EXPERIMENTAL PROCEDURE

EXPERIMENTAL PROCEDURE AND CHARACTERIZATION TECHNIQUES

EXPERIMENTAL PROCEDURE

A) THERMO-MECHANICAL SIMULATOR: Gleeble 3800 was used for thermo-

mechanically simulation the dynamic recrystallization under hot compression. A
cylindrical sample of 15×10mm diameter was used to perform the study. To
measure the temperature simultaneously during the deformation a thermocouple
was attached at the center of the specimen. The Thermo-Mechanical cycle
includes heating the material to 700,800 and 850 0C at 50C/s, holding for 5min
and 50% deformation was carried out at a strain rate of 0.01/s and quenched using
water. For 8000C deformation the strain rates were varied which include 0.1 and
0.001/s. In order to study the microstructural evolution at various stage of the
deformation the samples where quenched after 30, 40, 50 and 60% deformation

0
a 3-913 C
900
0 0
a 1-883 C 850 C
0
800 800 C
0
700 700 C
5m in
600
Tem perature C
0

500

400 
5 C /s
0 Q uenching
300

200

100

0
0 2 4 6 8 10
T im e (m in)

Fig.24: TMS cycle for 0.01/s strain rate at three different temperatures

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 EXPERIMENTAL PROCEDURE

5 m in
800

600
Tem perature C
0

0
5 C /s
400
  
 s  s  /s

200

Q uenching

0
0 5 10 15 20

T im e(m in)

Fig.25: TMS cycle at 8000C at three different strain rates

800
5m in

40%
600
Tem perature C

30% 60%
0

0
400 5 C /s

50%

200
Q uenching

0
0 2 4 6 8 10

Tim e (m in)

Fig.26: TMS cycle to study the microstructural evolution at 8000C -0.01/s strain rate.

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 EXPERIMENTAL PROCEDURE

CHARACTERISATION TECHNIQUES

A) OPTICAL EMISSION SPECTROSCOPY: Optical emission spectrometer gives

the elemental composition of a metal. The sample dimension required for OES is
15×15×5mm.Optical emission spectroscopy showed the following elements (wt.
%) in the Interstial free steel obtained from TATA STEEL C-0.005, Si-
0.0075, Mn-0.504, P-0.009, S-0.0012, Cr0.0260, Mo-0.00264, Ni-0.0175, Al-
0.0512, Nb-0.0174, Ti-0.0446, Co-0.002.
B) OPTICAL MICROSCOPY: Optical light microscopy was used to study the
microstructure of hot compressed samples. The hot compressed samples were cut
using a diamond cutter along the longitudinal direction of application of force.
The specimens were polished using SiC emery paper from
300/600/800/1200/1500/2000 grit size, and final cloth polishing was done using
alumina. 2% NITAL was used to etch the specimen.
C) XRAY DIFFRACTOMETRY: X-Ray Diffractometry of the emery and cloth
polished samples were carried out at a very slow scan rate of 20/min using
(Rigaku). The sample dimension used for the analysis was 8×5×3mm rectangular
sample.
D) VICKERS HARDNESS: Hardness of the deformed samples was carried out using
Vickers hardness tester at 5kg load and a dwell time of 12s.
E) THERMAL ANALYSIS: Differential scanning calorimetry study of a 60%
deformed sample was done to determine the approximate static recrystallization
and recovery temperature at a scan rate of 100C/min till 10000C.

SIMULATION:

A) FINITE ELEMENT ANALYSIS: FEA was done on IF steels with NbC, TiC,
TiN, and MnS precipitate to find the effect of size, shape and strain rate on the stress
concentration around the precipitate which is directly related to the dislocation
generation. The shapes of the precipitates for modeling were taken form experimental
results in [5]. The sample dimension was taken to be 15×10mm and the precipitate

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 EXPERIMENTAL PROCEDURE

dimension was 1mm side for square, 1mm diameter for circle and 1mm major axis for
ellipse. To study the precipitate size effect the size difference was 0.5mm and 1 mm
respectively. We adopt a unit cell model to investigate the effect of particle shape and
stress concentration on the mechanical behavior of the IF steel and its precipitates using
Student edition of Abaqus (6.12). Both particles and matrix are meshed by the four node
isoparametric elements (CPS4).

Assumptions

1. Material is homogenous
2. Material is isotropic
3. No adiabatic heat generation
4. The deformation is carried out at steady state temperature
5. No friction between the ramp and work piece
6. The bonding between the particles and the matrix is assumed to be perfect in the
analysis
7. The matrix is devoid of porosity

The material properties for IF steel were taken from the stress strain graph obtained under
compression test. For IF steel the youngs modulus was 200GPa and the poison ration is
0.3[35].

Table.3: Physical properties of the precipitates

Precipitate E (GPa) Density Poisson Reference

ratio
MnS 138 4 0.3 [34]
TiN 317 4.9 0.19 [36]
NbC 488 7.16 0.22 [37]
TiC 440 5.4 0.189 [36]

B) THERMO-CALC software [tcfe7 database] was used to draw the equilibrium

phase diagram and also the volume fraction of the precipitates for the composition
of steel obtained using optical emission spectrometry

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