Ball Mills

For instance, a ball mill, which is a powder-processing technique involving defor-

mation, cold welding, fracturing, and rewelding of powder particles, is used for
mechanical alloying.

From: The Science and Technology of Unconventional Oils, 2017

Related terms:

Ball Milling, Grinding Mills, Mechanical Alloying, Biomass, Nanoparticles, Kilns,

Bagasse Ash, Rod Mill

View all Topics

Quantum Nanostructures (QDs): An

Overview
D. Sumanth Kumar, ... H.M. Mahesh, in Synthesis of Inorganic Nanomaterials, 2018

3.6.1.1 Ball Milling

A ball mill is a type of grinder used to grind and blend bulk material into QDs/nanosize
using different sized balls. The working principle is simple; impact and attrition
size reduction take place as the ball drops from near the top of a rotating hollow
cylindrical shell. The nanostructure size can be varied by varying the number and
size of balls, the material used for the balls, the material used for the surface of
the cylinder, the rotation speed, and the choice of material to be milled. Ball mills
are commonly used for crushing and grinding the materials into an extremely fine
form. The ball mill contains a hollow cylindrical shell that rotates about its axis. This
cylinder is filled with balls that are made of stainless steel or rubber to the material
contained in it. Ball mills are classified as attritor, horizontal, planetary, high energy,
or shaker.

> Read full chapter

Mechanical Crushing and Grinding
Oleg D. Neikov, in Handbook of Non-Ferrous Metal Powders, 2009

Tumbling Ball Mills

Tumbling ball mills or ball mills are most widely used in both wet and dry systems,
in batch and continuous operations, and on a small and large scale.

Grinding elements in ball mills travel at different velocities. Therefore, collision force,
direction and kinetic energy between two or more elements vary greatly within
the ball charge. Frictional wear or rubbing forces act on the particles, as well as
collision energy. These forces are derived from the rotational motion of the balls
and movement of particles within the mill and contact zones of colliding balls.

By rotation of the mill body, due to friction between mill wall and balls, the latter
rise in the direction of rotation till a helix angle does not exceed the angle of
repose, whereupon, the balls roll down. Increasing of rotation rate leads to growth
of the centrifugal force and the helix angle increases, correspondingly, till the
component of weight strength of balls become larger than the centrifugal force.
From this moment the balls are beginning to fall down, describing during falling
certain parabolic curves (Figure 2.7). With the further increase of rotation rate, the
centrifugal force may become so large that balls will turn together with the mill body
without falling down. The critical speed n (rpm) when the balls are attached to the
wall due to centrifugation:

Figure 2.7. Displacement of balls in mill.

where Dm is the mill diameter in meters. The optimum rotational speed is usually
set at 65–80% of the critical speed. These data are approximate and may not be valid
for metal particles that tend to agglomerate by welding.

The minimal magnitude of ball size is calculated in millimeters from the equation:
where db.max is the maximum size of feed (mm); is compression strength (MPa); E
is modulus of elasticity (MPa); b is density of material of balls (kg/m3); D is inner
diameter of the mill body (m).

Generally, a maximum allowed ball size is situated in the range from D /18 to D/24.

The degree of filling the mill with balls also influences productivity of the mill and
milling efficiency. With excessive filling, the rising balls collide with falling ones.
Generally, filling the mill by balls must not exceed 30–35% of its volume.

Productivity of ball mills depends on drum diameter and the relation of drum
diameter and length. Optimum ratio between length L and diameter D, L:D is,
usually, accepted in the range 1.56–1.64.

The mill productivity also depends on many other factors: physical-chemical proper-
ties of feed material, filling of the mill by balls and their sizes, armor surface shape,
speed of rotation, milling fineness and timely moving off of ground product.

It is possible to make an approximate calculation of the capacity of a ball mill by

means of the equation:

where b.ap is the apparent density of the balls; l is the degree of filling of the mill
by balls; n is revolutions per minute; 1, and 2 are coefficients of efficiency of
electric engine and drive, respectively.

A feature of ball mills is their high specific energy consumption; a mill filled with
balls, working idle, consumes approximately as much energy as at full-scale capacity,
i.e. during grinding of material. Therefore, it is most disadvantageous to use a ball
mill at less than full capacity.

Ball mills have the following advantages:

• universality and high capacity

• permanence of a prescribed milling fineness by certain capacity over long

periods of time (with periodical addition of balls for compensation of their
wear)
• reliability and safety, simplicity of servicing.

Shortcomings of ball mills:

• unhandiness and large weight

• grinding high specific energy consumption; energy is mainly consumed on

wear of balls and wall armor, friction, heating of material, etc.
• noise during working.
Depending on the form of the body, ball mills are differentiated as cylindrical, tube
and conical.

Depending on the discharging method, they are differentiated:

• mills with free discharge of ground product through a hollow trunnion

• mills with discharge along all length of the drum through a cylindrical sieve

• mills with an external separation system, in which a prepared product is

separated from the under milled powder in separators outside of the mill
drum.

> Read full chapter

Mechanical Crushing and Grinding

Oleg D. Neikov, in Handbook of Non-Ferrous Metal Powders (Second Edition), 2019

Tumbling Ball Mills

Tumbling ball mills or ball mills are most widely used in both wet and dry systems,
in batch and continuous operations, and on small and large scales.

Grinding elements in ball mills travel at different velocities. Therefore, collision force,
direction, and kinetic energy between two or more elements vary greatly within the
ball charge. Frictional wear or rubbing forces act on the particles as well as collision
energy. These forces are derived from the rotational motion of the balls and the
movement of particles within the mill and contact zones of colliding balls.

By the rotation of the mill body, due to friction between the mill wall and balls, the
latter rise in the direction of rotation until a helix angle does not exceed the angle
of repose, whereupon the balls roll down. Increasing the rotation rate leads to the
growth of the centrifugal force and the helix angle increases, correspondingly, until
the component of the weight strength of balls becomes larger than the centrifugal
force. From this moment, the balls are beginning to fall down, describing certain
parabolic curves during the fall (Fig. 2.10).
Fig. 2.10. Displacement of balls in mill.

With the further increase of rotation rate, the centrifugal force may become so large
that balls will turn together with the mill body without falling down. The critical
speed n (rpm) when the balls remain attached to the wall with the aid of centrifugal
force is:

where Dm is the mill diameter in meters. The optimum rotational speed is usually
set at 65%–80% of the critical speed. These data are approximate and may not be
valid for metal particles that tend to agglomerate by welding.

The minimal magnitude of the ball size is calculated in millimeters from the equa-
tion:

where db.max is the maximum size of the feed (mm), is the compression strength
(MPa), E is the modulus of elasticity (MPa), b is the density of material of balls
(kg/m3), and D is the inner diameter of the mill body (m).

Generally, a maximum allowed ball size is situated in the range from D/18 to D/24.

The degree of filling the mill with balls also influences the productivity of the mill
and milling efficiency. With excessive filling, the rising balls collide with falling
ones. Generally, filling the mill by balls must not exceed 30%–35% of its volume.

The productivity of ball mills depends on the drum diameter and the relation of
∫ drum diameter and length. The optimum ratio between length L and diameter D,
L:D, is usually accepted in the range 1.56–1.64. The mill productivity also depends on
many other factors, including the physical-chemical properties of the feed material,
the filling of the mill by balls and their sizes, the armor surface shape, the speed of
rotation, the milling fineness, and the timely moving off of the ground product.
It is possible to make an approximate calculation of the capacity of a ball mill with
uneven armor by means of the equation:

where D is the drum diameter, L is the drum length, b.ap is the apparent density
of the balls, is the degree of filling of the mill by balls, n is the revolutions per
minute, and 1, and 2 are coefficients of efficiency of electric engine and drive,
respectively.

A feature of ball mills is their high specific energy consumption. A mill filled with
balls, working idle, consumes approximately as much energy as at full-scale capacity,
that is, during the grinding of material. Therefore, it is most disadvantageous to use
a ball mill at less than full capacity.

Ball mills have the following advantages:

• Universality and high capacity.

• Permanence of a prescribed milling fineness by certain capacity over long

periods of time (with periodical addition of balls for compensation of their
wear).
• Reliability and safety, simplicity of servicing.

Shortcomings of ball mills:

• Unhandiness and large weight.

• Grinding high specific energy consumption; energy is mainly consumed on

the wear of balls and wall armor, friction, heating of material, etc.
• Loud noise during working.

Depending on the form of the body, ball mills are differentiated as cylindrical,
tubular, and conical.

Depending on the discharging method, they are also differentiated as:

• Mills with free discharge of ground product through a hollow trunnion.

• Mills with discharge along the length of the drum through a cylindrical sieve.

• Mills with an external separation system in which a prepared product is

separated from the undermilled powder in separators outside the mill drum.

Milling time in tumbler mills is longer to accomplish the same level of blending
achieved in the attrition or vibratory mill, but the overall productivity is substantially
greater. Tumbler mills usually are used to pulverize or flake metals, using a grinding
aid or lubricant to prevent cold welding agglomeration and to minimize oxidation
[23].
Cylindrical Ball Mills differ usually in steel drum design (Fig. 2.11), which is lined
inside by armor slabs that have dissimilar sizes and form a rough inside surface. Due
to such juts, the impact force of falling balls is strengthened. The initial material is
fed into the mill by a screw feeder located in a hollow trunnion; the ground product
is discharged through the opposite hollow trunnion.

Fig. 2.11. Cylindrical ball mill.

Cylindrical screen ball mills have a drum with spiral curved plates with longitudinal
slits between them. The ground product passes into these slits and then through a
cylindrical sieve and is discharged via the unloading funnel of the mill body.

Conical Ball Mills differ in mill body construction, which is composed of two cones
and a short cylindrical part located between them (Fig. 2.12). Such a ball mill body is
expedient because efficiency is appreciably increased. Peripheral velocity along the
conical drum scales down in the direction from the cylindrical part to the discharge
outlet; the helix angle of balls is decreased and, consequently, so is their kinetic
energy. The size of the disintegrated particles also decreases as the discharge outlet
is approached and the energy used decreases. In a conical mill, most big balls take
up a position in the deeper, cylindrical part of the body; thus, the size of the balls
scales down in the direction of the discharge outlet.
Fig. 2.12. Conical ball mill.

For emptying, the conical mill is installed with a slope from bearing to one. In wet
grinding, emptying is realized by the decantation principle, that is, by means of
unloading through one of two trunnions.

With dry grinding, these mills often work in a closed cycle. A scheme of the conical
ball mill supplied with an air separator is shown in Fig. 2.13. Air is fed to the mill by
means of a fan. Carried off by air currents, the product arrives at the air separator,
from which the coarse particles are returned by gravity via a tube into the mill. The
finished product is trapped in a cyclone while the air is returned in the fan.

Fig. 2.13. Conical ball mill supplied by air separator, working in a closed cycle.

> Read full chapter

Developments in iron ore comminu-
tion and classification technologies
A. Jankovic, in Iron Ore, 2015

8.3.2.2 Ball mills

The ball mill is a tumbling mill that uses steel balls as the grinding media. The length
of the cylindrical shell is usually 1–1.5 times the shell diameter (Figure 8.11). The feed
can be dry, with less than 3% moisture to minimize ball coating, or slurry containing
20–40% water by weight. Ball mills are employed in either primary or secondary
grinding applications. In primary applications, they receive their feed from crushers,
and in secondary applications, they receive their feed from rod mills, AG mills, or
SAG mills.

Figure 8.11. Ball mill external appearance and internal view.

Ball mills are filled up to 40% with steel balls (with 30–80 mm diameter), which
effectively grind the ore. The material that is to be ground fills the voids between
the balls. The tumbling balls capture the particles in ball/ball or ball/liner events and
load them to the point of fracture.

When hard pebbles rather than steel balls are used for the grinding media, the mills
are known as “pebble mills.” As mentioned earlier, pebble mills are widely used in
the North American taconite iron ore operations. Since the weight of pebbles per
unit volume is 35–55% of that of steel balls, and as the power input is directly
proportional to the volume weight of the grinding medium, the power input and
capacity of pebble mills are correspondingly lower. Thus, in a given grinding circuit,
for a certain feed rate, a pebble mill would be much larger than a ball mill, with
correspondingly a higher capital cost. However, the increase in capital cost is justified
economically by a reduction in operating cost attributed to the elimination of steel
grinding media.

In general, ball mills can be operated either wet or dry and are capable of producing
products in the order of 100 μm. This represents reduction ratios of as great as
100. Very large tonnages can be ground with these ball mills because they are very
effective material handling devices. Ball mills are rated by power rather than capacity.
Today, the largest ball mill in operation is 8.53 m diameter and 13.41 m long with a
corresponding motor power of 22 MW (Toromocho, private communications).

> Read full chapter

Manufacture of Portland Cement

Peter del Strother, in Lea's Chemistry of Cement and Concrete (Fifth Edition), 2019

2.10 Clinker Grinding

2.10.1 Ball Mills

Modern ball mills consist of two chambers separated by a diaphragm. In the first
chamber the steel-alloy balls (also described as charge balls or media) are about
90 mm diameter. The mill liners are designed to lift the media as the mill rotates,
so the comminution process in the first chamber is dominated by crushing. In the
second chamber the ball diameters are of smaller diameter, between 60 and 15 mm.
In this chamber the lining is typically a ‘classifying lining’ which sorts the media so
that ball size reduces towards the discharge end of the mill. Here, comminution
takes place in the rolling point-contact zone between each charge ball. An example
of a two chamber ball mill is illustrated in Fig. 2.22.15
Fig. 2.22. Diagram of cement ball mill.(Based on an image from ThyssenKrupp
AG.15)

Much of the energy consumed by a ball mill generates heat. Water is injected into
the second chamber of the mill to provide evaporative cooling. Air flow through the
mill is one medium for cement transport but also removes water vapour and makes
some contribution to cooling.

Grinding is an energy intensive process and grinding more finely than necessary
wastes energy. Cement consists of clinker, gypsum and other components mostly
more easily ground than clinker. To minimise over-grinding modern ball mills are
fitted with dynamic separators (otherwise described as ‘classifiers’ or more simply as
‘separators’). The working principle is that cement is removed from the mill before
over-grinding has taken place. The cement is then separated into a fine fraction,
which meets finished product requirements, and a coarse fraction which is returned
to mill inlet. Recirculation factor, that is, the ratio of mill throughput to fresh feed is
up to three. Beyond this, efficiency gains are minimal.

2.10.2 Vertical Mills

For more than 50 years vertical mills have been the mill of choice for grinding raw
materials into raw meal. More recently they have become widely used for cement
production. They have lower specific energy consumption than ball mills and the
separator, as in raw mills, is integral with the mill body.
In the Loesche mill, Fig. 2.23,16 two pairs of rollers are used. In each pair the first,
smaller diameter, roller stabilises the bed prior to grinding which takes place under
the larger roller. Manufacturers use different technologies for bed stabilisation.

Fig. 2.23. Diagram of a vertical mill.(Courtesy of Loesche GmbH, Düsseldorf.)

2.10.3 The Performance of Ball Mill Relative to Vertical Mills

Comminution in ball mills and vertical mills differs fundamentally. In a ball mill, size
reduction takes place by impact and attrition. In a vertical mill the bed of material is
subject to such a high pressure that individual particles within the bed are fractured,
even though the particles are very much smaller than the bed thickness.

Early issues with vertical mills, such as narrower PSD and modified cement hydration
characteristics compared with ball mills, have been resolved. One modification has
been to install a hot gas generator so the gas temperature is high enough to partially
dehydrate the gypsum.
For many decades the two-compartment ball mill in closed circuit with a high-ef-
ficiency separator has been the mill of choice. In the last decade vertical mills have
taken an increasing share of the cement milling market, not least because the
specific power consumption of vertical mills is about 30% less than that of ball mills
and for finely ground cement less still. The vertical mill has a proven track record in
grinding blastfurnace slag, where it has the additional advantage of being a much
more effective drier of wet feedstock than a ball mill.

The vertical mill is more complex but its installation is more compact. The relative
‘installed’ capital costs tend to be site specific. Historically the installed cost has
tended to be slightly higher for the vertical mill.

2.10.4 Particle Size Distribution

PSD has an impact on workability and rate of strength gain.

The PSD of cement can be described to a good approximation by the Rosin–Ramm-

ler–Sperling–Bennett distribution (see DIN 66145, 1976-0417).

where

x is the particle diameter in micrometres,

R(x) the proportion by mass of particles larger than x.
x the position parameter, which corresponds to R(x) = 0.368.

The equation reduces to the straight line graph

where ‘n’ is the slope of the straight line.

Special graph paper is used with lglg(1/R(x)) on the abscissa and lg(x) on the ordinate
axes. The higher the value of ‘n’, the narrower the particle size distribution. The
position parameter is the particle size with the highest mass density distribution,
the peak of the mass density distribution curve.

Vertical mills tend to produce cement with a higher value of ‘n’. Values of ‘n’ normally
lie between 0.8 and 1.2, dependent particularly on cement fineness. The position
parameter is, of course, lower for more finely ground cements.

2.10.5 Characterisation of Separator Efficiency in a Ball Mill Circuit18

Separator efficiency is defined as specific power consumption reduction of the
mill open-to-closed-circuit with the actual separator, compared with specific power
consumption reduction of the mill open-to-closed-circuit with an ideal separator.

The reduction of sieve residues by comminution is considered to be a first order

process, represented by:
where

E is specific energy consumption

W is comminution index, and
R0 and Rf are sieve residues of fresh material and at mill outlet, respectively. R0
is taken to be unity.

As shown in Fig. 2.24, circulating factor is defined as mill mass flow, that is, fresh
feed plus separator returns. The maximum power reduction arising from use of an
ideal separator increases non-linearly with circulation factor and is dependent on Rf,
normally based on residues in the interval 32–45 μm. The value of the comminution
index, W, is also a function of Rf. The finer the cement, the lower Rf and the greater
the maximum power reduction. At C = 2 most of maximum power reduction is
achieved, but beyond C = 3 there is very little further reduction.

Fig. 2.24. Line diagram of ball mill with separator.

Over the last few decades separator efficiency has increased from about 25% to
75% as a result of improvements in separator design.

Separator particle separation performance is assessed using the Tromp curve, a

graph of percentage separator feed to rejects against particle size range. An example
is shown in Fig. 2.25. Data required is the PSD of separator feed material and of
rejects and finished product streams. The bypass and slope provide a measure of
separator performance.
Fig. 2.25. Example of Tromp curve.

The particle size is plotted on a logarithmic scale on the ordinate axis. The percentage
is plotted on the abscissa either on a linear (as shown here) or on a Gaussian scale.
The advantage of using the Gaussian scale is that the two parts of the graph can be
approximated by two straight lines.

The major cement manufacturers have their own calculation methodologies, manual
and/or computerised for calculation of separator efficiency and Tromp curves.

2.10.6 Measurement of PSD

The measurement of PSD of a sample of cement is carried out using laser-based
methodologies. It requires a skilled operator to achieve consistent results. Agglom-
eration will vary dependent on whether grinding aid is used. Different laser analysis
methods may not give the same results, so for comparative purposes the same
method must be used.

> Read full chapter

Ball and Rod Mills

Jean-Paul Duroudier, in Size Reduction of Divided Solids, 2016

3.1.2 Operation principle

The ball mill is a cylindrical drum (or cylindrical conical) turning around its horizontal
axis. It is partially filled with grinding bodies: cast iron or steel balls, or even flint
(silica) or porcelain bearings. Spaces between balls or bearings are occupied by the
load to be milled.
Following drum rotation, balls or bearings rise by rolling along the cylindrical wall
and descending again in a cascade or cataract from a certain height. The output is
then milled between two grinding bodies.

Ball mills could operate dry or even process a water suspension (almost always for
ores). Dry, it is fed through a chute or a screw through the unit’s opening. In a
wet path, a system of scoops that turn with the mill is used and it plunges into a
stationary tank.

> Read full chapter

Synthesis of Nanocomposites
Krishnasamy Ravichandran, ... Suyamprakam Gobalakrishnan, in Synthesis of Inor-
ganic Nanomaterials, 2018

Construction and Working

A ball mill consists of a hollow cylindrical chamber (Fig. 6.2) which rotates about
a horizontal axis, and the chamber is partially filled with small balls made of steel,
tungsten carbide, zirconia, agate, alumina, or silicon nitride having diameter gener-
ally 10 mm. The inner surface area of the chamber is lined with an abrasion-resistant
material like manganese, steel, or rubber. The magnet, placed outside the chamber,
provides the pulling force to the grinding material, and by changing the magnetic
force, the milling energy can be varied as desired. The ball milling process is carried
out for approximately 100–150 h to obtain uniform-sized fine powder. In high-en-
ergy ball milling, vacuum or a specific gaseous atmosphere is maintained inside
the chamber. High-energy mills are classified into attrition ball mills, planetary
ball mills, vibrating ball mills, and low-energy tumbling mills. In high-energy ball
milling, formation of ceramic nano-reinforcement by in situ reaction is possible.

Fig. 6.2. Schematic diagram of ball milling process.

It is an inexpensive and easy process which enables industrial scale productivity. As

grinding is done in a closed chamber, dust, or contamination from the surroundings
is avoided. This technique can be used to prepare dry as well as wet nanopowders.
Composition of the grinding material can be varied as desired. Even though this
method has several advantages, there are some disadvantages. The major disadvan-
tage is that the shape of the produced nanoparticles is not regular. Moreover, energy
consumption is relatively high, which reduces the production efficiency. This
technique is suitable for the fabrication of several nanocomposites, which include
Co- and Cu-based nanomaterials, Ni-NiO nanocomposites, and nanocomposites of
Ti,C [71].

> Read full chapter

Next-Generation Nanoadsorbents: Op-

portunities and Challenges
Hajira Tahir, Muhammad Saad, in Composite Nanoadsorbents, 2019

3.2.1 Synthesis of Iron Nanoparticles

Planetary ball mill was used to synthesize iron nanoparticles. The synthe-
sized nanoparticles were subjected to the characterization studies by X-ray dif-
fraction (XRD), and scanning electron microscopy (SEM) techniques using a
SIEMENS-D5000 diffractometer and Hitachi S-4800. For the synthesis of iron
nanoparticles, commercial iron powder having particles size of 10 μm was used. The
iron powder was subjected to planetary ball milling for various period of time. The
optimum time period for the synthesis of nanoparticles was observed to be 10 h
because after that time period, chances of contamination inclined and the particles
size became almost constant so the powder was ball milled for 10 h to synthesize
nanoparticles [11]. Fig. 12 shows the SEM image of the iron nanoparticles.
Fig. 12. SEM micrograph of iron nanoparticles.

> Read full chapter

Introduction
M. Sherif El-Eskandarany, in Mechanical Alloying, 2001

Vibratory Ball Mill.

The vibratory ball mill is another kind of high-energy ball mill that is used mainly for
preparing amorphous alloys. The vials capacities in the vibratory mills are smaller
(about 10 ml in volume) compared to the previous types of mills. In this mill, the
charge of the powder and milling tools are agitated in three perpendicular directions
(Fig. 1.6) at very high speed, as high as 1200 rpm.

Figure 1.6. Schematic drawing of a high-energy vibratory ball mill.(After Hashimoto

et al.)[43]

Another type of the vibratory ball mill, which is used at the van der Waals-Zeeman
Laboratory, consists of a stainless steel vial with a hardened steel bottom, and a
single hardened steel ball of 6 cm in diameter (Fig. 1.7).

Figure 1.7. Schematic illustration of the vibratory ball mill, which is used at the van
der Waals-Zeeman Laboratory.
The mill is evacuated during milling to a pressure of 10−6 Torr, in order to avoid
reactions with a gas atmosphere.[44] Subsequently, this mill is suitable for mechanical
alloying of some special systems that are highly reactive with the surrounding
atmosphere, such as rare earth elements.

> Read full chapter

Solid-state hydrogen storage nanoma-

terials for fuel cell applications
Prof. Dr.M. Sherif El-Eskandarany, in Mechanical Alloying (Third Edition), 2020

9.4.2 Synthesizing of nanocrystalline MgH2 powders by reactive

ball milling
In spite of the traditional approaches used for gas-solid reaction at relatively high
temperature, Calka et al.[58] and El-Eskandarany et al.[59] proposed a solid-state ap-
proach, the so-called reactive ball milling (RBM), used for preparations different
families of meal nitrides and hydrides at ambient temperature. This mechanical-
ly induced gas-solid reaction can be successfully achieved, using either high- or
low-energy ball-milling methods, as shown in Fig. 9.5. However, high-energy ball
mill is an efficient process for synthesizing nanocrystalline MgH2 powders using
RBM technique, it may be difficult to scale up for matching the mass production
required by industrial sector. Therefore, from a practical point of view, high-capacity
low-energy milling, which can be easily scaled-up to produce large amount of MgH2
fine powders, may be more suitable for industrial mass production.
Figure 9.5. Flowchart diagram presents two approaches used in KISR for preparing
nanocrystalline MgH2 powders, using high- and low-energy RBM technique under
hydrogen gas pressure.The chart elucidates the two approaches (cold rolling and
catalyzation) used to improve the hydrogen storage behavior of MgH2.

In both approaches but with different scale of time and milling efficiency, the
starting Mg metal powders milled under hydrogen gas atmosphere are practicing
to dramatic lattice imperfections such as twinning and dislocations. These defects
are caused by plastics deformation coupled with shear and impact forces generated
by the ball-milling media.[60] The powders are, therefore, disintegrated into smaller
particles with large surface area, where very clean or fresh oxygen-free active surfaces
of the powders are created. Moreover, these defects, which are intensively located
at the grain boundaries, lead to separate micro-scaled Mg grains into finer grains
capable to getter hydrogen by the first atomically clean surfaces to form MgH2
nanopowders.
Fig. 9.5 illustrates common lab scale procedure for preparing MgH2 powders, start-
ing from pure Mg powders, using RBM via (1) high-energy and (2) low-energy ball
milling. The starting material can be Mg-rods, in which they are processed via sever
plastic deformation,[61] using for example cold-rolling approach,[62] as illustrated in
Fig. 9.5. The heavily deformed Mg-rods obtained after certain cold rolling passes can
be snipped into small chips and then ball-milled under hydrogen gas to produce
MgH2 powders.[8]

9.4.2.1 High-energy reactive ball milling

Planetary ball mills are the most popular mills used in scientific research for syn-
thesizing MgH2 nanopowders. In this type of mill, the ball-milling media have
considerably high energy, because milling stock and balls come off the inner wall
of the vial and the effective centrifugal force reaches up to 20 times gravitational
acceleration. The centrifugal forces caused by the rotation of the supporting disc
and autonomous turning of the vial act on the milling charge (balls and powders).
Since the turning directions of the supporting disc and the vial are opposite, the
centrifugal forces alternately are synchronized and opposite. Therefore, the milling
media and the charged powders alternatively roll on the inner wall of the vial, and
are lifted and thrown off across the bowl at high speed.

In the typical experimental procedure, a certain amount of the Mg (usually in the

range between 3 and 10 g based on the vial’s volume) is balanced inside an inert
gas atmosphere (argon or helium) in a glove box and sealed together with certain
number of balls (e.g., 20–50 hardened steel balls) into a hardened steel vial (Fig. 9.5A
and B), using, for example, a gas-temperature-monitoring system (GST). With the
GST system, it becomes possible to monitor the progress of the gas-solid reaction
taking place during the RBM process, as shown in Fig. 9.5C and D. The temperature
and pressure changes in the system during milling can be also used to realize the
completion of the reaction and the expected end product during the different stages
of milling (Fig. 9.5D). The ball-to-powder weight ratio is usually selected to be in
the range between 10:1 and 50:1. The vial is then evacuated to the level of 10−3 bar
before introducing H2 gas to fill the vial with a pressure of 5–50 bar (Fig. 9.5B). The
milling process is started by mounting the vial on a high-energy ball mill operated
at ambient temperature (Fig. 9.5C).

9.4.2.2 Low-energy reactive ball milling

Tumbling mill is cylindrical shell (Fig. 9.6A–C) that rotates about a horizontal axis
(Fig. 9.6D). Hydrogen gas is pressurized into the vial (Fig. 9.6C) together with Mg
powders and ball-milling media, using ball-to-powder weight ratio in the range
between 30:1 and 100:1. Mg powder particles meet the abrasive and impacting force
(Fig. 9.6E), which reduce the particle size and create fresh-powder surfaces (Fig. 9.6F)
ready to react with hydrogen milling atmosphere.

Figure 9.6. Photographs taken from KISR-EBRC/NAM Lab, Kuwait, show (A) the
vial and milling media (balls) and (B) the setup performed to charge the vial with
50 bar of hydrogen gas. The photograph in (C) presents the complete setup of GST
(supplied by Evico-magnetic, Germany) system prior to start the RBM experiment
for preparing of MgH2 powders, using Planetary Ball Mill P400 (provided by Retsch,
Germany). GST system allows us to monitor the progress of RBM process, as indexed
by temperature and pressure versus milling time (D).

The useful kinetic energy in tumbling mill can be applied to the Mg powder particles
(Fig. 9.7E) by the following means: (1) collision between the balls and the powders; (2)
pressure loading of powders pinned between milling media or between the milling
media and the liner; (3) impact of the falling milling media; (4) shear and abrasion
caused by dragging of particles between moving milling media; and (5) shock-wave
transmitted through crop load by falling milling media. One advantage of this type
of mill is that large amount of the powders (100–500 g or more based on the mill
capacity) can be fabricated for each milling run. Thus, it is suitable for pilot and/or
industrial scale of MgH2 production. In addition, low-energy ball mill produces
homogeneous and uniform powders when compared with the high-energy ball mill.
Furthermore, such tumbling mills are cheaper than high-energy mills and operated
simply with low-maintenance requirements. However, this kind of low-energy mill
requires long-term milling time (more than 300 h) to complete the gas-solid reac-
tion and to obtain nanocrystalline MgH2 powders.

Figure 9.7. Photos taken from KISR-EBRC/NAM Lab, Kuwait, display setup of a
lab-scale roller mill (1000 m in volume) showing (A) the milling tools including the
balls (milling media and vial), (B) charging Mg powders in the vial inside inert gas
atmosphere glove box, (C) evacuation setup and pressurizing hydrogen gas in the
vial, and (D) ball milling processed, using a roller mill. Schematic presentations show
 the ball positions and movement inside the vial of a tumbler mall mill at a dynamic
mode is shown in (E), where a typical ball-powder-ball collusion for a low energy
tumbling ball mill is presented in (F).

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