Powder Technology 224 (2012) 19–27

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Powder Technology
journal homepage: www.elsevier.com/locate/powtec

Measuring the flowing properties of powders and grains

G. Lumay a, b, d,⁎, F. Boschini a, c, K. Traina a, c, S. Bontempi a, J.-C. Remy b, R. Cloots a, c, N. Vandewalle a, b
a
APTIS, Institute of Physics, University of Liege, Sart-Tilman, B-4000 Liège, Belgium
b
GRASP, Institute of Physics, University of Liege, B-4000 Liège, Belgium
c
LCIS-GreenMat, Institute of Chemistry, University of Liege, B-4000 Liège, Belgium
d
F.R.S.-FRNS, B-1000 Bruxelles, Belgium

a r t i c l e i n f o a b s t r a c t

Article history: A granular material is a complex system which exhibits non-trivial transitions between the static, the quasi-static
Received 7 February 2011 and the dynamical states. Indeed, an assembly of grains can behave like a solid or a fluid according to the applied
Received in revised form 23 September 2011 stress. In between solid and fluid granular states, very slow dynamics are observed. When a complete macro-
Accepted 11 February 2012
scopic characterization of a powder is needed, all these granular states have to be precisely analyzed. In this
Available online 19 February 2012
paper, we show how three measurement techniques can be used to measure the physical properties of a powder.
Keywords:
The measurements are based on classical tests modified to meet the recent fundamental researches on granular
Powder characterization materials. The static properties of the powder are analyzed through the shape of a heap. The quasi-static behavior
Flowability is studied with the analysis of the compaction dynamics. Finally, the dynamical regime is monitored through the
Angle of repose flow in a rotating drum. In order to illustrate how these measurements can be used in practical cases, analyses are
Packing fraction performed with three types of granular materials: silicon carbide abrasives, flours and rice. These selected
Cohesion materials allow to show the influence of the different parameters (grain size, grain size distribution, grain
Powder rheometer shape) on the macroscopic properties of the assembly. Moreover, these studies show the pertinence of the
parameters obtained with the proposed techniques for the rheological characterization of powders and grains.
© 2012 Elsevier B.V. All rights reserved.

1. Introduction phase segregation [5], jamming transition [6,7], complex rheological

Granular materials are ubiquitous in our daily lives and in industrial
applications. Indeed, almost every consumer product has been in a
granular state during its manufacturing process. However, in compari-
son with liquids and gasses, our understanding of the granular state
properties is poor. Therefore, any progress in the understanding of the
granular material behaviors could have huge consequences for the
industry. In particular, the measurement of the physical properties of
granular materials is an essential step during the development or the
optimization of an industrial process. In addition, the scaling between
the results obtained from the measurements in the laboratory and the
actual behavior of the powder in the production process represents a
difficult transition.
The annual number of scientific publications dedicated to granular
materials has increased from 30 in 1990 to 480 in 2010 [1]. A significant
part of these publications are related to fundamental studies which are
either theoretical or experimental [2–4]. During the last decade, granu-
lar material has aroused strong interest in the physics community due
to the links with glassy systems and due to puzzling behaviors like
⁎ Corresponding author at: GRASP, Institute of Physics, University of Liege, B-4000
Liège, Belgium.
E-mail address: geoffroy.lumay@ulg.ac.be (G. Lumay).
properties [8], etc. On the other hand, some publications are strongly
oriented to the applications. According to the authors in this study,
the link between the fundamental studies and the applied studies is
often too weak. For instance, when physicists are studying fundamen-
tally the phase segregation process [5], engineers are involved in the
improvement of the mixing process [9] and the cross references
between respective publications are poor. A long time has passed
between the fundamental study of a process involving granular materi-
al and the valorization of the fundamental knowledge in applications. In
particular, the methods used to characterize the physical properties of
granular materials can be strongly improved considering the recent
fundamental research. This point will be discussed in details.
A granular material is a complex system because its behavior
depends on the applied stress. When a collection of grains forms a pile
in a container, the material can be roughly compared to a solid. This is
the static state. However, if the container is sufficiently tilted, the gran-
ular material starts to flow [10]. In this dynamic state, the layer of grains
located at the surface could be seen as a liquid. Between the static and
the dynamic states, a granular assembly can experience a quasi-static
state. Indeed, if the pile is gently vibrated, the grains rearrange them-
selves inside the packing and the volume of the pile decreases slowly.
This slow dynamics has been the subject of many studies in the physics
community [12–18]. Finally, if the container is strongly agitated, the
grains experience free flights between some collisions with other grains
and with the container walls. In this case, the assembly behaves like a

0032-5910/$ – see front matter © 2012 Elsevier B.V. All rights reserved.
doi:10.1016/j.powtec.2012.02.015
20 G. Lumay et al. / Powder Technology 224 (2012) 19–27

Table 1
Empirical relation between the flow properties and the results obtained with two well-
a) Granular sugar
know powder tests (repose angle and Hausner ratio measurements) [40].

Flow property Angle of repose (°) Hausner ratio

Excellent 25–30 1.00–1.11

Good 31–35 1.12–1.18
Fair 36–40 1.19–1.25
Passable 41–45 1.26–1.34
Poor 46–55 1.35–1.45
Very poor 56–65 1.46–1.59
Very very poor >66 >1.60

dissipative gas. In any process, the granular materials can experience

some complex transitions between the static, the quasi-static and the b) Powdered sugar
dynamic states.
The motion and the jamming of the grains inside a pile are influ-
enced by (i) the steric repulsions, (ii) the friction forces and (iii) the
cohesive forces. The interactions with the surrounding fluid also influ-
ence the behavior of the grains inside the packing but this effect will
not be discussed further in this paper. The steric repulsion is related to
the geometry of the grains. The friction forces are influenced by the
surface properties and by the chemical nature of the grains. Finally,
the cohesive forces are induced by the presence of liquid bridges

1. Introduction
static quasi-static dynamic Fig. 2. Two typical heap shapes. (a) Conical heap shape obtained with a non cohesive
granular sugar. (b) Irregular heap of powdered sugar which is a cohesive granular material.

[19–21], electric charges [22], van der Waals interactions [23] and mag-
netic dipole– dipole interactions [24–28]. The granular materials can be
split in two categories: cohesive and non-cohesive granular materials.
In non-cohesive granular materials, the interaction between the grains
2. Measurement methods is mainly related to the steric repulsion and to the friction forces. There-
fore, the macroscopic properties of the assembly are governed by the
2.1 static 2.2 quasi-static 2.3 dynamic
geometry of the grains (shape and size distribution) and by the surface
GranuHeap GranuPaq GranuDrum properties of the grains. When the cohesive forces between the grains
become greater than the weight of one grain, the macroscopic proper-
ties are strongly influenced by the cohesion inside the packing [11].
Therefore, when the grains become smaller, the macroscopic properties
of the assembly are mainly governed by the cohesive forces.
Due to the complexity of granular materials, any single and simple
test method cannot characterize completely the physical properties of
heap compaction flowing a powder [29,30]. Indeed, the measurement method to analyze the
shape dynamics properties static, quasistatic and dynamic properties of a powder is strongly
different. Six methods are commonly reported to measure the powder
flowability: the angle of repose [31,32], compressibility index (or Haus-
3. Typical studies ner ratio) [33], flow in a rotating drum [34,35], flow through an orifice
[37], shear cell [38] and powder rheometers [39]. In addition, many
3.1 size 3.2 size distribution 3.3 shape variations of these methods are available. A measuring method has to
abrasives flours rice

Fig. 1. Organization of the paper. After an introduction on the physics of granular mate-
rials, methods of powder characterization based on 3 measurement techniques (Granu-
Heap, GranuPaq and GranuDrum) are proposed. This approach based on the association
of three techniques allows to investigate different granular states: the static, the quasi-
static and the dynamical states. More details about the measurement techniques are avail-
able on the APTIS website [41]. The analysis of three common granular materials shows
the pertinence of the parameters obtained with the proposed techniques for the rheolog-
ical characterization of powders and grains.
Fig. 3. Illustration of the GranuHeap measurement. The heap is formed on a cylindrical
support. A CCD camera takes pictures of the pile for different orientations. Then, a dedicat-
ed algorithm finds the position of the interface powder/air by image analysis. Finally, the
repose angle αr and the deviation σr from an ideal triangular heap (dashed lines) shape
are computed.
 G. Lumay et al. / Powder Technology 224 (2012) 19–27
Fig. 4. Sketch of the GranuPaQ measurement. The powder is placed in a metallic tube with
an initialization protocol described in the text. A light hollow cylinder is placed on the top
of the pile to keep it flat during the compaction process. The taps correspond to successive
free falls of the tube over a distance Z. After each tap, the height h of the pile is measured.
Finally, a compaction curve is obtained.
be easy to use, reproducible and sensitive. Furthermore, the results
obtained from the measurements have to be meaningful, easily inter-
pretable and easily usable to improve an industrial process. Table 1
shows the supposed relations between both angle of repose and Haus-
ner ratio and the flowability of the powder. These two simple tests and
these fully empirical relations are commonly used to have an idea about
the macroscopic properties of a powder. However, this is not sufficient
if a precise physical characterization of the powder is needed.
In this paper, we show how three revisited techniques can be used
to characterize the macroscopic properties of granular materials (see
Fig. 1). The first method (GranuHeap), based on the classical repose
angle measurement, gives information about the static properties of
the assembly. The second one (GranuPaq), based on the well known
tapped density measurement, estimates the quasistatic properties of a
granular pile. Finally, the GranuDrum quantifies the flow properties of
a granular material. To illustrate how these measurements can be
used in practical cases, three types of granular materials have been
analyzed. These granular materials are commonly encountered and
easy to find in the market: silicon carbide abrasives, flours and rice.
These selected materials allow to show respectively the influence of
the grain size, grain size distribution and grain shape on the macroscop-
ic properties of the assembly. Moreover, our studies show the
pertinence of the parameters obtained with the proposed techniques
for the rheological characterization of powders and grains.
1 2
n 1/2 n 1/2
η500
η500 -η0
2
η0
0 100 200 300 400 500
n
Fig. 5. Two typical compaction curves presenting the evolution of the packing fraction
η as a function of the tap number n. In this particular case, the initial η0 and the final
η500 packing fractions are the same for both compaction curves. Therefore, the Hausner
ratios are identical. The only difference between the two curves is the compaction
characteristic time τ (see Eq. (1)).
21
a) Granular sugar b) Powdered sugar
Ω Ω
Fig. 6. Two typical flows in a rotating drum. (a) Regular flow obtained with a non cohesive
granular sugar. (b) Irregular flow of powdered sugar which is a cohesive granular
material.
2. Measurement methods
2.1. Heap shape measurement
When grains are poured on a surface, they form a heap. Fig. 2 shows
two heaps of sugar. While the granular sugar forms a classical conical
heap, the powdered sugar forms a strongly irregular heap. Contrary to
the granular sugar, the powdered sugar is strongly cohesive due to the
small size of the grains. This example clearly shows that the heap
shape strongly depends on the grain properties. In particular, a cohesive
granular material gives a high value of the repose angle and strong
deviations from the conical shape [42]. Therefore, a precise measure-
ment of the heap shape gives some useful information about interac-
tions between the grains.
The angle of repose test is very sensitive to the method used to
create the heap. Therefore, an initialization protocol has to be defined.
Moreover, after the heap formation, the measurement of the repose
angle is not obvious. As shown in Fig. 2, the shape of the heap has to
be analyzed carefully. Therefore, the classical method which consists
in measuring the heap height h on a circular support of diameter b
and in calculating the angle with the relation tan(α) = 2h/b is subject
to caution.
In our measurements, an initialization tube with an internal diame-
ter equal to the support diameter is placed on the support. After filing
manually the tube with the sample of powder, the initialization tube
goes up at a constant speed of 5 mm/s. Therefore the powder flows
from the tube to form a heap on the cylindrical support (see Fig. 3).
This support can rotate slowly around its axis. Then, a CCD camera is
able to take pictures of the heap for different orientations. To obtain
the results presented in the next sections, 8 images separated by a rota-
tion of 22.5° were recorded. In this way, even if the heap shape is com-
plex and asymmetric, we are able to extract all the geometrical
information. From each picture of the heap, a dedicated algorithm
finds the position of the interface powder/air by image analysis. The
repose angle αr is the angle of the isosceles triangle which has the
same surface area as the heap. The isosceles triangle corresponds to
the ideal heap shape. In addition to this parameter, a cohesive index
50X
Fig. 7. Sketch of the GranuDrum measurement. A cylinder is half-filled with the powder
and rotates around his axis. For each rotating speed, a CCD camera takes 50 successive
images of the flow. A dedicated algorithm enables to measure the flowing angle αf and
the fluctuations σf of the flow from the shape of the granular/air interface.
22 G. Lumay et al. / Powder Technology 224 (2012) 19–27
σr is measured. This index σr corresponds to the deviation between the
heap interface and the ideal heap shape. For a non-cohesive powder, σr
is close to zero.
2.2. Compaction measurement
The Hausner ratio measurement is very popular for powder charac-
terization because of its simplicity and its rapidity. The recommended
procedure to measure the Hausner ratio is the following [40]. A powder
sample of 100 g is gently poured in a 250 ml glass cylinder. Then, the
initial volume V0 of the powder is measured by naked eyes. Afterward,
the pile experiences 500 calibrated taps and the final tapped volume Vf
is measured. The Hausner ratio is calculated with the relation Hr= V0/
Vf. Table 1 shows the empirical relations between the obtained Hausner
ratio and the flowability of the powder. This simple test has three major
drawbacks. First, the result of the measurement depends on the opera-
tor. Indeed, the filling method influences the initial volume V0. Second-
ly, the volume measurements by naked eyes induce strong errors on the
results. Finally, with this simple method, we completely miss the
compaction dynamics between the initial and the final measurements.
We have developed a protocol and an automated device (GranuPaq)
to perform an accurate measurement of the behavior of a granular
material submitted to a series of taps. The measurement is done in a
metallic tube to avoid the accumulation of electric charges during the
measurement. For that, all the parts of the device are connected to the
earth. The diameter and the length of the tube used to perform the stud-
ies presented in this paper are D = 26 mm and L = 100 mm for the anal-
ysis of the abrasives and of the flours and D = 35 mm and L = 150 mm
for the analysis of the rice. In order to obtain a reproducible and spatially
homogeneous initial packing, the following initialization protocol is
used. A narrower and bottomless tube is inserted into the measurement
tube. Afterward, the initialization tube is filled with the granular mate-
rial and is removed upward at a low and constant velocity v = 1 mm/s
leaving the grains to rearrange themselves in the measurement tube.
Then a light (11.5 g) aluminum hollow cylinder is gently placed on
the top of the pile to keep it flat during the compaction process (see
Fig. 4). To apply a tap on the packing, the tube goes up to a height of
Z ¼ 3 mm and experiences a free fall over the same height. After each
tap, a distance sensor measures the position of the hollow cylinder.
From this distance, the height h and the volume V of the pile are com-
puted. As the introduced mass of powder is known, the bulk density
ρbulk evolution as a function of the tap number n is calculated. The
bulk density is the ratio between the mass m and the volume V of the
powder. The packing fraction η is also calculated by dividing the bulk
density ρbulk by the true density ρtrue of the material. The fraction η
corresponds to the ratio between the volume occupied by the grains
and the volume of the pile.
Fig. 5 shows a sketch of two typical compaction curves. The Hausner
ratio extracted from both curves has exactly the same value. However,
the compaction dynamics are clearly different. Therefore, the Hausner
ratio is not sufficient to characterize the powder. An additional param-
eter is needed. We propose to measure a characteristic number of taps
to quantify the compaction speed while the Hausner ratio quantifies
the compaction ratio. Two methods could be used to perform this anal-
ysis. The first one is a geometrical method. From the compaction curve,
we measure the number of taps n1/2 needed to reach the middle of the
Table 2
Estimation of the uncertainties on the parameters obtained with the three powder
characterization methods. The measurements have been repeated five times with a
non cohesive and a cohesive granular material. Afterward the standard deviations
have been calculated. The obtained estimation of the uncertainties is presented in per-
centage of the results.
Granular αr σr η Hr n1/2 αf
Non cohesive 1% 13% 1% 1% 10% 2%
Cohesive 2% 14% 3% 3% 10% 5%
compaction process, i.e. to reach η = (η500 + η0)/2. The second method
is based on the fit with a physical model [12,18]:
ηð∞Þ−ηð0Þ
ηðnÞ ¼ ηð∞Þ−
ð1Þ
1 þ ln 1 þ nτ
where the fitting parameters η(∞) and τ are respectively the asymptotic
volume fraction and the compaction characteristic time. This compac-
tion characteristic time is expressed in number of taps. The parameter
η(∞) corresponds to the maximal packing fraction reachable by tapping
the powder. As the characteristic tap number n1/2, the characteristic
time τ gives an information about the compaction speed. The first one
(n1/2) is obtained directly from the compaction curve and the second
one (τ) is the result of the fit by a theoretical law. Therefore, if the the-
oretical law correctly fits the experimental data, the parameter τ does
not depend on the number of taps applied on the sample to perform
the measurement. One should note that both dynamical parameters
are linked by the relation n1/2 = (e − 1)τ.
2.3. Rotating drum measurement
Experimentally, the most practical geometry to study the flow of
granular materials is the rotating drum. This flow geometry has been
extensively studied [43–45,36], in particular with non cohesive granu-
lar materials. In this non-cohesive case, the flowing dynamics as a func-
tion of the rotating speed Ω is well known. At very low angular
velocities Ω, the flow is intermittent. The slope of the pile evolves
between the angle of repose ar and the maximum angle of stability θm.
At higher velocities, the flow becomes continuous. In this continuous
regime, the interface shape of the free surface is essentially flat for
low values of the Froude number Fr = RΩ2/g,where R is the drum radius
and g the gravitational acceleration. This flowing regime is presented in
Fig. 6(a). When the inertial effects become important, a well known
S-shape is observed [45]. Finally, when the Froude number Fr is higher
than the unity, a centrifugation is observed. In the case of cohesive
grains, the behavior of the granular assembly is more complex. In
particular, the continuous regime does not exist. Indeed, the cohesion
induces intermittencies in the whole range of rotating speed [46,47].
The flow of a cohesive powder in a rotating drum is presented in
Fig. 6(b).
The experimental setup (see Fig. 7) is a horizontal aluminum cylin-
der of diameter D = 84 mm and length L = 20 mm with glass side walls.
The drum is half-filled with the powder. The cylinder rotates around his
axis at an angular velocity Ω producing the flow of the grains. To per-
form the measurements, the rotating drum is backlighted and recorded
with a CCD camera. For each angular velocity, 50 images of the drum
separated by 0.5 s are recorded. On the images, the granular material
appears in black while the air appears in white. Then, the position of
the air/powder interface is determined by an edge detection. The aver-
age interface position and the fluctuations around this average position
are computed. From the fluctuations of the interface, the standard devi-
ation σf is calculated. This parameter is directly related to the cohesion
inside the drum. Indeed, in the range of considered rotating speed Ω,
a non-cohesive granular material leads to a continuous flow. From the
average interface position, the flowing angle αf is measured in the
center of the flow.
In our study, the rotating drum speed range is selected in order to
obtain a flat continuous flow with a non cohesive granular material
(see Fig. 6(a)). Therefore, with a non-cohesive granular material, the
flow can be fully characterized with the flowing angle αf. The second
parameter σf enables to quantify the cohesion inside the powder.
The rotating drum allows to measure the flow properties of a pow-
σf
der for different rotating speeds Ω. Therefore, the flowability is mea-
15% sured as a function of the shearing rates and rheological properties
15%
like shear thinning or shear thickening can be evaluated.
 G. Lumay et al. / Powder Technology 224 (2012) 19–27 23

a) b)

200μm 200μm

c) d)

100μm 5μm

Fig. 8. SEM micrographs of the silicon carbide abrasives. The micrographs are corresponding respectively to the average grain size of (a) 250 μm, (b) 100 μm, (c) 30 μm, and (d) 5 μm.

2.4. Measurement uncertainties
In order to estimate the uncertainties on the parameters obtained
with the three powder characterization methods, the measurements
have been repeated five times with a non cohesive and a cohesive gran-
ular material. The cohesive material is a silicon carbide abrasive with an
average grain size of 13 μm. The non-cohesive material is also a silicon
carbide abrasive but with larger grains (250 μm). The detailed analysis
of these materials is presented in the next section. The standard devia-
tions have been calculated. Table 2 presents the estimation of the uncer-
tainties for each parameter in percentage of the results.
3. Typical studies
a wide range of grain size d: 250, 170, 100, 80, 50, 30, 23, 13 and
5 μm. Some SEM micrographs of the grains are presented in Fig. 8. The
grains are angular, hard and monodisperse. The main characteristic
that differentiates these powders is the grain size d. Therefore, this
analysis allows to evaluate the influence of the grain size on the physical
properties of the assembly.
Fig. 9 shows the evolution of the macroscopic parameters obtained
with the GranuHeap measurement. The repose angle αr and the devia-
tion σr from the ideal heap are presented as a function of the grain size
d. Both parameters (αr and σr) decrease with the grain size in the range
d b 50 μm. Afterward, they are constant. The same behavior is observed
with the dynamical measures (αf and σf) obtained with the rotating
drum (see Fig. 11). Since σr and σf are related to the cohesion inside

3.1. Influence of the grain size 0.60

0.50
Silicon carbide abrasives of different grades have been analyzed
0.40
with the three characterization techniques. The selected grades cover
η

0.30
0.20 η500
η0
75
65 1.8

55 1.6
Hr
αr

1.4
45
1.2
35

6
40
5
4 30
n1/2
σr

3
20
2
1 10
0 0
0 50 100 150 200 250 0 50 100 150 200 250
d [μm] d [μm]

Fig. 9. Evolution of the repose angle αr and of the deviation σr from the ideal heap as a Fig. 10. Evolution of the parameters obtained with the GranuPaQ instrument (the initial
function of the grain size d for the silicon carbide abrasives. The measurements have η0 and final η∞ packing fractions, the Hausner ratio Hr and the compaction characteristic
been done with the GranuHeap instrument. time n1/2) as a function of the grain size d for the silicon carbide abrasives.
24 G. Lumay et al. / Powder Technology 224 (2012) 19–27

60
4 RPM the granular material, we can conclude that the cohesion plays an im-
55 6 RPM portant role when the grain size becomes lower than 50 μm. Above
10 RPM
50
d = 50 μm, the cohesion is negligible (σr = 0 and σf = 0). This effect
can also be seen on the SEM micrographs (see Fig. 8(d)). Indeed, the
αf

45 smallest grains are forming agglomerates due to the cohesion between

40 the grains.
This behavior is confirmed by the compaction measurements (see
35
Fig. 10). Indeed, the initial and the final packing fractions increase
with the grain size in the range d b 50 μm till a constant value when
60 d > 50 μm. For small grains (d b 50 μm), the cohesive forces between
the grains are able to stabilize a very loose packing. When the grain
50
size increases, the ratio between the weight of one grain and the cohe-
40
sive force acting on this grain increases. Therefore, the cohesive forces
σf

30 become unable to stabilize a loose packing. Moreover, when the initial

20 packing is loose, the tapping mechanism is able to modify the structure
10 of the assembly. Then, for cohesive granular material, the difference
between the initial and the final packing fraction is higher. This effect
0
0 50 100 150 200 250 is reflected by the evolution of the Hausner ratio as a function of the
d [μm] grain size d. Indeed, Hr decreases as a function of the grain size in the
range d b 50 μm till a constant value when d > 50 μm.
Fig. 11. Evolution of the flowing angle αf and of the deviation σf from the steady flow as The compaction characteristic time n1/2 shows a more complex
a function of the grain size d for the silicon carbide abrasives. The measurements have behavior. The decrease of n1/2 as a function of d in the cohesive range
been made with the GranuDrum instrument.
d b 50 μm is expected. The cohesive forces slow down the compaction
dynamics. The increase of n1/2 as a function of the grain size in the

a) b)

100μm 200μm

c) d)

50μm 100μm

e)

100μm

Fig. 12. SEM micrographs of the flours: (a) Anco fermentante, (b) Anco patisserie, (c) Francine complete, (d) Francine all purpose and (e) Francine fluid.
 G. Lumay et al. / Powder Technology 224 (2012) 19–27 25

12 72
Anco Ferm. 70
Anco pat.
10 Anco comp. 68

αr
Franc. all uses 66
Franc. Fluid
8 64
% Volume

62
6

4 2.5

σr
2.0
2
1.5
0
1 10 100 1000 1.0
14 16 18 20 22 24
grain size [μm] d(0,1) [μm]

Fig. 13. Grain size distributions obtained with a laser diffraction particle size analyzer
(Malvern, Mastersizer 2000) for the samples of flour.
range d > 50 μm is due to the fact that more energy is needed to move a
grain when the grains are larger and heavier. Moreover, when the size
of the grain increases, the effect of the wall becomes more important.
This geometrical effect could also explain the increase of n1/2.
All the measurements performed with the silicon carbide abrasives
show that the granular materials should be split in two categories.
Indeed, when the grain size is lower than 50 μm, the cohesive forces
inside the packing become larger than the other interactions. Of course,
the exact value of the grain size corresponding to the transition
between a non cohesive to a cohesive granular material will change as
a function of the nature of the grains and as a function of the humidity
[19–21]. However, this value of 50 μm can be used as practical criteria
to determine if the cohesion will play a relevant role.
3.2. Influence of the grain size distribution
Except some particular cases like abrasive material, many powders
are made of grains from different sizes. Therefore, the grain geometry
cannot be characterized by only one number. From the grain size distri-
bution, many parameters can be extracted: the average grain size, the
polydispersity, …. In order to study the link between the grain size dis-
tribution and the macroscopic properties of powders, five types of flour
available in supermarkets have been analyzed. Two flours are coming
from the company Anco: “fermentante” and “patisserie”. Three flours
are coming from the company Francine: “all purpose”, “complete” and
“fluid”. Some SEM micrographs of the grains are presented in Fig. 12.
Fig. 13 shows the grain size distributions for all the samples obtained
in a dry way with a laser diffraction particle size analyzer (Malvern,
Mastersizer Sirocco 2000). All the distributions are bi-modal. A first
Fig. 14. Evolution of the repose angle αr and of the deviation σr from the ideal heap as a
function of d(0, 1) obtained with the five samples of flour. The measurements have
been made with the GranuHeap instrument.
powders, small means a size inferior to around 50 μm. Therefore, the
smallest grains are expected to influence the behavior of a polydis-
persed powder. In order to measure the influence of the smallest parti-
cles, the results of the measurements are considered as a function of the
smallest grain size d(0,1). If this hypothesis on the strong influence of
the smallest grains is correct, the static and dynamic angle αr and αf,
the static and dynamic cohesive index σr and σf, the Hausner ratio
Hr and the compaction characteristic time n1/2 should decrease
with d(0,1). Moreover, the initial and the final packing fraction
should increase with d(0,1).
Fig. 14 presents the results obtained with the GranuHeap. The
decrease of the deviation σr from the ideal heap shape as a function of
d(0, 1) shows that the cohesion inside the flour depends on the smallest
grain size. This observation is confirmed by the analysis of the flow fluc-
tuations σf with the GranuDrum method (see Fig. 16). As expected, the
static angle αr and the flowing angles αf decrease with the smallest
grain size d(0, 1). One exception is observed with the “Francine fluid”
flour. For this flour, the parameters σr and σf corresponding to the cohe-
sion are low but the flowing angle αf is higher than the flowing angle of
the other flours. This exception to the general trend shows that only one
measurement is not sufficient to characterize the flowability of a pow-
der. The results obtained with the GranuPaq (see Fig. 15) are in agree-
ment with the other observations. Indeed, both compaction ratio Hr
and compaction characteristic time n1/2 decrease with d(0, 1). The
0.60
0.55
0.50
0.45
η

maximum is observed around 20 μm and a second one around

0.40
100 μm. A group of three flours exhibits very similar size distributions η500
0.35
(Anco ferm., Anco pat. and Francine all purpose). Two flours are strong- η0
ly different from this group: Francine fluid and Francine complete. Some 1.44
descriptors extracted from the grain size distribution are presented in 1.40
Table 3.
Hr

1.36
The analysis of the abrasive powder (see the previous section) has
1.32
shown that the cohesive forces strongly influence the macroscopic
1.28
properties when the grain size is small. We have shown that for
20
Table 3 1.8
n1/2

Descriptors extracted from the grain size distributions (see Fig. 13) obtained with the
1.6
flours: small grain size d(0,1), median grain size d(0.5) and standard deviation σ. All
the results are presented in micrometers. 1.4

Flour name d(0,1) d(0.5) σ

1.2
14 16 18 20 22 24
Francine fluid 22.7 136 67.1 d(0,1) [μm]
Anco fermentante 17.9 95.5 51.0
Francine all purpose 16 102.3 56.0
Fig. 15. Evolution of the parameters obtained with the GranuPaQ instrument (the initial
Anco patisserie 16.2 100.6 53.5
η0 and final η∞ packing fractions, the Hausner ratio Hr and the compaction characteristic
Francine complete 15.6 109.3 105.5
time n1/2) as a function of d(0, 1) obtained with the five samples of flour.
26 G. Lumay et al. / Powder Technology 224 (2012) 19–27

60 Table 4
58 Geometrical characteristics of the grains of rice used to perform the macroscopic prop-
erty measurements. The grains have been fitted by ellipses to obtain the major a and
56
the minor b axes. The standard deviations obtained on the measurement of a and b
54 are indicated. The ratios a/b give the elongation of the grains.
αf

52
Rice a [mm] b [mm] a/b
50
Risotti 6.1 ± 1.1 2.8 ± 0.6 2.2
48 4 RPM
6 RPM Long rice No 1 6.0 ± 1.5 2.2 ± 0.3 2.7
46 10 RPM Bosto Wok 6.7 ± 1.0 2.4 ± 0.3 2.8
Thai 6.7 ± 1.4 2.2 ± 0.3 3.0
Basmati 7.3 ± 1.1 1.9 ± 0.1 3.8
50

45
Fig. 18 shows that the elongation a/b influences the packing fraction
σf

40
35
30
25
14 16 18 20 22 24
d(0,1) [μm]
Fig. 16. Evolution of the flowing angle αf and of the deviation σf from the steady flow as
a function of d(0, 1) obtained with the five samples of flour. The measurements have
been made with the GranuDrum instrument.
evolution of the measured parameters as a function of the other grain
characteristics like the average grain size d(0, 5) and the polydispersity
do not lead to such a correlation.
All these results confirm that the flowability is enhanced for larger
values of d(0, 1). This conclusion is confirmed by the observation of
the SEM micrographs (Fig. 12). Indeed, the small grains are sticking
on the big ones and are able to form some cohesive bridges between
them. Therefore, the size of the smallest grains is a key parameter for
the characterization of a powder.
3.3. Influence of grain shape
For small grains, i.e. for grain diameters inferior to 50 μm, the macro-
scopic properties of a pile are mainly related to the cohesive forces
between the grains. For larger grains, the particle shape becomes an
important parameter. In order to show the influence of the particle
shape on the macroscopic parameters obtained from the analysis of
the flow in the drum and the compaction dynamics during the
tapped density test, rice grains with different elongations have been
considered. The heap shape analysis is not shown in this case.
To analyze the shape of the rice grains, five samples of approximate-
ly one hundred grains has been scanned with a classical office scanner
(see Fig. 17). Afterward, the images have been binarized and the black
and the compaction dynamics. The decrease of the packing fraction as a
function of the elongation of the grains is a well know effect [17].
Indeed, when the grains are longer, some large voids are present in
the pile. Moreover, when the elongation a/b increases, the mobility of
the grains inside the packing decreases due to steric frustrations [48].
This effect explains the increase of the compaction characteristic time
with the elongation (see Fig. 18). The point that does not follow the
general trends corresponds to the “Long rice No 1” which has a wider
grain length distribution due to the presence of broken grains.
As shown by Fig. 19, the flowing angle αf and the fluctuations of the
flowing interface σf increase with the grain elongation a/b. In this case,
the fluctuations of the flow σf is related the elongation of the grains, not
to cohesive forces. Indeed, grain elongations are known to induce inter-
mittencies in flows [49]. The flowing angle αf is found to increase with
the drum rotating speed Ω. This is a classical behavior with non cohesive
granular materials. This tendency has not been observed with the abra-
sives and with the flours probably due to an effect of rheofluidization.
4. Conclusion
Three well known powder characterization tests have been opti-
mized in the light of recent fundamental research on granular materials.
In order to illustrate how these measurements could be used in practical
cases, analyses are performed with three types of granular materials:
silicon carbide abrasives, flours and rice. The macroscopic analysis of
the mono-disperse abrasives of different grades has shown that the
cohesion between the grains becomes important when the grain diam-
eter is inferior to 50 μm. Moreover, the cohesion modifies the static, the
quasi-static and the dynamic properties of the pile. Indeed, the cohesion
0.60
0.56
η

0.52
shapes corresponding to the grains have been fitted with ellipses. This
simple method allows to obtain the major a and the minor b axes for
η500
0.48 η0
each grain. The result of this analysis is presented in Table 4. From the
“Risotti” to the “Basmati” rice, the elongation a/b evolves between 2.2 1.19
and 3.8. The “Long rice No 1” is particular because it contains a lot of 1.18
Hr

broken grains. Therefore, the standard deviation of the long axis a is 1.17
1.16
much larger than the other types of rice.
1.15

42

a 38
n1/2

34
b
30
26
1.6 2.0 2.4 2.8 3.2 3.6 4.0
a/b
Fig. 17. Analysis of the rice grain shape. (left) A sample of grains is scanned with a classical
office scanner. (middle) The image is binarized to obtain black shapes corresponding to Fig. 18. Evolution of the parameters obtained with the GranuPaQ instrument (the initial
the grains. (left) The black spots are fitted by ellipses to obtain the major a and the η0 and final η∞ packing fractions, the Hausner ratio Hr and the compaction characteristic
minor b axes for each grain. time n1/2) as a function of the grain elongation a/b for five samples of rice.
 G. Lumay et al. / Powder Technology 224 (2012) 19–27
60
4 RPM
6 RPM
57
10 RPM
54
51
αf
48
45
42
13
12
σf
11
10
9 powders, Powder Technology 189 (2009) 409.
8 intermittent granular flow, Physical Review E 81 (2010) 041309.
1.6 2.0 2.4 2.8 3.2 3.6 4.0
a/b
Fig. 19. Evolution of the flowing angle αf and of the deviation σf from the steady flow as
a function of the grain elongation a/b for five samples of rice. The measurements have
been made with the GranuDrum instrument.
strongly decreases the packing fraction of the pile and increases the
Hausner ratio Hr and the compaction characteristic time n1/2. The
angle of repose αr and the flowing angles αf are also increased by
the cohesion. In addition, the cohesion induces some fluctuations of
the flow and some irregularities at the surface of a pile. Concerning
the polydisperse powders, the analysis of different flours has shown
that the smallest grains influence the macroscopic properties of the
powder. For larger grains d > 50 μm, the particle shape becomes an
important parameter. In particular, the elongation of the grain influences
the macroscopic properties of the assembly.
Acknowledgments
GL thanks F.R.S.-FNRS, FB thanks the Walloon Region (First SO no 071/
6576) and KT thanks the Walloon Region (BIOFINA Convention no 6045)
for the financial support. This work has also been supported by INANO-
MAT project (IAP P6/17) of the Belgian Science Policy. Thanks to Catμ
(microscopy center of the University of Liège) for the SEM micrographs.
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