Showing papers on "Focused ion beam published in 2018"
TL;DR: Techniques are presented that accelerate image acquisition while greatly improving FIB-SEM reliability, allowing the system to operate for months and generating continuously imaged volumes > 106 µm3.
Abstract: A microscopy system for imaging a sample can include a scanning electron microscope system configured for imaging a surface layer of the sample and a focused ion beam system configured for generating an ion beam for milling the surface layer away from a sample after it has been imaged. A movable mechanical shutter can be configured to be moved automatically into a position between the sample and the scanning electron microscope system, so that when the electron beam is not imaging the sample the movable mechanical shutter is positioned between the sample and the scanning electron microscope system.
176 citations
TL;DR: The sensitivity of CH3 NH3 PbI3 to electron beam irradiation is examined and some simple guidelines for how to minimize electron-beam-induced artifacts when using EM to study hybrid perovskite materials are provided.
Abstract: Organic-inorganic hybrid perovskites, such as CH3 NH3 PbI3, have shown highly promising photovoltaic performance. Electron microscopy (EM) is a powerful tool for studying the crystallography, morphology, interfaces, lattice defects, composition, and charge carrier collection and recombination properties at the nanoscale. Here, the sensitivity of CH3 NH3 PbI3 to electron beam irradiation is examined. CH3 NH3 PbI3 undergoes continuous structural and compositional changes with increasing electron dose, with the total dose, rather than dose rate, being the key operative parameter. Importantly, the first structural change is subtle and easily missed and occurs after an electron dose significantly smaller than that typically applied in conventional EM techniques. The electron dose conditions under which these structural changes occur are identified. With appropriate dose-minimization techniques, electron diffraction patterns can be obtained from pristine material consistent with the tetragonal CH3 NH3 PbI3 phases determined by X-ray diffraction. Radiation damage incurred at liquid nitrogen temperatures and using Ga+ irradiation in a focused ion beam instrument are also examined. Finally, some simple guidelines for how to minimize electron-beam-induced artifacts when using EM to study hybrid perovskite materials are provided.
117 citations
TL;DR: The developed ReS2 ALD process highlights the potential of the material for applications beyond planar structure architectures and offers a route to an upgrade to an industrial scale.
Abstract: 2D materials research is advancing rapidly as various new "beyond graphene" materials are fabricated, their properties studied, and materials tested in various applications. Rhenium disulfide is one of the 2D transition metal dichalcogenides that has recently shown to possess extraordinary properties such as that it is not limited by the strict monolayer thickness requirements. The unique inherent decoupling of monolayers in ReS2 combined with a direct bandgap and highly anisotropic properties makes ReS2 one of the most interesting 2D materials for a plethora of applications. Here, a highly controllable and precise atomic layer deposition (ALD) technique is applied to deposit ReS2 thin films. Film growth is demonstrated on large area (5 cm × 5 cm) substrates at moderate deposition temperatures between 120 and 500 °C, and the films are extensively characterized using field emission scanning electron microscopy/energy-dispersive X-ray spectroscopy, X-ray diffractometry using grazing incidence, atomic force microscopy, focused ion beam/transmission electron microscopy, X-ray photoelectron spectroscopy, and time-of-flight elastic recoil detection analysis techniques. The developed ReS2 ALD process highlights the potential of the material for applications beyond planar structure architectures. The ALD process also offers a route to an upgrade to an industrial scale.
108 citations
TL;DR: In this article, the impact of moisture-induced chemical degradation and proton-lithium exchange on the Li-ion dynamics in the bulk and the grain boundaries and at the interface with lithium metal in highly Li-conducting garnet electrolytes is provided.
Abstract: In this work, we reveal the impact of moisture-induced chemical degradation and proton–lithium exchange on the Li-ion dynamics in the bulk and the grain boundaries and at the interface with lithium metal in highly Li-conducting garnet electrolytes. A direct correlation between chemical changes as measured by depth-resolved secondary ion mass spectrometry and the change in transport properties of the electrolyte is provided. In order to probe the intrinsic effect of the exchange on the lithium kinetics within the garnet structure, isolated from secondary corrosion product contributions, controlled-atmosphere processing was first used to produce proton-free Li6.55Ga0.15La3Zr2O12 (Ga0.15-LLZO), followed by degradation steps in a H2O bath at 100 °C, leading to the removal of LiOH secondary phases at the surface. The proton-exchanged region was analyzed by focused ion beam secondary ion mass spectrometry (FIB-SIMS) and found to extend as far as 1.35 μm into the Ga0.15-LLZO garnet pellet after 30 min in H2O. Im...
104 citations
TL;DR: Focused ion beam machining offers exciting new possibilities for the study of quantum materials through precise control over the shape and geometry of single crystals on the submicrometer scale as mentioned in this paper.
Abstract: Focused ion beam (FIB) machining promises exciting new possibilities for the study of quantum materials through precise control over the shape and geometry of single crystals on the submicrometer scale. It offers viable routes to fabricate high-quality mesoscale structures from materials that cannot yet be grown in thin-film form and to enhance the experimentally accessible signatures of new physical phenomena. Prototype devices can also be produced in a silicon-chip environment to investigate directly the materials application potential for future electronics. This review introduces the concepts of ion beam shaping of matter, discusses the role and extent of surface damage and material disorder inherent to these techniques, and gives an overview of recent experiments on FIB-structured crystals. Given the early stage of the field of FIB-fabricated quantum materials, much is yet to come, and emergent trends and future directions are also discussed.
96 citations
TL;DR: Three advanced imaging techniques were utilized correlatively, including the application of Xe+ plasma focused ion beam scanning electron microscopy (plasma FIB or PFIB), complemented by the Ga+ FIB method which is now frequently used to characterise porosity and organic/inorganic phases, together with transmission electron microscope tomography of the nano-scale pores.
Abstract: Pore characterization in shales is challenging owing to the wide range of pore sizes and types present. Haynesville-Bossier shale (USA) was sampled as a typical clay-bearing siliceous, organic-rich, gas-mature shale and characterized over pore diameters ranging 2 nm to 3000 nm. Three advanced imaging techniques were utilized correlatively, including the application of Xe+ plasma focused ion beam scanning electron microscopy (plasma FIB or PFIB), complemented by the Ga+ FIB method which is now frequently used to characterise porosity and organic/inorganic phases, together with transmission electron microscope tomography of the nano-scale pores (voxel size 0.6 nm; resolution 1-2 nm). The three pore-size scales each contribute differently to the pore network. Those 100 nm (greatest total volume hence determines fluid storativity). Four distinct pore types were found: intra-organic, organic-mineral interface, inter-mineral and intra-mineral pores were recognized, with characteristic geometries. The whole pore network comprises a globally-connected system between phyllosilicate mineral grains (diameter: 6-50 nm), and locally-clustered connected pores within porous organic matter (diameter: 200-800 nm). Integrated predictions of pore geometry, connectivity, and roles in controlling petrophysical properties were verified through experimental permeability measurements.
83 citations
TL;DR: A site-specific, cryogenic, focused ion beam (FIB) method is presented for the preparation of atom probe tomography specimens from a frozen liquid/solid interface, and the interface between water and a corroded boroaluminosilicate glass has been characterized by APT for the first time.
66 citations
TL;DR: It is shown that surface oxidation can be effectively suppressed using an entirely cryogenic protocol (during specimen preparation and during transfer) and that the nanostructure of other normally-liquid or soft materials may be able to be measured.
Abstract: We present sample transfer instrumentation and integrated protocols for the preparation and atom probe characterization of environmentally-sensitive materials. Ultra-high vacuum cryogenic suitcases allow specimen transfer between preparation, processing and several imaging platforms without exposure to atmospheric contamination. For expedient transfers, we installed a fast-docking station equipped with a cryogenic pump upon three systems; two atom probes, a scanning electron microscope / Xe-plasma focused ion beam and a N2-atmosphere glovebox. We also installed a plasma FIB with a solid-state cooling stage to reduce beam damage and contamination, through reducing chemical activity and with the cryogenic components as passive cryogenic traps. We demonstrate the efficacy of the new laboratory protocols by the successful preparation and transfer of two highly contamination- and temperature-sensitive samples—water and ice. Analysing pure magnesium atom probe data, we show that surface oxidation can be effectively suppressed using an entirely cryogenic protocol (during specimen preparation and during transfer). Starting with the cryogenically-cooled plasma FIB, we also prepared and transferred frozen ice samples while avoiding significant melting or sublimation, suggesting that we may be able to measure the nanostructure of other normally-liquid or soft materials. Isolated cryogenic protocols within the N2 glove box demonstrate the absence of ice condensation suggesting that environmental control can commence from fabrication until atom probe analysis.
62 citations
TL;DR: The ambient environment localized pulsed electrodeposition process for direct printing of three-dimensional (3D) freestanding nanotwinned-Copper (nt-Cu) nanostructures was demonstrated and revealed that the printed metal was fully dense, and was mostly devoid of impurities and microstructural defects.
Abstract: Nanotwinned-metals (nt-metals) offer superior mechanical (high ductility and strength) and electrical (low electromigration) properties compared to their nanocrystalline (nc) counterparts. These properties are advantageous in particular for applications in nanoscale devices. However, fabrication of nt-metals has been limited to films (two-dimensional) or template-based (one-dimensional) geometries, using various chemical and physical processes. In this Letter, we demonstrate the ambient environment localized pulsed electrodeposition process for direct printing of three-dimensional (3D) freestanding nanotwinned-Copper (nt-Cu) nanostructures. 3D nt-Cu structures were additively manufactured using pulsed electrodeposition at the tip of an electrolyte-containing nozzle. Focused ion beam (FIB) and transmission electron microscopy (TEM) analysis revealed that the printed metal was fully dense, and was mostly devoid of impurities and microstructural defects. FIB and TEM images also revealed nanocrystalline-nanot...
59 citations
TL;DR: This work reports 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 of as much as 200, paving the way for future nanoelectronic devices based on three- dimensional nanosuperconductors.
Abstract: Novel physical properties appear when the size of a superconductor is reduced to the nanoscale, in the range of its superconducting coherence length (ξ0). 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 WC1–x phase. The nanowires, which are grown vertically to the substrate, are felled on the substrate by means of a nanomanipulator for their el...
58 citations
TL;DR: A workflow to prepare samples and record high-quality tomograms of diverse model organisms, including infected and uninfected HeLa cells, amoebae, yeast, multicellular cyanobacteria, Pseudomonas aeruginosa and Escherichia coli cells is applied.
TL;DR: The combination of lithium trapping and apparent morphological densification evolution in NiO is believed to account for the degradation of the ECD properties upon long term cycling of the WO/WO/ITO/ NiO ECD.
Abstract: The visualization of the microstructure change and of the depth of lithium transport inside a monolithic ElectroChromic Device (ECD) is realized using an innovative combined approach of Focused Ion Beam (FIB), Secondary Ion Mass Spectrometry (SIMS) and Glow Discharge Optical Emission Spectroscopy (GDOES). The electrochemical and optical properties of the all-thin-film inorganic ECD glass/ITO/WO3/LiTaO3/NiO/ITO, deposited by magnetron sputtering, are measured by cycling voltammetry and in situ transmittance analysis up to 11 270 cycles. A significant degradation corresponding to a decrease in the capacity of 71% after 2500 cycles and of 94% after 11 270 cycles is reported. The depth resolved microstructure evolution within the device, investigated by cross-sectional cutting with FIB, points out a progressive densification of the NiO layer upon cycling. The existence of irreversible Li ion trapping in NiO is illustrated through the comparison of the compositional distribution of the device after various cycles 0, 100, 1000, 5000 and 11 270. SIMS and GDOES depth profiles confirm an increase in the trapped Li content in NiO as the number of cycles increases. Therefore, the combination of lithium trapping and apparent morphological densification evolution in NiO is believed to account for the degradation of the ECD properties upon long term cycling of the ECD.
TL;DR: It is found stronger plasmonic response with better field confinement in the antennas fabricated by electron beam lithography, which is attributed to their better structural quality, homogeneous thickness, and only moderate contamination mostly of organic nature.
Abstract: We present a comparative study of plasmonic antennas fabricated by electron beam lithography and direct focused ion beam milling. We have investigated optical and structural properties and chemical composition of gold disc-shaped plasmonic antennas on a silicon nitride membrane fabricated by both methods to identify their advantages and disadvantages. Plasmonic antennas were characterized using transmission electron microscopy including electron energy loss spectroscopy and energy dispersive X-ray spectroscopy, and atomic force microscopy. We have found stronger plasmonic response with better field confinement in the antennas fabricated by electron beam lithography, which is attributed to their better structural quality, homogeneous thickness, and only moderate contamination mostly of organic nature. Plasmonic antennas fabricated by focused ion beam lithography feature weaker plasmonic response, lower structural quality with pronounced thickness fluctuations, and strong contamination, both organic and inorganic, including implanted ions from the focused beam. While both techniques are suitable for the fabrication of plasmonic antennas, electron beam lithography shall be prioritized over focused ion beam lithography due to better quality and performance of its products.
TL;DR: A new cutting geometry is introduced for FIB lift-out sample preparation with plan-view geometry that provides clear viewing angles for monitoring the milling process, which solves the difficulty of judging whether the specimen has been entirely detached from the bulk material with the least possible damage to the surrounding materials.
TL;DR: In this article, the authors used the pillar indentation splitting test for assessing the fracture behavior of materials using micro-scale pillar samples, and found that FIB damage significantly increased the apparent toughness at smaller pillar sizes, but the influence diminishes to negligibility at pillar diameters.
TL;DR: A new approach based on an image-processing or deep-learning-based method for super-resolution of 3D images with such asymmetric resolution, so as to restore the depth resolution to achieve symmetric resolution.
Abstract: Scanning electron microscopy equipped with a focused ion beam (FIB-SEM) is a promising three-dimensional (3D) imaging technique for nano- and meso-scale morphologies. In FIB-SEM, the specimen surface is stripped by an ion beam and imaged by an SEM installed orthogonally to the FIB. The lateral resolution is governed by the SEM, while the depth resolution, i.e., the FIB milling direction, is determined by the thickness of the stripped thin layer. In most cases, the lateral resolution is superior to the depth resolution; hence, asymmetric resolution is generated in the 3D image. Here, we propose a new approach based on an image-processing or deep-learning-based method for super-resolution of 3D images with such asymmetric resolution, so as to restore the depth resolution to achieve symmetric resolution. The deep-learning-based method learns from high-resolution sub-images obtained via SEM and recovers low-resolution sub-images parallel to the FIB milling direction. The 3D morphologies of polymeric nano-composites are used as test images, which are subjected to the deep-learning-based method as well as conventional methods. We find that the former yields superior restoration, particularly as the asymmetric resolution is increased. Our super-resolution approach for images having asymmetric resolution enables observation time reduction.
TL;DR: In this paper, the individual effects of chloride (Cl−), calcium (Ca2+), and magnesium (Mg2+) ions on the CO2 corrosion behavior of carbon steel in simulated CO2 geologic storage environments (60 °C and 100 bar CO2).
TL;DR: In this paper, the authors presented highly sensitive pressure sensors using piezoresistive nanowires, which are locally fabricated on free standing structures with a high strain concentration, and showed significant 3-fold enhancement in the sensitivity in comparison to conventional structures.
TL;DR: This work demonstrates the devices fabricated by the FIB technique using InSe nanostructures for highly efficient broad-band optical sensing and light harvesting, which is critical for development of the 2D material-based ultrathin flexible optoelectronics.
Abstract: A photodetector using a two-dimensional (2D) low-direct band gap indium selenide (InSe) nanostructure fabricated by the focused ion beam (FIB) technique has been investigated. The FIB-fabricated InSe photodetectors with a low contact resistance exhibit record high responsivity and detectivity to the ultraviolet and visible lights. The optimal responsivity and detectivity up to 1.8 × 107 A W–1 and 1.1 × 1015 Jones, respectively, are much higher than those of the other 2D material-based photoconductors and phototransistors. Moreover, the inherent photoconductivity (PC) quantified by the value of normalized gain has also been discussed and compared. By excluding the contribution of artificial parameters, the InSe nanoflakes exhibit an ultrahigh normalized gain of 3.2 cm2 V–1, which is several orders of magnitude higher than those of MoS2, GaS, and other layer material nanostructures. A high electron mobility at room temperature reaching 450 cm2 V–1 s–1 has been confirmed to be one of the major causes of the ...
TL;DR: In this article, a focused ion-beam-based nanoscale kirigami is proposed as a 3D nanofabrication technique for window decorations, gift cards, festivals, and various ceremonies.
Abstract: Abstract Kirigami, i.e. the cutting and folding of flat objects to create versatile shapes, is one of the most traditional Chinese arts that has been widely used in window decorations, gift cards, festivals, and various ceremonies, and has recently found intriguing applications in modern sciences and technologies. In this article, we review the newly developed focused-ion-beam-based nanoscale kirigami, named nano-kirigami, as a powerful three-dimensional (3D) nanofabrication technique. By utilizing the topography-guided stress equilibrium induced by ion-beam irradiation on a free-standing gold nanofilm, versatile 3D shape transformations such as upward buckling, downward bending, complex rotation, and twisting of nanostructures are precisely achieved. It is shown that the generated 3D nanostructures possess exceptional geometries and promising photonic functionalities, including strongly interacting multiple Fano resonances, giant optical chirality, clear photonic spin Hall effects, and diffractive phase/polarization effects. The studies of such structures can build up novel platforms for versatile manufacturing techniques and be helpful to establish new areas in plasmonics, nanophotonics, optomechanics, MEMS/NEMS, etc., with the generation of exotic but functional nanostructures.
TL;DR: In this paper, a mathematically straightforward and robust approach based on the concept of eigenstrain was proposed for residual stress depth profiling at the resolution better than 50 nm by the application of a matrix factorization approach.
TL;DR: In this article, a novel thermophysical simulation method to precisely control the reaction conditions was designed to investigate molten aluminium/solid steel interfacial reactions, and the reaction layers between the materials were investigated by high-resolution transmission electron microscopy assisted by advanced focused ion beam technology.
TL;DR: This work develops a versatile technology enabling reconfigurable light-delivery that can be tailored to specific experimental needs by micro-structuring metal-coated tapered optical fibers and exploiting the resulting mode-division multiplexing/demultiplexing properties.
TL;DR: In this article, the exposure of sample to Focused ion beam leads to Ga-ion implantation, damage, material amorphisation, and the introduction of sources of residual stress; namely eigenstrain.
TL;DR: The possibility to create silicon nanostructure of truly tree-dimensional shape by means of the focused ion beam lithography is explored, and a 300 nm thin film of monocrystalline epitaxial silicon on sapphire is patterned with a chiral nanoscale relief.
Abstract: High refractive index makes silicon the optimal platform for dielectric metasurfaces capable of versatile control of light. Among various silicon modifications, its monocrystalline form has the weakest visible light absorption but requires a careful choice of the fabrication technique to avoid damage, contamination or amorphization. Presently prevailing chemical etching can shape thin silicon layers into two-dimensional patterns consisting of strips and posts with vertical walls and equal height. Here, the possibility to create silicon nanostructure of truly tree-dimensional shape by means of the focused ion beam lithography is explored, and a 300 nm thin film of monocrystalline epitaxial silicon on sapphire is patterned with a chiral nanoscale relief. It is demonstrated that exposing silicon to the ion beam causes a substantial drop of the visible transparency, which, however, is completely restored by annealing with oxidation of the damaged surface layer. As a result, the fabricated chiral metasurface combines high (50–80%) transmittance with the circular dichroism of up to 0.5 and the optical activity of up to 20° in the visible range. Being also remarkably durable, it possesses crystal-grade hardness, heat resistance up to 1000 °C and the inertness of glass.
TL;DR: A number of techniques to improve the quality of the acquired data, together with easy-to-implement methods to obtain "advanced" microstructural quantifications are presented to a solid oxide fuel cell cathode of interest to the electrochemistry community.
Patent•
27 Sep 2018TL;DR: In this article, a magnetic tape with ferromagnetic powder, a binding agent, and an oxide abrasive is presented, and ΔSFD in the longitudinal direction of the magnetic tape calculated by Expression 1 is equal to or smaller than 0.50.
Abstract: Provided are a magnetic tape, in which a magnetic layer includes a ferromagnetic powder, a binding agent, and an oxide abrasive, ΔSFD in a longitudinal direction of the magnetic tape calculated by Expression 1, ΔSFD=SFD 25° C. −SFD −190° C. , is equal to or smaller than 0.50, a logarithmic decrement acquired by a pendulum viscoelasticity test performed regarding a surface of the magnetic layer is equal to or smaller than 0.050, and an average particle diameter of the oxide abrasive obtained from a secondary ion image obtained by irradiating the surface of the magnetic layer with a focused ion beam is 0.04 μm to 0.08 μm, and a magnetic recording and reproducing device including this magnetic tape.
TL;DR: In this article, a time-temperature transformation (TTT) diagram of the eta to eta-Cu6Sn5 transformation was developed for a single grain of Cu6sn5 that is in intimate contact with adjacent Sn rich and Cu3sn phases.
TL;DR: In this article, micro-mechanical properties of Ti(C,N) and Zr(C-N) coatings deposited by chemical vapor deposition on a WC-Co cemented carbide substrate were examined by micro-compression testing using a nanoindenter equipped with a flat punch.
TL;DR: In this paper, a maskless implantation of an array of bright, single germanium vacancy (GeV) centers in diamond was demonstrated, and the single GeV creation ratio reached as high as 53% with the dose of 200 Ge+ ions per spot.
Abstract: Color centers in diamond are promising solid-state qubits for scalable quantum photonics applications. Amongst many defects, those with inversion symmetry are of an interest due to their promising optical properties. In this work, we demonstrate a maskless implantation of an array of bright, single germanium vacancy (GeV) centers in diamond. Employing the direct focused ion beam technique, single GeV emitters are engineered with the spatial accuracy of tens of nanometers. The single GeV creation ratio reaches as high as 53% with the dose of 200 Ge+ ions per spot. The presented fabrication method is promising for future nanofabrication of integrated photonic structures with GeV emitters as a leading platform for spin-spin interactions.