Maskless milling of diamond by a focused oxygen ion beam.
Ontology highlight
ABSTRACT: Recent advances in focused ion beam technology have enabled high-resolution, maskless nanofabrication using light ions. Studies with light ions to date have, however, focused on milling of materials where sub-surface ion beam damage does not inhibit device performance. Here we report on maskless milling of single crystal diamond using a focused beam of oxygen ions. Material quality is assessed by Raman and luminescence analysis, and reveals that the damage layer generated by oxygen ions can be removed by non-intrusive post-processing methods such as localised electron beam induced chemical etching.
Project description:We report on a method for integrating sub-wavelength resonant structures on top of optical fiber tip. Our fabrication technique is based on direct milling of the glass on the fiber facet by means of focused ion beam. The patterned fiber tip acts as a structured template for successive depositions of any responsive or functional overlay. The proposed method is validated by depositing on the patterned fiber a high refractive index material layer, to obtain a 'double-layer' photonic crystal slab supporting guided resonances, appearing as peaks in the reflection spectrum. Morphological and optical characterizations are performed to investigate the effects of the fabrication process. Our results show how undesired effects, intrinsic to the fabrication procedure should be taken into account in order to guarantee a successful development of the device. Moreover, to demonstrate the flexibility of our approach and the possibility to engineering the resonances, a thin layer of gold is also deposited on the fiber tip, giving rise to a hybrid photonic-plasmonic structure with a complementary spectral response and different optical field distribution at the resonant wavelengths. Overall, this work represents a significant step forward the consolidation of Lab-on-Fiber Technology.
Project description:Cryo-electron tomography (cryoET) has become a powerful technique at the interface of structural biology and cell biology, due to its unique ability for imaging cells in their native state and determining structures of macromolecular complexes in their cellular context. A limitation of cryoET is its restriction to relatively thin samples. Sample thinning by cryo-focused ion beam (cryoFIB) milling has significantly expanded the range of samples that can be analyzed by cryoET. Unfortunately, cryoFIB milling is low-throughput, time-consuming and manual. Here, we report a method for fully automated sequential cryoFIB preparation of high-quality lamellae, including rough milling and polishing. We reproducibly applied this method to eukaryotic and bacterial model organisms, and show that the resulting lamellae are suitable for cryoET imaging and subtomogram averaging. Since our method reduces the time required for lamella preparation and minimizes the need for user input, we envision the technique will render previously inaccessible projects feasible.
Project description:We present experimental and simulation results for focused ion beam (FIB) milling of microchannels in lithium niobate in this paper. We investigate two different cuts of lithium niobate, Y- and Z-cuts, and observe that the experimental material removal rate in the FIB for both Y-cut and Z-cut samples was 0.3 μm(3)/nC, roughly two times greater than the material removal rate previously reported in the literature but in good agreement with the value we obtain from stopping and range of ions in matter (SRIM) simulations. Further, we investigate the FIB milling rate and resultant cross-sectional profile of microchannels at various ion beam currents and find that the milling rate decreases as a function of ion dose and correspondingly, the cross-sectional profiles change from rectangular to V-shaped. This indicates that material redeposition plays an important role at high ion dose or equivalently, high aspect ratio. We find that the experimental material removal rate decreases as a function of aspect ratio of the milled structures, in good agreement with our simulation results at low aspect ratio and in good agreement with the material removal rates previously reported in the literature at high aspect ratios. Our results show that it is indeed easier than previously assumed to fabricate nanochannels with low aspect ratio directly on lithium niobate using the FIB milling technique.
Project description:We present a microfluidic platform for studying structure-function relationships at the cellular level by connecting video rate live cell imaging with in situ microfluidic cryofixation and cryo-electron tomography of near natively preserved, unstained specimens. Correlative light and electron microscopy (CLEM) has been limited by the time required to transfer live cells from the light microscope to dedicated cryofixation instruments, such as a plunge freezer or high-pressure freezer. We recently demonstrated a microfluidic based approach that enables sample cryofixation directly in the light microscope with millisecond time resolution, a speed improvement of up to three orders of magnitude. Here we show that this cryofixation method can be combined with cryo-electron tomography (cryo-ET) by using Focused Ion Beam milling at cryogenic temperatures (cryo-FIB) to prepare frozen hydrated electron transparent sections. To make cryo-FIB sectioning of rapidly frozen microfluidic channels achievable, we developed a sacrificial layer technique to fabricate microfluidic devices with a PDMS bottom wall <5 µm thick. We demonstrate the complete workflow by rapidly cryo-freezing Caenorhabditis elegans roundworms L1 larvae during live imaging in the light microscope, followed by cryo-FIB milling and lift out to produce thin, electron transparent sections for cryo-ET imaging. Cryo-ET analysis of initial results show that the structural preservation of the cryofixed C. elegans was suitable for high resolution cryo-ET work. The combination of cryofixation during live imaging enabled by microfluidic cryofixation with the molecular resolution capabilities of cryo-ET offers an exciting avenue to further advance space-time correlative light and electron microscopy (st-CLEM) for investigation of biological processes at high resolution in four dimensions.
Project description:Various nanoscale fabrication techniques are elaborated to form artificial nanoporous/nanochannel membranes to be applied for biosensing: one of the most prevalent is the micro-electromechanical systems (MEMS) compatible focused ion beam (FIB) milling. This technique can be easily adopted in micro- and nanomachining process sequences to develop composite multi-pore structures, although its precision and reproducibility are key points in the case of these thick multi-layered membranes. This work is to demonstrate a comprehensive characterisation of FIB milling to improve the reliability of the fabrication of solid state nanopore arrays with precisely predetermined pore geometries for a targeted molecule type to be recognised. The statistical geometric features of the fabricated nanopores were recorded as the function of the process parameters, and the resulting geometries were analysed in detail by high resolution scanning electron microscope (SEM), transmission electron microscope (TEM) and ion scanning microscopy. Continuous function of the pore diameter evolution rate was derived from the experimental results in the case of different material structures, and compared to former dissentient estimations. The additional metal layer was deposited onto the backside of the membrane and grounded during the ion milling to prevent the electrical charging of dielectric layers. The study proved that the conformity of the pore geometry and the reliability of their fabrication could be improved significantly. The applicability of the developed nanopore arrays for molecule detection was also considered by characterising the pore diameter dependent sensitivity of the membrane impedance modulation based measurement method.
Project description:Recent advances have made cryogenic (cryo) electron microscopy a key technique to achieve near-atomic-resolution structures of biochemically isolated macromolecular complexes. Cryo-electron tomography (cryo-ET) can give unprecedented insight into these complexes in the context of their natural environment. However, the application of cryo-ET is limited to samples that are thinner than most cells, thereby considerably reducing its applicability. Cryo-focused-ion-beam (cryo-FIB) milling has been used to carve (micromachining) out 100-250-nm-thin regions (called lamella) in the intact frozen cells. This procedure opens a window into the cells for high-resolution cryo-ET and structure determination of biomolecules in their native environment. Further combination with fluorescence microscopy allows users to determine cells or regions of interest for the targeted fabrication of lamellae and cryo-ET imaging. Here, we describe how to prepare lamellae using a microscope equipped with both FIB and scanning electron microscopy modalities. Such microscopes (Aquilos Cryo-FIB/Scios/Helios or CrossBeam) are routinely referred to as dual-beam microscopes, and they are equipped with a cryo-stage for all operations in cryogenic conditions. The basic principle of the described methodologies is also applicable for other types of dual-beam microscopes equipped with a cryo-stage. We also briefly describe how to integrate fluorescence microscopy data for targeted milling and critical considerations for cryo-ET data acquisition of the lamellae. Users familiar with cryo-electron microscopy who get basic training in dual-beam microscopy can complete the protocol within 2-3 d, allowing for several pause points during the procedure.
Project description:In recent years, nanomachining has attracted increasing attention in advanced manufacturing science and technologies as a value-added processes to control material structures, components, devices, and nanoscale systems. To make sub-micro patterns on these products, micro/nanoscale single-crystal diamond cutting tools are essential. Popular non-contact methods for the macro/micro processing of diamond composites are pulsed laser ablation (PLA) and electric discharge machining (EDM). However, for manufacturing nanoscale diamond tools, these machining methods are not appropriate. Despite diamond's extreme physical properties, diamond can be micro/nano machined relatively easily using a focused ion beam (FIB) technique. In the FIB milling process, the surface properties of the diamond cutting tool is affected by the amorphous damage layer caused by the FIB gallium ion collision and implantation and these influence the diamond cutting tool edge sharpness and increase the processing procedures. To protect the diamond substrate, a protection layer-platinum (Pt) coating is essential in diamond FIB milling. In this study, the depth of Pt coating layer which could decrease process-induced damage during FIB fabrication is investigated, along with methods for removing the Pt coating layer on diamond tools. The optimum Pt coating depth has been confirmed, which is very important for maintaining cutting tool edge sharpness and decreasing processing procedures. The ultra-precision grinding method and etching with aqua regia method have been investigated for removing the Pt coating layer. Experimental results show that when the diamond cutting tool width is bigger than 500 nm, ultra-precision grinding method is appropriate for removing Pt coating layer on diamond tool. However, the ultra-precision grinding method is not recommended for removing the Pt coating layer when the cutting tool width is smaller than 500 nm, because the possibility that the diamond cutting tool is damaged by the grinding process will be increased. Despite the etching method requiring more procedures to remove the Pt coating layer after FIB milling, it is a feasible method for diamond tools with under 500 nm width.
Project description:The development of xenon plasma focused ion-beam (Xe+ PFIB) milling technique enables site-specific sample preparation with milling rates several times larger than the conventional gallium focused ion-beam (Ga+ FIB) technique. As such, the effect of higher beam currents and the heavier ions utilized in the Xe+ PFIB system is of particular importance when investigating material properties. To investigate potential artifacts resulting from these new parameters, a comparative study is performed on transmission electron microscopy (TEM) samples prepared via Xe+ PFIB and Ga+ FIB systems. Utilizing samples prepared with each system, the mechanical properties of CrMnFeCoNi high-entropy alloy (HEA) samples are evaluated with in situ tensile straining TEM studies. The results show that HEA samples prepared by Xe+ PFIB present better ductility but lower strength than those prepared by Ga+ FIB. This is due to the small ion-irradiated volumes and the insignificant alloying effect brought by Xe irradiation. Overall, these results demonstrate that Xe+ PFIB systems allow for a more efficient material removal rate while imparting less damage to HEAs than conventional Ga+ FIB systems.
Project description:Hydrogen pick-up leading to hydride formation is often observed in commercially pure Ti (CP-Ti) and Ti-based alloys prepared for microscopic observation by conventional methods, such as electro-polishing and room temperature focused ion beam (FIB) milling. Here, we demonstrate that cryogenic FIB milling can effectively prevent undesired hydrogen pick-up. Specimens of CP-Ti and a Ti dual-phase alloy (Ti-6Al-2Sn-4Zr-6Mo, Ti6246, in wt.%) were prepared using a xenon-plasma FIB microscope equipped with a cryogenic stage reaching -135 °C. Transmission electron microscopy (TEM), selected area electron diffraction, and scanning TEM indicated no hydride formation in cryo-milled CP-Ti lamellae. Atom probe tomography further demonstrated that cryo-FIB significantly reduces hydrogen levels within the Ti6246 matrix compared with conventional methods. Supported by molecular dynamics simulations, we show that significantly lowering the thermal activation for H diffusion inhibits undesired environmental hydrogen pick-up during preparation and prevents pre-charged hydrogen from diffusing out of the sample, allowing for hydrogen embrittlement mechanisms of Ti-based alloys to be investigated at the nanoscale.
Project description:The controlled creation of defect centre-nanocavity systems is one of the outstanding challenges for efficiently interfacing spin quantum memories with photons for photon-based entanglement operations in a quantum network. Here we demonstrate direct, maskless creation of atom-like single silicon vacancy (SiV) centres in diamond nanostructures via focused ion beam implantation with ∼32 nm lateral precision and <50 nm positioning accuracy relative to a nanocavity. We determine the Si+ ion to SiV centre conversion yield to be ∼2.5% and observe a 10-fold conversion yield increase by additional electron irradiation. Low-temperature spectroscopy reveals inhomogeneously broadened ensemble emission linewidths of ∼51 GHz and close to lifetime-limited single-emitter transition linewidths down to 126±13 MHz corresponding to ∼1.4 times the natural linewidth. This method for the targeted generation of nearly transform-limited quantum emitters should facilitate the development of scalable solid-state quantum information processors.