Titulo de la
            Effect of composition and thermomechanical
                               presentación
            process on the austenite transformation in
            Nb-Mo microalloyed steels

                                   October 21, 2010 – Houston, Texas


                  N. Isasti, B. López and P. Uranga
                         puranga@ceit.es
                (CEIT and TECNUN, Univ. Navarra)

A. Leff, E. Toby, M. Hartshorne, C. Wrinkler and M. Taheri (Drexel U.)
                       M. Grimes (Lehigh U.)
Introduction

• Multiple microalloying for high performance
  grades:
  – High strength and low-T toughness
• Combined effect – synergies Nb-Mo
• Effect of thermomechanical route:
  – Recrystallized austenite
  – Deformed austenite
• Reducing grain size (unit size) in transformed
  phases:
  – strength and toughness improved
Steel compositions and Techniques

EXPERIMENTAL
Chemical compositions of steels (wt%)

     Steel    C     Mn      Si     Nb     Mo      Al      N
   CMn       0.05   1.58   0.05     -     0.01   0.03    0.005
   3NbMo0    0.05   1.6    0.06   0.029   0.01   0.028   0.005
   3NbMo16   0.05   1.58   0.04   0.03    0.16   0.027   0.005
   3NbMo31   0.05   1.57   0.05   0.028   0.31   0.028   0.005
   6NbMo0    0.05   1.56   0.05   0.06    0.01   0.028   0.004
   6NbMo16   0.05   1.6    0.05   0.061   0.16   0.03    0.005
   6NbMo31   0.05   1.57   0.05   0.059   0.31   0.031   0.005
Chemical compositions of steels (wt%)



   Steel    C     Mn      Si     Nb     Mo      Al     N

  6NbMo0   0.05   1.56   0.05   0.06    0.01   0.028 0.004

  6NbMo16 0.05    1.6    0.05   0.061   0.16   0.03   0.005

  6NbMo31 0.05    1.57   0.05   0.059   0.31   0.031 0.005
Experimental Procedure

• Bähr DIL805D deformation dilatometer
• Optical Microscopy
• Philips XL30cp Scanning Electron Microscope (SEM), using
TSL (TexSEM laboratories) MSC 2002 equipment.
• Field Emission Scanning Electron Microscope (FEG-SEM)
Jeol JSM-7000F, using HKL Channel5 EBSD
• Vickers hardness (HV 1 kg)
Schematics of thermomechanical schedules

   
      Temperature (ºC)

                         1250ºC, 5min
                            20ºC/s→         12s
                                                           ε=0.3, ε&& = 1s −−11
                                                  1150ºC, ε = 0.3, ε =1s-1
                                        20ºC/s→
                                                           5s
                                                                        ε = 0.4εε = 1s −−11
                                                                 900ºC, ε =0.4, ,&& =1s-1


                                         Cycle A                      Cycle B


                                                                Time (s)
Microstructural Characterization and Dilatometry Curves

RESULTS
Optical Micrographs
                                6NbMo0
           Cycle A    Cycle B




0.1 ºC/s                          PF+GF(+P)




0.5 ºC/s                          PF+QF+GF
Optical Micrographs
                                6NbMo0
           Cycle A    Cycle B




10 ºC/s                           QF+GF




                                  QF+GF+
100 ºC/s
                                   BF+M
Dilatometry curves
                                                                                                              6NbMo31
                                                                                                                Cycle B
         0.004                                                                  100
                       0.1ºC/s                                                                0.1ºC/s
                       0.5ºC/s                                                                0.5ºC/s




                                                     Transformed fraction (%)
                       10ºC/s                                                    80           10ºC/s
             0         100ºC/s                                                                100ºC/s


                                                                                 60
 ΔL/Lo




         -0.004
                                                                                 40

         -0.008
                                                                                 20


         -0.012                                                                  0
                  0   200        400    600    800                                    0      200        400    600    800
                            Temperature (ºC)                                                       Temperature (ºC)



              ΔL/L0 vs Temperature (ºC)                                                   Transformed Fraction vs
                                                                                             Temperature (ºC)
Dilatometry curves – Transfomation Rates
                                                                                              6NbMo31            Cycle B

                      0.6                                                            60
                                0.1ºC/s                                                         10ºC/s
                                0.5ºC/s                                                         100ºC/s
Transformation Rate




                                                               Transformation Rate
                      0.4                                                            40




                      0.2                                                            20




                       0                                                             0
                            0   200       400      600   800                              0     200       400      600   800
                                      Temperature (ºC)                                                Temperature (ºC)
Phase Stability Regions

CCT DIAGRAMS
CCT Diagrams
                                                                                                                                                     6NbMo0

                                          Cycle A                                                                                           Cycle B

                   1000                                                                                             1000
                   900                                                                                              900
                   800                                                                                              800                                    A
                                                            A                                                                                                                 PF
                   700                                                          PF                                  700
Temperature (ºC)




                                                                                                 Temperature (ºC)
                                                                                                                                                                        45% 65%
                                                                                       88%
                                                                      15%                                                                                                                   92%
                                                                                GF                                                                               25%     GF       P
                   600                                  GF+QF                                                       600                                    25%
                                                                                                                                                   GF+QF
                   500                                                                                              500                       BF
                                                BF
                                                                                                                                   Ms
                   400            Ms            M                                                                   400                       M


                   300                                                                                              300
                                                                                                                                       ºC/s   200 100 50   20    10 5    2    1       0.5     0.1
                   200             ºC/s   200 100 50   20   10 5      2     1    0.5     0.1                        200
                                                                                                                                       HV     268 265 257 227 215 210 209 197 185             160
                   100      6NbMo0 HV     279 275 272 240 220 207 204 202 197            191
                                                                                                                    100      6NbMo0
                            Cycle A                                                                                          Cycle B
                     0                                                                                                0
                          0.1     1           10                100         1000         10000                             0.1         1           10            100          1000           10000
                                                 Time (s)                                                                                            Time (s)
CCT Diagrams
                                                                                                                                                                   6NbMo16

                                               Cycle A                                                                                                   Cycle B

                   1000                                                                                                       1000
                   900                                                                                                        900
                   800                                                                                                        800
                                                                                                                                                                          A                PF
                                                                 A                    PF
                   700                                                                                                        700
Temperature (ºC)




                                                                                                           Temperature (ºC)
                                                                                                 87%                                                                                 55%
                                                                                                                                                                                            85%
                                                                            15%
                                                                                      GF                                                                                                        GF
                   600                                                                                                        600                                  GF+QF
                                                            GF+QF
                   500                             BF                                                                         500
                                                                                                                                                              BF
                   400                Ms       M                                                                              400
                                                                                                                                                                   85%
                                                                                                                                             Ms           M
                   300                                                                                                        300
                   200                  ºC/s   200 100 50   20       10 5   2     1        0.5     0.1                        200                 ºC/s   200 100 50      20   10 5   2     1      0.5   0.1

                   100          6NbMo16 HV     292 280 271 240 229 219 217 211 203                 199
                                                                                                                              100      6NbMo16 HV        270 268 264 248 234 219 213 212 204            157
                                Cycle A                                                                                                Cycle B
                     0                                                                                                          0
                          0.1         1             10               100          1000             10000                             0.1     1                10              100           1000        10000
                                                        Time (s)                                                                                                   Time (s)
                                                                                                                                                                                                                 
CCT Diagrams
                                                                                                                                                                 6NbMo31

                                                   Cycle A                                                                                             Cycle B
                                                                                                                                                                                                            

                   1000                                                                                                     1000
                   900                                                                                                      900
                                                                                                                                                                                 A
                   800                                                                                                      800
                                                                                                                                                                                      PF
                                                                     A
                   700                                                                                                      700
Temperature (ºC)




                                                                                                                                                                                                 93%




                                                                                                         Temperature (ºC)
                                                                                         PF                                                                                 19% 41% 65%
                                                                                                70%

                   600                                                   GF+QF           GF                                 600                                      GF+QF
                                                                                                                                                                                 GF

                   500                                                                                                      500                            BF
                                                       BF                                                                                                  75%
                   400                  Ms         M                                                                        400                 Ms     M
                   300                                                                                                      300
                   200                      ºC/s   200 100 50   20       10 5    2   1    0.5     0.1                       200                 ºC/s   200 100 50   20   10 5    2    1    0,5     0,1

                   100          6NbMo31 HV         311 298 292 260 236 220 214 213 212            210
                                                                                                                            100          6NbMo31 HV    299 292 282 241 232 215 213 201 176         147
                                Cycle A                                                                                                  Cycle B
                     0                                                                                                        0
                          0.1           1               10               100         1000        10000                             0.1          1            10          100          1000         10000
                                                            Time (s)                                                                                             Time (s)
                                                                                                                                                                                                            
                                     
Alloying and Retained Strain Effects

CCT ANALYSIS
Effect of Retained Strain on CCT
                                                                                                     6NbMo31
                    1000
                    900
                    800
                                                                A                   PF
                    700
 Temperature (ºC)




                                                                                GF
                    600                                             GF+QF

                    500
                                                  BF
                    400            Ms         M

                    300
                    200                ºC/s   200 100 50   20       10 5    2   1        0.5   0.1

                    100
                             6NbMo31
                      0
                           0.1     1               10               100         1000           10000
                                                       Time (s)
Mo Effect on CCT
                                                                                                       Cycle B
                     1000
                     900
                     800
                                                                  A
                                                                                      PF
                     700
  Temperature (ºC)




                                                                      GF+QF       GF
                     600
                     500                               BF

                     400                Ms         M

                     300
                     200                    ºC/s   200 100 50    20   10 5    2   1        0.5   0.1

                     100
                              Cycle B
                       0
                            0.1         1                   10        100         1000           10000
                                                             Time (s)
EBSD / SEM-FEGSEM

LOW COOLING RATE PHASES
Low CR-EBSD
                                            Cycle B
    Effect of Mo addition

  6NbMo0                6NbMo16             6NbMo31




                   Cooling Rate= 0.1 ºC/s
EBSD                                                       Cooling Rate= 0.1 ºC/s

                                                                              Cycle B
   Effect of Mo
                                   1.2


                                    1
       Accumulated Area Fraction



                                   0.8


                                   0.6


                                   0.4
                                                             0.1ºC/s
                                                                    6NbMo0
                                   0.2
                                                                    6NbMo16
                                                                    6NbMo31
                                    0
                                         105

                                         125
                                         135
                                         145
                                         155
                                           5
                                          15
                                          25
                                          35
                                          45
                                          55
                                          65
                                          75
                                          85
                                          95

                                         115




                                         Grain Size (Diameter µm)
EBSD / SEM-FEGSEM

IDENTIFICATION OF
SECONDARY PHASES
EBSD
                                              6NbMo16
   Identification of second phases             Cycle B
              Degenerated
   0.5 ºC/s                          1 ºC/s      M/A Islands
              Pearlite




                     Fe3C-1
                     MAD 0.538
Bainite + Martensite + (GF+QF)

HIGH COOLING RATE PHASES
High CR products – FEGSEM EBSD
                                                                 6NbMo16
    Image Quality (IQ)
                           20 ºC/s               100 ºC/s




       =50 µm; Map15; Step=0.2 µm; Grid700x700       =50 µm; Map15; Step=0.2 µm; Grid700x700
EBSD (Electron Backscatter
Diffraction)                                                                                    6NbMo16

    Misorientation Map
           20 ºC/s                                            100 ºC/s




            =50 µm; Map15; Step=0.2 µm; Grid700x700             =50 µm; Map15; Step=0.2 µm; Grid700x700




                                                      1-15º
                                                      >15º
EBSD (Electron Backscatter
Diffraction)                                                                               6NbMo16

    Inverse Pole Figure IPF (z)
              20 ºC/s                                100 ºC/s




           =50 µm; Map15; Step=0.2 µm; Grid700x700    =50 µm; Map15; Step=0.2 µm; Grid700x700
Final Remarks


• Effect of Mo and retained strain has been
  evaluated
  – Slight effect of Mo: increase in ferrite size
  – Strong effect of strain
• EBSD unit size measurements may be useful
  for toughness predictions
• The generated data will be the input for
  modeling
Acknowledgements


• Science and Innovation Ministry of Spain
  (MAT2009-09250)
• NSF and TMS. Conference Registration Fee
  Funding
• N . Isasti for all the experimental results and
  analysis (1st year PhD student)
• D. Jorge-Badiola: help on EBSD
Titulo de la
            Effect of composition and thermomechanical
                               presentación
            process on the austenite transformation in
            Nb-Mo microalloyed steels

                                   October 21, 2010 – Houston, Texas


                  N. Isasti, B. López and P. Uranga
                         puranga@ceit.es
                (CEIT and TECNUN, Univ. Navarra)

A. Leff, E. Toby, M. Hartshorne, C. Wrinkler and M. Taheri (Drexel U.)
                       M. Grimes (Lehigh U.)

Effect of thermomechanical process on the austenite transformation in Nb-Mo microalloyed steels

  • 1.
    Titulo de la Effect of composition and thermomechanical presentación process on the austenite transformation in Nb-Mo microalloyed steels October 21, 2010 – Houston, Texas N. Isasti, B. López and P. Uranga puranga@ceit.es (CEIT and TECNUN, Univ. Navarra) A. Leff, E. Toby, M. Hartshorne, C. Wrinkler and M. Taheri (Drexel U.) M. Grimes (Lehigh U.)
  • 2.
    Introduction • Multiple microalloyingfor high performance grades: – High strength and low-T toughness • Combined effect – synergies Nb-Mo • Effect of thermomechanical route: – Recrystallized austenite – Deformed austenite • Reducing grain size (unit size) in transformed phases: – strength and toughness improved
  • 3.
    Steel compositions andTechniques EXPERIMENTAL
  • 4.
    Chemical compositions ofsteels (wt%) Steel C Mn Si Nb Mo Al N CMn 0.05 1.58 0.05 - 0.01 0.03 0.005 3NbMo0 0.05 1.6 0.06 0.029 0.01 0.028 0.005 3NbMo16 0.05 1.58 0.04 0.03 0.16 0.027 0.005 3NbMo31 0.05 1.57 0.05 0.028 0.31 0.028 0.005 6NbMo0 0.05 1.56 0.05 0.06 0.01 0.028 0.004 6NbMo16 0.05 1.6 0.05 0.061 0.16 0.03 0.005 6NbMo31 0.05 1.57 0.05 0.059 0.31 0.031 0.005
  • 5.
    Chemical compositions ofsteels (wt%) Steel C Mn Si Nb Mo Al N 6NbMo0 0.05 1.56 0.05 0.06 0.01 0.028 0.004 6NbMo16 0.05 1.6 0.05 0.061 0.16 0.03 0.005 6NbMo31 0.05 1.57 0.05 0.059 0.31 0.031 0.005
  • 6.
    Experimental Procedure • BährDIL805D deformation dilatometer • Optical Microscopy • Philips XL30cp Scanning Electron Microscope (SEM), using TSL (TexSEM laboratories) MSC 2002 equipment. • Field Emission Scanning Electron Microscope (FEG-SEM) Jeol JSM-7000F, using HKL Channel5 EBSD • Vickers hardness (HV 1 kg)
  • 7.
    Schematics of thermomechanicalschedules   Temperature (ºC) 1250ºC, 5min 20ºC/s→ 12s ε=0.3, ε&& = 1s −−11 1150ºC, ε = 0.3, ε =1s-1 20ºC/s→ 5s ε = 0.4εε = 1s −−11 900ºC, ε =0.4, ,&& =1s-1 Cycle A Cycle B Time (s)
  • 8.
    Microstructural Characterization andDilatometry Curves RESULTS
  • 9.
    Optical Micrographs 6NbMo0 Cycle A Cycle B 0.1 ºC/s PF+GF(+P) 0.5 ºC/s PF+QF+GF
  • 10.
    Optical Micrographs 6NbMo0 Cycle A Cycle B 10 ºC/s QF+GF QF+GF+ 100 ºC/s BF+M
  • 11.
    Dilatometry curves 6NbMo31 Cycle B 0.004 100 0.1ºC/s 0.1ºC/s 0.5ºC/s 0.5ºC/s Transformed fraction (%) 10ºC/s 80 10ºC/s 0 100ºC/s 100ºC/s 60 ΔL/Lo -0.004 40 -0.008 20 -0.012 0 0 200 400 600 800 0 200 400 600 800 Temperature (ºC) Temperature (ºC) ΔL/L0 vs Temperature (ºC) Transformed Fraction vs Temperature (ºC)
  • 12.
    Dilatometry curves –Transfomation Rates 6NbMo31 Cycle B 0.6 60 0.1ºC/s 10ºC/s 0.5ºC/s 100ºC/s Transformation Rate Transformation Rate 0.4 40 0.2 20 0 0 0 200 400 600 800 0 200 400 600 800 Temperature (ºC) Temperature (ºC)
  • 13.
  • 14.
    CCT Diagrams 6NbMo0 Cycle A Cycle B 1000 1000 900 900 800 800 A A PF 700 PF 700 Temperature (ºC) Temperature (ºC) 45% 65% 88% 15% 92% GF 25% GF P 600 GF+QF 600 25% GF+QF 500 500 BF BF Ms 400 Ms M 400 M 300 300 ºC/s 200 100 50 20 10 5 2 1 0.5 0.1 200 ºC/s 200 100 50 20 10 5 2 1 0.5 0.1 200 HV 268 265 257 227 215 210 209 197 185 160 100 6NbMo0 HV 279 275 272 240 220 207 204 202 197 191 100 6NbMo0 Cycle A Cycle B 0 0 0.1 1 10 100 1000 10000 0.1 1 10 100 1000 10000 Time (s) Time (s)
  • 15.
    CCT Diagrams 6NbMo16 Cycle A Cycle B 1000 1000 900 900 800 800 A PF A PF 700 700 Temperature (ºC) Temperature (ºC) 87% 55% 85% 15% GF GF 600 600 GF+QF GF+QF 500 BF 500 BF 400 Ms M 400 85% Ms M 300 300 200 ºC/s 200 100 50 20 10 5 2 1 0.5 0.1 200 ºC/s 200 100 50 20 10 5 2 1 0.5 0.1 100 6NbMo16 HV 292 280 271 240 229 219 217 211 203 199 100 6NbMo16 HV 270 268 264 248 234 219 213 212 204 157 Cycle A Cycle B 0 0 0.1 1 10 100 1000 10000 0.1 1 10 100 1000 10000 Time (s) Time (s)  
  • 16.
    CCT Diagrams 6NbMo31 Cycle A Cycle B   1000 1000 900 900 A 800 800 PF A 700 700 Temperature (ºC) 93% Temperature (ºC) PF 19% 41% 65% 70% 600 GF+QF GF 600 GF+QF GF 500 500 BF BF 75% 400 Ms M 400 Ms M 300 300 200 ºC/s 200 100 50 20 10 5 2 1 0.5 0.1 200 ºC/s 200 100 50 20 10 5 2 1 0,5 0,1 100 6NbMo31 HV 311 298 292 260 236 220 214 213 212 210 100 6NbMo31 HV 299 292 282 241 232 215 213 201 176 147 Cycle A Cycle B 0 0 0.1 1 10 100 1000 10000 0.1 1 10 100 1000 10000 Time (s) Time (s)    
  • 17.
    Alloying and RetainedStrain Effects CCT ANALYSIS
  • 18.
    Effect of RetainedStrain on CCT 6NbMo31 1000 900 800 A PF 700 Temperature (ºC) GF 600 GF+QF 500 BF 400 Ms M 300 200 ºC/s 200 100 50 20 10 5 2 1 0.5 0.1 100 6NbMo31 0 0.1 1 10 100 1000 10000 Time (s)
  • 19.
    Mo Effect onCCT Cycle B 1000 900 800 A PF 700 Temperature (ºC) GF+QF GF 600 500 BF 400 Ms M 300 200 ºC/s 200 100 50 20 10 5 2 1 0.5 0.1 100 Cycle B 0 0.1 1 10 100 1000 10000 Time (s)
  • 20.
    EBSD / SEM-FEGSEM LOWCOOLING RATE PHASES
  • 21.
    Low CR-EBSD Cycle B Effect of Mo addition 6NbMo0 6NbMo16 6NbMo31 Cooling Rate= 0.1 ºC/s
  • 22.
    EBSD Cooling Rate= 0.1 ºC/s Cycle B Effect of Mo 1.2 1 Accumulated Area Fraction 0.8 0.6 0.4 0.1ºC/s 6NbMo0 0.2 6NbMo16 6NbMo31 0 105 125 135 145 155 5 15 25 35 45 55 65 75 85 95 115 Grain Size (Diameter µm)
  • 23.
  • 24.
    EBSD 6NbMo16 Identification of second phases Cycle B Degenerated 0.5 ºC/s 1 ºC/s M/A Islands Pearlite Fe3C-1 MAD 0.538
  • 25.
    Bainite + Martensite+ (GF+QF) HIGH COOLING RATE PHASES
  • 26.
    High CR products– FEGSEM EBSD 6NbMo16 Image Quality (IQ) 20 ºC/s 100 ºC/s =50 µm; Map15; Step=0.2 µm; Grid700x700 =50 µm; Map15; Step=0.2 µm; Grid700x700
  • 27.
    EBSD (Electron Backscatter Diffraction) 6NbMo16 Misorientation Map 20 ºC/s 100 ºC/s =50 µm; Map15; Step=0.2 µm; Grid700x700 =50 µm; Map15; Step=0.2 µm; Grid700x700 1-15º >15º
  • 28.
    EBSD (Electron Backscatter Diffraction) 6NbMo16 Inverse Pole Figure IPF (z) 20 ºC/s 100 ºC/s =50 µm; Map15; Step=0.2 µm; Grid700x700 =50 µm; Map15; Step=0.2 µm; Grid700x700
  • 29.
    Final Remarks • Effectof Mo and retained strain has been evaluated – Slight effect of Mo: increase in ferrite size – Strong effect of strain • EBSD unit size measurements may be useful for toughness predictions • The generated data will be the input for modeling
  • 30.
    Acknowledgements • Science andInnovation Ministry of Spain (MAT2009-09250) • NSF and TMS. Conference Registration Fee Funding • N . Isasti for all the experimental results and analysis (1st year PhD student) • D. Jorge-Badiola: help on EBSD
  • 31.
    Titulo de la Effect of composition and thermomechanical presentación process on the austenite transformation in Nb-Mo microalloyed steels October 21, 2010 – Houston, Texas N. Isasti, B. López and P. Uranga puranga@ceit.es (CEIT and TECNUN, Univ. Navarra) A. Leff, E. Toby, M. Hartshorne, C. Wrinkler and M. Taheri (Drexel U.) M. Grimes (Lehigh U.)