October 2002

Materials Letters 56 (2002) 200 – 209

www.elsevier.com/locate/matlet

Effect of processing parameters on the microstructure

and properties of an Nb microalloyed steel
Adem Bakkaloğlu*
Yıldız Technical University, Department of Metallurgical and Materials Engineering, Istanbul, Turkey

Received 10 August 2001; accepted 10 September 2001

Abstract

High strength low alloy (HSLA) steels have demonstrated superior mechanical properties through controlled rolling (CR). In
the present investigation, the effects of processing parameters, such as finish rolling temperature, rolling reduction, inter-pass
time and cooling rate, on the final microstructure and mechanical properties of a grade X52 type HSLA steel has been studied
by tensile and charpy impact tests and optical microscopy and scanning electron microscopy. To yield better mechanical
properties of X52 microalloyed steel grade, the optimization of the rolling process in the laboratory experiment and rolling mill
has been carried out. It has been found that the tensile and impact properties of X52 steel are significantly improved by
controlled rolling in the (a+g) two-phase region. The cause of such improvement in mechanical properties of the control-rolled
steel is correlated with changes in microstructure, i.e. ferrite grain refinement, a large number of subgrains and high dislocation
density. Furthermore, the low carbon contents exhibited by these steels cause evident improvement in their toughness and
weldability. Finally, a controlled rolling process in the (a+g) two-phase region of X52 steel plates has been suggested.
D 2002 Elsevier Science B.V. All rights reserved.

Keywords: Controlled rolling; Controlled cooling; Processing parameters; Microalloying; HSLA steel; Mechanical properties; (a + g) phase
region

1. Introduction important of which is grain refinement whereby both

Controlled rolling (CR) followed by controlled
cooling (CC) has been developed during the last
decade as one of the thermomechanical-controlled pro-
cesses for obtaining a good combination of strength,
toughness and weldability of high strength low alloy
(HSLA) steels in the hot rolled condition. The im-
provement in properties of CR – CC plates is associ-
ated with different strengthening mechanism, the most
*
Tel.: +90-212-261-86-74; fax: +90-212-259-70-70.
E-mail address: abakkal@yildiz.eu.tr (A. Bakkaloğlu).
strength and toughness are improved at the same time
[1,2]. To obtain optimum ferrite refinement, it is ne-
cessary to maximize the area of austenite grain boun-
dary per unit volume at the on-set of phase transfor-
mation, which may be achieved by controlled rolling
process [3].
Historically, carbon is known as the most important
chemical element for strengthening steel, but it has
detrimental effects on many technological properties
such as weldability and formability. Therefore, the ap-
plication of carbon strengthened steels is rather limited.
Furthermore, to achieve the required combination of
strength and toughness necessary for safety in con-

0167-577X/02/$ - see front matter D 2002 Elsevier Science B.V. All rights reserved.
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 A. Bakkaloğlu / Materials Letters xx (2002) 200–209
struction, expensive heat treatments such as quenching
and tempering are often needed. For wider application
of cost-effective high strength steels, physical metal-
lurgists now recommend the substitution of carbon by
other strengthening mechanisms. It is well known that
grain refinement is the most effective means to im-
prove both strength and toughness according to the
d 1/2 law [4]. This grain refinement is obtained by
careful control of the rolling conditions — time, tem-
perature and deformation during the whole production
process. The controlled rolling process is the industrial
technology to achieve this aim by combining the sha-
ping process with control of microstructure.
The grain size can be controlled by such factors as
deoxidation practice during steel producing and con-
trolled rolling. Small additions of Nb, V and Ti also
induce grain refinement [5]. The austenite grain boun-
daries are major ferrite nucleation sites and, therefore,
fine-grained austenite yields fine-grained ferrite. Con-
trolled rolling has produced appreciable grain refine-
ment providing controlled rolled steels with mech-
anical properties comparable to those of more highly
alloyed or heat treated steels. Therefore, it was deci-
ded to investigate the influences of various controlled
rolling process, involving deformation in the recrys-
tallization region, g non-recrystallization and (a + g)
regions, on the structure and properties of a niobium
containing HSLA steel.
Following the great progress of controlled rolling
practice over the last two decades, accelerated cooling
after hot rolling has currently been regarded as a
further advanced thermomechanical treatment in hot
rolling process. However, it is very important that
HSLA steel plates with low cost and high quality can
be manufactured using existing rolling mills in terms
of thermomechanical processing or so-called thermo-
mechanical control process. In general, thermome-
chanical control process of plates consists of both
controlled rolling and accelerated cooling after hot
rolling. So, the controlled rolling parameters (reheat-
ing temperature, reduction, deforming temperature,
inter-pass time) and cooling conditions (cooling rate
and finish cooling temperature) play a particularly
important role [6].
The aim of controlled rolling process of micro-
alloyed steels is to obtain required properties by
controlling the final microstructure. The final micro-
structure and mechanical properties depend strongly
201
on the chemical composition, controlled rolling pa-
rameters and cooling conditions of the plate [7]. The
present work is a laboratory study of the effects of the
processing parameters on the microstructure and prop-
erties of Standard pipeline grade X52 type API HSLA
steel.
2. Experimental procedure
The chemical composition of the steel used in this
investigation is given in Table 1. The steel was supplied
by the Erdemir Iron and Steel Factory, Turkey. The
steel was melted in a 120-ton oxygen blown converter,
slabbed, and hot rolled into plate on a semicontinuous
mini-rolling mill. Plate controlled rolling process fol-
lowed by controlled cooling tests were carried out on a
250-kN laboratory rolling mill with 160-mm diameter
rolls and rolling speed of 13 m min 1. In the present
work, slabs (20150150 mm) were reheated at 1150
jC for 1 h and were rolled to 7-mm thick plates with six
passes as two different rolling schedules.
The controlled rolling schedules used are shown in
Fig. 1. The first schedule is: reheating steel to rolling
temperature, rolling in the recrystallization region,
rolling in the (g + a) two-phase region, final cooling.
The second schedule is: reheating steel to rolling
temperature, rolling in the g non-recrystallization
region, rolling in the (a + g) two-phase region, final
cooling. The difference between these two schedules is
in first stage rolling: the g recrystallization temperature
range is used in the first schedule and the g non-
recrystallization region in the second schedule [8 –10].
It is observed that a total of 10– 20% reduction was
performed both in the recrystallization and the non-
recrystallization regions prior to the final rolling in the
(a + g) two-phase region. After the last rolling pass,
the result in total reduction was 35– 40%. The start
rolling temperatures of 950 jC for recrystallization
austenite region and 850 jC for non-recrystallization
austenite region were used. The finish rolling temper-
Table 1
Chemical composition of the steel used in investigation (wt.%)
Steel grade C Mn Si P S Nb V Al Ni
X52/AP15L 0.10 1.04 0.24 0.013 0.005 0.036 0.010 0.039 0.026
202 A. Bakkaloğlu / Materials Letters xx (2002) 200–209

3.1. Effect of process parameters on properties of

plates

3.1.1. Effect of rolling temperature

Fig. 2 shows the effect of finish rolling temperature
on the microstructure and mechanical properties for
two different hot rolling schedules. Both the tensile
strength and the yield strength of the rolled steel
increases significantly with decreasing finish rolling
temperature. Elongation decreased appreciably with
decreased finish rolling temperature. The impact tran-
sition temperature is measured as the average of upper
Fig. 1. Schematic representation of controlled rolling schedules ((I)
and lower shelf energy values. The transition temper-
schedule 1, (II) schedule 2). ature is taken as a measure of toughness property.
Similarly, as shown in Fig. 2, impact transition temper-
ature decreases with lowering the finish rolling temper-
atures were 740, 760, 780, 800, 820 jC in each ature from 850 to 740 jC, when tested in the lon-
process. The rolling temperature, cooling rate and
coiling temperatures were controlled and then samples
were cooled either by air, by forced air or by water to
600 jC at different cooling rates of 5, 10 and 20 in a
simulated manner on the laboratory mill.
Controlled rolling, tensile and impact testing, as
well as optical and scanning electron microscopies
were used in this study. Tensile specimens of
725 180-mm size were taken parallel to the rolling
direction and charpy impact specimens were received
perpendicular to the rolling direction of the plates. Flat
tensile specimens of 80-mm gauge length were tested
on a 10-ton instron machine at room temperature after
thermomechanical treatment at a strain rate of 0.05
s 1. Standard charpy test specimens (except thickness
of f7 mm.) of various thermomechanically treated
materials were prepared and tested at various temper-
atures on a standard charpy impact testing machine.
Metallographic samples representing all steels were
prepared using standard procedure. The leica imagine
analysis and linear intercept technique after etching in
2% nital was used for grain size measurements.

3. Experimental results

The reheating temperature, amount of reduction,

rolling schedules, deforming temperature, inter-pass
time, finish rolling temperature and cooling rate are Fig. 2. Effect of finish rolling temperature on the ferrite grain size
important controlled rolling parameters affecting and mechanical properties of steel plate. Final reduction is 30%
oystrength and toughness [11 – 13]. (5, schedule 2; D, schedule 1).
 A. Bakkaloğlu / Materials Letters xx (2002) 200–209 203

gitudinal rolling direction. The impact toughness of

steel is not only influenced by the controlled rolling
schedule, but also by the testing temperature. The
impact toughness (the impact transition temperatures
curves) as a function of test temperatures is shown in
Fig. 3 for both schedules 1 and 2. It can be seen that the
specimens treated with process schedule 2 are tougher
than the specimens treated with process schedule 1.
Better impact toughness is obtained at the finish rolling
temperature of 760 jC. In all cases, specimens are
soaked at 1150 jC for 1 h preceding rolling operations.

3.2. Effect of rolling reduction

The effect of the rolling reduction on the ferrite

grain size and mechanical properties of the steel plate
is summarized in Fig. 4. As shown in Fig. 4, there is
obvious effect of rolling reduction on the mechanical
properties in the temperature range 740– 850 jC. It
can be seen that the tensile and yield strength of rolled
steel increase appreciably and ductility decreases
slightly with the increase in rolling reduction, and
that impact toughness continuously increases when
the rolling reduction increases from 10% to 38%.
Similarly, as the reduction increases, the final average
grain size decreases parabolically.

Fig. 4. Effect of rolling reduction on the ferrite grain size and

mechanical properties of steel plate. Finish rolling temperature is
740 jC (5, schedule 2; D, schedule 1).

3.3. Effect of cooling rate

The mechanical properties of the experimental

Fig. 3. Comparison of the impact toughness of schedules 1 and 2
controlled rolling process (finish rolling temperature: 760 jC).
steels control rolled at 780 jC and subsequently cooled
at different cooling rates are shown in Fig. 5. Con-
trolled rolling plus accelerated cooling allow to
increase the yield and tensile strength more. However,
it decreases impact toughness. It is apparent from the
figure that the final microstructure and mechanical
properties are greatly influenced by cooling rate. The
tensile and yield strength of the steels rise as the cool-
ing rate increases, although the variation of strength
with cooling rates is smaller at higher rates than at
lower ones (<10 jC/s, i.e. cooled in the air or in the
forced air). At very high cooling rates, (20 jC/s, i.e.
cooled in water), the austenite transform to a ferrite –
204 A. Bakkaloğlu / Materials Letters xx (2002) 200–209

trolled rolling on HSLA steel is to achieve a very fine,

uniform ferrite grain size resulting in an increase in
yield strength and an improvement in toughness pro-
perties due to grain size refinement. Structural changes
in steels during controlled rolling are schematically il-
lustrated in Fig. 6. These changes are related to defor-
mation at three regions [16].
(1) Deformation in recrystallization region — In
this region, coarse austenite grain a is refined by
repeated deformation and recrystallization, which
produce the recrystallized grains b. During cooling
these grains would transform into relatively coarse
feritte bV.
(2) Deformation in non-recrystallization region —
In this region, deformation bands are formed in
elongated, unrecrystallized austenite c. During cool-
ing, ferrite would nucleate on the deformation bands
as well as gamma-grain boundaries, giving fine alpha-
grain cV.
(3) Deformation in the gamma – alpha region — In
this region, deformation bands continue to be formed
and also the deformed ferrite produces a substructure
d. After deformation, during cooling, unrecrystallized
austenite transforms into equiaxed alpha-grains, while
the deformed ferrite changes into the subgrains dV.

Fig. 5. Effect of cooling rate on the ferrite grain size, tensile pro-
perties and impact toughness of steel plate. Final rolling temperature
780 jC and final reduction is 25% (5, schedule 2; D, schedule 1).

martensite. The tensile and yield strength increased

significantly while elongation decreases slightly with
increasing the cooling rate from 5 to 20 jC/s. Impact
toughness decreased at higher cooling rates. The effect
of cooling rate on ferritic grain size is shown in Fig 5. It
is clear that grain size of ferrite decreases at increasing
cooling rate.

4. Structural changes in steel during controlled

rolling

Thermomechanical control processing (TMCP) has

been extensively applied to steel production, espe-
cially that of plate products [14,15]. In TMCP, a steel
is hot rolled to a necessary amount of reduction at a Fig. 6. Schematic illustration of changes in microstructure with
proper temperature. The primary objective of con- deformation during controlled rolling.
 A. Bakkaloğlu / Materials Letters xx (2002) 200–209
The formation of the deformation bands is one of
the principle features of controlled rolling. In the
conventional hot rolling, alpha-grains nucleate exclu-
sively at the gamma-grain boundaries, whereas in the
controlled rolling, the alpha-grain nucleation occurs at
both the grain interiors and grain boundaries, since the
deformation band is equivalent to gamma-grain boun-
dary with regard to the ferrite nucleation, the gamma-
grain can be considered as divided into several blocks
by deformation bands. This division allows one to
produce much more refined grain structure. The sec-
ond important feature of the controlled rolling is a
formation of subgrain structure during deformation in
two-phase region. The smaller the subgrain size, the
stronger its strengthening effect is.
5. Discussion
5.1. Mechanical properties
The above experimental results indicate that the
mechanical properties of rolled steel are closely asso-
ciated with the controlled rolling parameters used. As
shown in Fig. 2, controlled rolling schedule 2 allows
to further increase in the tensile and yield strength and
simultaneously to decrease the transition temperature
in comparison with controlled rolling schedule 1. On
the other hand, the tensile and yield strength of rolled
steel increases significantly, but the elongation
decreased gradually with lowering rolling temperature
within the (a + g) two-phase region. Similarly, impact
transition decreases with lowering the rolling temper-
ature from 850 to 740 jC both in the (a + g) two-
phase region and in the austenite non-recrystallization
region. The tensile and yield strength of the steel
rolled according to schedule 2 at 740 jC was higher
than of the steel rolled at 820 jC. For example, when
the rolling temperature was lowered from 850 to 740
jC, the yield strength of the steel increased from 330
to 425 MPa, while the ultimate tensile strength
increased from 430 to 528 MPa. The elongation
decreased from 38% to 27% and impact transition
temperature was 35 jC. Similar trend is found in
steel rolled according to schedule 1 as shown in Fig.
2. This is attributed to the finer grain size produced by
the lower rolling temperature. It has been reported that
a low hot rolling temperature in the austenite range
205
produces a pancake structure [17]. Since the austenite
grain boundary are major nucleation sites for ferrite,
the austenite grain boundary area is increased, and
because fine-grained austenite yields fine grain ferrite
[18], the result is fine-grained ferrite in the steel control
rolled at 740 jC. The transition temperature is lower
for steel rolled at 740 and 780 jC., as compared to that
rolled at higher temperatures (Fig. 2). As shown in Fig.
3, the steel control rolled according to schedule 2 at
760 jC exhibit better toughness than control rolled
according to schedule 1. Deformation at low temper-
ature in the (a + g) region resulted in a mixed grain size
and a high dislocation density. The results show that
ferrite, which formed during deformation in the (a + g)
region, does not undergo complete recovery and
recrystallization. As a consequence, the steel has a
higher tensile and yield strength and lower impact
transition temperature. Especially when the rolling
temperature is lower than 800 jC and the degree
reduction is 20 – 30%, better mechanical properties
are obtained.
To obtain a good combination of toughness and
strength, a fine grain structure is required. Grain size
depends on (a) the starting grain size at the austeniz-
ing temperature and (b) the controlled rolling and
subsequent controlled cooling [19]. In the present
work, attention was focused on the second point.
The hot rolling process has gradually become a much
more closely controlled operation and is increasingly
applied to low alloy steels with compositions carefully
chosen to provide optimum mechanical properties
when the hot deformation is complete. The most
efficient practical method for implementation of grain
refinement in high strength low alloy steel is con-
trolled rolling process. It relies on processing the
austenite in a temperature region of non-recrystalliza-
tion, and/or (a + g) region, thus offering more nucle-
ation sites for the transformation ferrite. In the last two
decades, several million tons of steel have been
produced every year by applying controlled rolling
in the metastable austenite region of niobium micro-
alloyed steels [20].
During hot deformation steel recrystallizes. At
relatively high temperatures, dynamic recrystallization
concurrent with the deformation is favored, while at
intermediate rolling temperatures, certain incubation
time to start the forming of new equiaxed grains,
called static recrystallization, is needed. The kinetics
206 A. Bakkaloğlu / Materials Letters xx (2002) 200–209
of this process depends on the status of the austenite
(grain size, chemical composition, etc.) and the defor-
mation parameters (temperature, reduction, strain
rate), thus determining also the final grain size. If
the deformation temperature is low enough to sup-
press recrystallization, the deformed austenite grains
remain elongated. During and in between the individ-
ual deformation steps, only dynamic and static soft-
ening by recovery is observed. Such a retardation of
recrystallization occurs already at higher temperatures
in higher alloyed steels with microalloying elements
being very effective in this context [20]. It is well
known that niobium is the most effective element in
retarding the recrystallization of deformed austenite
when it was initially in solid solution [21]. Therefore,
a finer ferrite grain results from the deformed austen-
ite. This achievement is maintained also when higher
cooling rates like in accelerated cooling are applied.
The greater the cooling rate, the finer the ferrite grain
size will be Fig. 5 indicates why the combination of
controlled rolling plus accelerated cooling is preferred
in practice.
5.2. Microstructure
The mechanical properties of the control-rolled steel
are related to their microstructures. Ferrite grain size is
influenced by rolling parameter in the (a + g) two-
phased region. Figs. 2 and 7 show the effect of rolling
temperature on ferrite grain size and microstructures.
The final average grain size decreases parabolically
Fig. 7. (a – c) Effect of rolling temperatures on the final microstructure of rolled steel according to schedule 2. Final reduction was 30%: (a) 740
jC, (b) 780 jC, (c) 820 jC.
with the decreasing finish rolling temperature for
schedules 1 and 2 rolling processes used in the present
work. As shown in Fig. 2, when the steel was soaked at
1150 jC, lowering the rolling temperature from 850 to
749 jC resulted in a decrease of the average ferrite
grain size from 20 to 8 Am. The reason for such
variation of ferrite grain size with rolling temperature
can be related to the recrystallization of a grains.
It is observed that the ferrite grain refinement is
mostly the result of austenite deformation below the
recrystallization temperature and accelerated cooling
after deformation; both processes increase the nucle-
ation of ferrite phase [22]. Several increase mecha-
nisms of nucleation rate of ferrite by deformation have
been put forward. These include an interrelation be-
tween the increased nucleation rate of ferrite with the:
(a) bulges formed by local austenite grain boundary
migration [23], (b) formation of subgrains near the
deformation austenite grain boundaries, and (c) strain
energy of the dislocations stored in deformed austen-
ite [24]. The grain refinement is obtained by control of
the rolling conditions — time, temperature and defor-
mations during the whole production process. Grain
refinement in steels is enhanced through a combina-
tion of controlled rolling and microalloying. The
primary grain refinement mechanism in controlled
rolling is the recrystallization of austenite during hot
deformation. Small additions of alloying elements like
Nb, V and Ti result in the formation of carbonitrides in
the microstructure. These very fine precipitates are
effective in preventing grain growth. By the use of
 A. Bakkaloğlu / Materials Letters xx (2002) 200–209 207

Fig. 8. (a – c) Effect of rolling reduction on the final microstructure of rolled steel according to schedule 2. Finish rolling temperature was 740
jC: (a) 15%, (b) 25%, (c) 35%.

controlled rolling, recrystallization is retarded during
the last passes.
The amount of reduction also has an influence on
ferrite size. Fig. 8 shows optical micrographs of steel
control rolled from 740 jC due to the amount of
reduction. It can be observed that the grain size of
ferrite decreases with increasing rolling reductions
regardless of which rolling schedule is used. During
rolling in the (a + g) two-phase region, both g and a
grains are compressed. The g grains are elongated and
the a grains transformed from the g become much
finer. Therefore, these a grains in the (a + g) two-
phase region are also elongated during rolling and
also become finer after recrystallization [8]. On the
other hand, substructure appears in ferrite grains when
deformation takes place in the (a + g) two-phase
region. As the reduction increases, the defect density
in ferrite grains become so high that dynamic recovery
structures finally appear in a grains. As this dynamic
recovery structure is quite stable, it is the main
strengthening factor in two-phase region rolling [25].
The microstructure after the control rolling process
consists of fine ferrite and transformation phases.
Control-rolled flat products have a ferritic – perlitic
and ferrite – martensite structure. The optical micro-
structure of X52 steel, rolled at 780 jC according to
schedule 1 and subsequently cooled at different cool-
ing rates, is shown in Fig. 9. In the air cooled and

Fig. 9. (a – c) Effect of different cooling rates on the final microstructure of rolled steel according to schedule 1. Finish rolling temperature 780
jC and final reduction was 30%, (a) 5 jC/s, (b) 10 jC/s, (c) 20 jC/s.
208 A. Bakkaloğlu / Materials Letters xx (2002) 200–209
Fig. 10. SEM micrographs of steel specimen control rolled at 760
jC and air cooled according to schedule 2. Specimens were soaked
at 1150 jC for 1 h preceding rolling operations.
forced air cooled conditions, the microstructure was
ferrite and pearlite, and in the water cooled conditions,
the microstructure was composed of ferrite and mar-
tensite, and martensite amount was essentially in the
range of 35 – 40%. The percentage of martensite
islands increased at an increase in cooling rate. The
specimens representing control-rolled steels were
examined in the scanning electron microscopy (Fig.
10). Small amounts of pearlite and a number of
dispersed niobium carbide particles were present in
the ferritic matrix. A favorable combination of
strength and toughness properties, which cannot be
achieved by heat treatment alone, is obtained. Further
refining of the structure can be achieved by acceler-
ated cooling from the rolling heat.
6. Conclusions
(1) The experimental results of this investigation
indicate that it is possible to improve the tensile and
impact properties of a X52 microalloyed steel by
suitable controlled rolling process in the (a + g) two-
phase region. Controlled rolling has produced appre-
ciable grain refinement providing control-rolled steels
with mechanical properties comparable to those of
more highly alloyed or heat treated steels.
(2) For the steel under investigation, optimum
tensile and impact properties are obtained through
the following treatment: Steels control rolled accord-
ing to schedule 2, were soaked at 1150 jC for 1 h,
rolled at 780 jC with 30% total reduction followed by
holding for 30 min at 780 jC and cooled in forced air
(cooling rate 10 jC/s). This thermomechanical proc-
ess produces a microstructure consisting of fine-
grained ferrite containing fine carbide precipitate
particles.
(3) In this study, excellent properties have been
achieved; i.e. typically 400 MPa yield strength, 495
MPa tensile strength, 32% elongation, 35 jC impact
transition temperature and maximum grain refinement
as 8 Am through controlled rolling.
(4) The results have shown that the plates produced
by this processing method posses uniform and fine
grain size as well as good strength and low temper-
ature toughness.
(5) The improvement in mechanical properties of
controlled rolled steel is due to the ferrite grain
refinement, the formation of subgrain, high disloca-
tion density, the low carbon content, precipitation
hardening and low alloying contents.
(6) Ferrite grain can be refined through controlled
rolling followed by accelerated cooling, and accumu-
late deformation of (a + g) two-phase region without
resort to high reduction at low finish rolling temper-
atures.
(7) Thermomechanical control process which
includes reheating of slabs, controlled rolling, and
accelerated cooling for the production of structural
grade plates is the industrial technology to achieve the
required combination of strength and toughness nec-
essary for safety in construction.
(8) Lowering the rolling temperature resulted in an
increase in the yield and tensile strength of steels
soaked at 1150 jC. For example, the yield strength of
the steel soaked at 1150 jC increased from 330 to 425
MPa, while the ultimate tensile strength increased
from 430 to 530 MPa when the rolling temperature
was lowered from 850 to 740 jC.
Acknowledgements
The author’s sincere thanks are accorded to Prof.
Dr. A. Topuz, Prof. Dr. M. Mars ß oğlu and Yıldız
Technical University Research Association for the
provision of experimental facilities.
 A. Bakkaloğlu / Materials Letters xx (2002) 200–209
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