Production of Fe nanoparticles from γ-Fe2O3 by high-pressure hydrogen reduction.

In this work, the reduction of iron oxide γ-Fe2O3 nanoparticles by hydrogen at high pressures is studied. Increasing the hydrogen pressure enables reduction of γ-Fe2O3 to α-Fe at significantly lower temperatures. At low pressures, a temperature of 390 °C is necessary whereas at 530 bar complete reduction can be realized at temperatures as low as 210 °C. This leads to significant improvement in the final particle morphology, maintaining high surface-to-volume ratio of the nanoparticles with an average size of 47 ± 5 nm which is close to that of the precursor γ-Fe2O3. Neck formation, coalescence and growth during reduction can be significantly suppressed. Investigations of magnetic properties show that saturation magnetization of the reduced α-Fe nanoparticles decreases with particle size from 209 A m2 kg-1 at 390 °C reduction temperature to 204 A m2 kg-1 at 210 °C. Coercivity for the fine iron particles reaches 0.076 T which exceeds the theoretical anisotropy field. This is attributed to nano-scale surface effects.

FIB based fabrication of an operative Pt/HfO2/TiN device for resistive switching inside a transmission electron microscope.

Recent advances in microelectromechanical systems (MEMS) based chips for in situ transmission electron microscopy are opening exciting new avenues in nanoscale research. The capability to perform current-voltage measurements while simultaneously analyzing the corresponding structural, chemical or even electronic structure changes during device operation would be a major breakthrough in the field of nanoelectronics. In this work we demonstrate for the first time how to electrically contact and operate a lamella cut from a resistive random access memory (RRAM) device based on a Pt/HfO2/TiN metal-insulator-metal (MIM) structure. The device was fabricated using a focused ion beam (FIB) instrument and an in situ lift-out system. The electrical switching characteristics of the electron-transparent lamella were comparable to a conventional reference device. The lamella structure was initially found to be in a low resistance state and could be reset progressively to higher resistance states by increasing the positive bias applied to the Pt anode. This could be followed up with unipolar set/reset operations where the current compliance during set was limited to 400 µA. FIB structures allowing to operate and at the same time characterize electronic devices will be an important tool to improve RRAM device performance based on a microstructural understanding of the switching mechanism.