Materials Science & Engineering A 626 (2015) 375–381

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Materials Science & Engineering A

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

Microstructure and phase transformation of wear resistant ductile iron

grinding balls by continuous cooling process
Ting Sun, Ren-bo Song n, Xu Wang, Peng Deng, Chun-jing Wu
School of Materials Science and Engineering, University of Science and Technology Beijing 100083, China

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

Article history: The hardenability of wear resistant ductile iron austenitized at different temperatures was analyzed by
Received 4 July 2014 Jominy end-quenching test, and continuous cooling transformation (CCT) curves were determined by
Received in revised form Gleeble 1500D. The temperature variety curves were recorded by thermocouples during the test, and the
7 November 2014
cooling rate curves were obtained. It was indicated that there were significant influences of austenitizing
Accepted 19 December 2014
Available online 31 December 2014
temperature and Jominy distance (DJ) on the cooling rate. All specimens had undergone three different
heat transfer mechanisms including film boiling mechanism, nucleate boiling mechanism and natural
Keywords: convection mechanism. Meanwhile, the cooling rate also had a distinct influence on the microstructure
Electron microscopy characteristics of ductile iron. The results of hardness test and microstructure observation indicated that
Hardness measurement
the specimen austenitized at 830 1C had the most suitable hardness distribution, with high hardness
Ferrous alloy
on the quenching end and high toughness inside. That means that the grinding balls present function
Casting
Phase transformation gradient characteristic can be obtained after continuous cooling. In addition, as to the specimen
austenitized at 780 1C, the hardness was lower for the partially austenitized mixture microstructure. As
to the specimen austenitized at 880 1C, the coarsing of the microstructure occurred, which affected the
mechanical properties significantly.
& 2014 Elsevier B.V. All rights reserved.

1. Introduction Up to now, numerous studies about ductile iron focus on the

The ductile iron has been used as an important engineering
material for years because of its attractive properties such as, good
ductility, high fatigue strength and fracture toughness, etc [1–3].
In addition, the diameter of the ball mill has increased than before
obviously, for improving the efficiency of ore crushing [4,5]. The
world's largest ball mill has reached 13 m in diameter at present, and
the service condition of high hardness and impact load requires
higher toughness and hardness of grinding ball. Benefiting from the
multiple advantages, ductile iron is endowed a potential ability to
adapt to service condition in ball mill [6,7]. Especially as the bainite-
martensite ductile iron, with better mechanical property, was con-
sidered to be a substitution of the traditional grinding ball such as
low chrome white cast iron and low manganese steel [8]. At present,
there are two common heat treatment processings for bainite–
martensite ductile cast iron. One is isothermal quenching process [9],
in this way, the ductile iron named as austempered ductile iron (ADI)
is obtained; The other is continuous cooling process [10], which is
more convenient, economical and practical.
n
Corresponding author. Tel.: þ 86 10 82377990.
E-mail address: songrb@mater.ustb.edu.cn (R.-b. Song).
influence of chemical component or heat treatment process, which
are the critical factors affect the microstructure and mechanical
properties of ductile iron. Yang [11] has invented a new austem-
pering process for austempered ductile cast iron (ADI), and found
that the novel two-step process has resulted in improved micro-
structural variables in the ADI matrix, and higher hardness, yield
strength and tensile strengths, but lower ductility compared to the
conventional single-step austempering process; Murcia [12] stu-
dies the fabrication of dual matrix structures (DMS) ductile cast
irons with martensitic and bainitic structures in the as-cast
condition, and found that mechanical behavior of the material
was improved obviously after heat treatment; Han [13], has
studied the effects of austempering temperature and time on
scuffing behavior of austempered Ni–Mo–Cu ductile iron. Other
methods to enhance the properties of the ductile iron were also
discussed; Li [10] has studied the chemical composition range and
the heat treatment of austenitic–bainitic ductile iron produced by
continuous cooling, results show that the mechanical properties of
austenitic–bainitic ductile iron produced by continuous cooling are
close to those of isothermally treated iron; Sun [14] has obtained
bainitic-martensitic-austenitic ductile iron by continuous cooling,
studied the wear behavior and wear mechanism under impact
load. Peng [15] has investigated the influence of boron on the

http://dx.doi.org/10.1016/j.msea.2014.12.078
0921-5093/& 2014 Elsevier B.V. All rights reserved.
376 T. Sun et al. / Materials Science & Engineering A 626 (2015) 375–381

microstructure and mechanical properties of carbide austempered
ductile iron (CADI); Ghaderi [16] examined the effect of graphite
morphologies on the tribological behavior of austempered cast
iron. Podgornik [17] improved the wear resistance of ductile iron
through local surface reinforcement. Although numerous previous
studies have been performed about the heat treatment process
and wear behavior of ductile iron, there is still no in-depth
research on the microstructure characteristics of grinding ball
with large diameter. As to the grinding ball with 110 mm in
diameter, the matrix and mechanical properties are very hard to
guarantee, for the restriction of material's hardenability. So, more
attention should be paid on the hardenability of ductile iron in the
as-cast condition.
In this study, Jominy end-quenching test was applied to
examine the hardenability of grinding ball. The standard speci-
mens were cut out of the grinding ball along the radial direction.
Thermocouples installed on the specimens were used to record
the variation temperature values during the quenching operation.
The CCT curves of ductile iron were obtained and the effect of
High carbon content can improve the graphitizing ability and
sphericize of graphite. However, the excessive carbon content
causes more nodulizer consumption, a large extent of graphite
floating, and a decrease in mechanical properties [18]. Proper
silicon content can prompt graphitizing, prevent carbide from
precipitating, and decrease the austenite stability. It also reduces
the grain size, promotes bainite transformation and increases the
toughness [19]. The adding of manganese can improve the hard-
enability, and decrease the manufacturing cost for its cheap price
in China. Manganese has more affinity with carbon than Fe, so it
can prevent carbon from diffusing and precipitating [20].
1000
900
800
700
A+G F+G
600

Temperiture/
different austenitizing temperatures on the proportion of micro- 500
structure was studied. The main goal of this paper is to provide an P+F+G
400
increased understanding of grinding ball hardenability and the B+G
relationship between microstructure evolution and cooling rate. 300

200

100
2. Materials and methods M+G
0

C, Si and Mn, the main alloy elements in ductile iron, have the -100
10 10 10 10 10
largest influence on the mechanical properties and cast-ability.
Time/ s
Table 1 Fig. 3. CCT curves of ductile iron.
Chemical composition of the wear resistant ductile iron (wt%).

Element C Si Mn P S Mg Re Table 2
Label of specimens of Jominy end-quenching tests.
Weight% 3.5 3.3 3.0 o 0.1% o 0.04% 0.038 0.045
Specimen Temperature (1C) DJ (mm)

A-1 780 2
A-2 780 5
A-3 780 10
A-4 780 20
A-5 780 50

B-1 830 2
B-2 830 5
B-3 830 10
B-4 830 20
B-5 830 50

C-1 880 2
C-2 880 5
C-3 880 10
C-4 880 20
C-5 880 50
Fig. 1. The cylindrical bar cut from grinding ball.

Fig. 2. (a) Size of standard Jominy specimen and locations of thermocouples and (b) Cooling of Jominy test.
 T. Sun et al. / Materials Science & Engineering A 626 (2015) 375–381 377

M M
G
M
Fe3C

M+B
M+B

M+B

M+B
B

B B
G
B
P

P P

P
P

Fig. 4. Microstructures at different DJ (a) 780 1C–2 mm; (b) 830 1C–2 mm; (c) 880 1C–2 mm; (d) 780 1C–5 mm; (e) 830 1C–5 mm; (f) 880 1C–5 mm; (g) 780 1C–10 mm;
(h) 830 1C–10 mm; (i) 880 1C–10mm; (j) 780 1C–20 mm; (k) 830 1C–20 mm; (l) 880 1C–20 mm; (m) 780 1C–30 mm; (n) 830 1C–30 mm; (o) 880 1C–30 mm; (p) 780 1C–
50 mm; (q) 830 1C–50 mm; (r) 880 1C–50 mm (M is short for martensite; B is short for bainite; G is short for graphite; P is short for pearlite; F is short for ferrite).

Therefore, the austenite is stabilized and the hardness and harden-
ability are improved.
The chemical composition of ductile iron has therefore been
determined as is listed in Table 1. The ductile iron was melted in a
30 kg medium-frequency coreless induction furnace. The melt was
kept at 1550 1C for 5 min, and treated by 2.5% MgSiRE8 for
spheroidization and 2.1% FeSi75 for inoculation [21]. The melt
was poured into the metal mold which can produce three balls
with 110 mm in diameter, as is shown in Fig. 1. The grinding balls
were demoulded and cooled down in the open air after 15 min.
AC1, AC3 and CCT curves were determined by thermal dilatometer.
Three iron cylinders (diameter: 32 mm) were cut from each of
grinding balls, with the same microstructure after same casting
processing. The bars were heated to 860 1C, kept for 30 min and
normalization annealed at air cooling system. The specimens were
prepared according to the standard size (diameter: 25 mm; length:
100 mm) for Jominy end-quenching test. The thermocouples were
installed inside the holes with diameter of 1.5 mm and depth of
378 T. Sun et al. / Materials Science & Engineering A 626 (2015) 375–381
70
Marstenite
(1) M+B
65
Bainite
Hardness /HRC
60 (2) B+P
55 Pearlite
(3)
50
45
0 10 20 30 40
Jominy Distance- DJ / mm
Fig. 5. The Jominy hardness curves.
10 mm. The holes were placed at different locations along the
Jominy specimen, with the distance from quenching end of 2 mm,
5 mm, 10 mm, 20 mm and 50 mm, respectively. The iron cylinders
are heated within the austenitic domain during a preset time and
cooled by a water jet on its lower end (Temperature of water must
be between 15 and 25 1C). AC1 and AC3 were 770 1C and 830 1C
respectively, according to thermal expansion experiment. The
specimens were heated up to 780 1C, 830 1C and 880 1C, respec-
tively, and kept for 30 min to provide a uniform temperature
distribution. The Jominy end-quenching operation generally lasted
for 25 min, and ten temperature values were recorded every
second by thermocouples, and the temperature variation curves
were obtained as a function of time. Hardness measurements are
carried out along the cylinder axis as a function of distance from
the quenched end (2 mm, 5 mm, 10 mm, 20 mm, 50 mm). The size
of the standard specimen, locations of thermocouples and cooling
of Jominy test are shown as Fig. 2. The microstructure was
observed by using the ZEISS DV4 optical and ZEISS EVO18 scan-
ning electron microscope.
3. Results
3.1. CCT curves of ductile iron
The CCT curves of ductile iron are shown in Fig. 3, where v is
the cooling rate. The temperatures of Ac1 and Ac3 are 780 1C and
830 1C respectively, and the starting temperature of martenstic phase
transformation (Ms) is 180 1C, that is attributed to the addition of Mn
and Si, which decrease the Ms obviously. According to the CCT curves,
both of the pearlite and ferrite transformation are postponed but
incubation period of pearlite transformation is longer than that of
ferrite transformation. That can be attributed to the content of Si,
which is conducive to the formation of ferrite and fine acicular
bainite. The main matrix of pearlite was contained in the ductile iron
under a lower continuous cooling rate (vo4 1C/s), and the micro-
structure of bainite can be obtained while cooling rate is fast enough
(4 1C/sovo16 1C/s). The main matrix of martensite was obtained
when the cooling rate exceeded 16 1C/s. As shown in Fig. 3, during
continuous cooling, the shortest incubation times of bainite trans-
formation is about 24 s, whereas those are about 61 s and 218 s for
pearlite and ferrite transformation.
3.2. Microstructure
The identification of the specimens is listed in Table 2. The
evolution of the microstructure along the cylinder axis of Jominy
specimens (A-780 1C, B-830 1C, C-880 1C) are shown in Fig. 4. As to
780 the specimen A, near the quenched end with the DJ of 2 mm and
830 5 mm, the matrix was mainly fine martensite and a low amount of
880 disperse ferrite. It is indicated that the specimen was partially
austenitized at 780 1C. As to the DJ of 10 mm, complex phase
structure of fine bainite and martensite formed, As the DJ
increased to 20 mm and 50 mm, amount of pearlite formed from
the austenite. For the higher austenitizing temperature, specimens
B and C, the matrix near the quenched end was mainly fine
martensite, which indicated that the specimens were all fully
austenitized at 830 1C and 880 1C. For the specimen B, as the DJ
increased to 10 mm, a complex structure developed, characterized
by the presence of a larger amount of fine bainite and Martensite.
Compared with specimen A, a mass of pearlite developed together
50 60 with a small amount of bainite at the DJ of 20 mm. At the DJ of
50 mm, the matrix of all specimens was formed by mainly pearlite
and Fe3C. In addition, the grain coarsening was occurred in the
specimen austenitized at 880 1C, compared with specimen A and B.
3.3. Hardness curves
In all specimens, the hardness value decreases with the DJ, as is
shown in Fig. 5. The most characteristic is that each of the
hardness curves has two locations, where the value of hardness
is decreased sharply, which divide the whole curve into three
parts. The first region has higher hardness values, which should be
attributed to the matrix of mainly martensite located near the
quenching end. Then the decrease of hardness value comes with
the appearance of bainite, for the lower hardness of bainite than
marstenite. In the second relative flat region, the range of the
region is wider than the first region, but the hardness values
become lower relatively, which indicates a transition from auste-
nite to bainite. Then the decrease of hardness value occurs on
account of the perlitic transformation, and the hardness continues
to decrease along the cylinder axis. In addition, obvious differences
in details between the hardness curves can be seen in the Fig. 5.
The hardness values near the quenching end drops from 64.3–63.5
HRC in specimen-B, 62.5–62.1 HRC in specimen-C, and 59.1 HRC to
57.9 HRC in specimen-A, so it is easy to find that specimen-B has
the largest value of hardness among the three specimens. In
addition, the hardness of specimen-C is lower than specimen A
and B at the DJ of 50 mm. Comparing Fig. 4q and r, the coarse
grains of pearlite can be seen in Fig. 4r, and the average grain
diameter reaches up to 87 μm by means of Image-tool. However,
the average grain diameter of pearlite in specimen B-5, which
undergoing the austenitization temperature of 830 1C, is about
38 μm. Meanwhile, the results of hardness measurement show
that, the hardness of at DJ of 50 mm, undergoing the austenitiza-
tion temperature of 830 1C and 830 1C are 49.1 HRC and 47.0 HRC
respectively. So That the hardness decrease of specimen C-5,
which undergoing the austenitization temperature of 880 1C, can
be attributed to the coarsening of microstructure.
4. Disscusion
4.1. The influences of austenitizing temperature and DJ to cooling
rate
Fig. 6 shows the cooling rate at different DJ. It is easy to find
that the cooling rates of all specimens have the same varying
tendency, which is increased sharply at high-temperature stage
and decreased rapidly with the decrease of temperature. That is
attributed to the transform of heat transfer mechanism [22–24]:
At the initial stage, the film boiling heat transfer mechanism
plays the leading role as the water film formed on the surface of
 T. Sun et al. / Materials Science & Engineering A 626 (2015) 375–381 379

-350 -250
780 780
-300 830 830
880 -200 880
-250 D =2mm D =5mm

-200 -150
Cooling rate/

Cooling rate/
-150
-100

-100
-50
-50

0 0
900 800 700 600 500 400 300 200 100 0 900 800 700 600 500 400 300 200 100 0
Temperature/ Temperature/

-50 -14
780 780
830 -12 830
-40 880 880
D =10mm -10 D =20mm

-30
-8
Cooling rate/

Cooling rate/

-20 -6

-4
-10
-2

0 0
900 800 700 600 500 400 300 200 100 0 900 800 700 600 500 400 300 200 100
Temperature/ Temperature/

-10
780
-8 830
880
-6 D =50mm

-4
Cooling rate/

-2

900 800 700 600 500 400 300 200

Temperature/
Fig. 6. The influence of austenitizing temperature to the cooling rate at different DJ.

specimen, which lead to a low heat exchange coefficient; With the
decrease of temperature, the nucleate boiling mechanism took
place of the film boiling mechanism, that enhance the cooling rate
sharply to the peak value; With the further decrease of tempera-
ture, natural convection mechanism plays the leading role, and the
cooling rate decreases gradually. So, all the specimens have
undergone three different heat transfer mechanisms of film
boiling mechanism, nucleate boiling mechanism and natural
convection mechanism. In addition, the influence of austenitizing
temperature on the cooling rate is weakened observably along
with the increase of DJ. As to the DJ of 2 mm and 5 mm, the
influence of austenitizing temperature is significant. The peak
values of cooling rate of specimens A, B, and C are 310 1C/s,
183 1C/s and 107 1C/s, respectively, as is shown in Fig. 6a, b. This
is attributed to the influence of temperature variations between
water jet and specimen on the heat exchange coefficient [25]. As to
the DJ of 10 mm and 20 mm, the influence of austenitizing
temperature on cooling rates is weakened observably (Fig. 6c, d).
As to the DJ of 50 mm, the cooling rates at austenitizing tempera-
ture of 780 1C, 830 1C and 880 1C almost have no difference, with
the average value of 1.9 1C/s (Fig. 6e). According to the cooling rate
curves, it is easy to find that there is significant influence of DJ on
380 T. Sun et al. / Materials Science & Engineering A 626 (2015) 375–381

the cooling rate. Fig. 7 shows the cooling rate as a function of
temperature of specimen austenitized at 880 1C, the peak value of
cooling rate decreases rapidly from 310 1C/s to 5.3 1C/s along the DJ.
4.2. The influence of cooling rate to microstructure and hardness
curves
As shown in Fig. 8, cooling curves of specimens A, B, and C were
superimposed on the CCT curves of the ductile iron. It is easy to
find that all the cooling curves of specimens at DJ of 2 mm and
5 mm pass through the martensitic transformation zone. That is
attributed to the higher peak cooling rate, compared with the
specimens at the DJ of 10 mm, 20 mm and 50 mm. For a higher
peak cooling rate can reduce the residence time at the high
temperature section about 600–8001C. So that the cooling curves
-350
Austenitized at 880
-300
-250
-200
Cooling rate/
at DJ of 2 mm and 5 mm can avoid the bainite transformation zone
completely. As to A-1 and A-2, the main matrix of A-1 and A-2 was
consisted of martensite, graphite and a small amount of retained
austenite, as is shown in Fig. 9a. Though the matrix of mainly
martensite has high hardness (63 HRC), but the brittleness of
martensite is harmful to toughness of ductile iron [26]. As to the
DJ of 10 mm, cooling curves of specimen A, B and C all pass
through the bainite transformation and martensite transformation
areas. Fig. 9 b shows the microstructure of A-3, the main matrix is
consisted of bainite, graphite and a small amount of martensite.
The fine acicular structure is the bainite, which appears as black;
the martensite appears as gray, as is marked by dotted line, which
has bigger size compared with bainite. The formation of bainite
enhances the comprehensive mechanical properties of material.
For the bainite has good toughness and high hardness [27],
meanwhile, the specific bainite/martensite complex microstruc-
ture always exhibits superior high cycle fatigue properties [28]. As
2mm the DJ increased to 20 mm and 50 mm, the cooling curves pass
5mm through the pearlite transformation area completely, and a large
10mm amount of pearlite is formed, as is shown in Fig. 9c, the matrix of
20mm specimen B-5 is mainly pearlite and graphite. It is indicated that
50mm the cooling rate decreases sharply with the DJ, especially at DJ of
50 mm. As mentioned before, the average cooling rate at DJ of

50 mm was only 2 1C/s approximately.

-150

-100 5. Conclusions

-50 (1) Specimen austenitized at 830 1C has the highest hardness

values and more suitable hardness distribution. As to the
0 specimen austenitized at 780 1C, the hardness is lower for
900 800 700 600 500 400 300 200 100 0 the partially austenitized mixture microstructure. The speci-
men austenitized at 880 1C have good hardenability, but the
Temperature/
coarsing of the microstructure at a higher austenitizing tem-
Fig. 7. Cooling rate curves of specimen austenitized at 880 1C. perature affects the hardness significantly.

1000 1000 1000

900 900 900
800 800 800 C-4
700 700 B-5 700 C-5
A+G A+G C-3
F+G F+G
600 600 600 C-2
500
B-3 B-4
500 500
B-2 P+F+G P+F+G
400 400 400
B+G C-1 B+G
300 300 B-1 300
200 200 200

100 100 M+G 100 M+G

0 0 0

-100 -100 -100

10 10 10 10 10 10 10 10 10 10 10 10 10 10 10

Time/ s Time/ s Time/ s

Fig. 8. Cooling curves of specimens superimposing on CCT curves: (a) A-780 1C; (b) B-830 1C; (c) C-880 1C.

G G
Fe3C P

B G
M
M

Fig. 9. Microstructure of B-1 (a); B-3 (b); B-5 (c).

 T. Sun et al. / Materials Science & Engineering A 626 (2015) 375–381
(2) The cooling rates of all specimens have the same varying
tendency, which is increased sharply at high-temperature
stage and decreased rapidly with the decrease of temperature,
for all the specimens have undergone three different heat
transfer mechanisms of film boiling mechanism, nucleate
boiling mechanism and natural convection mechanism.
(3) The influence of austenitizing temperature on the cooling rate
is weakened observably along with the increase of DJ. The
significant influence at quenching end is attributed to the
influence of temperature variations between water jet and
specimen on the heat exchange coefficient, the cooling rates at
different austenitizing temperatures almost have no difference
when the DJ is more than 20 mm.
(4) The ductile iron undergoes martensite, bainite, and pearlite
transformation along the cylinder axis during the continuous
cooling from 830 1C. It is indicated that the grinding ball is
regarded to have high hardness on the surface and high
toughness inside after continuous cooling, which presents
property gradient characteristic.
Acknowledgments
The authors would like to express their gratitude to the
Materials Testing Center at the University of Science and Technol-
ogy Beijing for access to the medium-frequency induction furnace,
Gleeble 1500D, Jominy end-quenching tester and thermal dilat-
ometer equipment.
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