2) sites during the annealing process.


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