Loss of grain boundary segregant during ion milling

Journal Article · Sat Jun 01 04:00:00 EDT 1991 · Journal of Electron Microscopy Technique; (United States)

DOI:https://doi.org/10.1002/jemt.1060180211· OSTI ID:5099305

Kenik, E A ^[1]

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1. Metals and Ceramics Division, Oak Ridge National Laboratory, Tennessee (United States)

It is shown that material segregated to grain boundaries can be lost during ion milling. This specimen preparation artifact has been studied in the case of bismuth in copper and has also been observed for phosphorus in stainless steel. The loss is associated with specimen heating during ion milling and can be alleviated by good clamping and cooling of the specimen during milling. Specimen heating permits grain boundary diffusion of the segregating element to the specimen surfaces with subsequent loss of segregant from the specimen by evaporation or sputtering during ion milling. Loss of bismuth during in situ heating to 200-300 degrees C is demonstrated. Therefore, care must be taken in specimen preparation for analytical electron microscopy measurement of such segregation. Similar effects may occur during ion milling of other materials, especially those where low thermal conductivity will result in high beam heating. In these cases, care must be taken to avoid loss of segregant during specimen preparation. Additional tests showed that no significant loss of segregant was observed during X-ray microanalysis, even at nominal room temperature and probe currents five-fold higher than that normally used for microanalysis.

• OSTI ID: 5099305
• Journal Information: Journal of Electron Microscopy Technique; (United States), Journal Name: Journal of Electron Microscopy Technique; (United States) Vol. 18:2; ISSN 0741-0581; ISSN JEMTE
• Country of Publication: United States
• Language: English

Related Subjects

36 MATERIALS SCIENCE
360101* -- Metals & Alloys-- Preparation & Fabrication
360102 -- Metals & Alloys-- Structure & Phase Studies
ALLOYS
BISMUTH
CHARGED PARTICLES
CHEMICAL ANALYSIS
COPPER
CRYSTAL STRUCTURE
ELECTRON MICROPROBE ANALYSIS
ELEMENTS
GRAIN BOUNDARIES
HIGH ALLOY STEELS
IONS
IRON ALLOYS
IRON BASE ALLOYS
MACHINING
METALS
MICROANALYSIS
MICROSTRUCTURE
MILLING
NONDESTRUCTIVE ANALYSIS
NONMETALS
PHOSPHORUS
SEGREGATION
STAINLESS STEELS
STEELS
TRANSITION ELEMENTS