SCIENCE &METROLOGY SOLUTIONS A Brief History A of Probe www.cameca.com www.cameca.com Thomas F. Kelly and John A. Panitz and JohnA. F. Kelly Thomas Pre - meeting Congress, M&M 2016 M&M Congress, meeting

SCIENCE & METROLOGY SOLUTIONS A Brief History of Atom Probe Atom of History Brief A SCIENCE &METROLOGY SOLUTIONS Ancestry of the Modern Atom Probe Atom Modern of the Ancestry July 24, 2016 24, July 2

SCIENCE & METROLOGY SOLUTIONS A Brief History of Atom Probe Atom of History Brief A Photograph of Professor Erwin W. Müller ( Müller W. Erwin Professor Photograph of SCIENCE &METROLOGY SOLUTIONS 1911 -1977 ErwinWilhelm Müller July July ): Father of High Field Nanoscience 24, 2016 3

SCIENCE & METROLOGY SOLUTIONS A Brief History of Atom Probe Atom of History Brief A 1935 - electron ̶ E + SCIENCE &METROLOGY SOLUTIONS Field Electron Emission Microscopy Emission Electron Field

Fluorescent Screen July July 24, 2016 E. W. Müller, W. E. Z. Phys. 120 120 (1943 ) 270 4

SCIENCE & METROLOGY SOLUTIONS A Brief History of Atom Probe Atom of History Brief A ■ ■ ■ ■ ■ ■ ■ Field desorption (and evaporation?) wasshown in1941 better nm ~2 than Eventually itwas concludedthatFEEM would resolveno Müller soughttoresolveatoms withFEEM Image resolutionimproved throughthelate1940’s FEEM needles with W Ba atomsandphthalocyanine moleculeswereobservedon FEEM patternsshowedclear crystallographicinformation a projectionpointas microscope Field electronemissionmicroscopy(FEEM)wasdeveloped SCIENCE &METROLOGY SOLUTIONS Field Electron Emission Microscopy Emission Electron Field July 24, 2016 24, July 5

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Fluorescent Screen July 24, 2016 24, July Field Ion Microscopy Ion Field 7

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SCIENCE & METROLOGY SOLUTIONS ■ ■ A Brief History of Atom Probe Atom of History Brief A FIM cinematography of mapped by were cascades Knock Vacancies observed - on damage SCIENCE & METROLOGY SCIENCE &METROLOGY SOLUTIONS Vacanciesimagedin FIM! July July 24, 2016 9

SCIENCE & METROLOGY SOLUTIONS A Brief History of Atom Probe Atom of History Brief A SCIENCE &METROLOGY SOLUTIONS July July 24, 2016 s FIM 1960s 10

SCIENCE & METROLOGY SOLUTIONS 40 K Tungsten Best Imaging Needle Voltage Gas Slight Laser Phosphor FIM & Field Heating Screen Field Evaporation Evaporation Movie

Adsorbed gas atoms ⇒ field ion image Specimen atoms ⇒ atom probe Movie Courtesy Baptiste Gault A Brief History of Atom Probe Atom of History Brief A SCIENCE & METROLOGY SCIENCE &METROLOGY SOLUTIONS 3D FIM Comes to Life! to Comes FIM 3D July July 24, 2016 • • • visible readily defects and Crystal structure locations atom on precision High positioned atoms of 100% 12

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SCIENCE & METROLOGY SOLUTIONS ■ ■ ■ ■ A Brief History of Atom Probe Atom of History Brief A How single detect to done atoms? been How Never Panitz assigned was the job spectrometermass magnetic sector a built toBarofsky asked was specimen Müller sought toa way identify atoms the in ■ He later suggested that they should try ToF should trythey that suggested He later SCIENCE & METROLOGY SCIENCE &METROLOGY SOLUTIONS July July Instrum. (1968) vol. 39, p. 83. 39,p. vol. (1968) Instrum. Mueller,Rev. McLane, Panitz, Sci. 24, 2016 The Atom Probe Atom The John A. Panitz A. John 14

SCIENCE & METROLOGY SOLUTIONS A Brief History of Atom Probe Atom of History Brief A Much of the following from Panitz 2014 Panitz from following the of Much SCIENCE & METROLOGY SCIENCE &METROLOGY SOLUTIONS Stuttgart, Germany 2014 Germany Stuttgart, and Microscopy Tomography Probe Atom Symposium Emission Field 54th International July 24, 2016 24, July 15

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SCIENCE & METROLOGY SOLUTIONS A Brief History of Atom Probe Atom of History Brief A SCIENCE &METROLOGY SOLUTIONS The Second Atom Probe - Probe Atom Second The July July 24, 2016 1968 21

SCIENCE & METROLOGY SOLUTIONS Muller and Panitz

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SCIENCE & METROLOGY SOLUTIONS ■ ■ ■ A Brief History of Atom Probe Atom of History Brief A pulsing mode in APTmode pulsing dominant the become Laser pulsinghas probed atom were First timenon Laboratories Sandia at probe atom Imaging the A laserwasadaptedto SCIENCE &METROLOGY SOLUTIONS - metals metals Pulsed Laser Atom Probe Atom Laser Pulsed July July 24, 2016 26

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SCIENCE & METROLOGY SOLUTIONS ■ ■ ■ 1988 A Brief History of Atom Probe Atom of History Brief A First operational3DAP SmithGeorge 1988 FallMRSpresented by Adapted aWedge APFIM 100 APFIM VG detectora astronomy from to SCIENCE & METROLOGY SCIENCE &METROLOGY SOLUTIONS - and- The Position The Strip Strip - Sensitive Atom Probe Atom Sensitive July July 24, 2016 30

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SCIENCE & METROLOGY SOLUTIONS A Brief History of Atom Probe Atom of History Brief A ■ ■ ■ ■ ■ Thermal pulsingwith electron beam Specimen in atomprobeispositive electrode Electron beamscanbe focusedtoverysmalldiameter Need toheatverysmall volumesforrapidcooling Thermal pulsingcanberoutetohighrepetition rates ■ ■ ~ Needed forhighmassresolving power 100 nm heated SCIENCE &METROLOGY SOLUTIONS Electron volume - Beam July July - 24, Pulsed Atom Probe Atom Pulsed 2016 35

SCIENCE & METROLOGY SOLUTIONS ■ ■ A Brief History of Atom Probe Atom of History Brief A specimen specimen the of image TEM a having of advantages There aremany analysis during imaging suggest naturally probe atom Electron beampulsingand SCIENCE & METROLOGY SCIENCE &METROLOGY SOLUTIONS Kelly, 1990 IFES meeting, Albuquerque meeting, IFES Kelly,1990 Atom Probe and (S)TEM and Probe Atom July July 24, 2016 36

SCIENCE & METROLOGY SOLUTIONS A Brief History of Atom Probe Atom of History Brief A Larson, Camus and Kelly, Camus Larson, 67 473. (1993) Science Surface Applied SCIENCE &METROLOGY SOLUTIONS Electron - Beam July July 24, - Pulsed Atom Probe Atom Pulsed 2016 37

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SCIENCE & METROLOGY SOLUTIONS A Brief History of Atom Probe Atom of History Brief A ■ ■ ■ ■ ■ rates of factors specimen Two keyresults: Lower voltagepulserscan achievemuchhigherrepetition Field emitterarrayshaddemonstrated fieldenhancement Scanning AtomProbeused anapertureelectrodecloseto Basic conundrum: ■ ■ ■ ■ ■ acceleration => high mass resolution over full field of view of field full over resolution mass high => acceleration Relative reduction inenergy spreadcanbe compensatedby post Use local electrodetoobtain highdatarates The fieldofviewwaslimitedtoabout of 3DAP tool analytical superlative is 3DAP Origins of Local Electrode Atom Probe Atom Electrode Local of Origins 10 SCIENCE &METROLOGY SOLUTIONS 1990 relative to remoteto relativeelectrode is too slow to be practical ( be practical slow to is too but 20 nm July 24, 2016 24, July 1 atom/s) 41

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SCIENCE & METROLOGY SOLUTIONS The LEAP 4000 X Near Full page on gradient background

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SCIENCE & METROLOGY SOLUTIONS A Brief History of Atom Probe Atom of History Brief A e) c) a) All scale bars are 5 are bars scale All David Larson led the way on FIB preparation of specimens of preparation on FIB waythe led Larson David μm : General Liftout Method Liftout General Ion Beam: Focused SCIENCE &METROLOGY SOLUTIONS f) d) b) 3 1 2 All scale bars are 1 are bars scale All a) e) c) July 24, 2016 24, July μm (except f which is 200nm) (exceptis which f ) d f) b) 50

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SCIENCE & METROLOGY SOLUTIONS