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Process Engineering With Planetary Ball Mills: Chemical Society Reviews February 2013
Process Engineering With Planetary Ball Mills: Chemical Society Reviews February 2013
Process Engineering With Planetary Ball Mills: Chemical Society Reviews February 2013
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Planetary ball mills are well known and used for particle size reduction on laboratory and pilot scales
for decades while during the last few years the application of planetary ball mills has extended to
mechanochemical approaches. Processes inside planetary ball mills are complex and strongly depend on
the processed material and synthesis and, thus, the optimum milling conditions have to be assessed for
each individual system. The present review focuses on the insight into several parameters like properties
of grinding balls, the filling ratio or revolution speed. It gives examples of the aspects of grinding and
illustrates some general guidelines to follow for modelling processes in planetary ball mills in terms of
refinement, synthesis’ yield and contamination from wear. The amount of energy transferred from the
milling tools to the powder is significant and hardly measurable for processes in planetary ball mills.
Received 7th November 2012 Thus numerical simulations based on a discrete-element-method are used to describe the energy
DOI: 10.1039/c3cs35455e transfer to give an adequate description of the process by correlation with experiments. The simulations
illustrate the effect of the geometry of planetary ball mills on the energy entry. In addition the imaging
www.rsc.org/csr of motion patterns inside a planetary ball mill from simulations and video recordings is shown.
Introduction
Grinding is one of the most important unit operations due to
the need for size reduction in chemical, pharmaceutical and
Technische Universität Braunschweig, Institute for Particle Technology, Volkmaroder
food industries. Planetary ball mills are suitable for wet and
Straße 5, 38104 Braunschweig, Germany. E-mail: c.burmeister@tu-braunschweig.de,
a.kwade@tu-braunschweig.de; Fax: +49 531391 9633; Tel: +49 531391 9643 dry, fine and ultra-fine grinding of particles down to the
† In dedication to the memory of Stefan Rosenkranz. nanometre size range due to the high stress intensities reached
This journal is c The Royal Society of Chemistry 2013 Chem. Soc. Rev.
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Chem. Soc. Rev. This journal is c The Royal Society of Chemistry 2013
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Filling ratio of grinding material or ball to powder ratio unwanted side reactions such as aldol reaction between ketones
These process parameters are apparently not completely and aldehydes15,30 or lead to the decomposition of supersaturated
independent of each other and play an important role in the solid solutions or metastable phases as it was found from
refinement of particles and in the kinetics when optimized for mechanochemical alloying of Al–Cu–Fe systems31,32 due to a
the best yield.6 On a local scale process parameter variation significant temperature increase.6 A high temperature increase
leads to changes in the nature of impacts, the stress frequency may be helpful when diffusion is required in powder alloying or
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and the stress energy as well as the amount of powder trapped the reaction is promoted by high temperatures.6 On the other
between colliding bodies.3 hand a lower revolution speed leads to less energy consumption
One of the most important parameters for synthesis and and hence to lower cost and a more energy efficient process.24
refinement is the specific energy that is transferred to the The selection of the material of milling balls is determined
powder. Processing at a laboratory scale enables a relatively by the reaction itself in a way that it will not induce side
tight control but for practical manufacturing methods large reactions or cause high abrasion and memory effects with
scale processes and due to the limitations of planetary mills reconstitution of the original structure (9).33 Mostly the used
other processing setups or milling devices are needed. The milling balls are made of tungsten carbide, steel, zirconia,
specific energy is used to adjust the required milling parameters corundum or agate.6,8,22,30,34,35 Balls with large diameter or
for a certain material or synthesis under different operating high density can provide higher impact energy during the
conditions. Also for comparison of different devices or set-ups collision event and, therefore, are applicable for reactions
the specific energy has to be considered.25,26 where the effect of particle refinement will lead to higher
The specific energy Ei can be obtained by relating the total surface activity. Higher surface activity benefits for instance
energy to the total mass of the powder as it is shown in the in catalytic reactions or in the formation of thermodynamically
following:27 stable products.6,15 Higher densities do not automatically lead
Pn to a higher energy transfer into the powder charge and thereby
j¼1 SEj DSFj SN SE
Ei ¼ t¼ (2) a higher yield. High stress intensities also can have a damaging
mP mP
effect on the product as the result of the energy dissipation in
The total amount of energy is determined by the frequency of heat.6,15
stress events DSFj at interval j, the average stress energy SEj at In some cases more ‘‘soft milling conditions’’ with low
interval j and the processing time t, which is equal to the ball-to-powder ratios and small ball sizes which intense the
product of the total number of stress events SN and the average frictional action are helpful to support amorphization and
stress energy SE. The stress energy SE describes the maximum metastable phase formation in alloying.6 Small balls are also
amount of energy which can be supplied to the product useful if no high intensity but more an efficient mixing and/or a
particles at one collision event and can be calculated from high number of collisions is required. In organic synthesis the
the relative impact velocity vj and the masses of the colliding diameter of the milling balls is crucial, if the overall mass is not
bodies m1 and m2 as given by eqn (3).20,27 The frequency and constant for example for Suzuki–Miyaura reaction where the
energy are on their part affected by the milling parameters yield significantly drops when the ball diameter is changed
mentioned above. from 15 mm to 10 mm at a constant ball number.22 However, if
a constant mass of milling balls and, thus, a constant filling
vj 2 m1 m2
SE ¼ (3) ratio is adjusted the product yield is unchanged independent
2ðm1 þ m2 Þ
from the ball diameter. This independency is in contrast to
The energy is supplied to the particles due to collisions of the particle refinement processes where the ball diameter influences
balls which are caused by the movement of the disk and pots. the product particle size.24 The number of balls depends on the
Thus the revolution speed is connected with the energy entry volume of the grinding chamber and is limited by the filling
and it influences yield as well as selectivity and can change the ratio r. It is known that for dry grinding a ball filling ratio of r =
formation of the powder as a result of temperature effects. It is 0.3 results in the most effective feed grinding.20 Depending on
well understood in the case of particle refinement and inorganic the size of the milling balls a certain amount of balls is
processing but deeper understanding is needed for mechano- necessary to guarantee a qualitative yield.24 A higher number
chemical approaches which are more complex and often differ of balls at constant density and diameter influence the reaction
from each other.15,24 due to the change in stress number. The correlation between
In most cases a minimum revolution speed is required to yield and number of balls seems to be almost linear for
reach a desired product yield or product quality. An increase in chemical synthesis.15,22 The use of too many balls will result
revolution speed often leads to higher yields or better substrate in only a low yield due to the restricted movement of balls
conversion at constant milling times as a result of the more inside the loaded pot.22 Otherwise in a charge with too few balls
efficient mixing and the increasing number of collisions.2,22,28 strong abrasion can take place and may not be in line with the
For some reactions the speed has no influence above a particular recommendation of the mill manufacturer.24 A mixture of balls
number of revolutions or no influence at all.24,29 The speed is with different size may randomize the motion of the ball charge
apparently limited by the design of the mill and also by in a way that without well-defined trajectories tracks in the pot
unwanted effects on the product. High speeds may induce are avoided.36–39
This journal is c The Royal Society of Chemistry 2013 Chem. Soc. Rev.
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The yield increases with milling time22,30,40 due to the The rapid increase may be explained from the dislodged
consistent increase in the number of ball collisions and the material acting as an additional abrasive component and from
total amount of transferred energy. However, decomposition of frictional heat which may change the material properties to a
the product can be observed with prolonged reaction time for more brittle material or the abrasion changes from the lower
some reactions.22 shelf to the upper shelf.49
The wear rate constant Kc can reach a minimum for a certain
Wear in planetary ball mills
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Chem. Soc. Rev. This journal is c The Royal Society of Chemistry 2013
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This journal is c The Royal Society of Chemistry 2013 Chem. Soc. Rev.
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It is calculated as the total sum of impact energy of collision expressed by a linear function.16,64,66 Therefore the specific
events n as given by eqn (5) and it is equivalent to eqn (2) for a energy can be used for prediction and estimation of the
constant grinding ball mass m.14,16,21,40 grinding rate and optimization of conditions.
Xn The particle size change during the experimental grinding
1
Ei ¼ mvj 2 (5) process can be described using an empirical equation:16
j¼1
4m P
Dt Dl Dl
¼ 1 expðKP tÞ þ
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(9)
However, the comparison between experimental results and D0 D0 D0
simulation data is challenging due to changes in composition,
with Dt/D0 as the normalized particle size and the grinding rate
particle size, morphology, structure and crystallinity.
KP. The correlation with experiments shows that the rate of size
The specific energy increases with increasing revolution
reduction KP increases with decreasing ball diameter at high
speed nR and increases linearly with the number of balls and,
rotational speeds while it is independent of ball size for low
thus, the number of collisions. Higher energy and/or the
speeds.66 KP increases with increasing revolution speed and
collision number will lead to a better mechanochemical activation
decreases with sample weight.16
and mechanical alloying which can also be seen from experimental
data. It can be seen that the rotation of the disk and pots in a Simulation of geometry scale-up
counterdirection (cf. Fig. 1) is more effective in grinding and
A geometrical scale up of fscale times of the mill size (pot
mechanochemical activation than the normal direction as
diameter dP, pot height h and revolution radius R) shall
a result of higher energy and higher number of collisions.
investigate the effect on the energy Ei. The computational
These computational results are in very good agreement with
predicted effect based on the dependencies in eqn (6) and (8)
experimental results.14,17
on the energy should be:
The mill geometry has a significant effect on the number of
balls and the speed that can be used as well as the ball motion Ei p fscale5 (10)
and has to be carefully considered. At a constant pot height to
As expected the simulated energy Ei increases with the geometry
diameter ratio the pot diameter influences the energy Ei which
factor fscale. The simulation results diverge slightly from the
can be explained from the ball motion in the pot.17
predicted value so within the change of the three parameters
Ei p d p 4 (6) pot diameter, height and revolution radius the energy depends on
The kinetic energy Ekin of a single ball is equal to the product Ei p fscale4.87 (11)
of the ball mass m, the pot diameter dP and the acceleration a
The error may be caused from the effect of other parameters
acting on a ball moving from one point to another. The
like ball diameter, filling ratio or the speed ratio which are not
acceleration can be expressed by the revolution radius R and
completely independent and lead to different motion and
the angular velocity O.16
collision patterns in the modified mill geometry.16
Ekin = 1/2mvj2 = madP (a = RO) (7)
Chem. Soc. Rev. This journal is c The Royal Society of Chemistry 2013
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Chem. Soc. Rev. This journal is c The Royal Society of Chemistry 2013