Fabrication of Atom Probe Tomography Specimens from Nanoparticles Using a Fusible Bi–In–Sn Alloy as an Embedding Medium

2019 ◽  
Vol 25 (2) ◽  
pp. 438-446 ◽  
Author(s):  
Se-Ho Kim ◽  
Ji Yeong Lee ◽  
Jae-Pyoung Ahn ◽  
Pyuck-Pa Choi
Keyword(s):  
Sodium Borohydride ◽  
Atom Probe Tomography ◽  
Iron Nanoparticles ◽  
Focused Ion Beam ◽  
Reduction Method ◽  
Ion Beam ◽  
Atom Probe ◽  
Sodium Borohydride Reduction ◽  
Embedding Medium ◽  
Cryogenic Conditions

AbstractWe propose a new method for preparing atom probe tomography specimens from nanoparticles using a fusible bismuth–indium–tin alloy as an embedding medium. Iron nanoparticles synthesized by the sodium borohydride reduction method were chosen as a model system. The as-synthesized iron nanoparticles were embedded within the fusible alloy using focused ion beam milling and ion-milled to needle-shaped atom probe specimens under cryogenic conditions. An atom probe analysis revealed boron atoms in a detected iron nanoparticle, indicating that boron from the sodium borohydride reductant was incorporated into the nanoparticle during its synthesis.

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

2020 ◽  
Author(s):  
Woo Jun Kwon ◽  
Jisu Ryu ◽  
Christopher H. Kang ◽  
Michael B. Schmidt ◽  
Nicholas Croy
Keyword(s):  
Sample Preparation ◽  
Atom Probe Tomography ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Region Of Interest ◽  
Atom Probe ◽  
Sample Volume ◽  
Cleaning Process ◽  
Site Specific ◽  
Sample Depth

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.

scholarly journals Practical Issues for Atom Probe Tomography Analysis of III-Nitride Semiconductor Materials

2015 ◽  
Vol 21 (3) ◽  
pp. 544-556 ◽  
Author(s):  
Fengzai Tang ◽  
Michael P. Moody ◽  
Tomas L. Martin ◽  
Paul A.J. Bagot ◽  
Menno J. Kappers ◽  
...  
Keyword(s):  
Atom Probe Tomography ◽  
Focused Ion Beam ◽  
Laser Energy ◽  
Ion Beam ◽  
Atom Probe ◽  
Specimen Preparation ◽  
Chemical Compositions ◽  
Pole Structure ◽  
Gan Heterostructure ◽  
Ga Content

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.

On the Precision Preparation of Samples for Atom Probe Tomography Using a Focused Ion Beam in a SEM

2018 ◽  
Vol 12 (1) ◽  
pp. 87-93 ◽  
Author(s):  
V. V. Khoroshilov ◽  
O. A. Korchuganova ◽  
A. A. Lukyanchuk ◽  
O. A. Raznitsyn ◽  
A. A. Aleev ◽  
...  
Keyword(s):  
Atom Probe Tomography ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Atom Probe

scholarly journals Laser-assisted atom probe tomography of semiconductors: The impact of the focused-ion beam specimen preparation

2018 ◽  
Vol 188 ◽  
pp. 19-23 ◽  
Author(s):  
J. Bogdanowicz ◽  
A. Kumar ◽  
C. Fleischmann ◽  
M. Gilbert ◽  
J. Houard ◽  
...  
Keyword(s):  
Atom Probe Tomography ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Atom Probe ◽  
Beam Specimen ◽  
Specimen Preparation ◽  
The Impact

Electron Beam-Induced Deposition for Atom Probe Tomography Specimen Capping Layers

2016 ◽  
Vol 23 (2) ◽  
pp. 321-328 ◽  
Author(s):  
David R. Diercks ◽  
Brian P. Gorman ◽  
Johannes J. L. Mulders
Keyword(s):  
Electron Beam ◽  
Atom Probe Tomography ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Atom Probe ◽  
Near Surface ◽  
Surface Features ◽  
Dicobalt Octacarbonyl ◽  
Electron Beam Induced Deposition

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.

Characterization of Nanoporous Materials with Atom Probe Tomography

2015 ◽  
Vol 21 (3) ◽  
pp. 557-563 ◽  
Author(s):  
Björn Pfeiffer ◽  
Torben Erichsen ◽  
Eike Epler ◽  
Cynthia A. Volkert ◽  
Piet Trompenaars ◽  
...  
Keyword(s):  
Atom Probe Tomography ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Atom Probe ◽  
Nanoporous Materials ◽  
Three Dimensions ◽  
Chemical Information ◽  
Nanoporous Material ◽  
Open Cell ◽  
Dicobalt Octacarbonyl

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.

scholarly journals Combining Atom-Probe Tomography and Focused-Ion Beam Microscopy to Study Individual Presolar Meteoritic Nanodiamond Particles

2013 ◽  
Vol 19 (S2) ◽  
pp. 974-975 ◽  
Author(s):  
D. Isheim ◽  
F.J. Stadermann ◽  
J.B. Lewis ◽  
C. Floss ◽  
T.L. Daulton ◽  
...  
Keyword(s):  
Atom Probe Tomography ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Atom Probe

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

Application of Focused Ion Beam to Atom Probe Tomography Specimen Preparation from Mechanically Alloyed Powders

2007 ◽  
Vol 13 (5) ◽  
pp. 347-353 ◽  
Author(s):  
Pyuck-Pa Choi ◽  
Tala'at Al-Kassab ◽  
Young-Soon Kwon ◽  
Ji-Soon Kim ◽  
Reiner Kirchheim
Keyword(s):  
Atom Probe Tomography ◽  
Structural Changes ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Atom Probe ◽  
High Energy ◽  
Specimen Preparation ◽  
Mechanically Alloyed ◽  
Cross Sectional ◽  
Beam Currents

Focused ion-beam milling has been applied to prepare needle-shaped atom probe tomography specimens from mechanically alloyed powders without the use of embedding media. The lift-out technique known from transmission electron microscopy specimen preparation was modified to cut micron-sized square cross-sectional blanks out of single powder particles. A sequence of rectangular cuts and annular milling showed the highest efficiency for sharpening the blanks to tips. First atom probe results on a Fe95Cu5 powder mechanically alloyed in a high-energy planetary ball mill for 20 h have been obtained. Concentration profiles taken from this powder sample showed that the Cu distribution is inhomogeneous on a nanoscale and that the mechanical alloying process has not been completed yet. In addition, small clusters of oxygen, stemming from the ball milling process, have been detected. Annular milling with 30 keV Ga ions and beam currents ≥50 pA was found to cause the formation of an amorphous surface layer, whereas no structural changes could be observed for beam currents ≤10 pA.

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