Technique for preparing cross‐section transmission electron microscope specimens from ion‐irradiated ceramics

Abstract

The general techniques necessary to produce a high-quality cross-sectioned ceramic specimen for transmission electron microscope observation are outlined. A particularly important point is that the width of the glued region between faces of the ceramic specimen must be less than 0.2 micron to prevent loss of the near-surface region during ion milling. A recently developed vise for gluing ceramic cross-section specimens is described, and some examples of the effect of glue thickness on specimen quality are shown.

Influence of irradiation spectrum and implanted ions on the amorphization of ceramics

“…Following irradiation, cross-section transmission electron microscope ( E M ) specimens were prepared by gluing the specimens face to face with a similar mechanically polished nonirradiated specimen, sectioning perpendicular to the irradiation surface, mechanical dimpling, and ion milling in a liquid nitrogen cooled stage (6 keV Ar+ ions, 15" sputtering angle) until perforation occurred at the glued interface [37]. The specimens were examined by TEM using a Philips CM12 microscope operating at 120 kV.…”

Effect of H and He irradiation on cavity formation and blistering in ceramics

“…1 shows the calculated (SRIM 2008 [21]) depth-dependent displacement damage and implanted gas ion profiles for 1 MeV H and He irradiated Al 2 O 3 for ion fluences of 1 Â 10 22 /m 2 . The maximum exposure fluences in this study were 1.7 Â 10 22 H/m 2 and 1 Â 10 22 He/m 2 , which correspond to calculated [21] peak damage and implanted gas ion concentrations of $3 dpa and $30 at.% H ($1 Â 10 5 appm H/dpa) and $34 dpa and $54 at.% He ($1.6 Â 10 4 appm He/dpa) for 1 MeV H and 1 MeV He ions, respectively, assuming an average displacement energy of 40 eV for all of the elements in the ceramics in this study. The minimum investigated H and He fluences in this study were $1 Â 10 21 /m 2 ($2 at.% H and $5 at.% He at peak implantation region).…”

“…Selected samples were prepared for cross-section transmission electron microscopy (TEM) using techniques that are described elsewhere [22]. The TEM specimens were examined in a Philips CM-12 or CM-30 electron microscope, operating at 120 and 300 keV, respectively.…”

Preparation for TEM of layered samples with fragile microstructure and weak layer interface

“…Zinkle et al (1991) point out that a too wide layer will lead to damage to the cross-section due to the fast milling rate of the glue. Before electron transparency was reached in the right area, the glue became very thin and did not protect the outer layer of the cross-section.…”