science & metrology solutions...science & metrology solutions science & metrology...

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S

SCIENCE & METROLOGY SOLUTIONS

www.cameca.com

A Brief History of Atom Probe

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

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Ancestry of the Modern Atom Probe

July 24, 2016A Brief History of Atom Probe 2

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Erwin Wilhelm Müller


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

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Field Electron Emission Microscopy


E. W. Müller, Z. Phys. 120 (1943) 270

Fluo

resc

ent S

cree

n

- electron

E +

1935

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


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


SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Field Ion Microscopy


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

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Field Ion Microscopy


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

Fluo

resc

ent S

cree

n

+ ion

+ E

1951

Gas supply

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Imaging Crystal Defects in FIM■ Surface atoms and

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

atoms produce large image in FIM


SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


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

cascades were mapped by cinematography of FIM


SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


1960s FIM


FIM & Field Evaporation

Movie

40 K Tungsten NeedleHelium GasPhosphor Screen

Best Imaging Voltage

Slight Laser Heating

Field Evaporation

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

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


3D FIM Comes to Life!


• 100% of atoms positioned

• High precision on atom locations

• Crystal structure and defects readily visible

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Compositional Contrast in FIM


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).

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


The Atom Probe


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

John A. Panitz

Müller sought a way to identify atoms in the ■specimenBarofsky 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■

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Much of the following from Panitz 2014

54th International Field Emission SymposiumAtom Probe Tomography and MicroscopyStuttgart, Germany 2014


SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


The Müller Group ~ 1968


Names in bold are part of the atom probe effort

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Original Atom-Probe Field Ion Microscope


1967

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Single Atom Detection Was Invented


Photograph of oscilloscope screen

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Data File: Oscilloscope Trace


Atom Hit

Polaroid picture of oscilloscope screen

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


First Publication on Atom Probe


SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


The Second Atom Probe - 1968


Muller and Panitz


SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


■ 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


Imaging Atom Probe: the Progenitor of Atom Probe Tomography

MRP of ■ 14 was achieved!

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Imaging Atom Probe 2.0: Curved MCPs


Tip at center of MCP ■curvatureAll parts of detector ■have same flight lengthHigh mass resolution ■over entire field of viewTomographic imaging ■possible

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

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Field Desorption Images of Single Specie


■ Time gate on MCPs

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Pulsed Laser Atom Probe■ A laser was adapted to

the Imaging atom probe at Sandia Laboratories

■ First time non-metals were atom probed

■ Laser pulsing has become the dominant pulsing mode in APT


SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


PLAP data - Molybdenum

■ Flight path was not optimized

■ No correction for flight distance across detector

■ Demonstrated laser pulsing for metals, insulators

■ Correct isotopic abundances


SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


New Groups Develop – University of Oxford


Professor George Smith

Early atom probe at Oxford

Congratulations to GeorgeMSA Distinguished Scientist Award

First atom probe expert

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


The Vacuum Generators APFIM 100

Developed in conjunction with ■Smith et al. at OxfordFirst commercial atom probe■


1975

http://arc.nucapt.northwestern.edu/images/7/72/Vg100.jpg


SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


The Position-Sensitive Atom Probe

■ Adapted a Wedge-and-Strip detector from astronomy to a VG APFIM 100

■ 1988 Fall MRS presented by George Smith

■ First operational 3DAP


1988





SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


The Position-Sensitive Atom Probe (PoSAP)


SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


The Commercial PoSAP


Manufactured by Kindbrisk (Oxford NanoScience)

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Tomographic Atom Probe


D. Blavette, A. Bostel, J. M. Sarrau, B. Deconihout, and A. Menand: An atom-probe for three dimensional tomography. Nature 363:432–435 (1993).

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


TAP Detector


SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Electron-Beam-Pulsed Atom Probe

Thermal pulsing can be route to high repetition rates ■Need to heat very small volumes for rapid cooling■

Needed for high mass resolving power■

Electron beams can be focused to very small diameter■■ ~100 nm heated volumeSpecimen in atom probe is positive electrode■

Thermal pulsing with electron beam■July 24, 2016A Brief History of Atom Probe 35

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Atom Probe and (S)TEM

Electron beam pulsing and ■atom probe naturally suggest imaging during analysisThere are many ■advantages of having a TEM image of the specimen


Kelly, 1990 IFES meeting, Albuquerque

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Electron-Beam-Pulsed Atom Probe


Larson, Camus and Kelly, Applied Surface Science 67 (1993) 473.

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


The Atom Probe Microscope


SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


There were Challenges to overcome

With Cryopump on■


Vibration• -free coolingField emission from electrode•

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Scanning Atom Probe

Nishikawa, O., Kimoto, M., Applied Surface Science (1994) vol. 76, pp. 424-430.


SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Origins of Local Electrode Atom ProbeBasic conundrum: ■■ 3DAP is superlative analytical tool but■ 3DAP of 1990 is too slow to be practical (1 atom/s)

The field of view was limited to about ■ 20 nm

Scanning Atom Probe used an aperture electrode close to ■specimenField emitter arrays had demonstrated field enhancement ■factors of 10 relative to remote electrodeLower voltage pulsers can achieve much higher repetition ■ratesTwo key results: ■

Use local electrode to obtain high data rates■Relative reduction in energy spread can be compensated by post ■acceleration => high mass resolution over full field of view


SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Local Electrode


Enables:Analysis of microtips and needlesHigh data collection ratesLarge field of view

Local Electrode

Specimen

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S

SCIENCE & METROLOGY SOLUTIONSSharp Flat Top

Microtips™ in the LEAP®

Local Electrode


Microtip Array

1 mm

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Solid Model of Alpha Prototype


Cryopump

Specimen and local electrode

Detector

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Alpha Prototype to LEAP 3000 – Circa 2001


The LEAP 4000 X

Near Full page on gradient background

The LEAP 5000July 24, 2016A Brief History of Atom Probe 47

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


There Are Many LEAP Models Anticipated


Quantum LEAPLEAP FrogLEAP of FaithLambeau LEAP

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


EIKOS IS Atom Probe Tomography

July 24, 2016

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Focused Ion Beam: General Liftout Method

50

a) b)

c) d)

e) f)

1

23

All scale bars are 5 μmA Brief History of Atom Probe July 24, 2016

All scale bars are 1 μm (except f which is 200nm)

c) d)

e) f)

a) b)

David Larson led the way on FIB preparation of specimens

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


The ATOM Project

O. Krivanek et al., Ultramicros. 108 (2008) 179.

Position–Sensitive Detector

Side-entry liquid He sample stage

STEM+LEAP


Build objective lens assembly with atom probe inside

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S



Project Tomo

Build objective lens ■assembly with atom probe inside

TEM+LEAP

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Specimen Holder for Project TOMO

Electron Beam

Evaporated Ions


SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S

SCIENCE & METROLOGY SOLUTIONSASAT

EELS

Properties

Diffraction

Atomic Structure

Computed Image

Atom Probe

STEM

Structure-Properties Microscopy

Electronic StructureElectronic Structure

AST

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


In the History of Microscopy, We are at an Inflection Point


Log

(Len

gth

Scal

e of

Kno

wle

dge)

Today Time

Telescopes

Microscopes

Macro

Micro

Mega

Human eye

1600Prehistory

Inflection point

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


The History of Microscopy

■ The history of microscopy is the pursuit of learning “more and more about less and less”

■ We have reached the atomic scale■ This marks an inflection point

■ The future of microscopy will be the pursuit of learning “more and more about more and more”


SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


Ancestry of the Modern Atom Probe


SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


We’ve made progress: From Müller


1951- FIM 1967 - APFIM1935 - FEM

SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


To Commercial Atom Probes

1990- PoSAP 2016 – LEAP 5000, EIKOS1975 – VG APFIM 100July 24, 2016A Brief History of Atom Probe 59



SCIE

NC

E &

MET

RO

LOG

Y SO

LUTI

ON

S


D

January 26, 2016Atomic-Scale Tomography, an Achievable Vision 60

science & metrology solutions...science & metrology solutions science & metrology...

Documents