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3D-investigations of electrically active interfaces in ZnO varistor materials have been performed using electron beam induced current (EBIC) contrast in the scanning electron microscope in combination with the focused ion beam workstation (FIB). The EBIC measurements were performed with spatial resolution better than 100 nm and the depth dependence of the signal was studied by variation of the acceleration voltage. The FIB was used for characterization of the subsurface geometry of electrically active grain boundaries. Experimental EBIC profiles, obtained by scanning the electron beam across grain boundaries, were compared with computer simulations using three different models for the electron–hole generation function. The EBIC contrast has been found to depend strongly on the geometric properties, i.e., the tilt of the grain boundary, and on asymmetries in the depletion region at the boundary. Calculations of the EBIC contrast taking these two effects into account show good agreement with experimental data. The “hot electron effect” close to the electrical breakdown voltage has been experimentally observed. The possibility to study asymmetry in the depletion region and the influence of the applied bias on the electrical properties of individual interfaces using the EBIC technique has been demonstrated. © 2002 American Institute of Physics.