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A direct nanowriting procedure using helium- and neon-focused ion beams and spin-coated organometallic thin films is introduced and applied to the fabrication of Pd-enriched metallic structures in a single lithography step. This process presents significant advantages over multi-step resist-based lithography and focused beam-induced deposition using gaseous precursors, such as its simplicity and speed, respectively. The optimized process leads to Pd-rich structures with low electrical resistivity values of 141 and 152 μΩ cm under Ne + or He + fluences of 1000 and 5000 μC cm -2 , respectively. These resistivity values correlate well with compositional and microstructural studies, indicating a high Pd metallic content in a dense structure with a few-nm grain size. The obtained results are compared to similar structures fabricated by direct electron and gallium beam nanowriting, demonstrating the full potential of nanopatterned Pd-based organometallic thin films under the most common focused charged beams. The practical applications of combining spin-coated organometallic thin films with focused beam nanowriting in micro- and nano-lithography modern procedures are also discussed in this contribution.

The vast repository of van der Waals (vdW) materials supporting polaritons offers numerous possibilities to tailor electromagnetic waves at the nanoscale. The development of twistoptics-the modulation of the optical properties by twisting stacks of vdW materials-enables directional propagation of phonon polaritons (PhPs) along a single spatial direction, known as canalization. Here we demonstrate a complementary type of directional propagation of polaritons by reporting the visualization of unidirectional ray polaritons (URPs). They arise naturally in twisted hyperbolic stacks with very different thicknesses of their constituents, demonstrated for homostructures of α -MoO 3 and heterostructures of α -MoO 3 and β -Ga 2 O 3 . Importantly, their ray-like propagation, characterized by large momenta and constant phase, is tunable by both the twist angle and the illumination frequency. Apart from their fundamental importance, our findings introduce twisted asymmetric stacks as efficient platforms for nanoscale directional polariton propagation, opening the door for applications in nanoimaging, (bio)-sensing, or polaritonic thermal management., (© 2024. The Author(s).)

Recent advances in quantum technologies are highly influencing the current technological scenario. Hybrid devices combining superconductors and topological insulators represent an excellent opportunity to study the topological superconducting phase, which offers interesting features that might have significant implications in the development of quantum sensing and quantum computing. Furthermore, focused ion beam techniques, whose versatility enables to create sophisticated devices with high degree of customization, can enhance the creation of complex devices. Here, we develop a novel approach for creating single-crystal devices that is applied to the fabrication of superconducting devices based on topological insulator Bi 2 Se 3 in a geometry characteristic of a superconducting quantum interference device. Characterization of these devices reveals that superconductivity is induced in our crystal and the supercurrent is modulated by applying an external magnetic field. These results open the way to tailoring the response of hybrid devices that combine superconductors and topological insulators by focused ion beam techniques., (© 2024. The Author(s).)

The investigation of precursor classes for the fabrication of nanostructures is of specific interest for maskless fabrication and direct nanoprinting. In this study, the differences in material composition depending on the employed process are illustrated for focused-ion-beam- and focused-electron-beam-induced deposition (FIBID/FEBID) and compared to the thermal decomposition in chemical vapor deposition (CVD). This article reports on specific differences in the deposit composition and microstructure when the (H 3 Si) 2 Fe(CO) 4 precursor is converted into an inorganic material. Maximum metal/metalloid contents of up to 90 at. % are obtained in FIBID deposits and higher than 90 at. % in CVD films, while FEBID with the same precursor provides material containing less than 45 at. % total metal/metalloid content. Moreover, the Fe:Si ratio is retained well in FEBID and CVD processes, but FIBID using Ga + ions liberates more than 50% of the initial Si provided by the precursor. This suggests that precursors for FIBID processes targeting binary materials should include multiple bonding such as bridging positions for nonmetals. In addition, an in situ method for investigations of supporting thermal effects of precursor fragmentation during the direct-writing processes is presented, and the applicability of the precursor for nanoscale 3D FEBID writing is demonstrated., Competing Interests: The authors declare no competing financial interest., (© 2024 American Chemical Society.)

Graphene is one of the most extensively studied 2D materials, exhibiting extraordinary mechanical and electronic properties. Although many years have passed since its discovery, manipulating single graphene layers is still challenging using standard resist-based lithography techniques. Recently, it has been shown that it is possible to etch graphene directly in water-assisted processes using the so-called focused electron-beam-induced etching (FEBIE), with a spatial resolution of ten nanometers. Nanopatterning graphene with such a method in one single step and without using a physical mask or resist is a very appealing approach. During the process, on top of graphene nanopatterning, we have found significant morphological changes induced in the SiO 2 substrate even at low electron dose values (<8 nC/μm 2 ). We demonstrate that graphene etching and topographical changes in SiO 2 substrates can be controlled via electron beam parameters such as dwell time and dose., (Copyright © 2024, Szkudlarek et al.)

We demonstrate the fabrication of sharp nanopillars of high aspect ratio onto specialized atomic force microscopy (AFM) microcantilevers and their use for high-speed AFM of DNA and nucleoproteins in liquid. The fabrication technique uses localized charged-particle-induced deposition with either a focused beam of helium ions or electrons in a helium ion microscope (HIM) or scanning electron microscope (SEM). This approach enables customized growth onto delicate substrates with nanometer-scale placement precision and in situ imaging of the final tip structures using the HIM or SEM. Tip radii of <10 nm are obtained and the underlying microcantilever remains intact. Instead of the more commonly used organic precursors employed for bio-AFM applications, we use an organometallic precursor (tungsten hexacarbonyl) resulting in tungsten-containing tips. Transmission electron microscopy reveals a thin layer of carbon on the tips. The interaction of the new tips with biological specimens is therefore likely very similar to that of standard carbonaceous tips, with the added benefit of robustness. A further advantage of the organometallic tips is that compared to carbonaceous tips they better withstand UV-ozone cleaning treatments to remove residual organic contaminants between experiments, which are inevitable during the scanning of soft biomolecules in liquid. Our tips can also be grown onto the blunted tips of previously used cantilevers, thus providing a means to recycle specialized cantilevers and restore their performance to the original manufacturer specifications. Finally, a focused helium ion beam milling technique to reduce the tip radii and thus further improve lateral spatial resolution in the AFM scans is demonstrated.

High-resolution micro- and nanostructures can be grown using Focused Electron Beam Induced Deposition (FEBID), a direct-write, resist-free nanolithography technology which allows additive patterning, typically with sub-100 nm lateral resolution, and down to 10 nm in optimal conditions. This technique has been used to grow magnetic tips for use in Magnetic Force Microscopy (MFM). Due to their high aspect ratio and good magnetic behavior, these FEBID magnetic tips provide several advantages over commercial magnetic tips when used for simultaneous topographical and magnetic measurements. Here, we report a study of the durability of these excellent candidates for high-resolution MFM measurements. A batch of FEBID-grown magnetic tips was subjected to a systematic analysis of MFM magnetic contrast for 30 weeks, using magnetic storage tape as a test specimen. Our results indicate that these FEBID magnetic tips operate effectively over a long period of time. The magnetic signal was well preserved, with a maximum reduction of 60% after 21 weeks of recurrent use. No significant contrast degradation was observed after 30 weeks in storage.

Epitaxial strain modifies the physical properties of thin films deposited on single-crystal substrates. In a previous work, we demonstrated that in the case of La 2/3 Ca 1/3 MnO 3 thin films the strain induced by the substrate can produce the segregation of a non-ferromagnetic layer (NFL) at the top surface of ferromagnetic epitaxial La 2/3 Ca 1/3 MnO 3 for a critical value of the tetragonality τ, defined as τ = | c - a | a , of τ C ≈ 0.024. Although preliminary analysis suggested its antiferromagnetic nature, to date a complete characterization of the magnetic state of such an NFL has not been performed. Here, we present a comprehensive magnetic characterization of the strain-induced segregated NFL. The field-cooled magnetic hysteresis loops exhibit an exchange bias mechanism below T ≈ 80 K, which is well below the Curie temperature of the ferromagnetic La 2/3 Ca 1/3 MnO 3 layer. The exchange bias and coercive fields decay exponentially with temperature, which is commonly accepted to describe spin-glass (SG) behavior. The signatures of slow dynamics were confirmed by slow spin relaxation over a wide temperature regime. Low-energy muon spectroscopy experiments directly evidence the slowing down of the magnetic moments below ~100 K in the NFL. The experimental results indicate the SG nature of the NFL. This SG state can be understood within the context of the competing ferromagnetic and antiferromagnetic interactions of similar energies.

NanoSQUIDs are quantum sensors that excel in detecting a small change in magnetic flux with high sensitivity and high spatial resolution. Here, we employ resist-free direct-write Ga + Focused Ion Beam Induced Deposition (FIBID) techniques to grow W-C nanoSQUIDs, and we investigate their electrical response to changes in the magnetic flux. Remarkably, FIBID allows the fast (3 min) growth of 700 nm × 300 nm nanoSQUIDs based on narrow nanobridges (50 nm wide) that act as Josephson junctions. Albeit the SQUIDs exhibit a comparatively low modulation depth and obtain a high inductance, the observed transfer coefficient (output voltage to magnetic flux change) is comparable to other SQUIDs (up to 1300 μV/ Φ 0 ), which correlates with the high resistivity of W-C in the normal state. We discuss here the potential of this approach to reduce the active area of the nanoSQUIDs to gain spatial resolution as well as their integration on cantilevers for scanning-SQUID applications., Competing Interests: There are no conflicts to declare., (This journal is © The Royal Society of Chemistry.)

Background : The use of a focused ion beam to decompose a precursor gas and produce a metallic deposit is a widespread nanolithographic technique named focused ion beam induced deposition (FIBID). However, such an approach is unsuitable if the sample under study is sensitive to the somewhat aggressive exposure to the ion beam, which induces the effects of surface amorphization, local milling, and ion implantation, among others. An alternative strategy is that of focused electron beam induced deposition (FEBID), which makes use of a focused electron beam instead, and in general yields deposits with much lower metallic content than their FIBID counterparts. Methods : In this work, we optimize the deposition of tungsten-carbon (W-C) nanowires by FEBID to be used as electrical contacts by assessing the impact of the deposition parameters during growth, evaluating their chemical composition, and investigating their electrical response. Results : Under the optimized irradiation conditions, the samples exhibit a metallic content high enough for them to be utilized for this purpose, showing a room-temperature resistivity of 550 μΩ cm and maintaining their conducting properties down to 2 K. The lateral resolution of such FEBID W-C metallic nanowires is 45 nm. Conclusions : The presented optimized procedure may prove a valuable tool for the fabrication of contacts on samples where the FIBID approach is not advised., Competing Interests: No competing interests were disclosed., (Copyright: © 2022 Orús P et al.)

The ability to create metallic patterned nanostructures with excellent control of size, shape and spatial orientation is of utmost importance in the construction of next-generation electronic and optical devices as well as in other applications such as (bio)sensors, reactive surfaces for catalysis, etc. Moreover, development of simple, rapid and low-cost fabrication processes of metallic patterned nanostructures is a challenging issue for the incorporation of such devices in real market applications. In this contribution, a direct-write method that results in highly conducting palladium-based nanopatterned structures without the need of applying subsequent curing processes is presented. Spin-coated films of palladium acetate were irradiated with an electron beam to produce palladium nanodeposits (PdNDs) with controlled size, shape and height. The use of different electron doses was investigated and its influence on the PdNDs features determined, namely: (1) thickness of the deposits, (2) atomic percentage of palladium content, (3) oxidation state of palladium in the deposit, (4) morphology of the sample and grain size of the Pd nanocrystals and (5) resistivity. It has been probed that the use of high electron doses, 30000 μ C cm -2 results in the lowest resistivity reported to date for PdNDs, namely 145 μ Ω cm, which is only one order of magnitude higher than bulk palladium. This result paves the way for development of simplified lithography processes of nanostructured deposits avoiding subsequent post-treatment steps., (© 2022 IOP Publishing Ltd.)

Since its discovery in 1911, superconductivity has represented an equally inciting and fascinating field of study in several areas of physics and materials science, ranging from its most fundamental theoretical understanding, to its practical application in different areas of engineering. The fabrication of superconducting materials can be downsized to the nanoscale by means of Focused Ion/Electron Beam Induced Deposition : nanopatterning techniques that make use of a focused beam of ions or electrons to decompose a gaseous precursor in a single step. Overcoming the need to use a resist, these approaches allow for targeted, highly-flexible nanopatterning of nanostructures with lateral resolution in the range of 10 nm to 30 nm. In this review, the fundamentals of these nanofabrication techniques are presented, followed by a literature revision on the published work that makes use of them to grow superconducting materials, the most remarkable of which are based on tungsten, niobium, molybdenum, carbon, and lead. Several examples of the application of these materials to functional devices are presented, related to the superconducting proximity effect, vortex dynamics, electric-field effect, and to the nanofabrication of Josephson junctions and nanoSQUIDs. Owing to the patterning flexibility they offer, both of these techniques represent a powerful and convenient approach towards both fundamental and applied research in superconductivity.

The critical current of a superconducting nanostructure can be suppressed by applying an electric field in its vicinity. This phenomenon is investigated throughout the fabrication and electrical characterization of superconducting tungsten-carbon (W-C) nanostructures grown by Ga[Formula: see text] focused ion beam induced deposition (FIBID). In a 45 nm-wide, 2.7 [Formula: see text]m-long W-C nanowire, an increasing side-gate voltage is found to progressively reduce the critical current of the device, down to a full suppression of the superconducting state below its critical temperature. This modulation is accounted for by the squeezing of the superconducting current by the electric field within a theoretical model based on the Ginzburg-Landau theory, in agreement with experimental data. Compared to electron beam lithography or sputtering, the single-step FIBID approach provides with enhanced patterning flexibility and yields nanodevices with figures of merit comparable to those retrieved in other superconducting materials, including Ti, Nb, and Al. Exhibiting a higher critical temperature than most of other superconductors, in which this phenomenon has been observed, as well as a reduced critical value of the gate voltage required to fully suppress superconductivity, W-C deposits are strong candidates for the fabrication of nanodevices based on the electric field-induced superconductivity modulation., (© 2021. The Author(s).)

Emergent technologies are required in the field of nanoelectronics for improved contacts and interconnects at nano and micro-scale. In this work, we report a highly-efficient nanolithography process for the growth of cobalt nanostructures requiring an ultra-low charge dose (15 μC cm -2 , unprecedented in single-step charge-based nanopatterning). This resist-free process consists in the condensation of a ∼28 nm-thick Co 2 (CO) 8 layer on a substrate held at -100 °C, its irradiation with a Ga + focused ion beam, and substrate heating up to room temperature. The resulting cobalt-based deposits exhibit sub-100 nm lateral resolution, display metallic behaviour (room-temperature resistivity of 200 μΩ cm), present ferromagnetic properties (magnetization at room temperature of 400 emu cm -3 ) and can be grown in large areas. To put these results in perspective, similar properties can be achieved by room-temperature focused ion beam induced deposition and the same precursor only if a 2 × 10 3 times higher charge dose is used. We demonstrate the application of such an ultra-fast growth process to directly create electrical contacts onto graphene ribbons, opening the route for a broad application of this technology to any 2D material. In addition, the application of these cryo-deposits for hard masking is demonstrated, confirming its structural functionality., Competing Interests: There are no conflicts to declare., (This journal is © The Royal Society of Chemistry.)

Topological insulators are materials with time-reversal symmetric states of matter in which an insulating bulk is surrounded by protected Dirac-like edge or surface states. Among topological insulators, Bi2Se3 has attracted special attention due to its simple surface band structure and its relatively large band gap that should enhance the contribution of its surface to transport, which is usually masked by the appearance of defects. In order to avoid this difficulty, several features characteristic of topological insulators in the quantum regime, such as the weak-antilocalization effect, can be explored through magnetotransport experiments carried out on thin films of this material. Here, we review the existing literature on the magnetotransport properties of Bi2Se3 thin films, paying thorough attention to the weak-antilocalization effect, which is omnipresent no matter the film quality. We carefully follow the different situations found in reported experiments, from the most ideal situations, with a strong surface contribution, towards more realistic cases where the bulk contribution dominates. We have compared the transport data found in literature to shed light on the intrinsic properties of Bi2Se3, finding a clear relationship between the mobility and the phase coherence length of the films that could trigger further experiments on transport in topological systems.

Focused ion beam induced deposition (FIBID) is a nanopatterning technique that uses a focused beam of charged ions to decompose a gaseous precursor. So far, the flexible patterning capabilities of FIBID have been widely exploited in the fabrication of superconducting nanostructures, using the W(CO) 6 precursor mostly in combination with a focused beam of Ga + ions. Here, the fabrication and characterization of superconducting in-plane tungsten-carbon (W-C) nanostructures by He + FIBID of the W(CO) 6 precursor is reported. A patterning resolution of 10 nm has been achieved, which is virtually unattainable for Ga + FIBID. When the nanowires are patterned with widths of 20 nm and above, the deposited material is superconducting below 3.5-4 K. In addition, nanowires with widths of 60 and 90 nm have been found to sustain long-range controlled nonlocal superconducting vortex transfer along 3 μm. Overall, these findings strengthen the capabilities of He + FIBID of W-C in the growth and patterning of in-plane superconducting nanodevices.

Focused-electron-beam-induced deposition (FEBID) is the ultimate additive nanofabrication technique for the growth of 3D nanostructures. In the field of nanomagnetism and its technological applications, FEBID could be a viable solution to produce future high-density, low-power, fast nanoelectronic devices based on the domain wall conduit in 3D nanomagnets. While FEBID has demonstrated the flexibility to produce 3D nanostructures with almost any shape and geometry, the basic physical properties of these out-of-plane deposits are often seriously degraded from their bulk counterparts due to the presence of contaminants. This work reviews the experimental efforts to understand and control the physical processes involved in 3D FEBID growth of nanomagnets. Co and Fe FEBID straight vertical nanowires have been used as benchmark geometry to tailor their dimensions, microstructure, composition and magnetism by smartly tuning the growth parameters, post-growth purification treatments and heterostructuring.

Topologically non-trivial structures such as magnetic skyrmions are nanometric spin textures of outstanding potential for spintronic applications due to their unique features. It is well known that Néel skyrmions of definite chirality are stabilized by the Dzyaloshinskii-Moriya exchange interaction (DMI) in bulk non-centrosymmetric materials or ultrathin films with strong spin-orbit coupling at the interface. In this work, we show that soft magnetic (permalloy) hemispherical nanodots are able to host three-dimensional chiral structures (half-hedgehog spin textures) with non-zero tropological charge. They are observed at room temperature, in absence of DMI interaction and they can be further stabilized by the magnetic field arising from the Magnetic Force Microscopy probe. Micromagnetic simulations corroborate the experimental data. Our work implies the existence of a new degree of freedom to create and manipulate complex 3D spin-textures in soft magnetic nanodots and opens up future possibilities to explore their magnetization dynamics.

Focused electron beam induced deposition (FEBID) is a direct-write nanofabrication technique able to pattern three-dimensional magnetic nanostructures at resolutions comparable to the characteristic magnetic length scales. FEBID is thus a powerful tool for 3D nanomagnetism which enables unique fundamental studies involving complex 3D geometries, as well as nano-prototyping and specialized applications compatible with low throughputs. In this focused review, we discuss recent developments of this technique for applications in 3D nanomagnetism, namely the substantial progress on FEBID computational methods, and new routes followed to tune the magnetic properties of ferromagnetic FEBID materials. We also review a selection of recent works involving FEBID 3D nanostructures in areas such as scanning probe microscopy sensing, magnetic frustration phenomena, curvilinear magnetism, magnonics and fluxonics, offering a wide perspective of the important role FEBID is likely to have in the coming years in the study of new phenomena involving 3D magnetic nanostructures.

Currently, the patterning of innovative three-dimensional (3D) nano-objects is required for the development of future advanced electronic components. Helium ion microscopy in combination with a precursor gas can be used for direct writing of three-dimensional nanostructures with a precise control of their geometry, and a significantly higher aspect ratio than other additive manufacturing technologies. We report here on the deposition of 3D hollow tungsten carbide nanowires with tailored diameters by tuning two key growth parameters, namely current and dose of the ion beam. Our results show the control of geometry in 3D hollow nanowires, with outer and inner diameters ranging from 36 to 142 nm and from 5 to 28 nm, respectively; and lengths from 0.5 to 8.9 µm. Transmission electron microscopy experiments indicate that the nanowires have a microstructure of large grains with a crystalline structure compatible with the face-centered cubic WC 1- x phase. In addition, 3D electron tomographic reconstructions show that the hollow center of the nanowires is present along the whole nanowire length. Moreover, these nanowires become superconducting at 6.8 K and show high values of critical magnetic field and critical current density. Consequently, these 3D nano-objects could be implemented as components in the next generation of electronics, such as nano-antennas and sensors, based on 3D superconducting architectures., (Copyright © 2020, Córdoba et al.; licensee Beilstein-Institut.)

Chirality plays a major role in nature, from particle physics to DNA, and its control is much sought-after due to the scientific and technological opportunities it unlocks. For magnetic materials, chiral interactions between spins promote the formation of sophisticated swirling magnetic states such as skyrmions, with rich topological properties and great potential for future technologies. Currently, chiral magnetism requires either a restricted group of natural materials or synthetic thin-film systems that exploit interfacial effects. Here, using state-of-the-art nanofabrication and magnetic X-ray microscopy, we demonstrate the imprinting of complex chiral spin states via three-dimensional geometric effects at the nanoscale. By balancing dipolar and exchange interactions in an artificial ferromagnetic double-helix nanostructure, we create magnetic domains and domain walls with a well-defined spin chirality, determined solely by the chiral geometry. We further demonstrate the ability to create confined 3D spin textures and topological defects by locally interfacing geometries of opposite chirality. The ability to create chiral spin textures via 3D nanopatterning alone enables exquisite control over the properties and location of complex topological magnetic states, of great importance for the development of future metamaterials and devices in which chirality provides enhanced functionality.

Focused Electron Beam Induced Deposition (FEBID) for magnetic tip fabrication is presented in this work as an alternative to conventional sputtering-based Magnetic Force Microscopy (MFM) tips. FEBID enables the growth of a high-aspect-ratio magnetic nanorod with customized geometry and composition to overcome the key technical limitations of MFM probes currently on the market. The biggest advantage of these tips, in comparison with CoCr coated pyramidal probes, lies in the capability of creating sharp ends, nearly 10 nm in diameter, which provides remarkable (topographic and magnetic) lateral resolution in samples with magnetic features close to the resolution limits of the MFM technique itself. The shape of the nanorods produces a very confined magnetic stray field, whose interaction with the sample is extremely localized and perpendicular to the surface, with negligible in-plane components. This effect can lead to a better analytical and numerical modelling of the MFM probes and to an increase in the sensitivity without perturbing the magnetic configuration of soft samples. Besides, the high-aspect ratio achievable in FEBID nanorod tips makes them magnetically harder than the commercial ones, reaching coercive fields higher than 900 Oe. According to the results shown, tips based on magnetic nanorods grown by FEBID can be eventually used for quantitative analysis in MFM measurements. Moreover, the customized growth of Co- or Fe-based tips onto levers with different mechanical properties allows MFM studies that demand different measuring conditions. To showcase the versatility of this type of probe, as a last step, MFM is performed in a liquid environment, which still remains a challenge for the MFM community largely due to the lack of appropriate probes on the market. This opens up new possibilities in the investigation of magnetic biological samples.

Focused electron beam induced deposition (FEBID) is a leading nanolithography technique in terms of resolution and the capability for three-dimensional (3D) growth of functional nanostructures. However, FEBID still presents some limitations with respect to the precise control of the dimensions of the grown nano-objects as well as its use on insulating substrates. In the present work, we overcome both limitations by employing electrically-biased metal structures patterned on the surface of insulating substrates. Such patterned metal structures serve for charge dissipation and also allow the application of spatially-dependent electric fields. We demonstrate that such electric fields can dramatically change the dimensions of the growing 3D nanostructures by acting on the primary electron beam and the generated secondary electrons. In the performed experiments, the diameter of Pt-C and W-C vertical nanowires grown on quartz, MgO and amorphous SiO 2 is tuned by application of moderate voltages (up to 200 V) on the patterned metal microstructures during growth, achieving diameters as small as 50 nm. We identify two competing effects arising from the generated electric fields: a slight change in the primary beam focus point and a strong action on the secondary electrons. Beam defocus is exploited to achieve the in situ modulation of the diameter of 3D FEBID structures during growth.

Novel schemes based on the design of complex three-dimensional (3D) nanoscale architectures are required for the development of the next generation of advanced electronic components. He + focused-ion-beam (FIB) microscopy in combination with a precursor gas allows one to fabricate 3D nanostructures with an extreme resolution and a considerably higher aspect ratio than FIB-based methods, such as Ga + FIB-induced deposition, or other additive manufacturing technologies. In this work, we report the fabrication of 3D tungsten carbide nanohelices with on-demand geometries via controlling key deposition parameters. Our results show the smallest and highest-densely packed nanohelix ever fabricated so far, with dimensions of 100 nm in diameter and aspect ratio up to 65. These nanohelices become superconducting at 7 K and show a large critical magnetic field and critical current density. In addition, given its helical 3D geometry, fingerprints of vortex and phase-slip patterns are experimentally identified and supported by numerical simulations based on the time-dependent Ginzburg-Landau equation. These results can be understood by the helical geometry that induces specific superconducting properties and paves the way for future electronic components, such as sensors, energy storage elements, and nanoantennas, based on 3D compact nanosuperconductors.

The growth of ferromagnetic nanostructures by means of focused-Ga + -beam-induced deposition (Ga + -FIBID) using the Co 2 (CO) 8 precursor has been systematically investigated. The work aimed to obtain growth conditions allowing for the simultaneous occurrence of high growth speed, good lateral resolution, low electrical resistivity, and ferromagnetic behavior. As a first result, it has been found that the competition between deposition and milling that is produced by the Ga + beam is a limiting factor. In our working conditions, with the maximum available precursor flux, the maximum deposit thickness has been found to be 65 nm. The obtained volumetric growth rate is at least 50 times higher than in the case of deposition by focused-electron-beam-induced deposition. The lateral resolution of the deposits can be as good as 50 nm while using Ga + -beam currents lower than 10 pA. The high metallic content of the as-grown deposits gives rise to a low electrical resistivity, within the range 20-40 µΩ·cm. Magnetic measurements confirm the ferromagnetic nature of the deposits at room temperature. In conclusion, the set of obtained results indicates that the growth of functional ferromagnetic nanostructures by Ga + -FIBID while using the Co 2 (CO) 8 precursor is a viable and competitive technique when compared to related nanofabrication techniques.

In this contribution, we compare the performance of Focused Electron Beam-induced Deposition (FEBID) and Focused Ion Beam-induced Deposition (FIBID) at room temperature and under cryogenic conditions (the prefix "Cryo" is used here for cryogenic). Under cryogenic conditions, the precursor material condensates on the substrate, forming a layer that is several nm thick. Its subsequent exposure to a focused electron or ion beam and posterior heating to 50 °C reveals the deposit. Due to the extremely low charge dose required, Cryo-FEBID and Cryo-FIBID are found to excel in terms of growth rate, which is typically a few hundred/thousand times higher than room-temperature deposition. Cryo-FIBID using the W(CO) 6 precursor has demonstrated the growth of metallic deposits, with resistivity not far from the corresponding deposits grown at room temperature. This paves the way for its application in circuit edit and the fast and direct growth of micro/nano-electrical contacts with decreased ion damage. The last part of the contribution is dedicated to the comparison of these techniques with other charge-based lithography techniques in terms of the charge dose required and process complexity. The comparison indicates that Cryo-FIBID is very competitive and shows great potential for future lithography developments., Competing Interests: The authors declare no conflict of interest. The funders had no role in the design of the study; in the collection, analyses, or interpretation of data; in the writing of the manuscript, or in the decision to publish the results.

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.

An ultra-fast method to directly grow metallic micro- and nano-structures is introduced. It relies on a Focused Ion Beam (FIB) and a condensed layer of suitable precursor material formed on the substrate under cryogenic conditions. The technique implies cooling the substrate below the condensation temperature of the gaseous precursor material, subsequently irradiating with ions according to the wanted pattern, and posteriorly heating the substrate above the condensation temperature. Here, using W(CO) 6 as the precursor material, a Ga + FIB, and a substrate temperature of -100 °C, W-C metallic layers and nanowires with resolution down to 38 nm have been grown by Cryogenic Focused Ion Beam Induced Deposition (Cryo-FIBID). The most important advantages of Cryo-FIBID are the fast growth rate (about 600 times higher than conventional FIBID with the precursor material in gas phase) and the low ion irradiation dose required (∼50 μC/cm 2 ), which gives rise to very low Ga concentrations in the grown material and in the substrate (≤0.2%). Electrical measurements indicate that W-C layers and nanowires grown by Cryo-FIBID exhibit metallic resistivity. These features pave the way for the use of Cryo-FIBID in various applications in micro- and nano-lithography such as circuit editing, photomask repair, hard masks, and the growth of nanowires and contacts. As a proof of concept, we show the use of Cryo-FIBID to grow metallic contacts on a Pt-C nanowire and investigate its transport properties. The contacts have been grown in less than one minute, which is considerably faster than the time needed to grow the same contacts with conventional FIBID, around 10 hours.

Under high-enough values of perpendicularly-applied magnetic field and current, a type-II superconductor presents a finite resistance caused by the vortex motion driven by the Lorentz force. To recover the dissipation-free conduction state, strategies for minimizing vortex motion have been intensely studied in the last decades. However, the non-local vortex motion, arising in areas depleted of current, has been scarcely investigated despite its potential application for logic devices. Here, we propose a route to transfer vortices carried by non-local motion through long distances (up to 10 micrometers) in 50 nm-wide superconducting WC nanowires grown by Ga + Focused Ion Beam Induced Deposition. A giant non-local electrical resistance of 36 Ω has been measured at 2 K in 3 μm-long nanowires, which is 40 times higher than signals reported for wider wires of other superconductors. This giant effect is accounted for by the existence of a strong edge confinement potential that hampers transversal vortex displacements, allowing the long-range coherent displacement of a single vortex row along the superconducting channel. Experimental results are in good agreement with numerical simulations of vortex dynamics based on the time-dependent Ginzburg-Landau equations. Our results pave the way for future developments on information technologies built upon single vortex manipulation in nano-superconductors.

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.

Novel physical properties appear when the size of a superconductor is reduced to the nanoscale, in the range of its superconducting coherence length (ξ 0 ). Such nanosuperconductors are being investigated for potential applications in nanoelectronics and quantum computing. The design of three-dimensional nanosuperconductors allows one to conceive novel schemes for such applications. Here, we report for the first time the use of a He + focused-ion-beam-microscope in combination with the W(CO) 6 precursor to grow three-dimensional superconducting hollow nanowires as small as 32 nm in diameter and with an aspect ratio (length/diameter) of as much as 200. Such extreme resolution is achieved by using a small He + beam spot of 1 nm for the growth of the nanowires. As shown by transmission electron microscopy, they display grains of large size fitting with face-centered cubic WC 1-x phase. The nanowires, which are grown vertically to the substrate, are felled on the substrate by means of a nanomanipulator for their electrical characterization. They become superconducting at 6.4 K and show large critical magnetic field and critical current density resulting from their quasi-one-dimensional superconducting character. These results pave the way for future nanoelectronic devices based on three-dimensional nanosuperconductors.

We show how nanocrystalline Co films formed by separated oblique nano-sheets display anisotropy in their resistivity, magnetization process, surface nano-morphology and optical transmission. After performing a heat treatment at 270 °C, these anisotropies decrease. This loss has been monitored measuring the resistivity as a function of temperature. The resistivity measured parallel to the direction of the nano-sheets has been constant up to 270 °C, but it decreases when measured perpendicular to the nano-sheets. This suggests the existence of a structural relaxation, which produces the change of the Co nano-sheets during annealing. The changes in the nano-morphology and the local chemical composition of the films at the nanoscale after heating above 270 °C have been analysed by scanning transmission electron microscopy (STEM). Thus, an approach and coalescence of the nano-sheets have been directly visualized. The spectrum of activation energies of this structural relaxation has indicated that the coalescence of the nano-sheets has taken place between 1.2 and 1.7 eV. In addition, an increase in the size of the nano-crystals has occurred in the samples annealed at 400 °C. This study may be relevant for the application in devices working, for example, in the GHz range and to achieve the retention of the anisotropy of these films at higher temperatures., Competing Interests: The authors declare no conflict of interest.

The implementation of three-dimensional (3D) nano-objects as building blocks for the next generation of electro-mechanical, memory and sensing nano-devices is at the forefront of technology. The direct writing of functional 3D nanostructures is made feasible by using a method based on focused ion beam induced deposition (FIBID). We use this technique to grow horizontally suspended tungsten nanowires and then study their nano-mechanical properties by three-point bending method with atomic force microscopy. These measurements reveal that these nanowires exhibit a yield strength up to 12 times higher than that of the bulk tungsten, and near the theoretical value of 0.1 times the Young's modulus (E). We find a size dependence of E that is adequately described by a core-shell model, which has been confirmed by transmission electron microscopy and compositional analysis at the nanoscale. Additionally, we show that experimental resonance frequencies of suspended nanowires (in the MHz range) are in good agreement with theoretical values. These extraordinary mechanical properties are key to designing electro-mechanically robust nanodevices based on FIBID tungsten nanowires.

In this work, we present a detailed investigation of the magnetic properties of cobalt nanospheres grown on cantilever tips by focused electron beam induced deposition (FEBID). The cantilevers are extremely soft and the cobalt nanospheres are optimized for magnetic resonance force microscopy (MRFM) experiments, which implies that the cobalt nanospheres must be as small as possible while bearing high saturation magnetization. It was found that the cobalt content and the corresponding saturation magnetization of the nanospheres decrease for nanosphere diameters less than 300 nm. Electron holography measurements show the formation of a magnetic vortex state in remanence, which nicely agrees with magnetic hysteresis loops performed by local magnetometry showing negligible remanent magnetization. As investigated by local magnetometry, optimal behavior for high-resolution MRFM has been found for cobalt nanospheres with a diameter of ≈200 nm, which present atomic cobalt content of ≈83 atom % and saturation magnetization of 10 6 A/m, around 70% of the bulk value. These results represent the first comprehensive investigation of the magnetic properties of cobalt nanospheres grown by FEBID for application in MRFM.

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.

Temperature dependent 55 Mn NMR study of Sm 0.55 Sr 0.45 MnO 3 is reported. Previous bulk magnetization measurements have shown that below T C ~ 125 K the sample is ferromagnetic metallic (FMM) and above T C 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.

Nascent molecular electronic devices, based on monolayer Langmuir-Blodgett films sandwiched between two carbonaceous electrodes, have been prepared. Tightly packed monolayers of 4-((4-((4-ethynylphenyl)ethynyl)phenyl)ethynyl)benzoic acid are deposited onto a highly oriented pyrolytic graphite electrode. An amorphous carbon top contact electrode is formed on top of the monolayer from a naphthalene precursor using the focused electron beam induced deposition technique. This allows the deposition of a carbon top-contact electrode with well-defined shape, thickness, and precise positioning on the film with nm resolution. These results represent a substantial step toward the realization of integrated molecular electronic devices based on monolayers and carbon electrodes., (© 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

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.

We report efficient vortex pinning in thickness-modulated tungsten-carbon-based (W-C) nanostructures grown by focused ion beam induced deposition (FIBID). By using FIBID, W-C superconducting films have been created with thickness modulation properties exhibiting periodicity from 60 to 140 nm, leading to a strong pinning potential for the vortex lattice. This produces local minima in the resistivity up to high magnetic fields (2.2 T) in a broad temperature range due to commensurability effects between the pinning potential and the vortex lattice. The results show that the combination of single-step FIBID fabrication of superconducting nanostructures with built-in artificial pinning landscapes and the small intrinsic random pinning potential of this material produces strong periodic pinning potentials, maximizing the opportunities for the investigation of fundamental aspects in vortex science under changing external stimuli (e.g., temperature, magnetic field, electrical current).

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.

Functional nanostructured materials often rely on the combination of more than one material to confer the desired functionality or an enhanced performance of the device. Here we report the procedure to create nanoscale heterostructured materials in the form of core-shell nanowires by focused electron beam induced deposition (FEBID) technologies. In our case, three-dimensional (3D) nanowires (<100 nm in diameter) with metallic ferromagnetic cores of Co- and Fe-FEBID have been grown and coated with a protective Pt-FEBID shell (ranging 10-20 nm in thickness) aimed to minimize the degradation of magnetic properties caused by the surface oxidation of the core to a non-ferromagnetic material. The structure, chemistry and magnetism of nanowire cores of Co and Fe have been characterized in Pt-coated and uncoated nanostructures to demonstrate that the morphology of the shell is conserved during Pt coating, the surface oxidation is suppressed or confined to the Pt layer, and the average magnetization of the core is strengthened up to 30%. The proposed approach paves the way to the fabrication of 3D FEBID nanostructures based on the smart alternate deposition of two or more materials combining different physical properties or added functionalities.

The investigation of three-dimensional (3D) ferromagnetic nanoscale materials constitutes one of the key research areas of the current magnetism roadmap and carries great potential to impact areas such as data storage, sensing, and biomagnetism. The properties of such nanostructures are closely connected with their 3D magnetic nanostructure, making their determination highly valuable. Up to now, quantitative 3D maps providing both the internal magnetic and electric configuration of the same specimen with high spatial resolution are missing. Here, we demonstrate the quantitative 3D reconstruction of the dominant axial component of the magnetic induction and electrostatic potential within a cobalt nanowire (NW) of 100 nm in diameter with spatial resolution below 10 nm by applying electron holographic tomography. The tomogram was obtained using a dedicated TEM sample holder for acquisition, in combination with advanced alignment and tomographic reconstruction routines. The powerful approach presented here is widely applicable to a broad range of 3D magnetic nanostructures and may trigger the progress of novel spintronic nonplanar nanodevices.

The successful application of focused electron (and ion) beam induced deposition techniques for the growth of nanowires on flexible and transparent polycarbonate films is reported here. After minimization of charging effects in the substrate, sub-100 nm-wide Pt, W, and Co nanowires have been grown and their electrical conduction is similar compared to the use of standard Si-based substrates. Experiments where the substrate is bent in a controlled way indicate that the electrical conduction is stable up to high bending angles, >50°, for low-resistivity Pt nanowires grown by the ion beam. On the other hand, the resistance of Pt nanowires grown by the electron beam changes significantly and reversibly with the bending angle. Aided by the substrate transparency, a diffraction grating in transmission mode has been built based on the growth of an array of Pt nanowires that shows sharp diffraction spots. The set of results supports the large potential of focused beam deposition as a high-resolution nanolithography technique on transparent and flexible substrates. The most promising applications are expected in flexible nano-optics and nanoplasmonics, flexible electronics, and nanosensing.