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Nanostructuring of 100 thousand tons
D. Ponge, J. Millan, L. Yuan, S. Sandlöbes, A. Kostka, P. Choi, T. Hickel,
                        J. Neugebauer, D. Raabe




                            Düsseldorf, Germany
                             WWW.MPIE.DE
                             d.raabe@mpie.de




        30. Nov. 2011   Dierk Raabe    GDCh Kolloquium Universität Duisburg-Essen
Nanostructures in 100 thousand tons




                                      www.mpie.de
The Düsseldorf Local Electrode Atom Probe (LEAP) Laboratory



LEAP 3000X HR, IMAGO Sci. Instr.
(since February 2009)

•    High spatial resolution
    (Dx ~ 0.2 nm, Dz ~ 0.1 nm)

•    High mass resolution
    (Dm/m = 1100, FWHM at 27 Da)

•    Fast data acquisition rate
    (max. ~ 2 Mio ions / min)

•    Large probed volumes
    (max. ~ 200 x 200 x 1000 nm3)

•    High detection sensitivity
    (min. ~ 10 ppm)

•    Pulsed laser
    (l = 532 nm, ~ 10 ps)


                                                              2/55
New materials for key technologies: Aero-space




                                                 3
New materials for key technologies: mobility on land and water




                                                                 4
New materials for key technologies: Power plants




                                                   5
New materials for key technologies: Green energy




                                                   6
New materials for key technologies: Health




                                             7
From atomistic understanding towards designing new materials




                                        D. Raabe et al. Scripta Materialia 60 (2009) 1141   8
Effect of aging on ductility
                             1400
                                       aged 450°C/48h                         2                                   Precipitation
                             1200                                                                                  hardening
Engineering Stress (MPa)




                                                    as-quenched
                             1000
                                                                                                             increase of austenite
                                                                                                                        ?
                              800                                         2                                   fraction during aging
                                            1       strain 0%                     strain 15%

                              600


                              400


                              200


                                01
                                 0              5               10        15                  20
                                                     Engineering Strain (%)
                                 -Fe (Martensite)
                                 -Fe (Austenite), vol. fraction 15-20%
                                                                                   D. Raabe et al. Scripta Materialia 60 (2009) 1141   9
Effect of cold rolling after aging
                            20
                                                                                                        12MnPH
                            18                    Why so much austenite 120 K below
                                                     equilibrium transformation?
                                                                                                         X-Ray
                            16
Fraction of Austenite (%)




                                                          ->’ (TRIP)
                            14
                                          
                            12        formation    aged
                            10          during     (450°C/48h)
                                        aging
                            8
                                     450°C/48h
                            6

                            4
                                               quenched
                            2

                            0
                                 0         5         10        15         20                 25                30

                                                   Cold Rolling Reduction, %
                                                                        D. Raabe et al. Scripta Materialia 60 (2009) 1141   10
APT results: Atomic map (12MnPH aged 450°C/48h)

               Martensite decorated by precipitations




                                  Austenite        ?
                       ?


Mn atoms                                                                   70 million ions
Ni atoms                                                                   Laser mode
Mn iso-concentration: 18 at.%                                              (0.4nJ, 54K)

                                                                      11
                                              Dmitrieva et al. Acta Mater 59 (2011)      11
Aging-induced austenite reversion

                                                                   Mn layer 1
                                                                   Mn layer 2
           Thermo-Calc 
        equilibrium Mn-conc.:                                              M                   A
     27 at. % Mn in austenite (A)
                                                           nominal 12 at.% Mn
 3 at. % Mn in ferrite (martensite) (M)                    depletion zone



                           Mn layer 2
                                          Mn layer 1




   M                                A                  M


                     Mn iso-concentration (18 at.% Mn)



                                                       Dmitrieva et al. Acta Mater 59 (2011)   12
Aging-induced austenite reversion

                                                             Mn layer 1
                                                             Mn layer 2
           Thermo-Calc 
                       Can      I push this idea further ?
        equilibrium Mn-conc.:                                        M                    A
                                                                                    A
                                                                                    M
     27 at. % Mn in austenite (A)
                                                          nominal 12 at.%
 3 at. % Mn in ferrite (martensite) (M)
                                                                                  aging



  Excellent agreement between                                          phase boundary
                                                                                 DICTRA
    experiment & simulation !



       Kinetic freezing and
 associated austenite reversion !



                                                  Dmitrieva et al. Acta Mater 59 (2011)       13
Growth of retained austenite 450°C/48h. 12MnPH

                                             1D. Conc. Profile - Manganese




                                  Maraging – TRIP Steel. APT                 14
Martensite relaxation & aging & nanoscale austenite reversion
650 MPa to 2 GPa
                                                     Ultra high strength and
                                                      corrosion resistance




 400°C aging: Ms-relaxation + prec. (aging) +
 austenite reversion

                   Fe-13.6Cr-0.44C (wt.%)
                                                                               15
Martensite relaxation & aging & nanoscale austenite reversion


                             at 5.45 at.% C, austenite forms at 400°C




C has ‘/’ shape in austenite layer: inheritance from austenite, Gibbs adsorption isotherm;
                                    C on martensite grain boundaries


C has ‘V’ shape in austenite layer: austenite reversion through partitioning and kinetic freezing

                                                                                                    16
Self-repair steels




                     17
Answering societies' grand challenges with complex alloys


         70% of all industrial innovations are associated with progress in
                       materials science and engineering

                  Specifically, metallic materials occupy key roles
                (energy, transportation, health, safety, infrastructure)


         Our mission: Designing new metallic alloys from first principles

         - Multiscale simulation
         - Multiscale characterization starting from the atomic scale
         - Synthesis, processing, testing




                                            www.mpie.de

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Universität duisburg-essen-raabe-dd ch-kolloquium

  • 1. Nanostructuring of 100 thousand tons D. Ponge, J. Millan, L. Yuan, S. Sandlöbes, A. Kostka, P. Choi, T. Hickel, J. Neugebauer, D. Raabe Düsseldorf, Germany WWW.MPIE.DE d.raabe@mpie.de 30. Nov. 2011 Dierk Raabe GDCh Kolloquium Universität Duisburg-Essen
  • 2. Nanostructures in 100 thousand tons www.mpie.de
  • 3. The Düsseldorf Local Electrode Atom Probe (LEAP) Laboratory LEAP 3000X HR, IMAGO Sci. Instr. (since February 2009) • High spatial resolution (Dx ~ 0.2 nm, Dz ~ 0.1 nm) • High mass resolution (Dm/m = 1100, FWHM at 27 Da) • Fast data acquisition rate (max. ~ 2 Mio ions / min) • Large probed volumes (max. ~ 200 x 200 x 1000 nm3) • High detection sensitivity (min. ~ 10 ppm) • Pulsed laser (l = 532 nm, ~ 10 ps) 2/55
  • 4. New materials for key technologies: Aero-space 3
  • 5. New materials for key technologies: mobility on land and water 4
  • 6. New materials for key technologies: Power plants 5
  • 7. New materials for key technologies: Green energy 6
  • 8. New materials for key technologies: Health 7
  • 9. From atomistic understanding towards designing new materials D. Raabe et al. Scripta Materialia 60 (2009) 1141 8
  • 10. Effect of aging on ductility 1400 aged 450°C/48h 2 Precipitation 1200 hardening Engineering Stress (MPa) as-quenched 1000 increase of austenite ? 800 2 fraction during aging 1 strain 0% strain 15% 600 400 200 01 0 5 10 15 20 Engineering Strain (%) -Fe (Martensite) -Fe (Austenite), vol. fraction 15-20% D. Raabe et al. Scripta Materialia 60 (2009) 1141 9
  • 11. Effect of cold rolling after aging 20 12MnPH 18 Why so much austenite 120 K below equilibrium transformation? X-Ray 16 Fraction of Austenite (%) ->’ (TRIP) 14  12 formation aged 10 during (450°C/48h) aging 8 450°C/48h 6 4 quenched 2 0 0 5 10 15 20 25 30 Cold Rolling Reduction, % D. Raabe et al. Scripta Materialia 60 (2009) 1141 10
  • 12. APT results: Atomic map (12MnPH aged 450°C/48h) Martensite decorated by precipitations Austenite ? ? Mn atoms 70 million ions Ni atoms Laser mode Mn iso-concentration: 18 at.% (0.4nJ, 54K) 11 Dmitrieva et al. Acta Mater 59 (2011) 11
  • 13. Aging-induced austenite reversion Mn layer 1 Mn layer 2 Thermo-Calc  equilibrium Mn-conc.: M A 27 at. % Mn in austenite (A) nominal 12 at.% Mn 3 at. % Mn in ferrite (martensite) (M) depletion zone Mn layer 2 Mn layer 1 M A M Mn iso-concentration (18 at.% Mn) Dmitrieva et al. Acta Mater 59 (2011) 12
  • 14. Aging-induced austenite reversion Mn layer 1 Mn layer 2 Thermo-Calc  Can I push this idea further ? equilibrium Mn-conc.: M A A M 27 at. % Mn in austenite (A) nominal 12 at.% 3 at. % Mn in ferrite (martensite) (M) aging Excellent agreement between phase boundary DICTRA experiment & simulation ! Kinetic freezing and associated austenite reversion ! Dmitrieva et al. Acta Mater 59 (2011) 13
  • 15. Growth of retained austenite 450°C/48h. 12MnPH 1D. Conc. Profile - Manganese Maraging – TRIP Steel. APT 14
  • 16. Martensite relaxation & aging & nanoscale austenite reversion 650 MPa to 2 GPa Ultra high strength and corrosion resistance 400°C aging: Ms-relaxation + prec. (aging) + austenite reversion Fe-13.6Cr-0.44C (wt.%) 15
  • 17. Martensite relaxation & aging & nanoscale austenite reversion at 5.45 at.% C, austenite forms at 400°C C has ‘/’ shape in austenite layer: inheritance from austenite, Gibbs adsorption isotherm; C on martensite grain boundaries C has ‘V’ shape in austenite layer: austenite reversion through partitioning and kinetic freezing 16
  • 19. Answering societies' grand challenges with complex alloys 70% of all industrial innovations are associated with progress in materials science and engineering Specifically, metallic materials occupy key roles (energy, transportation, health, safety, infrastructure) Our mission: Designing new metallic alloys from first principles - Multiscale simulation - Multiscale characterization starting from the atomic scale - Synthesis, processing, testing www.mpie.de