In the present work, we have synthesized three-dimensional (3D) reduced graphene oxide nanosheets (rGO NSs) containing iron oxide nanoparticles (FeO NPs) hybrids (3D FeO/rGO) by one-pot microwave approach. Structural and morphological studies reveal that the as-synthesized FeO/rGO hybrids were composed of faceted FeO NPs induced into the interconnected network of rGO NSs. The morphologies and structures of the 3D hybrids have been characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Raman spectroscopy and X-ray photoelectron spectrometer (XPS). The electrochemical studies were analyzed by cyclic voltammetry, galvanostatic charge/discharge measurements, and electrochemical impedance spectroscopy, which demonstrate superior electrochemical performance as supercapacitors electrode application. The specific capacitances of 3D hybrid materials was 455 F g at the scan rate of 8 mV s, which is superior to that of bare FeO NPs. Additionally, the 3D hybrid shows good cycling stability with a retention ratio of 91.4 after starting from ∼190 cycles up to 9600 cycles. These attractive results suggest that this 3D FeO/rGO hybrid shows better performance as an electrode material for high-performance supercapacitors.

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An effective postgrowth electrical tuning, via an oxygen releasing method, to enhance the content of non-noble metals in deposits directly written with gas-assisted focused-electron-beam-induced deposition (FEBID) is presented. It represents a novel and reproducible method for improving the electrical transport properties of Co-C deposits. The metal content and electrical properties of Co-C-O nanodeposits obtained by electron-induced dissociation of volatile Co(CO) precursor adsorbate molecules were reproducibly tuned by applying postgrowth annealing processes at 100 °C, 200 °C, and 300 °C under high-vacuum for 10 min. Advanced thin film EDX analysis showed that during the annealing process predominantly oxygen is released from the Co-C-O deposits, yielding an atomic ratio of Co:C:O = 100:16:1 (85:14:1) with respect to the atomic composition of as-written Co:C:O = 100:21:28 (67:14:19). In-depth Raman analysis suggests that the amorphous carbon contained in the as-written deposit turns into graphite nanocrystals with size of about 22.4 nm with annealing temperature. Remarkably, these microstructural changes allow for tuning of the electrical resistivity of the deposits over 3 orders of magnitude from 26 mΩ cm down to 26 μΩ cm, achieving a residual resistivity of ρ/ρ = 0.56, close to the value of 0.53 for pure Co films with similar dimensions, making it especially interesting and advantageous over the numerous works already published for applications such as advanced scanning-probe systems, magnetic memory, storage, and ferroelectric tunnel junction memristors, as the graphitic matrix protects the cobalt from being oxidized under an ambient atmosphere.

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