SummaryMetallic materials are known to be very sensitive to Gallium (Ga) focused ion beam (FIB) processing. Crystal defects formed by FIB irradiation degrade the transmission electron microscope image quality, and it is difficult to distinguish original defects from FIB process‐induced damage. A solution to this problem is the low acceleration voltage and low incident angle (LVLA) Argon ion milling, which can be incorporated as an extensional countermeasure for FIB damage removal and eventually for preparation of high‐quality lamellae. The transmission electron microscope image quality of iron single crystal could be improved by removing crystal defects using the low acceleration voltage and low incident angle Argon ion milling finish. Lamella quality of the processing result was almost similar with that of the conventional electrolytic polishing.As a practical application of the process, low damage lamella of stainless cast steel could be prepared. Effectiveness of the FIB system equipped with the low acceleration voltage and low incident angle Argon ion milling function as a tool to make high‐quality metallic material lamellae is illustrated.
Passive layers on various stainless steels were studied with an ion microanalyzer. An argon ion beam was directed on the specimen surface in an oxygen atmosphere. The use of oxygen atmosphere effectively minimized the difference in ion yields of the elements in the oxidized layers and matrices, making it possible to determine these elements with good reproducibility. 18% Cr–8% Ni and 18% Cr–8% Ni–0.4% Ti stainless steel was exposed to neutral water containing 8 ppm oxygen at 289 °C. The passive layers contained larger amounts of iron and smaller amounts of chromium than the matrices.
Quantitative analysis of hydrogen in titanium was investigated with an ion microanalyzer. Argon ions as primaries were accelerated at a voltage of 10 kV. The diameter and the current of the beam were 1 mm and 2 μA, respectively. A mass spectrum was measured at 2×10−7 Torr. It was found that the intensity ratio of m⁄e=49(48TiH+) and 46(46Ti+) can be used for the determination of hydrogen in titanium. A linear relation was obtained between the intensity ratio and hydrogen concentration determined by the standard vacuum fusion method. The present method was applied to determine the hydrogen concentration in the surface layer of a sample treated by cathodic polarization. It was observed that hydrogen concentrations in the surface layer were much higher than those in the bulk of the sample.
The sputtering rates of chromium,copper,germanium and gold films,which were prepared by a vacuum deposition method,were measured after oxygen ion bombardment. It was found that sputtering rates are proportional to the current density of primary oxygen ions.This relation can be used to determine the depth of a sputtered surface when beam parameters change,and allows to obtain the compositional depth profile of multi-layer metal films,prepared by vacuum deposition. 1.Introduction An ion microanalyzer is often used to determine the compositional depth profiles of multi-layer metal films deposited on metal and semiconductor substrates.In the compositional depth profiles reported up to now,elemental composition has usually been shown as a function of bombardment time.It would,however,be more desirable to give it as a function of depth.If the rate of sputtering of an element and the
Quantitative Analysis of High Temperature Alloys with an Ion Microanalyzer YOSHIAKI OKAZIMA*AND YUKIYOSHI AIZAWA* (Received31March1977) Quantitative analysis of constituent elements of high temperature alloys was investigated with an ion microanalyzer. Contents of constituent elements are different from one alloy to the other in high temperature alloys such as Inconel and Hastelloy and there is not a common main constituent like iron in low alloy steels.For calibrating methods,total ions and nickel ions were selected as a reference.The peak intensity ratio of each element to nickel is used,as it is assured that this is proportional to the concentration ratio in alloys.
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