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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.