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Review of Scientific Instruments / Volume 78 / Issue 3 / INVITED REVIEW ARTICLE
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Rev. Sci. Instrum. 78, 031101 (2007); http://dx.doi.org/10.1063/1.2709758 (20 pages)

Atom probe tomography

Thomas F. Kelly1 and Michael K. Miller2

1Imago Scientific Instruments Corporation, 5500 Nobel Drive, Madison, Wisconsin 53711
2Oak Ridge National Laboratory, P.O. Box 2008, Building 4500S, Mississippi 6136, Oak Ridge, Tennessee 37831-6136

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(Received 1 August 2005; accepted 14 January 2007; published online 30 March 2007)

The technique of atom probe tomography (APT) is reviewed with an emphasis on illustrating what is possible with the technique both now and in the future. APT delivers the highest spatial resolution (sub-0.3-nm) three-dimensional compositional information of any microscopy technique. Recently, APT has changed dramatically with new hardware configurations that greatly simplify the technique and improve the rate of data acquisition. In addition, new methods have been developed to fabricate suitable specimens from new classes of materials. Applications of APT have expanded from structural metals and alloys to thin multilayer films on planar substrates, dielectric films, semiconducting structures and devices, and ceramic materials. This trend toward a broader range of materials and applications is likely to continue.

© 2007 American Institute of Physics

Article Outline

  1. INTRODUCTION
    1. Historical background of the technology
      1. The field emission microscope
      2. The field ion microscope
    2. Atom probe technology
      1. Atom probe field ion microscope
      2. Pulsed-laser atom probe
      3. The three-dimensional atom probe
      4. The scanning atom probe and local electrode atom probe
  2. SPECIMEN PREPARATION
    1. Geometry and other factors
    2. Standard electropolishing methods
      1. Micropolishing
      2. Pulse polishing
    3. New methods
      1. Broad ion beam methods
      2. Focused ion beam methods
  3. APPLICATIONS
    1. Multiphase materials
    2. Segregation
      1. One-dimensional: Segregation to a dislocation
      2. Two-dimensional: Segregation to precipitate interfaces
    3. Multilayer films
      1. Interfaces in CoFe/Cu multilayers
      2. Metal/oxide layered structure
    4. High resistivity materials
      1. Silicon-based structures
      2. Rutile
      3. Magnetite
    5. Organic materials
    6. Advantages of APT as an analytical technique
    7. Limitations of APT as an analytical technique
      1. Specimen preparation
      2. High mechanical stress
      3. 60% detection efficiency
      4. Analyzed volume ≈ 106 nm3
    8. Where will APT have its impact in coming years?

EDITORIALLY RELATED

  1. Perspective: From field-ion microscopy of single atoms to atom-probe tomography: A journey: “Atom-probe tomography” [Rev. Sci. Instrum. 78, 031101 (2007)]
    David N. Seidman
    Rev. Sci. Instrum. 78, 030901 (2007)RSINAK000078000003030901000001

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KEYWORDS and PACS

Keywords

atom probe field ion microscopy, optical tomography

PACS

  • 07.78.+s

    Electron, positron, and ion microscopes; electron diffractometers

  • 42.30.Wb

    Image reconstruction; tomography

ARTICLE DATA

Digital Object Identifier
http://dx.doi.org/10.1063/1.2709758

PUBLICATION DATA

ISSN

0034-6748 (print)  
1089-7623 (online)

Publisher

$abstract.society.value is a Member of CrossRef American Institute of Physics

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Figures (17) Tables (1)

Figures (click on thumbnails to view enlargements)

FIG.1
(a) Schematic diagrams of the original or “classical” atom probe, (b) three-dimensional atom probe with different detectors, (c) local electrode atom probe, and (d) reflectron-compensated 3DAP (LARC shown).

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FIG.2
Evolution of typical sampled volumes by atom probe type.

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FIG.3
(a) Scanning electron microscopy (SEM) image of an electropolished specimen of an aluminum alloy. (b) Microtip specimen of a multilayer Al/SiO2/Si structure fabricated by broad ion beam milling with a diamond mask particle (Ref. 83). Cr was added to the basic structure as a control layer to aid in finding the original layers.

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FIG.4
(a) SEM image of posts cut in silicon by reactive ion etching. The posts are 100 μm tall and 4 μm in diameter. (b) SEM image of posts cut in a silicon wafer by a dicing saw. Components of a microelectronics device are present on the top of the posts.

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FIG.5
SEM image of an array of microtips fabricated in silicon.

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FIG.6
(Color) Copper (green) and phosphorus (red) atom distribution in a neutron-irradiated (fluence = 1.3×1023 n m−2 [E>1 MeV]) Fe-0.1% Cu, 1.6% Mn, 1.6% Ni model pressure-vessel steel. A high number density of ∼ 3-nm-diameter copper-enriched precipitates and a phosphorus-decorated dislocation are evident. The image on the right is a view along the dislocation that is visible in the left image between the arrows. The arrow in the right image points toward the precipitates that are visible on the dislocation. Specimen is courtesy of Professor G. R. Odette, University of California—Santa Barbara.

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FIG.7
(Color) Thin slice of a LEAP® image of Alloy 718 which is parallel to the analysis direction. The right hand side is the same image but with annotations added to illustrate the precipitate morphology. The matrix is the face-centered-cubic γ phase, the green regions are the DO22-ordered γ″ phase, and the red and blue regions are the L12-ordered γ′ phase. Specimen is courtesy Dr. M. G. Burke.

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FIG.8
(Color online) Aluminum isoconcentration surface of a CMSX4 nickel-based superalloy. A zone that is depleted in small γ ′ precipitates is evident in the γ matrix phase adjacent to the primary γ ′ precipitates. Specimen is courtesy of Professor R. Reed, University of British Columbia.

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FIG.9
(Color online) Phosphorus isoconcentration surface in a Pd40Ni40P20 bulk metallic glass showing a fine-scale isotropic interconnected network structure of two amorphous phases after annealing for 80 min at 340 °C. Specimen is courtesy of Dr. R. B. Schwarz, Los Alamos National Laboratory.

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FIG.10
(Color) Atom map and phosphorus contour maps of a selected volume in the vicinity of the dislocation in the pressure vessel steel from the decommissioned Palisades nuclear reactor. Red atoms are phosphorus and the green atoms are copper. Left figures are the views along the core of the dislocation and the right figures are along the dislocation. Some copper-enriched precipitates are evidently close to the core of the dislocation. The box is 20×20×50 nm3.

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FIG.11
(Color) APT evaluation of segregation of Mg to an Al3Sc/Al interface. (a) Image of a precipitate with an isoconcentration surface drawn at 18 at. % Sc. (b) Composition profile derived from a proximity histogram (Ref. 130) which shows the interfacial excesses of Al, Mg, and Sc measured by APT.

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FIG.12
(Color) Image and composition profile from a CoFe/Cu/CoFe/Ni multilayer stack in Ref. 133 with a comparison to a molecular dynamics simulation (Ref. 133) of the same structure. (a) 3DAP image, (b) composition profile obtained along the long axis of the image from bottom to top (which corresponds to the growth direction), (c) molecular dynamics model of the structure in (a), and (d) composition profile derived from (c).

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FIG.13
(Color) Image of a multilayer thin film stack with an aluminum oxide layer. Image obtained by Kuduz et al. (Ref. 138) on a tomographic atom probe.

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FIG.14
(Color) APT image of boron in silicon obtained on a pulsed-laser LEAP®. The image contains over 150×106 atoms. All 10boron atoms (blue dots) are shown and 0.3% of the silicon atoms (red dots) are displayed for clarity. The horizontal and vertical bars are 100 nm long.

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FIG.15
(Color) Image and composition profile through a high-k dielectric layer on silicon with a polysilicon overlayer.

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FIG.16
Mass spectrum from a metamorphic magnetite obtained on a voltage-pulsed atom probe. The spectrum shows many peaks, all of which can be identified.

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FIG.17
Mass spectrum of polypyrrole obtained from an energy-compensated one-dimensional atom probe. Most of the mass peaks can be identified with simple molecular ions.

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Tables

Table I. Measured composition of magnetite LP204-1 (Ref. 99).

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