Powder Technology 119 Ž2001.

257–268
www.elsevier.comrlocaterpowtec

Wet batch grinding of alumina hydrate in a stirred bead mill

H. Bel Fadhel, C. Frances )
´ Chimique UMR 5503 CNRSr INPT r UPS 18, Chemin de la Loge 31078 Toulouse Cedex 4, France
Laboratoire de Genie
Received 1 January 2000; received in revised form 1 October 2000; accepted 16 January 2001

Abstract

Experimental investigations on the wet batch comminution of an alumina hydrate in a stirred bead mill are presented. The influence of
some operating parameters Žmass solids concentration, initial size of particles, stirrer speed and beads size. on both the specific energy
and the size distribution of the ground product is discussed. The existence of a limit fineness has been put in evidence and the conditions
leading to a best efficiency of the process are defined.
A quantitative characterization of the morphology of the fragmented particles has led to the identification of the fragmentation path
occurring during the process. The analysis allows to interpret the evolution vs. time of the product size distributions characterized by a
multimodal pattern. q 2001 Elsevier Science B.V. All rights reserved.

Keywords: Grinding; Stirred media mill; Fragmentation; Size distribution

1. Introduction sufficiently stressed at a media contact, Ps , and the number

of particles in the chamber, Np :
Stirred bead mills are increasingly used in many indus- Nc Ps
trial applications for microgrinding, dispersion and disinte- SN s Ž 1.
Np
gration of solid particles in a wet phase. They are inten-
sively used for the production of paints, inks, fillers,
The number of media contacts is greatly influenced by the
coatings, pharmaceuticals, agrochemicals, ceramics, . . . .
hydrodynamic behaviour in the mill. It can be assumed
The importance of such mills increases steadily because of
that the number of media contacts in a stirred mill is
an increasing demand for fine and ultra-fine particles Žless
proportional to: the number of revolutions of the stirrer
than 1 mm.. Over the last few years, scientific research on
A N B, and the number of beads in the grinding chamber; a
stirred bead mills has been focused upon the relationships
function of beads size A d m B and the filling volume of the
between the comminution result and the specific energy
grinding media A wm B. The probability Ps depends on the
input w1–3x. Since the comminution process in stirred mills
type of grinding process. For the grinding of minerals and
is influenced mainly by the number of stresses imposed on
ceramic materials, Kwade et al. w4x demonstrated that Ps is
the product particle, described by the ‘stress number’, and
proportional to the active volume between two grinding
the stress intensity during each contact; the specific energy
beads, which is related to the media diameter. The follow-
can be considered as the product of stress intensity ŽSI.
ing relation for the stress number can then be derived:
and stress number ŽSN..
In a batch process, the average of stress events on each wm Ž 1 y ´ . Nt rs d p3
product particle is determined by the number of media SN A Ž 2.
contacts, Nc , the probability that a particle is caught and Ž 1 y wm Ž 1 y ´ . . d m2 rsusp cs

The stress intensity is determined above all by the kinetic

energy of the grinding media. It is thus proportional to the
mass of the beads and the square of the tangential velocity
)
Corresponding author. Tel.: q33-5-62-25-24-46; fax: q33-5-62-25-
of the grinding media. The latter can be considered as
23-45. proportional to the circumferential speed of the discs.
E-mail address: Christine.Frances@ensigct.fr ŽC. Frances.. Assuming that only single particles are stressed between

0032-5910r01r$ - see front matter q 2001 Elsevier Science B.V. All rights reserved.
PII: S 0 0 3 2 - 5 9 1 0 Ž 0 1 . 0 0 2 6 6 - 2
258 H. Bel Fadhel, C. Francesr Powder Technology 119 (2001) 257–268
the grinding media, Kwade and Schwedes w1x recommend
the use of the following relationship:
SI A d m3 rm Õ 2
Ž 3.
Thus, each process parameter which acts on the stress
number or the stress intensity, affects the specific energy
input and the comminution result. This theoretical ap-
proach is especially useful in accounting for process pa-
rameters and optimising operational conditions. Indeed, for
each product fineness, an optimum stress intensity of the
grinding media can be found, which leads to a minimum
specific energy input.
However, in such an approach, the comminution result
is generally only depicted by the median size of the
product. The product size distribution vs. grinding time
actually presents a more peculiar evolution with the ap-
pearance and disappearance of peaks in the distribution
pattern. Indeed, it is not uncommon that size reduction
processes involve bi- or multimodal particle size distribu-
tions, at least at some stages. This fact, which is often an
indication that the population is a mixture of subpopula-
tions, results from the fragmentation mechanism, induced
by the process, or the initial texture of the material.
The aim of this study is to analyse the influence of the
operating variables during batch wet grinding on both the
specific energy and the size distribution of the ground
product. A morphological study has also been conducted to
determine the fragmentation mechanism and explain the
presence of specific subpopulations in the ground product.
2. Experimental
The experimental material was an alumina hydrate Žgib-
bsite., Al 2 O 3 , 3H 2 O provided by Aluminium Pechiney
ŽGardanne, France.. Some physical and chemical proper-
ties of that material are given in Table 1. The initial
particles are agglomerates formed by an association of
large platelet shaped crystallites, constituted by a series of
pseudo-hexagonal plates. For the grinding experiments, the
suspension was made of gibbsite particles in an aqueous
solution of sodium metaphosphate at 4 grl in order to
avoid the agglomeration of fines after a few minutes of
grinding.
Grinding experiments were performed in a 0.6-l hori-
zontal, stirred ball mill ŽDrais Perl-Mill Eirich-Gruppe..
Table 1
Physical and chemical properties of gibbsite
Alumina hydrate Crystalline system Density Refraction index
hydrargillite monoclinic 2.42 1.57–1.59
Chemical Na 2 O CaO SiO 2
composition
ppm 1650 80 25
The mill consists of a glass chamber and a stirrer shaft
fitted with four stainless steel agitator disks. The agitation
speed was controlled by a pulley arrangement, giving four
speeds of 2130, 2810, 3660 and 4370 rpm. For cooling
purposes, the grinding chamber is equipped with a water
jacket in which cooling water, from a thermostatic bath,
flows. Glass beads were used as the grinding media.
The standard grinding chamber was replaced by a
chamber which allows sampling from inside the mill by
means of a syringe without stopping the grinding operation
allowing no disturbance of the grinding environment. Five
sampling points are thus distributed along the grinding
chamber which allow sampling at the inlet, in the chamber,
in each space between two disks and just before the
separation gap as illustrated in Fig. 1. For continuous
operation, the mill is fed by a suspension contained in a
20-l mixed tank by means of a peristaltic pump. The runs
reported here were performed in the batch mode. For this
purpose, the inlet and outlet ports were closed. The grind-
ing chamber was vertically oriented and partially filled
with the beads before introduction of the desired mass of
gibbsite. The required volume of sodium metaphosphate
aqueous solution was added in turn, and the agitator turned
manually to eliminate air trapped between the beads. At
last, the chamber volume was filled by the remaining load
of beads. Samples withdrawn from inside the mill during
the operation were diluted to an appropriate concentration,
then processed for 5 min under ultrasound, before size
analysis by a diffraction laser sizer using the Mie theory
ŽMalvern Mastersizer S.. To ensure that the samples were
representative of the whole charge, the particle size distri-
butions of samples withdrawn at different time intervals
from the two sampling points Ž1. and Ž3. were compared
ŽFig. 2.. The results show the particles are fully mixed
during discontinuous runs, even after a very short period of
time. So, for the proceeding experiments, samples were
withdrawn from the central sampling point Ž3..
The specific energy input can be experimentally deter-
mined by means of a torque-speed meter or by measuring
the electrical power input of the mills:
E Pt Prs t
Ev s s s Ž 4.
Vs Vs ms
Power characteristics of stirred bead mills are usually
defined using an approach developed from work on stirred
Hardness
Mohs’ scale
3
Fe 2 O 3 TiO 2 V2 O5 ZnO Soluble pH in
soda sol.
130 5 -5 17 30 8.2
 H. Bel Fadhel, C. Francesr Powder Technology 119 (2001) 257–268 259

Fig. 1. Grinding chamber of the stirred bead mill.

reactors. In order to establish relationships between power NR e and NF r are the stirrer Reynolds number and the
consumption and the process variables, dimensional analy- Froude number, respectively:
sis is required. For fixed stirrer geometry, the expression
is: NR e s ND 2rsusprmsusp Ž 7.
Np s f Ž NR e , NF r . Ž 5.
NFr s N 2 Drg Ž 8.
where Np is the power number Žalso called the Newton
number., analogous to a drag coefficient, it is defined as: The power number can be obtained using graphs where Np
is plotted vs. Reynolds number of the stirrer as a function
Np s Prrsusp N 3 D 5 Ž 6. of the grinding chamber volume and the operational pa-

Fig. 2. Comparison of the size distributions of samples from sampling points Ž1. and Ž3..
260 H. Bel Fadhel, C. Francesr Powder Technology 119 (2001) 257–268
rameters Žfilling ratio, beads size and nature. w5,6x. The
specific energy is then defined as:
Np N 3 D 5rsusp rs t
Ev s
ms
3. Effect of the parameters on the comminution results
In this study, four process parameters were selected for
investigation, namely the slurry density, initial size of
particles, stirrer speed and beads size. The operating pa-
rameters were varied in the following range:
Solids mass cs s 0.1; 0.2; 0.3
concentration
Material initial d p Ž0. s 63–71; 71–100; 100–125 mm
size Žclosed
sieved size
fractions.
Agitation N s 2130; 2810; 3360; 4370 rpm
speed
Bead size d m s 0.4–0.56; 1.2–1.4; 1.8–2.2 mm
The bead load Žthe percentage of the net mill volume
filled with beads. was kept constant at 80%.
The initial size distribution is characterized by a single
peak with a high intensity indicating that the product
contains quasi mono-sized particles. An example of the
evolution of the size distributions vs. time is given in Fig.
3. Whatever the operating conditions, fragment size is
characterized by a similar multimodal distribution. At the
first few seconds of grinding, the size distribution of the
Fig. 3. Typical evolution of the size distributions vs. grinding time.
initial load disappears providing coarse fragments and
fines with an average size of 0.4 mm. As grinding pro-
ceeds, the size distributions shifts towards smaller sizes
Ž 9. and the fraction of fines increases more and more until the
size of fragments reaches that of the fines. The influence
of the operating parameters on the product size distribution
has been investigated, analysing the evolution of the me-
dian size and the standard deviation of the distribution.
Figs. 4a, 5a, 6a, 7a and b present the evolution of the
median diameter vs. grinding time for different operating
conditions. Whatever the values of the operating parame-
ters, the median size sharply decreases during the first
minutes of grinding and then tends towards a limit size
around 0.4–0.5 mm. Obviously, the finer the fragments,
the lesser the chance of cracks and defaults in the volume
of the particles, hence the stronger the particles become.
Finally, a limit size is reached. This extreme fineness,
described by many authors w7x, corresponds to a dynamic
equilibrium. Here the fines produced by grinding aggregate
to each other leading to coarse particle production, this is
balanced by their subsequent down. The effect of the
operating parameters on the comminution of gibbsite can
only be investigated during the first 10 min. After this
period, the curves of the median sizes vs. time related to
the different runs meet and tend towards the same limit
fineness.
The evolution of the standard deviation vs. grinding
time ŽFigs. 4b, 5b, 6b, 7c. is characterized by a very sharp
increase followed by a progressive decrease later. The first
part of the curves corresponds to the simultaneous produc-
tion of coarse fragments and very small debris. The size
distributions initially spread between 0.1 and 100 mm.
 H. Bel Fadhel, C. Francesr Powder Technology 119 (2001) 257–268 261

Then, the coarser fragments are progressively broken and
the size distributions become narrower. The breakage of all
initial particles into finer pieces is extremely fast, and the
increase in standard deviation vs. time cannot be observed
in all curves since the first sampling points correspond to
grinding times equal or longer than 10 s.
3.1. Effect of the solids concentration
The solids concentration is usually considered as an
important parameter. An increase in the solids concentra-
tion leads to an increase in the number of particles and
hence the stress number, i.e. increase in the probability of
a particle to be in the stressing zone. However, the more
concentrated the suspension, the more viscous is the slurry
and the lesser the probability of contact between particle
and bead. The effect of the solids concentration on the
comminution result depends mainly on the material and
other operating conditions. Concerning the grinding of
limestone, Stehr and Schwedes w8x found that at a first
approximation, the effect of the solids concentration could
be well described by the specific energy; i.e. the median
diameter of the ground product plotted against the
volume-based energy input are well described by a single
straight line on a log–log graph. Thus, whatever the solids
concentration, a required fineness can be reached if the
corresponding specific energy is brought changing one or
another parameter. But at low solids concentration, more

Fig. 4. Effect of the solids concentration on Ža. the median diameter, Žb. the standard deviation of the size distribution and Žc. the specific energy.
262 H. Bel Fadhel, C. Francesr Powder Technology 119 (2001) 257–268

specific energy is required to achieve the same product
fineness w4x, since a particle is not necessarily caught at
each media contact. For higher solids concentrations, diffi-
culties arise in the flow of the suspension. Analysing the
batch grinding of black carbon in a stirred bead mill,
Varinot w9x found an optimum in the solids concentration
between 5% and 20% allowing a better efficiency. The
existence of the optimum was explained by a change in the
fragmentation mechanism, mainly abrasion at lower solids
concentration to fracture at higher concentrations. Fig. 4
presents the effect of the solids concentration for the
comminution of gibbsite on: the median size ŽFig. 4a., the
standard deviation of the size distribution ŽFig. 4b., and
the specific energy ŽFig. 4c.. Since the runs reported in
Fig. 4 were performed using the same chamber and stirrer
geometries and keeping constant the beads size and the
filling ratio, the specific energy is proportional to
N 3rsusp trm s , this has been reported in Fig. 4c x-axis. The
curves of the median size and the standard deviation vs.
time are practically superposed taking into account of the
variation of the position of the initial median size which
lies between 115 and 125 mm. Thus, the fragmentation
kinetics may be considered the same for the solids concen-
tration between 10 and 30 wt.%. Moreover, the energy
efficiency decreases on increasing the concentration. Due
to the rapid decrease in size, the difference in the solids

Fig. 5. Effect of the initial size of material on Ža. the median diameter, Žb. the standard deviation of the size distribution and Žc. the specific energy.
 H. Bel Fadhel, C. Francesr Powder Technology 119 (2001) 257–268 263

concentration is not enough to alter the grinding kinetics.
However, the specific energy needed to obtain a certain
value for the median size is high, especially with the dense
nature of the slurry. This is probably due to the increase of
the viscosity increasing the solids concentration.
3.2. Effect of the initial size of particles
The effect of the initial size of particles is not often
investigated in the literature since it is usually imposed by
the industrial production constraints. Fig. 5 illustrates the
effect of the initial size for the comminution of gibbsite.
On Fig. 5c, the median size has been plotted vs. N 3 t since
the mill and the stirrer geometries as well as the operating
conditions related to the beads and to the slurry were kept
constant. During the first minute of the operation, it can be
noticed that the smaller the initial size, the smaller the size
of the ground product; beyond this point, the median sizes
merge. The particles before grinding present the same
morphology whatever their size. Consequently, the frag-
mentation mechanisms are the same. The evolution of the
standard deviation ŽFig. 5b. during the first minute of the
comminution process shows that the size distribution
spreads over size especially as the initial size is large. This
is due to the production of very fine particles from the
very first seconds of grinding, whatever the initial particle
size. As mentioned before, the weight fraction of that
population of fines increases progressively. As grinding

Fig. 6. Effect of the agitation speed on Ža. the median diameter, Žb. the standard deviation of the size distribution and Žc. the specific energy.
264 H. Bel Fadhel, C. Francesr Powder Technology 119 (2001) 257–268
proceeds, the sizes of fragments become less dispersed and
the standard deviations are identical after 2 min of grind-
ing. Concerning the effect of the initial size on the specific
energy, the curve of the median size vs. the specific energy
slightly depends on the initial size for the lowest values of
the specific energy, i.e. during the first minutes of the
process. That result is coherent with the fact that the larger
the initial particle size, the greater the energy requirement,
for a given degree of fineness to be reached.
3.3. Effect of the agitation speed
The agitation speed is an important parameter since it
acts on the number of contacts between beads and the
intensity of collision. The effect of the agitation speed is
presented here in Fig. 6. The evolution of the median size
as function of the grinding time ŽFig. 6a. shows that the
higher the agitation speed, the more important the frag-
mentation kinetics and the more rapidly the limit fineness
is reached. The same behaviour is observed for the change
of the standard deviation vs. time ŽFig. 6b. indicating a
contraction of the size distribution more rapidly increasing
the agitation speed. For the slowest agitation speeds Ž2130
and 2810 rpm., it can be noticed that the standard devia-
tion increases first indicating that the size distributions
spread over size during the first minute of grinding. That
step cannot be observed for higher agitation speeds be-
cause it occurs during too short a time. Fig. 6c illustrates
the effect of the stirrer speed on the specific energy. The
evolution of the median diameter has been reported on this
graph as a function of N 3 t since the mill geometry and all
the operating conditions, except the agitation speed, were
kept constant for these runs. It can be observed that for
Fig. 7. Effect of the bead size on Ža. the median diameter for short grinding times, Žb. the median diameter on longer grinding times, Žc. the standard
deviation of the size distribution and Žd. the specific energy.
low values of the specific energy, i.e. during the first
minutes of the batch process, the stirrer speed has no effect
on the comminution result. That result agrees with those of
Stehr and Schwedes w8x and Schwedes and Bunge w10x,
who found that the median size could be described by a
power function vs. the volume-based energy input, giving
a single straight line when plotted on log–log diagram,
independently of the way this energy was achieved and
particularly, independently of the value of the stirring
speed. But, for higher energies, the efficiency decreases as
the stirrer speed is increased. Indeed, for constant specific
energies, the product becomes coarser with the speed.
Increasing the stirrer speed, the stress intensity and the
number of contacts between beads Žstress number. both
increase. The ground size distribution depends more of the
energy needed to break particles than of the energy dissi-
pated by the stirrer. That means that only a part of the
energy brought by the process is used in the comminution
step. So, in the case where the energy supplied is greater
than the energy actually needed for the fragmentation, the
added energy gives no advantage for the fineness reached
and for the process efficiency. The best efficiency is
obtained when the stress intensity produced by the beads is
just enough to break the intra-particles forces andror to
propagate cracks. The optimum efficiency obtained here is
for the slowest stirrer speed which has been used Ž2130
rpm.. This is probably due to the initial size of the material
which is rather coarse and to the good grindability of
gibbsite ŽMohs hardnesss 3.5.. A similar result has been
observed for the submicron dispersion of titanium dioxide
in the same apparatus and for similar operating conditions
w11x. Moreover, the added energy which is not used during
the comminution step is transformed into heat. Sometimes,
 H. Bel Fadhel, C. Francesr Powder Technology 119 (2001) 257–268
Fig. 7 Ž continued ..
the cooling system is not sufficient to balance the increase
of the temperature in the mill volume leading to work in
bad conditions and even to stop the process. So, during
discontinuous processes, lower stirrer speeds can lead more
slowly to a required product fineness but with a better
efficiency.
3.4. Effect of the beads size
Many investigations have shown that the size of the
grinding beads greatly affects the comminution results
w1–4,9–16x. Mankosa et al. w12x and other authors sug-
gested that the optimum ratio between beads and particles
sizes is 20r1. Relating to the batch comminution of
limestone using glass beads, Kwade et al. w1–4x showed
that the specific energy consumption can be considerably
reduced, by choosing an appropriate bead size in relation
to the required fineness. The evolution of the median size
265
and of the standard deviation of the size distribution vs.
grinding time for the batch grinding of gibbsite are re-
ported in Fig. 7Ža–c.. During the first minutes of the
grinding process ŽFig. 7a and c., the grinding rate and the
narrowing of the size distribution are more rapid using
coarser beads. The opposite tendency is then observed
ŽFig. 7b and c.. These results agree with those of the
literature given before. During the first period of the
operation, the median size of the particles ranges approxi-
mately between 100 and 10 mm and the larger beads
w1.8–2.2 mmx are more advantageous on the view point of
the time necessary to reach a required fineness. It can be
noticed that the ratio between beads and particles sizes lies
between 20 and 200. But, when the median size is lower
than a few microns, smaller beads w0.4–0.56 mmx, for
grinding times greater than 10 min, become more advanta-
geous. The limit fineness reached using these beads is
around 0.5 mm after 20 min. The ratio between beads and
266 H. Bel Fadhel, C. Francesr Powder Technology 119 (2001) 257–268

particles sizes is much greater than the one suggested by ber of erosions necessary to eliminate the particle silhou-
Mankosa et al. w12x even in this case. Using smaller beads ette Ž w 1 . and its residual set, with respect to its convex
would theoretically lead to a more rapid size reduction bounding polygon Ž w 2 . w17x. These descriptors are defined
during the second period of the operation. However, the by:
difference observed using small w0.4–0.56 mmx or interme-
V 1 s 2 w 1r'A and V 2 s 2 w 2r'A Ž 10 .
diate sized beads w1.2–1.4 mmx is not important, but the
profit from use of smaller beads would be limited. Con- Ž4. The 3D-complexity or simplicity Ž S . evaluated by a
cerning the effect of the beads size on the specific energy, partition-in-squares w18x. The zones between edges
results have been reported in Fig. 7d. As it has been Žborderline, facet edges. of an object Žparticle silhouette or
mentioned before, the specific energy, defined by Eq. Ž9. particle facets. are divided into squares of increasing size,
depends on the power number, a function of the grinding such that the total available area of the object is covered. A
chamber volume and the media characteristics. Since all distribution in number f Ž x . of squares of size x results:
the operating parameters except the beads size were kept
constant for the runs reported in Fig. 7, the ratio of the F Ž u . s f Ž u . d u where
H u s xr'A Ž 11 .
specific energy on the power number is proportional to
N 3 t. Thus, it can be interesting to analyse the position of The simplicity of the particle is then defined as:
the curves giving the median size vs. N 3 t for the different
beads sizes. The results confirm the conclusions given H 1yF facet Ž u. d u
before. The input specific energy can be significantly Ss Ž 12 .
reduced by choosing an adequate bead size, relating to the H 1 y Fsilhouette Ž u . d u
fineness required. It can also be noticed that whatever the
bead size, the curves tend towards the same limit of S may vary between 0 and 1: the lower the S, the more
fineness and the additional energy is lost. This is particu- complex is the structure.
larly obvious in Fig. 7d for the run performed with the Average values of FmaxrFmin , V 1 , V 2 and S as a
smallest beads. function of the grinding time have been reported in Table
2. The evolution of the morphological descriptors shows a
drastic change in the first instants of the operation, indicat-
4. Effect of comminution process on the particle mor- ing that fragment shape is completely different to the
phology shape of the initial particles. The evolution of the ratio
FmaxrFmin presents a maximum. Initially, the gibbsite
Whatever the operating conditions, the size of frag- particles have a global spherical shape, as it can be ob-
ments produced during the comminution operation is rep- served in Fig. 8a, and the calculated ratio of Feret diame-
resented by a multimodal distribution, as illustrated in Fig. ters is close to 1. The increase of FmaxrFmin during the
3. This reveals the production of fragments belonging to first period of grinding indicates that the fragments are
specific size classes coming from a quasi monodisperse more elongated than the initial particles. SEM photographs
material. A quantitative characterization of the morphology of ground gibbsite show two types of fragments are pro-
has been made in order to determine the fragmentation duced by chipping due to the rupture of grains joints on
route in relation with the initial structure of the material. the initial particles. One can observe platelet-shaped crys-
For this purpose, dried samples were observed by scanning tallites ŽFig. 8b. and pieces of agglomerates ŽFig. 8c..
electron microscopy ŽSEM., associated with a direct cap- After this period, the elongation of the fragments decreases
ture system of digital images ŽJeol TM 330A.. Professional because the platelet crystallites are broken in turn giving
image analysis package Visiloge 4.1.4 ŽNoesis, ´ Les Ulis, more rounded fragments.
France. and a software developed by Pons et al. w17,18x Moreover, the initial particles are rather compact Ž V 1 s
were used. The evolution of the morphology during the 0.75. and present a lesser number of concavities Ž V 2 s
grinding runs has been quantified by means of the follow-
ing various descriptors Table 2
Ž1. The projected surface area of the particle onto the Variation of the morphological descriptors vs. grinding time
image plane Ž A.. Time Fma x r Fmin V1 V2 S
Ž2. The maximal Ž Fmax . and minimal Ž Fmin . Feret diam-
0 1.30 0.753 0.045 0.25
eters obtained on the particle silhouette from which is 10 s 1.97 0.654 0.094 0.40
deduced the ratio of Fmax over Fmin , characterizing the 30 s 1.77 0.655 0.105 0.18
elongation of the particles. The ratio is equal to 1 for a 1 min 1.64 0.652 0.083 0.26
spherical object and greater than 1 for an elongated one. 1.5 min 1.70 0.651 0.096 0.14
4 min 1.71 0.686 0.082 –
Ž3. The compacity Ž V 1 . and the largest concavity Ž V 2 ..
5 min 1.46 0.691 0.100 0.15
They are determined by comparing the particle silhouette 10 min 1.48 0.697 0.086 0.18
to its convex bounding polygon, and estimating the num-
 H. Bel Fadhel, C. Francesr Powder Technology 119 (2001) 257–268
Fig. 8. Typical SEM photos of gibbsite: Ža. raw material before grinding and Žb and c. after 1 min of grinding.
0.045.. The compacity drastically decreases during the first
seconds of operation and slowly increases thereafter. At
the same time, V 2 sharply increases and stays approxi-
mately constant then. The elongated platelet crystals pro-
duced during the first step of the process are much less
robust than the raw material. This favours the creation of
concavities in the parent particles. Then the compacity
increases due to the increase in the percentage of very
small fragments, which are increasingly robust with pro-
gressive disappearance of concavities. The evolution of the
three-dimensional shape values shows a rapid simplifica-
tion of the structure during the first step of the process
indicating that the platelet-shaped crystallites have less
facets than the initial agglomerates. Due to their elongated
shape, these crystallites lay flat on the SEM sample holder
exhibiting a high simplicity. Later, S decreases vs. time
revealing the progressive complexification of the structure.
These fragments are small sandwiches of platelets which
due to their compactness are laying somewhat sideways on
the sample holder.
From the morphological analysis, the following frag-
mentation route can be drawn. The initial population of
particles constituted by spherical shaped, compact and
facetted agglomerates are broken giving two kinds of
fragments. The coarser fraction, the median size of which
varies from 100 to 10 mm is composed of platelet-shaped
267
crystals and pieces of agglomerates. These are more elon-
gated, less compact, and have more concavities and less
facets than the raw material. The finer fraction, which
progressively increases is made of very small fragments
less and less elongated but more compact with a rougher
surface.
5. Conclusions
The experimental investigations concerning the com-
minution of gibbsite in a stirred bead mill show that the
operating parameters affect the grinding rate, i.e. the time
necessary to reach a certain fineness, and the specific
energy consumption. Whatever the operating conditions,
the median size of the ground product tends towards a
limit size. Moreover, consider the following factors.
Ž1. The higher the density of the slurry, the higher the
specific energy needed to obtain a fixed median size.
Ž2. The larger the initial particles, the higher the energy
needed to reach a given degree of fineness.
Ž3. The higher the stirrer speed, the higher the grinding
rate and the specific energy consumption. The best effi-
ciency is obtained when the stress intensity produced by
the beads is enough to break the intra-particle forces, until
the achievement of the limit size. The added energy gives
268 H. Bel Fadhel, C. Francesr Powder Technology 119 (2001) 257–268

no advantage for the fineness reached or for the process t Grinding time wminx
efficiency and can even lead to overheating. Õ Circumferential speed of stirrer discs wmrsx
Ž4. The beads size strongly affects the comminution Vs Volume of particles in the mill wm3 x
result. The input specific energy can be significantly re- x Size wmmx
duced choosing an adequate beads size in relation to the wm Beads filling volumes volume of beads on the
fineness required. volume of the chamber w – x
Whatever the operating conditions, the size distribution ´ Porosity of the bulk of beads w – x
of the ground product is characterized by a multimodal rm Media density wkgrm3 x
pattern. The morphological analysis of the fragments pro- rs Particle density wkgrm3 x
duced during the comminution process suggests that the rsusp Suspension density wkgrm3 x
ground product is constituted by three types of fragments: msusp Viscosity of the suspension wPa sx
v1 Number of erosions to eliminate the particle sil-
large agglomerates, initially present, which disappear houette w – x
more or less quickly depending on the operating v2 Complement to v 1 with respect to the convex
conditions, hull w – x
intermediate sized fragments constituted by platelet- V1 Descriptor which characterizes the particle robust-
shaped crystallites and pieces of agglomerates, ness w – x
fine particles, which are very small debris. V2 Descriptor which characterizes the largest concav-
ity w – x
Considering that the fragments population is constituted
by three subpopulations, the multimodal size distributions
can be fitted using a linear combination of three monomodal
Acknowledgements
classical laws. The mathematical method used to treat the
experimental data and deduce the grinding kinetics has The morphological characterization has been performed
been applied to the dispersion of titanium dioxide w11x. at LSGC ŽLaboratoire des Sciences du Genie´ Chimique-
Future work will be focused on the application of this Nancy France.. Sincere gratitude is expressed to Dr. M.N.
procedure to the experimental data given in the present Pons and her research team for their contribution during
paper. this investigation.

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