Colloid Mills: Theory and Experiment
Alan G. King* and Santosh T. Keswani
In a colloid mill utilizing a rotating and a stationary plate, a
high shear field exists. Particles rotate, generating a lift
force moving them to the rotating plate. When particles col-
lide, a substantial energy transfer occurs because their sur-
face velocities are opposite. A mathematical model has been
developed relating the particle rotational speed to the
parameters of the colloid mill such as gap size, speed, slip
viscosity, and particle size distribution. A slurry of the
material being ground is forced into the gap. Grinding is
autogenous as a result of collisions between rotating parti-
cles. All of the material in the process stream is ground finer
than the gap setting and grinding can be optimized by
adjusting mill operating parameters. However, the mill is
not able to grind the incoming stream to submicrometer
sizes and there is molecular contamination from the surface
of the B,C cones.
I. Introduction
C olloid mills are widely used in industry to reduce the parti-
cle size of one phase suspended in a liquid vehicle. The
phase can be any state-gaseous, liquid, or solid. We are pro-
posing that comminution or emulsification occurs not directly
due to shear as proposed by Turner and McCarthy' but by
autogenous grinding empowered by the rotational kinetic
energy of particles in suspension. This paper proposes a theory,
discusses the governing equations of particles undergoing
shear, and shows how the rotational energy spectrum changes
with particle size, fluid viscosity, gap size, mill speed, and other
parameters in the system. Experimental data have been col-
lected to verify the theory.
This colloid mill was developed as part of a research program
on the processing of advanced ceramic powders. Part of the pro-
cessing involves the comminution of agglomerates which are
always present in any dry powdered raw material. In the process
of grinding, several requirements are necessary, especially for
powders used in advanced ceramics where powder properties
are critical. The grinding process has to grind all of the material.
Coarse agglomerates present in even a minuscule volume frac-
tion will severely degrade the strength and Weibull modulus of
the ceramic. For example, consider a bar 1 cm X 1 cm X 10 cm
composed of particles 1 pm in diameter. There are then lo4 X
lo4 X lo5 = lOI3 particles in the tensile bar. One coarse
agglomerate in the bar will severely reduce the tensile strength
by as much as 3- or 4-fold. There is also a requirement for mini-
mal contamination. Even if all of the powder is ground, the
grinding process itself can introduce contamination. There are
three kinds of contamination: mill ball chips, chemical impuri-
ties, and organic (polymer) particles. Ball or lining chips act
like coarse agglomerates. Also, if the mill adds significant wear
debris to the batch, there is usually a change in composition,
often leading to glassy phases on grain boundaries, and polymer
R.Scattergood-contributing editoi
Manuscript No. 195272. Received September 30,1992; approved March 30,1993.
*Member,American Ceramic Society.
769
Ferro Corporation, Cleveland, Ohio 4413 1
particles from the mill parts or mill lining bum out and leave
voids in the microstructure.
There is a need for a comminution process which addresses
these problems. We decided to develop a colloid mill where a
slurry flows between two plates (actually cones), one of which
is rotating with respect to the other.
Flat plate mills chatter at close gap settings so the two sur-
faces in this mill were designed to be conical in shape with a
120" included angle. The top male cone is the stator. It can be
moved axially to adjust the gap. The slurry is introduced
through a hole on the cone axis. The bottom cone is a matching
female part.
11. Colloid Mill Grinding Theory
We proposed that the major mechanism by which comminu-
tion occurs in a colloid mill is a consequence of particle rotation
and impingement in a shear field. Consider a spherical particle
in a shear field. Let us assume that the particle Reynolds num-
ber is small. In other words, viscous forces are large compared
with the inertia forces. Then the particle will have a motion sim-
ilar to a particle of fluid.
The particle will have three motions. It is translated along the
direction of flow, it rotates, and it is translated perpendicular to
the flow by a lift force which is a consequence of the particle
rotation as shown in Fig. 1. The shear stress generated by the
fluid shear will typically be less than 7 MPa, a value very low
compared to the stress required to fracture a hard material such
as alumina. However, as we calculate later, the fluid shear feeds
a large amount of rotational energy to the particles.
Figure 2 illustrates the interaction between two particles
rotating in the same direction. Even though the particles are
rotating in the same direction, when they contact each other,
their surfaces are moving in opposite directions. A large
amount of energy interchange can occur, causing grinding
action. Thus, rotational energy aids in the grinding process. In
contrast, when particles are translating and contact each other,
the amount of energy transferred depends on the relative veloci-
ties rather than the absolute velocities of the particles. If the
Reynolds numbers of the particles are small, then they will be
stator
5
1 L i f t For-ce
Fig. 1. Particle motion in a shear field.
710 Journal of the American Ceramic Society-King and Keswani
Stator
n particle and u is the kinematic viscosity). This equation is valid
8: \
Fluid Velocity
* Rotor
Fig. 2. Particles rotating in same direction wear each other.
translating at approximately the same velocities. Thus, there
will be a very small relative velocity difference between the
particles. Hence the amount of energy transferred will be small.
Thus, the translational energy of the particles will not contrib-
ute substantially to the grinding process.
The lift forces that are a consequence of the particle rotation
cause all particles to move toward the rotating cone. This
increases the concentration of particles near the rotating cone
and increases the probability of particle-to-particle interaction.
The particle distribution across the gap will be as shown sche-
matically in Fig. 3.
Having discussed qualitatively what we propose occurs in the
colloid mill, we next examine the equations that govern the
behavior of particles in the colloid mill.
( I ) Equations Governing the Rotational Energy of
Particles in the Colloid Mill
Let us consider a colloid mill being operated at an angular
velocity s and a gap setting h. Under steady-state conditions, the
shear stress will be constant across the gap at any radius.
Assuming that the fluid in the mill is Newtonian, the shear rate
will be constant across the gap. This shear rate at any radius, r,
is given by
G = (sr)/h
A particle in such a shear field rotates. The angular velocity of a
sphere in a shear field is given by’
R = (G/2)(1 - 0.0384ReG3”)
where R is the angular velocity, G is the shear rate (surface
speed of rotating anvil divided by gap), and Re, is the shear
n been calculated previously’ to be given by
Statop
p\ Fluid V e l o c i t y
i
i ““i L1‘t
c
ROlOf
Fig. 3. Particles concentrate near rotor because of lift forces.
Vol. 77, No. 3
Reynolds number (Re, = Gd’lu where d is the diameter of the
for particles whose Re, is less than 1. As the particle Reynolds
number increases, the particle rotates unsteadily until it hardly
rotates at all.’
The rotational kinetic energy of a particle is given by
RE = (Md2R2)/10 (3)
M is the mass of the particle, d is the diameter of the particle,
and R is the rotational speed of the particle. If the density of the
particle is @, then the rotational kinetic eneregy is given by
RE = (n@d5R2)/60 (4)
Thus, it can be seen that the rotational energy is proportional to
the diameter of a particle raised to the power 5 and the angular
velocity of a particle squared.
The angular velocity is directly proportional to the shear rate
G as shown in Eq. (2). For small particles with low Re,, the
angular velocity approaches half the shear rate. As the particle
Re, increases, the angular velocity becomes progressively
smaller than half the shear rate. However, if the Re, becomes
larger than 6, then particle rotation is unsteady.’ At larger Re,,
the viscous forces will be much smaller than inertia forces and
the particle will rotate very slowly, if at all.’
The key to attaining efficient grinding in the colloid mill is to
ensure that the Re, of the particles is small. There are three
ways to ensure that Re, = Gd2/u is kept small. One way to
ensure that Re, is small is to keep the shear rate, G, small. How-
ever, then the rotational energy fed into particles is small.
Another way to limit Re, is to limit the size of the particles.
Again, since the rotational energy of the particles is propor-
tional to the diameter raised to the power 5 , this method reduces
the energy that can be fed to the particles. Moreover, this limits
the usefulness of the colloid mill if it can only be used for very
fine particles. The best way to keep Re, small is to increase the
kinematic viscosity of the liquid in which the particles are sus-
pended. However, if the kinematic viscosity is increased sub-
stantially, then the throughput of the mill is reduced. So
optimizing the operating conditions of the mill requires
adjusting the gap size or the angular velocity of the mill and
adjusting the kinematic viscosity to obtain reasonable
(1) throughput.
The most efficient way to operate the mill is to ensure that
Re, for almost all incoming particles is less than 1 but not much
less than 0.1. Under these conditions, all particles are rotating at
(2) speeds close to half the shear rate and will therefore participate
in the autogenous grinding process.
A key feature of our autogenous grinding theory is the migra-
tion of particles to the rotating cone, increasing the local solids
loading, and increasing the changes of particle-to-particle inter-
actions. The lift force on a rotating sphere in a shear field has
F , = 1.615l~,dU,JRe~ (5)
where p is the dynamic viscosity, U, is the flow velocity in the
tangential direction, and d is the diameter of the particle. Equat-
ing this lift force with the drag force on a spherical particle pre-
dicted by Stokes’ law, one can calculate the terminal velocity in
the transverse direction, U,:
U, = 1.615UR,/Re,/(3.rr) (6)
We can see that the terminal velocity in the transverse direction
is of the same order as U , since Re, is of order 1. The distance
that a particle traverses in the tangential direction is of the order
of 1 m while the gap setting is only a few micrometers. Hence,
particles will migrate to the rotating cone very quickly after
entering the colloid mill and begin to have particle-to-particle
interactions resulting in autogenous grinding.
March 1994 Colloid Mills: Theory and Experiment
Having presented the equations of spherical particles in a
shear field, we can start examining the numerical results that we
obtain under typical colloid mill operating conditions.
(2) Discussion of Calculations
Colloid mills can run at very high speeds and at very small
gap settings. We can select a relatively low speed, say, 104.7
rad/s (1000 rpm). A typical gap setting may be 20 pm. At
a radius of 0.05 m, the shear rate, G, will be 2.6 X lo5 s-'.
Particles whose Re, is small will rotate at speeds of up to
1.4 X lo5rad/s.
When these rapidly rotating particles contact each other, this
energy is available for fracturing the particles. As the particles
touch each other and slow down, the fluid shear is able to feed
energy back to the particles, causing them to start rotating
again. A particle has sufficient residence time in the colloid mill
to rotate on the order of 10000 times. Assuming a collison or
interaction every rotation, a particle will have a large number of
collisions during its residence in the mill.
Since the rotational energy is proportional to the diameter
raised to the power 5 , the larger particles have considerably
more energy than the smaller particles. The key to the efficient
operating of the mill is to ensure that viscous forces are suffi-
cient to make the largest particles rotate at high speeds. This can
be achieved by having a high fluid viscosity and limiting the
shear.
In order to examine this behavior of the colloid mill, we have
calculated the rotational energies of spherical particles in the
shear field under a wide range of operating conditions. The
baseline conditions used in the calculations assume a radius of
0.04 m, a gap of 16 pm, and a fluid viscosity of 5 cP. Since the
rotational energies of micrometer-sized particles are small
140 r 5 r
0.02 rn
26
10
2
5 10 15 20 25 3 0 35 40
Fig. 4. Effect of cone radius on the particle rotation energy at differ-
ent cone angular velocities.
77 1
numbers, we have nondimensionalized the energies by dividing
by a constant (lo-'')).
Figure 4 shows the nondimensional rotational energy of
spherical particles in a colloid mill as a function of mill angular
velocity and radius of the mill. Let us examine the energies at a
radius of 0.02 m. We can see that as the angular velocity of the
mill increases, only smaller and smaller particles are able to
absorb energy from the fluid. Thus, at 42 rad/s, particles as large
as 30 pm have considerable rotational energy. Above 63 rad/s,
these larger particles have very little rotational energy. As the
shear increases, the Re, increases, and the viscous forces are
not able to keep up with the inertia forces and larger particles
tend to rotate at slower and slower speeds. On the other hand,
10-pm particles always rotate at high speed at a radius of 0.02
m and their energy increases as the angular velocity of the mill
increases.
The rotational energy spectrum is similar at radii of 0.04 and
0.06 m though the maximum value of the energy of the particles
is considerably lower as the radius increases, as the ordinate on
the graph shows. The largest particle which has rotational
energy decreases as the radius increases. This is because the
shear rate is increasing as the radius increases, and Re,
increases too. Figure 4 tells us that if 25-pm particles were to be
ground, then angular velocity should be around 42 radls and the
radius should be less than 0.04 to 0.05 m. On the other hand, if
10-Fm particles are to be ground, then one can operate the mill
at an angular velocity of 105 or even 157 rad/s.
Figure 5 shows the nondimensional rotational energies as a
function of angular velocity and gap setting. As the gap is
increased, larger and larger particles are able to rotate and the
amount of energy that the particles possess is higher. At any gap
setting, the largest size of particles that can absorb energy
decreases as the angular velocity increases.
":
* 24
P
e
-m
W
.-
0
I
4
8
m
I
a
5 10 15 20 25 30 35 40
160 r
32 prn
IA
50 60
Fig. 5. Effect of the gap on particle rotational energy at different cone
angular velocities.
712 Journal of the American Ceramic Society-King and Keswani
Figure 6 shows the effect of viscosity and angular velocity on
the nondimensional rotational energy. The striking feature in
these graphs is the 5-order increase in rotational energy as the
viscosity is increased. At low fluid viscosities, only very small
particles have significant rotational energies even at low angu-
lar velocities. As the fluid viscosity increases, larger and larger
particles have significant rotational energy. Thus, the largest
particle with significant rotational energy increases from 8 to 90
pm as viscosity increases from 0.1 N.s.m-’ (1 cP) to 10
N.s.m-2 (100 cP).
So far, we have looked only at the nondimensional rotational
energy of a single particle. The mass of a 1-pm particle is only
1/1000 that of a 10-pm particle. Typically, in any particle size
distribution, there are many small particles for every large parti-
cle. Hence, it is relevant to look at the rotational energy of the
entire particle size distribution.
Figure 7 shows the rotational energy spectrum of a typical
particle size distribution as a function of angular velocity. It can
be seen that as the angular velocity increases, the amount of
energy fed into smaller particles increases. The total amount of
energy fed into the system, which is the area under the curve,
can decrease or increase with angular velocity depending on the
conditions in the mill and the particle size distribution. At 63
rad/s, particles as large as 20 pm are absorbing significant
energy from the fluid. At 10.5 rad/s, only particles smaller than
18 pm are absorbing rotational energy from the shear field. At
209 rad/s, only particles less than 13 pm are absorbing energy.
Thus, there are two opposite effects at work here. Increasing the
angular velocity increases the shear rate and increases the
amount of energy that can be fed into the particles. However,
larger particles are no longer rotating. Thus, the amount of
42 radls
-105 radls
.209 radls
L,\,,,,A
8 Operating conditions were controlled and monitored by sen-
4 5 cps
, ,
5 10 15 20 25 30 35 40
8000 1 A
6000
4000
2000
60 a0 loo 120
-~ 40
20
Diameter, pm
Fig. 6. Effect of fluid viscosity on particle rotational energy at differ-
ent cone angular velocities.
Vol. 77, No. 3
B 32 c
I
40
Diameter ,jm
Fig. 7. Particle rotational energy spectrum for a certain size distribu-
tion of three cone velocities.
energy that is fed into the particles goes through a maximum as
the mill rotational speed is increased.
We postulate that the amount of grinding that is accom-
plished in the colloid mill is proportional to the amount of total
rotational energy that is fed into the particles. However, we
know that very small particles are not as easy to grind down
because they are less likely to contain structural flaws. If we
assume that the probability of the presence of structural flaws is
proportional to the volume of material, then a 1-p,m particle is
only 1/1000 as likely to have a flaw as a 10-pm particle. There-
fore, we can anticipate that the rotational energy of the small
particles is not likely to make as large a contribution to grinding
as the rotational energy of larger particles. Also, the maximum
flaw size in a particle is limited by its size.
Another factor that is very important in our model of the
autogenous grinding process is that both particles that interact
should be rotating. Thus, if the shear rate is such that only
smaller particles are rotating, then it is unlikely that the nonro-
tating larger particles will be ground down. If both particles are
rotating, then the grinding interaction will be very effective. So
we propose that the ideal grinding conditions are attained when
the conditions of shear are such that almost all of the particles in
the incoming slip are rotating.
The experiments relating to the model were conducted using
an aqueous suspension of a Bayer Process alumina (Alcoa’s
A-16 alumina). The alumina was preground to a d , of 27 pm
and a d,, of 7.5 pm. Coarser material was difficult to feed
through the mill without particle segregation which compro-
mised the data. The suspension contained 25 wt% alumina,
which is equivalent to 7.7 vol% solids.
sors. Figure 8 shows typical data collected by the system. The
gap was gradually reduced to 16 pm and adjusted to maintain a
flow rate of 0.76 cm3/s. The temperature of the mill increases
with time, closing the gap. Since the flow rate of the mill is pre-
dicted to be proportional to the gap raised to the power 3 , the
flow rate is a sensitive measure of the gap opening.
Figure 9 shows the particle size of the processed slip as the
speed is increased. There is a sharp drop in the d,, and d,, val-
ues at 105 rad/s. This scan was replicated twice to confirm the
relationship. Our model can explain the minimum in Fig. 9 as
follows.
Figure 10 shows the rotational kinetic energy of the slip as a
function of mill rotational speed. Also shown in the figure is the
particle size distribution. As the speed increases, more energy is
fed into the smaller particles, but larger particles are no longer
rotating. Figure 11 shows the total rotational energy for parti-
cles larger than 7.5 pm. It can be seen that this energy goes
through a maximum at around 105 rad/s. Thus, we feel that the
March 1994 Colloid Mills: Theory and Experiment

10

240

200

a 160
P
c
-
W
ID
120
.-s
dd

$ 80
re.

40

I I I I J
100 200 300 400 500 600 700
Time, 8 10 20 30 40 50
Diameter pm

Fig. 8. Typical mill operating parameters for a particular experiment. Fig. 10. Rotational kinetic energy of the slip at four cone velocities
for a particle size distribution.

I I I I I I I I

30 r 40 60 80 100 120
Speed ,rad/s
140 160

Fig. 11. Total rotational energy with cone speed for particles larger
than 7.5 p,m.

(1) Mill Design

I I I
100 200 300
Speed, rad/s
Fig. 9. Particle size parameters with cone velocity.
autogenous grinding in the colloid mill occurs because of the
interaction of rotating particles. By controlling the conditions in
the mill, it is possible to enhance the level of grinding very
substantially.
111. Design and Operation of the Colloid Mill
The colloid mill incorporates design elements which make
the alignment and control of the mill substantially more precise
than existing mills of a similar type. This provided precise con-
trol of the mill when processing ceramic particulates. This sec-
tion describes the design and the results of milling experiments.
Descriptions of disk attrition mills are given in the Chemical
Engineer’s H a n d b ~ o kSometimes
.~ called colloid or dispersion
mills, these devices include the Kady, Morehouse, and Premier
mills. They are reported not to do much actual grinding but
instead are used for breaking up agglomerates, dispersion of
particles, and emulsification.
The mill has a vertical axis and two matching B,C cones
which comprise the surfaces between which grinding occurs. It
is convenient to start from the male cone apex and describe the
mill upward through the constituent parts, then, starting again
from the female rotating cone, describe the mill moving down-
ward through the rotating parts.
When designing a high-speed rotating apparatus which will
sustain substantial axial and tangential loads, it is a very good
idea to work closely with your suppliers and to stay within their
specifications. This mill could have exposed the staff to sub-
stantial safety hazards if the design limits had not been taken
seriously and rigorously complied with.
Figure 12 is a schematic drawing of the working parts of the
mill. The assembly is mounted on an “H” beam support which
has a I-in.-thick stainless plate bolted to its front flange. The top
half of the assembly provides the vertical motion which adjusts
the gap between the cones. It also provides the alignment mech-
anism so that the two cones can be adjusted to be coaxial. The
lower assembly consists of the rotating cone, the spindle, and
motor drive.
( A ) Alignment Mechanism: The upper (male) cone is
shrunk fit into a stainless steel part to hold it firmly in place.
This part has a spherical upper surface which mates with
another spherical surface on the next part up the column. The
774 Journal of the American Ceramic Society-King and Keswani
n safety margin was achieved on fracture, and that enough of the
I an opening in the carrier block and proceeds through an axial
II I Carrler Block
Lateral
Allgnment ism
Angular
Allgnment
Slip Splas
Pan Lowar Cone
Fig. 12. Colloidal mill design, schematic.
center of the sphere is coincident with the projected apex of the
cone. The upper cone axis can thereby be adjusted in angle to
make the two cone axes parallel. The other end of the part con-
taining the female spherical surface has a flange for bolting it in
the carrier block. Both ends of the part contain oversize holes so
that the bolts holding the assembly together allow the cone to
float laterally into alignment after which the bolts are tightened.
The two cone axes are now coaxial. The remaining alignment
task is to assure that the two cone angles are exactly the same.
To accomplish this a slurry of fine diamond abrasive is ground
in the mill. The wear pattern on the stationary cone is used to
evaluate the precision of the alignment and determine when the
cone angles are identical.
( B ) Gap Setting Mechanism: The upper part of the
assembly rides on a ball slide and is moved vertically by a ball
screw. The axial load is taken by a thrust bearing. A stepping
motor connected to a gearbox provides rotary motion to the ball
screw. Tests have shown that the gap can be reproducibly con-
trolled to kO.25 pm.
(C) Lower Cone Assembly: Since the lower cone assem-
bly is designed to rotate at high speeds, careful attention was
given to the metallurgy, fit precision, and dynamic balance. The
rotor alloy was 17-4 pH stainless steel heat-treated to give a
0.2% maximum yield at 965 MPa (140000 psi) and an elonga-
tion of 14% to 16%. An analysis of both the stresses and elastic
deformation of the rotor were made to assure that an acceptable
Vol. 77, No. 3
interference fit was retained to hold the lower cone in place dur-
ing rotation. The cone assembly was dynamically balanced on
the rotating spindle after assembly.
( D ) Spindle: The spindle was a grinding wheel spindle
with high-contact-angle ball hearings. The high-angle special
bearings were needed to withstand the axial load. The bearings
were also equipped with strain gauges to measure both the axial
and tangential loads. Lubrication of the bearings was by an oil
mist system in order to lower the bearing operating temperature.
An analysis was made on the rotor-spindle assembly to
assure that it would not have a resonant frequency anywhere
over the speed range used.
( E ) Slip Delivery System: The ceramic powder being pro-
cessed is dispersed as a slurry in water. This slurry was pumped
either with a variable stroke diaphragm pump or from a stirred
pressure vessel, The slip delivery tube enters the mill through
hole in the upper cone into the gap. The upper cone has a com-
pounded angle in order to provide an initial wider gap so that
large (100 pm) particles can enter into the mill. Most of the
experimental work was on alumina (Alcoa’s A-16 alumina)
which has a d,, of 70 pm and a d , , of about 11 pm. Handling
this material in a slurry proved to be difficult as it settles out
readily. Since the mill at useful gap settings has a low flow rate,
settling and particle separation in the delivery system were trou-
blesome. The flow rate would surge, the tubing would plug up,
the pump values would plug up, and coarse particles would sep-
arate from the fines either by sedimentation or by filtering
through a pack of accumulated coarse material. This resulted in
several premature exultations of success as we mistakenly
believed that a phenomenal amount of grinding was occurring
when in actuality the mill delivery system was acting as a clas-
sifier. These problems were solved by reducing the diameter of
the feed tubing so that the slip velocity was high enough to
sweep along the coarse particles. We also added 30% partially
preground material to assist in suspension properties. This addi-
tion simulated the particle size distribution which would occur
in a feed stock from a grinding-classification circuit, and from
that rationale some legitimacy was attached. There was concern
that if the slurry feed was interrupted, overheating could occur
and the cones could fracture from thermal shock. This in fact
did happen. To prevent this from occurring again, an accumula-
tor was added to the feed. When flow ceased, a solenoid valve
opened and the pressurized water in the accumulator was forced
into the mill. This allowed time for either opening the gap or
shutting down the mill by hitting an emergency stop button.
( F ) Controls: The operating controls were set and
adjusted with a computer interface. These controls included
control of the gap with shaft encoders, and the pump displace-
ment. Speed was measured and controlled with a tachometer.
The motor speed was set manually. Safety shut-offs included
the accumulator solenoid, horse power upper limit, oil mist
malfunction, bearing temperatures, and maximum axial load.
(2) Experimental Results
The experimental results shown earlier which support the
theory were for a feed with a narrow particle size distribution.
In practice, the distribution will be broad. The following results
were obtained with a broad distribution.
(A) Grinding A-16 Alumina: A-16 alumina (Alcoa) was
used in much of the experimentation. Figure 13 shows the parti-
cle size distribution of A-16 unground (A-16 UG) and the dis-
tributions after one and two passes through the mill. The first
pass was at 104.7 rads/s (1000 rpm) with a 100-pm gap. A large
reduction in particle size is achieved in the first pass through the
mill as can be seen in the figure. There is an order of magnitude
reduction in the d,, size and a 20-fold reduction in the d,, size.
These data by themselves eliminate any credibility of grinding
occurring by crushing between the two cones as the gap size is
much larger than the ground material.
March 1994 Colloid Mills:Theory and Experiment
Fig. 13. Particle size reduction of A-16.
A-16 alumina has a sandlike consistency. The large agglomer-
ates are not “soft” in that they cannot be dispersed chemically
with stirring or ultrasonically. The ultimate crystallite size is 0.6
ym. The first pass through the mill breaks up the coarse
agglomerates into finer particles which are more difficult to mill
down. Typically in a ball mill 24 h is necessary to achieve a d,
of about 0.6 km. Our experience in a 1-S attritor mill (Union
Process) is that 4 h was required to achieve this particle size.
We concluded that the colloid mill is not effective in grinding
small, hard particles, especially using a low-viscosity liquid.
From the grinding theory described earlier, a great deal more
energy can be imparted to the particles in higher-viscosity liq-
uids. We tried this using an oil at 60 CPas the vehicle. While a
qualitative conclusion was drawn that grinding was more effec-
tive, we were not able to redisperse the material in order to
obtain a particle size distribution. In other systems, such as
paints, cosmetics, pharmaceuticals, tape casting slurries, or
thick film inks where the vehicle does have a higher viscosity,
our conclusion may be excessively restrictive.
Mill speed, gap setting, solids loading, feed rate, and pH
were varied. The results are shown in Fig. 14. Speed ranged
from 3 1 to 209 rads/s (300 to 2000 rpm). The gap setting ranged
from 70 to 100 km, the solids loading varied from 10 to 20
vol%, the feed rate from 0.0015 to 0.0075 L/s, and pH from 7 to
3. All of the particle size distributions over the range of condi-
tions fell within a narrow band shown in Fig. 14, indicating that
the process is insensitive to these variables over the range used.
We concluded that mechanical forces dominate the process.
( B ) Grinding Glass: An alkaline-earth borosilicate glass
was precrushed to 150 mesh (106 ym). It was then mixed into a
slurry with deionized water at 10% by weight solids loading.
100 -
80 -
C
c
60-
ii
aR
40 - f
20 -
0.1 i 10
Particle Size, pm
Fig. 14. Effect of changing mill parameters.
Particle Size, p m
The mill operating parameters are shown in Fig. 15. The speed
was held at 104.7 rad/s and the gap reduced sequentially from
40 to 12 ym. Figure 16 shows the particle size distribution at
five gap settings. As the gap was reduced, finer grinding
occurred. We had difficulty reproducing these results. How-
ever, the particle size reduction was confirmed microscopically
and the results are valid. The mill gap acts as a gate. Particles
larger than the gap are retained until they are ground further.
Unlike A-16, these particles are not agglomerates but solid
glass. Glass is easy to break into large pieces because of flaws
on the surface. It is difficult to grind because the scale is
reduced to where these flaws are no longer effective.
Shear stresses in the liquid by themselves would not contrib-
ute to comminution for two reasons. First, they are not high
enough and even if they were they would not be effective
because the particles will rotate.
(3) Operating Characteristics
We encountered a number of difficulties in the experimenta-
tion. These are worthy of some discussion in order to alert oth-
ers that these problems exist.
(A) Feeding Coarse Materials: A-16 UG is difficult to
handle because of its large particle size. It does help to suspend
the material by adding superground A-16 in a ratio 3:l UG/SG.
This poses its own hazards as the delivery system can readily
segregate the two fractions. The coarse material also tended to
form plugs in the delivery system, which resulted in surging,
feed oscillations, and filtering. Filtering by coarse plugs or seg-
regation in the delivery system results in erroneous particle size
data which can be misleading.
( B ) Wear: Hot-pressed B,C was chosen for the mill faces
because of its very high hardness, wear resistance, and
availability.
-
i: I
10
E 6
100
200 300 400 500 600 700
Time, s
Fig. 15. Mill operating parameters.
716 Journal of the American Ceramic Society-King and Keswani
Particle Size, )Im
Fig. 16. Particle size of a glass as the gap is changed.
Figure 17 shows the surface of the stationary cone after use.
A replica technique was used for the SEM photo. The replica
technique results in the grooves and ridges becoming inverted.
The grooves are about 12 p n wide. In the case of ceramic cut-
ting tools: the groove width correlated with the grain size of the
alumina tool. The mechanism which was proposed was that
when a grain is removed from the tool surface, the hole which
remains preferentially elongates along the direction of sliding.
The leading and trailing edges of the cavity are locations of
increased stresses and the hole evolves into a groove.
The photograph shows two types of wear. First, the surface is
striated and highly polished. Second, there are locations on the
surface where fracture and pullouts have occurred. The boron
concentration in the slip was substantially increased, also
reflecting appreciable cone wear.
Because of both the high hardness and the appearance of the
wear surface we believe that the wear mechanism is principally
chemical in nature and probably an oxidation reaction with
B,C. In a similar prototype mill of the same type, we observed
similar high wear on hot-pressed a-silicon carbide cones. Pref-
erentially, cones must be made from the same composition as
the material being ground if practical.
(C) Machine Compliance: The mill was designed for a
high operating speed as we believed at first that angular velocity
had beneficial effects on both comminution and productivity.
Because of this, a grinding machine spindle was chosen. We did
specify high contact angle ball bearings in order to sustain the
Fig. 17. Wear surface of the stationary cone.
Vol. 77, No. 3
high axial load. It turned out that the machine compliance was
not appropriate, and it was not possible to work at even moder-
ate slip pressures without forcing the gap open. In one experi-
ment the gap was progressively closed to -60 pm (60-pm
interference fit) without closing the gap. Later we came to better
understand the fluid mechanics of the mill. The high speeds are
not needed but extreme rigidity is. A better bearing choice
would be fairly large tapered roller and thrust bearings. The
mill’s supporting structure cantilevered the axis to where bend-
ing stresses were imparted to the structure. These stresses cause
the mill to bend like a bow. A more appropriate design is to
make the mill and structural axes coincidental so that the
stresses are compressive and tensile. With these changes, the
mill can operate at higher slip pressures and better gap size
control.
IV. Summary
Particles rotate in a shear field and are propelled toward the
moving surface, causing them to concentrate there. Even
though the particles are rotating in the same direction, when
they contact, their surfaces are moving in opposite directions.
This leads to a large exchange of energy which can cause parti-
cles to abrade and fracture.
The carrier liquid plays an important role in transmitting
shear forces to the particles. The shear Reynolds number gives
an indication of whether viscous forces will be adequate to
cause the particles to spin. Smaller particles spin at half the fluid
shear rate. Larger particles experience a slip and spin at pro-
gressively lower speeds. Thus, there is an optimum incoming
particle size distribution to achieve the most efficient grinding.
Apart from the size of incoming particles, the speed of the
colloid mill is an important independent variable. Larger parti-
cles can rotate at speeds close to half the shear rate at low mill
speeds but at higher mill speeds the fluid viscosity is not suffi-
cient to overcome the particle inertia forces.
The most important variable in the colloid mill is the viscos-
ity of the carrier liquid. Increasing the liquid viscosity from 1 to
100 CPincreased the maximum rotational energy by 5 orders of
magnitude. Thus, increasing the viscosity is an effective way to
grind larger particles in the mill. However, throughput of the
mill may be reduced substantially if the viscosity is increased
too sharply.
It is possible to select operating conditions of the colloid mill
or the viscosity of the fluid carrier to maximize grinding effi-
ciency. We think that it is reasonable to predict that the grinding
mechanism in other types of mills occurs by a similar process.
These include comminution devices in which particles are
March 1994 Colloid Mills: Theory and Experiment
entrained in a strong shear field. Included in these devices are
three roll mills, some types of mullers, plate mills, and homoge-
nizers. The theory is not limited to solid particles in a liquid but
with appropriate modifications for compressibility and surface
tension can also include liquid particles in an immiscible fluid
(homogenizers) and liquid particles in a gaseous fluid (two
fluid atomizers).
Glass was ground effectively and showed a significant effect
on grinding as the gap size was reduced. These gap sizes were
smaller than these used for A-16 UG. The gap acts as a gate
where particles larger than the gap cannot exit from the mill.
Previous hypotheses on the colloid mill grinding mecha-
nisms regard “shear” as the source of comminution. This
hypothesis fails to recognize that particles are not going to stand
still and just let the shear forces (which are small) tear them
apart, but they must rotate in the shear field as a consequence of
these forces. The particles are concentrated by lift forces and
autogenously grind each other up.
The mill design as described included some successful and
less successful features:
(A) Successful
(1) The gap adjustment mechanism.
( 2 ) Alignment mechanism and procedures.
(3) Cone design and ceramic cone retaining
structures.
(4) Instrumentation and controls.
(B) Less successful
(1) The cone material.
(2) Compliance of the structure.
(3) Overdesigned for speed capabilities.
777
The colloid mill described here was effective in breaking up
the coarse agglomerates of A-16 but was not so effective in fur-
ther reducing the particles to their ultimate crystallite size. The
principal reason for this is that the kinetic energy in the system
is not efficiently transferred to the fine particles which have a
high Reynolds number. The mill could be more effective if a
higher-viscosity liquid was used in the slurry. Some of our
experimental results suggested that this is a valid conclusion,
but it is not quantified in this paper.
Changes in the gap setting, speed, feed rate, pH, and solids
loading had relatively little effect on the particle size distribu-
tion of A-16 UG.
Acknowledgments: We would like to acknowledge the direct assistance
of L. W. Bergdorf and R. JSrol and the support and guidance of J. H. Heasley
and R. V. Hanington. Gary Braun provided initial support. Clyde M. Coffman
constructed an early version of the mill. Bob Simon did the detail design and
construction of the mill used in the study. Numerous suppliers were very helpful
in offering advice and assistance in the study.
References
‘H. E. Turner and H. E. McCarthy, “A Fundamental Analysis of Sluny Grind-
ing,”AIChEJ., 12 [4]784-89 (1966).
2R. Clift, J. R. Grace, and M. E. Weber, Bubbles, Drops and Particles;
pp. 25941. Academic Press, New York, 1978.
’R. H. Perry and C. H. Chilton, Chemical Engineer’s Handbook, 5th ed.;
pp. 8-41-8-43. McGraw-Hill, New York, 1973.
“A. G. King and W. M. Wheildon, Ceramics in Machining Processes;
pp. 1 4 W 3 . Academic Press, New York, 1966. 0