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Compositional and Structural Factors that Influence Hydrogen Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical Metallurgy Group MEMS Department Image Quality or Inverse Lattice Distortion LTP HTP

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Page 1: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Compositional and Structural Factors that Influence Hydrogen Induced Cracking and Hydrogen

Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li

Advisor: C. Isaac Garcia Ferrous Physical Metallurgy Group

MEMS Department

Image Quality or Inverse Lattice Distortion

LTP

HTP

Page 2: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

IMF Spring Meeting

HIC Program Progress Review

April 14, 2015.

Page 3: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Step A 8630 A 4340 B4340 1 B4340 2 B 4340 3 B 8630 1 B 8630 2 B 8630 3 C 1 C 2

UT 1Mhz Scan DONE DONE DONE DONE DONE DONE DONE DONE DONE PENDING

UT 5Mhz Scan DONE DONE DONE DONE DONE DONE DONE DONE DONE PENDING

UT 10Mhz Scan DONE DONE DONE DONE DONE DONE DONE DONE DONE PENDING

Sectioning DONE DONE DONE DONE DONE DONE DONE DONE DONE PENDING

Grinding/ Polishing DONE DONE DONE DONE DONE DONE DONE DONE DONE PENDING

Nital Etching DONE DONE DONE DONE DONE DONE DONE DONE DONE PENDING

Vickers Hardness Measurement

DONE DONE DONE DONE DONE PENDING DONE DONE DONE PENDING

Inclusion Size Measurement

DONE PENDING DONE DONE DONE DONE DONE DONE DONE PENDING

Le Pera Etching DONE DONE DONE DONE DONE DONE DONE DONE DONE PENDING

Modified Sodium Metabisulfite

PENDING PENDING DONE DONE DONE PENDING PENDING PENDING PENDING PENDING

Modified Le Pera Etching PENDING PENDING PENDING PENDING PENDING PENDING PENDING PENDING PENDING PENDING

SEM Inclusions analysis PENDING PENDING DONE DONE DONE PENDING PENDING PENDING PENDING PENDING

SEM Microstructure PENDING PENDING DONE DONE DONE PENDING PENDING PENDING PENDING PENDING

XRD PENDING PENDING PENDING PENDING PENDING PENDING PENDING PENDING PENDING PENDING

Hyper Probe PENDING PENDING PENDING PENDING PENDING PENDING PENDING PENDING PENDING PENDING

IMF October 2014 Meeting

Page 4: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Step A 8630 A 4340 B4340 1 B4340 2 B 4340 3 B 8630 1 B 8630 2 B 8630 3 C 1 C 2

UT 1Mhz Scan DONE DONE DONE DONE DONE DONE DONE DONE DONE DONE

UT 5Mhz Scan DONE DONE DONE DONE DONE DONE DONE DONE DONE DONE

UT 10Mhz Scan DONE DONE DONE DONE DONE DONE DONE DONE DONE DONE

Sectioning DONE DONE DONE DONE DONE DONE DONE DONE DONE DONE

Grinding/ Polishing DONE DONE DONE DONE DONE DONE DONE DONE DONE DONE

Nital Etching DONE DONE DONE DONE DONE DONE DONE DONE DONE DONE

Vickers Hardness Measurement

DONE DONE DONE DONE DONE DONE DONE DONE DONE DONE

Inclusion Size Measurement

DONE DONE DONE DONE DONE DONE DONE DONE DONE DONE

Modified Sodium Metabisulfite

DONE DONE DONE DONE DONE DONE DONE DONE DONE DONE

Modified Le Pera Etching DONE DONE DONE DONE DONE DONE DONE DONE DONE DONE

Inclusions analysis DONE DONE DONE DONE DONE DONE DONE DONE DONE DONE

SEM Microstructure DONE DONE DONE DONE DONE DONE DONE DONE DONE DONE

XRD DONE DONE DONE DONE DONE DONE DONE DONE DONE DONE

Hyper Probe DONE PENDING PENDING DONE PENDING PENDING PENDING PENDING PENDING PENDING

IMF Spring-April 2015 Meeting

Page 5: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

o Current Studies

• Advanced Microstructural Characterization • X-Ray Diffraction • Electron Backscattered Diffraction • Hyper-probe Chemical Analysis • FEA – CCT microstructural correlations • NDT/NDE – microstructure relations

o Results o Future work

Page 6: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Company A 4340 S1

C Mn P S Si Ni Cr Mo V Al Cu H

0.42 0.78 0.010 0.017 0.29 1.72 0.90 0.29 0.052 0.020 0.19 1.6ppm

Company A 4340 AC

C Mn P S Si Ni Cr Mo V Al Cu H

0.42 0.76 0.009 0.014 0.32 1.74 0.86 0.26 0.006 0.03 0.19 -

Company A 8630

C Mn P S Si Ni Cr Mo V Al Cu H

0.30 0.96 0.008 0.01 0.35 0.85 1.10 0.48 0.008 0.020 0.19 1.0ppm

Company A 8630 AC

C Mn P S Si Ni Cr Mo V Al Cu H

0.32 0.94 0.010 0.006 0.3 0.85 0.99 0.43 0.007 0.026 0.17 -

Company B 4340 05

C Mn P S Si Cr Ni Mo Cu Al V H

0.42 0.78 0.007 0.002 0.28 0.86 1.68 0.29 0.18 0.028 0.005 -

Chemical Composition Table (wt %)

Page 7: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Company B 4340 87

C Mn P S Si Cr Ni Mo Cu Al V H

0.41 0.78 0.009 0.018 0.34 0.86 1.67 0.22 0.17 0.028 0.006 -

Company B 8630

C Mn P S Si Cr Ni Mo Cu Al V H

0.3 0.89 0.009 0.008 0.32 0.47 0.44 0.16 0.16 0.03 0.002 -

Company C 4340 A

C Mn P S Si Ni Cr Mo V Al Cu H

0.41 0.74 0.011 0.002 0.3 0.85 0.99 0.43 0.007 0.026 0.17 -

Company C 4340 C

C Mn P S Si Ni Cr Mo V Al Cu H

0.42 0.74 0.011 0.006 0.3 1.86 0.85 0.25 0.006 0.026 0.17 -

Chemical Composition Table (wt%)

Page 8: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

-18

-15

-12

-9

-6

-3

0

0 10 20 30 40 50

35mm

32.8HRC

Pea

k A

mp d

B

Depth mm

5mm Edge

5mm Core

20mm

25mm

35mm

32.8 HRC

Company B 4340 Microstructures

Peak Amplitude - MIcrostructure

Page 9: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

-25

-20

-15

-10

-5

0

0 10 20 30 40 50 60

Depth mm

50mm

31.4HRC

Pea

k A

mp d

B

20mm

10mm

50mm

31.4 HRC

Company B 4340 Microstructures

Peak Amplitude - Microstructure

Page 10: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

-35

-30

-25

-20

-15

-10

-5

0

0 20 40 60 80 100 120 140

Pea

k A

mp d

B 50mm

100mm 10mm

10mm

110mm

50mm

100mm

-25

-20

-15

-10

-5

0

0 10 20 30 40 50 60

Depth mm

J2487-1-02 Core J2487-1-02 J2405-1-02

22.7HRC

32.9HRC

32.9HRC 31.7HRC

32.8HRC

30.3HRC

31.0HRC

31.4HRC

31.8HRC

29.4HRC 29.3HRC

4340 company A

Depth mm

Pea

k A

mp d

B

Signal response Peak Amplitude and Hardness between 4340 steel samples investigated

Process: Ingot – Soaking – Forging – Air Cooling

Process: Normalizing – Austenizing - Oil Quench - Temper

Page 11: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

-21

-19

-17

-15

-13

-11

-9

-7

-15

-14

-13

-12

-11

-10

-9

-8

-7

10mm

50mm

100mm

27.6HRC

26.7HRC

27.3HRC

32.2HRC 33.5HRC

26.5HRC

28.3HRC

10mm 20mm 30mm

25.7HRC

25.4HRC

28.2HRC

26.2HRC

J2487-4-02 J2499-3-02 J2499-1-02 8630 A

Signal response Peak Amplitude and Hardness between 8630 steel samples investigated

Process: Ingot – Soaking – Forging – Air Cooling

Process: Normalizing – Austenizing - Oil Quench - Temper

Page 12: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Signal response Peak Amplitude and Hardness between company A samples

-32

-27

-22

-17

-12

-7P

eak

Am

p d

B

10mm

10mm

50mm 110mm

50mm

100mm

8630 4340

* Same scanning parameters were used for both samples.

31.8HRC

29.4HRC 29.3HRC

27.6HRC

26.7HRC

27.3HRC

The microstructures generated by 8630 steel seems to produce lower signal attenuation than the microstructures generated by 4340 steel. The samples from Company A where used for this analysis cause have similar process and geometry.

Page 13: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

-35

-30

-25

-20

-15

-10

-5

0

0 10 20 30 40 50 60

Signal - Peak Amplitude –vs- Hardness & Type of Microstructure.

Martensite +

bainite

Ferrite Pearlite – fine Pearlite

Pearlite + some Pro

eutectoid cementite

Martensite-Austenite Pearlite – Coarse Pearlite

Effect of different types of microstructure on the sound propagation response

as measured by Peak Amplitude

Pe

ak A

mp

dB

Hardness HRC

Page 14: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

23

12

52 49

42

6.2 5

11 14

16

0

10

20

30

40

50

60

8630 A 8630 As Cast 8630 B 1 8630 B 3 8630 B 4

Inclusions Avg Size *

8630

4340

mic

ron

s

MnS Inclusion in Company A 4340 MnS Inclusion in Company B 8630 MnS Inclusion in Company B 8630

OM DIC SEM BSE

Inclusions Size Distribution

* 10 Inclusions measured for each sample

10um

Page 15: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Advanced Characterization

Differential Interference Contrast (DIC) X-Ray Diffraction (XRD) – Empyrean System Electron Backscattered Diffraction (EBSD) JEOL Hyper-Probe Microscopy

Page 16: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

J 2405-1-02

OM-DIC OM

M-A

Page 17: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

J 2405-1-02

Page 18: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

J 2405-1-02

5.2

94.8

gamma alpha

111 002 022

XRD – retained austenite

Page 19: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

J2487 -1-02

OM-DIC OM

Page 20: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

J2487 -1-02

Page 21: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

J2487 -1-02

111 002 022

4.9

95.1

gamma alpha

Retained Austenite

Page 22: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

J 2405 -1-03

OM-DIC OM

Page 23: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

J 2405 -1-03

111 002 022

2.7

97.3

gamma alpha

Retained Austenite

Page 24: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Ellwood 4340

Page 25: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Company A- 4340

No retained Austenite detected by XRD Small peak at 111 and 002 but no peak at 022

111 002 022

Page 26: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

J 2499 4 02

OM-DIC OM

Page 27: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

J 2499 4 02

Page 28: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

J 2499 4 02

111 002 022

7.2

92.8

gamma alpha

113

Retained Austenite

Page 29: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

J 2499 3 02

OM-DIC OM

Page 30: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

J 2499 3 02

Page 31: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

J 2499 3 02

No retained Austenite detected by XRD Small peak at 111 but no peak at 002 and 022

111 002 022

Page 32: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

30 40 50 60 70 80 90 100 1102Theta (°)

0

100

200

300

400

500

600

Inte

nsity (

counts

)

30 40 50 60 70 80 90 100 1102Theta (°)

0

200

400

600

Inte

nsity (

counts

)

50 60 70 80 90 100 1102Theta (°)

0

200

400

600

800

Inte

nsity (

counts

)

50 60 70 80 90 100 1102Theta (°)

0

100

200

300

400

500

Inte

nsity (

counts

)

50 60 70 80 90 100 1102Theta (°)

0

100

200

300

400

500

600

Inte

nsity (

counts

)

30 40 50 60 70 80 90 100 1102Theta (°)

0

200

400

600

800

Inte

nsity (

counts

)

50 60 70 80 90 100 1102Theta (°)

0

100

200

300

400

500

Inte

nsity (

counts

)

50 60 70 80 90 100 1102Theta (°)

0

200

400

600

800

Inte

nsity (

counts

)

50 60 70 80 90 100 1102Theta (°)

0

200

400

600

Inte

nsity (

counts

)

50 60 70 80 90 100 1102Theta (°)

0

100

200

300

400

500

Inte

nsity (

counts

)

50 60 70 80 90 100 1102Theta (°)

0

100

200

300

400

500

600Inte

nsity (

counts

)50 60 70 80 90 100 110

2Theta (°)

0

100

200

300

400

500

Inte

nsity (

counts

)

50 60 70 80 90 100 1102Theta (°)

0

200

400

600

800

1000

Inte

nsity (

counts

)

50 60 70 80 90 100 1102Theta (°)

0

100

200

300

400

500

600

Inte

nsity (

counts

)

50 60 70 80 90 100 1102Theta (°)

0

100

200

300

400

500

600

Inte

nsity (

counts

)

50 60 70 80 90 100 1102Theta (°)

0

200

400

600

800

1000

Inte

nsity (

counts

)

50 60 70 80 90 100 1102Theta (°)

0

200

400

600

800

1000

1200

Inte

nsity (

counts

)

30 40 50 60 70 80 90 100 1102Theta (°)

0

500

1000

1500

Inte

nsity (

counts

)

1,2 1,1 1,3 1,4 1,5 1,6

2,2 2,1 2,3 2,4 2,5 2,6

3,2 3,1 3,3 3,4 3,5 3,6

1,6

2,6

31,6

1,5

2,5

3,5

1,4

2,4

3,4

1,3

2,3

3,3

1,2

2,2

3,2

1,1

2,1

3,1

3.12%

3.09%

3.1%

0% 0% 0%

0%

0%

0%

2.97%

3.2%

3.0% 3.6% 0% 0%

0% 0%

2.98%

Sample Core

Using XRD a section from the sample B 1 4340 was analyzed in different locations from the surface to the center location. The objective was look for Gamma phase (Retained Austenite).

Bo

tto

m a

cco

rdin

g th

e U

T Sc

an

Page 33: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

50 60 70 80 90 100 1102Theta (°)

0

100

200

300

400

500

Inte

nsity (

counts

)Using XRD a section from the sample B -1-02 was analyzed in different points at the surface of one of the faces.

3.12%

3.09%

3.1%

0% 0% 0%

0%

0%

0%

2.97%

3.2%

3.0% 3.6%

0% 0%

0% 0%

2.98% 1,6

2,6

3,6

1,5

2,5

3,5

1,4

2,4

3,4

1,3

2,3

3,3

1,2

2,2

3,2

1,1

2,1

3,1

50 60 70 80 90 100 1102Theta (°)

0

200

400

600

800

1000

Inte

nsity (

counts

)

111 3,1

111 2,1

50 60 70 80 90 100 1102Theta (°)

0

100

200

300

400

500

600

Inte

nsity (

counts

)

1,1

111

50 60 70 80 90 100 1102Theta (°)

0

100

200

300

400

500

600Inte

nsity (

counts

)

111 3,2

Page 34: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

4340 Retained Austenite

Sample A AC B1 B2 B3 C1 C2

XRD Retained Austenite

0% 0% 4.9% 4% 5% 0% 0%

8630 Retained Austenite

Sample A AC B1 B2 B3

XRD Retained Austenite

0% 0% 3.1% 7.1% 0%

Summary of Retained Austenite Measurements

Page 35: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Advanced Characterization EBSD Analysis – IQ-Phase Balance and

Retained Austenite

Page 36: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Introduction

And Different microconstituents have different

dominant strengthening mechanisms

So we need... Clear identification and quantification of microconstituents

to understand, control, model and predict chemistry-processing-

microstructure-mechanical property relations!!

As we know... Steels may have multiphase and

complex microstructures.

Page 37: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Basic Assumptions for EBSD IQ Analysis

Different forms of ferrite (polygonal, non-polygonal, acicular, bainitic, martensitic) differ mainly in lattice distortion due to dislocations and solute interstitials, mainly carbon.

Page 38: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

What is EBSD-IQ?

SEM - FEG

Secondary e-

Back Scattered e-

{hkl}<uvw> GB Misorientation Image Quality

Page 39: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Line Broadening caused by dislocations in

Debye-Scherrer Diff. Pattern

Inte

ns

ity

(HKL)

ρ↑

ρ↓

Page 40: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

What is IQ?

The image quality parameter, IQ, describes the quality of an electron

backscatter diffraction pattern.

Internal Strain ε ~ 0

Internal Strain ε > 0

hkl

IIQ )( max ))((max KikuchiII pix

High Kikuchi band intensity

Low Kikuchi band intensity

High Image Quality

Low Image Quality

Page 41: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Fre

qu

en

cy o

r A

mo

un

t, V

f

Image Quality or Inverse Lattice Distortion

High

Distortion

Low IQ

(Bainite)

Low Distortion

High IQ

(Polygonal ferrite)

Output from EBSD-IQ Multi-peak Model

Page 42: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

The Hardness of Martensite in Dual-Phase Steels Used in the Automotive

Industry

By: Mark Iaboni

Joe Quinn*

Will Weissberg

Project Advisor: Prof. C. I. Garcia

MARTENSITE

FERRITE

Page 43: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Peak (IQ) Vol. % Phase

81.2 57.3 Polygonal Ferrite

57.1 18.2 Non-Rxn Ferrite

34.6 22.1 Martensite

23.2 2.4 Retained Austenite

0

0.05

0.1

0.15

0.2

0.25

0.3

0 10 20 30 40 50 60 70 80 90 100 110

IQ

Fre

qu

en

cy

EBSD Data without GB Contribution

Polygonal Ferrite

Non-Rxn Ferrite

Martensite

Retained Austenite

Sum of all simulated contributions

BDP-790

Phase Identification of DP-780 Steels based on EBSD-IQ Multiphase Analysis

Page 44: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Retained Austenite 0.8%

IQ IPF

Phases

Company A 4340

Page 45: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

EBSD Analysis over the company A 4340 sample and the amount of retained austenite obtained using this technique.

Iron Gama 0.008 Iron Alpha 0.992

Phase Total Fraction

Iron Gamma = Retained Austenite

Company A 4340

Page 46: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

43.40% - Tempered Martensite

56.60% - Martensite 0

5

10

15

20

25

0 10 20 30 40 50 60 70 80 90 100 110

Fre

qu

en

cy

IQ

EBSD Data withoutGB ContributionTempered Martensite

Sum of all simulatedcontributionsMartensite

Company A 4340

EBSD - IQ

Page 47: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Company B 4340

Retained Austenite 4.4%

Page 48: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

EBSD Analysis over the company B 4340 sample and the amount of retained austenite obtained using this technique.

Iron Gama 0.044 Iron Alpha 0.956

Phase Total Fraction

Iron Gamma = Retained Austenite

Company B 4340

Page 49: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

0

2

4

6

8

10

12

0 10 20 30 40 50 60 70 80 90 100 110

Fre

qu

en

cy

IQ

EBSD Datawithout GBContribution

Proeutectoideferrite

Non polygonalferrite

Sum of allsimulatedcontributions

Carbon richconstituyent

41.77% - Non Polygonl Ferrite

9.32% - Proeutectoide Ferrite

48.9% - Carbon rich constituyents

Company B 4340

Page 50: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Retained Austenite 2.6%

J 2499 4 02

IQ IPF

Phases

Page 51: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Iron Gama 0.026 Iron Alpha 0.974

Phase Total Fraction

EBSD Analysis over the company B 8630 sample and the amount of retained Austenite obtained using this technique.

Iron Gamma = Retained Austenite

Page 52: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

0

5

10

15

20

25

30

0 10 20 30 40 50 60 70 80 90 100 110

Fre

qu

en

cy

IQ

EBSD Data withoutGB ContributionFerrite

Sum of all simulatedcontributionsCarbon Rich

26.75% - Ferrite

73.25% - Carbon Rich Constituyents

Company B 8630

Page 53: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Advanced Characterization Hyper-Probe Analysis WDS

Page 54: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

SEM WDS

JEOL JXA-8530F (FEG) "Hyperprobe" electron probe microanalyzer (EPMA-electron microprobe )

Page 55: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical
Page 56: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Company B4340 Quantitative Chemical Analysis Using SEM WDS

No. C Si Mn Cr Ni P S

1 0.19 0.19 0.62 0.88 0.14 0 -0.02

2 0.89 0.29 5.42 1.51 0.09 0.02 17.85

3 0.84 0.3 0.94 1.08 0.2 0.02 0.14

4 0.34 0.26 0.9 1.05 0.12 0.02 0.09

5 0.54 0.26 0.79 0.91 0.09 0.01 0.11

6 0.43 0.29 0.8 1.16 0.16 0.02 0.11

Minimum 0.19 0.19 0.62 0.88 0.09 0 -0.02

Maximum 0.89 0.3 5.42 1.51 0.2 0.02 17.85

Average 0.54 0.27 1.58 1.1 0.13 0.01 3.05

Sigma 0.28 0.04 1.89 0.23 0.04 0.01 7.25

Page 57: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Company B4340 Quantitative Chemical Analysis Using SEM WDS

No. C Si Mn Cr Ni P S

1 0.19 0.19 0.62 0.88 1.14 0 -0.02

2 0.89 0.29 5.42 1.51 1.09 0.02 17.85

3 0.84 0.3 0.94 1.08 1.2 0.02 0.14

4 0.34 0.26 0.9 1.05 1.12 0.02 0.09

5 0.54 0.26 0.79 0.91 1.09 0.01 0.11

6 0.43 0.29 0.8 1.16 1.16 0.02 0.11

AVG 0.54 0.27 1.58 1.1 1.13 .01 3.05

Bulk 0.42 0.28 0.78 0.86 1.68 0.007 0.002

0

0.2

0.4

0.6

0.8

1

0 1 2 3 4 5 6 7

0.16

0.21

0.26

0.31

0 1 2 3 4 5 6 7

C

Si

0

1

2

3

4

5

6

0 1 2 3 4 5 6 7

Mn

0.6

0.8

1

1.2

1.4

1.6

0 1 2 3 4 5 6 7

Cr

Page 58: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Company B4340 TTT Diagram Bulk composition (continous line) vs Local Composition AVG (pointed line)

Page 59: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

No. C Si Mn Cr Ni P S

1 0.55 0.31 0.78 1.2 0.14 0.01 -0.02

2 0.48 0.28 0.91 1.18 0.11 0.01 0.03

3 0.47 0.31 0.86 1.24 0.12 -0.01 0.01

4 0.81 0.3 0.96 1.28 0.15 0.02 0.02

5 0.75 0.29 0.93 1.2 0.11 0.04 0.03

6 0.32 0.34 0.91 1.31 0.16 0.03 0.09

7 0.49 0.3 0.94 1.21 0.15 0.04 0.06

Minimum 0.32 0.28 0.78 1.18 0.11 -0.01 -0.02

Maximum 0.81 0.34 0.96 1.31 0.16 0.04 0.09

Average 0.55 0.3 0.9 1.23 0.13 0.02 0.03

Sigma 0.17 0.02 0.06 0.05 0.02 0.02 0.04

Company A8630 Quantitative Chemical Analysis Using SEM WDS

Page 60: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

No. C Si Mn Cr Ni P S

1 0.55 0.31 0.78 1.2 1.74 0.01 -0.02

2 0.48 0.28 0.91 1.18 1.71 0.01 0.03

3 0.47 0.31 0.86 1.24 1.72 -0.01 0.01

4 0.81 0.3 0.96 1.28 1.75 0.02 0.02

5 0.75 0.29 0.93 1.2 1.71 0.04 0.03

6 0.32 0.34 0.91 1.31 1.76 0.03 0.09

7 0.49 0.3 0.94 1.21 1.75 0.04 0.06

AVG 0.55 0.3 0.9 1.23 1.73 0.02 0.03

Bulk 0.30 0.35 0.96 1.1 1.74 0.008 0.01

Company A8630 Quantitative Chemical Analysis Using SEM WDS

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

0 1 2 3 4 5 6 7 8

0.25

0.27

0.29

0.31

0.33

0.35

0.37

0 1 2 3 4 5 6 7 8

C

Si

0.7

0.75

0.8

0.85

0.9

0.95

1

0 1 2 3 4 5 6 7 8

0.7

0.8

0.9

1

1.1

1.2

1.3

1.4

0 1 2 3 4 5 6 7 8

Mn

Cr

Page 61: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Company A8630 TTT and CCT Diagrams Bulk composition (continous line) vs Local Composition AVG (pointed line)

Page 62: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Future Work

o Complete Hyper-Probe Analysis o EBSD-IQ Phase Identification o FEA – CCT microstructural prediction

Page 63: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

J2405-1-02 (4340) Microstructure

Page 64: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

J2405-1-02 (4340) Microstructure

Page 65: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

J2499-3-02 (8630) Microstructure

Page 66: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

J2499-3-02 (8630) Microstructure

Page 67: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

J2405-1-02 (4340) Microstructure

Page 68: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

J2499-3-02 (8630) Microstructure

Page 69: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Cooling Procedure Simulation is based on FEA Software ANSYS

Page 70: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Company A 4340&8630 As Received Dimension Size (inch)

Center

Quarter

Surface

Page 71: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

A4340 Dimensions:4”X4”X5” Air-Cooled

Page 72: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

A4340 Dimensions:4”X4”X5” Oil-Quenched

Page 73: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

A8630 Dimensions:4”X4”X5” Air-Cooled

Page 74: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

A8630 Dimensions:4”X4”X5” Oil-Quenched

Page 75: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

A4340 – Microstructures Based on FEA and Jmat-Pro Predictions

Size 4”X4”X5” 20”X20”X20”

Surface QR CTR Surface QR CTR

Air-Cooled

Bainite Pearlite

Bainite Pearlite

Bainite Pearlite

Bainite Pearlite

Bainite Pearlite

Bainite Pearlite

Oil-Q Martensite Bainite

Bainite, Martensite

Bainite, Martensite

Martensite Bainite

Bainite Martensite

Bainite, Martensite

Water-Q Martensite Bainite, Martensite

Bainite, Martensite

Martensite Bainite, Martensite

Bainite, Martensite

Page 76: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

A8630- Microstructures Based on FEA and JMat-Pro Predictions

Size 4”X4”X5” 20”X20”X20”

Surface QR CTR Surface QR CTR

Air-Cooled Bainite Pearlite Ferrite

Bainite Pearlite Ferrite

Bainite Pearlite Ferrite

Bainite Pearlite Ferrite

Bainite Pearlite Ferrite

Bainite Pearlite Ferrite

OQ Martensite Bainite

Bainite Martensite

Bainite, Martensite

Martensite Bainite

Bainite Pearlite Ferrite

Bainite Pearlite Ferrite

WQ Martensite Bainite, Martensite

Bainite, Martensite

Martensite Bainite Pearlite Ferrite

Bainite Pearlite Ferrite

Page 77: Compositional and Structural Factors that Influence ... · Induced Cracking and Hydrogen Flaking in Steels Allan Arenas, Cai Shuai and Shiyi Li Advisor: C. Isaac Garcia Ferrous Physical

Thank you!