Film thickness and composition determination for binary alloys using backscattered electrons

The paper presents the results of an ellipsometric study of compacted powders of aluminum-based binary alloys containing 1,5 wt.% of rare earth elements (Sc, La, Ce, Sm) and cast aluminum-silicon alloys with the following compositions: Al–10Si–0,5Mg– 0,3Fe–0,1Ca and Al–12Si–0,6Mg–0,5Fe–0,5Ca–0,45Na. An immersion method was used to determine the optical constants of massive polycrystalline alloys obtained by remelting these powders in vacuum, as well as their oxide films for a wavelength λ = 0,6328 μm. Using the optical constants of these alloys, the dependence of their reflectivity on the surface oxide film thickness was calculated. It was found that an increase in the amount of the alloying component and intermetallic phases in the alloy decreases its reflectivity. In addition, the optical constants were used in the construction of modified Δ–ψ nomograms calculated using the Maxwell-Garnett equation that make it possible to determine the thicknesses of oxide films on particles and the volume fractions of metal in compacted powders, and to study the processes of their oxidation in air. It was shown that oxidation of aluminum ASD-4 powders and Al–1,5% REM binary alloys at 600 °C is described by a simple model where a decrease in the metal fraction leads to an increase in the oxide film thickness. It turned out that the oxidation of aluminum-silicon alloys is much faster and not described by this model, which may be due to the appearance of a liquid phase in the powder. A large number of metal droplets on the surface of particles increase the amount of metal on the studied tablet surface in general. The high oxidation rate of aluminumsilicon alloys in air can be explained by the surface activity of magnesium in relation to liquid aluminum.

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X-ray measurements of nanometer-thick tantalum oxide and hafnium oxide films on silicon substrates for thickness and composition determination

Powder Diffraction ◽

10.1017/s0885715612000425 ◽

2012 ◽

Vol 27 (2) ◽

pp. 87-91 ◽

Cited By ~ 2

Author(s):

F. J. Cadieu ◽

I. Vander ◽

Y. Rong ◽

R. W. Zuneska

Keyword(s):

Magnetron Sputtering ◽

Film Thickness ◽

Hafnium Oxide ◽

Tantalum Oxide ◽

High Mass ◽

Silicon Substrates ◽

Fluorescence Detector ◽

X Ray ◽

Mass Absorption ◽

Composition Determination

The thicknesses and oxygen concentration of tantalum oxide (TaO) and hafnium oxide (HfO) films, prepared by magnetron sputtering Ta and Hf in oxygen onto heated silicon (100) substrates, were measured by three different techniques. The first method uses X-ray reflectivity, which yields a thickness value independent of the film composition. The second method uses the simultaneous measurement of Ta and Hf fluorescence counts. For these <200-nm-thick films there is very little matrix effect so that the Ta and Hf fluorescence counts are expected to, and are observed to, increase linearly with the film thickness. The third method uses the attenuation of the Si Kα X-ray line from the underlying Si excited by a glancing incident X-ray beam for measurement. The TaO and HfO films were observed to grow for the sputtering conditions employed, in an initial mode characterized by a high mass absorption times density product and then grow as characterized by a lower mass absorption times density product. This change over occurred for the HfO films, at a film thickness of 13 nm. The change over occurred for the TaO films at a film thickness of 23 nm. Pure Ta and Hf films were also made by magnetron sputtering from Ta and Hf targets in argon. All X-ray measurements, including the reflectivity measurements, were made, with the addition of an X-ray fluorescence detector, using a Panalytical MRD system.

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Surface Films on Zircaloy-2 Samples Cracked in Neutral Aqueous NaCl by Stress Corrosion

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100070679 ◽

1973 ◽

Vol 31 ◽

pp. 46-47

Author(s):

R.A. Ploc

Keyword(s):

Electron Microscopy ◽

Transmission Electron Microscopy ◽

Film Thickness ◽

Stress Corrosion ◽

Zirconium Dioxide ◽

Surface Film ◽

Surface Films ◽

Continuous Layer ◽

Transmission Electron ◽

Product Film

Samples of low-nickel Zircaloy-2 (material MLI-788-see(1)), when anodically polarized in neutral 5 wt% NaCl solutions, were found to be susceptible to pitting and stress corrosion cracking. The SEM revealed that pitting of stressed samples was occurring below a 2000Å thick surface film which behaved differently from normal zirconium dioxide in that it did not display interference colours. Since the initial film thickness was approximately 65Å, attempts were made to examine the product film by transmission electron microscopy to deduce composition and how the corrosion environment could penetrate the continuous layer.

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Current State of Biological High-Resolution Scanning Electron Microscopy

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100102985 ◽

1988 ◽

Vol 46 ◽

pp. 180-181 ◽

Cited By ~ 1

Author(s):

Klaus-Ruediger Peters

Keyword(s):

High Performance ◽

Low Voltage ◽

Backscattered Electrons ◽

Lens Position ◽

Low Voltage Operation ◽

Signal Collection ◽

Probe Size ◽

Electron Microscopes ◽

Scanning Electron Microscopes ◽

Scanning Electron

A new generation of high performance field emission scanning electron microscopes (FSEM) is now commercially available (JEOL 890, Hitachi S 900, ISI OS 130-F) characterized by an "in lens" position of the specimen where probe diameters are reduced and signal collection improved. Additionally, low voltage operation is extended to 1 kV. Compared to the first generation of FSEM (JE0L JSM 30, Hitachi S 800), which utilized a specimen position below the final lens, specimen size had to be reduced but useful magnification could be impressively increased in both low (1-4 kV) and high (5-40 kV) voltage operation, i.e. from 50,000 to 200,000 and 250,000 to 1,000,000 x respectively.At high accelerating voltage and magnification, contrasts on biological specimens are well characterized1 and are produced by the entering probe electrons in the outmost surface layer within -vl nm depth. Backscattered electrons produce only a background signal. Under these conditions (FIG. 1) image quality is similar to conventional TEM (FIG. 2) and only limited at magnifications >1,000,000 x by probe size (0.5 nm) or non-localization effects (%0.5 nm).

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Development of a digital SEM

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s042482010008609x ◽

1991 ◽

Vol 49 ◽

pp. 358-359

Author(s):

A. Yamada ◽

A. Shibano ◽

K. Harasawa ◽

T. Kobayashi ◽

H. Fukuda ◽

...

Keyword(s):

Large Diameter ◽

Objective Lens ◽

Large Specimen ◽

Backscattered Electrons ◽

Digital Scanning ◽

Junction Type ◽

High Resolution Images ◽

Working Distance ◽

Type Detector ◽

Short Working

A newly developed digital scanning electron microscope, the JSM-6300, has the following features: Equipped with a narrower conical objective lens (OL), it allows high resolution images to be obtained easily at a short working distance (WD) and a large specimen tilt angle. In addition, it is provided with automatic functions and digital image processing functions for ease of operation.Conical C-F lens: The newly developed conical C-F objective lens, having low aberration characteristics over a wide WD range, allows a large-diameter (3-inch) specimen to be tilted up to 60° at short WD, and provides images with low magnifications starting at 10*. On the bottom of the lens, a p n junction type detector is provided to detect backscattered electrons (BE) from the specimen. As the narrower conical 0L increases the secondary electron (SE) detector's field intensity on the specimen surface, high SE image quality is obtained.

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Contrast in Scanning Images of Thin Crystals

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100095856 ◽

1972 ◽

Vol 30 ◽

pp. 520-521

Author(s):

S. Kimoto ◽

H. Hashimoto ◽

S. Takashima ◽

R. M. Stern ◽

T. Ichinokawa

Keyword(s):

Crystal Surface ◽

Solid Angle ◽

Incident Angle ◽

Intensity Variation ◽

Lattice Defects ◽

Scanning Microscope ◽

Electron Detector ◽

Backscattered Electrons ◽

Electron Image ◽

Backscattered Electron

The most well known application of the scanning microscope to the crystals is known as Coates pattern. The contrast of this image depends on the variation of the incident angle of the beam to the crystal surface. The defect in the crystal surface causes to make contrast in normal scanning image with constant incident angle. The intensity variation of the backscattered electrons in the scanning microscopy was calculated for the defect in the crystals by Clarke and Howie. Clarke also observed the defect using a scanning microscope.This paper reports the observation of lattice defects appears in thin crystals through backscattered, secondary and transmitted electron image. As a backscattered electron detector, a p-n junction detector of 0.9 π solid angle has been prepared for JSM-50A. The gain of the detector itself is 1.2 x 104 at 50 kV and the gain of additional AC amplifier using band width 100 Hz ∼ 10 kHz is 106.

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(111) Monocrystalline Nickel Films

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100095819 ◽

1972 ◽

Vol 30 ◽

pp. 512-513

Author(s):

T.E. Pratt ◽

R.W. Vook

Keyword(s):

Film Thickness ◽

Deposition Rate ◽

Room Temperature ◽

Narrow Range ◽

High Vacuum ◽

Residual Pressure ◽

Temperature Dependent ◽

Deposition Parameters ◽

Transmission Electron ◽

Substrate Temperatures

(111) oriented thin monocrystalline Ni films have been prepared by vacuum evaporation and examined by transmission electron microscopy and electron diffraction. In high vacuum, at room temperature, a layer of NaCl was first evaporated onto a freshly air-cleaved muscovite substrate clamped to a copper block with attached heater and thermocouple. Then, at various substrate temperatures, with other parameters held within a narrow range, Ni was evaporated from a tungsten filament. It had been shown previously that similar procedures would yield monocrystalline films of CU, Ag, and Au.For the films examined with respect to temperature dependent effects, typical deposition parameters were: Ni film thickness, 500-800 A; Ni deposition rate, 10 A/sec.; residual pressure, 10-6 torr; NaCl film thickness, 250 A; and NaCl deposition rate, 10 A/sec. Some additional evaporations involved higher deposition rates and lower film thicknesses.Monocrystalline films were obtained with substrate temperatures above 500° C. Below 450° C, the films were polycrystalline with a strong (111) preferred orientation.

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A Color Coded STEM/SEM Image Storage System

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100097880 ◽

1981 ◽

Vol 39 ◽

pp. 272-273

Author(s):

Y. Kokubo ◽

W. H. Hardy ◽

J. Dance ◽

K. Jones

Keyword(s):

Image Processing ◽

Electron Beam ◽

Storage System ◽

Particle Analysis ◽

Specific Information ◽

X Rays ◽

Sem Image ◽

Backscattered Electrons ◽

Wide Range ◽

Scanning Electron

A color coded digital image processing is accomplished by using JEM100CX TEM SCAN and ORTEC’s LSI-11 computer based multi-channel analyzer (EEDS-II-System III) for image analysis and display. Color coding of the recorded image enables enhanced visualization of the image using mathematical techniques such as compression, gray scale expansion, gamma-processing, filtering, etc., without subjecting the sample to further electron beam irradiation once images have been stored in the memory.The powerful combination between a scanning electron microscope and computer is starting to be widely used 1) - 4) for the purpose of image processing and particle analysis. Especially, in scanning electron microscopy it is possible to get all information resulting from the interactions between the electron beam and specimen materials, by using different detectors for signals such as secondary electron, backscattered electrons, elastic scattered electrons, inelastic scattered electrons, un-scattered electrons, X-rays, etc., each of which contains specific information arising from their physical origin, study of a wide range of effects becomes possible.

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