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Applied Mechanics and Materials Vol.

493 (2014) pp 721-726


Online available since 2014/Jan/08 at www.scientific.net
(2014) Trans Tech Publications, Switzerland
doi:10.4028/www.scientific.net/AMM.493.721

Effect of intercritical annealing temperature and holding time on


microstructure and mechanical properties of dual phase low carbon
steel
ALFIRANO1, a, SAMDAN Wibawa1, b, MAULUD Hidayat2, c
1

Department of Metallurgy Engineering, University of Sultan Ageng Tirtayasa, Cilegon, Indonesia


2

Division of Applied Research, PT. Krakatau Steel, Cilegon, Indonesia

alfirano@ft-untirta.ac.id, bsamdanwibawa@rocketmail.com, cmaulud.hidayat@krakatausteel.com

Keywords: Dual phase steel, martensite, ferrite, intercritical annealing, quenching, K, n

Abstract. Dual phase steels are an important advanced high strength steel, which have been widely
used in the automotive industry for vehicle components requiring light weight and safety. In this
study, the formation of dual phase structure with various volume fraction of martensite in a low
carbon steel SS400 during intercritical annealing were investigated. It was found that intercritical
annealing temperature and holding time affected the microstructure and mechanical properties of
dual phase low carbon steel. The specimens were heated at intercritical annealing temperature of
750oC, 775oC, 800oC and 825oC, for holding periods of 6-18 minutes, followed by water quenching
in order to get a dual phase ferrite and martensite. After quenching, it was obtained the optimal
annealing conditions at 800oC with a holding periods of 10 minutes. In this condition, the tensile
strength was increased up to 621 N/mm2 or 39.24% higher than the initial condition, while the
elongation decreased up to 13.8%. The hardness of specimens increased from 127.7 to 235.83 HVN
or up to 84.67% higher than the initial condition. Meanwhile the volume fraction of martensite was
24.08%. The higher the temperature of the heating value of grain growth rate constant (K)
increases. In addition, at the optimal poin, the value of K (grain growth rate constant) and n
(Avramis exponent) were 0.263 and 0.318, respectively, with activation energy (Q) of 3.98 J/mol.
Introduction
In order to decrease the energy consumption in automotive industry, optimization of well-known
materials and developing new materials with a high ratio of strength to density and a good
suitability for metal forming operation are still progressed [1, 2]. Dual phase steels are one of the
important steel products developed for the automotive industry, in which steel grade exhibiting high
strength and good formability is required so that weight of vehicle can be reduced for fuel saving
purpose. The pure dual phase microstructure consists of a matrix of soft a -ferrite grains,
strengthened by a finely dispersed, hard MA (MartensiteAustenite) constituent [3]. Thus, dual
phase steels have characteristic mechanical properties which include low yield strength and high
ultimate tensile strength as compared with conventional low-carbon steel [3]. The steel obtains its
specific properties from the low temperature transformation of intercritical austenite to lath-type
martensite. This transformation results in a non-uniform dislocation distribution and internal
stresses. The austenite, enriched in carbon during the processing, may not transform entirely into
martensite, resulting in the presence of small amounts of retained austenite. The amount of retained
austenite depends among others, on the hardenability of the transforming austenitic phase and the
size of the austenitic particles [4].
However, the combination of a good strength and ductility can be obtained by developing a dual
phase or multiphase steels through the heat treatment process. In this study, the microstructural
change in low carbon steel during intercritical annealing has been investigated with a focus on the
formation of dual phase structure with various volume fraction of martensite.

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Advances in Applied Mechanics and Materials

Experimental procedure
The chemical composition of the low carbon steel used in this study are shown in Table 1.
Table 1. Chemical composition of steel used in this study, wt%
C
0,1602
Al
0,0377
W
0,0041

Si
0,0078
V
0,0009
Ca
0,0010

Mn
0,6229
As
0,0017
Pb
0,0003

P
0,0086
N
0,0044
Sb
0,0041

S
0,0089
Mo
0,0023
Fe
<99,09

Cu
0,0153
Ti
0,0007
Co
0,0023

Ni
0,0133
Cr
0,0123
Sn
0,0025

Intercritical annealing was tested on tensile test sample with standard JIS Z 2201 test piece no 5.
The intercritical annealing temperatur behind A1 and A3.
A1 = 723 16,9 Ni + 29,1 Si 20,7 Mn - 16,9 Cr 11,5oC

(1)

A3 = 910 203 + 44,7 Si 15,2 Ni + 31,5 Mo + 104 V 16,7oC

(2)

Then, it was found that A1=710,32oC 11,5oC and A3=872 16,7oC. The specimens were heated at
intercritical annealing temperature of 750oC, 775oC, 800oC and 825oC, for holding periods of 6-18
minutes, followed by water quenching. For mechanical properties, the samples were cut in to two
parts. Parts one for tensile test and part two for hardness test. For tensile test sample with standard
JIS Z 2201 test piece no 5. A cross head speed of 10 mm/min was maintained upto the yield point
and, thereafter speed of 50 mm/min was maintained upto fracture. The strain to necking in each
specimen was recorded using an ektensometer. From the tensile test the yield strength, ultimate
tensile strength and % elongation were measured. For hardness test used macro vickers
hardness.The microstructures of samples were studied by optical microscopy. Martensite volume
fraction was measured by point counting method based on ASTM E562-83 standard.
Result and discussion
The microstructure of specimens before and after heat treatment is shown in Fig. 1. The
specimens before heat treatment were consisted of pearlite and ferrite phases (Fig. 1(a)).
Microstructures formed after the quenching were formed ferrite and martensite phase, which can be
seen in Fig. 1(b). Martensite was formed when the steel material is cooled rapidly from the
austenitic region.

Figure 1. Microstructure of specimens (a) before heat treatment and (b) after heat treatment at 775
o
C for 15 minutes, water quenched.

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Figure 2. Effect of heating time on (a) volume fraction of martensite and (b) hardness of specimens
heated at various temperature.
The effect of heating time on volume fraction of martensite at various temperature are shown in
Fig. 2(a). Volume fraction of martensite increases with increasing heating time. It shows that the
higher in heating temperature and the longer in holding time, it will produce more martensite. In the
A1 temperature austenite began to transform by eutectoid reaction into ferrite, cementite and
pearlite. If the temperature is increased above the A1 then carbon can dissolve into austenite, so that
the carbon was contained on ferrite gradually dissolved into the austenite. Because not only the
austenite formed from pearlite, but also the dissolution of ferrite [5]. Holding timeduring the heating
process aims to provide an opportunity for atoms to diffuse in austenite [6]. Austenite phase is
unstable if the steel is cooled rapidly from the austenitic region which has a fcc structure, therefore
the bcc structure will not formed because of the time which needed to complete the transformation
into bcc is not enough. Austenite has a higher carbon content than ferrite should remove carbon
from the solution, but due to the rapid cooling, carbon was trapped, so that bct structure or so-called
martensite was formed [7].
The hardness value of specimens can be seen on Fig. 2(b). The hardness value of the specimen
before heat treatment was 127.7 HVN. Heating was performed on the ferrite and austenite region.
Increased in hardness occurs caused by increasing in the volume fraction of martensite. The
difference of cooling rate between specimens before and after heat treatment can cause the
difference in phases; ferrite-pearlite and ferrite-martensite, respectively. In low carbon steel, ferrite
and pearlite usually were formed together and its hardness is determined by the carbon content, so
the hardness of low carbon steel will be affected by ferrite and pearlite content. While the
specimens were cooled in the quenched medium, generated the final structure of ferrite and
martensite, where the carbon content in the martensite is saturated. In can be cause increasing in
hardness value. Increasing heating temperature will increase the cooling rate so that martensite
easily formed. Increase in martensite volume led to the increasing of hardness value [4].
The effect of heating time on elongation at various temperatures is shown in Figure 3. The
volume fraction of martensite increases with increasing heating temperature and holding time, while
the volume fraction of ferrite decreases with increasing heating temperature and holding time.
Decrease in the volume fraction of ferrite and increase in volume fraction of martensite cause the
decrease of elongation, because the nature of the hard martensite and ferrite gertas increased while
that is resilient reduced [8,9]. Despite the decrease in elongation, the dual-phase ferrite-martensite
steels with a microstructure which is easily formed because it consists of a fixed and martensite
phase in a soft ferrite matrix [10]. The increase in temperature will increase cooling rate resulting a
decrease in strain. Decrease in strain can occur due to two factors, such as the residual stress during
the transformation of austenite to martensite during cooling and dislocations increases with
increasing volume of martensite [4].

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Advances in Applied Mechanics and Materials

Figure 3. Effect of heating time on elongation at various temperatures.

Figure 4. The effect of martensite volume fraction on tensile strength.


The effect of martensite volume fraction on tensile strength is shown in Fig. 4. At 750oC, tensile
strength shows the fluctuation value. This fluctuation of tensile strength can be caused by a
difference in the dimensions of the sample when cooled rapidly [11]. The presence of pearlite phase
is likely a lot compared to other heating temperature and the amount of pearlite volume fraction at a
temperature of 750oC heating at various times of fluctuating resistance values indicate fluctuating
tensile strength. In addition, the pearlite phase formed at temperatures of 750oC has a large grain
size. It is generally known steel with a large grain size will have low power [7].
At 775o C, increase in the volume fraction of martensite, it will improve the value of tensile
strength [9]. When compared to the initial material before intercritical annealing and quenching
process, where tensile strength was 446 N/mm2. Surely there is a very significant increase in tensile
strength including the volume fraction of martensite. This could be due to the structure of the soft
ferrite and hard martensite dual phase steel resulting in a strong and resilient. The main source of
strength dual-phase steel is located in the martensite microstructure acts as a strong and able to load
carrying constituent in the soft ferrite matrix. If the steel is supplied load voltages then there will be
propagated to the strong particle with the interfacial shear matrix [8]. Dual phase steel also has a
high rate of work hardening due to dislocation density resulting in high tensile strength [12].
Presence of dislocation density may impede the movement of other dislocations, due to the
constraints that the energy stored in the material to be increased so that the material becomes harder
and stronger.
At 825oC, the higher of volume fraction of martensite will lower the tensile strength. Tensile
strength values decrease because of the increase in the volume fraction of martensite beyond the
optimum value, where the nature of the hard martensite phase brittle causing atomic defects when
martensite formation that is the source of the rift. Because of the reduced ferrite will reduce bonding
between phases, then tensile strength values also decrease. According Smallman martensitic
structure optimum proportion of 20% [13]. Dual phase steel ferrite-martensite has martensite
volume ranged from 20% to 30% in the ferrite matrix including the advanced high strength stainless
steel (AHSS) making it suitable for applications in the automotive sector [14].

Applied Mechanics and Materials Vol. 493

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Kinetics of formation of austenite during the heating process at the point of intercritical
annealing has long been studied. This shows the kinetics of formation of austenite formation of
austenite in dual phase steel is diffusion control growth. Johnson-Mehl-Avrami equation (JMA)
with kolomogrov (JMAK) can be used for transformation of austenite during intercritical annealing.
The equation is as follows [7]:
f

= 1 exp (-Ktn)

(3)

By using the modified JMA equation, where a large volume of austenite is limited, then the
following equation:
ln [ln (1/(1- )] = n ln t + ln K

(4)

the austenite volume, f, can be considered to the volume of martensite. fe is an austenite volume at
equilibrium, the value can be found using the level rule Fe3C diagram. t is the holding time on
heating at the point of intercritical annealing. K is a constant growth rate of austenite, n is the
Avrami exponent. Through a modified JMA equation then can be searched value grain growth rate
constant (K) and the value of Avrami exponent (n) is obtained from the slope and intercept resulting
from linear equation relationship between ln [ln (1 / (1 - f / fe) ] versus ln t (Fig. 5). Using the data
from experiment (Fig. 5), the n and K value can be determined, as listed in Table 2.
Rate constant (K) is a parameter that depends on the temperature and velocity associated with
grain growth, nucleation frequency. So the higher the heating temperature intercritical annealing
point it will increase the value of K vice versa. While the Avrami exponent (n) depends on the
nucleation and growth processes and the grain nucleation rate has a significant effect on the value of
n [7].

Figure 5. The relationship between ln [ln (1 / (1 - f / fe) ] and ln t from experiment.


Table 2. n and K value from experimental data in various temperature.
Temperature
(oC)
750
775
800
825

Equilibrium volume
fraction of austenit,fe
0,2373
0,3494
0,5357
0,7635

Avramis
exponent (n)
0,409
0,266
0,279
0,318

Rate
constant (K)
0,072.
0,191
0,263
0,318

From data grain growth rate constant (K) can be searched through the magnitude of the
activation energy Arrhenius equation:
ln K = ln A (

(5)

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Advances in Applied Mechanics and Materials

Through the Arrhenius equation can be determined the value of activation energy (Q) and constant
(A) is obtained from the slope and intercept resulting from linear equation between ln K and 1/T.
From this relationship, activation energy (Q) and constant (A) will be 3,98 J/mol and 0,606,
respectively.
Summary
1. Dual phase steel shows an excellent combination between strength and ductility due to the
coexistence of harder (martensite) and softer (ferrite) phase in their microstructure.
2. The hardness, tensile strength and martensite volume increase with increasing heating
temperature and holding time. At the optimum point, the value of hardness, tensile strength and
martensite volume were 235.83 HVN (higher 84.67% than the initial value), 621 N/mm2, and
24,08 %, respectively. In the other hand, elongation decrease until 13.8% at the optimum poin.
3. At the optimum point, K and n value was 0.263 and 0.318, respectively with activation energy
(Q) of 3.98 J/mol.
References
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designs in steels, Semina, 2005.
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Advances in Applied Mechanics and Materials


10.4028/www.scientific.net/AMM.493

Effect of Intercritical Annealing Temperature and Holding Time on Microstructure and Mechanical
Properties of Dual Phase Low Carbon Steel
10.4028/www.scientific.net/AMM.493.721
DOI References
[13] A. Murugaiyan et al., Phase Transformations in Two C-Mn-Si-Cr Dual Phase Steels, ISIJ International.
46 (2006), 1489-1494.
http://dx.doi.org/10.2355/isijinternational.46.1489