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j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / i j m i n p r o

Effect of comminution on particle shape and surface roughness and their relation to

otation process

Mahmoud M. Ahmed

Mining and Metallurgical Engineering Department, Faculty of Engineering, Assiut University, Assiut 71516, Egypt

a r t i c l e

i n f o

Article history:

Received 23 July 2008

Received in revised form 8 February 2010

Accepted 22 February 2010

Available online 1 March 2010

Keywords:

Particle shape

Surface roughness

Fractal

Comminution

Flotation

Wettability

a b s t r a c t

The essential physical characteristics of the distinction of particles are size, shape and surface roughness.

Particle shape and surface roughness are considered important parameters in the prediction of the behavior

of particles individually or collectively. These parameters are of great importance to industries employing

various materials in a powder form. These parameters have not been currently reviewed satisfactory in the

mineral processing eld. Therefore, this research is concerned with the different methods used to estimate

the particle shape and surface roughness and also to relate these parameters with the behavior of some

mineral processing operations, especially comminution and otation processes.

The surface roughness of mineral particle inuences the fundamental processes of particlebubble

attachment and the other sub-processes in froth otation. The contact angle is dependent on the surface

roughness. The modication of the wettability due to surface roughness can be greatly enhanced in the

fractal surface; that is the fractal surface will be superrepellen (superwettable) to a liquid when the contact

angle is greater (less) than 90. Correlations were found between the shape properties, surface roughness

values and wettability.

The dry grinding produces relatively rough particle surfaces with a high concentration of microstructural

defects while the wet grinding produces smoother cleaner surfaces. The dry ground samples exhibited more

stable, higher loaded froths and faster otation kinetics.

2010 Elsevier B.V. All rights reserved.

1. Introduction

In addition to process variables, the processing of powder depends

to a large extent on the materials (purity, structure, density, etc.), bulk

properties, and the morphological characteristics (size, shape, texture,

etc.). Material characteristics are well understood and almost

completely known because the chemistry and physics of the materials

are highly developed. The morphological characteristics are not yet

developed and explored completely. The denitions of some

morphological characteristics like particle shape, size, and surface

roughness are still also evolving (Singh and Ramakrishnan, 1996).

The geometry of particle has a pronounced inuence on the

physical and chemical actions occurring on the particle surface

during the technological processes. This illustrates the importance of

the exact geometrical evaluation of the particles by means of

quantied particle parameters. These parameters can be used to

differentiate between different materials and to correlate them with

the different processes. The essential characteristics of the distinction of particles are size, shape and surface roughness (Castellini

E-mail address: mamoah@aun.edu.eg.

0301-7516/$ see front matter 2010 Elsevier B.V. All rights reserved.

doi:10.1016/j.minpro.2010.02.007

in the prediction of the behavior of particles and powders inuencing

the manner, in which they break, react, sinter, oat, agglomerate and

uidize (Clark, 1986). The distribution of particle sizes and shapes is

of great importance to industries employing various materials in a

powder form (Hurter and Clark, 1987). These include many of the

raw materials in civil and chemical engineering, pharmaceutical,

mining industries, pigments, metals, ceramics, pills, foods, and

industries interested with population of atmospheric dusts, smoke

and grit (Ulusoy et al., 2003).

The rst procedure used for describing the shape of a ne particle

was carried out by measuring simple linear parameters such as

the length, breadth and width. The ratios of these dimensions are

used as coefcients to describe the shape dependent property

(Sarkar and Chaudhuri, 1994). The methods used for estimating

the particle characteristics range from very simple such as the

determination of aspect ratio, elongation ratio or circularity to very

modern methods such as the use of Fourier analysis, delta analysis

and fractal geometry (Meloy and Williams, 1994; Singh and

Ramakrishnan, 1996; Singh and Ramakrishnan, 1996). The development of automated microscope techniques linked to computer dataprocessing systems (image analysis techniques) facilitated the

possibility of specifying the shape and surface roughness of a prole

by mathematical procedures (Meloy and Williams, 1994). Development of these methods may give a way to optimize the mineral

processing ow sheets not only on the basis of particle size

distribution but also by introducing the particle fractal properties

(Burstein et al., 1995).

Numerous factors inuence otation. Although particle hydrophobicity and size are important and have received much attention in

research, particle shape and roughness play a signicant role also, but

they have received much less attention.

The interaction between a solid particle and a gasliquid interface

controls the efciency of the otation process and has been

considered in detail (Ahmed, 1999; Ahmed et al., 1999).

The bubbleparticle interaction involves many stages, i.e. the

before-contact and after-contact interactions (Scheludko et al., 1968/

1969). The before-contact bubbleparticle interaction is strongly

affected by the long-range hydrodynamics when the bubble and the

particle are far from each other. It is controlled by the interfacial

physics e.g. interfacial dynamics, capillarity and colloidal interaction if

they are close enough.

The particle shape has a signicant inuence on otation behavior.

Many researchers have studied this relation qualitatively (Varbanov,

1984; Blake and Ralston, 1985; Ducker et al., 1989; Schmidt and Berg,

1996; Schmidt and Berg, 1997).

A few researchers have studied the effect of the surface roughness

on the otation process (Anfruns and Kitchener, 1997; Silverstein and

Breuer, 1993; Burstein et al., 1995; Ahmed, 1999; Ahmed et al., 1999;

Stechemesser and Ahmed, 1999).

The surface roughness of mineral particle inuences the fundamental processes of particlebubble attachment and the other subprocesses in froth otation.

Ahmed et al. (1998); Ahmed (1999); Ahmed et al. (1999) and

Stechemesser and Ahmed (1999) illustrated a modern and useful

approach, which was considered the rst attempt, to study the

quantitative effect of the surface roughness and shape of particle on

the detachment process of particle from the airliquid-interface by

means of a centrifuge technique and also on particle oatability

(under ideal conditions) using a modied Hallimond tube. It can be

supposed that the roughness of the solid surface has a decisive

inuence on otation effectiveness (Burstein et al., 1995). The

higher the surface roughness, the stronger is the detachment force

required to separate the particle from the bubble and hence a higher

otation recovery is obtained (Ahmed, 1999 and Ahmed et al.,

1999).

In froth otation, the probability of otation and hence the rate of

otation is directly determined by three microprocesses: collision,

adhesion and detachment (Trahar and Warren, 1976). To obtain an

improved understanding of the complete otation process, it is

necessary to analyze these three microprocesses quantitatively. The

ease with which the particle can be attached to the bubble and the

strength of detachment are considered very important when the

effectiveness of otation process is studied.

The differences in the values of detachment forces and hence the

otation effectiveness were markedly clear at the different degrees of

hydrophobicity for the same surface roughness (Ahmed, 1999 and

Ahmed et al., 1999). In addition, the difference in the values of

detachment forces increases with the increasing of the surface

roughness. At the lowest roughness, the difference in the value of

detachment force between the low and high hydrophobicity does not

exceed 1.5 * 105 N. This difference reached 7.1 * 105 N at the

highest roughness. This behavior may be attributed to the chemical

effects caused by adsorption of the silane lms on the surfaces having

different roughness. A surface with a lower roughness has a smaller

surface area compared to the surface of higher roughness and

therefore it reaches a maximum surface coverage at a lower

methylation time (lower contact angle) (Ahmed, 1999; Ahmed et al.,

1999).

181

sulde ores has been investigated (Feng and Aldrich, 2000). The dry

ground samples have relatively rough particle surfaces with a high

concentration of microstructural defects. The wet ground samples

have smoother and cleaner surfaces. The dry ground samples

exhibited more stable, higher loaded froths and faster otation

kinetics owing to the activated particle surfaces. Moreover, by

combining dry and wet grinding, the kinetics, the nal grades and

recoveries of the suldes were improved. In the otation of sand, the

dry ground sand showed signicantly faster otation kinetics and a

slightly higher otation yield than the wet ground sand. This

demonstrates that dry milling could improve otation kinetics

owing to the higher energy absorbed in the particles.

Particle shape and surface roughness are considered important

parameters for predicting the behavior of particles individually or

collectively. Therefore, this research paper is interested in the

different methods used for estimating the particle shape and surface

roughness and relating them with the behavior of some mineral

processing operations, especially comminution and otation

processes.

of particles

Particle shape is one of the most important measures and there is

no general shape factor available which clearly differentiates between

all possible kinds of shape (Podczeck, 1997). The development of the

automated microscope techniques linked to computer data-processing systems (image analysis techniques) facilitated the possibility of

using the methods of specifying the shape and surface roughness of a

particle prole by mathematical procedures (Meloy and Williams,

1994). A three-dimensional particle is projected in a plane to obtain

two-dimensional closed curve which is taken to estimate the particle

shape. The methods used to assess the particle shape and surface

roughness range from very simple methods such as the determination of aspect ratio, elongation ratio or circularity to very modern

methods such as the use of Fourier analysis, delta analysis and fractal

geometry (Meloy and Williams, 1994; Singh and Ramakrishnan, 1996

and Podczeck, 1997). These methods are reviewed in the following

sections:

This is the simplest method used for characterizing the particle

shape. Words like spherical, disc, blade, rod, granular, rounded,

angular, isometric, irregular, nodular, crystalline, oblong, acicular,

brous, dendritic and aky have been used to classify the particles

into different shape groups. Although this identication corresponds well with the human imagination, it is however quite

subjective (Singh and Ramakrishnan, 1996 and Stechemesser et al.,

1996).

In many industries, an old system called the vibrating table was

used for separating the particles according to their shapes. In this

device at, elongated or needle particles may be separated from

rounded particles by owing the particles over a tilted table. The

eccentric vibrating motion of the table drives all particles laterally

along the table; however, rounded particles roll down the inclined side

of the table at right angles to the motion of the at particles. Parallel

groves in the table may keep acicular particles from rolling (Meloy and

Williams, 1994).

182

particle

2.2.1. Shape factors

Flatness ratio and elongation ratio (Singh and Ramakrishnan,

1996; Burstein et al., 1995):

breadth B

thickness T

Flatness ratio =

Elongation ratio =

length L

:

breadth B

length of particle projection derived from the co-ordinates of the

projected area in one specied direction of measurement.

Factor of circularity characterizes the deviation from the circular

shape. It has a value of 1.0 for the spherical particle and its value is less

than 1.0 for the other shapes.

Sphericity (Singh and Ramakrishnan, 1996):

Sphericity =

:

actual surface area of the particle

5

shape of a particle approaches to a circle and a sphere, respectively.

External compactness (Kaye, 1981):

External compactness =

diameter of a circle of equal area 2

DA 2

=

:

diameter of embracing circle

DEm

6

Chunkiness (Kaye, 1981 and Kaye et al., 1992):

Chunkiness =

Bm

:

Lm

avg

i=1

180

"

#

2DX + DY + DP + DM + 8

CONC =

1:

2nedg: ncor:

11

12

This measure has a zero value for the convex particle and increases

with the increase of fracturing.

FO =

LENG

:

LCNV

13

DA

:

DFmax:

Jaggedness =

Circularity =

:

circumference of the particle

3

FK =

180

1 RDi

innovative procedures for determining the shape and surface

roughness of ne particle proles. These are Fourier analysis and

the fractal geometry (Kaye et al., 1992). Fractal geometry was

introduced to the scientic community by Mandelbrot (1997). He

illustrated how natural or real physical boundaries, which cannot be

adequately described by traditional or Euclidean geometry, can be

characterized using fractal geometry. Fractal geometry can be applied

for specifying the real physical boundaries which have no tangent, i.e.

curves that have no differential functions (Brown et al., 1993). Fractal

dimension is an interesting feature proposed recently to characterize

the surface roughness and self-similarity of a picture (Sarkar and

Chaudhuri, 1994). The practical signicance of the fractal dimension is

more than the other measures where it can be quantied through a

range of measuring scales and is expressed with a simple scalar

number. It is practically well suited to estimate the highly re-entrant

particle, which has sharp corners and indentations (Graf, 1991).

The basic methodology of determination the fractal dimension of a

projected prole is to measure the perimeter many times with

different scales of measurements, i.e. at a series of step lengths or

resolutions. Smooth particles have constant lengths of perimeter

while the rough particles have larger perimeter lengths with smaller

step lengths (Meloy and Williams, 1994). Particles, which display

fractal behavior, observe the following exponential relationship

(Clark, 1987; Kaye, 1991; Brown et al., 1993; Sarkar and Chaudhuri,

1994; Meloy and Williams, 1994; Brown et al., 1994a and Lee and

Chou, 1994):

Lr = cr

1F

14

Aspect ratio =

Lm

:

Bm

Roundness (Singh and Ramakrishnan, 1996):

just a few sides of equal lengths. With small step lengths, the particle

is modeled as a polygon with several sides of equal lengths.

Eq. (14) can be rewritten as follows:

log Lr = 1F log r + log C :

15

Ri = ncor

Roundness =

i=1

g

3 ncor

ij

Angularity = 180ij :

ri

i=1 j=1

The value of this factor ranges from 0 to .

10

By plotting log [L(r)] against log [r], the fractal dimension (F) can

be calculated from the absolute slope (1 F) of the best-tting line of

data in the plot. Such graph is known as Richardson plot and is

illustrated in Fig. 1 where 1.0 F 2.0. A fractal dimension value equal

to 1.0 is related to a Euclidean prole while the Brownian movement

will approximate to a fractal dimension value equal to 2.0. Large

slopes on the Richardson-graph correspond to a strong fracturing and

an irregular surface.

Fig. 1. Richardson plot of a particle prole (after Clark, 1987; Kaye, 1991; Brown et al.,

1993; Sarkar and Chaudhuri, 1994; Meloy and Williams, 1994; Brown et al., 1994a and

Lee and Chou, 1994).

estimated perimeter to the Feret's diameter of the particle as shown in

Fig. 2.

For natural systems, several dimensions may arise at various step

lengths. For mineral fragments, usually two linear portions with two

different slopes are observed on the Richardson plot through the step

length range used. This illustrates different irregularities at different

step lengths (different resolutions) as shown in Fig. 3. The region at the

smaller step lengths is known as the textural (surface roughness) region

while the structural (shape) region is at the coarser step lengths and

represents the gross boundary of the particle (Kaye et al., 1987; Kaye

and Clark, 1989; Graf, 1991; Kaye, 1991; Brown et al., 1993 and Brown

et al., 1994a). A sharp break point between the structure and the

texture is signicant where it is considered a rapid transition from one

fractal domain to the other. In many cases there is a gradual transition.

Graf (1991) concluded that the range, number and dimension of

fractal elements in a ne particle depend not only on the geometry of

the particle but also on the resolution limits (step lengths) of the

investigator. He listed four recommendations to remedy the problem

of scale sensitivity:

1. Scales of Richardson diagrams must be made by using both the

absolute and Feret-normalized measures. Absolute scales are

183

Fig. 3. Richardson plot showing the change in fractal dimension with the step length

where the perimeter estimated and step lengths have been normalized with respect to

Feret's diameter of the particle (after Kaye et al., 1987; Kaye and Clark, 1989; Graf,

1991; Kaye, 1991; Brown et al., 1993 and Brown et al., 1994a).

processes.

2. Select a constituent upper bound for the maximum step length.

When very large step lengths are used, changes in the perimeter

reect the trends of simple polygons rather than the geometry of

particle (Kaye, 1984).

3. Use the largest possible resolution. Poor resolution, which results

from the poor imaging or video limitations, can mask potentially

important textural elements.

4. Make interpretations with the help of physical models and physical

processes.

Various image analysis techniques have emerged over the last two

decades. In these techniques, the three dimensions of the particle (or

its projection in two-dimensional direction) are actually measured

(Hurter and Clark, 1987). The disadvantage of the two-dimensional

image analysis technique is that it gives no indication of the threedimensional geometry of the particle, where the technology is not

generally available for the three-dimensional digitization of the

particle surfaces (Clark, 1987). In earlier publications dealing with

the fractal structure of ne particle boundaries, the experimental

work was carried out manually. This was time consuming and the

amount of investigative work, which could be undertaken in a given

context, was limited (Kaye et al., 1987). Nowadays, several computer

aided image analysis procedures have been reported. The most

popular methods used for determination of the fractal dimension are

structured walk technique, equipaced polygon technique, dilatation

logic technique, the mosaic amalgamation technique and the line

scans triangulation technique (Schwarz and Exner, 1980; Kaye, 1984;

Clark, 1986; Kaye et al., 1987; Avnir, 1989 and Kaye et al., 1994).

2.4. Fourier analysis

Fig. 2. A particle prole with a maximum step length of 0.3 of Feret's diameter (after

Clark, 1987; Kaye, 1991; Brown et al., 1993; Sarkar and Chaudhuri, 1994; Meloy and

Williams, 1994; Brown et al., 1994a and Lee and Chou, 1994).

One of the most popular methods for shape analysis is the Fourier

analysis which determines the shape prole using Fourier coefcients

(Kaya et al., 1996). In Fourier analysis, rstly a reference point at the

center of prole is chosen. It is preferred to choose the centroid of the

prole treated as a useful reference point. Secondly, a point on the

periphery of the prole is chosen as the starting point for exploration of

the prole with a rotating vector. The maximum distance is then used as

a normalizing factor to summarize the magnitude of the vector as it

moves around the periphery of the prole with a uniform angular

velocity to generate what looks like a waveform (Schulze et al., 1989).

Two main procedures based on the Fourier analysis of a prole

may be applied to the morphologic characterization of a particle

(Singh and Ramakrishnan, 1996). The rst method is based on Fixed

Angular Boundary Sampling (FABS) (Luerkens et al., 1987) and the

184

(Bonifazi and Massacci, 1996).

3. Application of atomic force microscopy in measurement of

surface roughness

The atomic force microscopy (AFM) was rst described in 1986 by

Binnig et al. (1986) as a new technique for imaging the topology of

surfaces to a high resolution. Since then AFM has been used in the study

of surface science, both as an imaging and surface characterization

technique. AFM has a number of advantages over electron microscopy

techniques, primarily the ability to make measurements in a uid

environment, as well as, the capability to directly measure interaction

forces between surfaces (Johnson et al., 2006). Atomic force microscopy

is a technique able to quantitatively measure interactions between

single particle and interfacial boundaries (Johnson et al., 2006).

Surface properties like roughness, adsorption layers and surface

chemistry strongly affect the adhesion forces. Measurements of

particleparticle and particlesurface interactions in the gas phase are

carried out with an atomic force microscope (AFM). For modeling of

particle adhesion, computer-assisted empirical potential methods are

used. Parameters like absorbed water and surface roughness are

considered. Parameters for weak interactions from the Lifshitz theory

and gas adsorption data are extracted. Absorbing molecules can be used

as probes to measure dispersive forces (Goetzinger and Peukert, 2003).

Many methods are used to characterize the surface roughness of solid

particle for quality control and for nding the correlations with other

properties. In this study, the fractal analysis was used to describe the

surface roughness. Atomic force microscopy (AFM) was used to obtain

three-dimensional surface proles. The variation method was applied to

calculate the fractal dimensions. Fractal dimensions of four granule

samples, four powders, and two freeze-dried powders were measured. A

computer-program was written to implement the variation method. The

implementation was veried using the model surfaces generated by

fractional Brownian motion. The fractal dimensions of most particles and

granules are between 2.1 and 2.2, and are independent of the scan size

measured. The freeze-dried samples however show wide variation in the

values of fractal dimension, which are dependent on the scan size. As

scan size increases, the fractal dimension also increases up to 2.5. This

variation method allows calculating reliable fractal dimensions of

surface proles obtained by AFM. The estimates are dependent on the

algorithm and the digitized model size (i.e., number of data points of the

measured surface prole) used. The fractal dimension is also a function

of the observation scale (i.e. the scan size) used in the prole

measurement. The multi-fractal features and the scale-dependency of

fractal dimension result from the articial processes controlling the

surface morphology (Li and Park, 1998).

To obtain additional information on the surface roughness of the

studied samples, AFM scans are performed and root mean square (r.m.s.)

roughness is determined at different lateral scales (Gladyszewski et al.,

1998 and Hazra et al., 2001). The dened sizes are corresponding to

specic physical properties measured on generally irregular particles,

while most sizing techniques assume that particles are spherical in

shape. Direct physical particle sizes can be determined with an atomic

force microscope (Gwaze et al., 2007).

impact shattering and ball milling (Brown et al., 1993). The size

distributions of impact sample product were less than 2000 m

(median size = 250 m). The maximum size of ball milling sample

product was less than 3500 m (median size = 80 m). Fractal

analysis was performed on samples of the resulting comminution

products. The impact sample (formed by ballistic disintegration)

produces particles with higher boundary fractal dimensions than the

milled sample. The fractal dimension of the impact fragments

increases with decreasing size, whereas the milled particles displays

a more complex distribution. This behavior may be due to the

abrasion acting on fragmented particles in the ball mill which

smoothes off any protrusions. Also, it is possible that small amounts

of crushing (compressive failure) may have occurred from the

trapping of small particles between two larger balls. It is observed

that fragments produced by tensile fragmentation have a higher

fractal dimension than those produced by compressive fragmentation

(Brown et al., 1993).

The previous data was plotted on Gaussian probability graph

paper, as shown in Fig. 4, where the ordinate represents the

cumulative percentage of fractal dimension equal to or less than a

stated value. The fact that the fractal information gives straight line on

Gaussian probability paper is evidence that the fractal dimensions, in

a population of shattered rocks, are probably describable by a

Gaussian distribution function. Different comminution types occupy

also different regions on this type of chart, as indicated by Fig. 4 and

various charts could be constructed for different materials. The

implications are that if one requires a denite particle distribution, in

fractal terms, then the mechanism of size reduction can be selected

(Brown et al., 1993). There is clear evidence to support the concept

that the structural fractal dimension of a particle holds key

information upon its formation dynamics.

Another study was performed to investigate if the type of

pulverizer used to comminute limestone, a grade suitable for ue

gas desulphurization (FGD), inuences its behavior and use. At

present, more than 10 M tones of limestone are milled per year in

Europe for FGD purposes. The three pulverizers used are a laboratory

hammer mill, crushing rolls with smooth surfaces and a batch

laboratory ball mill. The failure mechanisms represented by these

devices can be broadly categorized as single and/or double impact

(hammer mill) and compression and shear failure (roll crusher). The

ball mill size reduction mainly takes place by the impact of balls on the

shape and surface roughness

Although many aspects of comminution have been reported, there

have been relatively few papers devoted to the effects on particle

shape and surface roughness. This area of powder technology is

neglected partly due to the difculties in measuring the shape and

surface roughness of particles and also because there are no

universally accepted denitions of shape (Kaya et al., 1996).

(a) Impact sample product (50 = 250 m). (b) Ball mill product ( 50 = 80 m) (after

Brown et al., 1993).

185

Variations in the limestone utilization are noted for the samples

comminuted by the three different techniques. The hammer-milled

sample having the highest value because it has the highest boundary

fractal population (Brown et al., 1994a and Brown et al., 1994b).

Experimental investigations on the comminution of gibbsite in four

different types of mills are presented. These include tests of dry grinding

in a tumbling ball mill, a shaker bead mill and an air jet mill, as well as,

tests of wet grinding in a tumbling ball mill and in a stirred bead mill. A

quantitative characterization of the size and shape of the ground

product was made in order to analyze the effect of the grinding stress on

the properties of a complex agglomerate crystal such as gibbsite. The

analysis allowed us to determine the fragmentation route occurring in

the mills. This led to the identication of two fragmentation paths

imposed during comminution processes. These involved different

phenomena: rupture of joints and chipping and breakage according to

the nature of the main stress (attrition or impact) (Frances et al., 2001).

Fig. 5. Fractal distribution data, for the FGD limestone fragments, illustrated on a

Gaussian probability graph paper (size = 38 m) (after Brown et al., 1994b).

et al., 1994b).

The limestone sample consists of 14.0 mm. It was pre-screened at

the quarry, from which a (4.0+1.7) mm size fraction was extracted to

produce an even feed for the pulverizing devices. Samples of this fraction

were comminuted by hammer milling (internal screen removed), roll

crushing and ball milling. The Raymond mill and roll crusher were

starvation fed, to reduce particleparticle interactions, and ball milling

was performed wet, with de-ionized water. In order to produce a very

narrow size range, to effectively negate size effects in acid digestion, the

resultant comminution products are screened at 38 m, and the undersize

classied using a Warman cyclosizer (elutriation technique). Cone ve on

the cyclosizer was chosen as the size band for investigation, (16.2+

12.7) m (0.5 m) (Brown et al., 1994b).

The populations of the structural boundary fractal dimensions of

the three sets of fragments are shown in Fig. 5. From this gure, it can

be shown that the particles are distributed according to Gaussian and

the three distributions are found to be signicantly different. This is

further evidence to support the concept that the structural boundary

fractal dimension of a particle holds key information upon its

formation dynamics. On the other hand, simple geometric shape

factors, i.e. circularity and aspect ratio did not detect any signicant

As well known, otation differs from most of the separation

processes by the fact that the conditions of separation directly depend

on surface properties and therefore also on comminution process. The

deformation mechanism in comminution has a great inuence on the

properties of mineral surfaces formed during grinding because the

geometrical heterogeneity of the surface determines the area reacting

with otation reagents. Moreover, the character of the interactions

between the reagents and minerals is also dependent on the

conguration of the surface (Ocepek et al., 1990).

The effect of dry and wet grinding on the otation of complex

sulde ores from the Merensky Reef in South Africa was investigated.

The sample was crushed in a jaw crusher and a rotary cone crusher to

100% passing 4 mm. For comparative purposes, an oxide ore (sand)

with a particle size of 3 mm was also investigated. The rod mill was

run at a constant speed of 80 rpm. Three samples were ground to

approximately 60% passing 75 m under the conditions of dry milling,

as well as wet milling with pulp concentrations of 66% and 90% solids.

During dry milling, nitrogen was fed to the mill to drive off oxygen

before milling started. The grinding results are as follows: dry milling

took 40 min to result 58.0% of 75 m. The dry ground sample had a

specic surface area of 1.23 m2/g. Wet milling at a pulp concentration

of 66% solids took 30 min to ensure that 57.5% of the sample passed

75 m. This sample had a specic surface area of 1.29 m2/g. Wet

Fig. 6. Topographic of the sulde particle surfaces by SEM: (a) wet grinding with 66% solids (% 75 m = 58.0, surface area = 1.23 m2/g) (b) wet grinding with 90% solids

(% 75 m = 57.5, surface area = 1.29 m2/g) and (c) dry grinding (% 75 m = 58.5, surface area = 1.25 m2/g) (after Feng and Aldrich, 2000).

186

of 75 m. This sample had a specic surface area of 1.25 m2/g.

Topographical examination of the ground particle surfaces by

scanning electron and atomic force microscopy showed that the dry

ground samples had relatively rough particle surfaces with a high

concentration of microstructural defects. The wet ground samples had

smoother, cleaner surfaces as shown in Fig. 6. Higher stresses were

included in the particles in the denser slurry (90% solids) and as a

consequence some defects also appeared on these particle surfaces.

When the same new surface formed, dry grinding consumed more

energy than wet grinding. This means that the particles in the dry

grinding conserved more energy, some of which existed in the form of

defects. These defects serve as active centers for spreading up particle

dissolution and reagent adsorption (Feng and Aldrich, 2000).

As a result, the activated particle surfaces from the dry ground ore

accelerate the dissolution of the particles, as well as, the adsorption of

reagents onto the particle surfaces. The dry ground samples exhibited

more stable, higher loaded froths and faster otation kinetics, owing

to the activated particle surfaces. High intensity conditioning of the

dry ground ores prior to otation could improve otation by cleaning

the particle surfaces through high shear force elds in the pulp.

Moreover, by combining dry and wet grinding, the kinetics, as well as,

the nal grades and recoveries of the suldes, could be improved as

shown in Figs. 7 and 8 (Feng and Aldrich, 2000).

Sand samples were ground under dry and wet milling conditions.

Dry milling took 50 min to ensure that 75% by mass of the sample

passed 75 m. The dry ground sample had a specic surface area of

1.68 m2/g. Wet milling at a pulp concentration of 66% solids took

37 min to ensure that 75% by mass of the sample passed 75 m. The

wet ground sample had a specic surface of 1.76 m2/g. Dry milling

consumed approximately 25% more energy than wet milling to

achieve more or less similar surface areas. Some of the energy

absorbed in the dry milling process was owed to particle deformation,

which was stored in the form of surface defects on the particles. In

addition, the particle surface was activated in the dry milling process.

The wet ground sample had a smooth particle surface and few loose

ne particles absorbed onto the surface, while the dry ground sample

had a rough particle surface and many small particles attached onto

the surface. Some defects appeared on the particle surface in the dry

ground sample, and these surface defects served as the active centers

during reagent adsorption. As illustrated in Fig. 9, the dry ground sand

showed signicantly faster otation kinetics and a slightly higher

otation yield than the wet ground sand. This demonstrates that dry

milling could improve otation kinetics, owing to the higher energy

absorbed in the particles (Feng and Aldrich, 2000).

In practice, dry milling of sulde ores is complicated by the

tendency of ne suldes to oxidize in air. This is not the case with

Fig. 7. Variations of sulfur recovery with otation time (after Feng and Aldrich, 2000).

Fig. 8. Variations of sulfur content with otation time (after Feng and Aldrich, 2000).

against the enhanced otation kinetics (Feng and Aldrich, 2000).

with wettability

Spreading of liquids on rough surfaces was studied experimentally

and theoretically. Seven liquids, with viscosities spanning over a few

orders of magnitude, were used on glass surfaces of ve different

values of average roughness, ranging from about 0.07 to about 40 m.

It is shown that the experimental data can be empirically correlated

by a power law. In addition, a simple theoretical model was presented,

which took into account the capillary ow of liquid into the roughness

grooves. Results of the theoretical calculations were shown to be in

good agreement with the experimental data (Apel-Paz and Marmur,

1999). The study of spreading on practical rough surfaces is difcult,

because the problem of dening roughness is a complex one.

Therefore, much work was done on spreading on surfaces with

well-dened grooves or roughness. Nonetheless, some measurements

of the kinetics of spreading of liquids on practical rough surfaces were

also made. These studies revealed that spreading of the liquid occurs

by two modes: on top of the rough surface and inside the capillary

grooves (Apel-Paz and Marmur, 1999).

At any interface between two phases (e.g. liquidsolid, liquidgas,

oilwater), the adjacent interfacial multi-molecular layers are subjected to an unsymmetrical force and consequently the interfacial

tension is the net result of these forces (Hazlett, 1990). Quantication

of the effect of surface roughness is difcult and somewhat

Fig. 9. Flotation result of sand samples under different milling environments: (a) wet

milling with 66% solids (% 75 m = 75.0, surface area = 1.76 m2/g) and (b) dry

milling (% 75 m = 75.0, surface area = 1.68 m2/g) (after Feng and Aldrich, 2000).

contact angle which cannot be measured directly (Hazlett, 1993).

At sharp corners, the contact angle can be assumed as a range of

values. Wenzel recognized this difculty and approached the problem

in terms of surface energies. Wetting of a solid surface occurs only if

there is a resulting decrease in free energy. The apparent equilibrium

contact angle is then determined by an integrated surface of uid

uid interaction and not by the conditions existing only at the point of

contact (Hazlett, 1990).

It is stated that the contact angle is dependent on the surface

roughness (Onda et al., 1996). The apparent contact angle for rough

surfaces could be expressed in terms of smooth surfaces (Hazlett,

1990 and Onda et al., 1996). The modication of the wettability due to

surface roughness can be greatly enhanced in the fractal surface; that

is the fractal surface will be superrepellent (superwettable) to a liquid

when the contact angle is greater (less) than 90 (Onda et al., 1996).

In a paper published by Ulusoy et al. (2003), experimental studies

to determine the shape properties, surface roughness and wettability

of quartz mineral (a very common component of many raw materials)

were performed for the products of ball, rod and autogenous mills.

Shape properties have been stated in terms of shape descriptors such

as elongation, atness, roundness and relative width. The measurements were carried out on the projections of particles using the

scanning electron microscope (SEM). Surface roughness values have

been determined on the pelleted surfaces of the ground powders. The

wettability characteristics (critical surface tension of wetting) of

quartz mineral were determined by micro-otation technique using

the EMDEE Micro-FLOT test tube. Finally, some correlations were

found between the shape properties, surface roughness values and

wettability. The results have shown that the critical surface tension of

wetting values increases with increasing roughness and roundness,

i.e. elongated and smooth particles having lower critical surface

tension of wetting values. This means that these particles have higher

hydrophobicity (Ulusoy et al., 2003).

A new method for the measurement of apparent contact angles on

real surfaces was developed. The method consists of vibrating the

surface, taking top-view pictures of the drop, monitoring the drop

roundness, and calculating the contact angle from the drop diameter

and weight. The use of this new method was demonstrated for various

rough surfaces having the same surface chemistry. In order to

establish the optimal vibration conditions, the proper ranges for the

system parameters (i.e., drop volume, vibration time, frequency of

vibration, and amplitude of vibration) were determined. The

reliability of the method was demonstrated by the fact that the

ideal contact angles of all surfaces, as calculated from the Wenzel

equation using the measured apparent contact angles, came out to be

practically identical. This ideal contact angle was compared with three

methods of calculation from values of advancing and receding contact

angles (Meirona et al., 2004).

In many systems there exists a contact angle hysteresis between

an advancing and receding contact angle, i.e. a different contact angle

may be measured depending upon whether the three-phase contact

(TPC) line is advancing or receding over a particle surface. The reason

for this hysteresis is generally ascribed to roughness and heterogeneity of the surface chemistry, although other factors may be of

importance, such as polymer coatings, etc. (Johnson et al., 2006).

7. Effect of the particle shape and surface roughness on the

otation behavior

The particle shape and its surface roughness have signicant

effects on the otation behavior. Many researchers have studied these

phenomena qualitatively (Anfruns and Kitchener, 1997; Varbanov,

1984; Blake and Ralston, 1985; Ducker et al., 1989; Silverstein and

Breuer, 1993; Schmidt and Berg, 1996 and Schmidt and Berg, 1997),

but few researchers (Burstein et al., 1995) studied these phenomena

187

measure them by quantied parameters. Ramesh and Somasundaran

(1990) decided that the shape of the particle has a substantial effect

on the force required to detach the particle from the gasliquid

interface. They found that homogeneous particles with a single

specic geometry would yield a single value for the detachment force.

On the other hand, a mixture of particles having the same contact

angle and a variety of shapes would yield a distribution of detachment

forces. Burstein et al. (1995) showed that the otation recoveries of

non-spherical particles are higher than that of spherical particles. A

possible explanation of this result might be attributed to the increase

of surface of non-spherical particles which leads to more adsorption of

surfactant and hence increasing otation recovery. This result is in a

conict with the result of Varbanov (1984) who concluded that, with

regard to practical otation, no major differences could be inferred

between the behaviors of spherical and non-spherical particles.

Schmidt and Berg (1996) investigated the role of particle shape on

otation using model particles of spherical and disc shapes. Their

results revealed that spherical particles oat better than disc or platy

particles. Spheres are deected away from bubble by ow but usually

attach if they contact the bubble surface. Discs often colloid with the

bubble edge-on and immediately bounce off and seldom attach to the

bubble due to the very short contact time. Alternatively, discs turn to

the side as they approach the bubble but seldom attach due to the

large thin lm drainage area. Schmidt and Berg (1997) in other

publication using a hydrodynamic model concluded that disc and

plate-shaped particles behave differently more than spherical

particles. Large disc-to-bubble ratios (N0.1) yield always greater

collision efciencies than those for equivalent spherical particles.

They found also that the large discs have always a lower probability of

attachment than equivalent spheres due to the higher tendency of

discs to bounce off the bubble surface after collision. For smaller discs,

the differences in the attachment efciency and otation behavior

between discs and spheres decrease and collision efciency become

the predominant step.

Wotruba (1991) in his Ph.D. thesis studied the inuence of corn

shape on the oatability of zirconium and microlith particles in a

pneumatic otation cell using prismatic, spherical and ellipsoidal

shapes. The most important conclusions of this thesis are that the corn

shape has an essential inuence on the oatability of zirconium.

Spherical and ellipsoidal particles have less oatability than prismatic

particles, independent of whether the spherical particles are rough or

not. The rst reason for this behavior is that the attachment process

with bubble is more difcult for spherical particles as compared to the

prismatic particles. The second reason is that the retreatment in the

liquid phase causes easier wetting on spherical particles than on

prismatic particles with edges. The strong inuence of the shape on

the oatability occurs at the range of (63 + 40) m, i.e. in a range

where the inuence of the turbulence on the stability of the particle/

bubble aggregate is not critical.

Few scientists studied the effect of surface roughness on the

otation process (Anfruns and Kitchener, 1997; Silverstein and

Breuer, 1993 and Burstein et al., 1995). Burstein et al. (1995)

concluded that the increase in the particle roughness (determined

in fractal terms) causes signicant intensication of the process of

collapse of lamellae near particle surfaces and reduction of froth

stability. Anfruns and Kitchener (1997) revealed that the particle

roughness ensures easy rupture of the wetting lm even when the

barrier is strengthened by the addition of low concentrations of

surfactant or when the contact angle is reduced from 87 to 30.

Ducker et al. (1989) have studied the otation of glass ballotini and

ground ballotini using a double-chained cationic surfactant. They

concluded that there are large differences in the otation properties of

these two materials. They interpreted these differences to the

difference in surface roughness between glass ballotini and ground

ballotini and not to the difference in their shapes. Anfruns and

188

and capture between the angular and smooth particles. They showed

that the strongly hydrophobic angular quartz particles are captured by

bubbles with 100% efciency whereas the capture efciency of

strongly hydrophobic glass ballotini particles is very much lower.

The 100% capture efciency of angular particles is attributed to the

jagged projections or asperities on the particle surface which are

leading to a local thinning and rupture of the wetting lm, i.e. the

otation rate is enhanced compared to the smooth surface of glass

ballotini. Anfruns and Kitchener (1997) also observed, for smooth

particles, that although the static contact angle is 30, they are not

captured at all. They concluded, with smooth particles, that the

capture rate is more sensitive to the operation of electrical doublelayer forces during the thinning of the liquid lm.

Ahmed et al. (1998); Ahmed (1999); Ahmed et al. (1999) and

Stechemesser and Ahmed (1999) illustrated a modern and useful

approach, which is considered the rst attempt, to study the

quantitative effect of the surface roughness and shape of particles on

the detachment process from the airliquid-interface by means of a

centrifuge technique and also on their oatability (under ideal

conditions) using a modied Hallimond tube. His study was carried

out on four different materials (spherical soda-lime-glass ballotini,

ground ballotini, glass sand and quartzite) of the same particle size

fraction (315 + 250) m. For estimation of the surface roughness of

the particle, three parameters used are as follows: textural fractal

dimension (Ft), factor of convexity (FO) and factor of concavity (CONC).

The following parameters are of interest for identifying the shape of

particle: structural fractal dimension (Fs) and factor of circularity (FK).

The values of studied parameters are determined by means of the

software IMAGE_C. The estimation of particle geometry was made as a

two-dimensional analysis of the digitized particle projection on a slide

in the position of the greatest stability. According to Kaye (1994), the

average structure is described with a sufcient precision at the position

of the greatest stability of the particle. From the results, it was found that

the four materials investigated are different in surface roughness of

particle. On the contrary, the particle shape of ground ballotini and the

quartzite is the same in comparison to the other materials investigated.

Nguyen et al. (1997a) have made a detailed analysis of the particle/

bubble attachment. There are three microprocesses (or elementary

steps) for the before-contact stage which may occur for successful

particle/bubble attachment:

1. thinning of the intervening liquid lm to a critical thickness where

the lm rupture begins,

2. rupture of the intervening liquid lm, i.e. formation of the threephase contact of a critical wetting radius (a hole) and,

3. expansion of the three-phase contact line from the critical radius to

form a stable wetting perimeter.

Schulze et al. (1989) have decided that in the technological

otation process, the three microprocesses mentioned above occur

simultaneously. Therefore it is impossible to determine unambiguously from the temporal course and the efciency of the total process

which one of the microprocesses is signicant in the course of the

process. Consequently this problem must be solved by investigating

the individual microprocesses separately.

Fig. 10 illustrates the effect of the surface roughness of particle

(quantied by the textural fractal dimension) on otation recovery at

different degrees of hydrophobicity. From this gure, it can be seen

that as the textural fractal dimension increases, the otation recovery

increases linearly at different degrees of hydrophobicity. Similar

relationships between the surface roughness (quantied by the factor

of convexity and the factor of concavity) and otation recovery were

also obtained (Ahmed, 1999 and Stechemesser and Ahmed, 1999).

From Fig. 10, it can be seen that the differences in the values of

otation recovery between the roughest material (quartzite) and the

smoothest material (soda-lime-glass ballotini) range from 24% (at

contact angle = 71) to 33.5% (at contact angle=78). This means

that although the small differences in the values of textural fractal

dimension of materials were examined, very great signicant

differences in the values of otation recovery between the smoothest

and the roughest material were obtained. This assures that the effect

of the surface roughness on the otation recovery is signicantly

effective.

From the previous results, it can be concluded that the roughness has

a signicant effect on the otation recovery. This may be attributed to

the fact that larger detachment forces are required to separate the rough

particle from bubble than to separate the smoother particle. The larger

detachment forces will indicate a strong adhesion force for the bubble

particle aggregates, which could reserve these aggregates to reach

the oat receiver and hence higher recovery is obtained (Ahmed et al.,

1999; Ahmed, 1999 and Stechemesser and Ahmed, 1999).

Fig. 10. Effect of the surface roughness of particles (quantied by the textural fractal dimension) on the otation recovery at different degrees of hydrophobicity (after Ahmed, 1999).

189

Fig. 11. Effect of the shape of particles (quantied by the structural fractal dimension) on the otation recovery at different degrees of hydrophobicity (after Ahmed, 1999).

the detachment process and then the effectiveness of otation

processes. This relationship is attributed to the larger values of

three-phase contact perimeter for rough particles more than the

smooth particles. Accordingly, a longer time, i.e. a larger detachment

force is required to separate the particles from the gasliquid interface

for rough materials more than that for the smooth materials (Ahmed

et al., 1999; Ahmed, 1999 and Stechemesser and Ahmed, 1999). This

interpretation is equivalent to the process of expansion of the threephase contact line on the surface of hydrophobic particle to attain the

dewetting case. In this process, Nguyen et al. (1997b) have observed

experimentally that the time of three-phase contact line expansion is

a function of the central angle, i.e. the radius of three-phase contact

line. From this result it was concluded that a particle with a larger

three-phase contact radius needs a longer time to arrive to the

dewetting case. This conclusion was exploited to support the results

mentioned above. In the detachment experiments (Ahmed et al.,

1999; Ahmed, 1999 and Stechemesser and Ahmed, 1999), a

contraction of three-phase contact line is occurring. This contraction

on the particle surface is leading to attain to the wetting case and

hence the particle is submerged into the liquid. This contraction needs

a longer time and then larger detachment forces (larger three-phase

contact perimeter) in the case of rough particles.

7.2. Effect of the particle shape on oatability

Fig. 11 shows the effect of the particle shape (quantied by the

structural fractal dimension) on otation recovery of the materials

examined at different degrees of hydrophobicity. From this gure, it

can be seen that as the structural fractal dimension increases from

1.020 to 1.043, the otation recovery slightly increases. Above this

value, any increase in the structural fractal dimension causes

signicant increase in otation recovery. This behavior is the same

at all the degrees of hydrophobicity (Ahmed, 1999 and Stechemesser

and Ahmed, 1999). Fig. 12 illustrates the effect of particle shape

(quantied by the factor of circularity) on otation recovery at

different degrees of hydrophobicity. From this gure, it can be seen

that as the particle shape increases (decreasing of the factor of

circularity), the otation recovery increases up to a certain point

above which an excessive increase in the particle shape will result in a

Fig. 12. Effect of the shape of particles (quantied by the factor of circularity) on the otation recovery at different degrees of hydrophobicity (after Ahmed, 1999).

190

decrease in the nal otation recovery. It can be also noticed that the

relationship between the particle shape and otation recovery has the

same behavior at all degrees of hydrophobicity (Ahmed, 1999 and

Stechemesser and Ahmed, 1999).

Comparison of the results shown in Figs. 11 and 12 displayed that

there is a clear difference in the behavior of otation recovery with the

particle shape (if this shape is quantied by the structural fractal

dimension or the factor of circularity). This means that the particle

shape is not as effective as the surface roughness in controlling the

otation recovery. This result may be ascertained also from Fig. 11. In

this gure, it can be observed that although the structural fractal

dimensions of ground ballotini and quartzite are almost the same

(these materials have the same shape), they have different otation

recoveries (Ahmed, 1999 and Stechemesser and Ahmed, 1999).

Figs. 11 and 12 showed also that the otation recoveries of ground

ballotini are higher than that of spherical ballotini at all degrees of

hydrophobicity. One of the possible explanations of this result may be

attributed to the increase of the particle surface with the rise of

structural fractal dimension of ground ballotini which leads to more

adsorption of surfactant (Burstein et al., 1995) and hence the increase

of otation recovery (Ahmed et al., 1999 and Ahmed, 1999). Other

reasons for this behavior are that the attachment with bubble is more

difcult for the spherical particles compared to the non-spherical

particles. The second reason is that the retreatment in the liquid phase

causes easier wetting on spherical particles than on non-spherical

particles (Wotruba, 1991). Ducker et al. (1989) interpreted these

differences to the difference in the surface roughness between glass

ballotini and ground ballotini and not to the difference in their shapes.

8. Conclusions

1. Particle shape and surface roughness are considered important

parameters in the prediction of the behavior of particle and powder.

2. The methods used to assess the particle shape and surface

roughness range from very simple methods such as the aspect

ratio, elongation ratio or circularity to very modern methods such

as Fourier analysis, delta analysis and fractal geometry.

3. The development of automated microscope techniques linked to

computer data-processing systems (image analysis techniques)

facilitate the possibility of specifying the particle shape and surface

roughness by mathematical procedures.

4. Particles of the impact crushing have higher boundary fractal

dimensions than the rotary milled particles.

5. The dry ground samples are more stable and have higher loaded

froths and faster otation kinetics. These samples have relatively

rough particle surfaces while the wet ground samples have

smoother and cleaner surfaces.

6. The contact angle is dependent on the surface roughness. At sharp

corners, the contact angle is assumed as a range of values. The

fractal surface will be superrepellent (superwettable) to a liquid

when the contact angle is greater (less) than 90.

7. There are large differences in the otation properties of glass

ballotini and ground ballotini due to the difference in surface

roughness.

8. The particle shape does not control clearly the otation recovery.

The surface roughness is responsible for the detachment process of

particle and the nal otation recovery more than its shape.

Nomenclature

maximum breadth of the prole projection on a direction at

BM

a right angle in which LM is measured

c

constant

DA

particle diameter of a circle of equal area

DEM

diameter of the embracing circle

D(Fmax.) Feret's diameter of the particle

Di

distance from the centroid of a particle to its edge

directions

F

fractal dimension

distance of the corner from the center of the maximum

gij

inscribed circle of radius ri for each of the three sections

through the long, intermediate and short axes of the prole

LCNV

circumference of the convex envelope of the particle

LENG

circumference of the particle projection

maximum length of the prole

LM

L(r)

particle perimeter length at step length (r)

number of concave corners of the particle

ncor

number of edges of the particle

nedg

r

step length

R

maximum inscribed radius of the particle

average particle radius (average over 180 two-degree

Ravg

increments)

radii of the curvature of ncor. (corners) of a projection or

Ri

section of the particle

angle of each corner

ij

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