Automated Sample Depth Targeting with Low kV Cleaning by Focused Ion Beam Microscopy for Atom Probe Tomography

Author(s):  
Woo Jun Kwon ◽  
Jisu Ryu ◽  
Christopher H. Kang ◽  
Michael B. Schmidt ◽  
Nicholas Croy

Abstract Focused ion beam (FIB) microscopy is an essential technique for the site-specific sample preparation of atom probe tomography (APT). The site specific APT and automated APT sample preparation by FIB have allowed increased APT sample volume. In the workflow of APT sampling, it is very critical to control depth of the sample where exact region of interest (ROI) for accurate APT analysis. Very precise depth control is required at low kV cleaning process in order to remove the damaged layer by previous high kV FIB process steps. We found low kV cleaning process with 5 kV and followed by 2kV beam conditions delivers better control to reached exact ROI on Z direction. This understanding is key to make APT sample with fully automated fashion.

Author(s):  
Jian-Shing Luo ◽  
Hsiu Ting Lee

Abstract Several methods are used to invert samples 180 deg in a dual beam focused ion beam (FIB) system for backside milling by a specific in-situ lift out system or stages. However, most of those methods occupied too much time on FIB systems or requires a specific in-situ lift out system. This paper provides a novel transmission electron microscopy (TEM) sample preparation method to eliminate the curtain effect completely by a combination of backside milling and sample dicing with low cost and less FIB time. The procedures of the TEM pre-thinned sample preparation method using a combination of sample dicing and backside milling are described step by step. From the analysis results, the method has applied successfully to eliminate the curtain effect of dual beam FIB TEM samples for both random and site specific addresses.


Author(s):  
Roger Alvis ◽  
Jeff Blackwood ◽  
Sang-Hoon Lee ◽  
Matthew Bray

Abstract Semiconductor devices with critical dimensions less than 20nm are now being manufactured in volume. A challenge facing the failure analysis and process-monitoring community is two-fold. The first challenge of TEM sample prep of such small devices is that the basic need to end-point on a feature-of-interest pushes the imaging limit of the instrument being used to prepare the lamella. The second challenge posed by advanced devices is to prepare an artifact-free lamella from non-planar devices such as finFETs as well as from structures incorporating ‘non-traditional’ materials. These challenges are presently overcome in many advanced logic and memory devices in the focused ion beam-based TEM sample preparation processes by inverting the specimen prior to thinning to electron transparency. This paper reports a highthroughput method for the routine preparation of artifact-free TEM lamella of 20nm thickness, or less.


2013 ◽  
Vol 19 (4) ◽  
pp. 1080-1091 ◽  
Author(s):  
Felipe Rivera ◽  
Robert Davis ◽  
Richard Vanfleet

AbstractTransmission electron microscopy (TEM) and focused ion beam (FIB) are proven tools to produce site-specific samples in which to study devices from initial processing to causes for failure, as well as investigating the quality, defects, interface layers, etc. However, the use of polymer substrates presents new challenges, in the preparation of suitable site-specific TEM samples, which include sample warping, heating, charging, and melting. In addition to current options that address some of these problems such as cryo FIB, we add an alternative method and FIB sample geometry that address these challenges and produce viable samples suitable for TEM elemental analysis. The key feature to this approach is a larger than usual lift-out block into which small viewing windows are thinned. Significant largely unthinned regions of the block are left between and at the base of the thinned windows. These large unthinned regions supply structural support and thermal reservoirs during the thinning process. As proof-of-concept of this sample preparation method, we also present TEM elemental analysis of various thin metallic films deposited on patterned polycarbonate, lacquer, and poly-di-methyl-siloxane substrates where the pattern (from low- to high-aspect ratio) is preserved.


2015 ◽  
Vol 21 (3) ◽  
pp. 544-556 ◽  
Author(s):  
Fengzai Tang ◽  
Michael P. Moody ◽  
Tomas L. Martin ◽  
Paul A.J. Bagot ◽  
Menno J. Kappers ◽  
...  

AbstractVarious practical issues affecting atom probe tomography (APT) analysis of III-nitride semiconductors have been studied as part of an investigation using a c-plane InAlN/GaN heterostructure. Specimen preparation was undertaken using a focused ion beam microscope with a mono-isotopic Ga source. This enabled the unambiguous observation of implantation damage induced by sample preparation. In the reconstructed InAlN layer Ga implantation was demonstrated for the standard “clean-up” voltage (5 kV), but this was significantly reduced by using a lower voltage (e.g., 1 kV). The characteristics of APT data from the desorption maps to the mass spectra and measured chemical compositions were examined within the GaN buffer layer underlying the InAlN layer in both pulsed laser and pulsed voltage modes. The measured Ga content increased monotonically with increasing laser pulse energy and voltage pulse fraction within the examined ranges. The best results were obtained at very low laser energy, with the Ga content close to the expected stoichiometric value for GaN and the associated desorption map showing a clear crystallographic pole structure.


Author(s):  
V. V. Khoroshilov ◽  
O. A. Korchuganova ◽  
A. A. Lukyanchuk ◽  
O. A. Raznitsyn ◽  
A. A. Aleev ◽  
...  

2018 ◽  
Vol 188 ◽  
pp. 19-23 ◽  
Author(s):  
J. Bogdanowicz ◽  
A. Kumar ◽  
C. Fleischmann ◽  
M. Gilbert ◽  
J. Houard ◽  
...  

2019 ◽  
Vol 9 (13) ◽  
pp. 2721 ◽  
Author(s):  
Cédric Barroo ◽  
Austin J. Akey ◽  
David C. Bell

Atom probe tomography is a well-established analytical instrument for imaging the 3D structure and composition of materials with high mass resolution, sub-nanometer spatial resolution and ppm elemental sensitivity. Thanks to recent hardware developments in Atom Probe Tomography (APT), combined with progress on site-specific focused ion beam (FIB)-based sample preparation methods and improved data treatment software, complex materials can now be routinely investigated. From model samples to complex, usable porous structures, there is currently a growing interest in the analysis of catalytic materials. APT is able to probe the end state of atomic-scale processes, providing information needed to improve the synthesis of catalysts and to unravel structure/composition/reactivity relationships. This review focuses on the study of catalytic materials with increasing complexity (tip-sample, unsupported and supported nanoparticles, powders, self-supported catalysts and zeolites), as well as sample preparation methods developed to obtain suitable specimens for APT experiments.


2016 ◽  
Vol 23 (2) ◽  
pp. 321-328 ◽  
Author(s):  
David R. Diercks ◽  
Brian P. Gorman ◽  
Johannes J. L. Mulders

AbstractSix precursors were evaluated for use as in situ electron beam-induced deposition capping layers in the preparation of atom probe tomography specimens with a focus on near-surface features where some of the deposition is retained at the specimen apex. Specimens were prepared by deposition of each precursor onto silicon posts and shaped into sub-70-nm radii needles using a focused ion beam. The utility of the depositions was assessed using several criteria including composition and uniformity, evaporation behavior and evaporation fields, and depth of Ga+ ion penetration. Atom probe analyses through depositions of methyl cyclopentadienyl platinum trimethyl, palladium hexafluoroacetylacetonate, and dimethyl-gold-acetylacetonate [Me2Au(acac)] were all found to result in tip fracture at voltages exceeding 3 kV. Examination of the deposition using Me2Au(acac) plus flowing O2 was inconclusive due to evaporation of surface silicon from below the deposition under all analysis conditions. Dicobalt octacarbonyl [Co2(CO)8] and diiron nonacarbonyl [Fe2(CO)9] depositions were found to be effective as in situ capping materials for the silicon specimens. Their very different evaporation fields [36 V/nm for Co2(CO)8 and 21 V/nm for Fe2(CO)9] provide options for achieving reasonably close matching of the evaporation field between the capping material and many materials of interest.


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