A) Total Apparent Volumetric Charge Filling including balls and excess slurry on top of the ball charge, plus the interstitial voids in between the balls expressed as a percentage of the net internal mill volume (inside liners).
B) Overflow Discharge Mills operating at low ball fillings slurry may accumulate on top of the ball charge; causing, the Total Charge Filling Level to be higher than the Ball Filling Level. Grate Discharge mills will not face this issue.
C) This value represents the Volumetric Fractional Filling of the Voids in between the balls by the retained slurry in the mill charge. As defined, this value should never exceed 100%, but in some cases particularly in Grate Discharge Mills it could be lower than 100%. Note that this interstitial slurry does not include the overfilling slurry derived from the difference between the Charge and Ball Filling.
D) Represents the so-called Dynamic Angle of Repose (or Lift Angle) adopted during steady operation by the top surface of the mill charge (the kidney) with respect to the horizontal. A reasonable default value for this angle is 32, but may be easily tuned to specific applications against any available actual power data.
The first step in mill design is to determine the power needed to produce the desired grind in the chosen ore. The most used equation, for this purpose, is the empirical Bond equation (Bond, 1960, 1961; Rowland and Kjos, 1978).
In this equation, E is the specific energy required for the grind, and F80 and P80 are the sizes in micrometers that 80% of the weight passes of the mill feed and product respectively. The parameter Wi, known as the work index of the ore, is obtained from batch bench tests first devised by Bond (1961). The power calculated on using equation 1, (Bond, 1961; Rowland and Kjos, 1978), relates to:
1) Rod milling a rod mill with a diameter of 2.44 meters, inside new liners, grinding wet in open circuit. 2) Ball milling a ball mill with a diameter of 2.44 meters, inside new liners, grinding wet in open circuit.
When the grinding conditions differ from these specified conditions, efficiency factors (Rowland and Kjos, 1978) have to be used in conjunction with equation 1. In general, therefore, the required mill power is calculated using the following equation
where n is the number of efficiency factors, EFi, used and fo is the feed rate of new ore to the mill. The power calculated from equation 2 can be looked up in published tables (Rowland and Kjos, 1978) and the correct mill size and type can be selected.
The philosophy in the development of the MRRC grinding simulation package was to build interactive software that could be used as an inexpensive means of providing a semi-quantitative check on a grinding mill design. In addition the software is designed to slot in to a general mineral processing package now undergoing development at the MRRC.
In Grinding, selecting (calculate)the correct or optimum ball sizethat allows for the best and optimum/ideal or target grind size to be achieved by your ball mill is an important thing for a Mineral Processing Engineer AKA Metallurgist to do. Often, the ball used in ball mills is oversize just in case. Well, this safety factor can cost you much in recovery and/or mill liner wear and tear.
Ball mill steel balls are consumables of the grinding plant, milling balls need to be replenished at intervals to ensure the grinding quality and grinding rate. How many balls in a ball mill can obtain the best grinding efficiency? Lets figure out. If you would like the ball mill price, contact us, quick respond!
The ball mill is one of the necessary equipment for the mine beneficiation plant, and the investment in the ball mill accounted for a large proportion of the entire beneficiation plant. The ball mill balls quality, quantity, and size will all affect the grinding effect of the ball mill. In addition, while grinding the ore block, the steel balls continuously wear and become smaller until it fails, so the grinding balls consumption is extremely large. If the ball mill is loaded with too many grinding balls, the steel balls are easily overlapped with each other, and the grinding effect is lost. Moreover, some of the steel balls are thrown before the height is raised, which reduces the grinding capacity as a whole and increases the power of the ball mill. If the ball mill contains too few balls and there is not enough capacity between the steel balls to grind the material, it will prolong the working time of the ball mill, which will not only consume a lot of energy, but also cause low grinding efficiency. Therefore, the rationality of ball mill ball loading Very important.
In general, the ball volume of the ball mill steel ball is lower than the horizontal line in the cylinder. It is better to control the ball amount at about 40-50%. For smaller ball mills, the ball balls accounts about 35% at best, this can effectively ensure that the steel ball can fall freely, so that creates a larger impact force.
Ball mill steel balls mainly include: cast iron balls, forged steel balls, rolled steel balls, and the diameter of ball mill steel balls usually is 20mm ~ 120mm, and the maximum steel ball diameter used by super large ball mill is 130mm ~ 150mm.
Generally, the newly installed ball mill has a running-in process. During the running-in process, the amount of steel balls is added for the first time, which accounts for 80% of the maximum ball load of the ball mill. Steel ball sizes are 120, 100, 80, 60, 40.
For example, the 100-150 tons ball mill has a maximum ball loading capacity of 9.5-10 tons. For the first time, 30% 40% of the steel balls (120mm and 100mm), 40% 30% of the medium balls (80mm) and 30% of the small balls (60mm and 40mm) were added. Why only 80% of steel balls are added in the running in process of the ball mill? Because after the ball mill is installed, the large and small teeth of the ball mill need to mesh, and the handling capacity (ore volume) should be gradually increased. After two or three days of normal continuous operation of the ball mill, stop the ball mill and check the meshing condition of the large and small gears. When everything is normal, open the manhole cover of the ball mill and add the remaining 20% steel balls for the second time.
Speaking from experience, after using the ball mill for a time, if the ball needs to be filled or replaced, the following two points can be used to determine whether the balls loading amount is reasonable.
1. Under the premise that the classifier overflow fineness and the ball mills ore supply amount are unchanged, the amount of sand returned is reduced, which indicates that the grinding function has been strengthened and the ball filling amount is suitable. At this time, the ball amount can be appropriately increased to increase grinding efficiency.
2. Observation of the sand return result of the classifier. If the particle size of the material close to the overflow is found to increase, it means that the ball mill steel ball proportion is insufficient, and the ball amount needs to be increased; otherwise, if the coarse particles increase in the return sand, it indicates that the number of big balls is relatively small, it should better add some big balls.
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.
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:
where Dm is the mill diameter in meters. The optimum rotational speed is usually set at 6580% of the critical speed. These data are approximate and may not be valid for metal particles that tend to agglomerate by welding.
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 3035% of its volume.
The mill productivity also depends on many other factors: physical-chemical properties 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.
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.
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).
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.
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).
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 1.561.64. 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.
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.
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 .
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.
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.
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.
The ball mill is a tumbling mill that uses steel balls as the grinding media. The length of the cylindrical shell is usually 11.5 times the shell diameter (Figure 8.11). The feed can be dry, with less than 3% moisture to minimize ball coating, or slurry containing 2040% 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.
Ball mills are filled up to 40% with steel balls (with 3080mm 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 3555% 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 100m. 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 8.53m diameter and 13.41m long with a corresponding motor power of 22MW (Toromocho, private communications).
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 90mm 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 15mm. 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
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.
For more than 50years 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.
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-efficiency 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.
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.
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.
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 3245m. 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.
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.
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 measurement of PSD of a sample of cement is carried out using laser-based methodologies. It requires a skilled operator to achieve consistent results. Agglomeration 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.
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 units opening. In a wet path, a system of scoops that turn with the mill is used and it plunges into a stationary tank.
Mechanochemical synthesis involves high-energy milling techniques and is generally carried out under controlled atmospheres. Nanocomposite powders of oxide, nonoxide, and mixed oxide/nonoxide materials can be prepared using this method. The major drawbacks of this synthesis method are: (1) discrete nanoparticles in the finest size range cannot be prepared; and (2) contamination of the product by the milling media.
More or less any ceramic composite powder can be synthesized by mechanical mixing of the constituent phases. The main factors that determine the properties of the resultant nanocomposite products are the type of raw materials, purity, the particle size, size distribution, and degree of agglomeration. Maintaining purity of the powders is essential for avoiding the formation of a secondary phase during sintering. Wet ball or attrition milling techniques can be used for the synthesis of homogeneous powder mixture. Al2O3/SiC composites are widely prepared by this conventional powder mixing route by using ball milling . However, the disadvantage in the milling step is that it may induce certain pollution derived from the milling media.
In this mechanical method of production of nanomaterials, which works on the principle of impact, the size reduction is achieved through the impact caused when the balls drop from the top of the chamber containing the source material.
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 generally 10mm. 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 100150h to obtain uniform-sized fine powder. In high-energy 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.
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 disadvantage 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 .
Planetary ball mill was used to synthesize iron nanoparticles. The synthesized nanoparticles were subjected to the characterization studies by X-ray diffraction (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 10m 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 10h because after that time period, chances of contamination inclined and the particles size became almost constant so the powder was ball milled for 10h to synthesize nanoparticles . Fig. 12 shows the SEM image of the iron nanoparticles.
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.
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).
The mill is evacuated during milling to a pressure of 106 Torr, in order to avoid reactions with a gas atmosphere. 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.
In spite of the traditional approaches used for gas-solid reaction at relatively high temperature, Calka etal. and El-Eskandarany etal. proposed a solid-state approach, the so-called reactive ball milling (RBM), used for preparations different families of meal nitrides and hydrides at ambient temperature. This mechanically 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.
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. 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, starting 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, using for example cold-rolling approach, 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.
Planetary ball mills are the most popular mills used in scientific research for synthesizing 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 10g based on the vials 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., 2050 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 103bar before introducing H2 gas to fill the vial with a pressure of 550bar (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).
Tumbling mill is cylindrical shell (Fig.9.6AC) 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 50bar 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 (100500g 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 300h) to complete the gas-solid reaction 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 (1000m 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).
Ball milling is often used not only for grinding powders but also for oxides or nanocomposite synthesis and/or structure/phase composition optimization [14,41]. Mechanical activation by ball milling is known to increase the material reactivity and uniformity of spatial distribution of elements . Thus, postsynthesis processing of the materials by ball milling can help with the problem of minor admixture forming during cooling under air after high-temperature sintering due to phase instability.
Ball milling technique, using mechanical alloying and mechanical milling approaches were proposed to the word wide in the 8th decade of the last century for preparing a wide spectrum of powder materials and their alloys. In fact, ball milling process is not new and dates back to more than 150 years. It has been used in size comminutions of ore, mineral dressing, preparing talc powders and many other applications. It might be interesting for us to have a look at the history and development of ball milling and the corresponding products. The photo shows the STEM-BF image of a Cu-based alloy nanoparticle prepared by mechanical alloying (After El-Eskandarany, unpublished work, 2014).
Ball milling, a shear-force dominant process where the particle size goes on reducing by impact and attrition mainly consists of metallic balls (generally Zirconia (ZrO2) or steel balls), acting as grinding media and rotating shell to create centrifugal force. In this process, graphite (precursor) was breakdown by randomly striking with grinding media in the rotating shell to create shear and compression force which helps to overcome the weak Vander Waal's interaction between the graphite layers and results in their splintering. Fig. 4A schematic illustrates ball milling process for graphene preparation. Initially, because of large size of graphite, compressive force dominates and as the graphite gets fragmented, shear force cleaves graphite to produce graphene. However, excessive compression force may damage the crystalline properties of graphene and hence needs to be minimized by controlling the milling parameters e.g. milling duration, milling revolution per minute (rpm), ball-to-graphite/powder ratio (B/P), initial graphite weight, ball diameter. High quality graphene can be achieved under low milling speed; though it will increase the processing time which is highly undesirable for large scale production.
Fig. 4. (A) Schematic illustration of graphene preparation via ball milling. SEM images of bulk graphite (B), GSs/E-H (C) GSs/K (D); (E) and (F) are the respective TEM images; (G) Raman spectra of bulk graphite versus GSs exfoliated via wet milling in E-H and K.
Milling of graphite layers can be instigated in two states: (i) dry ball milling (DBM) and (ii) wet ball milling (WBM). WBM process requires surfactant/solvent such as N,N Dimethylformamide (DMF) , N-methylpyrrolidone (NMP) , deionized (DI) water , potassium acetate , 2-ethylhexanol (E-H)  and kerosene (K)  etc. and is comparatively simpler as compared with DBM. Fig. 4BD show the scanning electron microscopy (SEM) images of bulk graphite, graphene sheets (GSs) prepared in E-H (GSs/E-H) and K (GSs/K), respectively; the corresponding transmission electron microscopy (TEM) images and the Raman spectra are shown in Fig. 4EG, respectively .
Compared to this, DBM requires several milling agents e.g. sodium chloride (NaCl) , Melamine (Na2SO4) [31,32] etc., along with the metal balls to reduce the stress induced in graphite microstructures, and hence require additional purification for exfoliant's removal. Na2SO4 can be easily washed away by hot water  while ammonia-borane (NH3BH3), another exfoliant used to weaken the Vander Waal's bonding between graphite layers can be using ethanol . Table 1 list few ball milling processes carried out using various milling agent (in case of DBM) and solvents (WBM) under different milling conditions.
Ball milling of graphite with appropriate stabilizers is another mode of exfoliation in liquid phase.21 Graphite is ground under high sheer rates with millimeter-sized metal balls causing exfoliation to graphene (Fig. 2.5), under wet or dry conditions. For instance, this method can be employed to produce nearly 50g of graphene in the absence of any oxidant.22 Graphite (50g) was ground in the ball mill with oxalic acid (20g) in this method for 20 hours, but, the separation of unexfoliated fraction was not discussed.22 Similarly, solvent-free graphite exfoliations were carried out under dry milling conditions using KOH,23 ammonia borane,24 and so on. The list of graphite exfoliations performed using ball milling is given in Table 2.2. However, the metallic impurities from the machinery used for ball milling are a major disadvantage of this method for certain applications.25
Reactive ball-milling (RBM) technique has been considered as a powerful tool for fabrication of metallic nitrides and hydrides via room temperature ball milling. The flowchart shows the mechanism of gas-solid reaction through RBM that was proposed by El-Eskandarany. In his model, the starting metallic powders are subjected to dramatic shear and impact forces that are generated by the ball-milling media. The powders are, therefore, disintegrated into smaller particles, and very clean or fresh oxygen-free active surfaces of the powders are created. The reactive milling atmosphere (nitrogen or hydrogen gases) was gettered and absorbed completely by the first atomically clean surfaces of the metallic ball-milled powders to react in a same manner as a gas-solid reaction owing to the mechanically induced reactive milling.
Ball milling is a grinding method that grinds nanotubes into extremely fine powders. During the ball milling process, the collision between the tiny rigid balls in a concealed container will generate localized high pressure. Usually, ceramic, flint pebbles and stainless steel are used.25 In order to further improve the quality of dispersion and introduce functional groups onto the nanotube surface, selected chemicals can be included in the container during the process. The factors that affect the quality of dispersion include the milling time, rotational speed, size of balls and balls/ nanotube amount ratio. Under certain processing conditions, the particles can be ground to as small as 100nm. This process has been employed to transform carbon nanotubes into smaller nanoparticles, to generate highly curved or closed shell carbon nanostructures from graphite, to enhance the saturation of lithium composition in SWCNTs, to modify the morphologies of cup-stacked carbon nanotubes and to generate different carbon nanoparticles from graphitic carbon for hydrogen storage application.25 Even though ball milling is easy to operate and suitable for powder polymers or monomers, process-induced damage on the nanotubes can occur.
Ball milling is a way to exfoliate graphite using lateral force, as opposed to the Scotch Tape or sonication that mainly use normal force. Ball mills, like the three roll machine, are a common occurrence in industry, for the production of fine particles. During the ball milling process, there are two factors that contribute to the exfoliation. The main factor contributing is the shear force applied by the balls. Using only shear force, one can produce large graphene flakes. The secondary factor is the collisions that occur during milling. Harsh collisions can break these large flakes and can potentially disrupt the crystal structure resulting in a more amorphous mass. So in order to create good-quality, high-area graphene, the collisions have to be minimized.
The ball-milling process is common in grinding machines as well as in reactors where various functional materials can be created by mechanochemical synthesis. A simple milling process reduces both CO2 generation and energy consumption during materials production. Herein a novel mechanochemical approach 1-3) to produce sophisticated carbon nanomaterials is reported. It is demonstrated that unique carbon nanostructures including carbon nanotubes and carbon onions are synthesized by high-speed ball-milling of steel balls. It is considered that the gas-phase reaction takes place around the surface of steel balls under local high temperatures induced by the collision-friction energy in ball-milling process, which results in phase separated unique carbon nanomaterials.
Conventional ball milling is a traditional powder-processing technique, which is mainly used for reducing particle sizes and for the mixing of different materials. The technique is widely used in mineral, pharmaceutical, and ceramic industries, as well as scientific laboratories. The HEBM technique discussed in this chapter is a new technique developed initially for producing new metastable materials, which cannot be produced using thermal equilibrium processes, and thus is very different from conventional ball milling technique. HEBM was first reported by Benjamin  in the 1960s. So far, a large range of new materials has been synthesized using HEBM. For example, oxide-dispersion-strengthened alloys are synthesized using a powerful high-energy ball mill (attritor) because conventional ball mills could not provide sufficient grinding energy . Intensive research in the synthesis of new metastable materials by HEBM was stimulated by the pioneering work in the amorphization of the Ni-Nb alloys conducted by Kock et al. in 1983 . Since then, a wide spectrum of metastable materials has been produced, including nanocrystalline , nanocomposite , nanoporous phases , supersaturated solid solutions , and amorphous alloys . These new phase transformations induced by HEBM are generally referred as mechanical alloying (MA). At the same time, it was found that at room temperature, HEBM can activate chemical reactions which are normally only possible at high temperatures . This is called reactive milling or mechano-chemistry. Reactive ball milling has produced a large range of nanosized oxides , nitrides , hydrides , and carbide  particles.
The major differences between conventional ball milling and the HEBM are listed in the Table 1. The impact energy of HEBM is typically 1000 times higher than the conventional ball milling energy. The dominant events in the conventional ball milling are particle fracturing and size reductions, which correspond to, actually, only the first stage of the HEBM. A longer milling time is therefore generally required for HEBM. In addition to milling energy, the controls of milling atmosphere and temperature are crucial in order to create the desired structural changes or chemical reactions. This table shows that HEBM can cover most work normally performed by conventional ball milling, however, conventional ball milling equipment cannot be used to conduct any HEBM work.
Different types of high-energy ball mills have been developed, including the Spex vibrating mill, planetary ball mill, high-energy rotating mill, and attritors . In the nanotube synthesis, two types of HEBM mills have been used: a vibrating ball mill and a rotating ball mill. The vibrating-frame grinder (Pulverisette O, Fritsch) is shown in Fig. 1a. This mill uses only one large ball (diameter of 50 mm) and the media of the ball and vial can be stainless steel or ceramic tungsten carbide (WC). The milling chamber, as illustrated in Fig. 1b, is sealed with an O-ring so that the atmosphere can be changed via a valve. The pressure is monitored with an attached gauge during milling.
where Mb is the mass of the milling ball, Vmax the maximum velocity of the vial,/the impact frequency, and Mp the mass of powder. The milling intensity is a very important parameter to MA and reactive ball milling. For example, a full amorphization of a crystalline NiZr alloy can only be achieved with a milling intensity above an intensity threshold of 510 ms2 . The amorphization process during ball milling can be seen from the images of transmission electron microscopy (TEM) in Fig. 2a, which were taken from samples milled for different lengths of time. The TEM images show that the size and number of NiZr crystals decrease with increasing milling time, and a full amorphization is achieved after milling for 165 h. The corresponding diffraction patterns in Fig. 2b confirm this gradual amorphization process. However, when milling below the intensity threshold, a mixture of nanocrystalline and amorphous phases is produced. This intensity threshold depends on milling temperature and alloy composition .
Figure 2. (a) Dark-field TEM image of Ni10Zr7 alloy milled for 0.5, 23, 73, and 165 h in the vibrating ball mill with a milling intensity of 940 ms2. (b) Corresponding electron diffraction patterns .
Fig. 3 shows a rotating steel mill and a schematic representation of milling action inside the milling chamber. The mill has a rotating horizontal cell loaded with several hardened steel balls. As the cell rotates, the balls drop onto the powder that is being ground. An external magnet is placed close to the cell to increase milling energy . Different milling actions and intensities can be realized by adjusting the cell rotation rate and magnet position.
The atmosphere inside the chamber can be controlled, and adequate gas has to be selected for different milling experiments. For example, during the ball milling of pure Zr powder in the atmosphere of ammonia (NH3), a series of chemical reactions occur between Zr and NH3 [54,55]. The X-ray diffraction (XRD) patterns in Fig. 4 show the following reaction sequence as a function of milling time:
The mechanism of a HEBM process is quite complicated. During the HEBM, material particles are repeatedly flattened, fractured, and welded. Every time two steel balls collide or one ball hits the chamber wall, they trap some particles between their surfaces. Such high-energy impacts severely deform the particles and create atomically fresh, new surfaces, as well as a high density of dislocations and other structural defects . A high defect density induced by HEBM can accelerate the diffusion process . Alternatively, the deformation and fracturing of particles causes continuous size reduction and can lead to reduction in diffusion distances. This can at least reduce the reaction temperatures significantly, even if the reactions do not occur at room temperature [57,58]. Since newly created surfaces are most often very reactive and readily oxidize in air, the HEBM has to be conducted in an inert atmosphere. It is now recognized that the HEBM, along with other non-equilibrium techniques such as rapid quenching, irradiation/ion-implantation, plasma processing, and gas deposition, can produce a series of metastable and nanostructured materials, which are usually difficult to prepare using melting or conventional powder metallurgy methods [59,60]. In the next section, detailed structural and morphological changes of graphite during HEBM will be presented.
Ball milling and ultrasonication were used to reduce the particle size and distribution. During ball milling the weight (grams) ratio of balls-to-clay particles was 100:2.5 and the milling operation was run for 24 hours. The effect of different types of balls on particle size reduction and narrowing particle size distribution was studied. The milled particles were dispersed in xylene to disaggregate the clumps. Again, ultrasonication was done on milled samples in xylene. An investigation on the amplitude (80% and 90%), pulsation rate (5 s on and 5 s off, 8 s on and 4 s off) and time (15 min, 1 h and 4 h) of the ultrasonication process was done with respect to particle size distribution and the optimum conditions in our laboratory were determined. A particle size analyzer was used to characterize the nanoparticles based on the principles of laser diffraction and morphological studies.