In situ transmission electron microscope (TEM) characterization techniques provide valuable information on structure–property correlations to understand the behavior of materials at the nanoscale. However, understanding nanoscale structures and their interaction with the electron beam is pivotal for the reliable interpretation of in situ/ex situ TEM studies. Here, we report that oxides commonly used in nanoelectronic applications, such as transistor gate oxides or memristive devices, are prone to electron beam induced damage that causes small structural changes even under very low dose conditions, eventually changing their electrical properties as examined via in situ measurements. In this work, silicon, titanium, and niobium oxide thin films are used for in situ TEM electrical characterization studies. The electron beam induced reduction of the oxides turns these insulators into conductors. The conductivity change is reversible by exposure to air, supporting the idea of electron beam reduction of oxides as primary damage mechanism. Through these measurements we propose a limit for the critical dose to be considered for in situ scanning electron microscopy and TEM characterization studies.

Ferroelectric oxide memristors are currently in the highlights of a thriving area of research aiming at the development of nonvolatile, adaptive memories for applications in neuromorphic computing. However, to date a precise control of synapse‐like functionalities by adjusting the interplay between ferroelectric polarization and resistive switching processes is still an ongoing challenge. Here, it is shown that by means of controlled electron beam radiation, a prototypical ferroelectric film of BaTiO3 can be turned into a memristor with multiple configurable resistance states. Ex situ and in situ analyses of current/voltage characteristics upon electron beam exposure confirm the quasi‐continuous variation of BaTiO3 resistance up to two orders of magnitude under the typical experimental conditions employed in electron beam patterning and characterization techniques. These results demonstrate an unprecedented effective route to locally and scalably engineering multilevel ferroelectric memristors via application of moderate electron beam radiation.

Memristors based on a double barrier design have been analysed by various nano spectroscopic methods to unveil details about its microstructure and conduction mechanism.The device consists of an AlO x tunnel barrier and a NbO y /Au Schottky barrier sandwiched between Nb bottom electrode and Au top electrode. As it was anticipated that the local chemical composition of the tunnel barrier, i.e. oxidation state of the metals as well as concentration and distribution of oxygen ions, have a major influence on electronic conduction, these factors were carefully analysed. A combined approach was chosen in order to reliably investigate electronic states of Nb and O by electron energy-loss spectroscopy as well as map elements whose transition edges exhibit a different energy range by energydispersive X-ray spectroscopy like Au and Al. The results conclusively demonstrate significant oxidation of the bottom electrode as well as a small oxygen vacancy concentration in the Al oxide tunnel barrier. Possible scenarios to explain this unexpected additional oxide layer are discussed and kinetic Monte Carlo simulations were applied in order to identify its influence on conduction mechanisms in the device. In light of the strong deviations between observed and originally sought layout, this study highlights the robustness in terms of structural deviations of the double barrier memristor device.

This communication is to elucidate the state-of-the-art of techniques necessary to gather information on a new class of nanoelectronic devices known as memristors and related resistive switching devices, respectively. Unlike classical microelectronic devices such as transistors, the chemical and structural variations occurring upon switching of memristive devices require cutting-edge electron microscopy techniques. Depending on the switching mechanism, some memristors call for the acquisition of atomically resolved structural data, while others rely on atomistic chemical phenomena requiring the application of advanced X-ray and electron spectroscopy to correlate the real structure with properties. Additionally, understanding resistive switching phenomena also necessitates the application not only of pre-and post-operation analysis, but also during the process of switching. This highly challenging in situ characterization also requires the aforementioned techniques while simultaneously applying an electrical bias. Through this review we aim to give an overview of the possibilities and challenges as well as an outlook onto future developments in the field of nanoscopic characterization of memristive devices.

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