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Materials Science & Engineering A 590 (2014) 323–328

Contents lists available at ScienceDirect

Materials Science & Engineering A


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

High toughness in the intercritically reheated coarse-grained (ICRCG)


heat-affected zone (HAZ) of low carbon microalloyed steel
Jun Hu a,n, Lin-Xiu Du a, Jian-Jun Wang b, Hui Xie a, Cai-Ru Gao a, R.D.K. Misra c
a
The State Key Laboratory of Rolling and Automation, Northeastern University, Shenyang 110819, China
b
Institute of Materials Research, School of Material and Metallurgy, Northeastern University, Shenyang 110819, China
c
Laboratory for Excellence in Advanced Steel Research, Center for Structural and Functional Materials, University of Louisiana at Lafayette, Lafayette,
LA 70504-4130, USA

art ic l e i nf o a b s t r a c t

Article history: Motivated by the small lattice mismatch between ferrite and vanadium nitride (VN), we describe here
Received 7 October 2013 the welding thermal cycle simulation that provides high toughness in the ICRCG HAZ of low carbon V–N
Accepted 21 October 2013 steel. This unique behavior is attributed to the formation of ultra-fine grained ferrite along prior austenite
Available online 26 October 2013
grain boundaries generated by the first pass welding thermal cycle with high misorientation boundaries,
Keywords: where V(C, N) precipitates provide potential nucleation sites for ferrite, leading to extraordinary
ICRCG HAZ refinement of martensite/austenite (M/A) constituent. Nitrogen stimulates the precipitation behavior
Peak temperature of V(C, N). The nucleation of high density of V(C, N) precipitates consumes carbon-content in the
Toughness austenite, leading to decrease in the carbon-content in the M/A constituent, with consequent decrease in
Ultra-fine grain
hardness. The increase in toughness is explained in terms of Griffith's crack propagation theory.
V–N microalloyed steel
& 2013 Elsevier B.V. All rights reserved.

1. Introduction austenite grain size, austenite preferentially nucleates and grows


along the prior austenite grain boundaries formed by the first pass
The high strength low alloy (HSLA) steels are characterized by welding thermal cycle (PAGB) and to some extent, along the
high strength–high toughness combination. However, the high bainite lath boundaries. These austenite islands are enriched in
strength–toughness combination can be deteriorated by welding carbon because of high diffusivity of carbon and higher solubility
thermal cycles leading to poor toughness in the heat affected zone in austenite, and are transformed to hard and brittle M/A con-
(HAZ) [1]. In single-pass welding, the low toughness region is stituents during the subsequent cooling, leaving a necklace type of
generally associated with the coarse-grained HAZ (CG HAZ) M/A constituent along the PAGB. The carbon content in M/A
because of the formation of undesirable microstructure, such as particles was experimentally observed to be  1.07–1.32 wt% even
coarse ferrite side-plates (upper bainite and Widmanstatten fer- if the overall carbon content of steel was  0.06 wt% [1,3]. The
rite) [2,3]. In the case of two overlaying beads, the CG HAZ of the ICRCG HAZ is generally characterized by lower toughness and is
first pass is reheated at different peak temperatures (Tp2) depend- inferior to UACG HAZ in low carbon steel. It was proposed that
ing on its distance from the fusion line of the second bead and can M/A constituent along the PAGB is the primary reason for the loss
be appropriately characterized as follows [4,5]: (1) a subcritically in toughness [1,3,5–7].
reheated CG HAZ (SRCG HAZ) region reheated above 500 1C and The increase in the strength of HSLA steels is primarily
below Ac1, (2) an intercritically reheated CG HAZ (ICRCG HAZ) obtained through precipitation hardening and refinement of grain
region reheated between Ac1 and Ac3, (3) a supercritically size by microalloying with Nb, V, and Ti, individually or in
reheated CG HAZ (SCRCG HAZ) region reheated between Ac3 and combination. The Nb, V, and Ti atoms in solution suppress the
1100 1C, and (4) an unaltered CG HAZ (UACG HAZ) region that is transformation of austenite to ferrite, while the microalloyed
not reheated or reheated above 1100 1C. precipitates and inclusions decrease the stability of austenite [8].
In the ICRCG HAZ, formed by multipass welding, parts of the It is proposed that in comparison to Nb(C, N) and Ti(C, N), Ti oxide
microstructure are transformed into austenite because second- and V carbonitride have relatively greater potential in nucleating
weld bead reheats the CG HAZ structure into the austenite/ferrite ferrite. The small lattice mismatch of VN (lattice parame-
two-phase field. On reheating a CG HAZ with a large prior ters ¼0.4139 nm) with ferrite (lattice parameters ¼0.2865 nm)
between (100)VN//(100)α planes facilitates ferrite nucleation
[9–15]. V coupled with N is considered to be effective in stimulat-
n
Corresponding author. Tel.: þ 86 24 83680250; fax: þ86 24 23906472. ing precipitation and enhancing grain refinement. The addition of
E-mail address: hujunral@163.com (J. Hu). N to the V-microalloyed steels decreases the incubation period for

0921-5093/$ - see front matter & 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.msea.2013.10.062
324 J. Hu et al. / Materials Science & Engineering A 590 (2014) 323–328

the precipitation of V carbonitride and increases the volume 1000 1C, and 1300 1C at the rate of 100 1C/s, and then held for
fraction because of higher solubility product of V and N [16]. With 1 s. The t8/5 was 20 s with the finish controlled temperature of
this in mind, we describe the effect of V(C, N) precipitates on 250 1C, and the welding input was equivalent to that in-service
microstructural evolution and toughness in ICRCG HAZ, an aspect welding of 26.0 kJ/cm. The experimentally measured welding
that does not seem to have been documented or explored. thermal cycle curves for HAZ simulations are shown in Fig. 1. Each
We have studied the microstructure, toughness, and hardness condition was studied five times. The temperature was controlled
in reheated CG HAZ of low carbon V–N steel under different Tp2 with an R-type thermocouple wire welded in the middle of the
conditions to elucidate the determining role of V(C, N) precipitates specimen and the accuracy was 71 1C during isothermal holding
on austenite transformation behavior. and 73 1C during the non-isothermal process. There was no
temperature gradient within the 5 mm radius. Therefore, the
microstructural observations and mechanical properties were
2. Experimental studied in this range.

2.1. Materials 2.3. Mechanical properties

The nominal chemical composition of the steel (in weight%) The specimens subjected to welding thermal cycle were
was 0.058 C–0.15 Si–1.8 Mn–0.002S–0.03 Al–0.12–0.18V, and machined to standard Charpy v-notch samples with the dimen-
0.015–0.02N, balance was Fe. The experimental steel was melted sions of 10 mm  10 mm  55 mm. The impact tests were con-
in vacuum induction furnace and cast as 150 kg ingot. The steel ducted at  20 1C using Instron Dynatup 9200 series instrumented
was controlled-rolled and subjected to two stages of continuous drop weight impact tester, consistent with ASTM E23 specification.
cooling [17]. The samples were cooled to  5 1C below the temperature of
Thermocalc calculations combined with TCFE6 database indi-  20 1C to take into consideration the rise in temperature during
cated the volume fraction of V(C, N) precipitates in equilibrium to the transfer of sample to the Charpy v-notch impact tester. The
be 0.16% at 800 1C. The start and end temperatures of transforma- Vickers microhardness was measured utilizing an FM700
tion of ferrite to austenite are 654 1C (Ae1) and 840 1C (Ae3). hardness-testing machine employing a load of 500 g and the
Therefore, Tp2 of 600 1C, 800 1C, 1000 1C, and 1300 1C are within indentation area covered the typical microstructural constituent.
the SRCG HAZ, ICRCG HAZ, SCRCG HAZ, and UACG HAZ, The toughness and hardness values data presented here are an
respectively. average of five measurements.

2.2. Weld simulation procedure 2.4. Microstructural characterization

The welding thermal cycle simulation was conducted using a The specimens for microstructural studies were polished using
thermo-mechanical simulator. The simulated specimens were cut standard metallographic procedure and etched with a 4 vol% nital
from the middle of as-rolled steel plate along the transverse solution and observed using a Leica DMIRM optical microscope
direction and then machined to dimensions of 11 mm  11 mm  (OM) and Zeiss Ultra 55 scanning electron microscope (SEM). The
55 mm. The temperature of welding thermal cycle was controlled chemical composition of the precipitates was determined by
by closed-loop control system using the 2-dimensional Rykalin energy-dispersive X-ray spectroscopy (EDX). For EBSD, the sample
mathematical model to simulate the welding process of plates was electrolytically polished in a solution of perchloric acid and
with 20 mm thickness. The mechanism of heating was ohmic ethyl alcohol. The EBSD maps were scanned by Flamenco software
heating and the mechanism of cooling was combined with natural with the step size of 0.3 μm, and analyzed by HKL-Channel 5 soft-
cooling and nitrogen cooling. In the first cycle, the pre-heating ware. The element analysis was studied by JEOL JXA-8230F type
temperature was chosen as 20 1C. The specimens were heated EPMA equipped with wavelength dispersive X-ray spectrometer
at the rate of 100 1C/s to 1300 1C, and then held for 1 s. The t8/5 (WDX). The carbon concentration map is a relative distribution
(time taken to cool from 800 1C to 500 1C) was 20 s with the rather than the actual distribution. The analysis of microcracks in
interpass temperature of 150 1C, and the welding input was impact toughness tested samples was conducted near the fracture
equivalent to that of in-service welding of 38.1 kJ/cm. In the surface. The polished samples were etched with a 4 vol% nital
second cycle, the specimens were heated to 600 1C, 800 1C, solution and observed by using a FEI Quanta 600 SEM.

Fig. 1. Experimentally measured welding thermal cycle curves for HAZ simulations: (a) two passes welding and (b) enlarged image of the second pass welding.
J. Hu et al. / Materials Science & Engineering A 590 (2014) 323–328 325

PAGB
Few ferrite at PAGB

Acicular ferrite

Granular bainite
10μm 10μm

Ferrite along PAGB


A large amount of
Ferrite along PAGB

Tempered granular bainite

Tempered acicular ferrite 10μm 10μm

Ferrite

Pearlite

10μm 10μm

Fig. 2. OM micrographs and EBSD image quality maps with grain boundary misorientation distribution: (a) OM micrograph at Tp2 150 1C; (b) EBSD map at Tp2 150 1C; (c) OM
micrograph at Tp2 800 1C; (d) EBSD map at Tp2 800 1C; (e) OM micrograph at Tp2 1000 1C; and (f) EBSD map at Tp2 1000 1C (For interpretation of the references to color in this
figure, the reader is referred to the web version of this article.).

3. Results and discussion

3.1. Microstructural evolution

Optical micrograph and EBSD image quality maps with grain


boundary misorientation distribution are presented in Fig. 2. In the
image quality map, the red lines represent the low misorientation
boundaries of 2–151 between two adjacent grains and the black
lines correspond to the high misorientation boundaries of 151 and
ICRCG HAZ larger than 151. The high misorientation grain/packet boundaries
can efficiently deflect or even arrest the propagation of cleavage
microcracks, whereas the low misorientation boundaries have less
ability to deflect the crack. As shown in Fig. 2a and b, the
microstructure consists of acicular ferrite, granular bainite, and a
small amount of polygonal ferrite along PAGB after first pass
Fig. 3. Impact absorbed energy at different Tp2 for simulated HAZ specimens. welding cycle with the interpass temperature of 150 1C, which is
326 J. Hu et al. / Materials Science & Engineering A 590 (2014) 323–328

M/A along PAGB

Ferrite along PAGB Similar C content

M/A inside PAGB

Acicular ferrite inside PAGB


5μm 5μm
Fig. 4. SEM micrograph and EPMA C distribution map for ICRCG HAZ specimen: (a) SEM micrograph and (b) EPMA C distribution map (For interpretation of the references to
color in this figure, the reader is referred to the web version of this article.).

V(C, N)

Ferrite along PAGB

2μm 500nm
Fig. 5. SEM micrograph and precipitate morphology for ICRCG HAZ specimen: (a) SEM micrograph and (b) precipitate morphology and chemical composition.

described as Tp2 of 150 1C without reheating. At Tp2 of 800 1C, the and acicular ferrite plates are in blue. The M/A constituents both
acicular ferrite and granular bainite distributed inside PAGB are along PAGB and interior PAGB are in yellow, thus the C-contents of
tempered, and the granular bainite along the PAGB is re- M/A constituent at and inside PAGB are similar. A very small area of
austenized and transformed to the  1–3 μm ultra-fine grain M/A constituent are in red. Therefore, the carbon concentration is
ferrite with high angle grain boundaries. Moreover, the fraction low at PAGB. Fig. 5 shows the  20–30 nm V(C, N) precipitates are
of high angle grain boundaries in unit area of ultra-fine grain present within the ferrite grain along PAGB and act as nucleation
ferrite is higher than the nearby acicular ferrite, as shown in Fig. 2c sites for fine ferrite. In our case, to the fine prior austenite grain size
and d. At Tp2 of 1000 1C, the austenization is nearly completed and and high density of ferrite nucleation sites in ICRCG HAZ, ultra-fine
fine austenite nucleates at PAGB and bainite laths. Furthermore, ferrite is nucleated along the PAGB.
the prior austenite grain size is further refined by recrystallization. SEM micrographs showing impact fracture surface morphology
On the subsequent cooling process, the polygonal ferrite, small and secondary cracks propagation paths underneath the fracture
degenerated pearlite, and M/A constituents are formed, as shown surface of specimen's radial zone at different Tp2 are presented in
in Fig. 2e and f. Fig. 6. The microstructure consists of acicular ferrite, granular
bainite, and a small amount of polygonal ferrite at Tp2 of 150 1C.
3.2. Mechanical properties The acicular ferrite intragranularly nucleates on V(C, N) precipi-
tates, and the granular bainite nucleates and grows from the PAGB
Fig. 3 shows the impact energy at different Tp2 for simulated [18,19]. Compared to acicular ferrite, granular bainite contains
HAZ specimens. The impact absorbed energy is 51.6, 56.5, 60.8, lower density of high angle grain boundaries. Therefore, the
111.0, and 48.6 J at Tp2 of 150 1C, 600 1C, 800 1C, 1000 1C, and microcrack propagates straight in granular bainite and leads to
1300 1C. The hardness is 260.17, 245.07, 257.13, 267.19, and relatively large cleavage facet size of the fracture surface, while the
253.2 HV, respectively, with the error in the range of 76 HV. propagation of the microcrack is deflected and finally arrested by
Compared to UACG HAZ, the hardness decreases and toughness acicular ferrite, resulting in small cleavage facet size, as shown in
increases in SRCG HAZ because of the tempering effect, while the Fig. 6a and b. At Tp2 of 800 1C, the granular bainite along the PAGB
toughness improvement in ICRCG HAZ is abnormal. The hardness is re-austenized and transformed to the  1–3 μm ultra-fine grain
increases in ICRCG HAZ and further enhances in SCRCG HAZ ferrite with high angle grain boundaries. As a consequence, the
because of the strengthening mechanism from the high angle microcracks are arrested by ultra-fine grain ferrite, and the
grain boundaries of fine ferrite. dimples and small cleavage facets of the fracture surface are
formed. Furthermore, the transgranular fracture characteristic
3.3. Microstructural characteristic-toughness relationship demonstrates high toughness of ultra-fine grain ferrite along
PAGB, as shown in Fig. 6c and d. It is proposed that the cleavage
Fig. 4 shows the SEM micrograph and EPMA carbon- fracture initiation can be dominated both by the size of crack
distribution map for ICRCG HAZ specimen. The M/A constituents initiators and by the fracture facet size, since the fracture facet size
are smaller than 1 μm and are uniformly distributed along dominates the critical condition for the propagation of micro-
PAGB and in the vicinity of fine ferrite. In the EPMA map, the cracks. The microstructure for a finer fracture facet size can
blue regions represent the low carbon content, yellow the medium prevent unstable cleavage fracture, even if relatively large crack
carbon content, and red represents high carbon content. The ferrite initiators exist. Crack arrestability is the principal factor in the
J. Hu et al. / Materials Science & Engineering A 590 (2014) 323–328 327

Large cleavage facet size

Microcrack propagating straightly


in granular bainite
20μm 5μm

Small cleavage facet size

Microcrack arrested by
ultra-fine grain ferrite at PAGB

Dimples

20μm 5μm

20μm 5μm
Fig. 6. SEM micrographs showing impact fracture surface morphologies and secondary cracks propagation paths underneath the fracture surface of specimens' radial zone at
different Tp2: (a) fracture surface at Tp2 of 150 1C; (b) propagation path at Tp2 of 150 1C; (c) fracture surface at Tp2 of 800 1C; (d) propagation path at Tp2 of 800 1C; (e) fracture
surface at Tp2 of 1000 1C; and (f) propagation path at Tp2 of 1000 1C.

process of cleavage fracture to failure [20]. It is also known that the in SCRCG HAZ, can be considered to represent the optimal
formation of ultra-fine ferrite can enhance the impact toughness schedule for heat treatment of low carbon V–N steel.
significantly [21]. Therefore, the improved toughness in ICRCG The M/A constituent and V(C, N) precipitates are crack initia-
HAZ is predominately attributed to the formation of the ultra-fine tors because of higher hardness than the surrounding substrate.
grain ferrite along PAGB in place of original granular bainite. At Tp2 According to the Griffith crack propagation theory, the coarse hard
of 1000 1C, the fine polygonal ferrite provides high cleavage phase assists microcrack initiation by reducing the initiation
fracture resistance as exhibiting the zig zag-shaped microcrack energy, especially when they are aggregated. For the dispersive
propagating path, and then the ductile dimples, tear ridges, and and granular phase, the microcrack size can be roughly regarded
very small cleavage facets dominate the entire radial zone of the as the maximum diameter, and the microcrack initiation energy
fracture surface (Fig. 6e and f). The welding thermal cycle para- decreases with increase in diameter [22]. The 20–30 nm V(C, N)
meters that provide maximum hardness-toughness combination precipitates are not detrimental to impact toughness because of
328 J. Hu et al. / Materials Science & Engineering A 590 (2014) 323–328

their small size. The M/A constituents, as the voids initiation sites, These welding thermal cycle parameters can also provide
their hardness, size, and area fraction are three important factors optimal schedule for hot-treatment of low carbon V–N steel.
that determine the impact toughness. The size and distribution of (3) The large size and necklace type of M/A constituent along the
M/A constituents at PAGB are partially influenced by the stability PAGB is hardly observable in the ICRCG HAZ. The  20–30 nm
of the under-cooled austenite. During the cooling process, under- V(C, N) precipitates are the nucleation sites of the fine ferrite
cooled austenite with high carbon concentration and Nb–Ti along PAGB, and leading to extraordinary refinement of M/A
soluble microalloy content stabilizes austenite until the martensite constituent to smaller than 1 μm. N stimulates the precipita-
transformation start temperature, such that the coarse M/A con- tion behavior of V(C, N). The nucleation of high density of V(C,
stituents are formed. In contrast, in the low C austenite with N) precipitates consumes the C-content in the austenite,
effective V(C, N) ferrite nucleation sites, the ferrite that is first leading to decrease in the hardness of M/A constituent due
nucleated divides the undercooled austenite into small segments to weak C concentration.
leading to refinement of M/A constituent. It is also suggested that (4) Compared to the low carbon Nb–Ti steel with lowest tough-
the hardness of M/A constituent increases monotonously with ness in ICRCG HAZ, the toughness in ICRCG HAZ is improved in
increase in C content [23]. High N-content stimulates the pre- low carbon V–N steel. This unique behavior is attributed to the
cipitation behavior of V(C, N). The formation of large amount of V formation of ultra-fine grained ferrite along PAGB with high
(C, N) precipitates consumes C-content in the austenite, and then misorientation boundaries in place of granular bainite with
the hardness of M/A constituent along PAGB decreases due to the low misorientation boundaries, and the crack propagation
low C concentration. energy is increased. Furthermore, crack initiation energy is
In summary, the impact toughness depends on the microcrack enhanced because the generation of large and hard M/A
initiation energy and microcrack propagation energy. For the crack constituent is avoided.
initiation energy, we have interestingly observed that the V(C, N)
precipitates significantly contribute to impact toughness in the
ICRCG HAZ through their beneficial effect of high density of ferrite
nucleation sites that divides the undercooled austenite into fine
segments, as a consequence of which M/A constituent is refined. Acknowledgments
Furthermore, the V(C, N) precipitates lower the C-concentration in
M/A constituent and decrease its hardness. The crack propagation The authors gratefully appreciate the financial support by the
energy is determined by the density of the high angle grain National Key Technology Research and Development Program of
boundaries. In this regard, the acicular ferrite and polygonal ferrite the Ministry of Science and Technology of China (Grant no.
have high angle grain boundaries, while the packets of granular 2011BAE13B03).
bainite consist of low angle grain boundaries. Furthermore, the
microcracks can be arrested by fine-grained ferrite (Fig. 6d and f),
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