A guide on FIB preparation of samples containing stress corrosion crack tips for TEM and atom-probe analysis.

The preparation of samples containing stress corrosion crack tips for 3D atom-probe tomography and transmission electron microscopy is of ultimate importance for understanding the mechanisms controlling crack propagation. In this paper, it will be shown that a focused ion beam machine equipped with an in situ micromanipulator is an ideal tool to systematically prepare such demanding samples. The methodology is described and discussed in detail, and several results are presented to demonstrate the potential of the technique.

[1]  R. Egerton.  Electron Energy-Loss Spectroscopy in the Electron Microscope , 1995, Springer US.

[2]  J. Titchmarsh,et al.  TEM investigations of intergranular stress corrosion cracking in austenitic alloys in PWR environmental conditions , 2003 .

[3]  L. E. Thomas,et al.  High‐resolution analytical electron microscopy characterization of corrosion and cracking at buried interfaces , 2001 .

[4]  John H. Booske,et al.  Three-dimensional atom mapping of dopants in Si nanostructures , 2005 .

[5]  K. Thompson,et al.  Observations of Si field evaporation. , 2007, Ultramicroscopy.

[6]  N. Browning,et al.  Atomic‐resolution electron energy‐loss spectroscopy in the scanning transmission electron microscope , 1995 .

[7]  Alfred Cerezo,et al.  Performance of an energy-compensated three-dimensional atom probe , 1998 .

[8]  K. F. Russell,et al.  Atom probe specimen preparation with a dual beam SEM/FIB miller. , 2007, Ultramicroscopy.

[9]  S. Ringer,et al.  Site-specific specimen preparation for atom probe tomography of grain boundaries , 2007 .

[10]  A. Petford-Long,et al.  Preparation of transmission electron microscopy cross-section specimens using focused ion beam milling , 2001 .

[11]  C. Grovenor,et al.  High-resolution imaging of complex crack chemistry in reactor steels by NanoSIMS , 2008 .

[12]  A. Petford-Long,et al.  Preparation of site specific transmission electron microscopy plan-view specimens using a focused ion beam system , 2001 .

[13]  M. Jenkins,et al.  Preparation of transmission electron microscopy cross‐section specimens of crack tips using focused ion beam milling , 2002, Journal of microscopy.

[14]  Alfred Cerezo,et al.  Atom probe tomography today , 2007 .

[15]  C. Grovenor,et al.  Using NanoSIMS to map trace elements in stainless steels from nuclear reactors , 2008 .

[16]  M. Sugiyama,et al.  Development of Atom Probe Specimem Preparation Techniques for Specific Regions in Steel Marterials , 2006, 2006 19th International Vacuum Nanoelectronics Conference.

[17]  Alfred Cerezo,et al.  Improvements in the mass resolution of the three-dimensional atom probe , 1996 .

[18]  D Lawrence,et al.  In situ site-specific specimen preparation for atom probe tomography. , 2007, Ultramicroscopy.

[19]  J. D. Olson,et al.  First Data from a Commercial Local Electrode Atom Probe (LEAP) , 2004, Microscopy and Microanalysis.

[20]  S. Ringer,et al.  Atom Probe Specimen Fabrication Methods using a Dual FIB/SEM , 2006, 2006 19th International Vacuum Nanoelectronics Conference.

[21]  S. Lozano-Perez.  Novel characterization of stress corrosion cracks , 2008 .