[PPT] - Dsseldorf, Germany Dierk Raabe, Res Metallica Symposium, Department PowerPoint Presentation

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From grains to atoms: ping-pong between experiment and simulation for understanding microstructure mechanisms Düsseldorf, Germany

P.-P. Choi, M. Kuzmina, J. Deges, M.J. Yao, O. Cojocaru-Miredin, I. Povstugar, C. Liebscher, M. Lipinska-Chwalek, S. Katnagallu,

D. Ponge, M. Herbig, C. Tasan, A. Stoffers, S. Sandlöbes, T. Hickel, J. Neugebauer, J. Mayer, C. Scheu, G. Eggeler, D. Raabe

Dierk Raabe, Res Metallica Symposium, Department of Materials Engineering, KU Leuven, May11th 2016

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Zeitalter tragen die Namen von Materialien

Experiment Models

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Complex materials: atomic scale view

Atom Probe: Imaging atoms Solar Cells High temperature materials Strong light- weight steels

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Complex materials: atomic scale view

Atom Probe: Imaging atoms Solar Cells High temperature materials Strong light- weight steels

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Atom Probe Tomography (APT)

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Ion sequence Position sensitive detector X1, Y1, ToF1 VDC Vp +



Time of flight

X2, Y2, ToF2 X3, Y3, ToF3 X4, Y4, ToF4 R  50 nm T 20–100 K X5, Y5, ToF5 …….. Time of flight  chemical identity Position of hit  X-Y coordinates Evaporation sequence  Z coordinate

r

The specimen is the lens 3D point cloud data

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Atom Probe Tomography (APT): directions for structure resolution

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can you get structure? It‘s a point cloud

approach 1: use evaporation anisotropy approach 2: combine APT withTEM / SEM / STEM

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

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Atom Probe Tomography (APT): evaporation anisotropy

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Atom Probe Tomography (APT): evaporation anisotropy

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Atom Probe Tomography (APT): evaporation anisotropy

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Atom Probe Tomography (APT): evaporation anisotropy

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(002) planes

Atom Probe Tomography (APT): evaporation anisotropy

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(111) planes

Atom Probe Tomography (APT): evaporation anisotropy

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(001) (012) (113) (112) (111) (011)

Field desorption image; example Fe3Al

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Herbig et al., phys rev let. 2014, Guo et al phys rev let. 2014

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[111] [-1-12] 0.33 nm 0.25 nm

Lattice plane reconstruction: APT crystallography

Fe3Al (only Al displayed)

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Atom probe crystallography: Chemistry and structure in 3D

Kuzmina et al. Science 349 (2015)

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2 nm

[111] [-1-12] 0.33 nm 0.25 nm

Lattice plane reconstruction: APT crystallography

Fe3Al (only Al displayed)

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Atom probe crystallography: Chemistry and structure in 3D

Kuzmina et al. Science 349 (2015)

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Experimental setup for correlative TEM–APT probing

Ga3+ 52° modified single- tilt TEM retainer sample

FIB: Tip is cut parallel to holder axis.

e-

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

Ions

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

Principle

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

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Li et al. phys rev let. 2014 Herbig et al., phys rev let. 2014

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Experimental setup for correlative TEM–APT probing

Ga3+ 52° modified single- tilt TEM retainer sample

FIB: Tip is cut parallel to holder axis.

e-

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

Ions

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

Principle

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

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Li et al. phys rev let. 2014 Herbig et al., phys rev let. 2014

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Correlative TEM-APT probe for 5D GB segregation analysis

BF-STEM micrograph of cold-drawn Fe-C (010) (00-1) (-100) e- beam Nano beam diffraction Scanning nano beam diffraction

100 nm

(ASTAR) Acta Mat 61 (2013) 3172, Herbig et al. phys rev let. 2014

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Carbon atoms

50 nm

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Correlative TEM-APT probe for 5D GB segregation analysis

5 crystal. parameters N chemical species

Herbig phys rev let., (2014); Kuzmina et al. Science 349 (2015) Li. phys rev. let (2014)

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Mn
Fe

Mn 11 at% isosurface Segregation at dislocation lines (ε=50% & 450°C/6h): Fe-9wt% Mn

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Kuzmina et al. Science 349 (2015) Li. phys rev. let (2014)

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Correlated microscopy LAGB (50%CR+450°C/6h) Fe-9%Mn

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Mn
Fe

Mn 11 at% isosurface

Kuzmina et al. Science 349 (2015) Li. phys rev. let (2014)

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Mn
Fe

Mn 11 at% isosurface Segregation at dislocation lines (ε=50% & 450°C/6h): Fe-9wt% Mn

21 Fe-Mn: segregation & reversion: trends for middle Mn steels

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Complex materials: atomic scale view

Atom Probe: Imaging atoms Solar Cells High temperature materials Strong light- weight steels

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Courtesy: Siemens

New materials for key energy technologies: Turbine materials

s

Source: Siemens

75% energy conversion via turbines <44% efficiency

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Courtesy: Siemens

New materials for key energy technologies: Turbine materials

Source: Siemens

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Example: 4th generation superalloys for turbine blades (SFB / TR 103)

20 nm

Al Co Re

iso. 56 at.% Ni

source GE

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Complex materials: atomic scale view

Atom Probe: Imaging atoms Solar Cells High temperature materials Strong light- weight steels

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Courtesy: Maybach, Siemens, ThyssenKrupp, VW, IG Metall Eng.

New materials for key energy technologies: Mobility

courtesy: R. Boesenkool, SMEA conference, Sheffield SUV sales, Germany

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Nanostructured Fe-based superalloy

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

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[100]/κ [010]/κ [001]/κ

HAADF-STEM

20nm

Characterizing Fe-Mn-Al-C /κ steel by correlative HRSTEM / APT

Al Mn/Fe C

DFT supercell of κ-carbide courtesy: P. Dey, T. Hickel

APT C  9.0 at.%

HRSTEM 2D structural analysis with atomic resolution

Coherency
Lattice parameter

gradient

Site occupancy
Interface structure

APT 3D chemical analysis with near atomic resolution

3D morphology
Elemental partitioning
Chemical gradients

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Nanostructured Fe-based superalloy

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

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SiO2 pattern

1µm

Strain map Experiments Spectral solver Digital model Strain map & stress map Simulations

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ICME applied to dual phase steel

Integrated Computational Materials Engineering: DP steel

Deformation Imaging & DIC Sectioning Indents

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Martensite: Hierarchical microstructure analysis

Integrated Computational Materials Engineering: DP steel

Morsdorf et al. Acta Mater 95 (2015) 366

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C

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33 Integrated Computational Materials Engineering: DP steel

In-situ tensile testing: role of coarse lath in martensite fracture

SEM – in-situ tensile

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Damage statistics in dual phase steels

34 Integrated Computational Materials Engineering: DP steel

DM: martensite damage; DM-F: martensite-ferrite decohesion

Tasan et al. Annu. Rev. Mater. Res.45 (2015) 391

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35 DAMASK.mpie.de

Düsseldorf Advanced MAterial Simulation Kit, DAMASK

> 15 years of development > 50 man years of expertise > 50.000 lines of code Pre- and post-processing Blends with MSC.Marc and Abaqus Standalone (FFT) spectral solver

Freeware, GPL 3

Crystal plasticity & phase field: Mechanics, damage, phase transformation, diffusion http://DAMASK.mpie.de

Many user groups

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Atom Probe: Imaging atoms Solar Cells High temperature materials Strong light- weight steels

Complex materials: atomic scale view

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Σ3 with steps and high EBIC contrast

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A. Stoffers, PRL, in press

Si C O 20 nm

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Σ3 facets in HR-STEM

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5 nm 2 nm

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APT reconstruction LEAP 5000

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Stoffers et al, 2015 PRL

Si C

nm

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Example Turbines Example LED Example Soft magnetic materials Example Thin film solar cells Example Hydrogen based energy Example Catalysis

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Message & Conclusions

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The Düsseldorf Max-Planck Team

www.mpie.de