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Ultramicroscopy 202 (2019) 121–127 Ultramicroscopy 202 (2019) 121–127 Contents lists available at ScienceDirect Ultramicroscopy journal homepage: www.elsevier.com/locate/ultramic An in-situ approach for preparing atom probe tomography specimens by T xenon plasma-focussed ion beam ⁎ ⁎ J.E. Halpina, , R.W.H. Webstera, H. Gardnerb, M.P. Moodyb, P.A.J. Bagotb, , D.A. MacLarena a SUPA, School of Physics and Astronomy, University of Glasgow, Glasgow G12 8QQ, UK b Department of Materials, University of Oxford, Parks Road, Oxford OX1 3PH, UK ARTICLE INFO ABSTRACT Keywords: A method for the rapid preparation of atom probe tomography (APT) needles using a xenon plasma-focussed ion Atom probe tomography beam (FIB) instrument is presented and demonstrated on a test sample of Ti-6Al-4V alloy. The method requires Sample preparation significantly less operator input than the standard lift-out protocol, is site-specific and produces needleswith Focussed ion beam minimal ion-beam damage; electron microscopy indicated the needle's surface amorphised/oxidised region to be less than 2 nm thick. The resulting needles were routinely analysable by APT, confirming the expected micro- structure and showing negligible Xe contamination. 1. Introduction microtip coupon, each isolated from its neighbours and milled to a needle-shape geometry. The entire process can be completed in a few Atom probe tomography (APT) has become an indispensable tool hours for amenable samples, but can take several for more problematic for advanced materials characterization, providing unique nano-scale materials. A number of steps in the process are vulnerable to critical insights into an ever-expanding range of materials. Aside from advances problems, which can reduce the yield. Problems include failure to re- in laser-pulsing, which have enabled the examination of more fragile, move sufficient material before attempting to extract the cantilever, less electrically-conductive specimens, a major improvement to APT mis-handling with the manipulator and poor adhesion of the finished methodology has come through the use of focussed ion beam (FIB) needle to the coupon posts. For the latter, even if the samples appear instruments for sample preparation, which have greatly improved sufficiently stable, the electric or thermal pulses applied during APT sample yield and facilitated site-specific analyses [1,2]. FIB methods analysis often cause complete sample fracture. While only very limited have enabled precise location selection of the nanometre-sized analysis statistical studies on sample yield have been carried out to date, we volumes for APT, and continue to facilitate development of correlative have routinely observed in particular materials such as perovskites the techniques that link APT data to results from a range of complementary failure of samples at this junction. The time-consuming nature of FIB electron microscopy methods, including, for example, scanning trans- preparation has in many institutions become a bottleneck that limits mission electron microscopy (STEM) and transmission Kikuchi diffrac- greater usage of APT. A second problem is ion damage caused by the Ga tion (TKD). These have been used to correlate grain boundary or- beam, which is a universal concern, and has complicated the analyses of ientations with chemistries [3]. Despite these successes, FIB-based titanium alloys [4], various steels [5,6] and zirconium alloys [7]. Care methods for APT sample preparation can be involved and user-in- must also be taken to avoid inducing additional crystalline phases tensive, particularly for novel classes of materials. The most common through heating/implantation under the Ga beam. In addition, the re- procedure, used regardless of material type, is termed the ‘lift-out’ activity of Ga can be problematic and materials such as III-V semi- method, whereby the user selects a region of interest, typically conductors [8–10] and aluminium alloys [11] readily react with im- ∼30 × 5 μm on the surface of the sample. The region is firstly coated in planted Ga, modifying the chemistry and causing, for example, a protective layer to limit beam damage from the procedure. The sur- embrittlement, that can reduce APT yield. Thus, whilst Ga FIB proces- rounding material is then milled away using a Ga ion beam before a sing of APT samples offers key advantages over electropolishing micromanipulator tool is brought into contact with one end of the methods [12,13], it has fundamental limitations and any improvements cantilever-shape, which must then be carefully extracted. Multiple in APT specimen preparation would be of significant benefit to the samples are positioned onto individual posts of a custom-fabricated Si materials science community. ⁎ Corresponding authors. E-mail address: [email protected] (P.A.J. Bagot). https://doi.org/10.1016/j.ultramic.2019.04.005 Received 15 February 2019; Received in revised form 4 April 2019; Accepted 10 April 2019 Available online 12 April 2019 0304-3991/ © 2019 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY license (http://creativecommons.org/licenses/BY/4.0/). J.E. Halpin, et al. Ultramicroscopy 202 (2019) 121–127 In the present work, we outline a promising approach for APT was milled at the side of the annulus (Fig. 1c) in order to improve sample preparation that does not require APT samples to be mounted visibility and ease of alignment with respect to the atom probe pulsed onto a separate coupon. We mill annular trenches directly into a flat laser. The routine then ran through a series of annular mills with sample to leave a central, free-standing shank with a geometry suitable carefully selected inner and outer radii at decreasing milling currents for APT. Direct fabrication of needles ‘in-situ’, without a separate mount (Fig. 1, d–f), resulting in a free-standing pillar with a 5 μm radius. For has been proposed previously [14], along with other strategies that use all annular mills, the scan direction was set as a circular path from outer masking to accelerate preparation times and minimise damage [15,16]. to inner diameter, ensuring the highest possible milling rates on the However, such in-situ needle fabrication has in general been limited to exposed edges. The outer diameter of the annular trenches illustrated is the edges of previously-thinned, wedge-shaped samples, because much ~250 μm, which is large enough to be visible under optical microscopy of the bulk material has already been removed and there is a convenient and to ensure that, when the sample is biased, the electric field at the path for any sputtered material to be removed during FIB milling tip is unaffected by the proximity of the sample's polished surface without re-deposition. In addition, the size of the annular trench re- outside of the milled region. The trench depth is 25 μm and each trench quired to isolate the APT needle from the electric field of the sur- takes of the order of 10s of minutes to mill, the rapidity of which il- rounding sample when biased necessitates high Ga currents and pro- lustrates one of the principal motivations for using P-FIB over Ga ion hibitively long milling times [14]. The performance of conventional Ga instruments. Moreover, as the software can work through a designated FIBs at high milling rates or currents is limited by increasing spot size of location map, it is feasible to have unattended fabrication of a number the liquid metal ion source (LMIS), which for high beam currents results of specimens, as shown by the set produced overnight in Fig. 1 h). in severely degraded performance [9]. However, FIB instruments Although drift correction was not necessary for the small number of equipped with a Xe plasma source (P-FIB) now deliver high beam needles prepared here, it could easily be incorporated into longer mil- currents along with far faster milling rates. The use of such Xe P-FIBs for ling routines. In a FIB-SEM system equipped with analytical capabilities APT sample preparation has been demonstrated previously [17], with such as electron back-scattered diffraction or energy dispersive x-ray the comparatively larger Xe ions showing a reduced penetration depth analysis, it is thus feasible to map the surface structure and chemistry of and increased sputter yield compared to Ga. TEM studies comparing Xe a planar sample, identify specific regions of interest for APT analysis, and Ga-based FIBs have shown a significant reduction, of up to 40%, in then leave the automated script to mill the annular trenches about those amorphous damage in Si using a Xe P-FIB [18]. Furthermore, the che- regions without user intervention. mically inert characteristics of Xe make such P-FIBs suitable for APT Below a 5 μm radius, direct observation of the needle is required so needle fabrication from Ga-sensitive materials. With these significant that milling and polishing can be stopped when it achieves an appro- advantages, we show a route to rapidly machine viable APT specimens priate radius. Thus, manual milling was performed using the same directly into the sample surface. The technique is site-specific, more methodology as that used to sculpt APT needles on coupons [4]. For the adaptable to microstructural features without lift-out limitations, and if smaller annular mills, the outer radius was fixed and only the inner the FIB is equipped with analytical techniques such as energy dispersive radii decreased, in order to avoid introduction of any additional sharp x-ray spectroscopy, they can be carried out prior to fabrication without peaks on the shank. Finally, the needles were finished with a low-en- need to adjust the stage geometry. Since the technique involves milling ergy polish at 5 kV and then 2 kV. This aspect of the methodology fol- without moving the sample, it is well suited to automation, further lows the same low-kV/low-energy ion polishing technique that is used reducing operator intervention.
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