Redistribution of Alloy Elements during Nickel Silicide Formation: Benefit of Atom Probe Tomography

2011 ◽  
Vol 309-310 ◽  
pp. 161-166 ◽  
Author(s):  
C. Perrin ◽  
K. Hoummada ◽  
I. Blum ◽  
A. Portavoce ◽  
M. Descoins ◽  
...  

The unique capabilities of atom probe tomography (APT) to characterize internal interfaces and layer chemistry with sub-nanometer scale resolution in three dimensions have been recently opened up to materials with poor electrical conductivity by the use of ultrafast laser pulses. The progress in sample preparation (focused ion beam) as well as in instrument performance enable now the analysis of relatively large volumes with typical diameters of 100 to 200 nm and depths of several hundred nm (this corresponds to an increase by several order of magnitude compared to the former instrument) of site specific samples. In this work, APT is used to study the effects of Pt on the formation and stability of Ni silicides. The precise location of this alloy element has been determined at the nanometer scale: In particular, APT allows us to quantify the amount of Pt in the grain boundaries (GB) of Ni2Si for about 100 different grain boundaries and thus to better characterize the GB diffusion and segregation.

2015 ◽  
Vol 21 (3) ◽  
pp. 557-563 ◽  
Author(s):  
Björn Pfeiffer ◽  
Torben Erichsen ◽  
Eike Epler ◽  
Cynthia A. Volkert ◽  
Piet Trompenaars ◽  
...  

AbstractA method to characterize open-cell nanoporous materials with atom probe tomography (APT) has been developed. For this, open-cell nanoporous gold with pore diameters of around 50 nm was used as a model system, and filled by electron beam-induced deposition (EBID) to obtain a compact material. Two different EBID precursors were successfully tested—dicobalt octacarbonyl [Co2(CO)8] and diiron nonacarbonyl [Fe2(CO)9]. Penetration and filling depth are sufficient for focused ion beam-based APT sample preparation. With this approach, stable APT analysis of the nanoporous material can be performed. Reconstruction reveals the composition of the deposited precursor and the nanoporous material, as well as chemical information of the interfaces between them. Thus, it is shown that, using an appropriate EBID process, local chemical information in three dimensions with sub-nanometer resolution can be obtained from nanoporous materials using APT.


2016 ◽  
Vol 22 (3) ◽  
pp. 583-588 ◽  
Author(s):  
Katherine P. Rice ◽  
Yimeng Chen ◽  
Ty J. Prosa ◽  
David J. Larson

AbstractThere are advantages to performing transmission electron backscattering diffraction (tEBSD) in conjunction with focused ion beam-based specimen preparation for atom probe tomography (APT). Although tEBSD allows users to identify the position and character of grain boundaries, which can then be combined with APT to provide full chemical and orientation characterization of grain boundaries, tEBSD can also provide imaging information that improves the APT specimen preparation process by insuring proper placement of the targeted grain boundary within an APT specimen. In this report we discuss sample tilt angles, ion beam milling energies, and other considerations to optimize Kikuchi diffraction pattern quality for the APT specimen geometry. Coordinated specimen preparation and analysis of a grain boundary in a Ni-based Inconel 600 alloy is used to illustrate the approach revealing a 50° misorientation and trace element segregation to the grain boundary.


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.


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 ◽  
...  

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.


2013 ◽  
Vol 19 (S2) ◽  
pp. 974-975 ◽  
Author(s):  
D. Isheim ◽  
F.J. Stadermann ◽  
J.B. Lewis ◽  
C. Floss ◽  
T.L. Daulton ◽  
...  

Extended abstract of a paper presented at Microscopy and Microanalysis 2013 in Indianapolis, Indiana, USA, August 4 – August 8, 2013.


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