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Elucidation of void defects by soft reduction in medium carbon steel via EBSD
and X-ray computed tomography

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DOI: 10.1016/j.matdes.2021.109978

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 Materials & Design 209 (2021) 109978

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Materials & Design

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

Elucidation of void defects by soft reduction in medium carbon steel via

EBSD and X-ray computed tomography
Naqash Ali a, Liqiang Zhang a,⇑, Hongwei Zhou b,⇑, Aonan Zhao a, Chaojie Zhang a, Yuan Gao c
a
School of Metallurgical Engineering, Anhui University of Technology, Maanshan 243002, China
b
School of Materials Science and Engineering, Anhui University of Technology, Maanshan 243002, China
c
School of Metallurgical and Ecological Engineering, University of Science and Technology Beijing (USTB), Beijing 100083, China

h i g h l i g h t s g r a p h i c a l a b s t r a c t

 Qualitative and quantitative analysis

of void defects by EBSD and X-ray
computed.
 Soft reduction technology can
effectively control the formation of
voids in medium carbon steel.
 Minimum reduction amounts can
compensate the solidification
shrinkage voids than the large and
without SR.
 Micro voids are coalesced to act as
crack propagation.

a r t i c l e i n f o a b s t r a c t

Article history: In this work, void formation in medium carbon ferrite-pearlite steel is investigated with soft reduction
Received 8 June 2021 (SR) technology as regards its initiation sites and governing factors: prior austenite grain size, grain
Revised 3 July 2021 boundary ferrite (GB-a) precipitation, pearlite block size and sub-grain boundaries misorientation. The
Accepted 7 July 2021
small and tightly packed pearlite colonies attached with GB-a and irregular broken cementite lamellae
Available online 10 July 2021
provide an easier path for void initiation at prior austenite grain boundary (PAGB) and pearlite colony
boundary respectively. 3-dimensional void morphology and void size including porosities with different
Keywords:
SR parameters were characterized via X-ray computed tomography (XCT). The total number of voids,
Microstructure
Void initiation
their sizes, and shape complexity are increased by increasing reduction amount, and serious void defects
Grain size are evident without the implementation of SR technology. The size of shrinkage void increases with
Soft reduction increasing reduction amount, which is twice without implementation of SR technology as compared with
X-ray computed tomography the high reduction amount of 6 mm. The total number of voids and their sizes was less along with porosi-
ties at minimum reduction amounts of 2 mm and 4 mm, which are small enough to compensate the
solidification shrinkage voids.
Ó 2021 The Author(s). Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND
license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

1. Introduction
⇑ Corresponding authors.
E-mail addresses: zhangsir508@163.com (L. Zhang), zzzhw.1@gmail.com Medium carbon steel with pearlitic microstructure is widely
(H. Zhou). used in modern society and has an attractive application in the

https://doi.org/10.1016/j.matdes.2021.109978
0264-1275/Ó 2021 The Author(s). Published by Elsevier Ltd.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
N. Ali, L. Zhang, H. Zhou et al. Materials & Design 209 (2021) 109978

railway industry due to remarkable wear resistance combined with 2. Experimental

high strength and ductility [1,2]. The excellent and comprehensive
performance of medium carbon pearlitic steel is closely related to 2.1. Material
the microstructure, as ferrite-pearlite microstructure has low
toughness, which limited it in lightweight potential [3]. The Soft reduction experiments were conducted with medium car-
microstructure of micro-alloyed steel could be easily refined with bon steel and its average chemical composition is presented in
the refinement of prior austenite grain to improve the impact Table 1.
toughness [4]. Therefore, the microstructural features namely prior
austenite grain size [5], ferrite precipitation along the austenite
2.2. Soft reduction experiments and microstructure characterization
grain boundary [6], and coarsening of pearlite colonies [7] have a
decisive role in the formation of internal voids and cracks. The
The weighted amount of steel scrap (650 g) was placed into the
voids formation during the casting process significantly reduces
graphite crucible with a diameter of 41 mm, and then it was put
mechanical properties of different steel grades due to degradation
into the vacuum furnace. The furnace temperature was raised to
of yield strength and fatigue resistance [8,9]. The irregular voids
1600 °C, and the fully molten metal was homogenized for 90 s to
appear on the surface of cast products and coalesced to form the
prevent the dispersion of gas bubbles while applying reduction
forging cracks, which harm the post-rolling products.
amount. The experimental schematic diagram is shown in Fig. 1.
Extensive numerical and experimental studies have been
The reduction amounts of 2 mm, 4 mm, and 6 mm with flat roller
proved that soft reduction (SR) technology could effectively reduce
were applied separately to each ingot and then air-cooled to obtain
the internal voids and cracks defects during the continuous casting
ferrite-pearlite microstructure. The blank ingot was air-cooled
process [10–13]. The compensation of solidification shrinkage by
without applying reduction amount to compare it with other sam-
the homogeneous flow of molten metal from surface towards the
ples. The ingots have approximately 40  60  40 mm3 specifica-
core of cast product is the basic principle of SR technology. There-
tions according to the different reduction amounts. Each ingot was
fore, the segregation of alloying elements becomes homogeneous
machined into two pieces along the longitudinal direction and one
across the entire area, which reduces the internal defects [14].
half was used for the further processing.
The temperature gradient from surface towards the center of cast
The small specimens of 10  10  2 mm3 were prepared from
product has an essential role in the void formation and the thresh-
the center region. The sandpapers of different grades and diamond
old of temperature gradient should be recognized to avoid the
paste were used for grinding and polishing purposes and then fol-
shrinkage voids [15]. The voids could not eliminate with a conse-
lowed by 3 vol% nital etching for microstructural analysis. The
quent heat treatment process and the best approach for the void
ferrite-pearlite microstructure and void defects were characterized
elimination is to identify its formation mechanism and governing
by optical (OM) and scanning electron microscope (SEM). Electron
factors to refine the microstructure. In contrast, the correlation
backscatter diffraction (EBSD) was used to elaborate the voids
between the austenite grain size and refinement of pearlite colo-
characteristics and microstructural features to calculate the grain
nies with void formation is rarely been addressed in the literature.
boundary misorientation. EBSD was equipped with HKL channel
Azghandi et al. found that the large voids with low sphericity were
5 at an acceleration voltage and step size of 20 kV and 0.2 lm
predominantly formed in materials with coarse grains, and pro-
respectively.
posed that twin or grain boundaries and second-phase particles
were preferential sites for void nucleation, depending on the
austenite grain size [16]. The void nucleation was delayed with 2.3. 3-dimensional analysis of void defect
the formation of small voids by reducing the grain size in austenitic
stainless [17], and also the void area fraction revealed a direct rela- 3-dimensional images of void defects in each sample were mea-
tionship with the grain size during the spall response of copper sured with X-ray computed tomography (XRT), using YXLON
[18]. Besides the austenite grain size, refinement of pearlite colo- micro-focus FF35 system at an acceleration voltage of 170 kV
nies is also beneficial for the control of void formation. The bound- and beam current of 135 mA. The flat panel detector possessed
aries of coarse pearlite colonies acted as the void nucleation site 249 mm  302 mm dimension, the pitch of 0.139 mm  0.139 m
due to the presence of broken cementite lamellae with high stress m and1  1 binning was applied during 3D tomograms acquisition.
concentration as compared to the fine pearlite colonies [19]. Simi- The geometrical magnification of the system was allowed for
larly, in the medium carbon steel, pits were also nucleated at the 1792  2176 pixels with exposure time of 333.3 ms. The position
boundaries of coarse pearlite colonies as studied by Kadowaki between detector and X-ray source remained fixed and region of
et al [20]. Therefore, the governing factors of voids formation interest (ROI) was selected by placing the sample closer to the
should be studied carefully to investigate the optimized SR detector during scanning. 3D tomograms were reconstructed from
parameters. 1800 projections and then it was processed for voids observation
The objective of our work is to investigate the void’s nucleation using VG Studio MAX 3.2 software (VGEasyPore) by various algo-
sites and governing factors that cause their nucleation in typical rithms to inspect the morphology and size of each void.
ferrite-pearlite steel microstructures. For the above purposes, scan-
ning electron microscopy (SEM) is used for the microstructure 3. Results and discussion
analysis, while the electron backscatter diffraction (EBSD) analysis
is used to identify the voids distribution (intergranular and intra- 3.1. Microstructural analysis
granular) and grain boundary misorientation. In addition, 3D voids
characteristics, e.g., porosity, voids morphology, and size as a func- Figs. 2 and 3 show OM and SEM micrographs of medium carbon
tion of SR amounts have been evaluated quantitatively via X-ray steel, which reveal the pearlitic microstructure with dominant
micro computed tomography. grain boundary ferrite (GB-a) after etching with 3 vol% nital solu-

2
N. Ali, L. Zhang, H. Zhou et al. Materials & Design 209 (2021) 109978

Table 1
Avg. chemical composition of investigated steel (wt.%).

C Mn Si P S Ni Cr
0.60 0.65 0.27 0.035 0.035 0.30 0.25

Fig. 1. Schematic diagram of experimental setup.

Fig. 2. Optical micrographs at different reduction amounts: (a) 2 mm, (b) 4 mm, (c) 6 mm, and (d) without SR.

Fig. 3. SEM microstructure along PAGB: (a) 2 mm, (b) 4 mm, (c) 6 mm, and (d) without SR.

tion. The dark and bright regions are pearlite (P) and GB-a respec-
tively, which form with and without SR technology due to air cool-
ing conditions. GB-a forms at 973 K, while pearlite nucleates from
the austenite grain boundary (PAGB) and grows into adjacent grain
at 873 K [21]. Pearlite formation along the PAGB is due to the K-S
orientation relationship of pearlite with the austenite grain into
which it grows [6]. The average prior austenite grain size is esti-
mated from GB-a with linear intercept method for reduction
amounts of 2 mm, 4 mm, 6 mm and without SR, which are
608 lm, 682 lm, 796 lm, and 903 lm respectively.
EBSD analysis was performed to examine the pearlite block
sizes and voids initiation mechanism under different SR parame-
ters. Fig. 4a, c, and g show the inverse pole map (IPF), which reveals
the randomly oriented pearlite blocks. Fig. 4b, d, f, and h show the
grain boundary maps, in which black lines indicate the high angle
grain boundaries (HAGBs) with misorientation > 15°, while the red
lines stand for the low angle grain boundaries (LAGBs) with misori-
entation 2–15°. All samples contain a large fraction of LAGBs,
which proves the presence of small pearlite colonies. The average
size of pearlite blocks is estimated from HAGBs with a linear inter-

3
N. Ali, L. Zhang, H. Zhou et al.
Fig. 4. EBSD (IPF) maps and the corresponding grain boundary maps with different
reduction amounts: (a, c, e, and g) IPF maps and (b, d, f, and h) grain boundary maps.
(a, b) 2 mm; (c, d) 4 mm; (e, f) 6 mm and (g, h) without SR.
cept method at reduction amounts of 2 mm, 4 mm, 6 mm and
without SR, which are 114 lm, 117 lm, 96 lm, and 147 lm
respectively.
3.2. Voids initiation sites and governing factors
Fig. 5 shows SEM images of void regions under different SR
parameters. Fig. 5c and d represent micro crack and large shrink-
age at high reduction amount of 6 mm and without SR technology
respectively. The shrinkage area contains large number of voids,
which are coalesced to form the cracks. Furthermore, the speci-
mens undergoing reduction amounts of 2 mm and 4 mm also have
small ellipsoidal voids, which might be resulted from micro voids
coalescence and will be proved by XCT in the following section.
These ellipsoidal voids coalesced to form the micro-cracks. The
EDS line spectrum reveals the absence of non-metallic inclusions
4
Materials & Design 209 (2021) 109978
at the center of voids from which the void can initiate, except silica
inclusion at the center of cracks which might be resulted from the
grinding and polishing of sample as shown in Fig. 5. Therefore, this
work investigated the preferable void initiation sites in the absence
of non-metallic inclusions. The voids and cracks are mainly located
inside of the austenite grain as revealed in Fig. 5b, c, and e. The
pearlite microstructure around the void is evident and the red
arrows indicated the lamellar directions of different pearlite colo-
nies. The different directions of lamellae at the upper and lower
sides of voids indicate that the void is initiated at the boundaries
of different pearlite colonies without the presence of inclusion
and is consistent with the study of Kadowaki et al. [20].
Fig. 6 shows the difference in the lamellar directions as indica-
tive of different pearlite colonies in which the bright areas are
cementite lamellae and dark areas are ferrite. The interlamellar
spacing was estimated to be 0.22 lm, 0.32 lm, 0.47 lm, and
0.44 lm at reduction amount of 2 mm, 4 mm, 6 mm, and without
SR respectively. Fig. 6a and b represent the fine pearlite colonies
with relatively identical direction of cementite lamellae. As shown
in Fig. 6c and d, the cementite lamellae have irregular morphology
especially in Fig. 6d, which reveals the degenerated pearlite (DP)
microstructure. Furthermore, in both cases the intersecting lamel-
lae indicated by the red dashed area in Fig. 6c and degenerated
pearlite (DP) are responsible for the coarse pearlite colonies. Dur-
ing soft reduction experiment, stress increases with increasing
the reduction amount accompanied by dislocation density, which
increases at the ferrite/cementite interface and cementite lamellae
break. The broken lamellae connect to form the micro cracks while
the fine pearlite colonies have a small stress concentration [19].
Fig. 7 shows the microstructural quantification at different SR
parameters and an increasing trend of porosity is evident with
increasing reduction amounts to 6 mm. The decrease in porosity
is related with the refinement of pearlite colonies, which in turn
depends on the identically oriented cementite lamellae. Further-
more, SR have little influence on pearlite block size. At reduction
amount of 2 mm and 4 mm, small coarse grains than other cases
significantly decreases the porosity fraction due to the fine pearlite
colonies. At reduction amount of 6 mm, the small pearlite block
size with maximum porosity is evident, which confirms the pres-
ence of small tightly packed pearlite colonies and has a significant
intersection of cementite lamellae. Infact, each prior austenite
grain in pearlitic steel contains a large number of tightly packed
pearlite colonies and these colonies have irregular and broken
lamellae. These broken lamellae have higher dislocation density
due to the stress concentration, which is proved in the following
section. Therefore, voids can be easily initiated at the boundaries
of different pearlite colonies and coalesced to form large ellipsoidal
voids. Furthermore, the void initiation mechanism along the PAGB
and different pearlite colony boundaries is elaborated with EBSD
analysis.
3.2.1. Void initiation at GB-a and pearlite colony boundaries
Fig. 8a shows the band contrast image which reveals the GB-a
with triangular morphology attached by a small and tightly packed
pearlite colony at reduction amount of 2 mm. The grain boundary
map (Fig. 8c and f) shows a high fraction of LAGBs along the PAGB,
which are associated with different orientations of pearlite colo-
nies inside the block [22]. Pearlite colonies have intersecting
cementite lamellae attached with GB-a, which increases the dislo-
cation density and voids start to initiate at the colony boundary.
Fig. 8c shows the high fraction of LAGBs at the periphery of void
regions, which exhibits the strain concentration caused by the
higher deviation of atoms from equilibrium position. Fig. 8d and
f show the intergranular void growth along GB-a without SR tech-
nology, which are coalesced to form a large ellipsoidal void. The
small areas of different colors attached with GB-a in the IPF map
N. Ali, L. Zhang, H. Zhou et al.
Fig. 5. SEM images of defected areas: (a,b) micro voids at 2 mm and 4 mm respectively, (c) micro crack at 6 mm, and (d,e) shrinkage voids and crack without SR.
Fig. 6. SEM images of pearlite colonies: (a) 2 mm, (b) 4 mm, (c) 6 mm, and (d) without SR.
Fig. 7. The quantification of porosity (%), average prior autenite grain size and
pearlite block size with different soft reduction parameters.
(Fig. 8f) indicate a high fraction of tightly packed small pearlite
colonies, and dislocation density around the ellipsoidal void
becomes maximum, which promotes its propagation. Infact, the
crack captured in SEM images is due to the micro voids coales-
cence. The large cracks formed due to the abnormally large austen-
ite grains with blocky ferrite along the PAGB [23]. The strength of
5
Materials & Design 209 (2021) 109978
GB-a is only 25% as compare to proeutectoid ferrite, which
increases the stress concentration due to the thermal or deforma-
tion stress. Therefore, GB-a weakens the PAGB by making it brittle
and decreases the thermo-plasticity of solidified microstructure.
GB-a associated with tightly packed pearlite colonies provides an
easier path for the intergranular void initiation.
Besides the tightly packed pearlite colonies and GB-a, the
large coarse austenite grains have a decisive role in the void for-
mation. Coarse grains can deform easily than the fine grains
caused by the combined effect of dislocations, which forms the
dislocation cells and promote void growth [24]. Prior austenite
grain size of solidified ingot structure is directly related to the
temperature and cooling homogeneity of molten metal. Prior
austenite grains continue to aggregate and grow abnormally with
a larger size than the primary grains. The ferrite phases were also
fully developed at the grain boundaries, as the temperature
reaches to 1300℃ or even higher. Dippenaar et al. referred the
larger austenitic grain about 1000 lm or greater in diameter as
blown grain, which had a significant role in the formation of
cracks [5]. During solidification, the shell of the cast ingot was
solidified earlier than the center region with lowering the tem-
perature from 1600 °C to room temperature. Therefore, a temper-
ature gradient exists from outer surface towards the core of ingot
and a columnar dendritic structure develops in the direction of
this temperature gradient along with the coarsening of
microstructure. The formation of shrinkage voids is due to the
N. Ali, L. Zhang, H. Zhou et al. Materials & Design 209 (2021) 109978

Fig. 8. Void initiation at GB-a: (a, d) EBSD band contrast images, (b, e) corresponding IPF maps and (c, f) grain boundary maps. (a-c) 2 mm and (d-f) without SR.

contraction of these aggregated dendritic arms, which could not
feed completely by the molten metal and interlock with each
other [28]. Moreover, the non-homogeneous cooling leads to the
shrinkage in solidified shell which generates an air gap at the
center region along with coarsening of austenite grains. Approxi-
mately blown grains are evident at reduction amount of 6 mm
and without SR technology, which weakens the bonding forces
between the grains. The voids can easily initiate at the grain
boundaries and coalesced to form the micro cracks by applying
small stress. Therefore, void’s morphology is a function of grain
size and small spherical voids are formed at reduction amount
of 2 mm and 4 mm, while the large and ellipsoidal voids are
formed at 6 mm and without SR technology due to coarse and
larger grain sizes from 608 lm to 903 lm.

Fig. 9. EBSD characterizations of void initiation at PAGB and pearlite colony boundaries at reduction amount of 2 mm. (a) band contrast image, (b) IPF map, (c) grain boundary
map, (d-f) Kernel average misorientation (KAM) map of voids at pearlite colony boundaries, and (g) KAM map of intergranular voids.

6
N. Ali, L. Zhang, H. Zhou et al. Materials & Design 209 (2021) 109978

To further investigate the voids initiation mechanism at PAGB exist in the vicinity of voids, which infact are due to the broken
and different pearlite colony boundaries, the band contrast images, cementite lamellae as shown in Fig. 10e. The KAM maps reveal a
inverse pole figures, and their corresponding kernel average high strain localizations around the already coalesced voids with
misorientation (KAM) maps are shown in Fig. 9. KAM is an an average diameter of 20 lm and 29 lm at reduction amount of
approach which shows a relationship between plastic deformation 4 mm and without SR respectively. Therefore, the boundaries of
and microstructural misorientation [18], and the high KAM values pearlite colonies are easily available sites for the void initiation,
present the high dislocation density. Voids are observed at PAGBs and its growth depends on the intersecting cementite lamellae to
and also in the grain interiors at reduction amount of 2 mm form the large ellipsoidal and shrinkge voids. The small intragran-
(Fig. 8a and b). For example, the voids in regions d, e, and f ular voids can grow into the bigger elongated voids by increasing
(Fig. 9d, e, and f) and in region g (Fig. 9g) are located inside of the tensile stress [28].
the PAGBs but further at the pearlite colony boundaries (intragran-
ular voids) and the PAGB (intergranular voids) respectively. Pear-
3.2.2. Micro void coalescence and crack formation at high reduction
lite block boundaries inside PAGB can be distinguished by HAGBs
amount
(Fig. 9c). The visible colors changing in the KAM map inside of
Fig. 11(a-d) represents the zigzag propagation of micro voids
two different pearlite blocks indicates the presence of cementite
through the pearlite colony boundaries at a high reduction amount
lammelae with high strain localization around each void as shown
of 6 mm, which coalesced to form micro crack. The KAM map
in Fig. 9d and e. Similarly, the strain localization is also maximum
shows a highly localized deformation field around the micro-
around each void located at colony boundaries as compare to the
crack than the isolated voids, as strain concentration at the colony
intergranular voids (Fig. 9f and g). EBSD cannot provide the misori-
boundaries exceeds from the maximum limit that the boundaries
entation values across the voids, rather the average misorientation
can tolerate. The high angle boundaries (Fig. 11c) correspond to
angle across the sub-grain boundaries of different pearlite colonies
the different pearlite blocks, which have a major role in the crack
connected with each void [25]. The average misorientation across
deviation or arrest. Voids and cracks grow through the boundaries
the block boundary associated with voids is 20-40°, which acts
of pearlite colonies and are deviated and stopped when met with
as an energy barrier and restricts the void growth at the block
the block boundaries. Similar results were reported by Zhou
boundary. The misorientation for colony boundaries is less than
et al., who found that the cleavage crack propagated through the
10°. Therefore, voids initiate at the pearlite colony boundary due
adjacent pearlite colonies and changed its direction at a block
to the low energy path and avoid the high energy barriers (block
boundary [29]. According to the theory of plasticity, higher misori-
boundaries), while intergranular void formation is due to the small
entation act as an energy barrier. The crack preferably propagates
and tightly packed pearlite colonies attached with GB-a.
toward the energy minimization path and avoids the high energy
Fig. 10a shows a high dislocation density at the block boundary
barriers [30]. Therefore, the high angle boundaries of the pearlite
from which a large ellipsoidal void is initiated. These dislocations
block at the crack tip can effectively hinder its propagation. Fur-
mainly possess the lamellar features with altering colores called
thermore, for all analyzed cases, the voids are not initiated at the
the disturbed zone as shown in Fig. 10b. The disturbed zone is
twin grain boundaries consistent with previous research reports
formed by the increased strain gradients close to the grain bound-
[18,28]. However, Fig. 10(e-h) shows a typical crack, which is prop-
ary due to non-uniform elastic–plastic incompatibility with the
agating through the sub-grain boundaries of different pearlite
adjacent grains and piles up of different dislocations [26], and
blocks. The high fraction of twin grain boundaries and highly
stress concentration have a crucial role to control the crack nucle-
misoriented 20–60° small dislocations (disturbed zones) are evi-
ation [27]. The void from the disturbed zone is not located at the
dent around the crack path, which leads to a high strain localiza-
PAGB but its peripheries are in contact with tightly packed pearlite
tion at the peripheries of the crack. It can be inferred that the
colony boundaries. Without SR technology, the disturbed zones
increasing reduction amount increases the stress concentration at

Fig. 10. EBSD characterizations of void initiation at different pearlite colony boundaries: (a-c) at 4 mm, (d-f) without SR.

7
N. Ali, L. Zhang, H. Zhou et al.
Fig. 11. EBSD characterizations at reduction amount of 6 mm: (a-d) micro void coalescence at pearlite colony boundaries and (e-h) crack propagation along the pearlite block
boundaries.
the PAGB and the pearlite colony boundaries. Therefore, the cracks
grow from stress concentration towards the stress-free areas. The
transformation from small voids to crack defects mainly depends
on the SR parameters, as the refined pearlite microstructure is evi-
dent at minimum reduction amount of 2 mm and 4 mm, while the
coarse and DP are obtained with 6 mm and without implementa-
tion of SR respectively. The voids have the following microstruc-
tural characteristics.
 These are associated with tightly packed small pearlite colony
boundaries possessing a small misorientation angle of approxi-
mately 10°, followed by low energy path and high strain local-
ization, while the block boundaries associated with voids have a
high misorientation of approximately 20–40°.
 The micro voids are coalesced to form the large ellipsoidal
voids, which are mainly surrounded by small and highly misori-
ented dislocations (disturbed zones) of 20-60°. A high strain
localization exists around the already coalesced large ellipsoidal
voids to form micro-cracks.
3.3. Statistical analysis of voids
3.3.1. Porosity
Fig. 12 shows a typical 3D rendering observed by X-ray com-
puted tomography (XCT) to illustrate the porosity in each sample.
It is evident that the porosity increases with increasing reduction
amount from 2 mm to 6 mm and is much higher without the
implementation of SR. Moreover, a high fraction of small isolated
and approximately spherical voids is obvious in Fig. 12a and b.
With increasing reduction amount to 6 mm and without imple-
mentation of SR, the small spherical voids were coalesced and
turned into elongated voids as shown in Fig. 12c and d. The statis-
tics of voids are shown in Table 2 and Table 3 at different reduction
amounts. Table 2 demonstrates the total number of voids, total,
maximum and average void volume, and porosity in each sample.
The morphology of voids is represented by the size of its major axis
and the aspect ratio (minor to major axis), which are detailed in
Table 2, and two different morphologies including gas pores and
shrinkage voids are identified. The gas pores are formed due to
8
Materials & Design 209 (2021) 109978
air entrapment and release of hydrogen gas during the casting pro-
cess and exhibit a spherical shape, while the volume contraction
during the solidification process leads to the shrinkage voids,
which are characterized by irregular shapes [31].
The number of voids and their volume has almost linear
increasing trend with increasing reduction amount from 2 mm to
6 mm as shown in Fig. 13. The least number of voids with their
lowest total volume is obtained at reduction amount of 2 mm.
However, the maximum major axis for this case is a little higher
than at 4 mm as shown in Fig. 14, which is due to the presence
of few irregular voids at the center of the specimen. At reduction
amount of 4 mm, the number of voids increases but a significant
decrease in total volume of voids and maximum major axis is
observed. Most of the voids are very small, which might be coa-
lesced to form the shrinkage voids. With increasing reduction
amount to 6 mm, the number of voids is less but the total volume
of the void defect and maximum major axis increases to a large
extent. It confirms the micro voids coalescence to form the large
irregular voids, as a result the number of voids decreases, and their
morphology changes from elongated to micro cracks and shrinkage
voids. As the aspect ratio decreases from 0.5 towards 0, corre-
sponding to an increase of the major axis, the voids changed from
spherical to the elongated shape [32]. Mainly at aspect ratio of 0.3–
0.5 the voids have larger major axis with the elongated morphol-
ogy, which presents the thin plates without branches [33]. There-
fore, the large elongated voids have the same morphology to the
micro cracks. The 3D voids morphology show a sheet with frac-
tured branches at aspect ratio < 0.2 with maximum major axis,
which indicates the shrinkage voids. Therefore, the results of XCT
and EBSD are consistent with each other. Without SR technology,
high saturation of 2187 voids occurs with their highest total vol-
ume and maximum major axis than all cases with soft reduction
processing, which implies that the SR technology can effectively
control the formation of voids and crack defects in medium carbon
steel.
3.3.2. Void size
From the perspective of void size distribution, Fig. 15 represents
the size of the void’s major axis distribution. Overall, the majority
N. Ali, L. Zhang, H. Zhou et al. Materials & Design 209 (2021) 109978

Fig. 12. 3-dimensional reconstruction of void defects: (a) 2 mm, (b) 4 mm, (c) 6 mm, and (d) without SR.

Table 2
Summary of voids statistics and characteristics at different SR parameters.

Reduction amount (mm) Total No. of voids (count) Total volume of voids (mm3) Porosity (%) Avg. void volume (mm3) Max. void volume (mm3)
2 247 0.11388 0.073 0.00012 0.00729
4 962 0.23294 0.163 0.00024 0.00444
6 933 0.37763 0.231 0.00041 0.00994
Without SR 2187 0.61079 0.461 0.00028 0.05285

Table 3
Summary of void size and their morphologies at different SR parameters.

Reduction amount (mm) Avg. major axis (mm) Max. major axis (mm) Avg. aspect ratio Min. aspect ratio Max. aspect ratio
2 0.0553 0.74 0.410 0.09 0.7
4 0.1292 0.59 0.509 0.25 0.75
6 0.1632 0.99 0.396 0.14 0.7
Without SR 0.116 1.82 0.535 0.13 0.75

of voids at reduction amount of 2 mm and 4 mm have the major
axis in range of 0–200 lm, while porosity was little increased in
the sample at reduction amount of 4 mm with a small and constant
average void volume due to increase in the number of gas pores.
With increasing reduction amount to 6 mm, the majority of voids
has major axis in the 0–400 lm range and has maximum porosity
despite a small number of voids due to the increase in average void
volume, which in turn is responsible for micro void coalescence
9
phenomenon. Without SR technology, several voids have their
major axis between 800 and 1900, which indicates the severe
shrinkage voids and cracks defect as discussed in the following
section.
3.3.3. Voids morphology
The detail about the different shapes of voids in terms of the
aspect ratio (minor to major axis) is depicted in Fig. 16. The sche-
N. Ali, L. Zhang, H. Zhou et al.
Fig. 13. Total number of voids and total volume of voids as a function of different
SR parameters.
Fig. 14. Total number of voids and maximum major axis of voids as a function of
different SR parameters.
matic of void shape is included in each histogram and the voids are
further categorized into strip, ellipsoids, and spherical shapes
according to the work of Garlea et al [32]. The voids are ellipsoids
at aspect ratio (minor to major axis) of 0.5, which turn into strip
shape as the aspect ratio decreases from 0.5 to 0, and become
spherical from elongated ellipsoids with increasing of aspect ratio
from 0.5 towards 1. The spherical voids are referred as gas pores,
while the strip to elongated ellipsoidal shape with aspect ratio of
10
Materials & Design 209 (2021) 109978
0.1–0.5 will be likely to form the shrinkage voids, which are further
detailed in the next section. In all cases, the voids exhibit strip
towards the ellipsoidal shapes.
3.3.4. 3-dimensional morphology of solidification shrinkage voids
Another approach to understanding the typical void morphol-
ogy is to plot the aspect ratio (minor to major axis) as a function
of the void’s major axis as shown in Fig. 17. With this perspective,
the gas pores, and solidification shrinkage can be easily distin-
guished. 3D morphologies of shrinkage voids are extremely com-
plex and larger, which exhibit irregular, angular, and large strips.
According to Li et al. the shrinkage defect formed by a cluster of
interlocked micro voids and always larger in size and more irregu-
lar in morphology due to a large number of aggregated dendrites.
[34]. The shrinkage voids contain ring-like and sharp tips features
existing in shrinkage defects. Cui et al. found that the ring-like
structure was due to the anisotropic growth of equiaxed crystals,
while the sharp tips induced certain stress at the rolling stage
and decrease the rolling yield [33]. Therefore, the shrinkage voids
are consisted on multiple branches which are connected with
bridges and might be extended in adjacent grains. The maximum
major axis of shrinkage voids was increased with increasing reduc-
tion amount. Without the implementation of SR amount, the sev-
ere shrinkage defect is evident and its major axis is twice as
compared to the major axis of shrinkage void at high reduction
amount of 6 mm. With increasing reduction amount to 6 mm,
the shrinkage voids are fully developed and will be further inter-
locked to initiate the micro cracks due to high stress concentration
at grain boundaries as discussed in the previous section. The over-
all major axis for different void morphologies is very small at min-
imum reduction amount of 2 mm and 4 mm than the high
reduction amount of 6 mm and without SR technology. The soft
reduction technology reduces the size of shrinkage voids from fol-
lowing aspects: (1) it breaks the bridges of the coarse equiaxed
grains and promotes the flow of molten metal towards the center
of ingot to compensate the solidification shrinkage; (2) it homoge-
nizes the temperature gradient and alloying segregation at the
solidification end to control the formation of shrinkage defects.
Therefore, soft reduction technology has a significant impact to
control the internal void defects. The optimum reduction parame-
ters are quite changing, and in our work, its efficiency is best at
minimum reduction amount of 2 mm and 4 mm, which is small
enough to compensate the shrinkage voids. Furthermore, the num-
ber of voids is also less with decreased porosity and overall major
axis as compared to the high reduction amount and without SR
technology. Thome et al. defined the optimum SR parameter as
the minimum reduction amount which is necessary to compensate
the shrinkage cavity during the solidification process without the
formation of internal cracks [35]. Li et al. concluded that reducing
the soft reduction amount from 3 mm to 2 mm lowers the critical
stress value to control the internal defects formation [11].
N. Ali, L. Zhang, H. Zhou et al. Materials & Design 209 (2021) 109978

Fig. 15. Major axis size distribution of voids at different soft reduction parameters.

Fig. 16. Voids distribution for aspect ratio at different SR parameters: (a) 2 mm and 4 mm, and (b) 6 mm and without SR.

11
N. Ali, L. Zhang, H. Zhou et al. Materials & Design 209 (2021) 109978

Fig. 17. Relationship between the voids major axis and aspect ratio with corresponding 3D morphology of shrinkage voids and gas pores: (a) 2 mm, (b) 4 mm, (c) 6 mm, and
(d) without SR.

12
N. Ali, L. Zhang, H. Zhou et al.
4. Conclusions
In this work, the void defects in medium carbon steel were ana-
lyzed by a comparative study with increasing soft reduction
amount from 2 mm to 6 mm and without SR technology. The cor-
relation between different SR parameters and voids formation was
determined by qualitative and quantitative results from
microstructure analysis, porosity, voids size, and void morphology
to investigate the optimized reduction amounts. The experiment
can present the following conclusions:
1. In medium carbon steel with ferrite-pearlite structure, the pear-
lite colony boundaries and the PAGB with enrichment of GB-a
acted as the void initiation sites. In the coarse austenite grain,
GB-a associated with tightly packed small pearlite colony
boundaries possessing a small misorientation angle of approxi-
mately 10° provides an easier path for the intergranular void
initiation. These voids coalesced to form the large ellipsoidal
voids and cracks surrounded by small and highly misoriented
20-60° dislocations (disturbed zones), at high reduction amount
and without the implementation of SR.
2. Small and tightly packed pearlite colonies have irregular and
broken cementite lamellae with higher dislocation density,
and voids can be easily initiated at the boundaries of different
pearlite colonies. The propagation of large ellipsoidal voids is
deviated and stopped when met with the high angle boundaries
of pearlite blocks.
3. The small number of voids with less porosity and their lowest
total volume is obtained at reduction amount of 2 mm. With
increasing reduction amount to 4 mm and 6 mm, the number
of voids is approximately the same, but a significant decrease
in the total volume of voids and maximum major axis is
observed for 4 mm than at reduction amount of 6 mm, which
confirms the micro voids coalescence to form the cracks at high
reduction amounts.
4. The number of voids increases with increasing reduction
amount, and high saturation of voids with severe defects was
obtained without SR technology.
5. The size of shrinkage void increases with increasing reduction
amount, which is twice in case of without implementation of
SR technology as compare with high reduction amount of
6 mm. Therefore, SR technology has a significant impact to con-
trol the void defects, and reduction amounts of 2 mm and 4 mm
are small enough to compensate the solidification shrinkage
voids.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
Acknowledgement
The successful completion of this project is benefited from the
financial support provided by the National Natural Science Founda-
tion of China (51874001, U1760108).
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