A technique for improved focused ion beam milling of cryo-prepared life science specimens

The combination of focused ion beam and scanning electron microscopy with a cryo‐preparation/transfer system allows specimens to be milled at low temperatures. However, for biological specimens in particular, the quality of results is strongly dependent on correct preparation of the specimen surface. We demonstrate a method for deposition of a protective, planarizing surface layer onto a cryo‐sample, enabling high‐quality cross‐sectioning using the ion beam and investigation of structures at the nanoscale.     

应用聚焦离子束/电子束技术的碳纳米管探针制备工艺研究

提出利用电子束诱导铂沉积和聚焦离子束铣削技术,实现碳纳米管原子力显微镜探针针尖的制备和结构优化研究。结合高分辨率扫描电子显微镜观测和纳米操纵仪,利用电子束诱导铂沉积实现碳纳米管固定到普通原子力显微镜探针末端,可实现直径小于10nm的纳米管探针制备。提出基于聚焦离子束铣削和照射技术实现对纳米管针尖的长度、角度的精确调控优化,纳米管探针的角度调控精度优于1°。     

Effect of gallium focused ion beam milling on preparation of aluminium thin foils

Focussed ion beam milling has greatly extended the utility of the atom probe and transmission electron microscope because it enables sample preparation with a level of dimensional control never before possible. Using focussed ion beam it is possible to extract the samples from desired and very specific locations. The artefacts associated with this sample preparation method must also be fully understood. In this work, issues specifically relevant to the focussed ion beam milling of aluminium alloys are presented. After using the focussed ion beam as a sample preparation technique it is evident that gallium will concentrate in three areas of the sample: on the surface, on grain boundaries and at interphase boundaries. This work also shows that low-energy Ar ion nanomilling is potentially quite effective for removing gallium implantation layers and gallium from the internal surfaces of aluminium thin foils.     

Deposition and focused ion beam milling of anticorrosive CrC coatings on tool steel substrates

For micro replication, the base of a die should be ductile and the surface layer that will undergo processing should have a good machining response to various tool-making processes. At the same time, the resulting working surfaces of the tooling cavities should be hard; having low roughness, low wettability and high erosion resistance. To achieve such diverse properties, nano-crystalline CrC coatings deposited onto 12% Cr tool steel were investigated in this research. To verify the properties of such coatings various metallographic techniques were applied. In particular, the corrosion resistance was studied by means of potentiodynamic anodic polarisation. A scanning transmission electron microscopy analysis of the structure was performed on samples prepared with focused ion beam (FIB) machining. The mechanical properties and grain size distribution were determined and statistically analysed. In addition, X-ray diffraction, scanning electron microscopy and atomic force microscopy were used in studying the surface properties of these coatings. To investigate the response of the CrC coatings to micro- and nano-structuring technologies with high specific energy, a series of rectangular trenches were produced by FIB milling. The effects of the ion beam current, exposure time and ion fluence on the sputtering yield and roughness of the produced micro-structures were especially investigated. Some essential parameter windows for performing FIB milling with relatively high sputtering rates, higher than 1?µm/min, and at the same time achieving the best possible surface integrity were determined during the experiments.     

Preparation of site-specific cross-sections of heterogeneous catalysts prepared by focused ion beam milling

Focused ion beam (FIB) milling offers a novel approach to preparation of site‐specific cross‐sections of heterogeneous catalysts for examination in the transmission electron microscope (TEM). Electron‐transparent sections can be obtained without the need to embed or grind the original sample. Because the specimen can be imaged in the FIB with submicrometre resolution before, during and after milling it is possible to select precisely the region from which the section is removed and to control the thickness of the section to within tens of nanometres. The ability to produce sections in this way opens the possibility of studying a range of catalyst systems that have previously been impossible to examine with the TEM.     

Focused ion beam milling for prototyping 2D and 3D photonic structures

Focused ion beam (FIB) milling is widely used in fields such as the semiconductor industry and materials science research. The direct writing and small fea     

Quantitative off-axis electron holography of GaAs p-n junctions prepared by focused ion beam milling

Focused Ion beam (FIB) prepared GaAs p-n junctions have been examined using off-axis electron holography. Initial analysis of the holograms reveals an experimentally determined built-in potential in the junctions that is significantly smaller than predicted from theory. In this paper we show that through combinations of in situ annealing and in situ biasing of the specimens, by varying the intensity of the incident electron beam, and by modifying the FIB operating parameters, we can develop an improved understanding of phenomena such as the electrically 'inactive' thickness and subsequently recover the predicted value of the built-in potential of the junctions.
PACS numbers: 85.30.De     

Preparation of transmission electron microscopy cross-section specimens of crack tips using focused ion beam milling

The preparation of transmission electron microscope (TEM) thin foil specimens from metal alloys containing cracks is usually thwarted by the difficulty in preventing preferential erosion of material along the flanks and at the tips of cracks. Recent developments in focused ion beam (FIB) micromachining methods have the potential to overcome this inherent problem. In this article we describe the development of new procedures, one using FIB alone and the other using a combination of FIB with more conventional ion milling to generate TEM specimens that largely retain the microstructural information at stress corrosion cracks in austentic alloys. Examples of corrosion product phase identification and interfacial segregation are included to verify that detailed information is not destroyed by ion bombardment during specimen preparation.     

Transmission electron microscopy of fluorapatite–gelatine composite particles prepared using focused ion beam milling

In this paper, synthetic fluorapatite–gelatine composite particles are prepared for transmission electron microscopy (TEM) studies using two methods based on focused ion beam (FIB) milling. TEM studies on the FIB‐prepared specimens are compared with TEM observations on samples prepared using an ultramicrotome. The results show that ultramicrotome slicing causes significant cracking of the apatite, whereas the ion beam can be used to make high‐quality, crack‐free specimens with no apparent ion beam‐induced damage. The TEM observations on the FIB‐prepared samples confirm that the fluorapatite composite particles are composed of elongated, preferentially orientated grains and reveal that the grain boundaries contain many small interstices filled with an amorphous phase.     

Direct and transmission milling of suspended silicon nitride membranes with a focused helium ion beam

Helium ion milling of suspended silicon nitride thin films is explored. Milled squares patterned by scanning helium ion microscope are subsequently investigated by atomic force microscopy and the relation between ion dose and milling depth is measured for both the direct (side of ion incidence) and transmission (side opposite to ion incidence) regimes. We find that direct-milling depth varies linearly with beam dose while transmission-milling depth varies with the square of the beam dose, resulting in a straightforward method of controlling local film thickness.     

Effects of focused ion beam milling on electron backscatter diffraction patterns in strontium titanate and stabilized zirconia

This study investigates the effect of focused ion beam (FIB) current and accelerating voltage on electron backscatter diffraction pattern quality of yttria-stabilized zirconia (YSZ) and Nb-doped strontium titanate (STN) to optimize data quality and acquisition time for 3D-EBSD experiments by FIB serial sectioning. Band contrast and band slope were used to describe the pattern quality. The FIB probe currents investigated ranged from 100 to 5000 pA and the accelerating voltage was either 30 or 5 kV. The results show that 30 kV FIB milling induced a significant reduction of the pattern quality of STN samples compared to a mechanically polished surface but yielded a high pattern quality on YSZ. The difference between STN and YSZ pattern quality is thought to be caused by difference in the degree of ion damage as their backscatter coefficients and ion penetration depths are virtually identical. Reducing the FIB probe current from 5000 to 100 pA improved the pattern quality by 20% for STN but only showed a marginal improvement for YSZ. On STN, a conductive coating can help to improve the pattern quality and 5 kV polishing can lead to a 100% improvement of the pattern quality relatively to 30 kV FIB milling. For 3D-EBSD experiments of a material such as STN, it is recommended to combine a high kV FIB milling and low kV polishing for each slice in order to optimize the data quality and acquisition time.     

Conventional and back-side focused ion beam milling for off-axis electron holography of electrostatic potentials in transistors

Off-axis electron holography is used to characterize a linear array of transistors, which was prepared for examination in cross-sectional geometry in the transmission electron microscope (TEM) using focused ion beam (FIB) milling from the substrate side of the semiconductor device. The measured electrostatic potential is compared with results obtained from TEM specimens prepared using the more conventional 'trench' FIB geometry. The use of carbon coating to remove specimen charging effects, which result in electrostatic fringing fields outside 'trench' specimens, is demonstrated. Such fringing fields are not observed after milling from the substrate side of the device. Analysis of the measured holographic phase images suggests that the electrically inactive layer on the surface of each FIB-milled specimen typically has a thickness of 100 nm.     

TEM foil preparation of sub-micrometre sized individual grains by focused ion beam technique

Analysis of presolar silicate grains provides new knowledge on interstellar and circumstellar environments and can be used to test models of the Galactic chemical evolution. However, structural information of these grains is rare because sample preparation for transmission electron microscopy is very difficult due to the small dimensions of these grains (<0.5 μm). With the use of the focused ion beam technique thin foils from these grains for transmission electron microscopy analysis can be prepared. Nevertheless, reaching the required precision of some tens of nanometres for the preparation of the transmission electron microscopy foil in the place of interest is not trivial. Furthermore, in the current samples, the grain of interest can only be identified by its different isotopic composition; i.e. there is no contrast difference in scanning electron microscopy or transmission electron microscopy images which allow the identification of the grain. Therefore, the grain has to be marked in some way before preparing the transmission electron microscopy foil. In the present paper, a method for transmission electron microscopy foil preparation of grains about 200 to 400 nm in diameter is presented. The method utilizes marking of the grain by Pt deposition and milling of holes to aid in the exact orientation of the transmission electron microscopy foil with respect to the grain. The proposed method will be explained in detail by using an example grain.     

A review of focused ion beam sputtering

This paper reviews the applications of focused ion beam (FIB) sputtering for micro/nano fabrication. Basic principles of FIB were briefly discussed, and then empirical and fundamental models for sputtering yield, material removal rate, and surface roughness were presented and compared. The empirical models were more useful for application compared to fundamental models. Fabrication of various micro and nano structures was discussed. Trimmed atomic force microscope (AFM) tips were tested in measurement and imaging of high aspect ratio nanopillars where higher accuracy and clarity were observed. Micromilling tool fabricated using FIB sputtering was used to machine microchannels. Slicing and dwell time control approaches on FIB sputtering were presented for the fabrication of three dimensional microcavities. The first approach is preferred for practical applications. The maximum aspect ratio of 13:1 of the microstructures was achieved. The minimum size of the nanopore was in the range of 2–10 μm. Cavities of microgear of 70 μm outside diameter were sputtered with submicrometer accuracy and 2–5 nm average surface roughness. The microcavities were then filled with polymer in a subsequent micromodling process. The replicated microcomponents were inspected with scanning electron microscope where faithful duplication of accuracy and surface texture of the cavity was observed.     

Preparation of TEM samples of metal–oxide interface by the focused ion beam technique

This paper describes a procedure to prepare metal–oxide interfaces for transmission electron microscopy by the focused ion beam technique. The advantage of this procedure is to allow the observation of metal–oxide interfaces of irradiated samples with a homogeneous thickness without the need to have an instrument inside laboratories that are specialized for the manipulation of irradiated materials. A transmission electron microscopy sample is prepared by this method and analysed.     

Focussed ion beam milling at grazing incidence angles

A combined scanning electron microscope and focussed ion beam instrument is suitable for micro- and nanopatterning, cross-sectioning and subsequent imaging, of specimens at room temperature as well as under cryo conditions. In order to reveal internal details, samples are conventionally milled with the ion beam positioned perpendicular to the sample surface. Using this approach certain limitations are frequently encountered, e.g. accumulation of redeposited material, shadowing effects, image distortion and a limited imaging area. Here we show an approach in which samples are pre-trimmed using a microtome to obtain a sample block face that is parallel to the ion beam. This new grazing incidence geometry eliminates the need for removal of bulk material with the ion beam and enables immediate fine polishing of a pre-selected area of interest. Many of the limitations previously described are avoided and in addition milling time is reduced, whilst creating larger cross-sectional areas. Another advantage is that electron imaging can be accomplished by tilting the sample surface perpendicular to the electron beam, providing a geometrically undistorted image. The proposed approach is suitable for materials that can be microtomed, both in ambient and cryogenic conditions, and proves to be of particular benefit for biological and food samples.     

Reduction of electrical damage in specimens prepared using focused ion beam milling for dopant profiling using off-axis electron holography

GaAs specimens containing p-n junctions have been prepared using focused ion beam (FIB) milling for examination using off-axis electron holography. By lowering the FIB operating voltage from 30 to 8 kV, we have shown a systematic reduction of the electrically 'inactive' thickness from 220 to 100 nm, resulting in a significant increase in the step in phase measured across the junctions as well as an improvement in the signal-to-noise ratio. We also show that the step in phase measured across the junctions can be influenced by the intensity of the electron beam.     

The prospects of a subnanometer focused neon ion beam

The success of the helium ion microscope has encouraged extensions of this technology to produce beams of other ion species. A review of the various candidate ion beams and their technical prospects suggest that a neon beam might be the most readily achieved. Such a neon beam would provide a sputtering yield that exceeds helium by an order of magnitude while still offering a theoretical probe size less than 1-nm. This article outlines the motivation for a neon gas field ion source, the expected performance through simulations, and provides an update of our experimental progress.     

Subcutoff microwave driven plasma ion sources for multielemental focused ion beam systems

A compact microwave driven plasma ion source for focused ion beam applications has been developed. Several gas species have been experimented including argon, krypton, and hydrogen. The plasma, confined by a minimum B multicusp magnetic field, has good radial and axial uniformity. The octupole multicusp configuration shows a superior performance in terms of plasma density (~1.3 x 10(11) cm(-3)) and electron temperature (7-15 eV) at a power density of 5-10 Wcm(2). Ion current densities ranging from a few hundreds to over 1000 mA/cm(2) have been obtained with different plasma electrode apertures. The ion source will be combined with electrostatic Einzel lenses and should be capable of producing multielemental focused ion beams for nanostructuring and implantations. The initial simulation results for the focused beams have been presented.