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Afshin Mehrabia , Hassan Sharifia , Mohsen Asadi Asadabadb , Reza Amini Najafabadic , Ali Rajaeed
a Department of Materials Science and Engineering, Shahrekord University, Shahrekord, Iran.
b NuclearScience and Technology Research Institute, Tehran, Iran.
c Department of Metallurgy and Materials Engineering, Golpayegan University of Technology, Golpayegan, Iran.
d Department of Materials and Polymer Engineering, Hakim Sabzevari University, Sabzevar, Iran.
phasized that IQ heat treatment was one of the best methods ond and third treatments were IQ treatments, which were
for the formation of dual-phase microstructure. The simpli- applied for the formation of ferritic–martensitic microstruc-
city of thermal cycles and lack of the need for molten salt tures. The difference between the two treatments was se-
baths, which were expensive and caused environmental ha- lected as the intercritical annealing temperature. Equations
zards, made it more applicable in future applications [21]. (1) and (2) were used to determine the critical temperatures
To date, IQ treatment has not been employed to create of A1 and A3 lines, which are lower and upper transforma-
the dual-phase microstructure for AISI 4340 steel. The aim tion temperatures, respectively, based on the contents of C,
of this study is to investigate the effect of inducing dual- Mn, Si, Ni, Mo, Cr, As, W and V (wt.%) [23].
phase microstructure on mechanical properties (tensile
strength, hardness, elongation and especially impact en- A1 ¼ 723 10:7Mn 16:9Ni þ 29:1Si þ 16:9Cr
ergy) of AISI 4340 steel via two different intermediate þ290As þ 6:38W ð1Þ
quenching treatments. Furthermore, the results of this in-
vestigation were compared with conventional Q&T and pffiffiffi
A3 ¼ 910 203 C 15:2Ni þ 44:7Si þ 104V
tempered IQ treatments. Finally, the optimum conditions
for achieving the highest impact energy are revealed. þ31:5Mo þ 13:1W ð2Þ
Using the values in Table 1, A1 and A3 critical temperatures
2. Experimental procedure were calculated as 711.1 and 781.5 8C, respectively.
Heat treatment samples were prepared by cutting AISI 4340 To reveal the microstructures of the heat-treated and nor-
steel rolled sheet with 4 mm thickness. The chemical com- malized samples via optical microscopy, the ground and
position of the steel sheet was determined by quantometer polished surfaces of the samples were immersed in Nital
analysis and is given in Table 1 according to a previous etch solution (96 ml ethanol and 4 ml nitric acid) for 12 s
study [22]. at room temperature.
Image-J Software was employed to analyze the metallo-
2.2. Heat treatment graphic images, determine the size of ferrite and martensite
phases, and calculate the volume fraction of each phase.
The primary samples were subjected to normalizing treat- The procedure was repeated on five different spots of each
ment to obtain Widmanstätten ferrite and fine microstruc- specimen.
ture. The samples were heated in a furnace at 900 8C for To confirm the identification of the ferrite and martensite
1 h and were kept to cool down to reach room temperature. phases, microhardness testing was carried out using the
To compare the microstructural and mechanical properties, Vickers method (HV). The indentation force was 100 g for
five different treatments were designed with the conditions 15 s and it was replicated at five different points.
presented in Table 2. The aim was to induce five different
microstructures of tempered martensitic, dual-phase micro- 2.4. Determination of mechanical properties
structures with different volume fractions of ferrite and
martensite, and tempered dual-phase microstructures. The The surfaces of the samples with different microstructures
first treatment was a conventional Q&T treatment. The sec- were ground by 1000-Grit sandpaper and the hardness of
Table 1. Chemical composition of the AISI 4340 steel used in this study.
Alloy elements C Mn Cr Ni Si Mo S P Fe
wt.% 0.38 0.68 0.98 1.805 0.32 0.31 0.018 0.011 Balance
the samples was measured according to the Rockwell C austenite phase (which is transformed to martensite later)
method (HRC). To increase the accuracy of the measure- was affected by ferrite growth [24].
ments, the hardness tests were performed on five spots and Figure 1d shows a micrograph of IQ2. The microstruc-
the average values were reported. ture also consists of a mixture of ferrite and martensitic
To study the tensile properties of the specimens, tensile phases, and martensite in this microstructure is composed
testing was carried out in accordance with the ASTM E8M of a mixture of lathy, island-like and plate-like morpholo-
standard; the test was performed using a GUNT Hamburg gies in the ferrite grain boundaries and between the ferrite
tensile machine (model WP 310, Germany) at room tem- grains. As shown in Fig. 1d, most of the grains have polygo-
perature at a speed of 20 mm min–1. nal morphology. This can be explained by the fact that IQ2
Moreover, impact test samples were prepared according underwent a higher intercritical temperature with respect
to ASTM E23 standard and tested on a Santam impact tester to IQ1 and experienced a longer path compared to IQ1 dur-
(model 300AE, Iran) at room temperature using pendulum ing cooling. As a result, needle-like ferrite grains, which
energy of 300 J. were created by IQ2 treatment, experienced more epitaxial
growth. However, the extent of epitaxial growth is low en-
2.5. Fractography ough in a way that it does not result in the growth of ferrite
grains. Additionally, as shown in Table 3, the average dia-
Fracture surfaces of the tensile test samples were examined meter of ferrite grains in IQ1 is larger than that of IQ2.
and analyzed using Zeiss scanning electron microscope Furthermore, in some regions of the IQ2 microstructure,
(SEM) (model EVO 18, Germany). the epitaxial growth of ferrite grains near two ferrite
wedges caused the formation of large polygonal ferrite
grains. Shi et al. demonstrated the occurrence of this growth
3. Results and discussion in HSLA dual-phase steels and described its effect on the
mechanical properties [3, 25].
3.1. Microstructural analysis During the first cycle of IQ treatment, the specimen was
quenched in oil from the austenite region to form martensite
Figure 1a shows the ferritic–pearlitic microstructure of the islands in the primary austenite grains. During the second
normalized (N) sample. The bright phase is the eutectoid cycle, the specimen was heated to a certain temperature to
ferrite while the dark phase is pearlite. As is evident, the apply intercritical annealing. By heating the unstable mar-
normalizing treatment resulted in a microstructure consist- tensitic structure to the intercritical region, the martensite
ing of a mixture of pearlite and ferrite phases. By observing volume fraction reduced and the retained austenite was
the image, it can be seen that there is no pearlite band transformed to fine cementite, other carbides and/or ferrite.
spread in the rolling direction of the sample; on the con- The formed ferrites acted as the nuclei for ferrite formation
trary, it was located along the Widmanstätten ferrite [10]. in IQ. During intercritical annealing, ferrite nucleation in-
Figure 1b is a micrograph of the Q&T with a martensitic creased and finer ferrites with better dispersion resulted
structure. Coarse tempered lathy martensite and austenite due to the development of high-energy regions (regions
matrix are visible as dark and bright phases, respectively. with high dislocation density caused by martensitic trans-
During the first cycle of Q&T treatment, the microstruc- formation) and the presence of the martensite island bound-
ture consisted of coarse martensite plates. During the sec- aries. By analyzing both IQ1 and IQ2, it was found that the
ond cycle (at 210 8C), the plates were broadened, disloca- martensite phase was continuous in both of the microstruc-
tion density lowered and the carbon content of martensite tures. However, by increasing the martensite volume frac-
declined. Earlier studies reported that this phenomenon led tion in IQ2, the morphology of martensite was more similar
to higher ductility and transformation of retained austenite to island-like martensite. The major difference between the
to ferrite and cementite [16]. two microstructures was the ferrite and martensite volume
Figure 1c displays the micrograph of sample IQ1. The re- fractions, ferrite grain size and the morphologies of the
sulting microstructure consists of ferrite and martensite phases [1, 26].
phases. Ferrite grains are the bright phase and martensite By comparing Fig. 1b, c, and d, it is evident that coarse
plates are the dark phase. As can be seen, the martensite is lathy martensite was present in Q&T; while there was no
composed of a mixture of lathy and island-like morphologies evidence of martensitic plate in IQ1 and IQ2, which was
formed at the ferritic grain boundaries and between the fer- due to the fine and compact lathy martensite. Moreover, be-
rite grains. At this point, microhardness testing was em- cause the ferrite resulting from IQ1 treatment was finer, it
ployed to confirm the identification of the ferrite and marten- had lower volume fraction compared to that in the IQ2
site phases. The mean microhardness of the martensite and treatment. On the other hand, a high volume fraction of aus-
ferrite was calculated as 590 and 220 HV for IQ1, respec- tenite with larger grain size formed during the IQ treatment
tively. The values were then compared to the microstructural caused the formation of large martensite islands with more
observations and confirm the results. Due to the fact that IQ1 continuity in IQ2.
was subjected to intercritical annealing at 720 8C, this tem- Figure 1e and f shows micrographs of tempered IQ1 and
perature is considered as the low critical temperature. Since IQ2 treatments, respectively. Ferrite presents with bright
it is close to the critical temperature of A1, IQ1 experienced shading, while martensite and carbides with dark shades,
a shorter path in the intercritical region during cooling. Con- respectively. It can be seen that during the tempering treat-
sequently, the formed lathy morphology underwent low epi- ment iron and other carbides formed at the grain boundaries
taxial growth. Also, most of the ferrite grains maintained of martensite and ferrite. Also, because of the reduction of
their Widmanstätten or wedge-shaped morphology. Speich martensite volume fraction, the morphology of martensite
et al. described that during IQ treatment the distribution of islands changed and they became finer.
Fig. 1. Optical micrographs of: (a) normalized sample, (b) conventional quench and temper treatment, (c) first intermediate quenching, (d) second
intermediate quenching, (e) first intermediate quenching followed by tempering, and (f) second intermediate quenching followed by tempering.
Heat treatment Ferrite volume fraction (%) Martensite volume fraction (%) Average diameter of ferrite
grains (lm)
Q&T 0 100 –
IQ1 51 49 4.2
IQ2 39 61 3.2
IQ1&T 57 43 4.3
IQ2&T 65 35 3.2
In Fig. 1e, it is clear that in addition to the formation of morphology was finer and the dislocation density percent-
carbide and cementite at the grain boundaries, there are age was higher in IQ2. Therefore, IQ2 was harder than
many martensite islands between the ferrite grains. But in IQ1. By tempering the IQ1 and IQ2 at 210 8C, the disloca-
Fig. 1f, it can be seen that the number of martensite islands tion density in the ferrite grains decreased, resulting in low
has decreased and small islands are located among the fer- ferrite hardness, plus martensite volume fraction declined
rite grains, while the lathy martensite has remained at the and its morphology changed. Researchers have demon-
ferrite boundaries. During tempering the dual-phase micro- strated that the above-mentioned reasons can lead to a re-
structure at 210 8C, the carbon of martensite and ferrite dif- duction in the hardness of IQ1&T and IQ2&T in compari-
fused to austenite, and iron carbides formed at the grain son to IQ1 and IQ2, respectively [16, 30, 31]. Earlier it
boundaries. In fact, because of tempering, all the carbides was indicated that martensitic hardness decreased with in-
coarsened, causing carbon depletion. For this reason, there creasing martensitic volume fraction and reduction of its
exists the possibility of the transformation of unstable mar- carbon content. Additionally, by increasing the martensite
tensite and reduction of martensite volume fraction. Also, volume fraction and decreasing the ferrite grain size, more
during the tempering cycle, the closed boundaries, marten- dislocations accumulate in the ferrite grains, which annihi-
sitic islands, and plates decreased and the dislocation den- lated by tempering at 200 8C for 1 h. This increase in dislo-
sity reduced. After tempering the dual-phase microstruc- cation density led to an increase in the hardness of ferrite
tures at 210 8C, the formed or coarsened carbides have in dual-phase steels [27, 32, 33].
reduced the carbon of martensite, retained austenite and fer-
rite, causing a change in volume fraction and morphology 3.3. Tensile properties
of the unstable martensite.
Therefore, it was discovered that by tempering the dual- The data obtained from the tensile testing of the specimens
phase microstructure in the range of 200 – 600 8C for 1 h, are presented in Table 4. In this table, the highest strength
the carbon of martensite was depleted to austenite, the mor- is related to Q&T. On the other hand, among dual-phase mi-
phology of martensite changed and a fraction of austenite crostructures, IQ1 and IQ2&T have the highest and the low-
transformed to carbide, cementite or ferrite. Moreover, est strengths, respectively.
martensite volume fraction changed and the cementite in According to Table 4, it can be seen that Q&T had yield
the boundary of martensite and ferrite was coarsened. Also, and tensile strengths of 1 692.5 and 1 824.68 MPa, respec-
it was found that during the tempering, the dislocation den- tively. Hence, the sample was considered as UHSS. Low
sity in the boundary and inside the ferrite grains reduced. In elongation (8.62 %) and high hardness of Q&T implies the
fact, during the tempering process, carbides are formed in very low formability of this structure. Based on the results,
the ferrite grains, which causes the carbon to be depleted IQ1 had higher formability than Q&T since its yield
from supersaturated ferrite. Although the formation of the strength to tensile strength ratio is 0.89, which indicates
carbides in ferrite grains reduced the hardness of ferrite, the higher deformation ability of the IQ1 microstructure.
the presence of these carbides could act as obstacles against IQ2 with a ferritic–martensitic dual-phase microstructure
dislocation motion [18, 27 – 29].
3.2. Hardness
Heat treatment Yield strength (YS) Ultimate tensile strength YS/UTS ratio Elongation (%)
(MPa) (UTS) (MPa)
and hardness of 43 HRC has a lower strength and higher carbon content and dislocation density declined during tem-
hardness compared to IQ1, which is due to high martensite pering. As a result, the hardness of the IQ1 after tempering
volume fraction and elevated dislocation density in ferrite reduced by 3 HRC (i. e. IQ1&T). Of course, many fine car-
grains. bides were formed and dispersed in IQ1&T microstructure
By comparing and analyzing the heat treatment parame- in both ferrite and martensite phases. The distribution of
ters, it was determined that due to the increase in the mar- fine and hard carbide particles in both phases and the pre-
tensite volume fraction and high hardness of ferrite in IQ2, sence of island-like martensite caused the locking of many
compared to the IQ1, the hardness of IQ2 was 3 HRC high- dislocations during loading that improved the strength of
er than IQ1. This is important because martensite plays a re- IQ1&T.
inforcing role in a dual-phase microstructure and its hard- For IQ2&T, martensite carbon content decreased due to
ness affects the strength of the dual-phase steel. However, the low carbon content of martensite and ferrite, presence
with an increase in the martensitic volume fraction and of primary carbides in IQ2 microstructure, the formation
hardness of IQ2, it was expected that the strength of IQ2 of secondary carbides and growth of carbides during tem-
microstructure would be much higher than IQ1. On the con- pering. However, since the carbon content of martensite in
trary, by comparing the tensile properties it was seen that IQ2 was higher than in IQ1, after tempering treatment the
the tensile strength of IQ2 was not only equal but also lower decline of martensite volume fraction was more severe in
than IQ1 (112.6 MPa lower). This is inconsistent with pre- IQ2&T than IQ1&T. On the other side, the morphology of
vious results regarding the mechanical properties of dual- martensite in the IQ2&T changed further and the number
phase steel. Early studies claimed that by increasing the of martensite islands decreased and became finer. This
martensite volume fraction, the strength of dual-phase change in morphology facilitated dislocation motion and
steels increased but since the martensite hardness in the the annihilation of dislocations during tempering resulted
dual-phase microstructure was the controlling parameter in severe strength drop in IQ2&T. It was shown that a great
for strength, the strength of these steels did not increase in reduction of strength in dual-phase steels took place by
linear dependence. It was reported that the reduction in tempering at a certain temperature because of carbide coar-
hardness of martensite could be due to many factors includ- sening and decline of martensite volume fraction [37].
ing carbide formation during the first cycle of IQ treatment
and lack of dissolution of entire carbides during this treat-
ment [34]. The strength of dual-phase steels could be in- 3.4. Impact test
creased by improving the hardness of ferrite and martensite,
and parameters contributing to increasing dislocation den- Most of the previous studies around the AISI 4340 steel
sity in these phases [35]. For instance, by referring to the have been carried out to improve the impact properties. In
Hall–Petch equation Peng and Preban indicated that with the present study, it was attempted to achieve the highest
decreasing ferrite grain size, both yield and tensile strengths impact properties ever reported via intercritical quenching
of dual-phase steels improved. They contended that it was and formation of dual-phase microstructure (Fig. 3).
due to the increase of ferrite grain boundaries, which led to
increased ferrite/martensite interfaces in addition to high
dislocation density in the grain and grain boundaries, and
improve the hardness of ferrite [36]. Also, Li et al. also
proved that the strength of HSLA dual-phase steels directly
depended on the hardness of martensite. They showed that
the strength of dual-phase steels did not rise linearly with
the increase of the martensitic volume fraction due to the
reduction of martensite carbon content and the hardness of
martensite after increasing the martensite volume fraction
[37]. Similarly, for IQ1&T due to the high carbon content
of martensite in IQ1, there was no significant change in
martensite morphology after tempering (Fig. 1e) and its is-
land-like morphology was kept almost intact. These islands
prevented the dislocation motion and increased the disloca-
tion density during loading. It was evident that martensite Fig. 3. Impact energy of the specimens with different heat treatments.
. The dual-phase microstructure of AISI 4340 steel, ob- increase the strength depending on the variation of mi-
tained by IQ treatment has the highest toughness, the crostructure and morphology.
highest elongation and the highest impact energy ever . Tempering leads to the emergence and severe growth of
reported. Analyzing the fracture surfaces confirmed the carbides. It can change the morphology of martensite in
ductile fracture mechanism, which is desirable. a dual-phase microstructure that does not provide desir-
. Tempering of ferritic–martensitic dual-phase micro- able properties. In general, it can be claimed that the fer-
structure reduces the hardness of the steel but does not ritic–martensitic dual-phase microstructure does not re-
have a significant effect on elongation, impact energy quire tempering treatment.
and strength ratio. On the other hand, it may reduce or
Fig. 5. SEM micrographs of fracture surface of tensile test samples: (a) Q&T, (b) normalized, (c) IQ1&T, (d) IQ1, (e) IQ2, and (f) IQ2&T.