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Register a new userAnalyzing Nanogranularity of Focused Electron-Beam-Induced Deposited (FEBID) Materials by Electron Tomography
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Nanogranular material systems are promising for a variety of applications in research and development. Their physical properties are often determined by grain sizes, shapes, mutual distances and by the chemistry of the embedding matrix With focused electron beam induced deposition arbitrarily shaped nanocomposite materials can be designed, where metallic, nanogranular structures are embedded in a carbonaceous matrix. Using post-growth electron beam curing, these materials can be tuned for improved electric transport or mechanical behavior. Such an optimization necessitates a thorough understanding and characterization of the internal changes in chemistry and morphology, which is where conventional projection based imaging techniques fall short. Here, we apply scanning transmission electron tomography to get a comprehensive picture of the distribution and morphology degree of embedded Pt nanograins after initial fabrication, and we demonstrate the impact of electron beam curing, which leads to condensed regions of interconnected metal nanograins.
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Focused electron beam induced deposition (FEBID) is a direct-write method for the fabrication of nanostructures whose lateral resolution rivals that of advanced electron lithography but is in addition capable of creating complex three-dimensional nano-architectures. Over the last decade several new developments in FEBID and focused electron beam induced processing (FEBIP) have led to a growing number of scientific contributions in solid state physics and materials science based on FEBID-specific materials and particular shapes and arrangements of the employed nanostructures. In this review an attempt is made to give a broad overview of these developments and the resulting contributions in various research fields encompassing mesoscopic physics with nanostructured metals at low temperatures, direct-write of superconductors and nano-granular alloys or intermetallic compounds and their applications, the contributions of FEBID to the field of metamaterials, and the application of FEBID structures for sensing of force or strain, dielectric changes or magnetic stray fields. The very recent development of FEBID towards simulation-assisted growth of complex three-dimensional nano-architectures is also covered. In the review particular emphasis is laid on conceptual clarity in the description of the different developments, which is reflected in the mostly schematic nature of the presented figures, as well as in the recurring final sub-sections for each of the main topics discussing the respective challenges and perspectives.
We have prepared iron microwires in a combination of focused electron beam induced deposition (FEBID) and autocatalytic growth from the iron pentacarbonyl, Fe(CO)5, precursor gas under UHV conditions. The electrical transport properties of the microwires were investigated and it was found that the temperature dependence of the longitudinal resistivity (rhoxx) shows a typical metallic behaviour with a room temperature value of about 88 micro{Omega} cm. In order to investigate the magnetotransport properties we have measured the isothermal Hall-resistivities in the range between 4.2 K and 260 K. From these measurements positive values for the ordinary and the anomalous Hall coefficients were derived. The relation between anomalous Hall resistivity (rhoAN) and longitudinal resistivity is quadratic, rhoAN rho^2 xx, revealing an intrinsic origin of the anomalous Hall effect. Finally, at low temperature in the transversal geometry a negative magnetoresistance of about 0.2 % was measured.
We demonstrate the use of individual magnetic nanowires (NWs), grown by focused electron beam induced deposition (FEBID), as scanning magnetic force sensors. Measurements of their mechanical susceptibility, thermal motion, and magnetic response show that the NWs posses high-quality flexural mechanical modes and a strong remanent magnetization pointing along their long axis. Together, these properties make the NWs excellent sensors of weak magnetic field patterns, as confirmed by calibration measurements on a micron-sized current-carrying wire and magnetic scanning probe images of a permalloy disk. The flexibility of FEBID in terms of the composition, geometry, and growth location of the resulting NWs, makes it ideal for fabricating scanning probes specifically designed for imaging subtle patterns of magnetization or current density.
Crystallography, the primary method for determining the three-dimensional (3D) atomic positions in crystals, has been fundamental to the development of many fields of science. However, the atomic positions obtained from crystallography represent a global average of many unit cells in a crystal. Here, we report, for the first time, the determination of the 3D coordinates of thousands of individual atoms and a point defect in a material by electron tomography with a precision of ~19 picometers, where the crystallinity of the material is not assumed. From the coordinates of these individual atoms, we measure the atomic displacement field and the full strain tensor with a 3D resolution of ~1nm^3 and a precision of ~10^-3, which are further verified by density functional theory calculations and molecular dynamics simulations. The ability to precisely localize the 3D coordinates of individual atoms in materials without assuming crystallinity is expected to find important applications in materials science, nanoscience, physics and chemistry.
In the majority of cases nanostructures prepared by focused electron beam induced deposition (FEBID) employing an organometallic precursor contain predominantly carbon-based ligand dissociation products. This is unfortunate with regard to using this high-resolution direct-write approach for the preparation of nanostructures for various fields, such as mesoscopic physics, micromagnetism, electronic correlations, spin-dependent transport and numerous applications. Here we present an in-situ cleaning approach to obtain pure Co-FEBID nanostructures. The purification procedure lies in the exposure of heated samples to a H$_2$ atmosphere in conjunction with the irradiation by low-energy electrons. The key finding is that the combination of annealing at $300^circ$C, H$_2$ exposure and electron irradiation leads to compact, carbon- and oxygen free Co layers down to a thickness of about 20,nm starting from as-deposited Co-FEBID structures. In addition to this, in temperature-dependent electrical resistance measurements on post-processed samples we find a typical metallic behavior. In low-temperature magneto-resistance and Hall effect measurements we observe ferromagnetic behavior.
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