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Understanding microstructure formation by 3D analysis in the micro, nano and atomic scale Chair of Functional Materials Frank Mcklich Michael Engstler, Jeni Barrireiro, Dominik Britz Concept of the Institute Chair of Functional Materials

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Chair of Functional Materials

Understanding microstructure formation by 3D analysis in the micro, nano and atomic scale

Frank Mücklich Michael Engstler, Jeni Barrireiro, Dominik Britz

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Chair of Functional Materials

Internationality Flavio Soldera

Material Engineering Center Saarland Steinbeis Research Center

Innovation & Transfer

Institute Functional Materials Saarland University

Basic Research

Aluminium Michael Engstler

Concept of the Institute

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 2 Electr.Contacts Kim Trinh Antimicrobial Michael Hans Energetic Mat. Christoph Pauly Surface Design Carsten Gachot Steel Dominik Britz Atom Probe Jeni Barrirero

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Chair of Functional Materials

  • surface stability
  • new contact materials
  • metallic materials Cu, Pt, Ni..
  • energetic Materials (RuAl)
  • CNT based materials
  • architectured surfaces
  • topography, phases, grains
  • Laser Interference Metallurgy
  • micro / nano tribology
  • new functionalities (bio…)

New Materials New Surfaces

Research Focal Points of the Institute

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 3

New insights into the microstructure of materials 3D  Micro – Nano – Atomic Scale

Image analysis – Stereology – Tomography - 3D analysis

  • surface stability
  • new contact materials
  • metallic materials Cu, Pt, Ni..
  • energetic Materials (RuAl)
  • CNT based materials
  • architectured surfaces
  • topography, phases, grains
  • Laser Interference Metallurgy
  • micro / nano tribology
  • new functionalities (bio…)
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Chair of Functional Materials

3D microstructure:  quantitative key to understand the genesis of processing and correlation to properties

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 4

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Chair of Functional Materials

the right property at the right place

 various steels - aluminium - magnesium - CFRP …

magnesium agnesium soft, well malleable soft, well malleable deep eep-drawing steel drawing steel strong, well malleable trong, well malleable mulitphase steel ulitphase steel higher strength steels

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 5

Quelle: Porsche

highest strength steels (TRIP, TWIP) Al-based materials

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Chair of Functional Materials

Al-Si alloys for light weight engines

Hypoeutectic

primary Al-dendrites and Al-Si eutectic

binary phase diagramm

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 6

Al-Si eutectic at 577°C and 12,6% Si Alloys with 5-14% Si are of importance

„modification“

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Chair of Functional Materials

Al-Si – microstructure morphology change  tremendous impact on mechanical properties

same processing (T, t,…) same Al:Si ratio

  • understand mechanism?
  • already optimum?

colour: different cooling rate

Courtesy T.Herfurth, Foundry Institute Düsseldorf IfG

Stiff and tough!!!

Modification

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 7

deformation energy (a.u.) plastic deformation (bending, a.u.) deformation energy (a.u.) plastic deformation (bending, a.u.)

colour: different cooling rate

Courtesy T.Herfurth, Foundry Institute Düsseldorf IfG

stiff but brittle! Stiff and tough!!!

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Chair of Functional Materials

Tomography at the micro / submicro scale (X-ray-CT, Synchrotron)

Zn Zn2Mg (Al Mg (Al2Cu) F < 0.4 Cu) F < 0.4 Al Al3(Sc,Zr Sc,Zr) F > 0.4 ) F > 0.4 → 0.17 vol% 0.17 vol% > 1500/mm > 1500/mm3

  • pores (LA)

pores (LA)

  • Zn

Zn2

2Mg (Al

Mg (Al2

2Cu)

Cu)

  • Al

Al3

3(Sc,Zr)

(Sc,Zr) (HA) (HA) 0.3 vol% 0.3 vol% 16 16-17 vol% 17 vol% Pores Intermetallics

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 8

28.10.2015

0.09 × 0.11 × 0.07 mm3 0,27 × 0,29 × 0,12 mm3 Visualization of dendrites

  • J. Kastner et al,

Materials characterization 62, 99-107 (2011)

0.5 mm

Lab-CT: Resolution: µm - sub-µm Volume: 10

  • 10 µm³

10 18

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Chair of Functional Materials

(100 µm)3 (1 mm)3 (10 mm)3

X-ray Tomography

(Synchrotron)

Microstructure Analysis  Scale Bridging

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 9 1 nm 10 nm 100 nm 1 µm 10 µm 100 µm (100 nm)3 (1 µm)3 (10 µm)3

APT STEM FIB/SEM

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Chair of Functional Materials

Tomography in the nano scale:  FIB/SEM-nanotomography

Serial Sectioning

SEM Imaging FIB, Ga-Ions Sputtering (10nm precision)

 Well established contrasts in SEM available

correlated 2D-images „Pixel“ x-y 3D-Images „Voxel“ x-y-z

3D-Reconstruction

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 10

SEM-View

 Well established contrasts in SEM available

BSE SE EBSD Fe C Mg S EDX

Resolution: 10-30nm Volume: 10 -10 µm³

4 5

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Chair of Functional Materials

Al-Si (7% Si) primary Al eutectic Si

100ppm Sr doping

„Al-Si modification“ = Si eutectic morphology change caused by 100ppm doping  disconnecting Si eutectic

72 x 100 x 38 µm3 37 x 17 x 35 µm3

unmodified modified

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 11

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Consequences for mechanical properties  3D visualization of local mean curvature

unmodified eutectic silicon Sr-modified eutectic silicon

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 12

  • flat thin plate-like structures
  • high curvature at edges

 Sharp notches: cracking!

  • rounded corals
  • spatial curvature distribution

 ductility and elongation

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Chair of Functional Materials

Growth of Si into the AlSi eutectic melt

Undistorted growth of Si

  • Growth along the (111) planes in [211] direction
  • Si-plates, (111) planes parallel to the surface

Twin plane re-entrant edge (TPRE) – mechanism [1]

  • Branching of the Si-plates by twinning

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 13 [1] Kobayashi, K.F. und Hogan, L.M. Journal of Materials Science. 1985, Bd. 20, S. 1961‐1975.

[1]

EBSD

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The re-entrant twin grooves are poisoned by the modifying element  Radius (Sr:Si) = 1.5  max. effect! Multiplication of twins Activation of all twin systems

Doping induced twinning – “poisoning” of growth

Doping Induced Twinning – Theory [Lu et al.]

  • Impurities (like Sr) cause twinning
  • Branching of the Si-structure

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 14

TPRE mechanism is retarded/hindered Multiplication of twins Activation of all twin systems

Sr at twins in Si and at the Al-Si interface ?  TEM and Atom Probe Tomography

Lu, Shu‐Zu und Hellawell Metallurgical Transactions A. 1987, Bd. 18A, S. 1721‐1733.

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TEM: compare eutectic Si (unmodified/modified)

unmodified eutectic silicon

  • planar interface Si-Al
  • planar twin planes
  • Small spherical particles

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 15

Sr-modified eutectic silicon

  • curved interface Si-Al
  • Irregular twin planes
  • Small spherical particles
  • Rod-shaped particles

Jenifer Barrirero, Michael Engstler, Naureen Ghafoor, Niels de Jonge, Magnus Odén, Frank Mücklich; Journal of Alloys and Compounds 611 (2014) 410–421

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Chair of Functional Materials

Al-Si Sample

(Temp. 40 Kelvin)

+

t I t1 t I

(x1|y1|z=„1“) (x2|y2|z=„2“)

HV

_

UHV

Looking for the Decisive Role of 100ppm Sr Doping  Tomography in Atomic Scale

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 16

t t2

(x2|y2|z=„2“)

HV pulse Laser pulse

  • r

Resolution: 0.5 nm Volume: 10 -10 µm³

  • 3
  • 4
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Segregations of Sr AND Al inside of the Si-Eutectic  ratio Al : Sr is constant !

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 17

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Segregations of Sr AND Al inside of the Si-Eutectic  ratio Al : Sr is constant !

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 18 Barrirero et al., Journal of Alloys and Compounds 611 (2014) 410

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Constant atomic ratio Al : Sr  what does that mean?

The Si growth is restricted by the formation of clusters of SrAl2Si2 at the solidification front

 explain the presence of Aluminium in the crystallographic defects?

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 19

SrAl4 SrAl2Si2 (τ1)

577±1º 12.2 at.%

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If that is true – than also modifications with Na atoms  should work alike ?

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 20

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Al:Sr

Modification via phase formation at solidification front?  Significant difference in the ratio - Al:Sr > Al:Na

The Si growth is restricted by the formation of clusters of NaAlSi at the solidification front. (confirmation of analogy for Sr)

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 21

Al:Na

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deviations from the composion ratio of perfect phases?  limitation of contributing Al atoms

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 22

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Sr modification Al:Sr ≈ 2 Na modification Al:Na ≈ 1

Conclusion: cluster formation might be predicted  by phase composition at the ternary eutectic point

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 23

Al2Si2Sr cluster formation at the solidification front AlSiNa cluster formation at the solidification front

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If that is true – than also modification with Eu  should result in a constant ratio of Al:Eu

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 24

Li et al - Acta Materialia 84 (2015) 153 - 163

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If that is true – than also modification with Eu  should result in a constant ratio of Al:Eu

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 25

Silicon Aluminium Europium

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Al Si Eu

Conclusion: for modification with Eu the atomic ratio  Al:Eu = 2:1 and the corresponding phase should be...

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 26

Al2Si2Eu

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Chair of Functional Materials

How to optimize such microstructures?

micro macro nano

FIB-SEM tomography X-ray tomography 3D simulation

  • f mechanical

properties

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 27

nano

FIB-SEM tomography correlative TEM and APT 3D microstructure simulation

  • f larger volumes

propose growth mechanism

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Stochastical microstructural modelling of relevant structural scenarios for Al-Si

Step 3: From graph structure to corals colony: dilation Step 2: Competitive growth model: 'birth-and-death' process Step 1: Single coral model: multivariate time series

  • time series approach: curvature of the corals
  • 'win/lose' criterion: spatial expansion of branches
  • 'birth-and-death' process: distances between corals
  • Matérn hardcore process: intensity of the number of corals
  • dilation: volume fraction

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 28

Stochstical geometry and virtual microstructure Collaboration Volker Schmidt (University of Ulm)

  • time series approach: curvature of the corals
  • 'win/lose' criterion: spatial expansion of branches
  • 'birth-and-death' process: distances between corals
  • Matérn hardcore process: intensity of the number of corals
  • dilation: volume fraction
  • G. Geiselmann; O. Stenzel; A. Kruglova; F. Muecklich, V. Schmidt
  • Comp. Materials Science 69(2013)289-298
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Starting from FIB/SEM tomographic data

Real data cube 1) Stems extraction Skeletonization 2)

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 29

Polygonal track: (α1; β1; l1)T, (α2; β2; l2)T... αi – azimuthal angle βi – polar angle li – length of a segment Stems extraction 3)

  • G. Geiselmann; O. Stenzel; A. Kruglova; F. Muecklich, V. Schmidt
  • Comp. Materials Science 69(2013)289-298
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Experimental and virtual microstructure  verification by 3D measures

Sample VV SV [m-1] MV [m-2] χv [m-3] NV [m-3]

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 30

Original structure Virtual structure Sample VV SV [m-1] MV [m-2] χv [m-3] NV [m-3]

Real 0,14 5,27e+5 3,84e+11 4,80e+15 1,04e+16 Simulated 0,13 4,95e+5 4,80e+11 4,65e+15 1,32e+16

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Experimental and virtual Al-Si microstructure –  simulate mechanically properties

Pure Al Statistical Al-Si network microstructure Virtual Al-Si Microstructure Real Al-Si Microstructure

Stress [a.u.] METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 31

Virtual Al-Si Microstructure

Strain [a.u.]

Homogeni- zation, virtual mechanics and FEM Colaboration Stefan Diebels (Saarland University)

M.Roland; A. Kruglova; N. Harste, F. Mücklich; S. Diebels Image Analysis and Stereology 33(2014)1, 29-37

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m

10-10 10-9 10-8 10-7 10-6 10-5 10-4 10-3 10-2 10-1 100 101

Å nm µm mm cm m atomar nano mikro 3D Atomsonden- Tomographie FIB/REM Nanotomographie Röntgen-CT Elektronen- (TEM) Tomographie mikroskopische Serienschnitttomographie

Tomography – Trying to Bridge the Gap Between  Relevant Resolution vs. Adequate Sampling Volume

mm µm nm atom

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 32 m

10-10 10-9 10-8 10-7 10-6 10-5 10-4 10-3 10-2 10-1 100 101

Å nm µm mm cm m atomar nano mikro 3D Atomsonden- Tomographie FIB/REM Nanotomographie Röntgen-CT Elektronen- (TEM) Tomographie mikroskopische Serienschnitttomographie

Atom Probe TEM FIB-SEM Metallographic X-Ray T o m o g r a p h y

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Scale bridging  also up to larger sampling volume

(100 µm)3 (1 mm)3 (10 mm)3

X-ray Tomography

(Synchrotron)

Mechanical Serial Sectioning

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 33 1 nm 10 nm 100 nm 1 µm 10 µm 100 µm (100 nm)3 (1 µm)3 (10 µm)3

APT STEM FIB/SEM Mechanical Serial Sectioning

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Sample surface  measuring

Metallographic serial sectioning  improved hight resolution (example steel)

removal [µm] Removal rate [µm/min] removal [µm] removal rate [µm/min]

Status quo: 0.42 ± 0.038 µm

D Britz, J Webel, F Mücklich Dörrenbächer (steel) award 2014

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 34 Sample surface  polishing Polishing tool removal rate [µm/min] number of sections

Status quo: 0.42 ± 0.038 µm Resolution: >250nm Volume: 10 -10 µm³

7 10…22

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Improved hight resolution by color etching  contrast without material removal

Dominik Britz

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 35

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Color Etching (Beraha) Orientation dependent layer formation

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 36

(100) (101) (111)

 Orientation dependent height profile EBSD

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Additional microstructure information  by metallographic tomography

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 37

Measurement in 2D  Effect of connectivity 200 400 600 800 1000 Euler number Particles 4000 8000 12000 16000 20000 Euler number Particles Measurement in 3D  Effect of connectivity

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Chair of Functional Materials

Metallographic Tomography of large Volume  discover connectivties over large distances

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 38

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Chair of Functional Materials

Internationality Flavio Soldera

Material Engineering Center Saarland Steinbeis Research Center

Innovation & Transfer

Institute Functional Materials Saarland University

Basic Research

Aluminium Michael Engstler

Thank you for you attention

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 39 Electr.Contacts Kim Trinh Antimicrobial Michael Hans Energetic Mat. Christoph Pauly Surface Design Carsten Gachot Steel Dominik Britz Atom Probe Jeni Barrirero

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Contact: Chair of Functional Materials Saarland University

  • Prof. Dr.-Ing. Frank Mücklich

Campus D3 3 66123 Saarbrücken Tel.: +49 681 302 70500

Thank you for your attention.

Contact: Chair of Functional Materials Saarland University

  • Prof. Dr.-Ing. Frank Mücklich

Campus D3 3 66123 Saarbrücken Tel.: +49 681 302 70500

www.mec-s.de info@mec-s.de Chair of Functional Materials www.fuwe.uni-saarland.de

muecke@matsci.uni-sb.de

Hisham Aboulfadl

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Chair of Functional Materials

How to Analyze the 3D Microstructure?  Stereology versus Tomography?

Stereology of particles general shape assumptions valid convex particles representative microstructure volume No need for tomography often less effort for statistical reliability

Spherical Polyhedral equiaxial Non equiaxial

METZ: 3D Microstructure Analysis | Frank Mücklich| muecke@matsci.uni-sb.de 41

Tomography

Topological information non convex particles not isolated particles Complex 3D shape complex arrangement local inhomogeneity