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Materials Characterization 56 (2006) 59 65

Effect of cooling rate on structure and properties of an ultra-low


carbon HSLA-100 grade steel
A. Ghosh a, S. Das b, S. Chatterjee a,*, P. Ramachandra Rao c
a

Department of Metallurgy and Materials Engineering, Bengal Engineering and Science University, Shibpur, Howrah, 711103, India
b
National Metallurgical Laboratory, Jamshedpur, 831 007, India
c
Institute of Armament Technology (Deemed University), Pune, Girinagar, 411 025, India
Received 2 August 2005; received in revised form 21 September 2005; accepted 24 September 2005

Abstract
An ultra-low carbon HSLA-100 grade steel was subjected to two stage forging operation followed by different post-cooling
techniques. Higher strength value obtained at a faster cooling rate of 35 8C/s is due to highly dislocated acicular ferrite structure
along with fine precipitation of microalloying carbides and/or carbonitrides. At a slower cooling rate of 1.15 8C/s the strength value
drops with an increase in ductility due to larger volume fraction of less dislocated polygonal ferrite structure. The strength value
remained almost unchanged with a further decrease in cooling rate to 0.68 8C/s due to the formation of predominantly polygonal
ferrite microstructure. At slower post-cooling rates high impact toughness value obtained at ambient and at  40 8C testing
temperature is due to fine grained polygonal ferrite microstructure. At all post-cooling conditions the change in impact toughness
value at ambient and at 40 8C temperature was found to be negligible due to the ultra-low carbon content of the steel.
D 2005 Elsevier Inc. All rights reserved.
Keywords: HSLA forging; Acicular ferrite; Polygonal ferrite; MA (martensiteaustenite) constituents; Microalloying precipitates; Mechanical
properties

1. Introduction
HSLA-100 and HSLA-80 grade steels are Cu bearing low carbon steels which were developed by the US
navy in the mid-1980s [1]. The continuous cooling
transformation behaviours of these types of steels
have been explored by earlier researchers [2 4]. The
microstructural characterization of as rolled and tempered HSLA-100 steels has been reported [57]. The
structure and properties of these steels at various pro* Corresponding author.
E-mail address: ghosh_ari@yahoo.com (A. Ghosh),
sdas@csnml.ren.nic.in (S. Das), schatterjee46@yahoo.com
(S. Chatterjee), diriat@hotmail.com (P. Ramachandra Rao).
1044-5803/$ - see front matter D 2005 Elsevier Inc. All rights reserved.
doi:10.1016/j.matchar.2005.09.014

cessing conditions have also been studied by the previous researchers [810]. However, in most of the cases
the steels were processed in rolling route, either in
direct quenched (DQ) technique or in rolled quenched
(RQ) conditions [9,10]. On the other hand, another
processing route, i.e. forging, has also been established
as an alternative route to rolling in processing of microalloying steels [11]. Forging route derives advantages
of structural homogeneity and better soundness due to
application of isotropic deformation. Previous attempts,
by the present authors, have been directed towards the
development of HSLA forging using primarily HSLA80 grade steels and it has been reported that variation in
post-cooling rate engenders a variety of microstructures, which alters the strength properties significantly

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A. Ghosh et al. / Materials Characterization 56 (2006) 5965

[12,13]. Later newer alloy designs have been introduced where the carbon content of the steels was
reduced to 0.006 wt.% for better weldability and corrosion resistance and it has been found that a substantial
amount of strength along with a negligible difference of
toughness value at ambient temperature and at  40 8C
can be obtained by application of a two-stage forging
operation [14]. The dislocation substructure, along with
fine microalloying precipitates resulted from thermomechanical controlled processing, is mainly responsible
for achieving high strength level and toughness of such
ultra-low carbon HSLA steel. The effects of cooling
rates on structure and properties of HSLA-100 or
HSLA-80 grade steels have been reported elsewhere
[15,16]. However, the effect of cooling rates on ultralow carbon HSLA-100 grade steel has not been explored much.
In the present study the carbon content of a HSLA100 grade steel has been lowered down to 0.005 wt.%
and a two-stage controlled forging operation was
applied. Subsequently, the forged slabs were cooled in
different cooling media. The present study evaluates the
structure and properties of this ultra-low carbon steel
processed by this forging technique.
2. Experimental procedure
In this investigation an ultra-low carbon steel was
melted in an air induction furnace and cast in a metal
mould. The chemical composition of the steel, as analyzed in Quantovac and LECO, is shown in Table 1.
Ingots of 50  50 mm cross section were reheated at
1200 8C for 2 h. Forging was carried out in a one-ton
capacity down stroke power hammer in two stages. In
stage I, 50% deformation was achieved by six repeated
strokes in the temperature range of 11001050 8C to
reduce the cross section of the slab to 35  35 mm. In
Stage II another 50% deformation was achieved by
similar six repeated strokes in the temperature range
of 850800 8C to obtain the final cross section of
25  25 mm. Subsequently, the forged slabs were subjected to water quenching (WQ), air cooling (AC) or
sand cooling (SC). Temperatures at different stages of
forging and during cooling were measured by thermoTable 1
Chemical composition of the steel (wt.%)
C

Si Mn Cr Mo Ni Cu Ti Nb Al V

# C. E.

0.005 0.009 0.006 0.28 1.23 0.57 0.55 3.50 2.1 0.01 0.05 0.02 0.005 0.85
#C:E: C Mn Si = 6 Ni Cu = 15
Cr Mo V = 5 0:85:

Fig. 1. Schematic diagram of controlled forging operation.

couples inserted into the forged bars and also by infrared pyrometer (MINOLTA/LAND-52 CYCLOPS-52).
The schematic diagram of the forging operation is
shown in Fig. 1. Optical metallographic samples prepared by conventional grinding and polishing techniques were etched with 2% nital solution and observed
in a light microscope. Thin foils for transmission electron microscopy (TEM) were prepared by twin jet
polishing in an electrolyte of 90% acetic acid and
10% perchloric acid. Thin samples were observed in a
Transmission Electron Microscope (Philips CM200
with EDAX) at 200 kV operating voltage. The chemical
compositions of precipitates were determined by
energy dispersive X-ray (EDS). Tensile testing was
carried out in an Instron tensile testing machine
(Model No. 4204) keeping a constant cross head
speed of 8.3  10 3 mm/s. Standard impact specimens
(ASTM; vol. 03.01: E2396) were prepared and
Charpy impact testing was carried out at room temperature and at  40 8C.
3. Results and discussion
3.1. Microstructure
The optical microstructures of the steel at various
post-cooling conditions show mainly ferritic structure,
Fig. 2. An overall fine structure (25 Am grain size) has
been obtained in the steel at different cooling rates from
a final forging temperature of 800 8C and the structural
fineness has been increased with increasing cooling
rate. The fine grain structure is due to the contribution
of the second stage deformation in controlled thermomechanical processing. Prior austenite grain boundaries
have not been observed for any post-cooling conditions, Fig. 2.

A. Ghosh et al. / Materials Characterization 56 (2006) 5965

61

austenite. Hence, the diffusion of carbon has become


favorable at high temperature and facilitates the
formation of polygonal or quasi-polygonal ferrite.
Polygonal ferrite generally starts to nucleate at prior
austenite grain boundaries and grow into the grains.
Hence, a predominant polygonal ferrite structure results
in the absence of prior austenite grain boundaries,
Fig. 2b and c.
It is interesting to observe in optical micrographs
(Fig. 2) some dark particles are randomly distributed in

Fig. 2. Optical micrographs of the steel at different post-cooling rates


(a) 35 8C/s (water-quenched) (b) 1.15 8C/s (air-cooled) (c) 0.68 8C/s
(sand-cooled).

TEM examination shows an acicular ferrite structure


at a faster cooling rate of 35 8C/s, Fig. 3a. At cooling
rates of 1.15 and 0.68 8C/s the structure is polygonal or
quasi-polygonal ferrite, Fig. 3b and c. Faster cooling
from the 800 8C final forging temperature suppressed
the formation of polygonal ferrite and has favored
the formation of acicular ferrite. The slower cooling
rates of 1.15 and at 0.68 8C /s from the final forging
temperature of 800 8C have allowed sufficient time to
pass into the high temperature transformation region of

Fig. 3. Bright field TEM of the steel at different post-cooling rates


(a) 35 8C/s (b) 1.15 8C/s (c) 0.68 8C/s.

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A. Ghosh et al. / Materials Characterization 56 (2006) 5965

steel is shown in the electron images, Fig. 6a and b. In


the sand-cooled steel similar types of globular or
chunky-shaped second phase particles were observed
and are shown in the bright field image with inset
SADP, Fig. 7a. The dark field is taken with the arrowed
(101) martensite spot and shown in Fig. 7b.
This steel contains microalloying elements of Nb
and Ti which are well known as strong carbide formers.
In low carbon steel these microalloying elements form
fine carbide and carbonitride precipitates, which
enhance the strength of the steel [18,19]. It is obviously
interesting to explore the precipitation behaviour of
such microalloying elements when the carbon content
of the steel is 0.005 wt.%. The bright field images of the
steel cooled at 35 8C/s show fine microalloying carbide
and carbonitride precipitates 2030 nm in size with
regular geometric shapes in the dislocated acicular ferrite lath, Fig. 8a. The precipitate size increases at
1.15 8C/s post-cooling rate (25 45 nm in size) and
their occurrence is mainly onto the dislocations,
Fig. 8b and c. In the steel sand-cooled at 0.68 8C/s
these precipitates become larger in size (30 90 nm) and
a low dislocation density is observed in the polygonal
ferrite, Fig. 8d. EDS analyses were performed for the
Fig. 4. Bright field TEM shows interlath dark particles (arrowed) at
different cooling rates. (a) 35 8C/s (b) 1.15 8C/s.

the matrix; these are generally second phase particles as


observed by earlier workers in low carbon and ultra-low
carbon HSLA steels [214]. Krauss and his colleagues
[2,3] have identified these second phase particles as
martensite austenite (MA) constituents or retained austenite, whereas Fonda and Spanos [17] have designated
these particles as nonaligned second phase particles in
ultra-low carbon steels.
In the present investigation TEM was employed to
identify these second phase particles in this ultra-low
carbon steel. At magnified bright field image, a high
dislocation density in the acicular ferrite lath has been
observed along with thin dark interlath regions, Fig. 4a.
The dislocations in the acicular ferrite lath are seen to
interact with fine microalloying precipitates. The interlath dark regions have become globular or chunky
shaped at 1.15 8C /s cooling rate and these particles
are probably MA constituents, Fig. 4b. The magnified
bright field image of air-cooled steel shows twinned
martensite in the interlath regions along with inset
selected area diffraction pattern (SADP), Fig. 5a. The
dark field is taken with the arrowed (101) twinned
martensite spot and shown in Fig. 5b. The separations
of the twins are found to be 69 nm. The presence of
retained austenite in the interlath region of air-cooled

Fig. 5. TEM shows twinned martensite in the interlath dark regions of


air-cooled steel. (a) Bright field with inset SADP. (b) Dark field.

A. Ghosh et al. / Materials Characterization 56 (2006) 5965

63

ular ferrite structure obtained at rapid cooling from the


800 8C final forging temperature. The strength value
drops on slower cooling in air or sand air cooling due
to the predominantly polygonal ferrite structure which
contains a lower less dislocation density and coarsened
microalloying precipitates.
The effect of cooling rate and impact toughness
values at ambient and sub-ambient temperatures are
shown in Fig. 10. For the air-cooled steel, the room
temperature toughness was 175 J and dropped slightly
to 158.15 J at  40 8C, Fig. 10. The ambient temperature toughness value was nearly 33% lower for the
water-quenched sample compared to that of the aircooled sample. No significant change in toughness
was observed between air and sand-cooled steel at
ambient and sub-ambient temperatures.
The most interesting result is that the toughness of
this steel remained almost unchanged from ambient
temperature and  40 8C for different post-cooling
conditions due to the ultra-low carbon content of the
steel. The fine-grained polygonal ferrite structure
obtained by controlled thermo-mechanical processing
has resulted in a high toughness value at the slower
cooling rates. A comparatively lower toughness value
Fig. 6. TEM shows retained austenite in the interlath dark regions of
air-cooled steel. (a) Bright field. (b) Dark field with (002)g reflection.

cuboid or rectangular shaped particles; one of these is


shown in Fig. 8e. From the EDS it is seen that the
precipitate is enriched with Ti, Nb and also Cu. Hence,
it is a complex type of precipitate which combines
Ti/Nb carbide or carbonitride along with Cu.
4. Mechanical properties
The effect of cooling rate on tensile properties of
the steel is shown in Fig. 9. The UTS and YS values
obtained in water-quenched steels are 974 and 888 MPa,
respectively, which are well above of the commercial
HSLA-100 grade steel [1]. The strength value drops to
863 MPa UTS and 704 MPa YS on air cooling. However, the percent in elongation in air-cooled steel has
been increased to 19.1% from the 15.3% value observed for the water-quenched steel. The strength
values change marginally when the post-cooling rate
is further decreased to 0.68 8C/s. The UTS and YS
values obtained in sand-cooled steel are 868 and
726 MPa along with 21.4% elongation.
The high strength in water-quenched steel is mainly
due to the fine grain structure obtained by the controlled forging operation and the highly dislocated acic-

Fig. 7. TEM shows MA constituents in sand-cooled steel. (a) Bright


field with inset SADP. (b) Dark field.

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A. Ghosh et al. / Materials Characterization 56 (2006) 5965

Fig. 8. TEM shows precipitates in the steel at different post-cooling rates. (a) Bright field at 35 8C/s. (b) Bright field with SADP inset at 1.15 8C/s.
(c) Dark field of (b) with arrowed precipitate spot in SADP. (d) Bright field at 0.68 8C/s. (e) EDS from a precipitate.

at the higher post-cooling rate may be due to the


predominantly acicular structure in the steel.
5. Conclusions
The following conclusions can be drawn from this
present study:
(1) By applying controlled thermo-mechanical processing a fine-grained structure has been obtained
in this steel. The transformation product obtained

Fig. 9. Effect of cooling rate on tensile properties of the steel.

at a fast post-cooling rate (water cooling) is predominantly acicular ferrite. The microstructure
changes to polygonal or quasi-polygonal ferrite
when the cooling rate is slowed down to 1.15 or
0.68 8C/s by air or sand cooling, respectively.
(2) The strength level obtained at the faster cooling
rate of 35 8C/s is 974 MPa UTS and 888 MPa
YS, respectively, along with 15.3% elongation.
This high strength level has been obtained due to
the highly dislocated acicular ferrite structure

Fig. 10. Effect of cooling rate on impact toughness of the steel.

A. Ghosh et al. / Materials Characterization 56 (2006) 5965

along with fine precipitation of microalloying


carbides/carbonitrides. The strength value drops
to 863 MPa UTS and 704 MPa YS at a slower
cooling rate of 1.15 8C/s with an increase in
ductility (19.1% elongation). The less dislocated
polygonal ferrite structure obtained at the slower
cooling rate decreases the strength value with an
increase in ductility. The strength value remained
almost unchanged with a further decrease in cooling rate to 0.68 8C/s as the predominant microstructure remained polygonal ferrite.
(3) At slower post-cooling rates, high impact toughness values obtained at ambient temperatures and
at  40 8C due to the formation of a polygonal
ferrite microstructure. Due to the ultra-low carbon
content of the steel the difference in impact
toughness values at ambient and at  40 8C temperature was found to be negligible for steels
cooled in air or in sand.
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