Mass Sensing for the Advanced Fabrication of Nanomechanical Resonators.

We report on a nanomechanical engineering method to monitor matter growth in real time via e-beam electromechanical coupling. This method relies on the exceptional mass sensing capabilities of nanomechanical resonators. Focused electron beam-induced deposition (FEBID) is employed to selectively grow platinum particles at the free end of singly clamped nanotube cantilevers. The electron beam has two functions: it allows both to grow material on the nanotube and to track in real time the deposited mass by probing the noise-driven mechanical resonance of the nanotube. On the one hand, this detection method is highly effective as it can resolve mass deposition with a resolution in the zeptogram range; on the other hand, this method is simple to use and readily available to a wide range of potential users because it can be operated in existing commercial FEBID systems without making any modification. The presented method allows one to engineer hybrid nanomechanical resonators with precisely tailored functionalities. It also appears as a new tool for studying the growth dynamics of ultrathin nanostructures, opening new opportunities for investigating so far out-of-reach physics of FEBID and related methods.

NanoSQUID Magnetometry on Individual As-grown and Annealed Co Nanowires at Variable Temperature.

Performing magnetization studies on individual nanoparticles is a highly demanding task, especially when measurements need to be carried out under large sweeping magnetic fields or variable temperature. Yet, characterization under varying ambient conditions is paramount in order to fully understand the magnetic behavior of these objects, e.g., the formation of nonuniform states or the mechanisms leading to magnetization reversal and thermal stability. This, in turn, is necessary for the integration of magnetic nanoparticles and nanowires into useful devices, e.g., spin-valves, racetrack memories, or magnetic tip probes. Here, we show that nanosuperconducting quantum interference devices based on high critical temperature superconductors are particularly well suited for this task. We have successfully characterized a number of individual Co nanowires grown through focused electron beam induced deposition and subsequently annealed at different temperatures. Magnetization measurements performed under sweeping magnetic fields (up to ∼100 mT) and variable temperature (1.4-80 K) underscore the intrinsic structural and chemical differences between these nanowires. These point to significant changes in the crystalline structure and the resulting effective magnetic anisotropy of the nanowires, and to the nucleation and subsequent vanishing of antiferromagnetic species within the nanowires annealed at different temperatures.

Competition between Superconductor - Ferromagnetic stray magnetic fields in YBa2Cu3O7-x films pierced with Co nano-rods.

Superconductivity and ferromagnetism are two antagonistic phenomena that combined can lead to a rich phenomenology of interactions, resulting in novel physical properties and unique functionalities. Here we propose an original hybrid system formed by a high-temperature superconducting film, patterned with antidots, and with ferromagnetic nano-rods grown inside them. This particular structure exhibits the synergic influence of superconductor (SC) - ferromagnetic (FM) stray fields, in both the superconducting behaviour of the film and the three-dimensional (3D) magnetic structure of nano-rods. We show that FM stray fields directly influence the critical current density of the superconducting film. Additional functionalities appear due to the interaction of SC stray fields, associated to supercurrent loops, with the non-trivial 3D remanent magnetic structure of FM nano-rods. This work unravels the importance of addressing quantitatively the effect of stray magnetic fields from both, the superconductor and the ferromagnet in hybrid magnetic nano-devices based on high temperature superconductors.

55Mn NMR observation of colossal magnetoresistance effect in Sm0.55Sr0.45MnO3.

Temperature dependent 55Mn NMR study of Sm0.55Sr0.45MnO3 is reported. Previous bulk magnetization measurements have shown that below T C ~ 125 K the sample is ferromagnetic metallic (FMM) and above TC it is charge ordered and insulating. In present report, we show that from zero-field NMR a single line double-exchange (DE) signal is observed at temperatures up to 139 K, which is due to a presence of FMM clusters also above T C. The intensity of the DE line follows the temperature dependence of the magnetization measured at 0.01 T. When a magnetic field up to 2 T is applied at 139 K (i.e. 14 K above T C), a strong increase in NMR intensity of the DE line is observed indicating that content of FMM regions increases. This reveals that metallicity is induced in the material by the applied magnetic field and explains the observed colossal magnetoresistance (CMR) effect at the microscopic level. The observation agrees with previous results, which confirm that the percolation of the FMM clusters is responsible for the CMR effect. The shift of the resonant frequency in the applied field is three times smaller compared to decrease expected from gyromagnetic ratio, which indicates an antiferromagnetic coupling between the FMM clusters.

Plasmonic control of extraordinary optical transmission in the infrared regime.

We demonstrate that the spectral location of extraordinary optical transmission (EOT) resonances in metallic arrays of rectangular holes can be plasmonically tuned in the near and mid-infrared ranges. The experiments have been performed on patterned gold films. We focus on a subset of localized resonances occurring close to the cut-off wavelength of the holes, λ c. Metals are usually regarded as perfect electric conductors in the infrared regime, with an EOT cut-off resonance found around λ c = 2 L for rectangular holes (L being the long edge). For real metals, the penetration of the electromagnetic fields is simply seen as effectively enlarging L. However, by changing the hole short edge, we have found that λ c varies due to the excitation of gap surface plasmon polaritons. Finite-element calculations confirm that in these high aspect ratio rectangles with short edges two important aspects have to be taken into account in order to explain the experiments: the finite conductivity of the metal and the excitation of gap-surface plasmons inside the nanoholes.

Electrical conductivity of oxidized-graphenic nanoplatelets obtained from bamboo: effect of the oxygen content.

The large-scale production of graphene and reduced-graphene oxide (rGO) requires low-cost and eco-friendly synthesis methods. We employed a new, simple, cost-effective pyrolytic method to synthetize oxidized-graphenic nanoplatelets (OGNP) using bamboo pyroligneous acid (BPA) as a source. Thorough analyses via high-resolution transmission electron microscopy and electron energy-loss spectroscopy provides a complete structural and chemical description at the local scale of these samples. In particular, we found that at the highest carbonization temperature the OGNP-BPA are mainly in a sp(2) bonding configuration (sp(2) fraction of 87%). To determine the electrical properties of single nanoplatelets, these were contacted by Pt nanowires deposited through focused-ion-beam-induced deposition techniques. Increased conductivity by two orders of magnitude is observed as oxygen content decreases from 17% to 5%, reaching a value of 2.3 × 10(3) S m(-1) at the lowest oxygen content. Temperature-dependent conductivity reveals a semiconductor transport behavior, described by the Mott three-dimensional variable range hopping mechanism. From the localization length, we estimate a band-gap value of 0.22(2) eV for an oxygen content of 5%. This investigation demonstrates the great potential of the OGNP-BPA for technological applications, given that their structural and electrical behavior is similar to the highly reduced rGO sheets obtained by more sophisticated conventional synthesis methods.

Spin-to-charge conversion using Rashba coupling at the interface between non-magnetic materials.

The Rashba effect is an interaction between the spin and the momentum of electrons induced by the spin-orbit coupling (SOC) in surface or interface states. Its potential for conversion between charge and spin currents has been theoretically predicted but never clearly demonstrated for surfaces or interfaces of metals. Here we present experiments evidencing a large spin-charge conversion by the Bi/Ag Rashba interface. We use spin pumping to inject a spin current from a NiFe layer into a Bi/Ag bilayer and we detect the resulting charge current. As the charge signal is much smaller (negligible) with only Bi (only Ag), the spin-to-charge conversion can be unambiguously ascribed to the Rashba coupling at the Bi/Ag interface. This result demonstrates that the Rashba effect at interfaces can be used for efficient charge-spin conversion in spintronics.

Improvement of domain wall conduit properties in cobalt nanowires by global gallium irradiation.

Applications based on the movement of domain walls (DWs) in magnetic nanowires (NWs) require a good DW conduit behavior, i.e. a significant difference between DW nucleation and propagation fields. In this work, we have systematically studied how this property evolves in cobalt NWs grown by focused electron beam induced deposition (FEBID) as a function of global gallium irradiation, for irradiation doses up to 1.24 × 10(17) ions cm(-2). Whereas for high doses the DW conduit is lost, below 6.42 × 10(15) ions cm(-2) the difference between the two fields increases with irradiation, becoming up to ∼9 times larger than for non-irradiated wires, due to a strong increase in the nucleation field, while the propagation field remains approximately constant. This behavior stems from two effects. The first effect is a decrease in the magnetic volume of the parasitic halo around the NW, typically present in FEBID nanostructures, leading to the disappearance of weak nucleation centers. The second effect is the formation of a 20 nm outer shell with Co crystals about twice the size of those forming the NW core, causing a net increase of the local magnetocrystalline anisotropy. The results presented here are important for the potential use of magnetic NWs grown by FEBID in DW-based devices, and might also be of interest for magnetic NWs fabricated by other techniques.

Quantitative in situ magnetization reversal studies in Lorentz microscopy and electron holography.

A generalized procedure for the in situ application of magnetic fields by means of the excitation of the objective lens for magnetic imaging experiments in Lorentz microscopy and electron holography is quantitatively described. A protocol for applying magnetic fields with arbitrary in-plane magnitude and orientation is presented, and a freeware script for Digital Micrograph(™) is provided to assist the operation of the microscope. Moreover, a method to accurately reconstruct hysteresis loops is detailed. We show that the out-of-plane component of the magnetic field cannot be always neglected when performing quantitative measurements of the local magnetization. Several examples are shown to demonstrate the accuracy and functionality of the methods.

Magnetic field-induced dissipation-free state in superconducting nanostructures.

A superconductor in a magnetic field acquires a finite electrical resistance caused by vortex motion. A quest to immobilize vortices and recover zero resistance at high fields made intense studies of vortex pinning one of the mainstreams of superconducting research. Yet, the decades of efforts resulted in a realization that even promising nanostructures, utilizing vortex matching, cannot withstand high vortex density at large magnetic fields. Here, we report a giant reentrance of vortex pinning induced by increasing magnetic field in a W-based nanowire and a TiN-perforated film densely populated with vortices. We find an extended range of zero resistance with vortex motion arrested by self-induced collective traps. The latter emerge due to order parameter suppression by vortices confined in narrow constrictions by surface superconductivity. Our findings show that geometric restrictions can radically change magnetic properties of superconductors and reverse detrimental effects of magnetic field.

Correlations among magnetic, electrical and magneto-transport properties of NiFe nanohole arrays.

In this work, we use anodic aluminum oxide (AAO) templates to build NiFe magnetic nanohole arrays. We perform a thorough study of their magnetic, electrical and magneto-transport properties (including the resistance R(T), and magnetoresistance MR(T)), enabling us to infer the nanohole film morphology, and the evolution from granular to continuous film with increasing thickness. In fact, different physical behaviors were observed to occur in the thickness range of the study (2 nm < t < 100 nm). For t < 10 nm, an insulator-to-metallic crossover was visible in R(T), pointing to a granular film morphology, and thus being consistent with the presence of electron tunneling mechanisms in the magnetoresistance. Then, for 10 nm < t < 50 nm a metallic R(T) allied with a larger anisotropic magnetoresistance suggests the onset of morphological percolation of the granular film. Finally, for t > 50 nm, a metallic R(T) and only anisotropic magnetoresistance behavior were obtained, characteristic of a continuous thin film. Therefore, by combining simple low-cost bottom-up (templates) and top-down (sputtering deposition) techniques, we are able to obtain customized magnetic nanostructures with well-controlled physical properties, showing nanohole diameters smaller than 35 nm.

Magnetic properties of epitaxial discontinuous Fe/MgO multilayers.

We report magnetic, dynamic and transport properties of discontinuous metal-insulator multilayers Fe/MgO grown on amorphous Corning glass and single-crystalline MgO (001) substrates. The films of structure Substrate/MgO (3 nm)/[Fe (0.6 nm)/MgO (3.0 nm)] x 10 were prepared in ultra-high vacuum conditions using Pulsed Laser Deposition. It was shown that conditions of epitaxial growth are favorable for MgO substrates. As a result a substantial increase of tunneling magnetoresistance caused by spin-filtering effect was observed and reasonably theoretically explained. The value of TMR - 9.2% at room temperature in 18 kOe magnetic field is three times higher comparing to that for the samples grown on Corning glass substrates.

Tailoring the physical properties of thin nanohole arrays grown on flat anodic aluminum oxide templates.

The introduction of voids in a magnetic thin-film alters the stray field distribution and enables the tailoring of the corresponding physical properties. Here we present a detailed study on thin magnetic nanohole arrays (NhAs) grown on top of hexagonally-ordered anodic aluminum oxide (AAO) substrates. We address the effect of AAO topography on the corresponding electrical and magneto-transport properties. Optimization of the AAO topography led to NhAs with improved resistance and magnetoresistance responses, while retaining their most important feature of enhanced coercivity. This opens new pathways for the growth of more complex structures on AAO substrates, a crucial aspect for their technological viability.

Quantitative biomolecular sensing station based on magnetoresistive patterned arrays.

The combination of magnetoresistive sensors and magnetic labeling of bioanalytes, which are selectively captured by their complementary antibody in the proximity of the sensor is a powerful method in order to attain truly quantitative immunological assays. In this paper we present a technical solution to exploit the existing spin valve technology to readout magnetic signals of bio-functionalized magnetic nanoparticles. The method is simple and reliable, and it is based on a discrete scan of lateral flow strips with a precise control of the contact force between sensor and sample. It is shown that the signal of the sensor is proportional to the local magnetization produced by the nanoparticles in a wide range of concentrations, and the sensitivity thresholds in both calibration samples and real immunorecognition assays of human chorionic gonadotropin hormone are well below the visual inspection limit (5.5 ng/ml). Furthermore the sample scanning approach and the reduced dimensions of the sensors provide unprecedented spatial resolution of the nanoparticle distribution across the supporting nitrocellulose strip, therefore enabling on-stick control references and multi-analyte capability.

Correlation between the magnetic imaging of cobalt nanoconstrictions and their magnetoresistance response.

Scanning transmission x-ray microscopy (STXM) and magnetoresistance (MR) measurements are used to investigate the magnetic behavior of a nanoconstriction joining two micrometric electrodes (a pad and a wire). The reversal of the magnetization under variable external static magnetic fields is imaged. By means of a detailed analysis of the STXM images at the nanocontact area, the MR is calculated, based on diffusive anisotropic-MR. This MR agrees well with that obtained from electrical transport measurements, allowing a direct correlation between the MR signal and the magnetic reversal of the system. The magnetization behavior depends on the sample thickness and constriction dimensions. In 40 nm-thick samples, with 20 × 175 nm(2) contact areas, the magnetization at the two sides of the constriction forms a net angle of 90°, with a progressive evolution of the magnetization structure between the electrodes during switching. The MR in those cases has a more peaked shape than with 20 nm-thick electrodes and 10 × 80 nm(2) contact areas, where the magnetization forms 180° between them, with a wide domain wall pinned at the constriction. As a consequence of this configuration, a plateau in the MR is observed for about 20 Oe.

Focused electron beam induced etching of titanium with XeF2.

Titanium is a relevant technological material due to its extraordinary mechanical and biocompatible properties, its nanopatterning being an increasingly important requirement in many applications. We report the successful nanopatterning of titanium by means of focused electron beam induced etching using XeF(2) as a precursor gas. Etch rates up to 1.25 × 10(-3) µm(3) s(-1) and minimum pattern sizes of 80 nm were obtained. Different etching parameters such as beam current, beam energy, dwell time and pixel spacing are systematically investigated, the etching process being optimized by decreasing both the beam current and the beam energy. The etching mechanism is investigated by transmission electron microscopy. Potential applications in nanotechnology are discussed.

Direct observation of stress accumulation and relaxation in small bundles of superconducting vortices in tungsten thin films.

We study the behavior of bundles of superconducting vortices when increasing the magnetic field using scanning tunneling microscopy and spectroscopy at 100 mK. Pinning centers are given by features on the surface corrugation. We find strong net vortex motion in a bundle towards a well-defined direction. We observe continuous changes of the vortex arrangements, and identify small displacements, which stress and deform the vortex bundle, separated by larger rearrangements or avalanches, which release accumulated stress.

Fe:O:C grown by focused-electron-beam-induced deposition: magnetic and electric properties.

We systematically study the effect of oxygen content on the magneto-transport and microstructure of Fe:O:C nanowires deposited by focused-electron-beam-induced (FEBID) deposition. The Fe/O ratio can be varied with an Fe content varying between ∼ 50 and 80 at.% with overall low C content (≈16 ± 3 at.%) by adding H(2)O during the deposition while keeping the beam parameters constant as measured by energy dispersive x-ray (EDX) spectroscopy. The room-temperature magnetic properties for deposits with an Fe content of 66-71 at.% are investigated using the magneto-optical Kerr effect (MOKE) and electric magneto-transport measurements. The nanostructure of the deposits is investigated through cross-sectional high-resolution transmission electron microscopy (HRTEM) imaging, allowing us to link the observed magneto-resistance and resistivity to the transport mechanism in the deposits. These results demonstrate that functional magnetic nanostructures can be created, paving the way for new magnetic or even spintronics devices.

Determination of the percolation threshold in Fe/MgO magnetic granular multilayers.

The evolution of the morphology, magnetic and transport properties of Fe(t nm)/MgO(3.0 nm) multilayers with respect to the nominal metallic layer thickness was investigated. A comparison with existing experimental data on discontinuous metal-insulator multilayers, ultrathin epitaxial Fe films on MgO substrates and granular cermet films is made. It is confirmed that the deposition conditions and the material composition play a crucial role in the percolation process. Nominal thicknesses of Fe layers at which an infinite metallic cluster is formed and the conditions for continuous Fe coverage were determined. Different methods of percolation threshold detection were analysed. We show that investigation of the temperature dependence of resistance in nanostructures could lead to an overestimation of the percolation threshold value, while magnetic measurements alone could lead to its underestimation.

Magnetization reversal in individual cobalt micro- and nanowires grown by focused-electron-beam-induced-deposition.

We systematically study individual micro- and nanometric polycrystalline cobalt wires grown by focused-electron-beam-induced-deposition. The deposits were grown in a range of aspect ratios varying from 1 up to 26. The minimum lateral dimension of the nanowires was 150 nm, for a thickness of 40 nm. Atomic force microscopy images show beam-current-dependent profiles, associated with different regimes of deposition. The magnetization reversal of individual nanowires is studied by means of the spatially resolved magneto-optical Kerr effect. Abrupt switching is observed, with a systematic dependence on the wire's dimensions. This dependence of the coercive field is understood in magnetostatic terms, and agrees well with previous results on cobalt wires grown with different techniques. The influence of compositional gradients along the structural profile on the magnetic reversal is studied by using micromagnetic simulations. This work demonstrates the feasibility of using this technique to fabricate highly pure magnetic nanostructures, and highlights the advantages and disadvantages of the technique with respect to more conventional ones.