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

Highlights: • Quantitative nanoanalysis of nanometre-sized precipitates in a steel matrix. • Spectral fitting using standards is superior to traditional quantification approaches. • Composition, thickness and volume with a precision and accuracy of a few percent. • Carbon in matrix detectable, and surface oxide composition also quantified. • Detection sensitivity around the 1 unit cell level for most elements in the precipitate. ABSTRACTNanometre-sized Ti_xV_(1−x)C_yN_z 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 L_2,3-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.