Preparation of cross-sectional TEM samples for low-angle ion milling

McCaffrey, J. P.; Barna, Á.

doi:10.1002/(sici)1097-0029(19970301)36:5<362::aid-jemt3>3.0.co;2-n

Cited by 15 publications

(1 citation statement)

References 5 publications

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“…Indeed there is a large variety of classical sample preparation techniques such as fracturing, mechanical polishing, broad ion milling, etc., that can be used to prepare high quality TEM specimens~Walck, 1996;McCaffrey & Barna, 1997!. However, they all share two major drawbacks: specimen faces are not coplanar and lamellae can be prepared only with limited site specificity.…”

Section: Introductionmentioning

confidence: 99%

Improved Focused Ion Beam Target Preparation of (S)TEM Specimen—A Method for Obtaining Ultrathin Lamellae

2012

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Specimen quality is vital to (scanning) transmission electron microscopy (TEM) investigations. In particular, thin specimens are required to obtain excellent high-resolution TEM images. Conventional focused ion beam (FIB) preparation methods cannot be employed to reliably create high quality specimens much thinner than 20 nm. We have developed a method for in situ target preparation of ultrathin TEM lamellae by FIB milling. With this method we are able to routinely obtain large area lamellae with coplanar faces, thinner than 10 nm. The resulting specimens are suitable for low kV TEM as well as scanning TEM. We have demonstrated atomic resolution by Cs-corrected high-resolution TEM at 20 kV on a FIB milled Si specimen only 4 nm thick; its amorphous layer measuring less than 1 nm in total.

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Section: Introductionmentioning

confidence: 99%

Improved Focused Ion Beam Target Preparation of (S)TEM Specimen—A Method for Obtaining Ultrathin Lamellae

2012

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Experiment Design Philosophy

2023

In‐Situ Transmission Electron Microscopy Experiments

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Preparation of high‐quality ultrathin transmission electron microscopy specimens of a nanocrystalline metallic powder

Riedl

Gemming

Mickel

et al. 2011

Microscopy Res & Technique

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This article explores the achievable transmission electron microscopy specimen thickness and quality by using three different preparation methods in the case of a high-strength nanocrystalline Cu-Nb powder alloy. Low specimen thickness is essential for spatially resolved analyses of the grains in nanocrystalline materials. We have found that single-sided as well as double-sided low-angle Ar ion milling of the Cu-Nb powders embedded into epoxy resin produced wedge-shaped particles of very low thickness (<10 nm) near the edge. By means of a modified focused ion beam lift-out technique generating holes in the lamella interior large micrometer-sized electron-transparent regions were obtained. However, this lamella displayed a higher thickness at the rim of ≥30 nm. Limiting factors for the observed thicknesses are discussed including ion damage depths, backscattering, and surface roughness, which depend on ion type, energy, current density, and specimen motion. Finally, sections cut by ultramicrotomy at low stroke rate and low set thickness offered vast, several tens of square micrometers uniformly thin regions of ∼10-nm minimum thickness. As major drawbacks, we have detected a thin coating on the sections consisting of epoxy deployed as the embedding material and considerable nanoscale thickness variations.

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Preparation of cross-sectional TEM samples for low-angle ion milling

Cited by 15 publications

References 5 publications

Improved Focused Ion Beam Target Preparation of (S)TEM Specimen—A Method for Obtaining Ultrathin Lamellae

Improved Focused Ion Beam Target Preparation of (S)TEM Specimen—A Method for Obtaining Ultrathin Lamellae

Experiment Design Philosophy

Preparation of high‐quality ultrathin transmission electron microscopy specimens of a nanocrystalline metallic powder

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