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    SCIENCE & METROLOGY SOLUTIONS

    www.cameca.com

    A Brief History of Atom Probe

    Thomas F. Kelly and John A. Panitz Pre-meeting Congress, M&M 2016

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    Ancestry of the Modern Atom Probe

    July 24, 2016A Brief History of Atom Probe 2

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    Erwin Wilhelm Müller

    July 24, 2016A Brief History of Atom Probe 3

    Photograph of Professor Erwin W. Müller (1911-1977): Father of High Field Nanoscience

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    Field Electron Emission Microscopy

    July 24, 2016A Brief History of Atom Probe 4

    E. W. Müller, Z. Phys. 120 (1943) 270

    Fl uo

    re sc

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    cr ee

    n

    - electron

    ̶ E +

    1935

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    Field Electron Emission Microscopy

    ■ Field electron emission microscopy (FEEM) was developed as a point projection microscope

    ■ FEEM patterns showed clear crystallographic information ■ Ba atoms and phthalocyanine molecules were observed on

    W needles with FEEM ■ Image resolution improved through the late 1940’s ■ Müller sought to resolve atoms with FEEM ■ Eventually it was concluded that FEEM would resolve no

    better than ~2 nm ■ Field desorption (and evaporation?) was shown in 1941

    July 24, 2016A Brief History of Atom Probe 5

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    Field Ion Microscopy

    July 24, 2016A Brief History of Atom Probe 6

    Erwin Müller at Penn State

    • FEEM tips were routinely cleaned by reversing the bias

    • Practitioners of FEEM noticed: • Field ions were emitted during

    reverse bias • Müller sought, and found, a way

    to increase the signal of field ions: H, He gas

    • Intensity of field ion signal varied with gas pressure

    • In early 1950s, this was pursued for imaging the tip surface

    • Atoms at ledges were seen

    • Early field ion images (FIM) had higher resolution than FEEM

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    Field Ion Microscopy

    July 24, 2016A Brief History of Atom Probe 7

    First images ever of atoms (on ledges of tip surface): Summer 1951, Müller First atomically resolved lattice on surface: October 11, 1955, Bahadur and Müller

    Fl uo

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    cr ee

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    + ion

    + E ̶

    1951

    Gas supply

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    Imaging Crystal Defects in FIM ■ Surface atoms and

    defects are visible in FIM ■ E.g. Self-interstitial

    atoms produce large image in FIM

    July 24, 2016A Brief History of Atom Probe 8

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    Vacancies imaged in FIM! ■ Vacancies observed ■ Knock-on damage

    cascades were mapped by cinematography of FIM

    July 24, 2016A Brief History of Atom Probe 9

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    1960s FIM

    July 24, 2016A Brief History of Atom Probe 10

  • FIM & Field Evaporation

    Movie

    40 K Tungsten Needle Helium Gas Phosphor Screen

    Best Imaging Voltage

    Slight Laser Heating

    Field Evaporation

    Adsorbed gas atoms ⇒ field ion image Specimen atoms ⇒ atom probe Movie Courtesy Baptiste Gault

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    3D FIM Comes to Life!

    July 24, 2016A Brief History of Atom Probe 12

    • 100% of atoms positioned

    • High precision on atom locations

    • Crystal structure and defects readily visible

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    Compositional Contrast in FIM

    July 24, 2016A Brief History of Atom Probe 13

    In this field ion micrograph of boron-doped nickel aluminide (Ni3Al), the bright dots are individual boron atoms that have segregated to a grain boundary (arrowed).

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    The Atom Probe

    July 24, 2016A Brief History of Atom Probe 14

    Mueller, Panitz, McLane, Rev. Sci. Instrum. (1968) vol. 39, p. 83.

    John A. Panitz

    Müller sought a way to identify atoms in the ■ specimen Barofsky was asked to built a magnetic sector ■ mass spectrometer

    He later suggested that they should try ToF■

    Panitz was assigned the job■ How to detect single atoms? Never been done■

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    Much of the following from Panitz 2014

    54th International Field Emission Symposium Atom Probe Tomography and Microscopy Stuttgart, Germany 2014

    July 24, 2016A Brief History of Atom Probe 15

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    The Müller Group ~ 1968

    July 24, 2016A Brief History of Atom Probe 16

    Names in bold are part of the atom probe effort

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    Original Atom-Probe Field Ion Microscope

    July 24, 2016A Brief History of Atom Probe 17

    1967

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    Single Atom Detection Was Invented

    July 24, 2016A Brief History of Atom Probe 18

    Photograph of oscilloscope screen

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    Data File: Oscilloscope Trace

    July 24, 2016A Brief History of Atom Probe 19

    Atom Hit

    Polaroid picture of oscilloscope screen

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    First Publication on Atom Probe

    July 24, 2016A Brief History of Atom Probe 20

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    The Second Atom Probe - 1968

    July 24, 2016A Brief History of Atom Probe 21

  • Muller and Panitz

    July 24, 2016A Brief History of Atom Probe 22

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    ■ Tip tilting not needed ■ Flight distance 11.38 cm to center ■ Observe field ion image or field desorption image ■ Mass analyze all atoms within a field of view

    July 24, 2016A Brief History of Atom Probe 23

    Imaging Atom Probe: the Progenitor of Atom Probe Tomography

    MRP of ■ 14 was achieved!

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    Imaging Atom Probe 2.0: Curved MCPs

    July 24, 2016A Brief History of Atom Probe 24

    Tip at center of MCP ■ curvature All parts of detector ■ have same flight length High mass resolution ■ over entire field of view Tomographic imaging ■ possible

    Detector technology for recording each ion impact position was not yet inven

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