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Post-growth purification of Co nanostructures prepared by focused electron beam induced deposition

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 Publication date 2015
  fields Physics
and research's language is English




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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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Recently, focused electron beam induced deposition has been employed to prepare functional magnetic nanostructures with potential in nanomagnetic logic and sensing applications by using homonuclear precursor gases like Fe(CO)5 or Co2(CO)8. Here we show that an extension towards the fabrication of bi-metallic compounds is possible by using a single-source heteronuclear precursor gas. We have grown CoFe alloy magnetic nanostructures from the HFeCo3(CO)12 metal carbonyl precursor. The compositional analysis indicate that the samples contain about 80 at% of metal and 10 at% of carbon and oxygen. Four-probe magnetotransport measurements are carried out on nanowires of various sizes down to a width of 50 nm, for which the room temperature resistivity of 43~$muOmega$cm is found. Micro-Hall magnetometry reveals that 50~nm$times$250~nm nanobars of the material are ferromagnetic up to the highest measured temperature of 250 K. Finally, the TEM microstructural investigation shows that the deposits consist of a bcc Co-Fe phase mixed with a FeCo2O4 spinel oxide phase with nanograins of about 5 nm diameter.
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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.
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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.
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