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Characterisation of elastomer prepared from ground tyre rubber:

Morphological and granulometric study

Article  in  Plastics Rubber and Composites · June 2009

DOI: 10.1179/174328909X388026

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Characterisation of elastomer prepared from
ground tyre rubber: morphological and
granulometric study
C. Ferrer-Giménez1, J. López-Martı́nez1, A. Nadal-Gisbert1, E. M. Cuerda-Correa2
and A. Macı́as-Garcı́a*3
The characterisation of an elastomer prepared from ground tyre rubber has been carried out in
terms of both morphological and granulometric studies. A large number of waste tyres are
discarded every year. These residuals represent a crucial environmental problem. Thus, the
redemption and recycling of waste tyres constitute a research field of great interest nowadays. In
this connection, the study of the size distribution of particulates is of the utmost importance. In the
present work, the morphological study of a ground tyre rubber previously prepared has been
carried out. The use of SEM techniques indicates that the powder is not completely uniform. The
granulometric study of the powder was carried out by applying the Rosin–Rammler and Gates–
Gaudin–Schuhmann models. The particle size distribution of the sample here studied
satisfactorily fits the Rosin–Rammler model, especially for mesh sizes above 0?250 mm.
According to the results of this study, a homogeneous behaviour of the sinterised product
during the thermocompression process is expected.
Keywords: Granulometry, Particle size distribution, Elastomeric residual powder

Introduction (PSD) analysis of a material may be obtained depending

Over 330 million waste tyres are discarded every year.1
Ground tyres can be used in civil engineering applica-
tions, for example as an additive in road pavement.2
Other applications include playground surface,3 rubber
roofs,4 drainage systems5 and floor mats.6 A major
market for scrap tyres is their utilisation as solid fuels,7
especially in cement kilns.8 In spite of these applications,
tyres are frequently dumped in the open. Trituration is
the first step in the processing of used tyres. The product
obtained from this step is commonly referred to in the
literature as recycled vulcanised particle rubber, crumb
rubber and ground tyre rubber (GTR).9–11 This latter
denomination will be used hereafter in the present work.
Many methods, of varying complexities, have been
developed to determine the size distribution of particu-
lates.12–20 Particle size influences a number of para-
meters of powder materials and is commonly considered
to be one of the most important single physical
characteristics. It is to be noted that radically different
information concerning the particle size distribution
1
Departamento de Ingenierı́a Mecánica y de Materiales, Escuela
Politécnica Superior de Alcoy. Paseo del Viaducto, 1. E-03801-Alcoy,
Spain
2
Departamento de Quı́mica Inorgánica, Universidad de Extremadura,
Avda de Elvas s/n. E-06071-Badajoz, Spain
3
Departamento de Ciencia de Materiales, Universidad de Extremadura,
Avda de Elvas s/n. E-06071-Badajoz, Spain
*Corresponding author, email amacias@materiales.unex.es
on the characterisation techniques used.21–23 Hence, the
election of the analysis technique will depend on the
ultimate goal of the characterisation. Different forms
may be used to express the results of a PSD analysis.
Among these forms, the most usual ones are binning by
particle diameter indicating the nominal mesh sizes, or
by PSD, in grams or in percentage by weight of each
fraction [differential distribution, as the cumulative
percentage of sizes below a given value (undersize) and
as the cumulative percentage of size above a given value
(oversize)].24,25
The aim of this work was to carry out the
morphological study of a GTR previously prepared as
well as to obtain the distribution function F(w) (mass
fraction) and density function f(w) (the number of
particles binned between two given mesh sizes) of a
GTR sample by applying the Rosin–Rammler (RR) and
Gates–Gaudin–Schuhmann (GGS) mathematical mod-
els to the PSD data obtained by sieving through
different size meshes.26
Materials and experimental methods
Preparation of samples
Samples were prepared from tyre waste. A star or tooth
mill was used to grind the raw material in order to yield
a granulate of suitable particle size and to make a
preliminary elimination of impurities. A further reduc-
tion of particle size and separation of impurities was

ß Institute of Materials, Minerals and Mining 2009

Published by Maney on behalf of the Institute
Received 5 August 2007; accepted 21 April 2009
DOI 10.1179/174328909X388026 Plastics, Rubber and Composites 2009 VOL 38 NO 5 195
Ferrer-Giménez et al. Characterisation of elastomer prepared from GTR

carried out, passing the product through a hammer mill. vibrating table. In order to optimise the process, two
The purified granulate was then passed through a blade different intensities of the vibration power, namely 40
mill to yield the final different PSDs. and 67% were applied. In both cases the experimental
Particles above 1 mm diameter find commercial time was equal to 15 min.
applications, whereas those with diameter below The resulting values allow one to obtain the experi-
0?200 mm possess little practical interest. The present mental PSD curves. These represent the percentages by
study focuses on the latter kind of powder, as it presents weight versus particle size.
a high added value due to the number of steps involved The application of mathematical models to the
in its treatment. experimental data of PSD curves makes it possible to
obtain the corresponding distribution and density
Morphological study functions. A bibliographic revision reveals that the most
A JEOL/JSM6300 scanning electronic microscope commonly used models are the RR and GGS.28–30 The
(SEM) of acceleration voltage comprised between 1 RR model is particularly suited to represent powders
and 170 kV and 3 nm maximal resolution was used. The obtained by grinding, milling and crushing operations.
samples were placed in the film deposition equipment in In many grinding cases, mainly during the last stages of
order to be covered by a carbon film, which enables its the process, the cumulative PSD is found to follow the
study under the SEM equipment. RR equation, the parameters of which can be used as
The shape of the particles was analysed by measuring essential criteria to the operation progress.31 This model
different shape parameters, namely shape factor SF,
has been applied to a number of particulate systems such
elongation x and size y as described by Exner27
as stream sediments and mine tailings,32 bovine serum
SF was calculated as
albumin based microspheres,33 circulating fluid bed
C2 boiler ashes34 and pharmaceutical aerosols,35 etc. On
SF ~ (1) the contrary, the applicability of the GGS model
4pA
appears to be limited to the field of metallurgy.36,37
where A and C are area and perimeter of the particles
Hence, the experimental data have been fitted to the RR
respectively.
model, the GGS one being applied for comparative
Elongation x and size y were calculated as
purpose only.
a The distribution function provided by the RR model
x~ (2)
b is

m 
A w
y~ (3) F(w)~1{exp { (4)
ab l
where a and b are the width and height of a given where F(w)is the distribution function, w is the particle
particle. Such parameters were measured by considering diameter and m is a characteristic parameter of the
the particle as inscribed inside a rectangle. Next, the granulometric distribution. A non-linear regression of
diagonals of such a rectangle were used to calculate its the F(w) plot has been carried out in order to test the
width a and height b. Thus, a particle inscribed inside a applicability of the RR distribution function to the PSD
square (i.e. a5b) would lead to a value of elongation as well as to calculate its fitting parameters. The
x51. This value may correspond either to a square or to correlation coefficient may be used as the parameter
a circle but, in any case the particle would show for goodness of fit.
equiaxial symmetry. The density function in the RR model will be
The size factor y describes the degree of occupation of 
m 
a given particle inside the rectangle within the particle is m m{1 w
f(w)~ m w exp { (5)
inscribed. Hence, a perfectly square-shaped particle l l
would present a value of y51. The same applies to a
perfectly rectangular particle. On the contrary, a circular Table 1 Values of elongation, size and shape factor
particle would show a value of y,1. corresponding to square, circle and rectangle*
The shape factor SF is indicative of the sharpness of Factor Circle Square Rectangle (a51.5b)
the particle. A value of SF51 corresponds to a circle and
SF51?27 to a square, whereas values approaching Elongation x 1 1 1.5
infinite indicate straight lines. Hence, sharp particles a
x~
showing large values of perimeter C and small values of b
Size factor y 0.79 1 1
area A would lead to very large values of SF. A
As an example, the values of elongation x size factor y y~
ab
and shape factor SF calculated for a circle, a square and Shape factor SF 1 1.27 1.33
a rectangle (for which a has been considered to be equal C2
SF ~
to 1?5 times b) are shown in Table 1. 4pA
*a5width; b5height; A5area; C5perimeter. (see diagram below)
Granulometric study
The granulometric study of the sample was carried out
with the aid of a sieves tower CISA RP.09, by weighing
the quantity of sample retained in each sieve. Stainless
steel sieves, having mesh sizes equal to 0?063, 0?100,
0?125, 0?250, 0?500, 1?000, 1?25 and 2?000 mm were used
in the present study. The tower was placed on a

196 Plastics, Rubber and Composites 2009 VOL 38 NO 5

 Ferrer-Giménez et al. Characterisation of elastomer prepared from GTR

1 Images (SEM) of powder retained by a,c 125 mm and b,d 250 mm sieves

The use of the RR model may provide valuable help to
carry out the modelling during the design phase of
milling circuits. For instance, it facilitates making
correct use of the particle sizes to obtain more
homogeneous cork agglomerate samples in the cork
industry.38 On the other hand, as indicated above, the
GGS equation has found favour in the metaliferous
mining industry since 1940 due to its relative uncompli-
cateness. Such an equation is defined as


w m
F(w)~ (6)
wmax
where F(w) is the fraction of the sample finer than size w,
w is the particle diameter, wmax is the maximum particle
diameter of the distribution (size modulus), and m
(distribution modulus) is an adjustable parameter.
Again, a non-linear regression software has been used
in order to test the applicability of this model to the
samples under study in the present work. Analogously
to that exposed in the RR model, a GGS density
function may be defined
mwm{1
f(w)~ (7)
wm
max
Results and discussion
Morphological analysis
Figure 1a and b shows the SEM images of the
granulometric distribution in the 0?125 and 0?250 mm
sieves at a magnification of 680. From both images a
variation in the sizes of the particles retained in the sieve
may be observed. Figure 1c and d show the aforesaid
granulometric distribution observed at a magnification
of 6200. Several shapes and sizes may be observed in
these images. Thus, the morphology of the elastomer is
not homogeneous. Moreover, the grains appear to be
covered by a certain amount of fine powder.
Since, as exposed below, over 97% of the GTR sample
is retained in the 0?125, 0?250 and 0?500 mm sieves, the
shape parameters (i.e. elongation, size factor and shape
factor) have been determined only for the fraction of
sample retained in these mesh sizes. Table 2 summarises
these parameters together with their corresponding
typical deviations. The weighed average and typical
deviation of each of the shape parameters have also been
included in this table.
The values of the elongation x summarised in this
table suggest that the particles cannot be considered as
equiaxial. However, the sample fractions retained in the
0?125 mm and 0?500 meshes tend to be more homo-
geneous in terms of equiaxiality than that retained in
the 0?250 mm sieve. This assertion is corroborated by
the SEM images depicted in Fig. 1. On the other hand,
the value of the size factor is, in all cases, below the ideal
value corresponding to a circle (i.e. 0?785). This fact is
attributable to the irregular serrated edge of the particles
as a consequence of the grinding procedure. This leads
to a less efficient occupation of the circumscribed
rectangle and, thus, to lower values of the size factor.

Table 2 Values of shape factor corresponding to three different mesh sizes

Mesh size

0.125 mm 0.250 mm 0.500 mm Weighed average

Factor x y SF x y SF x y SF x y SF

Average 1.191 0.656 1.486 1.321 0.691 1.326 1.140 0.581 1.635 1.222 0.630 1.495
Typical deviation 0.176 0.108 0.160 0.066 0.139 0.132 0.146 0.100 0.053 0.099 0.119 0.128

Plastics, Rubber and Composites 2009 VOL 38 NO 5 197

Ferrer-Giménez et al. Characterisation of elastomer prepared from GTR

3 Plot of distribution function versus particle size

2 Particle size distribution curve obtained by sieving

Finally, the values of the shape factor are, in all cases,
above that corresponding to a rectangle for which
a51?5b (i.e., SF51?32, see Table 1). This fact confirms
the predominance of non-equiaxial oblong forms.
The determination of the shape parameters provides
an useful information regarding the eventual behaviour
of the samples in different industrial processes such as
the thermal compaction by sintering. In this connection,
it must be born in mind that the main factor that
conditions the initial step of the compaction process is
the sliding of particles on each other. The values of the
shape parameters summarised in Table 2 suggest that
the GTR sample here studied presents favourable
characteristics to be thermally compacted. Further-
more, due to the elastomeric nature of the GTR powder
the elastic deformations start at relatively low compac-
tion pressure39,40 thus favouring the trend of the powder
to adopt less oblong and more spherical shapes.
Consequently, the friction coefficient decreases and the
compaction degree of the product increases.
Large values of the shape factor and small values of
size factor, as it is the case in the present study, result in
the presence of a large number of contact points between
the solid particles during the sintering process. Hence,
the mechanical resistance of the sintered product
increases noticeably due to the revulcanisation process
that takes place, mainly, in the contact points between
the particles.41,42
Particle size analysis
Table 3 summarises the values of the weights of the
different particle sizes obtained in the sieving operations,
as well as the cumulative percentages by weight. The
corresponding PSD curve is depicted in Fig. 2, which
shows that most of the sieved mass is retained in three
sieves (i.e. those of mesh size equal to 0?250, 0?500 and
1?000 mm). As expected, an increase in the stirring
power results in a slight variation of the size distribution
to lower values of mesh size. Thus, for the experiments
carried out at 40% stirring power, the cumulative mass
percentage equals 97?4% for the above mentioned sieves,
whereas at a higher value of stirring power (i.e. 67%)
96?8% of the total mass is retained in such sieves.
The distribution function, F(w), obtained by fitting the
experimental results of Fig. 2 to equation (4) is depicted
in Fig. 3. This function may represent the fraction by
volume, by mass, or by the number of particles. The
value of the function at a given point represents the
fraction of the number of particles (mass or volume) that
is below a given size.
On the other hand, the number of particles (expressed
as particle mass or volume) whose diameters are
comprised between two sizes (i.e. w1 and w2) is given
by the area under the curve in that interval
ð w2
F(w2 ){F(w1 )~ f(w)d(w) (8)
w1

Table 3 Particle size distribution of GTR

Cumulative percentage Cumulative percentage

Sample Range of sizes, mm Mesh size, mm Fraction, g Fraction, % (under weight), % (over weight), %

P-40% ,0.063 0.063 1.0 0.50 0.50 99.50

0.063–0.100 0.100 1.2 0.60 1.10 98.90
0.100–0.125 0.125 2.1 1.05 2.14 97.86
0.125–0.250 0.250 70.1 34.89 37.03 62.97
0.250–0.500 0.500 84.5 42.06 79.09 20.91
0.500–1.000 1.000 41.0 20.41 99.50 0.50
1.000–1.250 1.250 0.9 0.45 99.95 0.05
1.250–2.000 2.000 0.1 0.05 100.00 0.00
P-67% ,0.063 0.063 0.4 0.20 0.20 99.80
0.063–0.100 0.100 0.4 0.20 0.40 99.60
0.100–0.125 0.125 0.8 0.40 0.80 99.20
0.125–0.250 0.250 65.1 32.52 33.32 66.68
0.250–0.500 0.500 83.4 41.66 74.98 25.02
0.500–1.000 1.000 45.3 22.63 97.60 2.40
1.000–1.250 1.250 4.4 2.20 99.80 0.20
1.250–2.000 2.000 0.4 0.20 100.00 0.00

198 Plastics, Rubber and Composites 2009 VOL 38 NO 5

 Ferrer-Giménez et al. Characterisation of elastomer prepared from GTR

Table 5 Fitting parameters of RR and GGS models

Rosin–Rammler Gates–Gaudin–Schuhmann

Parameter P-40% P-67% Parameter P-40% P-67%

l 0.3923 0.4192 wmax 1.4452 1.4728

m 2.1636 2.1662 m 0.5908 0.6143
R2 0.9942 0.9939 R2 0.8320 0.8438

"
2:17 #
w
F(w)~1{exp { : (10)
0 42

As expected, only a slight difference in the values of the

4 Plot of density function versus particle size
The density function, f(w), defined by equation (5) and
plotted in Fig. 4 corresponds to the slope of the
distribution function plotted versus the particle diameter
w at each point. In other words, this function represents
the differential curve corresponding to the percentage of
particles of a certain size. The presence of a PSD curve
analogous to that shown in Fig. 2 indicates that the
material under study is well suited to be analysed using
this type of model.
The two above-described models were applied to the
experimental results given in Table 3 and depicted in
Fig. 2. Table 4 summarises the distribution and density
functions of the samples, whereas the fitting parameters
of the RR and GGS models are listed in Table 5. From
the values of the correlation coefficients R2 it may be
concluded that the RR model provides a better fitting
than the GGS for the PSD of the samples here studied.
In fact, the RR model provides the best approximation
of the PSD of different kinds of materials, as previously
reported in the literature.43 Furthermore, the RR model
is the most commonly used function for approximation
of the PSD in Europe and several studies in the field
prove that this formula can give the best approach to the
PSD of the mass of ground industrial products.31
The resulting distribution functions obtained by
application of RR model are given by the following
expressions
for sample P-40%
"
: #
w 2 16
F(w)~1{exp { : (9)
0 39
for sample P-67%
fitting parameters l and m corresponding to both
samples is observed. Equations (9) and (10) have been
used to plot the solid lines depicted in Fig. 3. It may be
observed that, in both cases, the predicted values (solid
line) satisfactorily fit the experimental data for values of
w above 0?250 mm. Slight deviations occur for values of
particle sizes below 0?125 mm, probably due to a more
significant contribution of the experimental error.
On the other hand, the density functions obtained by
applying the RR model to the samples under study are
given by the following equations
for sample P-40%
"
2:16 #
:16 w
f(w)~16:38w exp { :
1
(11)
0 39
for sample P-67%
"
: #
1:17 w 2 17
f(w)~14:24w exp { : (12)
0 42
The density functions corresponding to both samples are
shown in Fig. 4. The application of the distribution and
density functions to the PSD data allows one to
extrapolate (with estimative purpose only) the percen-
tage of material smaller than a certain particle diameter
w at points that do not correspond to the sieving
classification system used, thus obtaining information at
the extremes of the particle size diagrams.
The experimental results here exposed have made it
possible to perform a precise characterisation of GTR
samples in terms of PSD. A number of mechanical and
rheological properties of particulated systems are
markedly affected by PSD. It is known that the
maximum packing fraction that this kind of systems
may achieve is the hexagonal close packing of 0?74,
although in practice, it rarely exceeds random close

Table 4 Distribution and density functions of samples

P-40% P-67%

Cumulative percentage (under weight), % w F(w) f(w) Cumulative % weight, under w F(w) f(w)

0.50 0.063 0.005 0.644 0.20 0.063 0.002 0.557

1.10 0.100 0.011 1.067 0.40 0.100 0.004 0.929
2.14 0.125 0.021 1.340 0.80 0.125 0.008 1.172
37.03 0.250 0.370 2.239 33.32 0.250 0.333 2.041
79.09 0.500 0.791 1.349 74.98 0.500 0.750 1.467
99.50 1.000 0.995 0.008 97.60 1.000 0.976 0.020
99.95 1.250 0.999 0.000 99.80 1.250 0.998 0.000
100.00 2.000 1.000 0.000 100.00 2.000 1.000 0.000

Plastics, Rubber and Composites 2009 VOL 38 NO 5 199

Ferrer-Giménez et al. Characterisation of elastomer prepared from GTR
packing of 0?639.44 Further research is being carried out
at present by the authors’ research group dealing with
the thermocompressibility of the GTR sample here
studied with promising results. The PSD has proved to
be a determinant factor in this connection.
Conclusions
From all the above exposed, the following conclusions
may be drawn.
1. The morphology of the elastomer is not completely
homogeneous and the grains are covered by a certain
amount of fine powder.
2. The serrated morphology of the powder is the
result of the cryogenic grinding procedure.
3. The use of SEM techniques indicates that the
particles of samples are mostly non-equiaxial.
4. The shape parameters (i.e. elongation, size factor
and shape factor) have been calculated by applying the
Exner method. This technique has demonstrated to be
efficient for the analysis of the morphology of the GTR
sample.
5. The morphological analysis performed according
to the Exner model indicates that the GTR powder
exhibits a moderate elongation degree, a low degree of
space filling and a moderate sharpness. These results are
corroborated by the SEM images.
6. The PSD of the sample satisfactorily fits to the RR
model. Since the granulometric distribution strongly
influences the characteristics of the sinterised product,
the fit of the PSD to a theoretical model allows one to
test the potential deviations from the ideal distribution.
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