Accepted Manuscript

Improved mechanical properties of mild steel via combination of deformation,

intercritical annealing, and quench aging

Sheida Nikkhah, Hamed Mirzadeh, Mehran Zamani

PII: S0921-5093(19)30535-0
DOI: https://doi.org/10.1016/j.msea.2019.04.071
Reference: MSA 37821

To appear in: Materials Science & Engineering A

Received Date: 6 March 2019

Revised Date: 16 April 2019
Accepted Date: 17 April 2019

Please cite this article as: S. Nikkhah, H. Mirzadeh, M. Zamani, Improved mechanical properties of mild
steel via combination of deformation, intercritical annealing, and quench aging, Materials Science &
Engineering A (2019), doi: https://doi.org/10.1016/j.msea.2019.04.071.

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 ACCEPTED MANUSCRIPT

Improved mechanical properties of mild steel via combination of

deformation, intercritical annealing, and quench aging

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Sheida Nikkhah, Hamed Mirzadeh1, Mehran Zamani

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Abstract

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Processing of dual phase steel with fine ferrite grains containing nanometric carbides and chain-

like morphology of martensite from a 0.035C-0.005N-0.035Si-0.268Mn mild steel was realized

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via application of high cold rolling reductions, intercritical heat treatment, and room-temperature
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aging, which showed a yield stress (YS) of 450 MPa and ultimate tensile strength (UTS) of 700

MPa. It was revealed that significant enhancements in tensile properties can be achieved
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compared to the separate effects of intercritical annealing (YS of 130 MPa and UTS of 385

MPa), cold rolling and intercritical annealing (YS of 300 MPa and UTS of 600 MPa), and
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quench aging (YS of 275 MPa and UTS of 520 MPa). The results were rationalized based on the
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grain size strengthening, aging effect, and work-hardening behavior.

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Keywords: DP steels; Mechanical properties; Quench aging; Intercritical annealing.

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Corresponding author. Tel.: +982182084080; Fax: +982188006076. E-mail address: hmirzadeh@ut.ac.ir (H. Mirzadeh).

Affiliation of all authors: School of Metallurgy and Materials Engineering, College of Engineering, University of Tehran, P.O.
Box 11155-4563, Tehran, Iran

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1. Introduction

The microstructure of low-carbon dual-phase (DP) steels is normally composed of ferrite and

martensite, which results in favorable strength-ductility balance required for automotive and other

industrial applications [1-5]. As a result, research works on the optimization of mechanical properties

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of DP steels are currently underway. In this respect, the main focus has been on the microstructural

refinement [6-10]. Among the various grain refining routes, the intercritical annealing of cold

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deformed martensitic microstructures has been found to be advantageous, where the formation of

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recrystallized ferrite during heating to the intercritical annealing temperature is responsible for the

ferrite grain refinement and formation of grain-boundary martensite with the chain-like morphology

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[11-14]. This kind of microstructure provides improved work-hardening behavior. Besides grain
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refinement, the bake hardening effect is also known as one of the most effective post intercritical

annealing phenomena for improving the mechanical properties of DP steels [15-19]. Interestingly,
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room-temperature aging (quench aging) via formation of fine carbide precipitates in ferrite has been

shown recently as a viable method for enhancing the properties of low-silicon DP steels [20].
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Flat-rolled mild steels with <0.10 wt.% C and <0.4 wt.% Mn have been recently used to process
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high-formability DP steels with low strengths [20-23]. In this regard, a DP steel with yield stress

(YS) of 130 MPa and ultimate tensile strength (UTS) of 385 MPa has been processed based on the
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chemical composition (wt%) of 0.035C-0.005N-0.035Si-0.268Mn [21]. However, the low strength

negates the usefulness of good formability properties. In this respect, Nouroozi et al. [22] showed
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that by cold rolling and intercritical annealing, it is possible to process a DP steel with YS of 300
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MPa and UTS of 600 MPa via microstructural refinement. In another front, Zamani et al. [20]

unveiled the remarkable quench aging potential of this low-silicon steel with the ability to enhance

the yield stress up to 150 MPa, where DP steel with YS of 275 MPa and UTS of 520 MPa was

obtained. These works imply that cold working prior to intercritical annealing and the subsequent

quench aging can be simultaneously used to optimize the properties of this steel. As a result, this

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paper is dedicated to evaluate the synergy of these parameters for the first time to improve the

properties of 0.035C-0.27Mn-0.03Si steel.

2. Experimental details

The as-received sheet was a St12 mild steel (thickness of 1.6 mm and chemical composition of

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0.035C-0.005N-0.035Si-0.268Mn, wt%) with ferritic-pearlitic microstructure. Austenitization (1050

°C for 15 min), water quenching, cold rolling reductions of 40% (thickness of 0.95 mm) and 80%

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(thickness of 0.32 mm), intercritical annealing (at 800 °C and 850 °C for 1 min), water quenching,

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and room-temperature aging (for ~ 216 h) were applied. In this regard:

(I) Based on the systematic study of Najafkhani et al. [23] on the grain growth behavior during

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intercritical annealing of cold rolled martensite, intercritical annealing time of 1 min was considered
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as the optimum holding time to obtain DP microstructures with the finest grain size.

(II) According to the results of Nouroozi et al. [22] on the intercritical annealing of cold rolled
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martensite, better work-hardening behavior can be obtained after intercritical annealing temperature

at 850 °C compared to 800 °C.

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(III) Based on the study of Zamani et al. [20] on the quench aging behavior, lower intercritical
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annealing temperatures result in higher concentrations of carbon in ferrite in the intercritical

annealing region with the consequent greater quench aging effect. For instance, at the intercritical
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annealing temperatures of 750, 800, and 850 °C, the concentration of carbon in ferrite (and the
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change in the yield stress before and after aging) was found to be 0.019 wt% (169 MPa), 0.011 wt%
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(158 MPa), and 0.003 wt% (40 MPa), respectively [20].

(IV) The choice of aging time was based on the study of Zamani et al. [20], which showed that the

DP samples can be fully aged at room temperature for ~ 216 h.

Based on (II) and (III), the intercritical annealing temperature of 800 °C was considered as the base

condition and the temperature of 850 °C was applied for comparison. The applied processing routes

are summarized in Table 1, where a name has been assigned to each sample.

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Table 1: Processing details of the DP samples.

Sample Primary processing Intercritical annealing Temperature Aging

DP0N800 As-received [20] 800 °C No
DP0Y800 As-received [20] 800 °C Yes
DP40N800 40% rolled 800 °C No

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DP40Y800 40% rolled 800 °C Yes
DP80N800 80% rolled 800 °C No
DP80Y800 80% rolled 800 °C Yes

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DP80Y850 80% rolled 850 °C Yes
DPNouroozi 50% rolled [22] 850 °C No

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After etching by the LePera and Nital solutions, the field-emission scanning electron microscopy (FEI

Nova 450) was used for revealing the microstructures. Tensile samples with gauge length of 25 mm

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(ASTM E8 standard) were used and tensile testing at room temperature with the constant cross-head
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speed of 1 mm/min using a SANTAM STM-20 universal testing machine was carried out. The tests were

repeated once to insure the reproducibility of results. Microhardness measurements were based on the
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Vickers hardness test under a load of 10 g.

3. Results and discussion

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Table 2 summarizes the resultant tensile properties and average grain size of the DP samples, where it
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can be seen that by (I) increasing the rolling reduction, (II) subjecting to the aging treatment, and (III)

increasing the intercritical annealing temperature, the yield stress and tensile strength increase. These
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results will be discussed in the following sections.

Table 2: Tensile properties and average grain size of the DP samples.

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Sample YS (MPa) UTS (MPa) Total Elongation (%) Average ferrite grain size (µm)
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DP0N800 130 385 42

17.1 ± 1.4
DP0Y800 275 520 28
DP40N800 215 490 31
11.9 ± 1
DP40Y800 340 580 21
DP80N800 310 590 31
8.5 ± 0.7
DP80Y800 435 675 19
DP80Y850 450 700 18 9.4 ± 0.8
DPNouroozi 300 600 35 11.5 ± 1

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Figure 1a shows the effects of aging (compare DP0Y800 [20] with DP0N800 sample), cold

rolling (compare DP40N800 with DP0N800 sample), and combined effect of cold rolling and

intercritical annealing at a higher temperature (compare DPNouroozi [22] with DP0N800 sample).

It can be seen that aging (DP0Y800 sample) can significantly enhance the yield stress and tensile

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strength, which has been related to the precipitation of carbides in ferrite during room-

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temperature aging as shown by Zamani et al. [20].

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Figure 1: (a) Tensile stress-strain curves of DP0N800, DP40N800, DP0Y800, and DPNouroozi samples
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and (b) Work-hardening plots of DP0N800 and DP40N800 samples.

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Cold rolling before intercritical annealing (DP40N800 sample) also exhibits a similar enhancement

effect, which is partly related to the microstructural refinement induced by this process. In fact, grain

refinement was achieved via formation of equiaxed and recrystallized ferrite during heating to the

intercritical annealing temperature [11] as summarized in Table 2 and is shown in Figures 2a, 2b,

and 2c. Since the DP40N800 and DP80N800 steels have been intercritically annealed from the cold

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rolled state, the dislocation strengthening of cold rolling should be studied. Therefore, the

microhardness of the ferrite phase in these samples was measured, which resulted in the values of

137 ± 3, 182 ± 4, and 189 ± 5 for DP0N800, DP40N800, and DP80N800 samples, respectively. This

reveals that this factor also takes part in the strengthening of these steels regardless of the grain

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refinement effect.

As can be seen in Figure 2a, the microstructure of DP0N800 steel is composed of coarse-grained

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ferrite (average grain size of 17.1 µm) with large martensite islands. However, a finer ferrite grain

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size of 11.9 µm and chain-like morphology of martensite can be seen for the DP40N800 sample in

Figure 2d and Figure 2e. It can be seen in Figure 2e that ferrite grains are surrounded by the chain-

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like martensite islands. This can enhance the work-hardening behavior as shown in Figure 1b, where
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at each strain, it can be seen that the work-hardening rate ( θ = dσ / dε ) of DP40N800 is higher than

that of DP0N800 sample.

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Figure 2: SEM images, where F, M, and C denote ferrite, martensite, and carbide, respectively.

As can be seen in Figure 1a, the combined effect of cold rolling and intercritical annealing at higher

temperature of 850 °C (DPNouroozi) is quite effective in enhancement of tensile properties (YS of 300

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MPa and UTS of 600 MPa). In this case, fine grain size and chain-like morphology of martensite

were characterized as the main factors for the enhanced tensile properties [22].

These results reveal the possibility of enhancement of mechanical properties by simultaneous

application of cold working, intercritical annealing, and quench aging. Therefore, for the

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enhancement of mechanical properties, the cold rolling reductions of 40% and 80%, the intercritical

annealing temperatures of 800 °C and 850 °C, and room-temperature aging were considered as

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shown in Table 1. The tensile stress-strain curves are shown in Figure 3a.

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Figure 3: Summary of tensile test results: (a) Stress-strain curves of DP0N800, DP40Y800, DP80Y800,

and DP80Y850 samples and (b) Hall-Petch plots for unaged and aged samples at rolling reductions of 0,

40, and 80%, (c) Tensile strength versus rolling reduction for unaged and aged samples, and (d) Yield

ratio versus rolling reduction for unaged and aged samples. Due to the difference in the applied

intercritical annealing temperature, the DP80Y850 sample has not been included in (b), (c), and (d).

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It can be seen in Figure 3a that via 40% rolling, intercritical annealing, and aging (DP40Y800

sample), tensile properties enhance significantly, where DP steel with YS of 340 MPa and UTS

of 580 MPa can be obtained. Compared to the DP0N800 sample (DP steel with YS of 130 MPa

and UTS of 380 MPa), this is a remarkable enhancement. Comparison with the corresponding

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unaged sample in Figure 1a (with YS of 215 MPa and UTS of 490 MPa) reveals that aging is

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very effective in this regard (~ 100 MPa increase in both yield and tensile strengths). Figure 3a

also reveals that a higher cold reduction of 80% (DP80Y800 sample) has positive effect of the

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enhancement of tensile properties (with YS of 435 MPa and UTS of 675 MPa).

Figure 3b reveals that the yield stress enhances by increasing the cold rolling reduction, which

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can be related to the grain refinement effect (Table 1). Moreover, after aging, the level of yield
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stress increases significantly. It can be also seen that the Hall-Petch slope for the unaged and

aged samples are nearly the same but the friction stress (the overall resistance of the crystal
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lattice to dislocation movement [24]) for the aged samples is ~ 140 MPa higher. The latter is
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related to the extra strengthening mechanism of precipitation hardening.

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Figure 3c shows that the tensile strength also enhances by increasing the cold rolling reduction

before and after aging. However, the difference between tensile strengths of unaged and aged
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samples decreases by increasing the cold rolling reduction. This implies a decrease in the effect

of aging on the enhancement of tensile strength. Figure 3d summarizes the obtained values of
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yield ratio (YS/UTS [25]). It can be seen that by increasing the cold rolling reduction, the yield
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ratio increases. Moreover, after aging, the values of yield ratio are higher than 0.5. The latter

indicates that the enhancement of mechanical properties by aging has been achieved mainly by

increasing the yield stress. However, the work-hardening behaviors should be considered to

rationalize the observed trend of the tensile strength in Figure 3c, where the required plots are

shown in Figure 4.

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Figure 4: Work-hardening rate plots for the unaged and aged samples.

It can be seen that the work-hardening exponent (n-value) at the coincidence point of the work-
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hardening rate (θ) and flow stress (σ) curves decreases considerably via aging treatment. In fact,
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based on the Considére criterion, plastic instability of strain-rate-insensitive materials occurs

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when the strain-hardening rate (θ) coincides with the flow stress (σ), i.e. σ ≥ dσ / dε [24].

Therefore, the lower work-hardening capacity of the aged samples results in the rapid fall of θ,
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and hence, the θ curve meets the σ curve quickly. For the 80% rolled sample, the rapid fall of θ

is more pronounced when compared with the 0% rolled sample (Figure 4). This is responsible
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for the decreased ∆UTS of aged and unaged conditions when comparing the 80% and 0% rolled
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samples.

For the DP80Y850 sample, based on the reduction of 80%, intercritical annealing at 850 °C, and

aging, a DP steel with YS of 450 MPa and UTS of 700 MPa was obtained (Figure 3a). The

microstructure of this sample has been shown in Figure 2f, and Figure 2g, where it can be seen

that its ferrite grain size is ~ 9.4 µm on average. Moreover, the higher magnification image

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(Figure 2h) reveals the precipitated nanometric carbides with average particle size of 40 nm

inside ferrite grains. The precipitation of carbides during quench aging of low-silicon steels has

been also reported by Zamani et al. [20] and Chang [26]. This is the best tensile properties

obtained for this steel so far and might be advantageous for application of these sheets in the

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industry.

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4. Summary

The possibility of enhancement of mechanical properties of 0.035C-0.005N-0.035Si-0.268Mn

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mild steel by simultaneous application of cold working, intercritical annealing, and quench aging

was studied. It was revealed that by increasing the rolling reduction in thickness, intercritical

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annealing, and subsequent room-temperature aging, it is possible to process a DP steel with YS
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of 450 MPa and UTS of 700 MPa with a microstructure comprising of fine ferrite grains
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containing nanometric carbide precipitates of ~ 40 nm and chain-like morphology of martensite

on the grain boundaries. This steel shows significant enhancement when compared to the
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separate effects of intercritical annealing (DP steel with YS of 130 MPa and UTS of 385 MPa),
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cold rolling and intercritical annealing (DP steel with YS of 300 MPa and UTS of 600 MPa), and

quench aging (DP steel with YS of 275 MPa and UTS of 520 MPa).
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Acknowledgment
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The authors would like to greatly thank the members of the Advanced Steels and
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Thermomechanically Processed Engineering Materials Laboratory for their help and support.

Financial support by the University of Tehran is also gratefully acknowledged.

Data availability

The authors stated that the processed data required to reproduce these findings were available in

this manuscript.

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