Original Research Paper

A study on the effect of process parameters in stirred ball mill

O.Y. Toraman
a,
*
, D. Katrcoglu
b
a
Mining Engineering Department, Nigde University, 51245 Nigde, Turkey
b
Graduate School of Natural and Applied Sciences, Nigde University, 51245 Nigde, Turkey
a r t i c l e i n f o
Article history:
Received 28 October 2009
Received in revised form 11 January 2010
Accepted 26 February 2010
Available online 6 March 2010
Keywords:
Fine grinding
Stirred ball mill
Process parameters
Statistical design
a b s t r a c t
An experimental study on the ne grinding of calcite powder (d
50
= 62.16 lm) using a 0.75 l laboratory
stirred ball mill has been carried out. The effects of various operating factors, such as grinding time
(min), stirrer speed (rpm), slurry density (wt.%) and ball lling ratio on ne grinding was studied under
batch wet conditions using alumina balls, 95% purity with diameters 3.54.0 mm. A series of laboratory
experiments using 2
4
full factorial designs was conducted to determine the optimum grinding parame-
ters. The test results showed that the stirrer speed and grinding time have strong effects on the grinding
efciency, based on the value of specic surface area (m
2
/g).
2010 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder
Technology Japan. All rights reserved.
1. Introduction
Recently, the need for ne particles in various industrial pro-
cesses has increased in the eld of preparing raw powders. There-
fore, the research in ne grinding has gained more importance.
Stirred ball mills produce ne and super ne material very effec-
tively, due to their easy processing, simple construction, high size
reduction rate and low wear contamination. Over the past decade,
stirred mills have begun to be used extensively in many industries,
including mineral, coal, ceramic, metallurgy, paint, chemical, agri-
culture, food, medicine and energy [13]. On the other hand, two
grinding modes including dry and wet modes are applied in the
grinding processes. The choice between dry and wet grinding is
inuenced by several factors. The condition of the raw material
and the downstream use as a powder or slurry determinate the
grinding process in many cases [4]. When wet grinding, impact ac-
tion is created by the constant impinging of the grinding media due
to its irregular movement. Shearing action is present as the balls
(media) in their random movement are spinning in different rota-
tion and, therefore, exerting shearing forces on the adjacent slurry.
As a result, both liquid shearing force and media impact force are
present. Such combined shearing force and impact results in the
size reduction as well as good dispersion [5]. Calcite powder
(CaCO
3
) is a salt, widely used in the ground form in paints, food,
and pharmaceuticals and as ller in the papermaking process; it
permits the production of brighter paper with greater resistance
to yellowing and ageing. Moreover, when used as a part of the
coating of the paper, it provides higher opacity, printability, ink
receptivity and smoothness. It is also used as ller in the plastic
industry to improve heat resistance, hardness, color fastness and
material stability [6].
The objective of this study is to investigate the effects of process
variables, such as grinding time, stirrer speed, slurry concentration
and ball lling ratio on mill grinding performance. For this, batch
wet grinding tests were performed in a laboratory stirred ball mill
using statistical design.
2. Experimental
2.1. Materials
Calcite powder (d
50
= 62.16 lm) used in the grinding experi-
ments was from Nigde, Turkey. Chemical properties of the sample
are shown in Table 1. The grinding media selected for the tests was
3.54.0 mm alumina balls. The physical properties of grinding
media are presented in Table 2.
2.2. Method
In the current study, grinding tests were carried out in a ver-
tical type stirred media mill Standard-01 Model manufactured by
Union Process (USA) (Fig. 1). The net volume of the milling cham-
ber is 0.75 l. In order to reduce the amount of wear from materi-
als of the mill, the grinding chamber is made of ceramic (Al
2
O
3
).
For cooling purposes, the grinding chamber is also equipped with
a water jacket for cooling. The grinding experiment was carried
out as a batch process in which samples were taken from the
0921-8831/$ - see front matter 2010 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.
doi:10.1016/j.apt.2010.02.018
* Corresponding author. Tel.: +90 388 2252290; fax: +90 388 2250112.
E-mail address: otoraman@nigde.edu.tr (O.Y. Toraman).
Advanced Powder Technology 22 (2011) 2630
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j our nal homepage: www. el sevi er . com/ l ocat e/ apt
pot at a determined grinding time interval. After each test, all of
the media and ground samples were removed from the mill, and
the media were separated from the products by sieving. In order
to investigate the effect of experimental parameters, such as
grinding time, stirrer speed, slurry density and bead lling ratio
(bulk volume related to the net volume of the grinding chamber)
on the specic surface area of the products, a series of experi-
ments were carried out. A Wet Laser Diffraction Particle Sizer
Malvern 2000 Ver. 2.00 with Hydro 2000 MU attachment (Mal-
vern Co., Ltd., UK) was used for the analysis of the feed and the
ground products. A dispersant was applied during the preparation
of the sample for sizing. Each test was repeated three times and
the values reported are a mean average.
In the current study, the process performance (grinding ef-
ciency) of grinding inorganic powder into ne particles using wet
grinding with a stirred ball mill was investigated by examining
how specic surface areas of ground products are affected by the
process parameters. In other words, the main goal was to establish
best set of variables that could be used in grinding for producing
the maximum specic surface area. The specic surface area is
one of the basic properties of the powder and is generally repre-
sented by the total surface area of all particles contained in a unit
mass of powder.
The specic surface area (m
2
/g) (SSA), derived from Lecoq et. al.
[7]:
SSA 6=q

s
d3; 2 1
Here q
s
is the specic gravity for calcite (t/m
3
); d(3,2) is the sur-
face-volume diameter, calculated from the Malvern MasterSizer
according to:
d3; 2
P
x
k
dk
3
P
x
k
dk
2
2
where x
k
is the number fraction of detected size d
k
(number, %) and
d
k
is the mean size of detected class (lm).
3. Statistical design
In the statistical design of the experiments, the effects of several
factors were studied, to determine the primary and interaction
effects of each. The effect of a variable is the change produced by
varying the level of that variable. When the effect of one variable
depends on the level of another, the two factors are said to interact
[8]. The success of ne grinding depends on the selection of suit-
able parameters and the optimization of these parameters necessi-
tates many tests. The total number of required experiments can be
reduced by employing a factorially designed series, using the Yates
technique [9].
In the present work, the main and interaction effects of four
variables on the ne grinding were investigated. All 2
4
full factorial
unreplicated experiments were carried out, to evaluate the main
and interaction effects of each variable in calcite grinding. Yates
notation was used in this work to name each treatment. For exam-
ple, treatment abcd was the experimental run in which the vari-
ables a (grinding time), b (stirrer speed), c (slurry density) and d
(ball lling ratio) were set to their high level. Sixteen sets of trials
are required according to the equation N = 2
n
, where N is the num-
ber of trials and n is the number of variables. The variables and the
levels of each of the 2
4
designs, along with the actual and coded
values of the variables of the experiments, are presented in Table 3.
The highest level was designated + and the lowest level was des-
ignated . According to the basic principles of experimental de-
sign, three experiments were carried out at the base level (Center
Point Response, CPR) to estimate the error and standard deviation.
Note that the initial setting (level) of operating parameters for ne
grinding with the stirred mill were: grinding time, 10 min; stirrer
speed, 300 rpm; slurry concentration, 30.0 wt.% and ball lling ra-
tio (% of mill volume), 40%; as shown in Table 3. The tests are listed
in Table 4 along with the alternative levels that were used in the
experiments.
4. Results and discussion
In this study, main and interaction effects of four variables on
the specic surface area (m
2
/g) of the ground product were inves-
tigated. In other words, the main goal has been to establish the
optimal set of variables that could be used in grinding to obtain
maximum specic surface area.
The Yates technique was used for the statistical design of 2
4
experiments (four being the number of parameters) and analysis
of the results. Table 5 shows the experimental conditions and the
resulting specic surface area (m
2
/g) in each experiment. The
experimental conditions were arranged in what is known as the
Yates order.
Table 5 combines the Yates technique with ANOVA (analysis of
variance) to simplify the decision about the signicance of the
parameters investigated. The procedure used to prepare the table
is as follows:
(i) The upper half of column (3) is obtained by adding succes-
sive pair responses, and the lower half is obtained by sub-
tracting successive pairs. Columns (4), (5) and (6) are
calculated in the same way.
(ii) Tests are repeated three times at the center points to estimate
the error associated with the determination of an individual
response which is required to test statistical signicance.
Table 2
Physical properties of grinding media.
Composition Density (t/m
3
) Hardness
Al
2
O
3
(95%) + SiO
2
(5%) 3.6 >1200 HV
Fig. 1. A stirred ball mill used in the experiments.
Table 1
Chemical composition (wt.%) of calcite.
CaCO
3
MgCO
3
Fe
2
O
3
SiO
2
Al
2
O
3
Total
99.5 0.2 0.01 0.01 0.02 99.74
O.Y. Toraman, D. Katrcoglu/ Advanced Powder Technology 22 (2011) 2630 27
(iii) The ANOVA procedure is applied.
(iv) The table value of F (1,16) for a = 0.05 is compared with the
calculated F value.
(v) If F
Calculated
> F
Table
, then decision is effective (E); If
F
Calculated
< F
Table
, then decision is not signicant (NS).
Statistical models to predict the specic surface area (m
2
=g)
can be built up using Yates data analysis (Table 5). These
models can be used to analyze the residues and check the
assumption about the experimental error distribution of the fac-
torial designs [10]. The regression equation with interactive
terms can be written as:
Y b
0
b
1
X
1
b
2
X
2
b
3
X
1
X
2
b
4
X
3
b
5
X
1
X
3
b
6
X
2
X
3
b
7
X
1
X
2
X
3
b
8
X
4
b
9
X
1
X
4
b
10
X
2
X
4
b
11
X
1
X
2
X
4
b
12
X
3
X
4
b
13
X
1
X
3
X
4
b
14
X
2
X
3
X
4
b
15
X
1
X
2
X
3
X
4
3
where Y is the response (specic surface area, SSA), X
1
is the grind-
ing time, X
2
is the stirrer speed, X
3
is the slurry density and X
4
is the
ball lling ratio.
The models for the specic surface area (m
2
/g) of the ground
calcite, which are based on Eq. (4), are formed using the effects
of each variable that are signicant at the 95% or higher condence
level, and are given below:
Y 1:78 0:2512X
1
0:3362X
2
0:0662X
1
X
2
0:2025X3
0:1562X
4
0:0825X
3
X
4
0:0625X
2
X
3
X
4
R
2
0:9316
Here, Y is the specic surface area (m
2
/g). The coefcient of
determination, R
2
, was used to check the models ability to accu-
rately predict the specic surface area. It is determined from the
following equation:
R
2
1
X
y
i
y
^
i

2
X
y
i
y

i

2
n o n h i
5
Here, y
^
is the predicted response variable and y

is the mean
experimental value. If R
2
is 1, then the prediction is nearly perfect.
However, if R
2
is zero, the model has little value. The empirical
models were found to accurately estimate the response variable
as indicated by an R
2
value (0.9316). The analysis of the residuals
in the specic surface area is shown in Fig. 2. According to these
results, the model was a good t that 93.16% of the variation could
be explained well by the model.
The primary effects of each variable on specic surface area that
are signicant at the 95% condence level are shown in Fig. 3. The
order of signicance is b > a > c > d. The stirrer speed (b) and
Table 3
Parameter codes and parameter values of the experiments.
Parameters Unit Parameter code Yates symbol Low level () Base level High level (+)
Grinding time min X
1
a 10 15 20
Stirrer speed rpm X
2
b 300 400 500
Slurry density wt.% X
3
c 30 45 60
Ball lling ratio % X
4
d 40 50 60
Table 4
2
n
factorial design matrix.
Exp. No. Factor levels
a b c d
1
2 +
3 +
4 + +
5 +
6 + +
7 + +
8 + + +
9 +
10 + +
11 + +
12 + + +
13 + +
14 + + +
15 + + +
16 + + + +
Table 5
Yates technique combined with ANOVA for specic surface area (m
2
/g) response.
Yates Order SSA Column Column Column Total effect (TE) [TE]
2
/16 D.F. F
Calculated
(7)/(8)Se
2
F
Table
(1,16,0.05) Decision
1 2 3 4 5 6 7 8 9 10 11
1 1.16 2.78 6.97 12.98 28.46 50.623225
a 1.62 4.19 6.01 15.48 4.02 1.010025 1 81.45362903 4.49 E
b 1.81 2.50 8.88 2.26 5.38 1.809025 1 145.8891129 4.49 E
ab 2.38 3.51 6.60 1.76 1.06 0.070225 1 5.663306452 4.49 E
c 0.99 3.85 1.03 2.42 3.24 0.6561 1 52.91129032 4.49 E
ac 1.51 5.03 1.23 2.96 0.04 0.0001 1 0.008064516 4.49 NS
bc 1.40 2.41 1.00 0.30 0.20 0.0025 1 0.201612903 4.49 NS
abc 2.11 4.19 0.76 0.76 0.88 0.0484 1 3.903225806 4.49 NS
d 1.67 0.46 1.41 0.96 2.50 0.390625 1 31.50201613 4.49 E
ad 2.18 0.57 1.01 2.28 0.50 0.015625 1 1.260080645 4.49 NS
bd 2.27 0.52 1.18 0.20 0.54 0.018225 1 1.469758065 4.49 NS
abd 2.76 0.71 1.78 0.24 0.46 0.013225 1 1.066532258 4.49 NS
cd 1.21 0.51 0.11 0.40 1.32 0.1089 1 8.782258065 4.49 E
acd 1.20 0.49 0.19 0.60 0.44 0.0121 1 0.975806452 4.49 NS
bcd 1.71 0.01 0.02 0.08 1.00 0.0625 1 5.040322581 4.49 E
abcd 2.48 0.77 0.78 0.80 0.72 0.0324 1 2.612903226 4.49 NS
SSA: specic surface area (m
2
/g); DF: degree of freedom; E: effective; NS: not signicant (a) grinding time (min); (b) stirrer speed (rpm); (c) slurry density (wt.%); (d) ball
lling ratio (%). Center Point Responses (CPR); (1) 2.01 m
2
/g, (2) 2.05 m
2
/g, (3) 2.22 m
2
/g.
S
2
e

P
3
i1
CPRi CPRaverage
2
2
S
2
e
0; 0124.
28 O.Y. Toraman, D. Katrcoglu/ Advanced Powder Technology 22 (2011) 2630
grinding time (a) have strong effects on the grinding efciency,
based on the value of specic surface area (m
2
/g). They have posi-
tive effects and their total effects (TE) are 4.02 and 5.38, respec-
tively (Fig. 3). It has been known that the stirrer speed is one of
the most important parameters since it acts on the number of con-
tacts between beads and the intensity of collision [11]. The effect of
stirring speed on specic surface area was studied by conducting a
series of grinding tests. The results show that as stirring speed is
increased (from300 to 500 rpm) the specic surface area increases.
On the other hand, the specic surface area of ground products is
also increased with the increase of grinding time. For instance, a
grinding time of 20 min. produced a median size of 5.65 lm with
its specic surface area of 2.11 m
2
/g, while at 10 min. a median size
of 12.64 lm with the 1.40 m
2
/g of was obtained. The variable slur-
ry density (c) has negative effect and its total effect (TE) is 3.24
(Fig. 3). The decrease in grinding efciency, based on the value of
specic surface area, at 60% solids may be attributed to an increase
in suspension viscosity. Because of this, it can be suggested that the
use of a viscosity modier may be benecial for ne grinding at
high per cent solids. The specic surface area of ground products
is also increased with the increase of all lling ratio (d). It has a po-
sitive effect and its total effect (TE) is 2.50 (Fig. 3). Moreover, the
ab, bcd interactions have positive effect whereas that of cd has neg-
ative effect on the specic surface area of the ground product of
ne grinding of calcite. Fig 4 shows the particle size distribution
of the best result, and Table 6 shows the particle size values (d
10
,
d
50
and d
98
) of the ground products.
5. Conclusions
A series of wet grinding experiment using calcite powder in a
vertical type stirred mill have been carried out in order to investi-
gate the inuence of various experimental parameters, such as
grinding time, stirrer speed, slurry density and ball lling ratio
on the particle size distribution and specic surface area of the
ground products. A series of laboratory experiments using 2
4
full
factorial designs was conducted to determine the optimum grind-
ing parameters. According to results from analysis of variance (AN-
OVA), the value of the determination coefcient (R
2
= 0.9316)
indicates that the model was a good t that 93.16% of the variation
could be explained well by the model. The stirrer speed (b) and
grinding time (a) have strong effects on the grinding efciency,
based on the value of specic surface area (m
2
/g). Their effects
are positive. The specic surface area of ground products is also in-
creased with the increase of all lling ratio (d). It has a positive ef-
fect. The variable slurry concentration (c) has a negative effect.
Based on the value of specic surface area, it is proposed that pro-
cess performance can be improved by carrying out low slurry con-
centration and high stirrer speed, grinding time and ball lling
levels.
Acknowledgement
The authors would like to thank the Nigde University Scientic
Research Projects Directorate (Project No. FEB2009/11) for funding
of this research work.
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y = 1.0113x - 0.0507
R
2
= 0.9316
0
0.5
1
1.5
2
2.5
3
0 0.5 1 1.5 2 2.5 3
Experimental (m
2
/g)
C
a
l
c
u
l
a
t
e
d

(
m
2
/
g
)
Fig. 2. Analysis of the specic surface area residuals.
-4
-3
-2
-1
0
1
2
3
4
5
6
a b c d
Fig. 3. Main effects of variables on specic surface area. (a) Grinding time, (b)
stirrer speed, (c) slurry concentration and (d) ball load (% of ball mill volume).
0
20
40
60
80
100
0.1 1 10 100 1000
Particle size, micron
C
u
m
u
l
a
t
i
v
e

f
i
n
e
r
,

%
feed
product
Fig. 4. Particle size distributions of the feed and best product (grinding time,
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balls, 4 + 3.5 mm).
Table 6
The particle size values (d
10
, d
50
and d
98
) of the ground products.
Products Particle size (lm)
d
10
d
50
d
98
1 2.07 15.71 58.32
2 1.49 7.59 28.22
3 1.32 6.60 25.30
4 1.10 3.94 4.81
5 2.41 22.7 112.95
6 1.42 11.82 54.67
7 1.60 12.64 51.87
8 1.09 5.65 23.28
9 1.36 8.04 45.95
10 1.16 4.60 20.93
11 1.08 4.50 20.30
12 0.99 3.13 12.99
13 1.92 15.20 66.60
14 1.94 15.54 74.93
15 1.39 7.30 29.61
16 1.00 3.99 15.12
O.Y. Toraman, D. Katrcoglu/ Advanced Powder Technology 22 (2011) 2630 29
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