International Journal of Minerals, Metallurgy and Materials

Volume 26, Number 2, February 2019, Page 202

https://doi.org/10.1007/s12613-019-1725-9

Mechanical and corrosion properties of low-carbon steel prepared by friction

stir processing

Li-ying Huang1,2), Kuai-she Wang1,2), Wen Wang1,2), Kai Zhao1,2), Jie Yuan1,2), Ke Qiao1,2),
Bing Zhang1,2), and Jun Cai1,2)
1) School of Metallurgical Engineering, Xi’an University of Architecture and Technology, Xi’an 710055, China
2) National and Local Joint Engineering Research Center for Functional Materials Processing, Xi’an University of Architecture and Technology, Xi’an 710055, China
(Received: 9 April 2018; revised: 6 June 2018; accepted: 11 June 2018)

Abstract: Low-carbon steel plates were successfully subjected to normal friction stir processing (NFSP) in air and submerged friction stir
processing (SFSP) under water, and the microstructure, mechanical properties, and corrosion behavior of the NFSP and SFSP samples were
investigated. Phase transformation and dynamic recrystallization resulted in fine-grained ferrite and martensite in the processed zone. The
SFSP samples had smaller ferrites (5.1 μm), finer martensite laths (557 nm), and more uniform distribution of martensite compared to the
NFSP samples. Compared to the base material (BM), the microhardness of the NFSP and SFSP samples increased by 19.8% and 27.1%, re-
spectively because of the combined strengthening effects of grain refinement, phase transformation, and dislocation. The ultimate tensile
strengths (UTSs) of the NFSP and SFSP samples increased by 27.1% and 38.7%, respectively. Grain refinement and martensite transforma-
tion also improved the electrochemical corrosion properties of the low-carbon steel. Overall, the SFSP samples had better mechanical proper-
ties and electrochemical corrosion resistance than the NFSP samples.

Keywords: low-carbon steel; friction stir processing; microstructure; mechanical properties; corrosion

1. Introduction dies have investigated FSP/FSW for various steels (e.g., in-
terstitial free steel [15], stainless steel [16], super-austenitic
Low-carbon steels are widely used in automobiles, con- steel [17], and structural steel [18]), there are only few stu-
structions, and other industrial fields [1] because of their dies on FSP of low-carbon steels. Sekban et al. [19] found
abundance, low cost, ease of smelting, and good formabil- that the ferrite grain size of a low-carbon steel decreased
ity [2−3]. However, their industrial application is limited by from 25 to 3 µm during FSP. The grain refinement increased
low hardness, strength, and corrosion resistance [4]. the strength, which was tested under uniaxial loading. In ad-
Friction stir processing (FSP) is a new severe plastic de- dition to the grain refinement, the phase transformation dur-
formation (SPD) technique [5] developed based on friction ing FSP also affects the mechanical properties of low-carbon
stir welding (FSW) [6−8], during which the material is broken steels. In another study, the same group of authors also
and mixed under the intense plastic deformation. At such con- demonstrated that the structures of the stir zone and
ditions the grains become refined because of dynamic recrys- heat-affected zone mainly comprised martensite, ferrite,
tallization [9]. Under forced cooling conditions, ultra-fine and Widmanstätten ferrite, and a mixture of ferrite and cementite,
even nano-sized grains can be obtained [10−12]. Additionally, while the structure of base material (BM) consisted only of
FSP is a simple and environment-friendly technology and can ferrite and pearlite; the microstructural changes improved
be used to prepare large-area ultrafine-grained plates [13]. the hardness and strength [20].
In the past, most of the FSP/FSW-related research fo- Grain refinement and phase transformation also affect
cused mainly on magnesium [14] and aluminum [8] alloys corrosion properties [21]. Zhang et al. [22], as well as few
as well as other low-melting metals. Although several stu- other researchers, have studied FSW effects on friction-stir
Corresponding authors: Kuai-she Wang E-mail: [email protected]; Wen Wang E-mail: [email protected]
© University of Science and Technology Beijing and Springer-Verlag GmbH Germany, part of Springer Nature 2019
L.Y. Huang et al., Mechanical and corrosion properties of low-carbon steel prepared by friction stir processing 203

welded joints of high nitrogen-content stainless steel, consi- processes had the same parameters: rotation rate of 950
dering microstructural evolution and pitting corrosion beha- r/min, travel speed of 60 mm/min, and 0.2 mm thickness
vior; they observed that FSW could reduce the coarse inclu- reduction. A WC cylindrical stir tool (without stir pin) with a
sions and refine the grains, thus improving the pitting resis- flat shoulder of 14 mm diameter was used.
tance of friction-stir welded joints. However, to the best of The microstructure of the processed zone (PZ) was ex-
our knowledge, there is no related research on the corrosion amined by scanning electron microscopy (SEM, JSM-6700F)
property of low-carbon steels prepared by FSP, which is and transmission electron microscopy (TEM, JEM-200CX).
mostly because of the difficulty of processing and complex The grain size of ferrite and width of the martensite laths were
phase transformation during FSP. measured by linear intercept method. Samples for SEM were
Considering the engineering applications of low-carbon cut perpendicularly to the processing direction and then
steels, their corrosion properties, in addition to the mechan- etched with a solution of 4vol% nitric acid + 96vol% alcohol.
ical properties, should be improved. Thus, the goal of our The samples for TEM were cut parallel to the processing
study is to investigate the influences of normal friction stir direction, and the thin foils for TEM observations were pre-
processing (NFSP) in air and submerged friction stir processing pared by double-jet electrolytic polishing in an electrolyte
(SFSP) under water on the microstructure, mechanical consisting of 100 mL perchloric acid and 900 mL alcohol.
properties, and corrosion properties of low-carbon steels. A 401 MVD sclerometer was used to measure the micro-
hardness of the samples along the middle of the cross sec-
2. Experimental tion under a load of 1.96 N for a dwell time of 10 s.

2.1. Material and processing 2.2. Room temperature tensile test

For the experiments, 3 mm plate of Q235 low-carbon The room temperature tensile tests were conducted on an
steel with a nominal chemical composition (wt%) of 0.18 C, Instron 8801 testing machine at an initial strain rate of 1 ×
0.45 Mn, 0.03 Si, 0.045 P, and 0.055 S (balance: Fe) was used. 10–3 s–1. The samples were cut along the transverse direction,
The low-carbon steel plates were subjected to NFSP and ensuring that the gauge section was located in the PZ (Fig.
SFSP along the rolling direction of the plates. Both 1). Each set of tensile tests was conducted three times.

Fig. 1. Schematic of the FSP and dimension of the tensile test sample (mm). AS and RS represent advancing and retreating sides,
respectively.

2.3. Electrochemical test frequency range of 100 kHz to 10 mHz. The electrochemi-
Potentiodynamic polarization curves and electrochemical cal corrosion morphology after cleaning (with a solution of
impedance spectroscopy (EIS) were performed in 3.5wt% HCl (50 mL) + distilled water (500 mL) + C6H12N4 (3.5 g))
NaCl solution at room temperature using a PARSTAT4000 was observed by SEM. Each set of electrochemical corro-
electrochemical analyzer. Samples with a dimension of 10 sion tests was conducted three times.
mm × 10 mm × 3 mm were cut from PZ. A three-electrode The corrosion rate of each sample was calculated as the
system, consisting of a platinum counter electrode, a satu- following [23]:
rated calomel electrode, and a working electrode, was used. Mi
v = 3.27 × 10−3 × corr (1)
Potentiodynamic polarization curve tests were performed in nρ
a scanning range of −0.5 to 1 V at a scanning rate of 1 where v is the corrosion rate, mm/a; icorr is the corrosion
mV·s–1. EIS tests were carried out at the open circuit poten- current density, μA/cm2; ρ is the density of the working
tial using a sinusoidal wave with an amplitude of 10 mV at electrode, g/cm3, M is the relative atomic mass, and n is the
204 Int. J. Miner. Metall. Mater., Vol. 26, No. 2, Feb. 2019

charge number of the working electrode. ples were 14 mm and were influenced by the shoulder. With
an increase of the depth along the normal direction, the in-
3. Results and discussion fluence of the shoulder on the width of the samples de-
creased gradually, as well as the PZ width.
3.1. Macrostructure
During FSP, plastic flow of the metal occurred under
compressive and shear stresses applied by the shoulder of
the stir tool. The plastic flow of the metal near the shoulder
was larger because of the larger stress and frictional heat. The
plastic flow became smaller farther away from the shoulder.
The cross sections of the NFSP and SFSP samples had a
basin-like shape (Fig. 2), and three obvious regions could be Fig. 2. Cross-sectional macrostructure of the NFSP (a) and
distinguished: PZ, thermo-mechanically affected zone, and SFSP (b) samples.
BM. Because of the cooling effect of water, frictional heat in
3.2. Microstructure
the PZ dissipated more easily; therefore, the PZ area of the
SFSP sample was smaller than that of the NFSP sample The microstructure of BM, NFSP, and SFSP samples (Fig.
(Figs. 2(a) and 2(b)). The PZ depths of the NFSP and SFSP 3) show that the BM sample mainly comprised ferrite and
samples were 1.9 and 1.3 mm, respectively. The widths of pearlite. The equiaxed ferrite grains were coarse and
the PZ on the top surface of both the NFSP and SFSP sam- non-uniformly distributed, and the average grain size of the

Fig. 3. SEM (a, c, e) and TEM (b, d, f) images of the samples: (a, b) BM; (c, d) NFSP; (e, f) SFSP.
L.Y. Huang et al., Mechanical and corrosion properties of low-carbon steel prepared by friction stir processing 205

ferrite was about 11.3 μm (Fig. 3(a)). Pearlites were mainly Fig. 5 shows stress–strain curves of the BM, NFSP, and
distributed along the ferrite grain boundaries (Fig. 3(b)). SFSP samples at room temperature, and the tensile strength
However, the microstructure of the NFSP sample changed test results are summarized in Table 1. The ultimate tensile
significantly compared to that of the BM sample, and a strengths (UTS) of the low-carbon steel increased signifi-
dual-phase microstructure comprising ferrite and martensite cantly after NFSP and SFSP, while the elongation to failure
was observed (Fig. 3(c)). The average width of the marten- (EL) decreased only slightly. The UTS and EL of the BM
site laths was 1.5 μm (Fig. 3(d)). The phase transformation sample was 470 MPa and 51.4%, respectively. Compared
during NFSP of the low-carbon steel indicates that the with BM, the UTS of the NFSP and SFSP samples increased
processing temperature is higher than Ac1 (The temperature by 27.0% and 38.7%, respectively. The ELs of the NFSP
at which the ferrite begins to transform into austenite during and SFSP sample were 47.1% and 45.6%, respectively,
heating) [24−25]. At this temperature range, some of the ini- which is slightly lower than that of the BM.
tial ferrite transformed into austenite and then into marten-
site during the subsequent cooling. Dynamic recrystalliza-
tion of ferrite occurred during NFSP, and its final average
grain size was 7.8 µm.
The microstructure of the SFSP sample is similar to that
of the NFSP sample: both had a dual-phase microstructure
consisting of ferrite and martensite (Fig. 3(e)). However,
because of the faster cooling rate, the ferrite grains of the
SFSP sample were finer with an average grain size of 5.1
μm. Additionally, the SFSP sample had more lath martensite
with uniform distribution, and its laths were finer with an
average width of 557 nm (Fig. 3(f)).
Fig. 5. Stress–strain curves of the BM, NFSP, and SFSP sam-
3.3. Microhardness and tensile properties ples.
Fig. 4 shows the microhardness of the cross sections of Table 1. Tensile strength test results for low-carbon steel at
the BM, SFSP, and NFSP samples. The average microhard- room temperature
ness values in the PZ of the NFSP and SFSP samples were
Sample UTS / MPa EL / %
HV 160.1 and HV 169.8, respectively, which are 19.8% and
27.1% higher than that of the BM sample, respectively. BM 470 ± 2 54.1 ± 0.2
These differences are attributed to the ferrite grain refine- NFSP 597 ± 4 47.1 ± 0.3
ment and martensite transformation. The SFSP sample had a SFSP 652 ± 2 45.6 ± 0.2
higher microhardness than the NFSP sample because of
further refinement of ferrite grains, increase of martensite The ferrite grains of both NFSP and SFSP samples
content, and finer martensite laths. seemed noticeably refined. At the same time, lath martensite
appeared in the samples. Martensite has a high hardness and
strength; therefore, the strengthening of grain refinement,
dislocation, and the presence of a secondary phase made the
UTSs of the two samples much higher than that of the BM
sample. The UTS of the SFSP sample is higher than that of
the NFSP sample because of the higher content of finer lath
martensite and its more uniform distribution. Moreover, the
fine grains can prevent crack propagation [26]; therefore, the
plasticity of the FSP-treated low-carbon steel is improved.
On the other hand, the lath martensite formed in low-carbon
steels has a low carbon content and uniform carbide distri-
bution, as well as an uneven dislocation distribution and a
Fig. 4. Distribution of microhardness in cross-section of the low-density dislocation zone, which provides space for dis-
BM, NFSP, and SFSP samples. location activity. The dislocation motion can alleviate the
206 Int. J. Miner. Metall. Mater., Vol. 26, No. 2, Feb. 2019

local stress concentration. Therefore, the strength of tion density. However, the fine-grained materials prepared
low-carbon steels increases after FSP, yet the plasticity does by FSP had a much lower ductility loss, which was mainly
not decrease noticeably [27]. because of a low dislocation as well as a high ratio of
Strength and elongation are important mechanical prop- high-angle grain boundaries.
erties of low-carbon steels, and they are often inversely
3.4. Electrochemical corrosion
proportional: the elongation decreases with an increase of
strength. In low-carbon steels prepared by other SPD tech- 3.4.1. Potentiodynamic polarization curve and EIS tests
niques, elongation also decreases significantly with an in- Fig. 6(a) shows potentiodynamic polarization curves of
crease in strength. Lee et al. [28] reported that the UTS of a the BM, NFSP, and SFSP samples. Corrosion potentials
low-carbon steel prepared by accumulative roll-bonding (Ecorr), corrosion current densities (icorr), and corrosion rates
technology was about three times higher than that of the BM, (v, calculated by Eq. (1)) are summarized in Table 2. Values
and the elongation dropped largely from 60% to <20%. of Ecorr, icorr, and v of the NFSP and SFSP samples are both
Singh et al. [29] prepared a high-strength ultrafine-grained lower than those of the BM sample, and values of Ecorr, icorr,
low-carbon steel by equal channel angular pressing and and v of the SFSP sample are lower than those of the NFSP
found that the UTS increased from 367 to 1009 MPa, while sample. The decrease of corrosion potential indicates that
the elongation decreased from 41% to 1%. They demon- FSP-prepared low-carbon steel is more susceptible to corro-
strated that the main reason for the low ductility of the sion and can more easily form a passive film. The density of
SPD-fabricated fine-grained materials was the high disloca- the passive film directly affects the corrosion rate.

Fig. 6. Potentiodynamic polarization curves (a) and Nyquist plots (b) of the BM, NFSP, and SFSP samples in 3.5wt% NaCl solu-
tion.

Table 2. Electrochemical parameters for the BM, NFSP, and sistance.

SFSP samples Nyquist plots of the NFSP and SFSP samples were fitted
Sample Ecorr / mV icorr / (μA·cm–2) v / (mm·a–1) by Zsimpwin software to obtain an equivalent electrical cir-
BM −632.6 31.5 0.367 cuit (EEC), which is shown in Fig. 7. Both samples have the
NFSP −644.3 16.2 0.189 same EEC, indicating the same corrosion mechanism. In the
SFSP −656.9 14.3 0.167 EEC diagram, Rs is the solution resistance, Rt is the charge
transfer resistance, Q is the constant phase angle element,
Meanwhile, the Nyquist plots (Fig. 6(b)) of the NFSP, and n is the dispersion coefficient. Rt is an important index
SFSP, and BM samples only show capacitive loops, where- for corrosion resistance evaluation. The higher the Rt value,
by the same electrochemical corrosion behavior is demon- the denser the passive film and the stronger the resistance to
strated for all three samples. Generally, the larger the di- ion and charge conduction. Rt has an inverse relationship
ameter of a capacitive loop, the higher the corrosion resis- with the corrosion rate.
tance. Based on the experimental results of polarization and Table 3 summarizes the fitting values of the EEC com-
EIS tests, it can be concluded that the corrosion resistances ponents. The Rt values decrease in the following order:
of the NFSP and SFSP samples are both higher than that of SFSP > NFSP > BM. Thus, the SFSP sample is more resis-
the BM sample. The SFSP sample has the best corrosion re- tant to corrosion, followed by the NFSP and then BM sam-
L.Y. Huang et al., Mechanical and corrosion properties of low-carbon steel prepared by friction stir processing 207

ples. These results agree with the potentiodynamic polariza- most severe corrosion was in the BM sample, as its corrosion
tion curve and EIS results. pits were more abundant, bigger, and deeper (Fig. 8(a)).
This severe pitting corrosion was very uniform (Fig. 8(b)).
Corrosion morphology changed noticeably after FSP.
Less corrosion pits were observed in the NFSP sample,
which were smaller and much shallower (Fig. 8(c)). The
corrosion degree and surface roughness of the whole sample
Fig. 7. Equivalent electrical circuit of the EIS.
was not as severe as that of the BM sample (Fig. 8(d)); thus,
Table 3. Fitting values of the equivalent electrical circuit the electrochemical corrosion resistance of the NFSP sample
components was improved.
Samples Rs / (Ω·cm2) Q / (10–4 F·cm–2) n Rt / (Ω·cm2) The change of the electrochemical corrosion morphology
BM 3.417 4.726 0.8475 581.7 of the SFSP sample was especially noticeable (Figs. 8(e)
NFSP 6.487 3.712 0.8534 685.9 and 8(f)). The number of pits on the surface of SFSP sample
SFSP 0.625 7.164 0.8482 711.7 was further reduced, and the pits were the smallest and
shallowest. These characteristics are consistent with the re-
3.4.2. Electrochemical corrosion morphology sults of potentiodynamic polarization curve and EIS tests,
Fig. 8 shows SEM images of the electrochemical corro- which indicate that FSP can improve electrochemical corro-
sion morphologies of the BM, NFSP, and SFSP samples. The sion resistance of low-carbon steels, especially SFSP.

Fig. 8. Electrochemical corrosion morphologies of the samples: (a, b) BM; (c, d) NFSP; (e, f) SFSP.
208 Int. J. Miner. Metall. Mater., Vol. 26, No. 2, Feb. 2019

Grain refinement and martensite formation after FSP are Influence of high deformation on the microstructure of
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