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Materials Science and Engineering A 437 (2006) 436445

Impact toughness and microstructure relationship in niobium- and


vanadium-microalloyed steels processed with varied cooling
rates to similar yield strength
S. Shanmugam a , R.D.K. Misra a, , T. Mannering b , D. Panda b , S.G. Jansto c
aCenter for Structural and Functional Materials and Department of Chemical Engineering,
University of Louisiana at Lafayette, LA 70504-4130, USA
b Nucor-Yamato Steel, P.O. Box 1228, 5929 East State Highway 18, Blytheville, AR 72316, USA
c Reference Metals, 1000 Old Pond Road, Bridgeville, PA 15017, USA

Received 12 July 2006; accepted 3 August 2006

Abstract
We describe here the relationship between microstructure and impact toughness behavior as a function of cooling rate for industrially processed
Nb- and V-microalloyed steels of almost similar yield strength (60 ksi). Both Nb- and V-microalloyed steels exhibited increase in toughness
with increase in cooling rates during processing. However, Nb-microalloyed steels were characterized by relatively higher toughness than the
V-microalloyed steels under identical processing conditions. The microstructure of Nb- and V-microalloyed steels processed at conventional
cooling rate, primarily consisted of polygonal ferritepearlite microconstituents, while Nb-microalloyed steels besides polygonal ferrite and
pearlite contained significant fraction of degenerated pearlite. The microstructure of Nb- and V-microalloyed steels processed at relatively higher
cooling rate contained degenerated pearlite and lath-type (acicular) ferrite in addition to the primary ferritepearlite constituents. The fraction
of degenerated pearlite was higher in Nb-microalloyed steels than in the V-microalloyed steels. In both Nb- and V-microalloyed steels the
precipitation characteristics were similar with precipitation occurring at grain boundaries, dislocations, and in the ferrite matrix. Fine-scale
(510 nm) precipitation was observed in the ferrite matrix of both the steels. The selected area diffraction (SAD) pattern analysis revealed that
these fine precipitates were MC type of niobium and vanadium carbides in the respective steels and followed BakerNutting orientation relationship
with the ferrite matrix. The microstructural studies suggest that the increase in toughness of Nb-microalloyed steels is attributed to higher fraction
of degenerated pearlite in the steel.
2006 Elsevier B.V. All rights reserved.

Keywords: Microalloyed steels; Precipitation; Degenerated pearlite

1. Introduction mal alloying content and to obtain good toughness. It also facil-
itates the development of high strength steels with low carbon
Currently, there is a strong interest to study thermomechan- and manganese content, and consequently improved weldability
ical processing and accelerated cooling of high strength low [2]. The lowering of ferrite transformation temperature intro-
alloy steels to derive mechanical property benefits, notably duced by higher cooling rate promotes ferrite nucleation rate
strengthtoughness combination [18]. It is known that cooling at the austenite grain boundaries and in the grain interior. The
rate after the last reduction and coiling temperature has signifi- enhanced nucleation density restricts grain growth because of
cant effect on the ultimate microstructure of steels. Accelerated impingement of mutual grains, resulting in ferrite grain refine-
cooling is one of the methods to strengthen the steels with mini- ment [2]. Additionally, the volume fraction of non-equilibrium
phases increases with higher cooling rates [16]. Thus, accel-
erated cooling after controlled rolling produces a fine-grained
Corresponding author at: Center for Structural and Functional Materials and microstructure and promotes the formation of low transforma-
Department of Chemical Engineering, University of Louisiana at Lafayette, P.O.
Box 44130, Lafayette, LA 70504-4130, USA. Tel.: +1 337 482 6430;
tion temperature products, such as degenerated pearlite, bainitic
fax: +1 337 482 1220. ferrite, acicular ferrite or bainite and martensiteaustenite
E-mail address: dmisra@louisiana.edu (R.D.K. Misra). constituent in microalloyed steels [1,2,5,6]. In general, the

0921-5093/$ see front matter 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2006.08.007
S. Shanmugam et al. / Materials Science and Engineering A 437 (2006) 436445 437

strength of CMn steels is enhanced because of replacement of h-position with the web horizontal, the width is close to 24 in.
pearlite phase by lath-like bainite using high cooling rate [1]. The 103 refers to nominal weight in lbs/ft.
Majority of the bainitic microstructures obtained in low Mean grain size was determined by the linear intercept
carbon-microalloyed steels are described as bainitic ferrite method. Intercept lengths were determined and then converted
or acicular ferrite and granular bainite. Sometimes a mixed to nominal grain size using standard tables. Tensile tests were
microstructure is also obtained in HSLA low carbon steels done according to ASTM E8 and ASTM A370 specifications
at high cooling rate [18]. As the cooling rate increases, the and Charpy v-notch impact test was carried out according to
phase transformation temperature, Ar3 , decreases and transfor- ASTM E23 and ASTM A673 standards.
mation occurs at a rate such that it passes through the two-phase Small coupons were cut from the beams and mounted for
region quickly and dynamic precipitation of ferrite is mini- metallographic examination. Standard grinding and polishing
mum [3]. Also, the deformation enhances the transformation techniques were employed, and specimens were etched with
driving force and accelerates the continuous cooling transfor- 2% nital. Light microscopy and scanning electron microscopy
mation, shifting the pearlite transformation curve of CCT dia- (JEOL 6300F) imaging techniques were used to obtain low mag-
gram to the right. When the cooling rate is increased to the nification images that revealed the overall microstructure. The
extent that the ferrite transformation temperature is surpassed, a amount of different microstructural constituents was estimated
fully bainitic microstructure is obtained [8]. Accelerated cooling with conventional point-counting techniques in association with
refines bainitic microstructure and is attributed to the increase a square point grid as described below. The metallographic mea-
in the driving force for the nucleation rate of ferrite subunits as surements were made on at least 20 fields-of-view in order to
a consequence of reduction in the bainite transformation start obtain representative data for stereological analysis.
temperature [6,7]. A decrease in the bainite transformation start Stereological analysis was adopted as one of the approach
temperature increases the difference in the free energy between to understand the underlying differences in toughness of steels,
austenite and bainite that favoring the formation of bainite. The since our recent work indicated that small differences in tough-
growth of fine bainitic ferrite laths is controlled by nucleation ness of steels with similar yield strength can be explained in
rate of subunits, which in turn strongly depends on the driving terms of stereological parameters, notably, contiguity ratio [9].
force (undercooling) for the phase transformation reaction [6,7]. The parameters determined for stereological analysis were vol-
Considering that currently, there is increased demand for high ume fraction, mean intercept length, and contiguity ratio.
strength structural beams with superior toughness, we are pur- The volume fraction of ferrite VV was calculated using the
suing microalloying approach to process structural beams with systematic point count method. Ferrite grain size and pearlite
high strengthtoughness combination. The present paper is an colony size was estimated in terms of mean intercept length
effort in this direction, where the focus is to study the effect of (L ) determined by the following expression [9]:
cooling rate on the mechanical behavior and relate to microstruc-
tural features. = VV LT
L (1)
N
2. Steel composition and experimental methods where VV is the volume fraction of ferrite phase, N the number
of ferrite grains intercepted by the test lines and LT is the line
The chemical composition range of Nb- and V-microalloyed length of the test lines.
steels is presented in Table 1. The composition range meets The ferrite contiguity ratio C was calculated by Eq. (2) [9]:
the ASTM specification A992. The niobium content required 2(SV ) 2(PL )
to obtain the desired yield strength of 5560 ksi was approx- C = = (2)
(SV )P + 2(SV ) (PL )P + 2(PL )
imately one third of the vanadium content. The processing
conditions were similar for both Nb- and V-microalloyed steels where (PL ) is the number of point intersections per unit
with no intentional differences. The processing parameters are length of the test line with ferriteferrite, (PL )P the num-
not described here due to proprietary reasons. A representative ber of point intersections per unit length of the test line with
beam size is W24 103; the designated size means that the ferritepearlite boundaries, (SV ) the surface area per unit vol-
nominal depth of beam is 24 in., when the beam is lying in the ume of ferriteferrite boundaries and (SV )P is the surface area
per unit volume of ferritepearlite boundaries.
Table 1 Contiguity is defined as the fraction of the total interface
Chemical composition range of Nb- and V-microalloyed steels area of phase that is shared by grains of the same phase. Thus,
Elements Nb-microalloyed steel (wt.%) V-microalloyed steel (wt.%) ferrite contiguity ratio is indicative of the amount of ferrite that is
continuous, i.e., it tells how much ferrite is adjacent to the ferrite.
C 0.0300.100 0.0300.100
It is calculated by finding the ratio of number of ferriteferrite
Mn 0.5001.500 0.5001.500
V 0.001 0.0200.050 grain boundaries to the total number of grain boundaries in the
Nb 0.0200.050 0.001 microstructure (Eq. (2)). From Eq. (2), contiguity ratio will vary
Si 0.150.25 0.150.25 from 0 to 1.
P 0.0100.020 0.0100.020 Transmission electron microscopy was carried out on thin
S 0.0150.025 0.0150.025
foils of Nb- and V-microalloyed steels. These foils were prepared
N 0.0090.010 0.0090.010
by cutting thin wafers from the steel samples, and grinding them
438 S. Shanmugam et al. / Materials Science and Engineering A 437 (2006) 436445

to 100 m in thickness. Three-millimeter discs were punched Fig. 1 shows the variation in impact toughness of Nb- and V-
from the wafers and electropolished using a solution of 10% microalloyed steels as a function of cooling rate. It may be
perchloric acid in acetic acid electrolyte. Foils were examined noted that both the steels generally experienced improvement in
with a JEOL FEG TEM/STEM operated at 200 kV. toughness with increase in cooling rate. However, the toughness
improvement appeared to be greater for the Nb-microalloyed
3. Results and discussion steel as compared to the V-microalloyed steel.

3.1. Tensile and impact behavior 3.2. Microstructures of Nb- and V-microalloyed steels

Tensile properties of Nb- and V-microalloyed steels are listed Representative scanning electron micrographs of Nb- and V-
in Table 2 for conventionally/normally cooled beams. Both the microalloyed steels are presented in Figs. 2 and 3. The low-
steels exhibited similar yield strength, tensile strength, and per- and high-magnification micrographs of Nb-microalloyed steels
cent elongation. Almost similar values were obtained at inter- processed at conventional (low) and high cooling rates are
mediate and high cooling rates. However, there was variation in presented in Fig. 2a, b and c, d, respectively. Similarly, the
toughness of the two steels as schematically depicted in Fig. 1. micrographs of V-microalloyed steels processed at conventional
and high cooling rates are presented in Fig. 3a, b and c, d,
respectively. The primary microstructural constituents of Nb-
Table 2
Representative room temperature tensile properties of Nb- and V-microalloyed and V-microalloyed steels processed at conventional and high
steels cooling rates were polygonal ferrite, pearlite, and degenerated
pearlite. It may, however, be noted that the fraction of degen-
Properties Nb-microalloyed steel V-microalloyed steel
erated pearlite was high for the steels subjected to relatively
Yield strength (ksi) 5760 5861 high cooling rate (Fig. 1b and Table 3), and at a given cooling
Tensile strength (ksi) 7274 7576
rate, the Nb-microalloyed steel contained significantly higher
% Elongation 2326 2325
amount of degenerated pearlite (Fig. 2c and d) as compared
to the V-microalloyed steels (Fig. 3c and d). The average fer-
rite grain size of both the steels processed at conventional and
high cooling rates was similar (2629 m). The quantitative
metallographic data for Nb- and V-microalloyed steels are sum-
marized in Table 3.
The microstructures of Nb- and V-microalloyed steels pro-
cessed at conventional (normal) cooling rate are presented in
Figs. 4 and 5. The general microstructure and the dislocation
substructure in ferrite of Nb-microalloyed steels are presented in
Fig. 4a and b, respectively. The representative low magnification
TEM micrographs show large polygonal ferrite grains with high
dislocation density. There were some grains that were virtually
free of dislocations. Fig. 5a and b shows the general microstruc-
ture and dislocation density in ferrite of V-microalloyed steels.
Representative bright field TEM micrographs of Nb- and V-
microalloyed steels subjected to relatively high cooling rate
are presented in Figs. 6 and 7. Two types of ferrite morpholo-
gies (polygonal ferrite and lath-type ferrite) were observed in
both the steels. The microstructure of Nb-microalloyed steels
showing regions of polygonal ferrite, lath-type ferrite grains
and degenerated pearlite are presented in Fig. 6. Similarly, the
microstructures of V-microalloyed steels that contain polygonal
ferrite, lath-type ferrite grain structure and degenerated pearlite
are presented in Fig. 7. At higher cooling rates, it is anticipated
that austenite transforms to fine ferrite crystals in the interme-
diate temperature range as compared to the conventional ferrite
structure. In Figs. 6 and 7, the ferrite grains in groups of parallel
laths are termed as acicular ferrite or bainitic ferrite [10].

3.2.1. Degenerate pearlite


Degenerated pearlite is formed by nucleation of cementite
Fig. 1. (a) Room temperature Charpy v-notch impact toughness and (b) % degen- at ferrite/austenite interfaces followed by carbide-free ferrite
erated pearlite of Nb- and V-microalloyed steels. layers enclosing the cementite particles in the transformation
S. Shanmugam et al. / Materials Science and Engineering A 437 (2006) 436445 439

Fig. 2. Representative low- and high-magnification scanning electron micrographs of Nb-microalloyed steel processed at (a and b) conventional and (c and d) high
cooling rates. The micrographs (b) and (d) show degenerated pearlite.

temperature between normal pearlite and upper bainite [11]. ficient carbon diffusion to develop continuous lamellae [12].
A schematic diagram illustrating the formation mechanism of It is reported that the interface between ferrite and cementite
degenerated pearlite is presented in Fig. 8. Since the advanc- in degenerated pearlite is wider than the conventional pearlite,
ing ferrite/austenite is enriched with carbon by partitioning thus the ferrite grain boundary area of the controlled-rolled steels
process, it is believed that cementite nucleation takes place at that contains degenerated pearlite is higher as compared to the
ferrite/austenite interface boundary. Similar to lamellar pearlite, conventionally processed steel [13]. A typical bright field TEM
degenerated pearlite is also formed by diffusion process and con- micrograph of degenerated pearlite formed in Nb-microalloyed
sidering its morphology, the difference is attributed to the insuf- steel is presented in Fig. 9a and the corresponding selected

Fig. 3. Representative low and high magnification scanning electron micrographs of V-microalloyed steel processed at (a and b) conventional and (c and d) high
cooling rates. The micrograph (d) shows degenerated pearlite.
440 S. Shanmugam et al. / Materials Science and Engineering A 437 (2006) 436445

Table 3
Microstructural features of Nb- and V-microalloyed steels
Properties Nb-microalloyed steels V-microalloyed steels

Conventional cooling rate Higher cooling rate Conventional cooling rate Higher cooling rate

Ferrite
Area fraction (%) 82.4 3.1 82.8 0.02 83 2.5 82.8 3.8
Mean intercept length (L
) (m) 27 1.5 27 2.8 28.9 3 25.9 1
Contiguity ratio (C ) 0.74 0.76 0.77 0.74
Pearlite
Area fraction (%) 9.6 3.1 1.2 1.9 17 2.3 8.2 2.9
Mean intercept length (L
) (m) 10.3 0.7 10.2 0.7 8.4 0.9 8.9 1
Degenerated pearlite
Area fraction (%) 8 0.9 16 2 91

Fig. 4. Bright field TEM micrographs of Nb-microalloyed steels processed at conventional (or normal) cooling rate showing (a) polygonal ferrite structure and (b)
dislocation substructure in ferrite.

area diffraction (SAD) pattern is shown in Fig. 9b. The SAD 3.3. Precipitation in Nb- and V-microalloyed steels
pattern analysis suggested that the cementite platelets exhibit
[1 1 2] //[1 2 2]Fe3 C orientation relationship with ferrite matrix, Fig. 10a and b shows grain boundary precipitation and pre-
which is close to Pitsch orientation relationship that is com- cipitation on dislocations in ferrite region of Nb-microalloyed
monly observed in lamellar pearlite. Degenerated pearlite is a steels, while Fig. 11a shows precipitation in ferrite matrix
microstructural constituent believed to promote toughness in together with the corresponding selected area diffraction (SAD)
steel [13]. pattern in Fig. 11b. The SAD pattern analysis indicated that

Fig. 5. Bright field TEM micrographs of V-microalloyed steels processed at conventional (or normal) cooling rate showing (a) polygonal ferritepearlite structure
and (b) dislocation substructure in ferrite.
S. Shanmugam et al. / Materials Science and Engineering A 437 (2006) 436445 441

Fig. 6. Bright field transmission electron micrographs of Nb-microalloyed steels processed at relatively high cooling rate showing (a) polygonal ferrite structure (b)
lath-type (acicular) ferrite structure and (c) degenerated pearlite.

Fig. 7. Bright field transmission electron micrographs of V-microalloyed steels processed at relatively high cooling rate showing (a) polygonal ferrite structure, (b)
lath-type (acicular) ferrite structure and (c) degenerated pearlite.

Fig. 8. Schematic diagram illustrating the formation mechanism of degenerated pearlite.

Table 4
Precipitate characteristics of Nb- and V-microalloyed steels
Properties Nb-microalloyed steels V-microalloyed steels

Conventional cooling rate Higher cooling rate Conventional cooling rate Higher cooling rate

Mean particle size (d) (nm) 5.25 3.5 7.5 4.5 10.3 4 8 4.3
Mean inter-particle spacing (nm) (50 measurements) 66 37 50 29 62 31 44 18
Particle density (no. of particles/0.5 m2 ) 280 320 210 375
442 S. Shanmugam et al. / Materials Science and Engineering A 437 (2006) 436445

Fig. 9. Bright field TEM micrographs of Nb-microalloyed steels showing (a) degenerated pearlite and (b) SAD pattern analysis for degenerated pearlite shown in
(a).

Fig. 10. Bright field TEM micrographs of Nb-microalloyed steels showing (a) grain boundary precipitation and (b) precipitation on dislocations.

Fig. 11. Bright field TEM micrograph of Nb-microalloyed steels showing (a) fine-scale precipitation in the ferrite matrix and (b) corresponding SAD pattern analysis
for the precipitate and the matrix.
S. Shanmugam et al. / Materials Science and Engineering A 437 (2006) 436445 443

Fig. 12. Bright field TEM micrographs of V-microalloyed steels showing (a) grain boundary precipitation and (b) precipitation on dislocations.

the fine precipitates were MC type of cubic niobium carbides cooling. The precipitation of microalloying elements occurs dur-
and the precipitates exhibited [1 0 0] //[1 1 0]NbC BakerNutting ing various stages of thermomechanical processing of steels. At
orientation relationship with the ferrite matrix. Grain boundary soaking temperatures, the microalloying elements, Nb and V, are
precipitation and precipitation on dislocations in ferrite region taken into solution depending on the limitation imposed by the
of V-microalloyed steels was also observed and is presented solubility product. For carbide and nitride forming elements, the
in Fig. 12. Fig. 13a shows precipitation in ferrite matrix of V- solubility in austenite at any given temperature depends on C and
microalloyed steels and the corresponding selected area diffrac- N content of the steel. When the temperature is lowered during
tion (SAD) pattern is shown in Fig. 13b. In a manner similar to cooling, supersaturation of these solute elements increases and
Nb-microalloyed steel the SAD pattern analysis indicated that precipitation begins at favorable kinetic conditions. Deforma-
the fine precipitates were MC type of cubic vanadium carbides tion of austenite introduces large amount of lattice defects such
and the precipitates exhibited a cubecube [0 0 1] //[0 0 1]VC as dislocations and vacancies that assist the diffusional process
BakerNutting orientation relationship with the ferrite matrix. that control the precipitation kinetics. As a result, strain induced
The characteristics of precipitates in terms of mean particle precipitation occurs at the prior austenite grain boundaries or
size, mean inter-particle distance and particle density in ferrite defects. In summary, the Nb- and V-microalloyed steels exhib-
matrix of both Nb- and V-microalloyed steels are summarized ited similar precipitation behavior in ferrite and the size range
in Table 4. was from 5 to 10 nm (Table 4). It is reported that the effec-
The above results suggest that Nb- and V-microalloyed steels tive size range for precipitation hardening is 520 nm [9,14].
experienced strain induced precipitation at grain boundaries, and These fine precipitates exhibited BakerNutting orientation rela-
dislocations, while the fine precipitates in ferrite formed during tionship (Figs. 11b and 13b) with the ferrite matrix of Nb- and

Fig. 13. Bright field TEM micrograph of V-microalloyed steels showing (a) fine-scale precipitation in the ferrite matrix and (b) corresponding SAD pattern analysis
for the precipitate and the matrix.
444 S. Shanmugam et al. / Materials Science and Engineering A 437 (2006) 436445

Fig. 14. Schematic illustration of deformation of cementite in lamellar pearlite and degenerated pearlite.

V-microalloyed steels, confirming that the precipitation occurred nantly bainitic ferrite with increase in cooling rate is responsi-
in ferrite. ble for the strengthtoughness combination of Nb-microalloyed
steels at high cooling rate.
3.4. Toughness behavior of Nb- and V-microalloyed steels
4. Conclusions
In the present case the microstructural parameters that are
likely to influence toughness are ferrite grain size, degenerated 1. At conventional cooling rates employed in the mill, the
pearlite, and acicular ferrite. A finer grain size and higher conti- microstructure of Nb- and V-microalloyed steels primarily
guity ratio is expected to impart higher toughness. From Table 3, contained polygonal ferritepearlite, while Nb-microalloyed
it may be noted that the ferrite grain size and ferrite contiguity steels contained significant fraction of degenerated pearlite.
ratio are similar for both the steels processed at conventional The Nb- and V-microalloyed steels processed at relatively
and relatively high cooling rates. However, there are significant higher cooling rate compared to conventional or normal
differences in the area fraction of degenerated pearlite for the cooling rate contained degenerated pearlite and lath-type
two steels (Fig. 1b and Table 3). A schematic diagram illus- (acicular) ferrite in addition to the primary ferritepearlite
trating the nature of cementite plates present in the lamellar constituents. The fraction of degenerated pearlite was higher
pearlite and degenerated pearlite and its effect on plastic defor- in Nb-microalloyed steels than in the V-microalloyed steels.
mation is presented in Fig. 14a and b. It is reported that the 2. Both Nb- and V-microalloyed steels exhibited similar precip-
cementite thickness in degenerated pearlite is finer as compared itation characteristics with precipitation at grain boundaries,
to the conventional pearlite (Fig. 14b), and hence the volume dislocations and in the ferrite matrix. Fine-scale (510 nm)
fraction of cementite and ferrite are different in the former as precipitation occurred in the ferrite matrix of both the steels.
compared to the latter [15]. Coarse pearlite deforms inhomo- The SAD pattern analysis revealed that these fine precipitates
geneously (Fig. 14a) with strain localized in narrow slip bands, were MC type niobium and vanadium carbides in the respec-
where as fine degenerated pearlite is expected to experience uni- tive steels and obeyed BakerNutting orientation relationship
form strain distribution during deformation. It is also shown that with the ferrite matrix.
the steels containing degenerated pearlite with specific cementite 3. The Nb- and V-microalloyed steels experienced improve-
thickness exhibit maximum ductility [15]. It is also reported that ment in toughness with increase in cooling rates during
though cementite is characterized by hard and brittle in nature, it processing. However, Nb-microalloyed steels seem to exhibit
can endure large strain when the cementite platelets are thinner relatively higher toughness than the V-microalloyed steels
[16]. Thus, at present, we believe that the increase in the tough- during processing at conventional and high cooling rates. The
ness of Nb- and V-microalloyed steels at relatively high cooling increase in toughness of Nb-microalloyed steels is attributed
rate is a consequence of higher fraction of degenerated pearlite to its higher fraction of degenerated pearlite in the steel.
and the presence of lath-type ferrite. While, the higher toughness
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