Imaging of fullerene-like structures in CNx thin films by electron microscopy; Sample preparation artefacts due to ion-beam milling

Zs Czigány, J. Neidhardt, I. F. Brunell, L. Hultman

Research output: Contribution to journalArticle

21 Citations (Scopus)

Abstract

The microstructure of CNx thin films, deposited by reactive magnetron sputtering, was investigated by transmission electron microscopy (TEM) at 200kV in plan-view and cross-sectional samples. Imaging artefacts arise in high-resolution TEM due to overlap of nm-sized fullerene-like features for specimen thickness above 5nm. The thinnest and apparently artefact-free areas were obtained at the fracture edges of plan-view specimens floated-off from NaCl substrates. Cross-sectional samples were prepared by ion-beam milling at low energy to minimize sample preparation artefacts. The depth of the ion-bombardment-induced surface amorphization was determined by TEM cross sections of ion-milled fullerene-like CNx surfaces. The thickness of the damaged surface layer at 5° grazing incidence was 13 and 10nm at 3 and 0.8keV, respectively, which is approximately three times larger than that observed on Si prepared under the same conditions. The shallowest damage depth, observed for 0.25keV, was less than 1nm. Chemical changes due to N loss and graphitization were also observed by X-ray photoelectron spectroscopy. As a consequence of chemical effects, sputtering rates of CNx films were similar to that of Si, which enables relatively fast ion-milling procedure compared to carbon compounds. No electron beam damage of fullerene-like CNx was observed at 200kV.

Original languageEnglish
Pages (from-to)163-173
Number of pages11
JournalUltramicroscopy
Volume94
Issue number3-4
DOIs
Publication statusPublished - Apr 1 2003

Keywords

  • Fullerene structures
  • HRTEM
  • Ion-bombardment-induced amorphization
  • Low-energy ion-milling

ASJC Scopus subject areas

  • Electronic, Optical and Magnetic Materials
  • Atomic and Molecular Physics, and Optics
  • Instrumentation

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