ball mill process condition

ball milling - an overview | sciencedirect topics

ball milling - an overview | sciencedirect topics

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photo shows the STEM-BF image of a Cu-based alloy nanoparticle prepared by mechanical alloying (After El-Eskandarany, unpublished work, 2014).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 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 [63]. 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, 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) [22], N-methylpyrrolidone (NMP) [26], deionized (DI) water [27], potassium acetate [28], 2-ethylhexanol (E-H) [29] and kerosene (K) [29] 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 [29].

Compared to this, DBM requires several milling agents e.g. sodium chloride (NaCl) [30], 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 [19] while ammonia-borane (NH3BH3), another exfoliant used to weaken the Vander Waal's bonding between graphite layers can be using ethanol [33]. 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 as a mechanochemical technique has been extensively used for grinding of materials to fine particles and for the formation and modification of inorganic solids. Mechanochemistry is a branch of solid-state chemistry in which intramolecular bonds are broken mechanically by using an external mechanical energy followed by additional chemical reactions [109]. Its use in synthetic organic chemistry is comparatively limited but has attained more attention during the last decade. A study proposed the importance of ball milling in synthetic organic chemistry, which has been widely documented [110]. Many reports in the literature have shown that high-speed ball milling (HSBM) is appropriate for a variety of organic transformations and for the expansion of environmentally benevolent chemical reactions [111, 112]. HSBM in solvent-free circumstances is considered as a feasible alternative to wet chemistry. It is based on the similar principles as that of mortar and pestle, which utilizes mechanical actions to convert reactants to products during the course of the reaction [113, 114]. The mills are effective at creating small particle sizes, which has allowed them to demonstrate their amazing characteristics. The ball milling time is an important factor in nanostructure materials synthesis. It has been demonstrated that an increase in the milling time increases microhardness of synthesized materials [115]. Different numbers, sizes, shapes, and materials of the ball bearings used could influence mixing and impact energy and thus the efficiency of the reaction. Using no ball bearing predictably gave the least amount of mixing and energy resulting in the lowest percent conversion to product.

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.

Ball milling is another technique which was reported very recently for the production of NFC. In this method, a cellulose suspension is placed in a hollow cylindrical container, partially filled with balls (e.g., ceramic, zirconia, or metal). While the container rotates, cellulose is disintegrated by the high energy collision between the balls. Zhang etal. [114] studied the process of NFC production from once-dried bleached softwood kraft pulp suspension at a solid concentration of 1wt% using ball milling. They showed the influence of the process conditions such as the ball size and ball-to-cellulose weight ratio on the morphology of the produced NFC. An average diameter of 100nm was reported for the disintegrated fibers. The control of the processing parameters was necessary to prevent cellulose decrystallization and to produce cellulose nanofibers rather than short particles.

Ball milling is one of the earliest approach for BNNTs synthesis [59]. The process involves extensive ball milling of boron powder for a long period of time (up to 150h) in NH3 gas followed by annealing at high temperature (up to 1300C) in N2 environment. It was suggested that a nitriding reaction was induced between boron powder and NH3 gas due to high energy milling, resulting in metastable disordered BN nanostructures and boron nanoparticles. BNNTs were grown from these reactive phase during a subsequent high-temperature annealing of the powder in ammonia ambient. It is proposed that BN nanoparticles formed during the milling process act as nucleation sites for growth during annealing process. Apart from them, contaminant Fe nanoparticles introduced during the milling process also served as catalyst for the growth. However, the quality and purity of BNNTs grown by ball milling was not satisfactory.

In the following years, various works have been done to increase the throughput and improve quality of BNNTs using ball-milling process. Li et. al. showed that addition of catalyst during the milling process can help to increase the production yield [60]. As an example, boron powder and 10% of Fe(NO3)3 was milled in NH3 atmosphere at 250 KPa pressure. Annealing the milled powder at N2+15% H2 gas environment at 1100C mostly resulted in bamboo-like BNNTs. Heating the same milled powder at 1300C in NH3 environment resulted in the growth of cylindrical BNNTs with diameters approximately 10nm. Other metal-based compounds such as nickel boride (NiBx) [61] and Li2O [62] are also reported as catalysts to enhance the yield of BNNTs growth. Though large quantity of BNNTs can be synthesized via this process, shortcoming was that the BNNTs are usually bamboo-like structured and contain B/BN reactants (amorphous boron particles and BN bulky flakes) as impurities.

ball mills - an overview | sciencedirect topics

ball mills - an overview | sciencedirect topics

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 [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.

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 [70]. 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 [71].

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 [11]. 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.[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.

In spite of the traditional approaches used for gas-solid reaction at relatively high temperature, Calka etal.[58] and El-Eskandarany etal.[59] 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.[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, 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,[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]

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 mill maintenance & installation procedure

ball mill maintenance & installation procedure

Am sure your BallMill is considered the finest possible grinding mill available. As such you will find it is designed and constructed according to heavy duty specifications. It is designed along sound engineering principles with quality workmanship and materials used in the construction of the component parts. YourBallMill reflects years of advancement in grinding principles, materials, and manufacturing techniques. It has been designed with both the operators and the erectors viewpoints in mind. Long uninterrupted performance can be expected from it if the instructions covering installation and maintenance of the mill are carried out. You may be familiar with installing mills of other designs and manufacture much lighter in construction. YourBallis heavy and rugged. It should, therefore, be treated accordingly with due respect for its heavier construction.

The purpose of this manual is to assist you in the proper installation and to acquaint you a bit further with the assembly and care of this equipment. We suggest that these instructions be read carefully and reviewed by everyone whenever involved in the actual installation and operation of the mill. In reading these general instructions, you may at times feel that they cover items which are elementary and perhaps not worthy of mention; however in studying hundreds of installations, it has been found that very often minor points are overlooked due to pressure being exerted by outside influences to get the job done in a hurry. The erection phase of this mill is actually no place to attempt cost savings by taking short cuts, or by-passing some of the work. A good installation will pay dividends for many years to come by reduced maintenance cost.With the modern practice of specialized skills and trades, there is often a line drawn between responsibilities of one crew of erectors and another. Actually the responsibility of installation does not cease with the completion of one phase nor does it begin with the starting of another. Perhaps a simple rule to adopt would be DO NOT TAKE ANYTHING FOR GRANTED. This policy of rechecking previously done work will help guarantee each step of the erection and it will carefully coordinate and tie it into subsequent erection work. To clarify or illustrate this point, take the example of concrete workers completing their job and turning it over to the machinist or millwright. The latter group should carefully check the foundation for soundness and correctness prior to starting their work.

Sound planning and good judgement will, to a great extent, be instrumental in avoiding many of the troublesome occurrences especially at the beginning of operations. While it is virtually impossible to anticipate every eventuality, nevertheless it is the intention of this manual to outline a general procedure to follow in erecting the mill, and at the same time, point out some of the pitfalls which should be avoided.

Before starting the erection of the mill, adequate handling facilities should be provided or made available, bearing in mind the weights and proportions of the various parts and sub-assemblies. This information can be ascertained from the drawings and shipping papers.

The gearing, bearings, and other machined surfaces have been coated with a protective compound, and should be cleaned thoroughly with a solvent, such as Chlorothene, (made by Dow Chemical). Judgement should be exercised as to the correct time and place for cleaning the various parts. Do not permit solvents, oil or grease to come in contact with the roughened top surfaces of the concrete foundation where grouting is to be applied; otherwise proper bonding will not result.

After cleaning the various parts, the gear and pinion teeth, trunnion journals and bearings, shafting and such, should be protected against rusting or pitting as well as against damage from falling objects or weld splatter. All burrs should be carefully removed by filing or honing.

Unless otherwise arranged for, the mill has been completely assembled in our shop. Before dismantling, the closely fitted parts were match marked, and it will greatly facilitate field assembly to adhere to these match marks.

The surfaces of all connecting joints or fits, such as shell and head flanges, trunnion flanges, trunnion liner and feeder connecting joints, should be coated with a NON-SETTING elastic compound, such as Quigley O-Seal, or Permatex to insure against leakage and to assist in drawing them up tight. DO NOT USE WHITE LEAD OR GREASE.

Parts which are affected by the hand of the mill are easily identified by referring to the parts list. In general they include the feeder, feed trunnion liner, discharge trunnion liner if it is equipped with a spiral, spiral type helical splitter, and in some cases the pan liners when they are of the spiral type. When both right and left hand mills are being assembled, it is imperative that these parts which involve hand be assembled in the correct mill.

Adequate foundations for any heavy equipment, and in particular grinding mills, are extremely important to assure proper operation. The foundation should preferably be in one piece, that is, with a reinforced slab footing (so called mat) extending under both trunnion bearing foundations as well as the pinion bearing foundation. If possible or practical, it should be extended to include also the motor and drive. With this design, in the event of some movement, the mill and foundation will tend to move as a unit. ANY SLIGHT SETTLING OF FOUNDATIONS WILL CAUSE BEARING AND GEAR MISALIGNMENT, resulting in excessive wear and higher maintenance costs. It has been found that concrete foundations on a weight basis should be at least 1 times the total weight of the grinding mill with its grinding media.

Allowable bearing pressure between concrete footings and the soil upon which the foundation rests should first be considered. The center of pressure must always pass through the center of the footing. Foundations subject to shock should be designed with less unit pressure than foundations for stationary loads. High moisture content in soils reduces the amount of allowable specific pressure that the ground can support. The following figures may be used for preliminary foundation calculations.

Portland cement mixed with sand and aggregate in the proper proportions has come to be standard practice in making concrete. For general reference cement is usually shipped in sacks containing one cubic foot of material. A barrel usually holds 4 cubic feet. Cement will deteriorate with age and will quickly absorb moisture so it should be stored in a dry place. For best results the sand and gravel used should be carefully cleaned free of humus, clay, vegetal matter, etc.

Concrete may be made up in different mixtures having different proportions of sand and aggregate. These are expressed in parts for example a 1:2:4 mixture indicates one bag of cement, 2 cubic feet of sand, and 4 cubic feet of gravel. We recommend a mixture of 1:2:3 for ball mill and rod mill foundations. The proper water to sand ratio should be carefully regulated since excess water increases the shrinkage in the concrete and lends to weaken it even more than a corresponding increase in the aggregate. Between 5 to 8 gallons of water to a sack of cement is usually recommended, the lower amount to be used where higher strength is required or where the concrete will be subject to severe weathering conditions.

Detailed dimensions for the concrete foundation are covered by the foundation plan drawing submitted separately. The drawing also carries special instructions as to the allowance for grouting, steel reinforcements, pier batter, foundation bolts and pipes. During concrete work, care should be taken to prevent concrete entering the pipes, surrounding the foundations bolts, which would limit the positioning of the bolts when erecting the various assemblies. Forms should be adequately constructed and reinforced to prevent swell, particularly where clearance is critical such as at the drive end where the gear should clear the trunnion bearing and pinion bearing piers.

For convenience in maintenance, the mill foundations should be equipped with jacking piers. These will allow the lifting of one end of the mill by use of jacks in the event maintenance must be carried out under these conditions.

Adequate foundations for any heavy equipment, and in particular Marcy grinding mills, are extremely important to assure proper operation of that equipment. Any slight settling of foundations will cause bearing and gear misalignment, resulting in excessive wear and higher maintenance costs. It has been found that concrete foundations on a weight basis should be approximately 1 times the total weight of the grinding mill with its grinding media.

Allowable bearing pressure between concrete footings and the soil upon which the foundation rests should first be considered. The center of pressure must always pass through the center of the footing. Foundations subject to shock should be designed with less unit pressures than foundations for stationary loads. High moisture content in soils reduces the amount of allowable pressure that that material can support. The following figures may be used for quick foundation calculations:

Portland cement mixed with sand and aggregate in the proper proportions has come to be standard practice in making concrete. For general reference cement is usually shipped in sacks containing one cubic foot of material. A barrel usually consists of 4 cubic feet. Cement will deteriorate with age and will quickly absorb moisture so it should be stored in a cool, dry place. The sand and gravel used should be carefully cleaned for best results to be sure of minimizing the amount of sedimentation in that material.

Concrete may be made up in different mixtures having different proportions of sand and aggregate. These are expressed in parts for example a 1:2:4 mixture indicates one bag of cement, 2 cubic feet of sand, and 4 cubic feet of gravel. We recommend a mixture of 1:2:3 for ball mill and rod mill foundations. The proper water to sand ratio should be carefully regulated since excess water will tend to weaken the concrete even more than corresponding variations in other material ratios. Between 5 to 8 gallons of water to a sack of cement is usually recommended, the lower amount to be used where higher strength is required or where the concrete will be subject to severe weathering conditions.

We recommend the use of a non-shrinking grout, and preferably of the pre-mixed type, such as Embeco, made by the Master Builders Company of Cleveland, Ohio. Thoroughly clean the top surfaces of the concrete piers, and comply with the instructions of the grouting supplier.

1. Establish vertical and horizontal centerline of mill and pinion shaftagainst the effects of this, we recommend that the trunnion bearing sole plate be crowned so as to be higher at the center line of the mill. This is done by using a higher shim at the center than at the endsand tightening the foundation bolts of both ends.

After all shimming is completed, the sole plate and bases should be grouted in position. Grouting should be well tamped and should completely fill the underside of the sole plate and bases. DO NOT REMOVE THE SHIMS AFTER OR DURING GROUTING. When the grout has hardened sufficiently it is advisable to paint the top surfaces of the concrete so as to protect it against disintegration due to the absorption of oil or grease.

If it is felt that sufficient accuracy in level between trunnion bearing piers cannot be maintained, we recommend that the grouting of the sole plate under the trunnion bearing opposite the gear end be delayed until after the mill is in place. In this way, the adjustment by shimming at this end can be made later to correct for any errors in elevation. Depending on local climatic conditions, two to seven days should he allowed for the grouting to dry and set, before painting or applying further loads to the piers.

Pinion bearings are provided of either the sleeve type or anti-friction type. Twin bearing construction may use either individual sole plates or a cast common sole plate. The unit with a common sole plate is completely assembled in our shop and is ready for installation. Normal inspection and cleaning procedure should be followed. Refer to the parts list for general assembly. These units are to be permanently grouted in position and, therefore, care should be taken to assure correct alignment.

The trunnion bearing assemblies can now be mounted on their sole plates. If the bearings are of the swivel type, a heavy industrial water-proof grease should be applied to the spherical surfaces of both the swivels and the bases. Move the trunnion bearings to their approximate position by adjustment of the set screws provided for this purpose.

In the case of ball mills, all internal wearing parts will pass through the manhole, whereas in the case of open end rod mills they will pass through the discharge trunnion opening. When lining the shell, start with the odd shaped pieces around the manhole opening if manholes are furnished. Rubber shell liner backing should be used with all cast type rod mills shell liners. If the shell liners are of the step type, they should be assembled with the thin portion, or toe, as the leading edge with respect to rotation of the mill.

Lorain liners for the shell are provided with special round head bolts, with a waterproof washer and nut. All other cast type liners for the head and shell are provided with oval head bolts with a cut washer and nuts. Except when water proof washers are used, it is advisable to wrap four or five turns of candle wicking around the shank of the bolt under the cut washer. Dip the candle wicking in white lead. All liner bolt threads should be dipped in graphite and oil before assembly. All liner bolt cuts should be firmly tightened by use of a pipe extension on a wrench, or better yet, by use of a torque wrench. The bolt heads should be driven firmly into the bolt holes with a hammer.

In order to minimise the effect of pulp race, we recommend that the spaces between the ends of the shell liners and the head liners or grates be filled with suitable packing. This packing may be in the form of rubber belting, hose, rope or wood.

If adequate overhead crane facilities are available, the heads can be assembled to the shell with the flange connecting bolts drawn tightly. Furthermore, the liners can be in place, as stated above, and the gear can be mounted, as covered by separate instructions. Then the mill can be taken to its location and set in place in the trunnion bearings.

If on the other hand the handling facilities are limited it is recommended that the bare shell and heads be assembled together in a slightly higher position than normal. After the flange bolts are tightened, the mill proper should be lowered into position. Other intermediate methods may be used, depending on local conditions.

In any event, just prior to the lowering of the mill into the bearings the trunnion journal and bushing and bases should be thoroughly cleaned and greased. Care should be taken not to foul the teeth in the gear or pinion. Trunnion bearing caps should be immediately installed, although not necessarily tightened, to prevent dirt settling on the trunnions. The gear should be at least tentatively covered for protection.

IMPORTANT. Unless the millwright or operator is familiar with this type of seal, there is a tendency to assume that the oil seal is too long because of its appearance when held firmly around the trunnion. It is not the function of the brass oil seal band to provide tension for effective sealing. This is accomplished by the garter spring which is provided with the oil seal.

Assemble the oil seal with the spring in place, and with the split at the top. Encircle the oil seal with the band, keeping the blocks on the side of the bearing at or near the horizontal center line so that when in place they will fit between the two dowel pins on the bearing, which are used to prevent rotation of the seal.

Moderately tighten up the cap screws at the blocks, pulling them together to thus hold the seal with its spring in place. If the blocks cannot be pulled snuggly together, then the oil seal may be cut accordingly. Oil the trunnion surface and slide the entire seal assembly back into place against the shoulder of the bearing and finish tightening. Install the retainer ring and splash ring as shown.

In most cases the trunnion liners are already mounted in the trunnions of the mills. If not, they should be assembled with attention being given to match marks or in some cases to dowel pins which are used to locate the trunnion liners in their proper relation to other parts.

If a scoop feeder, combination drum scoop feeder or drum feeder is supplied with the mill, it should be mounted on the extended flange of the feed trunnion liner, matching the dowel pin with its respective hole. The dowel pin arrangement is provided only where there is a spiral in the feed trunnion liner. This matching is important as it fixes the relationship between the discharge from the scoop and the internal spiral of the trunnion liner. Tighten the bolts attaching the feeder to the trunnion liner evenly, all around the circle, seating the feeder tightly and squarely on its bevelled seat. Check the bolts holding the lips and other bolts that may require tightening. The beveled seat design is used primarily where a feeder is provided for the trunnion to trunnion liner connection, and the trunnion liner to feeder connection. When a feeder is not used these connecting joints are usually provided by a simple cylindrical or male and female joint.

If a spout feeder is to be used, it is generally supplied by the user, and should be mounted independently of the mill. The spout should project inside the feed trunnion liner, but must not touch the liner or spiral.

Ordinarily the feed box for a scoop tender is designed and supplied by the user. The feed box should be so constructed that it has at least 6 clearance on both sides and at the bottom of the scoop. This clearance is measured from the outside of the feed scoop.

The feed box may be constructed of 2 wood, but more often is made of 3/16 or plate steel reinforced with angles. In the larger size mills, the lower portion is sometimes made of concrete. Necessary openings should be provided for the original feed and the sand returns from the classifiers when in closed circuit.

A plate steel gear guard is furnished with the mill for safety in operation and to protect the gear and pinion from dirt or grit. As soon as the gear and pinion have been cleaned and coated with the proper lubricant, the gear guard should be assembled and set on its foundation.

Most Rod Mills are provided with a discharge housing mechanism mounted independently of the mill. This unit consists of the housing proper, plug door, plug shaft, arm, and various hinge pins and pivot and lock pins. The door mechanism is extra heavy throughout and is subject to adjustment as regard location. Place the housing proper on the foundation, level with steel shims and tighten the foundation bolts. The various parts may now be assembled to the housing proper and the door plug can be swung into place, securing it with the necessary lock pins.

After the mill has been completely assembled and aligned, the door mechanism centered and adjusted, and all clearances checked, the housing base can be grouted. The unit should be so located both vertically and horizontally so as to provide a uniform annular opening between the discharge plug door and the head liners.

In some cases because of space limitation, economy reasons, etc., the mill is not equipped with separate discharge housing. In such a case, the open end low discharge principal is accomplished by means of the same size opening through the discharge trunnion but with the plug door attached to lugs on the head liner segments or lugs on the discharge trunnion liner proper. In still other cases, it is sometimes effected by means of an arm holding the plug and mounted on a cross member which is attached to the bell of the discharge trunnion liner. In such cases as those, a light weight sheet steel discharge housing is supplied by the user to accommodate the local plant layout in conjunction with the discharge launder.

TRUNNION BEARING LUBRICATION. For the larger mills with trunnion bearings provided with oil seals, we recommend flood oil lubrication. This can be accomplished by a centralized system for two or more mills, or by an individual system for each mill. We recommend the individual system for each mill, except where six or more mills are involved, or when economy reasons may dictate otherwise.

In any event oil flow to each trunnion bearing should be between 3 to 5 gallons per minute. The oil should be adequately filtered and heaters may be used to maintain a temperature which will provide proper filtration and maintain the necessary viscosity for adequate flow. The lines leading from the filter to the bearing should be of copper tubing or pickled piping. The drain line leading from the bearings to the storage or sump tank should be of adequate size for proper flow, and they should be set at a minimum slope of per foot, perferably per foot. Avoid unnecessary elbows and fittings wherever possible. Avoid bends which create traps and which might accumulate impurities. All lines should be thoroughly cleaned and flushed with a solvent, and then blown free with air, before oil is added.

It is advisable to interlock the oil pump motor with the mill motor in such a way that the mill cannot be started until after the oil pump is operating. We recommend the use of a non-adjuslable valve at each bearing to prevent tampering.

When using the drip oil system it is advisable to place wool yarn or waste inside a canvas porous bag to prevent small pieces of the wool being drawn down into the trunnion journal. If brick grease is used, care should be taken in its selection with regard to the range of its effective temperature. In other words, it should be pointed out that brick grease is generally designed for a specific temperature range. Where the bearing temperature does not come up to the minimum temperature rating of the brick grease, the oil will not flow from it, and on the other hand if the temperature of the bearing exceeds the maximum temperature rating of the brick grease, the brick is subject to glazing; therefore, blinding off of the oil. This brick should be trimmed so that it rests freely on the trunnion journal, and does not hang up, or bind on the sides of the grease box.

When replacing the brick grease, remove the old grease completely. Due to the extended running time of brick grease, there is usually an accumulation of impurities and foreign matter on the top surface, which is detrimental to the bearing.

Where anti-friction bearings are supplied, they are adequately sealed for either grease or oil lubrication. If a flood system is used for the trunnion bearings and it is adequately filtered, it can then be used for pinion bearings with the same precautions taken as mentioned above, with a flow of to 1 gallons per minute to each bearing.

These lubricants can be applied by hand, but we highly recommend some type of spray system, whether it be automatic, semi-automatic or manually operated. It has been found that it is best to lubricate gears frequently with small quantities.

Start the lubrication system and run it for about ten minutes, adjusting the oil flow at each bearing. Check all of the bolts and nuts on the mill for tightness and remove all ladders, tools and other obstructions prior to starting the mill.

Before starting the mill, even though it is empty, we recommend that it be jogged one or two revolutions for a check as to clearance of the gear and its guard, splash rings, etc. The trunnion journal should also be checked for uniform oil film and for any evidence of foreign material which might manifest itself through the appearance of scratches on the journal. If there are any scratches, it is very possible that some foreign material such as weld splatter may have been drawn down into the bushing, and can be found imbedded there. These particles should be removed before proceeding further.

If everything is found to be satisfactory, then the mill should be run for ten to fifteen minutes, and stopped. The trunnion bearings should be checked for any undue temperature and the gear grease pattern can be observed for uniformity which would indicate correct alignment.

It should be noted that with an empty mill the reactions and operating characteristics of the bearings and gearing at this point are somewhat different than when operating with a ball or rod charge. Gear noises will be prominent and some vibration will occur due to no load and normal back-lash. Furthermore, it will be found that the mill will continue to rotate for some time after the power is shut off. Safety precautions should therefore he observed, and no work should be done on the mill until it has come to a complete stop.

We have now reached the point where a half ball or rod charge can be added, and the mill run for another six to eight hours, feeding approximately half the anticipated tonnage. The mill should now be stopped, end the gear grease pattern checked, and gear and pinion mesh corrected, if necessary, according to separate instructions.

The full charge of balls or rods can now be added, as well as the full amount of feed, and after a run of about four to six days, ALL BOLTS SHOULD AGAIN BE RETIGHTENED, and the gear and pinion checked again, and adjusted if necessary.

Where starting jacks are provided for the trunnion bearings of the larger sized mills, they should be filled with the same oil that is used for the lubrication of the trunnion bearings. Before starting the mill they should be pumped so as to insure having an oil film between the journal and the bushing.

When relining any part of the mill, clean away all sand from the parts to be relined before putting in the new liners. For the head liners and shell liners you may then proceed in the same manner used at the time of the initial assembly.

Before relining the grate type discharge head, it is advisable to refer to the assembly drawings and the parts list.Because of such limitations as the size of the manhole opening, and for various other reasons, it will be found that the center discharge liner and cone designs vary. The cone may be a separate piece or integral with either the trunnion liner, or the router discharge liner. Furthermore, it will be found in some mills that the center discharge liner is held by bolts through the discharge head, whereas in other cases it depends upon the clamping effect of grates to hold it in position. In any event, the primary thing to remember in assembling the discharge grate head parts is the fact that the grate should be first drawn up tightly towards the center discharge liner by adjusting the grate set screws located at the periphery of the discharge head. This adjustment should be carried out in progressive steps, alternating at about 180 if possible and in such a manner that, the center discharge liner does not become dislodged from its proper position at the center of the mill. These grate set screws should be adjusted with the side clamp bar bolts loosened. After the grates have been completely tightened with the set screws, check for correct and uniform position of each grate section. The side clamp bar bolts may now be lightened, again using an alternate process. This should result in the side clamp bars firmly bearing against the beveled sides of the grates. The side clamp bars should not hear against the lifter liners.

When new pan liners are installed, they should be grouted in position so as to prevent pulp race in the void space between the discharge head and the pan liner. Another good method of preventing this pulp race is the use of the sponge rubber which can be cemented in place.

After the mill is erected, in order to avoid overlooking both obvious and obscure installation details, we recommend the use of a check list. This is particularly recommended for multiple mill installations where it is difficult to control the different phases of installation for each and every mill. Such a check list can be modeled after the following:

No. 1 Connecting Bolts drawn tight. A. Head and Shell flange bolts. B. Gear Connecting, bolts. No. 2 Trunnion studs or bolts drawn up tight. No. 3 Trunnion liner and feeder connecting bolts or studs drawn up tight. No. 4 Feeder lip bolts tightened. No. 5 Liner bolts drawn up tight. No. 6 Gear. A. Concentric B. Backlash C. Runout D. Joint bolts drawn up tight. No. 7 Coupling and Drive alignment and lubrication. No. 8 Bearings and Gearing cleaned and lubricated. No. 9 Lubrication system in working order with automatic devices including alarms and interlocking systems.

We further recommend that during the first thirty to sixty days of operation, particular attention be given to bolt tightness, foundation settlement and condition of the grouting. We suggest any unusual occurrence be recorded so that should trouble develop later there may be a clue which would simplify diagnosing and rectifying the situation.

As a safety precaution, and in many cases in order to comply with local safety regulations, guards should be used to protect the operators and mechanics from contact with moving parts. However, these guards should not be of such a design that will prevent or hinder the close inspection of the vital parts. Frequent inspection should be made at regular intervals with particular attention being given to the condition of the wearing parts in the mill. In this way, you will be better able to anticipate your needs for liners and other parts in time to comply with the current delivery schedules.

When ordering repair or replacement parts for your mill, be sure to identify the parts with the number and description as shown on the repair parts list, and specify the hand and serial number of the mill.

By following the instructions outlined in this manual, mechanical malfunctions will be eliminated. However, inadvertent errors may occur even under, the most careful supervision. With this in mind, it is possible that some difficulties may arise. Whenever any abnormal mechanical reactions are found, invariably they can be attributed to causes which though sometimes obvious are often hidden. We sight herewith the most common problems, with their solutions.

Cause A GROUT DISINTEGRATION. Very often when the grouting is not up to specification the vibration from the mill tends to disintegrate the grouting. In most instances the disintegration starts between the sole plate and the top surface of the grouting near or at the vertical centerline of the mill. As this continues, the weight of the mill causes the sole plate and trunnion bearing base to bend with a resultant pinching action at the side of the bearing near the horizontal center line of the mill. This pinching will cut off and wipe the oil film from the journal and will manifest itself in the same manner as if the lubrication supply had been cut off. If the grout disintegration is limited to about . 050 and does not appear to be progressing further, the situation can be corrected by applying a corresponding amount of shimming between the trunnion bearing base and the sole plate near the centerline of the mill in such a fashion that the trunnion bearing base has been returned to its normal dimensional position. If, on the other hand, the grouting is in excess of . 050 and appears to be progressing further, it is advisable to shut down operations until the sole plate has been re grouted.

Cause B HIGH SPOT ON THE BUSHING. While all BallMill bushings are scraped in the shop to fit either a jig mandrel or the head proper to which it is to be fitted, nevertheless there is a certain amount of seasoning and dimensional change which goes on in the type of metals used. Therefore if high spots are found, the mill should be raised, the bushings removed and rescraped. Bluing may be used to assist in detecting high spots.

Cause C INSUFFICIENT OIL FLOW. Increase the oil supply if it is a flood oil system. If brick grease is used, it is possible that the particular grade of brick may not be applicable to the actual bearing temperature. Refer to the remarks in this manual under the paragraph entitled Lubrication.

Cause E EXCESSIVE RUBBING ON THE SIDE OF THE BUSHING. This comes about due to the improper setting of the bearings in the longitudinal plane. In some cases, particularly on dry grinding or hot clinker grinding mills, the expansion of the mills proper may account for this condition. In any event, it can be remedied by re-adjusting the bearing base on the sole plate longitudinally at the end opposite the drive.

There are many more lubricant suppliers, such as E. F. Houghton and Co. , or Lubriplate Division of Fiske Bros. Refining Co. In making your final selection of lubricants, you should consider the actual plant conditions as well as the standardization of lubricants. New and improved lubricants are being marketed, and we, therefore, suggest that you consult your local suppliers.

ball mill - an overview | sciencedirect topics

ball mill - an overview | sciencedirect topics

The ball mill accepts the SAG or AG mill product. Ball mills give a controlled final grind and produce flotation feed of a uniform size. Ball mills tumble iron or steel balls with the ore. The balls are initially 510 cm diameter but gradually wear away as grinding of the ore proceeds. The feed to ball mills (dry basis) is typically 75 vol.-% ore and 25% steel.

The ball mill is operated in closed circuit with a particle-size measurement device and size-control cyclones. The cyclones send correct-size material on to flotation and direct oversize material back to the ball mill for further grinding.

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.

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).

Planetary ball mills. A planetary ball mill consists of at least one grinding jar, which is arranged eccentrically on a so-called sun wheel. The direction of movement of the sun wheel is opposite to that of the grinding jars according to a fixed ratio. The grinding balls in the grinding jars are subjected to superimposed rotational movements. The jars are moved around their own axis and, in the opposite direction, around the axis of the sun wheel at uniform speed and uniform rotation ratios. The result is that the superimposition of the centrifugal forces changes constantly (Coriolis motion). The grinding balls describe a semicircular movement, separate from the inside wall, and collide with the opposite surface at high impact energy. The difference in speeds produces an interaction between frictional and impact forces, which releases high dynamic energies. The interplay between these forces produces the high and very effective degree of size reduction of the planetary ball mill. Planetary ball mills are smaller than common ball mills, and are mainly used in laboratories for grinding sample material down to very small sizes.

Vibration mill. Twin- and three-tube vibrating mills are driven by an unbalanced drive. The entire filling of the grinding cylinders, which comprises the grinding media and the feed material, constantly receives impulses from the circular vibrations in the body of the mill. The grinding action itself is produced by the rotation of the grinding media in the opposite direction to the driving rotation and by continuous head-on collisions of the grinding media. The residence time of the material contained in the grinding cylinders is determined by the quantity of the flowing material. The residence time can also be influenced by using damming devices. The sample passes through the grinding cylinders in a helical curve and slides down from the inflow to the outflow. The high degree of fineness achieved is the result of this long grinding procedure. Continuous feeding is carried out by vibrating feeders, rotary valves, or conveyor screws. The product is subsequently conveyed either pneumatically or mechanically. They are basically used to homogenize food and feed.

CryoGrinder. As small samples (100 mg or <20 ml) are difficult to recover from a standard mortar and pestle, the CryoGrinder serves as an alternative. The CryoGrinder is a miniature mortar shaped as a small well and a tightly fitting pestle. The CryoGrinder is prechilled, then samples are added to the well and ground by a handheld cordless screwdriver. The homogenization and collection of the sample is highly efficient. In environmental analysis, this system is used when very small samples are available, such as small organisms or organs (brains, hepatopancreas, etc.).

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.[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.

A ball mill is a relatively simple apparatus in which the motion of the reactor, or of a part of it, induces a series of collisions of balls with each other and with the reactor walls (Suryanarayana, 2001). At each collision, a fraction of the powder inside the reactor is trapped between the colliding surfaces of the milling tools and submitted to a mechanical load at relatively high strain rates (Suryanarayana, 2001). This load generates a local nonhydrostatic mechanical stress at every point of contact between any pair of powder particles. The specific features of the deformation processes induced by these stresses depend on the intensity of the mechanical stresses themselves, on the details of the powder particle arrangement, that is on the topology of the contact network, and on the physical and chemical properties of powders (Martin et al., 2003; Delogu, 2008a). At the end of any given collision event, the powder that has been trapped is remixed with the powder that has not undergone this process. Correspondingly, at any instant in the mechanical processing, the whole powder charge includes fractions of powder that have undergone a different number of collisions.

The individual reactive processes at the perturbed interface between metallic elements are expected to occur on timescales that are, at most, comparable with the collision duration (Hammerberg et al., 1998; Urakaev and Boldyrev, 2000; Lund and Schuh, 2003; Delogu and Cocco, 2005a,b). Therefore, unless the ball mill is characterized by unusually high rates of powder mixing and frequency of collisions, reactive events initiated by local deformation processes at a given collision are not affected by a successive collision. Indeed, the time interval between successive collisions is significantly longer than the time period required by local structural perturbations for full relaxation (Hammerberg et al., 1998; Urakaev and Boldyrev, 2000; Lund and Schuh, 2003; Delogu and Cocco, 2005a,b).

These few considerations suffice to point out the two fundamental features of powder processing by ball milling, which in turn govern the MA processes in ball mills. First, mechanical processing by ball milling is a discrete processing method. Second, it has statistical character. All of this has important consequences for the study of the kinetics of MA processes. The fact that local deformation events are connected to individual collisions suggests that absolute time is not an appropriate reference quantity to describe mechanically induced phase transformations. Such a description should rather be made as a function of the number of collisions (Delogu et al., 2004). A satisfactory description of the MA kinetics must also account for the intrinsic statistical character of powder processing by ball milling. The amount of powder trapped in any given collision, at the end of collision is indeed substantially remixed with the other powder in the reactor. It follows that the same amount, or a fraction of it, could at least in principle be trapped again in the successive collision.

This is undoubtedly a difficult aspect to take into account in a mathematical description of MA kinetics. There are at least two extreme cases to consider. On the one hand, it could be assumed that the powder trapped in a given collision cannot be trapped in the successive one. On the other, it could be assumed that powder mixing is ideal and that the amount of powder trapped at a given collision has the same probability of being processed in the successive collision. Both these cases allow the development of a mathematical model able to describe the relationship between apparent kinetics and individual collision events. However, the latter assumption seems to be more reliable than the former one, at least for commercial mills characterized by relatively complex displacement in the reactor (Manai et al., 2001, 2004).

A further obvious condition for the successful development of a mathematical description of MA processes is the one related to the uniformity of collision regimes. More specifically, it is highly desirable that the powders trapped at impact always experience the same conditions. This requires the control of the ball dynamics inside the reactor, which can be approximately obtained by using a single milling ball and an amount of powder large enough to assure inelastic impact conditions (Manai et al., 2001, 2004; Delogu et al., 2004). In fact, the use of a single milling ball avoids impacts between balls, which have a remarkable disordering effect on the ball dynamics, whereas inelastic impact conditions permit the establishment of regular and periodic ball dynamics (Manai et al., 2001, 2004; Delogu et al., 2004).

All of the above assumptions and observations represent the basis and guidelines for the development of the mathematical model briefly outlined in the following. It has been successfully applied to the case of a Spex Mixer/ Mill mod. 8000, but the same approach can, in principle, be used for other ball mills.

The Planetary ball mills are the most popular mills used in MM, MA, and MD scientific researches for synthesizing almost all of the materials presented in Figure 1.1. In this type of mill, the milling media have considerably high energy, because milling stock and balls come off the inner wall of the vial (milling bowl or 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, as schematically presented in Figure 2.17.

However, there are some companies in the world who manufacture and sell number of planetary-type ball mills; Fritsch GmbH (www.fritsch-milling.com) and Retsch (http://www.retsch.com) are considered to be the oldest and principal companies in this area.

Fritsch produces different types of planetary ball mills with different capacities and rotation speeds. Perhaps, Fritsch Pulverisette P5 (Figure 2.18(a)) and Fritsch Pulverisette P6 (Figure 2.18(b)) are the most popular models of Fritsch planetary ball mills. A variety of vials and balls made of different materials with different capacities, starting from 80ml up to 500ml, are available for the Fritsch Pulverisette planetary ball mills; these include tempered steel, stainless steel, tungsten carbide, agate, sintered corundum, silicon nitride, and zirconium oxide. Figure 2.19 presents 80ml-tempered steel vial (a) and 500ml-agate vials (b) together with their milling media that are made of the same materials.

Figure 2.18. Photographs of Fritsch planetary-type high-energy ball mill of (a) Pulverisette P5 and (b) Pulverisette P6. The equipment is housed in the Nanotechnology Laboratory, Energy and Building Research Center (EBRC), Kuwait Institute for Scientific Research (KISR).

Figure 2.19. Photographs of the vials used for Fritsch planetary ball mills with capacity of (a) 80ml and (b) 500ml. The vials and the balls shown in (a) and (b) are made of tempered steel agate materials, respectively (Nanotechnology Laboratory, Energy and Building Research Center (EBRC), Kuwait Institute for Scientific Research (KISR)).

More recently and in year 2011, Fritsch GmbH (http://www.fritsch-milling.com) introduced a new high-speed and versatile planetary ball mill called Planetary Micro Mill PULVERISETTE 7 (Figure 2.20). The company claims this new ball mill will be helpful to enable extreme high-energy ball milling at rotational speed reaching to 1,100rpm. This allows the new mill to achieve sensational centrifugal accelerations up to 95 times Earth gravity. They also mentioned that the energy application resulted from this new machine is about 150% greater than the classic planetary mills. Accordingly, it is expected that this new milling machine will enable the researchers to get their milled powders in short ball-milling time with fine powder particle sizes that can reach to be less than 1m in diameter. The vials available for this new type of mill have sizes of 20, 45, and 80ml. Both the vials and balls can be made of the same materials, which are used in the manufacture of large vials used for the classic Fritsch planetary ball mills, as shown in the previous text.

Retsch has also produced a number of capable high-energy planetary ball mills with different capacities (http://www.retsch.com/products/milling/planetary-ball-mills/); namely Planetary Ball Mill PM 100 (Figure 2.21(a)), Planetary Ball Mill PM 100 CM, Planetary Ball Mill PM 200, and Planetary Ball Mill PM 400 (Figure 2.21(b)). Like Fritsch, Retsch offers high-quality ball-milling vials with different capacities (12, 25, 50, 50, 125, 250, and 500ml) and balls of different diameters (540mm), as exemplified in Figure 2.22. These milling tools can be made of hardened steel as well as other different materials such as carbides, nitrides, and oxides.

Figure 2.21. Photographs of Retsch planetary-type high-energy ball mill of (a) PM 100 and (b) PM 400. The equipment is housed in the Nanotechnology Laboratory, Energy and Building Research Center (EBRC), Kuwait Institute for Scientific Research (KISR).

Figure 2.22. Photographs of the vials used for Retsch planetary ball mills with capacity of (a) 80ml, (b) 250ml, and (c) 500ml. The vials and the balls shown are made of tempered steel (Nanotechnology Laboratory, Energy and Building Research Center (EBRC), Kuwait Institute for Scientific Research (KISR)).

Both Fritsch and Retsch companies have offered special types of vials that allow monitoring and measure the gas pressure and temperature inside the vial during the high-energy planetary ball-milling process. Moreover, these vials allow milling the powders under inert (e.g., argon or helium) or reactive gas (e.g., hydrogen or nitrogen) with a maximum gas pressure of 500kPa (5bar). It is worth mentioning here that such a development made on the vials design allows the users and researchers to monitor the progress tackled during the MA and MD processes by following up the phase transformations and heat realizing upon RBM, where the interaction of the gas used with the freshly created surfaces of the powders during milling (adsorption, absorption, desorption, and decomposition) can be monitored. Furthermore, the data of the temperature and pressure driven upon using this system is very helpful when the ball mills are used for the formation of stable (e.g., intermetallic compounds) and metastable (e.g., amorphous and nanocrystalline materials) phases. In addition, measuring the vial temperature during blank (without samples) high-energy ball mill can be used as an indication to realize the effects of friction, impact, and conversion processes.

More recently, Evico-magnetics (www.evico-magnetics.de) has manufactured an extraordinary high-pressure milling vial with gas-temperature-monitoring (GTM) system. Likewise both system produced by Fritsch and Retsch, the developed system produced by Evico-magnetics, allowing RBM but at very high gas pressure that can reach to 15,000kPa (150bar). In addition, it allows in situ monitoring of temperature and of pressure by incorporating GTM. The vials, which can be used with any planetary mills, are made of hardened steel with capacity up to 220ml. The manufacturer offers also two-channel system for simultaneous use of two milling vials.

Using different ball mills as examples, it has been shown that, on the basis of the theory of glancing collision of rigid bodies, the theoretical calculation of tPT conditions and the kinetics of mechanochemical processes are possible for the reactors that are intended to perform different physicochemical processes during mechanical treatment of solids. According to the calculations, the physicochemical effect of mechanochemical reactors is due to short-time impulses of pressure (P = ~ 10101011 dyn cm2) with shift, and temperature T(x, t). The highest temperature impulse T ~ 103 K are caused by the dry friction phenomenon.

Typical spatial and time parameters of the impactfriction interaction of the particles with a size R ~ 104 cm are as follows: localization region, x ~ 106 cm; time, t ~ 108 s. On the basis of the obtained theoretical results, the effect of short-time contact fusion of particles treated in various comminuting devices can play a key role in the mechanism of activation and chemical reactions for wide range of mechanochemical processes. This role involves several aspects, that is, the very fact of contact fusion transforms the solid phase process onto another qualitative level, judging from the mass transfer coefficients. The spatial and time characteristics of the fused zone are such that quenching of non-equilibrium defects and intermediate products of chemical reactions occurs; solidification of the fused zone near the contact point results in the formation of a nanocrystal or nanoamor- phous state. The calculation models considered above and the kinetic equations obtained using them allow quantitative ab initio estimates of rate constants to be performed for any specific processes of mechanical activation and chemical transformation of the substances in ball mills.

There are two classes of ball mills: planetary and mixer (also called swing) mill. The terms high-speed vibration milling (HSVM), high-speed ball milling (HSBM), and planetary ball mill (PBM) are often used. The commercial apparatus are PBMs Fritsch P-5 and Fritsch Pulverisettes 6 and 7 classic line, the Retsch shaker (or mixer) mills ZM1, MM200, MM400, AS200, the Spex 8000, 6750 freezer/mill SPEX CertiPrep, and the SWH-0.4 vibrational ball mill. In some instances temperature controlled apparatus were used (58MI1); freezer/mills were used in some rare cases (13MOP1824).

The balls are made of stainless steel, agate (SiO2), zirconium oxide (ZrO2), or silicon nitride (Si3N). The use of stainless steel will contaminate the samples with steel particles and this is a problem both for solid-state NMR and for drug purity.

However, there are many types of ball mills (see Chapter 2 for more details), such as drum ball mills, jet ball mills, bead-mills, roller ball mills, vibration ball mills, and planetary ball mills, they can be grouped or classified into two types according to their rotation speed, as follows: (i) high-energy ball mills and (ii) low-energy ball mills. Table 3.1 presents characteristics and comparison between three types of ball mills (attritors, vibratory mills, planetary ball mills and roller mills) that are intensively used on MA, MD, and MM techniques.

In fact, choosing the right ball mill depends on the objectives of the process and the sort of materials (hard, brittle, ductile, etc.) that will be subjecting to the ball-milling process. For example, the characteristics and properties of those ball mills used for reduction in the particle size of the starting materials via top-down approach, or so-called mechanical milling (MM process), or for mechanically induced solid-state mixing for fabrications of composite and nanocomposite powders may differ widely from those mills used for achieving mechanically induced solid-state reaction (MISSR) between the starting reactant materials of elemental powders (MA process), or for tackling dramatic phase transformation changes on the structure of the starting materials (MD). Most of the ball mills in the market can be employed for different purposes and for preparing of wide range of new materials.

Martinez-Sanchez et al. [4] have pointed out that employing of high-energy ball mills not only contaminates the milled amorphous powders with significant volume fractions of impurities that come from milling media that move at high velocity, but it also affects the stability and crystallization properties of the formed amorphous phase. They have proved that the properties of the formed amorphous phase (Mo53Ni47) powder depends on the type of the ball-mill equipment (SPEX 8000D Mixer/Mill and Zoz Simoloter mill) used in their important investigations. This was indicated by the high contamination content of oxygen on the amorphous powders prepared by SPEX 8000D Mixer/Mill, when compared with the corresponding amorphous powders prepared by Zoz Simoloter mill. Accordingly, they have attributed the poor stabilities, indexed by the crystallization temperature of the amorphous phase formed by SPEX 8000D Mixer/Mill to the presence of foreign matter (impurities).

ball mill operation -grinding circuit startup & shutdown procedure

ball mill operation -grinding circuit startup & shutdown procedure

After the grinding circuit has been brought up to normal operating conditions, the operator must monitor the various process variables and alarms. Most of these variables are monitored in the mill control room, however, the operator is also required to sample and analyse process streams and read local indicators.

The ball mill is susceptible to variations in ore hardness resulting in various grinds at constant throughput, or alternatively, various tonnages at constant grind. The variation in grind is not directly determined. However, a changing cyclone overflow density, at a constant tonnage rate and feed density, would be indicative of changing ore hardness and in that case the tonnage fed to the ball mill should be changed accordingly.

The ore feed rate to the ball mill is controlled by the weightometer located on the mill feed conveyor which can be manually adjusted with in the control room to give a constant weight reading. The signal from the weightometer increases or decreases the belt feeder speed and adjusts the water addition to the ball mill (as a function of the actual weight reading). Both weight control and the proportion of water can be adjusted in the control room.

The water rationing controller must be adjusted programmatically to give the desired ball mill discharge density (normally 60-65% solids). The ball mill discharge density should be checked manually at regular intervals and adjustment made to water ratio controller setpoint to adjust the ball mill discharge density.

The grinding circuit operator must ensure that the ball mill runs properly loaded and gives the correct ore grind. A major practical indication of mill loading is the sound made by the mill. A properly loaded mill will have a deep rhythmic roar, while an under loaded mill will have a metallic rattling type noise and an overloaded mill will be quite silent.

The operator must manually measure the cyclone overflow and underflow densities regularly. An increase in overflowdensity is indicative of softer ore and will soon be accompanied by a lowering of power draw at the mill and a change of sound indicating that the mill is becoming under loaded. To compensate, feed tonnage must be increased. Similarity, a decrease in the cyclone overflow density is indicative of harder ore and this will be accompanied eventually by a coking of the mill. Feed to the ball mill must be reduced.

In the event of an emergency, the mill feed conveyor is shut down individually or by stopping the operating cyclone feed pump. The ball mill must be shut down separately. All equipmentshutdowns are performed locally or from the MCC located in the mill control room.

condition monitoring of ball mill with hd technologies - cbm connect

condition monitoring of ball mill with hd technologies - cbm connect

Orcem in the Netherlands manufactures a special concrete called ECO2cem. One of the advantages of ECO2cem is that during the production process less CO2 is produced, making ECO2cem a very environment-friendly product. Orcem has two production plants, one in the Netherlands and one in Ireland (Ecocem). Both plants have used the VCM system from SPM Instrument for years with the LR/HR and dBm/dBc techniques; however, Orcem and Ecocem were both very interested in the new SPM HD technology. After long discussions, both plants decided to switch from the VCM system to the newer Intellinova system and with fabulous results, which are highlighted in chapter 2. To produce ECO2cem, Orcem uses furnace slag. This slag is a waste product of a steel mill. Iron ore, calcium, and cokes are melted in a blast furnace at 1500C, producing a liquid cast iron. Due to the low density of the non-iron parts, called furnace slag, the slag floats to the surface and is used for the production of the ECO2cem consisting of mainly calcium, aluminum and silicon.

During the period from May 2014 until September 2014, a serious problem was detected well before any serious consequences occurred. Readings from the input shaft of the gearbox showed a clear bearing damage. Approximately three months before the alarm, SPM HD measurements indicated this bearing failure. After this initial bearing problem, another problem evolved on the output shaft and the decision was made to replace the complete gearbox with a renovated one. The gearbox was replaced on the 5th of June, resulting in green condition evaluation for all measuring points again. Yet another problem caught was a fan bearing that needed to be replaced because it had been damaged during installation. Since the previous online system (VCM) was replaced with the Intellinova series of online systems, the SPM HD measuring technique has proven able to measure bearing damages with exceptional prewarning times, giving the customer the opportunity to plan for repair/exchange of the defective machinery and the ability to check the quality of maintenance work done by contractors. For more information about the different cases, please refer to chapter 5.

There are many different types of mills; ball mills, rod mills, SAG (Semi-Autogenous Grinding) and autogenous mills. In a ball mill, steel or stone balls are mixed with the ore and during rotation of the drum the ore is ground, by friction and compression, into a suitable fineness for the next step in the process. The main component of all mills is a rotating drum, turning with a suitable speed, gearbox, and motor. The mill is a very important part of the milling process in the cement industry. In many cases, the entire process can be severely limited or completely stopped if the mill ceases to operate and close observation of mill equipment condition is therefore essential. An unplanned stop must be avoided at almost any cost. Many years ago, SPM Instrument installed a VCM system on the mill gearbox and motor.

Besides the gearbox, the electric motor and the support bearings of the girth wheel are equipped with shock pulse and vibration transducers. Other applications monitored are a fan and a wind sifter. In total, sixteen shock pulse transducers and eight vibration transducers are connected to an Intellinova standard system. Shock pulse transducers are installed on all bearing positions. Vibration transducers are installed on the input shaft DE (V) and output shaft NDE (H/A). RPM is measured using a proximity switch facing the motor shaft.

The first signs of bearing damage were visible around May 5th, 2014, using only the SPM HD measuring technique. The SPM HDm value was fluctuating, and when looking at the spectra, the first signs of BPFO harmonics could be seen. Later the HDm and HDc values were both increasing and a significant increase was seen from the 29th of July. The decision was made to plan for a replacement. Around September 2014, the spectrum was full of BPFO harmonics.

The decision was made to implement the newly introduced HD ENV technique. Because there was no vibration transducer on the input shaft NDE, the decision was made to install a transducer with a magnet base at that point in order to acquire extra data on the developing bearing damage. Two bands were used; Filter 3 (500Hz -10KHz) and Filter 4 (5KHz 40KHz). The transducer was installed on the 25th of September. When analyzing the spectra and time signal, there were clear signs of an inner race damage. The time signal showed a clear BPFIM signal. Below is the trend graph from the same measuring point, using the HD ENV technology.

The pictures show damage on the inner and outer raceway; however, the inner raceway is the most damaged. The outer race was not visible in the HD ENV measurements. On the other hand, the inner race damage was not visible on the SPM HD measurements. This demonstrates the added value of using complementary measuring technologies like SPM HD and HD ENV.

The first signs of bearing damage were visible around the end of June 2014, using the SPM HD measuring technique. From that date on, the BPFI trend was increasing and fluctuating. From the end of March 2015, the values elevated even further. The gearbox was replaced on June 5th and this resulted in a green evaluation for all measuring points again. The bearing was examined and the inner race damage was confirmed by the gearbox supplier.

The drive end shock pulse measuring point has been elevated since measurement started; the alarm and alert levels were already adjusted in the past. The bearings for the exhaust fan were replaced because the shock pulse spectra started showing the BS and BSFM defect frequencies from the 2nd half of 2014.

When the new bearing was installed, the HDc readings increased further, meaning lack of lubrication and therefore high load on the bearing. This normally indicates the bearing mounted incorrectly. When the spectrum was investigated, the FTF and BS frequencies were visible. The service provider who replaced the bearing was called and the decision was made to change the bearing once more. After this 2nd exchange, the overall value and the cage rate (FTF) evaluation dropped to normal values again.

The combination of vibration and SPM HD shock pulse measurement is ideal for this type of application. The shock pulse technology is very suitable for the detection of bearing damages in noisy environments like the gearbox in this case study. Vibration technology is optimal for low frequency related fault conditions like unbalance, loose gears and misalignment. Thanks to the sensitivity of the SPM system and the long pre-warning times, maintenance actions could be planned well in advance. The contribution of the condition monitoring system is evident as it was able to detect two bearing damages during the warranty period. As a result of this, the gearbox was replaced without any cost for Orcem.

7.1 Customer references Jeroen Bmer, Plant Manager at Orcem Moerdijk says: Without any doubt, SPM HD is the preferred method for condition monitoring of our rotating equipment. Mills, fans etc. are subject to demanding operating conditions and over the years we have been able to avoid countless component failures thanks to the sensitivity of the SPM HD measuring technique, which we use to monitor all our auxiliary equipment. For the extension of our production facility, to become in operation in 2017, we will use the SPM Technology.

Robbert has a mechanical engineering background. Involved in condition monitoring since 2012, Robbert holds an ISO 18436-2 CAT III certification. Robbert is mainly involved in vibration analysis reporting, customer training and support.

optimization of ball milling parameters to produce centella asiatica herbal nanopowders | springerlink

optimization of ball milling parameters to produce centella asiatica herbal nanopowders | springerlink

Nanopowders of Centella asiatica was produced using planetary ball mill by varying milling parameters such as milling time, mass concentration, and bead amount. Particle size analysis employing photon correlation spectroscopy was carried out to record the effect of milling parameters on the particle size produced. The morphology of milled powders was also analyzed using a field emission scanning electron microscope. The bioactive component, asiatic acid, was extracted from various sizes of C. asiatica powders, and its extraction yield at different powder size was calculated by high-performance liquid chromatography. Optimization of milling parameters was found to be a crucial step in determining the content of asiatic acid extracted. In this study, the highest amount of asiatic acid extracted was 25.4 mg/g, obtained at moderate conditions of the following milling parameters: 4 h of milling time, 1.2% (w/v) concentration of powder, and 25 g of bead load.

Centella asiatica is a perennial plant that mostly grows in the tropical and subtropical climate. It is known as mandukarpani (Indian), gotu kala (Chinese), or pennywort (English). It is commonly used as a wound-healing agent and for treatment of mental disorders and skin cancer. Studies also show that the herb extract could increase collagen production and strengthen tensile strength [1]. Thus, this herb is widely used in formulations of cosmetic and pharmaceutical products and possesses high commercial value. All these therapeutic effects are mainly contributed by the triterpene glycosides, mainly asiatic acid and asiaticoside (Figure1). Asiatic acid, a pentacyclic triterpene, is the aglycone form of asiaticoside which consists of a sugar moiety: a trisaccharide containing -L-rhamnopyranoside linked to the disaccharide gentiobiose [2]. Although the pharmacological effect of asiaticoside has been well known, some data suggest that asiatic acid is the actual component responsible for the plant's therapeutic effects since asiaticoside is being hydrolyzed to asiatic acid in vivo[35]. Thus, asiatic acid can be considered as the bioactive compound of C. asiatica. [4]. Recent studies showed that asiatic acid could treat liver fibrosis [6], protect primary neurons against C2-ceramide-induced apoptosis [7], inhibit acetylcholinesterase [8], and induce neurotoxicity. Furthermore, modification of asiatic acid functional groups have been carried out with the aim of improving the compound's potential as a hepatoprotective agent [9, 10].

Natural products have been important sources of drugs and will continue to play an important role as a major source of new drugs in the years to come [1113]. Normally, bioactive components exist in a low concentration; thus, an effective method is urgently needed to retrieve the analyte from their cell matrix. Many methods have been introduced such as ultrasonic extraction (UE), microwave-assisted extraction, accelerated solvent extraction, pressurized hot water extraction [1416], and supercritical/subcritical extraction [17, 18]. However, the extraction efficiency of each method is greatly dependent on the particle size of plant material itself [19, 20]. Among the methods, UE has been known for their extraction efficiency with reduced processing time and solvent consumption [14].

Ball milling is a common method in the size reduction of material. The milling process produces nanopowders through the impact forces generated by action of centrifugal forces. Milling parameters such as milling time, mass concentration, and bead amount are important parameters that need to be considered in producing superfine powders. In this research, our aim is to investigate the effect of particle size on the amount of asiatic acid extracted employing high-performance liquid chromatography (HPLC).

To obtain a uniform distribution of particle size in the nanometer range, milling parameters such as milling time, mass concentration, and bead amount were varied. The results as shown in Figure2 indicate that each set of milling condition produced different particle sizes of powder. Varying milling time, mass concentration, and bead amount from 2 to 8 h, 0.4% to 2.8% (w/v), and 5 to 100 g varied the particle size from 408.8 to 191.1, 237.1 to 581.1, and 442.6 to 212.8 nm, respectively. Statistically, increasing milling time from 2 to 4 h significantly reduced the particle size since sufficient energy was provided for size reduction. However, no significant reduction in particle size was observed after an extended milling time of 4 to 8 h. This is due to the fibrous structure of plant material itself which limited further size reduction [21]. An increase of particle size from 237.1 to 581.13 nm was observed as mass concentration is increased from 0.4% to 2.8% (w/v). Increase of mass concentration led to inefficient energy distribution in the milling process caused by the weak interaction between bead media and particles [22]. At a higher mass concentration, the viscosities of slurries increase and the distance between individual particles is reduced leading to ineffective particle capture by the grinding beads. The higher viscosities will then weaken the motion of grinding media; thus, velocity of grinding media and kinetic energy of bead decreased tremendously leading to ineffective milling operation [23]. The study on the effect of bead amount on particle size showed an inverse correlation. The smallest particle size (212.8 nm) was achieved with the highest amount (100 g) of bead load, and the largest particles size (442.6 nm) was found with the lowest bead amount (5 g). This can be understood by the limited amount of beads present in the reaction. With a low amount of bead load, the limiting reactant is the bead itself since the low numbers of bead present in the physical reaction will cause a reduction in the collision frequency due to limited amounts of bead per mass powder and reduced energy efficiency. Similarly, with higher bead amount, the energy efficiency would be higher, as reported by He et al. [22].

As shown in Figure3, the microstructures of coarse and milled powders showed a huge reduction of the size of nanopowders from the micropowder. It proves that the impact of collision in the milling process has tremendously broken down the micropowder to nanosize powder. The nanopowders exist in random structure in an agglomerated form. This is common since a higher surface energy possessed by the nanoparticles caused them to aggregate once it goes into a solid-state condition [24].

To evaluate the amount of asiatic acid extracted, each powder from each set of milling condition was extracted and analyzed using HPLC. From the HPLC chromatogram, asiaticoside was eluted for 8 min (tR = 8 min), while asiatic acid had a tR of 23 min. This method shows a good separation of the two compounds for both micro- and nanosamples (Figure4). As shown in Figure4, all milled samples showed no presence of asiaticoside, and we believe that asiaticoside have been hydrolyzed to asiatic acid during the milling process. As shown in Figure5, increasing the milling time, mass concentration, and bead amount from 2 to 8 h, 0.4% to 2.8% (w/v), and 5 to 100 g during grinding significantly varied the amount of asiatic acid extracted from 4.5 to 25.4 mg/g, from 2.3 to 25.4 mg/g, and from 4.1 to 25.4 mg/g, respectively. The difference in the amount of asiatic acid extracted could be caused by the degree of efficiency of extraction due to the difference in particle size of the powder and the ability of asiatic acid to retain their structure during the milling process. Each set of milling time (2, 4, 6, and 8 h) showed a reduction of particles to nanosize range. We further observed that a shorter milling time of 2 h produced a lower yield of asiatic acid content compared to 4 h of milling which could be explained by the difference in particle size of the powder as shown in Figure2. Interestingly, after 6 h of milling, the content of asiatic acid reduced tremendously as compared to after 4 h of milling, and the amount is further reduced after 8 h of milling. At this time, further nanosize reduction has occurred, and the energy the milling process may have degraded the asiatic acid and consequently reduce the amount of asiatic acid extracted. Kormin also reported that the asiatic acid content in C. asiatica juice extract reduced significantly at higher temperatures [25]. Other findings have also showed that heat is an important factor that should be considered in extracting bioactive compound from plants. Effect of heat in the extraction of saponins from ginseng was clearly significant as the level of ginsenosides Rg1, Re, Rb1, Rc, R2, Rb3, and Rd decreased after the steaming process [26]. The same trend was also observed in experiments that investigate the effect of bead amounts on asiatic acid content. Effect of the nanopowders in improving extraction of asiatic acid can be clearly observed by varying mass concentrations. The parameter values range from 0.4% to 2.8% (w/v) because our preliminary study showed that at this range, nanopowders range from 100 to 1,000 nm could be produced. Above these values, the milled product produced a greater size of particle (microrange). In this experiment, samples that were ground at 0.4% and 1.2% (w/v) showed a high amount of asiatic acid (24.5 and 25.4 mg/g) extracted due to increased extraction efficiency caused by smaller particle size that resulted from efficient energy distribution in the milling process. When milled at a higher concentration (2.0% (w/v)), the asiatic acid content was reduced to 13 mg/g, and further milling at 2.8% (w/v) caused a further drop in the extracted asiatic acid content (2.3 mg/g). The sudden drop in the amount of extracted asiatic acid amount was probably due a lower extraction efficiency caused by a larger particle size (500.7 and 581.7 nm). In this study, optimized milling parameters for the extraction of asiatic acid from C. asiatica is 4 h of milling time, 1.2% (w/v) mass concentration, and 25 g of bead load. To our knowledge, this method yields the highest amount of extracted asiatic acid from the plant compared to other methods previously reported which ranges from 7 to 14 mg/g [15, 17].

Generally, extraction of plant material involved two physical phenomena: diffusion through the cell wall and washing out the analyte into extraction solvent. Using nanopowders in the extraction of bioactive compound uses the same principles as using micron powders, but the only difference lies in the particle size used in the extraction. In this section, we discuss how the unique properties of nanopowders results in higher extraction yields.

Size reduction prior to extraction has been reported to be a crucial step to obtain from the plant matrix [15, 19, 27, 28]. The reduction in size is reported to enhance the contact ratio between plant cell and the surrounding solvent [28]. In our study, the higher amount of asiatic acid extracted from milled samples can be explained by the amazing properties of nanoparticles contributed by an increase in surface area and the reduction of diffusional distance of the particles (Figure6) [29]. Decreasing the particle size to the nanometer range caused an increase of surface area, leading to a higher number of cells directly exposed to the extraction by the solvent [28]. Based on Noyes-Whitney equation [30], the dissolution velocity of particles increases due to surface area enlargement as described in Equation1:

where dc/dt is the rate of dissolution velocity, D is the diffusion coefficient, A is the surface area of the solid, C s is the concentration of the solid in the diffusion layer surrounding the solid, and C x is the concentration of the solid in the bulk dissolution medium. The dissolution velocity dc/dt described in the above equation also depends on the concentration gradient (C s - C x )/h where h, the diffusional distance is reduced for smaller particles [31]. Due to the reduced h, the concentration gradient of nanoparticles is large (Figure5) [29, 32] which causes the dissolution velocity to increase. This will enhance the diffusion of solvent into the cell wall, which in turn will allow the rapid release of active ingredients from the cell matrix of the plant. This is also supported by the phenomena where the disrupted cell wall structure of the plant material itself cause the active compound in the inner cytoplasm to be exposed directly while not being released from cell walls making effective ingredients dissolve out rapidly [33]. Past studies have shown that nanonization will allow the rapid release of active component from their cytoplasm matrix [3436] and help improve the extraction of bioactive components of plants.

In general, we have provided further proof that nanonization of plant material played an important role in contributing to the extraction yield of bioactive compounds from plant materials. In this research, we have successfully produced nanopowders of C. asiatica by planetary ball milling. Our findings showed that a smaller particle size gave a higher extraction yield of asiatic acid compared to a bigger particle size. However, if the particle size is too small, the extraction yield of the compound will be reduced due to the effect of heat and pressure in the milling jar. As a conclusion, optimized milling parameters for high extraction yield of asiatic acid from C. asiatica was found to be 4 h of milling time, 1.2% (w/v) concentration of powder, and 25 g of bead load.

Asiaticoside and asiatic acid standards (Biopurify Chegdu, Sichuan, China) were purchased from Sigma-Aldrich Corporation (St. Louis, MO, USA), acetonitrile (LC grade) was purchased from Fisher Chemicals, and methanol (HPLC grade) was purchased from Friedemann Schmidt (Berlin, Germany). Distilled water was purified using a Milli-Q water purification system (Millipore, Bedford, MA, USA).

The plant material was washed with running tap water and rinsed with distilled water to remove dirt and contaminants. The clean plant material was stored in an oven at 50C and was left to dry for 3 days. The dried plant material was ground using a conventional rotor mixer. The ground powder was then sieved through a 250-m sieve and stored at 4C prior to the ball milling process.

Ball milling is a common mechanical process to produce superfine powders. In this research, a planetary ball mill was chosen as a grinding tool due to its simplicity. The sieved powder was first mixed with Pluronic F127 and milled at different mass concentrations (0.4%, 1.2%, 2.0%, and 2.8% (w/v)) at a constant milling time (4 h) and fixed bead amount (25 g). The resulting milling product was freeze-dried and analyzed for their physical characteristics. The best condition of milling (% (w/v)) was determined by the size of powder yielding the highest amount of asiatic acid extracted. This condition was then applied at different milling times (2, 4, 6, and 8 h) and different bead amounts (5, 25, 50, and 100 g), and the sample was analyzed for their physical characteristic and amount of asiatic acid extracted.

Prior to the measurement, nanosuspensions of each sample were taken and adjusted to 0.01% (w/v) and introduced into a disposable cuvette to be measured in triplicates. z-Average and polydispersity were recorded. Field emission scanning electron microscopy (FESEM; SMT SUPRA 40VP, Carl Zeiss AG, Oberkochen, Germany) imaging was carried out by placing 10 L of the nanosuspension onto a glass slide and stored in an electronic desiccator (temperature 20C, humidity 18% RH) for drying purposes. The dried samples were then coated with gold (approximately 10-nm thick) and were placed onto an adhesive tape on the FESEM stub.

Coarse powder (0.5 g) was weighed and sonicated for 1 h using an ultrasonic processor (UP400S Ultrasonic Processor, Hielscher Ultrasonics GmbH, Teltow, Germany) at 60% amplitude and 1 cycle. The solids were removed by gravitational filtration, and the filtrate was collected. The nanopowders were also extracted in the same manner as above. The extract was dissolved in methanol (1 mg/mL) before being subjected to HPLC analysis.

The chromatographic separation was based on a modified method of Inamdar et al. [37] using a Zorbax Eclipse XDB-C18 4.6 150 mm (Agilent Technologies, Inc., Santa Clara, CA, USA), 5 m at 25C. The mobile phase, solvent A (ultrapure water) and solvent B (acetonitrile), was delivered at a flow rate of 1.0 mL min-1. Gradient elution was employed with the ratio of A/B and varied as follows: 0 min, 80:20 and 35 min, 45:55. Standards or samples were introduced into the HPLC using an Agilent 1200 G1367B auto sampler, injection volume was 40 L, and the detection wavelength was 206 nm. The amount of asiatic acid was determined using a standard calibration curves.

Hereby I, Muhammad Zuhairi Bin Borhan declare that as the author of the manuscript, have or do not have a direct financial relation with the commercial identities mentioned in my paper that might lead to a conflict of interest for any of the authors.

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MZBB: Mainly involve in all laboratory works; Experimental Design, Sample preparation, Analysis sample; Mainly involve in preparation of manuscript. RA: Assisting in all laboratory works; Extraction of compound, HPLC Analysis; Assisting in preparation of manuscript. MR: Assisting in all laboratory works; FESEM Analysis, Particle Size Analysis; Assisting in preparation of manuscript. SA: Assisting in all laboratory works; FESEM Analysis, Particle Size Analysis, HPLC Analysis; Assisting in preparation of manuscript.

Open Access This article is distributed under the terms of the Creative Commons Attribution 2.0 International License (https://creativecommons.org/licenses/by/2.0), which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

Borhan, M.Z., Ahmad, R., Rusop, M. et al. Optimization of ball milling parameters to produce Centella asiatica herbal nanopowders. J Nanostruct Chem 3, 79 (2013). https://doi.org/10.1186/2193-8865-3-79

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