Spectrum imaging of complex nanostructures using DualEELS: II. Absolute quantification using standards.

Nanometre-sized TixV(1-x)CyNz precipitates in an Fe20%Mn steel matrix with a thickness range from 14 to 40 nm are analysed using DualEELS. Their thicknesses, volumes and compositions are quantified using experimental binary standards and the process used to give robust results is described. Precisions of a few percent are achieved with accuracies that are estimated to be of a similar magnitude. Sensitivities are shown to be at 0.5-1 unit cells range in the thinnest matrix region, based on the assumption that a sub-lattice is fully populated by the element. It rises to the 1-2 unit cell range for the metals and 2-3 unit cells for the non-metal in the thickest matrix region. The sensitivities for Ti and N are greater than those for V and C respectively because the O K-edge from surface oxide needs to be separated from the V L2,3-edge, and the C K-edges from C in the matrix and amorphous C on the surface have to be separated from the C in the precipitate itself. Separation of the contributions from the bulk and the surface is demonstrated, showing that there is significant and detectable C in the matrix but no O, while there is significant O but little C in the surface oxide. Whilst applied to precipitates in steel in this work, the approach can be adapted to many multi-phase systems.

Accurate measurement of absolute experimental inelastic mean free paths and EELS differential cross-sections.

Methods are described for measuring accurate absolute experimental inelastic mean free paths and differential cross-sections using DualEELS. The methods remove the effects of surface layers and give the results for the bulk materials. The materials used are VC0.83, TiC0.98, VN0.97 and TiN0.88 but the method should be applicable to a wide range of materials. The data was taken at 200keV using a probe half angle of 29mrad and a collection angle of 36mrad. The background can be subtracted from under the ionisation edges, which can then be separated from each other. This is achieved by scaling Hartree-Slater calculated cross-sections to the edges in the atomic regions well above the threshold. The average scaling factors required are 1.00 for the non-metal K-edges and 1.01 for the metal L-edges (with uncertainties of a few percent). If preliminary measurements of the chromatic effects in the post-specimen lenses are correct, both drop to 0.99. The inelastic mean free path for TiC0.98 was measured as 103.6±0.5nm compared to the prediction of 126.9nm based on the widely used Iakoubovskii parameterisation.