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Materials Science and Engineering A 534 (2012) 465475

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Materials Science and Engineering A


journal homepage: www.elsevier.com/locate/msea

Microstructural modications and changes in mechanical properties during


cyclic heat treatment of 0.16% carbon steel
Atanu Saha a , Dipak Kumar Mondal b , Koushik Biswas c , Joydeep Maity b,
a
b
c

NDT and Metallurgy Group, Central Mechanical Engineering Research Institute, Durgapur 713209, West Bengal, India
Department of Metallurgical and Materials Engineering, National Institute of Technology Durgapur, Durgapur 713209, West Bengal, India
Department of Metallurgical and Materials Engineering, Indian Institute of Technology, Kharagpur 721302, West Bengal, India

a r t i c l e

i n f o

Article history:
Received 10 October 2011
Received in revised form
15 November 2011
Accepted 26 November 2011
Available online 8 December 2011
Keywords:
Low carbon steel
Cyclic heat treatment
Grain renement
Dislocation generation
Grain boundary diffusion
Divorced eutectoidal reaction
Cementite network

a b s t r a c t
In this work an annealed 0.16 wt% carbon steel was subjected to cyclic heat treatment process that consisted of repeated short-duration (6 min) holding at 910 C (above Ac3 temperature) followed by forced air
cooling. A typical microstructural development, not so common for low carbon hypoeutectoid steel, was
observed. The main features involved were: (i) a substantial grain renement (mainly at initial stage), (ii)
generation of dislocations (at initial stage) and its annihilation (at later stage) and (iii) generation of grain
boundary network of cementite and cementite cluster owing to divorced eutectoidal reaction. In low carbon steel, the presence of large proportion of grain boundary areas promoted grain boundary diffusion
of carbon during short-duration holding. This phenomenon nally led to the generation of grain boundary cementite network and cluster through divorced eutectoidal reaction. Unlike high carbon steel, the
contribution of divorced eutectoidal reaction to spheroidization was not so signicant. For higher cycles
(58 cycles) substantial presence of grain boundary cementite and cementite cluster deteriorated the
strength property. However, quite a high strength (UTS = 455 MPa) was achieved for this low carbon steel
with two cycles of heat treatment due to ne ferrite grain size, high dislocation density and adequate
proportion of ne lamellar pearlite in the microstructure.
2011 Elsevier B.V. All rights reserved.

1. Introduction
The various noble microstructural changes and their effects
on process kinetics and material properties have established the
potential of cyclic (repeated) heat treatment techniques in recent
years. Out of a few investigations carried out so far, the cyclic
austempering process was found to accelerate bainitic transformation in 1080 steel [1]. On the other hand, an accelerated grain
growth was observed in AlK-grade steel (0.05% C, 0.05% Al and
45 ppm N) using a cyclic annealing process [2]. In these investigations, the non-equilibrium temperature reversal effect is explained
as the prime factor to cause excitation (energy increase) of atoms,
thereby reducing the activation energy so as to enhance the process
kinetics. Apart from this basic hypothesis, in true sense, the defect
generation during cyclic heat treatment (that would raise the system energy and lower down the activation energy) and its effects
on microstructural evolution were not studied in details. The thermal cycling (swinging annealing) of 5 C around Ac1 temperature
was known to accelerate spheroidization process in medium and
high carbon steels [3]. In a recent investigation, a typical cyclic heat

Corresponding author. Tel.: +91 343 2754733; fax: +91 343 2547375.
E-mail address: joydeep maity@yahoo.co.in (J. Maity).
0921-5093/$ see front matter 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2011.11.095

treatment process adopted by the present authors [4] involving


repeated short duration holding above Ac3 temperature followed
by forced air cooling has accelerated the spheroidization process to
a greater extent in 0.6 wt% C steel. The lamellar disintegration led
to spheroidized cementite generation. After 8 cycles of heat treatment a good combination of strength and ductility was obtained
with a microstructure mostly containing ne ferrite grains and
spheroidized cementite. The microstructural observations in correlation with properties were studied. However, the generation of
defects (such as dislocations and lamellar faults) during cyclic heat
treatment and its effect on process mechanism were not investigated in details. In this research work an annealed low carbon
steel (containing 0.16% C) is subjected to the typical cyclic heat
treatment process that consists of repeated short-duration (6 min)
holding at 910 C (above Ac3 temperature) followed by forced air
cooling. The microstructural evolution along with generation of
defects with regard to phase transformations involved and its effect
on mechanical properties have been investigated in details.
2. Experimental procedure
As-received material for cyclic heat treatment was a homogenizing annealed 0.16% C steel. The homogenizing annealing was
carried out at 1100 C for a period of 60 min. Chemical composition

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A. Saha et al. / Materials Science and Engineering A 534 (2012) 465475

Table 1
Chemical composition of as-received steel (wt%).
C

Si

Mn

Cr

Ni

Al

Cu

Fe

0.158

0.151

0.612

0.021

0.025

0.027

0.034

0.016

0.003

Balance

of the steel as analyzed by an optical emission spectrometer (WAS,


FMSN: 01G 00 26) is given in Table 1. Annealed steel bars of
dimension 105 mm 14 mm 9 mm were subjected to cyclic heat
treatment for different number of cycles, viz. 1-cycle, 2-cycle, 3cycle, 5-cycle and 8-cycle. Each cycle consisted of inserting the
specimen in an electric resistance furnace at 910 C (50 C above
Ac3 temperature, 860 C) and holding for 6 min, followed by forced
air cooling to the room temperature. The temperature control accuracy of the electric resistance furnace was 5 C. In each cycle,
the airow rate was maintained at 6 m3 /h. This accounted for a
cooling time of 4 min and 30 s in each cycle with an average cooling rate of 195 C/min. In order to study the extent of cementite
dissolution and elemental distribution, as-received homogenizing
annealed specimen and specimen heat treated for 1-cycle of similar dimension were heated to 910 C, held for 6 min and quenched
in ice-brine solution. Thereafter, all specimens were sectioned to
small pieces and polished with successive grades of emery papers
up to 1000 grit size followed by cloth polishing with 1 m diamond
paste. These specimens were etched by 2% NITAL and examined
under metallurgical microscopes (LEICA, REICHERT, POLYVAR2 and
LEICA, DM-2500 M, Germany). The size of ferrite grains in terms of
average grain diameter was measured as per ASTM E112 standard
[5]. The hardness of all the specimens was measured in a Vickers
hardness testing machine (BIE, BV-250(S), Miraj, India) using 30 kg
load. In order to investigate mechanical properties, standard tensile test was carried out for as-received and cyclic heat-treated
specimens with 25 mm gauge length in a servohydraulic universal testing machine (INSTRON 8516, UK) of 100 kN capacity at
a crosshead speed of 0.03 mm/s. For each heat treatment condition three specimens were tested and the mean value along with
standard deviation of the mechanical properties was reported. Further, the polished and etched metallographic specimens and the
fractured surfaces of tensile tested specimens were examined in
a Scanning Electron Microscope (Hitachi, S-3000 N, Japan) under
secondary electron image mode. Thereafter, the area% of different phases present in the microstructure was determined using
graphical point count method onto the SEM micrographs of metallographic specimens. During point counting 12 image frames were
considered for each heat treatment condition with a total count of
about 12,000 points. The elemental distribution of selected specimens was studied in a scanning electron microscope (ZEISS EVO
60, Germany) equipped with wavelength dispersive X-ray spectroscopy (WDS) detector (INCA Penta FET, Oxford, UK). Finally,
selected heat-treated specimens, in the form of thin foils, were
studied under a high resolution transmission electron microscope
(JEM-2100, JEOL, Japan).
3. Results and discussions

Fig. 1(a)(f). The variation of ferrite grain size with heat treatment
cycles is presented in Table 2 and graphically shown in Fig. 2. In
homogenizing annealed condition the ferrite grain size is quite
large (47 m) due to prolong holding at high temperature and subsequent slow furnace cooling. On execution of rst heat treatment
cycle the grain size drastically reduces to 9 m. It further reduces
to 8 m in next cycle (2-cycle) and remained almost constant up
to 5 cycles of heat treatment. On application of prolong cyclic heat
treatment (8 cycles) the grain size marginally reduces to 7 m.
In order to study the mechanism of grain renement the
homogenizing annealed specimen and the specimen subjected to
1 heat treatment cycle were heated to 910 C for 6 min and subsequently quenched in ice-brine solution. Optical microstructures
of these quenched specimens in polished and etched condition at
higher magnication are shown in Fig. 3 (a) and (b). The specimen quenched from 910 C with 6 min holding after homogenizing
annealing treatment exhibits ne nucleated prior austenite grains
(Fig. 3(a)). The initial microstructure of the homogenizing annealed
specimen (Fig. 1(a)) consists of coarse proeutectoid ferrite grains
and pearlite areas mainly at the locations of grain boundary triple
point junction (GTJ). In the present study the heat treatment temperature (910 C) is not only the temperature of about 50 C above
Ac3 temperature of 0.16% C steel, but also is the temperature where
the polymorphic transformation of -iron to -iron occurs. In fact
the ferrite-to-austenite transformation is a diffusionless massive
polymorphic transformation that occurs extremely fast [6]. Therefore, either proeutectoid ferrite region or eutectoidal ferrite (ferrite
in pearlite) transforms to austenite quite rapidly. Again, proeutectoid ferrite begins to transform to austenite (with nucleation of ne
austenite grains) at high-energy sites, such as grain boundary of ferrite, interface of pearlite colony and ferrite grain. Particularly, the
interface of pearlite colony and ferrite grain is reported to act as the
potential site for autenitization since the cementite decomposition
yields carbon to the transformation front lowering the transformation temperature [7]. Accordingly, nucleated ne austenite grains
are observed (Fig. 3(a)). On the other hand, in pearlite region,
austenitization starts at the interface of ferritecementite lamellae and the ferrite region transforms to austenite quite rapidly.
However, the dissolution of cementite in austenite is a diffusioncontrolled slow process [6,8]. The holding time at 910 C being
short (6 min), the cementite dissolution remains incomplete. This
is reected in the presence of partially dissolved cementite lamella
at the prior pearlitic region (Fig. 3(a)). The presence of partially
dissolved cementite is more clearly visible in SEM secondary electron image (Fig. 4). The presence of undissolved cementite is
reported to impede the growth of austenite grains [8]. Therefore,
on holding the homogenizing annealed specimen at 910 C for
6 min the microstructure (Fig. 3(a)) contains ne austenite grains
(at prior proeutectoid ferrite region) and partially dissolved

3.1. Microstructural evaluation


In the present study the application of cyclic heat treatment
results in signicant microstructural changes, namely, (i) renement of ferrite grain, (ii) disintegration of cementite lamellae into
cementite network, cementite clusters and cementite spheroid, and
(iii) dislocation generation and annihilation.
3.1.1. Renement of ferrite grain
The optical microstructures of the homogenizing annealed
specimen and cyclically heat-treated specimens are shown in

Table 2
Grain size of ferrite for different heat treatment cycles.
Number of heat treatment cycles

Average grain diameter (m)

0 (Homogenizing annealed condition)


1
2
3
5
8

46.74
9.29
8.30
8.28
8.27
7.38

A. Saha et al. / Materials Science and Engineering A 534 (2012) 465475

467

Fig. 1. Optical microstructures of the homogenizing annealed specimen and cyclically heat treated specimens: (a) homogenizing annealed (0-cycle); (b) 1-cycle; (c) 2-cycle;
(d) 3-cycle; (e) 5-cycle; (f) 8-cycle. P, pearlite; F, proeutectoid ferrite.

cementite embedded in austenite (at prior pearlite location i.e., at


GTJ). The ne austenite grains are obtained with the short duration
holding and the presence of undissolved cementite that cease the
grain growth. Fine ferrite grains evolve from these ne austenite

grains during forced air cooling on execution of actual heat treatment cycle (Fig. 1(b)). Therefore grain size is substantially reduced
(from 47 m to 9 m) with 1-cycle of heat treatment. Thereafter, on
execution of further heat treatment cycles (2-cycle onwards) grain

Table 3
Result of graphical point count analysis.
Number of heat treatment cycles

0 (Homogenizing annealed condition)


1
2
3
5
8

Microconstituents (area %)
Ferrite

Pearlite

Grain boundary network of


cementite and cementite cluster

Isolated cementite spheroid

76.78
74.90
74.81
82.09
76.52
75.63

23.22
21.34
20.06
9.40
6.81
4.93

Negligible
3.76
5.13
8.51
15.77
18.37

Negligible
Negligible
Negligible
Negligible
0.90
1.07

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A. Saha et al. / Materials Science and Engineering A 534 (2012) 465475

Fig. 2. Variation of ferrite grain size with heat treatment cycles.

size does not change much (or marginally reduces). This is because,
after one heat treatment cycle, the initial grain size of ferrite itself
is very small and the cooling rate remains same. Therefore, during short duration holding at 910 C the size of nucleated austenite
grains and newly generated ferrite grains from these nucleated
austenite grains during cooling do not differ much from initial ferrite grain size. This is well supported by the observed size of the
nucleated prior austenite grain in the specimen heat treated for
1-cycle (910 C, 6 min, forced air cooling) and thereafter held
at 910 C for 6 min followed by quenching in ice-brine solution
(Fig. 3(b)). The most of the nucleated austenite grains in Fig. 3(b)
possess grain size similar to that observed in Fig. 3(a). The marginal
reduction in overall grain size (98 m) is due to the probable
nucleation of a few ner austenite grains (as indicated in Fig. 3(b))
at certain locations of the dislocations (high energy sites) generated
during cyclic heat treatment. The detail of dislocation generation is
discussed in Section 3.1.3.
3.1.2. Disintegration of cementite lamellae
Apart from grain renement, other signicant microstructural modication with cyclic heat treatment is the disintegration
of cementite lamellae into grain boundary cementite network,
cementite clusters and cementite spheroids. Therefore, the phases
evolved on cyclic heat treatment of homogenizing annealed coarse
ferritepearlite microstructure (Fig. 5) are free ferrite, pearlite,
grain boundary cementite network, cementite clusters and cementite spheroids. The percentages of different micro-constituents as
obtained from SEM images using graphical point count method
are presented in Table 3. The homogenizing annealed (0-cycle)
specimen (that involves nearly equilibrium cooling) contains 77%
ferrite and 23% pearlite which closely matches with that obtained
(80% ferrite and 20% pearlite) from standard FeFe3 C phase diagram using lever rule. On execution of 1-cycle, the pearlite content
slightly decreases as grain boundary network of cementite appears
in the microstructure. Isolated cementite spheroids and cementite clusters are negligible in the microstructure. The appearance
of cementite network is not normally observed in hypoeutectoid
0.16% C steel. In the present study, probably for the rst time
cementite network is identied in hypoeutectoid steel with this
typical heat treatment process. The WDS elemental mapping and
corresponding SEM image (Fig. 4) of the specimen quenched from
910 C with 6 min holding after homogenizing annealing treatment
exhibits wide variation of carbon concentration. The holding time
of 6 min is too short for complete dissolution of cementite lamella.
Thus, at GTJ the dissolution of cementite lamella remains incomplete. Accordingly, as explained earlier (Section 3.1.1), a region
of partially dissolved cementite embedded in carbon enriched

Fig. 3. Optical microstructures of the specimens quenched from 910 C with 6 min
holding: (a) after homogenizing annealing; (b) after 1 cycle. NG, Nucleated grains;
PDC, Partially dissolved cementite; FNG, Finer nucleated grain.

austenite is developed at GTJ (prior pearlitic region). Away from


this there exists low carbon austenite region (in the interior part of
prior proeutectoid ferrite grains) which converts into low carbon
martensite (almost ferrite) on quenching that appears as darker
region in SEM image (Fig. 4).
SEM images of the specimen subjected to single heat treatment cycle are presented in Fig. 6(a) and (b). The low carbon
austenite region (grain interior where carbon could not diffused
to) eventually transforms to ferrite (appearing dark) on forced air
cooling (Fig. 6(a)). On the other hand the high carbon austenite
regions (developed at GTJ) undergo two different types of transformation modes. These are indicated as Site 1 and Site 2 in
Fig. 6(a) (at lower magnication) and Fig. 6(b) (at higher magnication). The transformation product at Site 1 is ne pearlite
surrounded by thin network of proeutectoid cementite. This is
the site of normal eutectoidal transformation under air cooling
where concentration of carbon in austenite slightly exceeds eutectoid composition (0.8%). This is the prior pearlitic region (at GTJ)
that contains partially dissolved cementite lamellae embedded in
austenite at 910 C. During cooling a thin network of proeutectoid
cementite is developed at the boundary and remaining austenite
transforms to ne pearlite following eutectoidal transformation.
The undissolved cementite would facilitate the pearlitic transformation since cementite is known to be the active nucleus for
pearlitic transformation [9,10]. At Site 2, a grain boundary network
(often discontinuous) of cementite is observed. The WDS elemental mapping of the quenched specimen (where high temperature
elemental distribution is retained) exhibiting the distribution of

A. Saha et al. / Materials Science and Engineering A 534 (2012) 465475

469

Fig. 4. SEM secondary electron image and WDS elemental mapping of the specimen quenched from 910 C with 6 min holding after homogenizing annealing treatment. PDC,
Partially dissolved cementite; LC, Low carbon region; HC, High carbon region.

carbon (Fig. 4) indicates carbon enrichment at the grain boundary


region. Therefore, at 910 C, after partial cementite dissolution in
prior pearlite region (at GTJ), the dissolved carbon diffuses preferentially along the grain boundary region of nucleated austenite
grains (not effectively towards grain interior). The nucleation of
austenite grains itself initiates at prior proeutectoid ferrite grain
boundary or at proeutectoid ferritepearlite interface as discussed
earlier. The grain boundary is the defect enriched region where
atomic diffusion is faster than the lattice diffusion [11]. Therefore,
even with short holding time (6 min) at 910 C, the diffusion of carbon preferably occurs along the grain boundary region. This makes
the austenite grain boundary region almost saturated with carbon with carbon content much higher than eutectoid composition
(0.8%). During non-equilibrium forced air cooling, at rst proeutectoid cementite network precipitates out of austenite. Thereafter,
the remaining austenite at grain boundary undergoes divorced
eutectoid transformation where the eutectoid cementite nucleates
and grows on proeutectoid cementite network, and the eutectoid
ferrite phase joins with adjacent low carbon ferrite region. Therefore, the typical lamellar morphology is not obtained at Site 2 and
the grain boundary network of cementite (GNC) originates.
SEM images of the specimen subjected to 2 cycles of heat treatment are presented in Fig. 7(a) and (b). The overall microstructure
is somewhat similar to that obtained with single heat treatment
cycle except relatively ner grain size and more proportion of GNC.
The cementite network is more uniform and much thicker. This
is attributed to the fact that on execution of rst heat treatment
cycle a substantial grain renement takes place generating more
grain boundary sites for diffusion. Therefore, in the next cycle (2nd
cycle) while holding at 910 C the grain boundary diffusion of carbon is augmented generating more prominent cementite network
at grain boundary. Besides, the magnied image of pearlite region
(Site 1) of the specimen subjected to 2 cycles of heat treatment
exhibits the simultaneous evidence of thickening of cementite
lamella (nucleation of cementite spheroid) and fragmentation of

cementite lamella (Fig. 7(b)). In this regard, the TEM investigation


carried out under dark eld image mode of the specimen subjected
to single heat treatment cycle reveals the generation of defect
enriched region (appearing as dark kink) in the cementite lamella
of pearlite at Site1. This is shown in Fig. 8 along with selected
area diffraction pattern (SADP) of the cementite lamella. The nonequilibrium forced air cooling is expected to generate these defect
sites, conventionally termed as lamellar fault sites [4,12,13]. These
are the sites of higher chemical potential (higher energy). In next
cycle (2nd cycle) during holding at 910 C carbon diffusion is likely
to occur preferentially at these defect sites in two ways. Firstly,
carbon would diffuse from lamellar fault site of cementite to adjacent austenite causing the dissolution of cementite. This results

Fig. 5. SEM secondary electron image of the homogenizing annealed 0.16% C steel
specimen. P, pearlite; F, proeutectoid ferrite.

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A. Saha et al. / Materials Science and Engineering A 534 (2012) 465475

Fig. 6. SEM secondary electron images of the specimen subjected to single heat
treatment cycle: (a) lower magnication; (b) higher magnication. P, pearlite (at
Site 1); Cm, cementite (at Site 1); GNC, grain boundary network of cementite (at
Site 2); F, ferrite.

in rapid fragmentation of cementite lamella. Secondly, within a


cementite lamella carbon would diffuse from fault site (region of
higher chemical potential) to adjacent at surface (region of lower
chemical potential) causing the thickening of cementite lamella,
in other words, the nucleation of cementite spheroid [4,12,13].
Therefore, the generated lamellar faults in cementite lamella
are the sites for lamellar fragmentation and spheroid nucleation
(Fig. 7(b), Fig. 8). In the next heat treatment cycle (3rd cycle) during

Fig. 7. SEM secondary electron images of the specimen subjected to two heat treatment cycles: (a) lower magnication; (b) Pearlite region at higher magnication. P,
pearlite (at Site 1); Cm, cementite (at Site 1); GNC, grain boundary network of cementite (at Site 2); F, ferrite; TCL, thickening of cementite lamella; FCL, fragmentation
of cementite lamella.

holding at 910 C these fragmented cementite lamellae would dissolve more readily in austenite and subsequent grain boundary
diffusion of carbon would be more pronounced. Such evidences
are observed in the SEM images (Fig. 9(a) and (b)) of the specimen subjected to 3 cycles of heat treatment. At many locations
the cementite lamellae of pearlite get rapidly dissolved in austenite and diffused to grain boundary region. During forced air

Fig. 8. TEM dark eld image of the specimen subjected to single heat treatment cycle exhibiting generation of lamellar fault in cementite lamella and corresponding SADP.

A. Saha et al. / Materials Science and Engineering A 534 (2012) 465475

471

Fig. 9. SEM secondary electron images of the specimen subjected to three heat treatment cycles: (a) lower magnication; (b) higher magnication showing dissolution
of pearlite generating grain boundary cementite and ferrite. P, pearlite (at Site 1);
Cm, cementite (at Site 1); GNC, grain boundary network of cementite (at Site 2); DP
(F), dissolved pearlite (transformed ferrite); F, ferrite.

Fig. 10. SEM secondary electron images of the specimen subjected to ve heat treatment cycles: (a) lower magnication; (b) higher magnication. DGP, Degenerated
pearlite (at Site 1); Cm, cementite (at Site 1); GNC, grain boundary network of cementite (at Site 2); F, ferrite, FCm, ne precipitate of cementite in ferrite matrix; CC,
cementite cluster; CS, cementite spheroid.

cooling, GNC originates through divorced eutectoid reaction and


the low carbon austenite (at prior pearlitic region) transforms
to ferrite. Such process is clearly identied in the SEM image at
higher magnication (Fig. 9(b)). However, still at a few locations
pearlite (sometimes in fragmented form) appears through normal eutectoidal reaction (Fig. 9(a)). In this way, particularly from
3-cycle onwards, with increasing heat treatment cycles the proportion of GNC increases and the proportion of pearlite drastically
decreases (Table 3). The SEM images of metallographic specimens subjected to 5 and 8 cycles of heat treatment are shown
in Figs. 10(a) and (b), 11(a) and (b), respectively. For these higher
heat treatment cycles the amount of pearlite is reduced to a great
extent in the microstructure. This happens due to the conversion
of pearlite areas into ferrite areas and GNC with repeated cyclic
heat treatment as already discussed. Also, these ferrite areas (originated through pearlite dissolution and carbon diffusion towards
grain boundary) for higher cycles of heat treatment contain ne
precipitate of cementite (FCm). During repeated holding at 910 C,
as pearlite dissolves and carbon atom diffuses away towards grain
boundary, a small amount of carbon still remains in the austenite
grain interior. While cooling in forced air, under non-equilibrium
condition, the grain interior of austenite would transform to ferrite with subsequent ne precipitation of cementite. The remaining
pearlite regions in the microstructure are not exactly lamellar,
rather present in degenerated form due to partial dissolution. These
are indicated as degenerated pearlite (DGP) in the SEM images.

Apart from the presence of thick network of cementite, free ferrite


and small amount of pearlite, a little proportion of isolated cementite spheroid (about 1%) and clusters of cementite connected with
the cementite network are also visible. The cementite clusters (CC)
are originated from carbon-enriched region around GTJ through
divorced eutectoidal reaction at higher cycles of heat treatment.
These carbon-enriched regions are developed through dissolution
of pearlite (situated at GTJ) in austenite and subsequent diffusion of carbon towards grain boundary region. At higher cycles,
grain boundary region being already occupied by undissolved network of cementite, the diffused carbon atoms tend to accumulate
around GTJ. These regions transform to cementite clusters. During
cooling, the cementite would nucleate at undissolved cementite
network and grow in different directions forming clusters. On the
other hand, the origin of cementite spheroid (CS) nucleation is
the diffusion of carbon atom in a cementite lamella from lamellar fault site to adjacent at surface causing lamellar thickening,
as explained earlier (Fig. 7(b)). While the major part (at portion)
of fragmented lamella gets dissolved and subsequent diffusion of
carbon contributes to grain boundary cementite network and cluster formation, the thickened part of cementite lamella (nucleated
spheroid) eventually gets detached. It grows further and appears
in the microstructure as isolated spheroid at higher cycles of heat
treatment. However, in low carbon (0.16% C) steel, due to availability of large ferrite grain boundary sites, the disintegration of
cementite lamella leads to mainly the grain boundary cementite

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A. Saha et al. / Materials Science and Engineering A 534 (2012) 465475

Fig. 12. TEM bright eld image of a cementite spheroid.

Fig. 11. SEM secondary electron images of the specimen subjected to eight heat
treatment cycles: (a) lower magnication; (b) higher magnication. DGP, Degenerated pearlite (at Site 1); Cm, Cementite (at Site 1); GNC, Grain boundary network of
cementite (at Site 2); F, ferrite, FCm, ne precipitate of cementite in ferrite matrix;
CC, cementite cluster; CS, cementite spheroid.

network and cluster formation. The contribution of spheroidization is negligible. After 8 cycles of heat treatment the amount of
isolated cementite spheroid is extremely small (1%). The TEM bright
eld image of a cementite spheroid in the specimen subjected to 8
cycles of heat treatment is shown in Fig. 12. Therefore, on execution
of 8 heat treatment cycles the microstructure mainly contains free
ferrite, grain boundary cementite network and cluster and a small
amount of pearlite. In this context it is important to note that, in
a recent investigation [4,13] carried out by the present authors on
steel of higher carbon content (0.6% C), owing to absence of grain
boundary sites, disintergration of cementite lamellae mainly led to
spheroidization and no cementite network was obtained.
3.1.3. Dislocation generation and annihilation
The TEM bright eld micrographs of ferrite grain region for
the specimen subjected to different cycles of heat treatment are
shown in Fig. 13(a)(d). The presence of dislocation is not so
prominent in homogenizing annealed condition (Fig. 13(a)). This
is expected since during homogenizing annealing at higher temperature (1100 C) for 1 h the nucleation and growth of strain free
austenite grains eliminate most part of pre-existing line defects
and subsequent slow furnace cooling does not generate much
thermal stress. On execution of rst heat treatment cycle apart
from the lamellar fault generation in cementite lamella (Fig. 8)
new dislocation lines appear in the ferrite grains as shown in
Fig. 13(b). The probable reason of dislocation generation is the

development of stress during non-equilibrium forced air cooling


of the steel. The co-efcient of thermal expansion of iron based ferrite matrix (11.7 106 K1 ) and that of cementite (5.3 106 K1 )
are different [14,15]. Therefore, owing to differential contraction
between ferrite matrix and newly developed grain boundary network of cementite, dislocations are generated in ferrite matrix
during forced air cooling. Apart from the stress due to differential contraction, thermal stress and transformation stress may also
be operative. Ferrite has quite high thermal conductivity, while
cementite has poor thermal conductivity, due to an unfavorable
crystal structure [16]. Therefore, temperature gradient would exist
between different microconstituents leading to thermal stress.
On the other hand, stress may develop during transformation of
austenite to ferritecementite aggregate as it involves an increase
in volume by 4% for steel containing 0.16% C [17]. After 2 cycles
of heat treatment, the dislocation density of ferrite grains further
increases (Fig. 13(c)) due to second cycle of stress development.
Here closely spaced dislocation loops (often intersecting) of high
density are observed. However, after 8 cycles of heat treatment dislocation density is drastically reduced in ferrite matrix (Fig. 13(d))
indicating the annihilation of dislocations. In initial cycles (12
cycles), highly dense dislocation structure is developed which
would increase the free energy of the system. As the initial free
energy of the system is increased, in case of higher number of
cycles the activation energy required for annihilation of dislocations becomes much lower which could be easily overcome by
the thermal energy during holding at high temperature. Therefore,
even with short holding time (6 min) at 910 C, the nucleation of
strain free austenite grains result in elimination of dislocations at
higher cycles of heat treatment.
3.2. Mechanical properties and fractured surface
The variation of hardness and mechanical properties with
number of heat treatment cycles is given in Table 4 and graphically presented (mean values) in Fig. 14. SEM fractographs of
tensile tested specimens are shown in Fig. 15(a)(f). The hardness and strength properties (yield strength and ultimate tensile
strength) initially increase up to 2 cycles and then decrease. Accordingly, the ductility property (% elongation) initially decreases and

A. Saha et al. / Materials Science and Engineering A 534 (2012) 465475

473

Fig. 13. TEM bright eld micrographs of ferrite grain region of the specimens subjected to different heat treatment cycles: (a) 0-cycle; (b) 1-cycle; (c) 2-cycle; and (d) 8-cycle.

Fig. 14. Variation of mechanical and hardness properties with number of heat treatment cycles.

thereafter increases. The homogenizing annealed 0.16% C steel


specimen possesses low strength and high ductility following the
known characteristics of low carbon annealed steel. Typical fractured surface (Fig. 15(a)) exhibits large dimples generated through
micro-void coalescence which is the common failure characteristic of low carbon steel where microstructure is dominated by
soft ferrite phase. On execution of single heat treatment cycle
strength and hardness property increase due to substantial grain
renement (Table 2; Fig. 2) and generation of dislocation in the
microstructure (Fig. 13(b)). The fractured surface exhibits the presence of characteristic dimples (Fig. 15(b)). The dimple size is much
smaller due to smaller ferrite grain size as compared to that in
homogenizing annealed condition. After 2 cycles of heat treatment further improvement of strength is observed. In fact, the
specimen subjected to 2 cycles of heat treatment exhibits highest
strength (UTS = 455 MPa) and hardness (135 HV). This is attributed
to the ner grain size of ferrite (8 m), high dislocation density
in the ferrite grain region (Fig. 13(c)) and adequate proportion of

474

A. Saha et al. / Materials Science and Engineering A 534 (2012) 465475

Fig. 15. SEM fractographs of the tensile tested specimens: (a) 0-cycle; (b) 1-cycle; (c) 2-cycle; (d) 3-cycle; (e) 5-cycle; and (f) 8-cycle.

Table 4
Results of tensile test and hardness test.
Number of heat treatment cycles

Properties (mean standard deviation)


Ultimate tensile strength (MPa)
Yield strength (MPa)

0 (Homogenizing annealed condition)


1
2
3
5
8

200
323
338
283
279
284

15
9
9
5
12
12

338
423
455
402
394
404

15
3
4
6
12
14

% Elongation
42
38
36
39
40
39

4
3
1
3
2
1

Hardness (HV)
103
129
135
124
120
125

2
1
1
1
1
1

A. Saha et al. / Materials Science and Engineering A 534 (2012) 465475

ne lamellar pearlite in the microstructure. The fractured surface


exhibits small dimples (Fig. 15(c)), microstructure being dominated by ne ferrite grains. On execution of another heat treatment
cycle (third cycle) strength property is reduced. The corresponding
fracture surface (Fig. 15(d)) exhibits directionally oriented interconnecting elongated dimples, as a whole appearing like a void
sheet. This indicates the failure initiation at certain sites of grain
boundary cementite network causing material failure at lower
load. However, the cementite network is not continuous across
the grain boundary of ferrite and since the major proportion of
microstructure contains soft ferrite phase, the overall failure is not
intergranular, rather transgranular dimple rupture through microvoid coalescence. Therefore, ductility is not reduced. In case of 5 and
8 cycles of heat treatment, typical irregular shaped voids possessing
geometric similarity with cementite clusters have been observed
on the fractured surfaces (Fig. 15(e) and (f)). It was explained earlier
that due to continual grain boundary diffusion of carbon cementite
clusters are developed in the microstructure for higher cycles (58
cycles) of heat treatment. In such cases, these cementite clusters
act as the failure initiation sites and relatively lower strength is
achieved as compared to 2 cycles of heat treatment.
4. Conclusion
(i) The cyclic heat treatment process consisting of repeated short
duration holding at 910 C (above Ac3 ) followed by forced air
cooling leads to a new type of microstructural development in
0.16 wt% C steel. The main features include grain renement,
dislocation generation (in early cycles) and annihilation (in
higher cycles) and development of grain boundary cementite
network and clusters through divorced eutectoidal reaction.
(ii) The major extent of grain renement takes place at early stages
(up to 2 cycles) through nucleation of ne austenite grains
and their transformation to ne ferrite grains during forced air
cooling. The growth of nucleated austenite grains is restricted
by the short holding time (6 min) and the presence of undissolved cementite.
(iii) The early stages of cyclic heat treatment exhibit the generation
of dislocations in ferrite grains which disappear at higher heat
treatment cycles.
(iv) During short duration holding, the partial dissolution of
cementite in austenite and diffusion of dissolved carbon preferably along grain boundary result in the development of carbon
enriched areas at the triple point junction and grain boundary regions. During forced air cooling, these areas transform
to pearlite (through normal eutectoidal reaction) and grain
boundary network of cementite (through divorced eutectoidal
reaction), respectively. Moreover, the non-equilibrium cooling

475

in rst cycle causes the generation of lamellar faults in cementite lamellae which augments fragmentation of lamellae in the
second cycle. As a consequence, the dissolution of cementite
lamellae (dissolution of pearlite) is augmented in subsequent
cycles. Particularly from 3-cycle onwards, as the cyclic heat
treatment progresses, the dissolution of pearlite and diffusion of dissolved carbon towards grain boundary result in
the further generation of grain boundary cementite network
and cementite cluster through divorced eutectoidal reaction.
Accordingly, the proportion of lamellar pearlite (normal eutectoidal transformation product) drastically decreases in the
microstructure. The contribution of lamellar disintegration to
spheroidization is negligible.
(v) After 8 cycles of heat treatment the microstructure mainly
contains ferrite grains and grain boundary network of cementite along with cementite clusters. The cementite network and
cementite clusters act as failure initiation sites to deteriorate
strength of the steel at higher cycles of heat treatment.
(vi) In this investigation, the highest strength (455 MPa) in 0.16 wt%
C steel is achieved with 2 cycles of heat treatment, not with
conventional heat treatment involving single cycle. This is
attributed to ne ferrite grain size, high dislocation density
of ferrite grains, an adequate amount of ne lamellar pearlite
and lower proportion of grain boundary cementite in the
microstructure.

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