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At least 19 records

Tin–Lead Liquid Metal Alloy Source for Focused Ion Beams

Focused Ion Beam (FIB) systems are increasingly utilized in nanotechnology for nanostructuring, surface modification, doping, and rapid prototyping. Recently, their potential for quantum applications has been explored, leveraging FIB’s direct-write capabilities for in situ single ion implantation, which is crucial for fabricating single photon emitters. Color centers in diamond can function as qubits and are of particular interest due to their capacity to store and transmit quantum information. While Group-IV color centers exhibit high brightness, they require low temperatures to retain coherence. However, lead-vacancy in diamond (PbV) operates at the higher end (4 K) of this temperature spectrum due to larger ground-state splitting, making them particularly interesting. In this context, our study presents results for lead (Pb)-containing alloys with eutectic points below 600 °C and results on using tantalum (Ta) and titanium (Ti) as emitter materials for a Pb liquid metal alloy ion source. We show that a standard FIB system is able to resolve the different Pb isotopes and achieve nanoscale spot sizes, as required for quantum information science applications.

color center↗

Thermoreflectance Detection of Point Defects Resulting from Focused Ion Beam Milling

Focused ion beam (FIB) milling is a commonly used tool for nanoscale material processing, such as for transmission electron microscopy (TEM) sample preparation, or the creation of fiducial markers prior to other processes and measurements. During milling, a high energy ion beam is used to remove material via sputtering. The expelled target material may return to the sample surface however, affecting subsequent measurements. Beam spreading or irradiation due to neutral gallium may also irradiate a larger area than intended. Extensive research has explored the effects of FIB milling on the prepared TEM sample, but few have looked at the effects of milling on the properties of the sample surrounding the milled region. We use multiple pump-probe laser-based techniques (time domain thermoreflectance and steady-state thermoreflectance) to measure the spatial extent of FIB-induced surface/subsurface changes on a series of silicon wafers milled at multiple currents and doses. We supplement these measurements with high-resolution scanning transmission electron microscopy, energy dispersive X-ray spectroscopy, stylus profilometry, and time-of-flight secondary ion mass spectroscopy. We find a sample surface affected by the FIB up to 1 mm from where milling occurred, with a notable dependence on the ion beam current. We also note remarkably high sensitivity to surface defects using the thermoreflectance metrologies, including detection where other measurements failed.

defects↗

Subsurface Characteristics of Metal-Halide Perovskites Polished by an Argon Ion Beam

Focused ion beam (FIB) techniques have been frequently used to section metal-halide perovskites for microstructural investigations. However, the ion beams directly irradiating the sample surface may alter its properties far different from those of pristine, potentially leading to modified deterioration mechanisms under aging stressors. Here, we combine complementary approaches to measure the subsurface characteristics of polished perovskites and identify the chemical species responsible for the measured properties. Analysis of the experimental results in conjunction with Monte Carlo simulations indicates that atomic displacements and local heating occur in the first ≈15 nm of the subsurface of methylammonium lead iodide (MAPbI 3 ) by glancing-angle Ar + beam irradiation (4 kV at 3°). The lead-rich, iodine-deficient surface promotes rapid phase segregation under thermal aging conditions. On the other hand, despite the subsurface modification, our experiments confirm that the rest of the MAPbI 3 bulk retains the material integrity. Our observation supports that polished perovskites could serve in studying the properties of bulk or buried junctions far away from the altered subsurface with care.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

On the role of self-generated magnetic fields in focused ion beams driven by intense picosecond laser pulses

We investigate the physics of ion beam focusing in the interaction of intense picosecond laser pulses with concave foils, using two-dimensional particle-in-cell simulations. Curved targets have been observed to deliver brighter multi-MeV ion beams than flat targets, and they could be used to ignite pre-compressed ICF fusion capsules in a scheme called ion fast ignition. Focusing is achieved by shaping the target and relying on an ion acceleration mechanism in which the ions are accelerated normal to the target surface; subsequently, the plasma expansion grows magnetic fields that advect with the plasma and deflect ions away from the target symmetry axis, causing the focal spot to shift downstream from its geometric location. The drop in both electric and magnetic field strengths in the expanding plasma makes the ion beam envelope asymmetric with respect to the focusing plane.

Focused ion beam↗

Focused ion beam milling of polycrystalline diamond

Focused ion beam (FIB) technology has a large potential for precise milling of ultrahard materials such as diamond. However, studies of the sputtering of diamond with ion species and energies relevant to the FIB technology are scarce. Here, we report a systematic study of the sputtering of polycrystalline diamond surfaces with ion beams in a wide range of ion energies (2 - 30 keV), incident beam angles (0 - 80°), and ion masses (N, O, Ar, and Xe). Results show that the sputter yield is relatively insensitive to ion energy but strongly depends on the ion species and incident beam angles. Bombardment with O ions results in sputter yields that are significantly larger than ballistic predictions due to chemical etching effects. Characteristic surface ripples develop for oblique beam incidence angle irradiation. The critical beam tilt angle for the onset of ripple formation and the wavelength of the ripples depend on ion species and energies. Ripples appear to suppress ion reflection at high beam tilt angles and, hence, a peak in the sputter yield angular dependence. In conclusion, these results have direct implications for the development of process parameter maps for high-precision ion-beam milling of diamond.

36 MATERIALS SCIENCE↗

Expanding the Energy Range from eV to MeV and Fabrication of Sources Enabling Novel Focused Ion Beam Nanofabrication and Modification

Multi-species focused ion beam (FIB) has the capability of running a variety of ion species allowing tailoring of the ion to the application enabling new applications of FIB such as localized doping and the creation of single defect centers. Also, through variation of the ion energy from eV to MeV, specific depths within the sample can be targeted enabling targeting of deeply buried layers inaccessible by traditional FIB systems. The combination of these capabilities opens up new areas of study including quantum information science and 2D materials.

47 OTHER INSTRUMENTATION↗

Controlled semiconductor quantum dot fabrication utilizing focus ion beam

In this project, we experimented the focused ion beam (FIB) based fabrications of semiconductor quantum dots (QDs) by using metal nano particles (NPs) (e.g., Al) on semiconductor as a template and by means of the FIB induced direct metal-to-QD conversion. We have examined effect of the experimental conditions, including Ga + ion energy and dose as well as substrate temperature. The results of experiments have shown AlGaSb QD formation on GaSb substrate can be achieved under certain conditions but there are many challenges about the techniques, including compositional nonuniformity of the QDs formed, partial conversion of the metal NP to QD, and high defect concentration in the QDs.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

New Directions in Focused Ion Beam Induced Deposition for the Nanoprinting of Functional 3D Heterostructures

The focused ion beam (FIB) microscope is well established as a high-resolution machining instrument capable of site-selectively removing material down to the nanoscale. Beyond subtractive processing, however, the FIB can also add material via a technique known as focused ion beam induced deposition (FIBID). Using FIBID, the FIB can thus be employed for the direct-write of complex nanostructures. This work explores new directions in three-dimensional FIBID nanoprinting, harnessing unique features of helium and neon FIBs. In particular, the superior spatial resolution of these novel FIBs is leveraged to fabricate precise multimaterial architectures, an isotope effect is used to create satellite deposits, and dose-controlled implantation of the gaseous ions is used to engineer internal voids. In the context of voids, the fabrication of hollow nanopillars by helium-FIBID due to concurrent milling (as shown previously by others) is revisited. Insight into the chemical and structural composition of the nanostructures is obtained using advanced electron microscopy, accurately revealing buried interfaces, crystallite distributions, chemical compositions, and material transformations. Next-generation devices and technologies that could be enabled by the novel heterostructures demonstrated here are discussed, setting the stage for the potential evolution of FIBID into a versatile platform for functional nanomaterials design and fabrication.

FIBID↗

Optical interference for the guidance of cryogenic focused ion beam milling beyond the axial diffraction limit

Cryogenic focused ion beam (Cryo-FIB) milling has become a standard step in the cryogenic electron tomography (Cryo-ET) workflow and is required to thin cells to electron-semitransparency. However, this destructive process removes the vast majority of the cellular material and raises a critical question: what thin section should be preserved for Cryo-ET analysis? Using a tri-coincident cryogenic FIB-SEM-LM system, we identify an interferometric optical response that can be used for targeting lamella production to fluorescently labeled structures with accuracy beyond the diffraction limit. Here we demonstrate this approach using synthetic samples of fluorescent beads embedded in micron-scale droplets of amorphous ice. We then apply the approach to capture virions inside host cells. Successful targeting is confirmed by Cryo-ET revealing clusters of virions in intracellular vesicles. The method does not require any fluorescent fiducials or axial registration and can be performed on any fluorescently labeled structure that is visible in widefield fluorescence microscopy.

Cryoelectron microscopy↗

Toward Automated Plasma Focus Ion Beam Instrument Calibration for Materials Processing [Poster]

To accelerate the transition to autonomous focused ion beam (FIB) microscopy, we require an objective figure of merit (FOM) for assessing calibration. For our purposes, these FOMs related to beam astigmatism, quad, and focus. Intelligent calibration integrated into scripted workflows will enable fully automated sample preparation workflows that produce higher quality samples with less operator time.

97 MATHEMATICS AND COMPUTING↗

High–Yield Deterministic Focused Ion Beam Implantation of Quantum Defects Enabled by In Situ Photoluminescence Feedback

Focused ion beam implantation is ideally suited for placing defect centers in wide bandgap semiconductors with nanometer spatial resolution. However, the fact that only a few percent of implanted defects can be activated to become efficient single photon emitters prevents this powerful capability to reach its full potential in photonic/electronic integration of quantum defects. Here an industry adaptive scalable technique is demonstrated to deterministically create single defects in commercial grade silicon carbide by performing repeated low ion number implantation and in situ photoluminescence evaluation after each round of implantation. An array of 9 single defects in 13 targeted locations is successfully created—a ≈70% yield which is more than an order of magnitude higher than achieved in a typical single pass ion implantation. The remaining emitters exhibit non-classical photon emission statistics corresponding to the existence of at most two emitters. This approach can be further integrated with other advanced techniques such as in situ annealing and cryogenic operations to extend to other material platforms for various quantum information technologies.

36 MATERIALS SCIENCE↗

Plasma Focused Ion Beam Milling of High-Aspect-Ratio Holes in Diamond

Plasma focused ion beam (PFIB) technology has a great potential for applications requiring rapid micro-machining of high-aspect-ratio features. Here, we use 30-keV Ar, Xe, and O 2 ion beams to study PFIB milling of high-aspect-ratio circular holes in polycrystalline diamond. Our results show that Xe and O 2 ion beams have the highest milling efficiency for low-aspect-ratio and high-aspect-ratio hole milling, respectively. Each ion beam species produces holes with its characteristic shape and wall surface morphology. In conclusion, based on these results, we demonstrate a “hybrid” hole milled in a two-step process with Xe and O 2 ion beams with the geometry and wall morphology attractive for the attachment of a fuel fill tube to the inertial confinement fusion capsule.

ICF targets↗

Rethinking radiation effects in materials science using the plasma-focused ion beam

This work demonstrates the viability of using a plasma-focused ion beam (PFIB) as a new platform to carry out radiation effects studies in solids. While materials subjected to irradiation in either nuclear reactors or energetic particle accelerators experience limitations with respect to inaccuracies in both flux measurements and lack of precise control of irradiation areas, we demonstrate a new irradiation technique that allows the exposure of a single specimen in multiple areas, at multiple doses, and in site-specific dependencies - all with flux variations on the order of only 1%. This versatile technique also allows materials to be exposed to significantly higher irradiation dose rates than conventional accelerators. To validate the new methodology, we selected the classical example of ion-beam-induced amorphization of pure single-crystal Si. By pioneering the use of the PFIB for radiation effects studies in materials science, we were able to exploit, in both micro- and nanometer-sized detail, the differences in electron image contrast arising from crystalline versus amorphous solid-state phases in classical semiconductors subjected to irradiation, thus providing new insights on amorphization mechanisms. This methodology opens new research frontiers at the fringe of materials science with promising applications beyond the scope of materials at extremes such as in nanopatterning, nanodevices and nanoarchitectonics.

36 MATERIALS SCIENCE↗

Effects of Focused Ion Beam Lithography on La 2– x Sr x CuO 4 Single Crystals

Focused ion beam (FIB) milling is a mask-free lithography technique that allows the precise shaping of 3D materials on the micron and sub-micron scale. The recent discovery of electronic nematicity in La 2–x Sr x CuO 4 (LSCO) thin films triggered the search for the same phenomenon in bulk LSCO crystals. With this motivation, we have systematically explored FIB patterning of bulk LSCO crystals into micro-devices suitable for longitudinal and transverse resistivity measurements. We found that several detrimental factors can affect the result, ultimately compromising the possibility of effectively using FIB milling to fabricate sub-micrometer LSCO devices, especially in the underdoped regime.

36 MATERIALS SCIENCE↗

Lithium source for focused ion beam implantation and analysis

In this work, we present a new Li source for focused ion beam applications. Based on an AuSi eutectic alloy, Li is added as an impurity to minimize effects from degradation when exposed to air. We show the source is stable over the course of an hour and spot sizes ≲10 nm can be achieved. The Li beam can achieve hundreds of nanometer ranges in semiconductors with minimal damage being generated along the path length. The source performance is evaluated through a high-resolution ion beam induced charge collection experiment on an Si-based detector. Further application of the source for ion beam analysis is numerically explored; the example investigated is based on probing a semiconductor heterostructure through a Rutherford backscattering experiment, where the Li beam can reveal information that is inaccessible with either low energy or high energy He projectiles used as probes.

36 MATERIALS SCIENCE↗

Novel Focused Ion Beam Liftouts for Spatial Characterization of Spherical Biominerals With Transmission Electron Microscopy

Abstract Focused ion beam (FIB) is frequently used to prepare electron- and X-ray-beam-transparent thin sections of samples, called lamellae. Typically, lamellae are prepared from only a subregion of a sample. In this paper, we present a novel approach for FIB lamella preparation of microscopic samples, wherein the entire cross-section of the whole sample can be investigated. The approach was demonstrated using spherical, porous, and often hollow microprecipitates of biologically precipitated calcium carbonate. The microprecipitate morphology made these biogenic samples more fragile and challenging than materials commonly investigated using FIB lamellae. Our method enables the appropriate orientation of the lamellae required for further electron/X-ray analyses after attachment to the transmission electron microscopy (TEM) grid post and facilitates more secure adhesion onto the grid post. We present evidence of autofluorescence in bacterially precipitated vaterite using this lamella preparation method coupled with TEM selected area diffraction. This innovative approach allows studying biomineralization at the micro to nano scales, which can provide novel insights into bacterial responses to microenvironmental conditions.

47 OTHER INSTRUMENTATION↗