Correlative and simulation supported atomprobe ...

Correlative and simulation supported atomprobe tomography: advances and limitations D. Raabe, B. Gault, A. Breen, Y. Chang, M. Yao, D. Ponge, M. Herbig, C. Liebscher, S. Katnagallu, G. Dehm, C. Scheu, A. Stoffers, A. Nematollahi, J. Neugebauer

Düsseldorf, Germany

Physical Review Letters 112 (2014) pp. 126103

Science 349 (2015) 1080-1083

Dierk Raabe, Workshop on Possibilities and Limitations of Quantitative Materials Modeling and Characterization 2017,

Atom Probe Tomography (APT): directions for structure resolution Use evaporation anisotropy

See e.g. Gault, Breen, Cairney, Ringer, Miller

FIM++

See e.g. Dagan, Moody, Danoix

See e.g. Herbig, Seidman, Gorman

See e.g. Schmitz, Dunin-Borkowski, Larson

Combine APT with TEM / SEM / STEM

Image the tip and simulate field 1

Example Use evaporation anisotropy

APT crystallography

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Atom Probe Tomography : APT crystallography

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Atom Probe Tomography : APT crystallography

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Atom Probe Tomography : APT crystallography

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Atom Probe Tomography : APT crystallography

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Atom Probe Tomography : APT crystallography

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Combine APT with TEM / STEM: Probe tip before evaporation

APT & TEM / STEM / SEM (& DFT / MD)

S. Jiang et al. Nature (2017) M. Kuzmina et al Science (2015) Y. Li et al. phys rev let. (2014) M. Herbig et al., phys rev let. (2014) M. Koyama et al. Science (2017) M. Herbig et al. Ultramicroscopy (2015) 8

Experimental setup for correlative TEM–APT probing

Ga3+

Principle

Ions e-

sample modified singletilt TEM retainer

52°

FIB: Tip is cut parallel to holder axis.

TEM: During tilt around holder axis tip always stays in focus range, whole sample in focus (!).

APT: Defined sample orientation in all instruments makes it possible to merge information.

S. Jiang et al. Nature (2017) M. Kuzmina et al Science (2015) Y. Li et al. phys rev let. (2014) phys rev let. (2014) M. Koyama et al. Science (2017) M. Herbig et al. Ultramicroscopy (2015)

M. Herbig et al.,

Guo et al phys rev let. 2014, Duarte et al. Science 341, 372 (2013)

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Experimental setup for correlative TEM–APT probing

Ga3+

Principle

Ions e-

sample modified singletilt TEM retainer

52°

FIB: Tip is cut parallel to holder axis.

TEM: During tilt around holder axis tip always stays in focus range, whole sample in focus (!).

APT: Defined sample orientation in all instruments makes it possible to merge information.

S. Jiang et al. Nature (2017) M. Kuzmina et al Science (2015) Y. Li et al. phys rev let. (2014) phys rev let. (2014) M. Koyama et al. Science (2017) M. Herbig et al. Ultramicroscopy (2015)

M. Herbig et al.,

Guo et al phys rev let. 2014, Duarte et al. Science 341, 372 (2013)

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Fe-30%Mn-8%Al-1.2%C – 10-18% weight reduction

Nanostructured Fe-based superalloy

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HRSTEM on Fe-Mn-Al-C /κ steel [001]/κ

HAADF-STEM

[010]/κ [100]/κ

APT C  9.0 at.% 20nm ABF-STEM

Yao, MJ; et al. Acta Materialia,106,,229-238,2016;

Al

Mn/Fe C

Nature 544, 460–464 (27 April 2017)

Collaboration with Lipinska-Chwalek, Liebscher, Mayer, Dehm, Scheu (TEM), Dey, Hickel, Neugebauer (DFT), Yao, Herbig, Gault (ATP)

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HRSTEM on Fe-Mn-Al-C /κ steel [001]/κ

disordered- HAADF-STEM

ordered-k

[010]/κ

(002) planes

[100]/κ

APT C  9.0 at.% 20nm ABF-STEM

Al

Mn/Fe C

Collaboration with Lipinska-Chwalek, Liebscher, Mayer, Dehm, Scheu (TEM), Dey, Hickel, Neugebauer (DFT), Yao, Herbig, Gault (ATP)

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Regular nanoparticle arrays by discontinuous precipitation

J.-B. Seol, S.-H. Na, B. Gault, J.-E. Kim, J.-C. Han, C.-G. Park & D. Raabe, Scientific Reports 7, Article number: 42547 (2017)

Fe with 0.2 C and a total of 0.3 at. % Ti, Mo, and V 14

Regular nanoparticle arrays by discontinuous precipitation Fe with 0.2 C and a total of 0.3 at. % Ti, Mo, and V

J.-B. Seol, S.-H. Na, B. Gault, J.-E. Kim, J.-C. Han, C.-G. Park & D. Raabe, Scientific Reports 7, Article number: 42547 (2017) 15

Regular nanoparticle arrays by discontinuous precipitation

J.-B. Seol et al., Scientific Reports 7, Article number: 42547 (2017)

5nm 16

Σ3 facets in HR-STEM

5 nm 17

APT reconstruction LEAP 5000

Si C

nm ongoing work

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10^24 particle number density in maraging; strength by APB

NiAl B2 / cubic martensite matrix low lattice misfit (0.03 - 0.04 %)

Nature 544, 460–464 (27 April 2017)

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10^24 particle number density in maraging; strength by APB

Nature 544, 460– 464 (27 April 2017) 20

Atom Probe Tomography (APT): directions for structure resolution FIM++

See e.g. Dagan, Moody, Danoix

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Seeing atoms in 3D: A more holistic approach

Atom probe

TEM/STEM/ EELS

FIM Simulation

G. Larson

APT analysis directions

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Use FIM atom coordinates for MD relaxation Collaboration with Oxford FIM / APT group: P. Baggot, M. Moody, D. Haley, A. London, M. Dagan

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3D FIM on tungsten

from Michal Dagan, Baptiste Gault, George Smith, Paul Bagot & Michael Moody 24

Simulation, rescaling, towards automation Create a sphere out of the perfect lattice

Find the nearest number of atoms for each atom on the layers chosen

Remove the atom from the layer.

Randomly select among the atoms which have same probability of evaporation

Calculate the intensity based on nearest neighbors

Create a priority list for evaporation based on the intensities

de Castilho, Caio MC, and David R. Kingham. "Resolution of the field ion microscope." Journal of Physics D: Applied Physics 20.1 (1987): 116. Chen, Y. C., and D. N. Seidman. "On the atomic resolution of a field ion microscope." Surface Science 26.1 (1971): 61-84. Moore, A. J. W., and J. A. Spink. "Field evaporation from tungsten and the bonding of surface atoms." Surface Science 12.3 (1968): 479-496.

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FIM Simulation

Using supervised machine learning to directly identify the coordinates of the atoms from experiments.

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Molecular Relaxation

PyIron

APT, FIM, STEM / TEM, EBSD, TKD, EELS, VASP, kMC, LAMMPS 27

Use FIM atom coordinates for MD relaxation

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Use FIM atom coordinates for MD relaxation

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Relaxation by phase field crystal method

On FIM data-1

Simulations from Sai Tang 30

Possibilities and limitations

Driving force: want to image atoms, not atomic columns APT limits: local magnification, local field calculation, evaporation theory Multi-beam correlative probing: On a good way and giving results on complex multicomponent materials Specimen exchange among instruments: UHV, cryo, machine decoupling, on the way, summer 2017 Coupling with simulations and machine learning: APT+MD; FIM+MD, much to do Chemically sensitive FIM: need to do theory on imaging gas – tip

APT on organics: ill-defined chopping

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