NiO Test Specimens for Analytical Electron Microscopy: Round-Robin Results

Improvements in instrumentation for energy-dispersive X-ray microanalysis (EDX) and electron energy-loss spectroscopy (EELS) have underlined the need for suitable standards for measuring performance. We report the results from several laboratories that were supplied with a test specimen consisting of a thin film of nickel oxide supported on a molybdenum grid. The Ni-K_α/Mo-K_α count ratio was used as an indication of number of stray electrons and/or X-rays in the TEM column; the Ni-K_α peak/background ratio provided a measure of the total background in the EDX spectrum, including bremsstrahlung contributions and the effect of detector electronics. By providing values typical of current instrumentation, the results illustrate how the test specimen can be used to evaluate TEM/EDX systems prior to purchase, during installation, and (periodically) during operation. The NiO films were also used to test EELS acquisition and quantification procedures: measured Ni/O elemental ratios were all within 10% of stoichiometry.