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Preparation of thin section samples for TEM using Ar ion slicing
Feizpour, Darja ...
Ion milling, electrolytic polishing and focused ion beam (FIB) processing are techniques used for specimen preparation for transmission electron microscopy (TEM) analysis. A new alternative approach ...to these kind of specimen preparations is presented using a Jeol EM-09100IS Ion Slicer. The instrument irradiates an argon ion beam on the specimen and thins it. Specimens of silicon wafer and different duplex stainless steels (DSS), thickness of around 500 m, were cut out of a bulk material in rectangular area of 0.5-1.0 mm * 2.8 mm (bulk cross section preparation) or 1.0 mm * 2.0 mm (plane surface preparation). The specimens were thinned to less than 100 m with Jeol Handy Lap, mounted on an Ion Slicer specimen holder, partially masked with a shield belt (bulk cross section preparation) or specimen support ring (plane surface preparation), and further thinned with an argon ion beam. The beam was tilted to 1.2° or 1.4°. The slicing process started at the pressure of 10-4Pa and alternated between the front and the backside or just the frontside of the specimens. Accelerating voltage of 6 kV, argon gas flow rate of 7.2 or 7.3 and side change interval of 30 s were chosen. After a large thin area of the specimens up to 300 m * 700 m was obtained, a small hole was generated in the thinnest region of the specimens. Polishing was used with a tilt angle of 0.5°, at accelerating voltage of 2 kV and side change interval of 15 s or 40 s. The total time of slicing was 3 h and 48 min for Si and 1 h and 15 min or 9 h and 40 min for DSS. The specimens were after slicing further analyzed on atomic level by high resolution TEM using Jeol JEM-2100 at 200 kV.
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