EEL spectroscopic tomography: Towards a new dimension in nanomaterials analysis

Electron tomography is a widely spread technique for recovering the three dimensional (3D) shape of nanostructured materials. Using a spectroscopic signal to achieve a reconstruction adds a fourth chemical dimension to the 3D structure. Up to date, energy filtering of the images in the transmission electron microscope (EFTEM) is the usual spectroscopic method even if most of the information in the spectrum is lost. Unlike EFTEM tomography, the use of electron energy-loss spectroscopy (EELS) spectrum images (SI) for tomographic reconstruction retains all chemical information, and the possibilities of this new approach still remain to be fully exploited. In this article we prove the feasibility of EEL spectroscopic tomography at low voltages (80 kV) and short acquisition times from data acquired using an aberration corrected instrument and data treatment by Multivariate Analysis (MVA), applied to FexCo(3−x)O4@Co3O4 mesoporous materials. This approach provides a new scope into materials; the recovery of full EELS signal in 3D.

► EELS–SI tomography was performed at low voltage and low acquisition times.
► MVA has been applied for noise reduction and information extraction.
► Tomographic reconstruction has been achieved for chemical information.
► Elemental distribution extraction in 3D has been proved.