Powder Technology 224 (2012) 1927

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

Measuring the owing 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 Lige, Belgium

GRASP, Institute of Physics, University of Liege, B-4000 Lige, Belgium
c
LCIS-GreenMat, Institute of Chemistry, University of Liege, B-4000 Lige, Belgium
d
F.R.S.-FRNS, B-1000 Bruxelles, Belgium
b

a r t i c l e

i n f o

Article history:
Received 7 February 2011
Received in revised form 23 September 2011
Accepted 11 February 2012
Available online 19 February 2012
Keywords:
Powder characterization
Flowability
Angle of repose
Packing fraction
Cohesion
Powder rheometer

a b s t r a c t
A granular material is a complex system which exhibits non-trivial transitions between the static, the quasi-static
and the dynamical states. Indeed, an assembly of grains can behave like a solid or a uid according to the applied
stress. In between solid and uid granular states, very slow dynamics are observed. When a complete macroscopic characterization of a powder is needed, all these granular states have to be precisely analyzed. In this
paper, we show how three measurement techniques can be used to measure the physical properties of a powder.
The measurements are based on classical tests modied to meet the recent fundamental researches on granular
materials. The static properties of the powder are analyzed through the shape of a heap. The quasi-static behavior
is studied with the analysis of the compaction dynamics. Finally, the dynamical regime is monitored through the
ow in a rotating drum. In order to illustrate how these measurements can be used in practical cases, analyses are
performed with three types of granular materials: silicon carbide abrasives, ours and rice. These selected
materials allow to show the inuence of the different parameters (grain size, grain size distribution, grain
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
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 comparison 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
difcult transition.
The annual number of scientic publications dedicated to granular
materials has increased from 30 in 1990 to 480 in 2010 [1]. A signicant
part of these publications are related to fundamental studies which are
either theoretical or experimental [24]. During the last decade, granular 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

Lige, Belgium.
E-mail address: geoffroy.lumay@ulg.ac.be (G. Lumay).
0032-5910/$ see front matter 2012 Elsevier B.V. All rights reserved.
doi:10.1016/j.powtec.2012.02.015

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

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 fundamentally 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 material 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 sufciently tilted, the granular material starts to ow [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 themselves 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 [1218]. Finally, if the container is strongly agitated, the
grains experience free ights between some collisions with other grains
and with the container walls. In this case, the assembly behaves like a

20

G. Lumay et al. / Powder Technology 224 (2012) 1927

Table 1
Empirical relation between the ow properties and the results obtained with two wellknow powder tests (repose angle and Hausner ratio measurements) [40].
Flow property

Angle of repose ()

Hausner ratio

Excellent
Good
Fair
Passable
Poor
Very poor
Very very poor

2530
3135
3640
4145
4655
5665
>66

1.001.11
1.121.18
1.191.25
1.261.34
1.351.45
1.461.59
>1.60

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

some complex transitions between the static, the quasi-static and the
dynamic states.
The motion and the jamming of the grains inside a pile are inuenced by (i) the steric repulsions, (ii) the friction forces and (iii) the
cohesive forces. The interactions with the surrounding uid also inuence 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 inuenced by the
surface properties and by the chemical nature of the grains. Finally,
the cohesive forces are induced by the presence of liquid bridges

a) Granular sugar

b) Powdered sugar

1. Introduction
quasi-static

static

dynamic

2. Measurement methods
2.1 static

2.2 quasi-static

2.3 dynamic

GranuHeap

GranuPaq

GranuDrum

heap
shape

compaction
dynamics

flowing
properties

3. Typical studies
3.1 size

3.2 size distribution

3.3 shape

abrasives

flours

rice

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.

[1921], electric charges [22], van der Waals interactions [23] and magnetic dipole dipole interactions [2428]. 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
is mainly related to the steric repulsion and to the friction forces. Therefore, the macroscopic properties of the assembly are governed by the
geometry of the grains (shape and size distribution) and by the surface
properties of the grains. When the cohesive forces between the grains
become greater than the weight of one grain, the macroscopic properties are strongly inuenced 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
a powder [29,30]. Indeed, the measurement method to analyze the
static, quasistatic and dynamic properties of a powder is strongly
different. Six methods are commonly reported to measure the powder
owability: the angle of repose [31,32], compressibility index (or Hausner ratio) [33], ow in a rotating drum [34,35], ow through an orice
[37], shear cell [38] and powder rheometers [39]. In addition, many
variations of these methods are available. A measuring method has to

r
Fig. 1. Organization of the paper. After an introduction on the physics of granular materials, methods of powder characterization based on 3 measurement techniques (GranuHeap, GranuPaq and GranuDrum) are proposed. This approach based on the association
of three techniques allows to investigate different granular states: the static, the quasistatic and the dynamical states. More details about the measurement techniques are available 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 rheological 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 dedicated algorithm nds the position of the interface powder/air by image analysis. Finally, the
repose angle r and the deviation r from an ideal triangular heap (dashed lines) shape
are computed.

G. Lumay et al. / Powder Technology 224 (2012) 1927

21

a) Granular sugar

b) Powdered sugar

Fig. 6. Two typical ows in a rotating drum. (a) Regular ow obtained with a non cohesive
granular sugar. (b) Irregular ow of powdered sugar which is a cohesive granular
material.
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 at 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 interpretable and easily usable to improve an industrial process. Table 1
shows the supposed relations between both angle of repose and Hausner ratio and the owability 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 sufcient
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 rst 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 quanties the ow 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 nd in the market: silicon carbide abrasives, ours and rice.
These selected materials allow to show respectively the inuence of
the grain size, grain size distribution and grain shape on the macroscopic 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
n 1/2

2
n 1/2

500

500 -0

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 measurement of the heap shape gives some useful information about interactions 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 dened.
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() = 2h/b is subject
to caution.
In our measurements, an initialization tube with an internal diameter equal to the support diameter is placed on the support. After ling
manually the tube with the sample of powder, the initialization tube
goes up at a constant speed of 5 mm/s. Therefore the powder ows
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 rotation of 22.5 were recorded. In this way, even if the heap shape is complex and asymmetric, we are able to extract all the geometrical
information. From each picture of the heap, a dedicated algorithm
nds the position of the interface powder/air by image analysis. The
repose angle r 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
0
0

100

200

300

400

500

Fig. 5. Two typical compaction curves presenting the evolution of the packing fraction
as a function of the tap number n. In this particular case, the initial 0 and the nal
500 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 (see Eq. (1)).

Fig. 7. Sketch of the GranuDrum measurement. A cylinder is half-lled with the powder
and rotates around his axis. For each rotating speed, a CCD camera takes 50 successive
images of the ow. A dedicated algorithm enables to measure the owing angle f and
the uctuations f of the ow from the shape of the granular/air interface.

22

G. Lumay et al. / Powder Technology 224 (2012) 1927

r is measured. This index r corresponds to the deviation between the

heap interface and the ideal heap shape. For a non-cohesive powder, r
is close to zero.

compaction process, i.e. to reach = (500 + 0)/2. The second method

is based on the t with a physical model [12,18]:

2.2. Compaction measurement

The Hausner ratio measurement is very popular for powder characterization 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 nal 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 owability of the powder. This simple test has three major
drawbacks. First, the result of the measurement depends on the operator. Indeed, the lling method inuences the initial volume V0. Secondly, 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 nal 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 studies presented in this paper are D = 26 mm and L = 100 mm for the analysis of the abrasives and of the ours 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 lled with the granular material 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 at during the compaction process (see
Fig. 4). To apply a tap on the packing, the tube goes up to a height of
Z 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 computed. As the introduced mass of powder is known, the bulk density
bulk 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 is also calculated by dividing the bulk
density bulk by the true density true of the material. The fraction
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 sufcient to characterize the powder. An additional parameter is needed. We propose to measure a characteristic number of taps
to quantify the compaction speed while the Hausner ratio quanties
the compaction ratio. Two methods could be used to perform this analysis. The rst 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 ve 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 percentage of the results.
Granular

Hr

n1/2

Non cohesive
Cohesive

1%
2%

13%
14%

1%
3%

1%
3%

10%
10%

2%
5%

15%
15%

0


1 ln 1 n

where the tting parameters () and are respectively the asymptotic

volume fraction and the compaction characteristic time. This compaction characteristic time is expressed in number of taps. The parameter
() corresponds to the maximal packing fraction reachable by tapping
the powder. As the characteristic tap number n1/2, the characteristic
time gives an information about the compaction speed. The rst one
(n1/2) is obtained directly from the compaction curve and the second
one () is the result of the t by a theoretical law. Therefore, if the theoretical law correctly ts the experimental data, the parameter 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).
2.3. Rotating drum measurement
Experimentally, the most practical geometry to study the ow of
granular materials is the rotating drum. This ow geometry has been
extensively studied [4345,36], in particular with non cohesive granular materials. In this non-cohesive case, the owing dynamics as a function of the rotating speed is well known. At very low angular
velocities , the ow is intermittent. The slope of the pile evolves
between the angle of repose ar and the maximum angle of stability m.
At higher velocities, the ow becomes continuous. In this continuous
regime, the interface shape of the free surface is essentially at for
low values of the Froude number Fr = R2/g,where R is the drum radius
and g the gravitational acceleration. This owing 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 ow of a cohesive powder in a rotating drum is presented in
Fig. 6(b).
The experimental setup (see Fig. 7) is a horizontal aluminum cylinder of diameter D = 84 mm and length L = 20 mm with glass side walls.
The drum is half-lled with the powder. The cylinder rotates around his
axis at an angular velocity producing the ow of the grains. To perform 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 average interface position and the uctuations around this average position
are computed. From the uctuations of the interface, the standard deviation f is calculated. This parameter is directly related to the cohesion
inside the drum. Indeed, in the range of considered rotating speed ,
a non-cohesive granular material leads to a continuous ow. From the
average interface position, the owing angle f is measured in the
center of the ow.
In our study, the rotating drum speed range is selected in order to
obtain a at continuous ow with a non cohesive granular material
(see Fig. 6(a)). Therefore, with a non-cohesive granular material, the
ow can be fully characterized with the owing angle f. The second
parameter f enables to quantify the cohesion inside the powder.
The rotating drum allows to measure the ow properties of a powder for different rotating speeds . Therefore, the owability is measured as a function of the shearing rates and rheological properties
like shear thinning or shear thickening can be evaluated.

G. Lumay et al. / Powder Technology 224 (2012) 1927

a)

23

b)

200m

c)

200m

d)

100m

5m

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

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 ve times with a non cohesive and a cohesive granular material. The cohesive material is a silicon carbide abrasive with an
average grain size of 13 m. The non-cohesive material is also a silicon
carbide abrasive but with larger grains (250 m). The detailed analysis
of these materials is presented in the next section. The standard deviations have been calculated. Table 2 presents the estimation of the uncertainties 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 m. 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 inuence 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 r and the deviation r from the ideal heap are presented as a function of the grain size
d. Both parameters (r and r) decrease with the grain size in the range
d b 50 m. Afterward, they are constant. The same behavior is observed
with the dynamical measures (f and f) obtained with the rotating
drum (see Fig. 11). Since r and f are related to the cohesion inside

3.1. Inuence of the grain size

0.60

Silicon carbide abrasives of different grades have been analyzed

with the three characterization techniques. The selected grades cover

0.50
0.40
0.30

500
0

0.20

65

1.8

55

1.6

Hr

75

45

1.2

35
6
5
4
3
2
1
0

40

n1/2

1.4

30
20
10

50

100

150

200

250

d [m]
Fig. 9. Evolution of the repose angle r and of the deviation r from the ideal heap as a
function of the grain size d for the silicon carbide abrasives. The measurements have
been done with the GranuHeap instrument.

50

100

150

200

250

d [m]
Fig. 10. Evolution of the parameters obtained with the GranuPaQ instrument (the initial
0 and nal packing fractions, the Hausner ratio Hr and the compaction characteristic
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) 1927

60

4 RPM
6 RPM
10 RPM

55

50
45
40
35

60

50
40
30
20
10
0

50

100

150

200

250

d [m]
Fig. 11. Evolution of the owing angle f and of the deviation f from the steady ow as
a function of the grain size d for the silicon carbide abrasives. The measurements have
been made with the GranuDrum instrument.

a)

the granular material, we can conclude that the cohesion plays an important role when the grain size becomes lower than 50 m. Above
d = 50 m, the cohesion is negligible (r = 0 and f = 0). This effect
can also be seen on the SEM micrographs (see Fig. 8(d)). Indeed, the
smallest grains are forming agglomerates due to the cohesion between
the grains.
This behavior is conrmed by the compaction measurements (see
Fig. 10). Indeed, the initial and the nal packing fractions increase
with the grain size in the range d b 50 m till a constant value when
d > 50 m. For small grains (d b 50 m), the cohesive forces between
the grains are able to stabilize a very loose packing. When the grain
size increases, the ratio between the weight of one grain and the cohesive force acting on this grain increases. Therefore, the cohesive forces
become unable to stabilize a loose packing. Moreover, when the initial
packing is loose, the tapping mechanism is able to modify the structure
of the assembly. Then, for cohesive granular material, the difference
between the initial and the nal packing fraction is higher. This effect
is reected by the evolution of the Hausner ratio as a function of the
grain size d. Indeed, Hr decreases as a function of the grain size in the
range d b 50 m till a constant value when d > 50 m.
The compaction characteristic time n1/2 shows a more complex
behavior. The decrease of n1/2 as a function of d in the cohesive range
d b 50 m is expected. The cohesive forces slow down the compaction
dynamics. The increase of n1/2 as a function of the grain size in the

b)

200m

100m

c)

d)

50m

100m

e)

100m
Fig. 12. SEM micrographs of the ours: (a) Anco fermentante, (b) Anco patisserie, (c) Francine complete, (d) Francine all purpose and (e) Francine uid.

G. Lumay et al. / Powder Technology 224 (2012) 1927

12

72
70
68
66
64
62

2.5

% Volume

10

Anco Ferm.
Anco pat.
Anco comp.
Franc. all uses
Franc. Fluid

25

2.0

1.5
0
1

10

100

1.0
14

1000

16

grain size [m]

18

20

22

24

d(0,1) [m]

3.2. Inuence 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 distribution, many parameters can be extracted: the average grain size, the
polydispersity, . In order to study the link between the grain size distribution and the macroscopic properties of powders, ve types of our
available in supermarkets have been analyzed. Two ours are coming
from the company Anco: fermentante and patisserie. Three ours
are coming from the company Francine: all purpose, complete and
uid. 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 rst
maximum is observed around 20 m and a second one around
100 m. A group of three ours exhibits very similar size distributions
(Anco ferm., Anco pat. and Francine all purpose). Two ours are strongly different from this group: Francine uid and Francine complete. Some
descriptors extracted from the grain size distribution are presented in
Table 3.
The analysis of the abrasive powder (see the previous section) has
shown that the cohesive forces strongly inuence the macroscopic
properties when the grain size is small. We have shown that for

powders, small means a size inferior to around 50 m. Therefore, the

smallest grains are expected to inuence the behavior of a polydispersed powder. In order to measure the inuence of the smallest particles, the results of the measurements are considered as a function of the
smallest grain size d(0,1). If this hypothesis on the strong inuence of
the smallest grains is correct, the static and dynamic angle r and f,
the static and dynamic cohesive index r and f, the Hausner ratio
Hr and the compaction characteristic time n1/2 should decrease
with d(0,1). Moreover, the initial and the nal packing fraction
should increase with d(0,1).
Fig. 14 presents the results obtained with the GranuHeap. The
decrease of the deviation r from the ideal heap shape as a function of
d(0, 1) shows that the cohesion inside the our depends on the smallest
grain size. This observation is conrmed by the analysis of the ow uctuations f with the GranuDrum method (see Fig. 16). As expected, the
static angle r and the owing angles f decrease with the smallest
grain size d(0, 1). One exception is observed with the Francine uid
our. For this our, the parameters r and f corresponding to the cohesion are low but the owing angle f is higher than the owing angle of
the other ours. This exception to the general trend shows that only one
measurement is not sufcient to characterize the owability of a powder. The results obtained with the GranuPaq (see Fig. 15) are in agreement with the other observations. Indeed, both compaction ratio Hr
and compaction characteristic time n1/2 decrease with d(0, 1). The

range d > 50 m 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 m, 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
[1921]. However, this value of 50 m can be used as practical criteria
to determine if the cohesion will play a relevant role.

Fig. 14. Evolution of the repose angle r and of the deviation r from the ideal heap as a
function of d(0, 1) obtained with the ve samples of our. The measurements have
been made with the GranuHeap instrument.

0.60
0.55
0.50
0.45
0.40
0.35

500
0

1.44
1.40

Hr

Fig. 13. Grain size distributions obtained with a laser diffraction particle size analyzer
(Malvern, Mastersizer 2000) for the samples of our.

1.36
1.32
1.28

Flour name

d(0,1)

d(0.5)

Francine uid
Anco fermentante
Francine all purpose
Anco patisserie
Francine complete

22.7
17.9
16
16.2
15.6

136
95.5
102.3
100.6
109.3

67.1
51.0
56.0
53.5
105.5

n1/2

20
Table 3
Descriptors extracted from the grain size distributions (see Fig. 13) obtained with the
ours: small grain size d(0,1), median grain size d(0.5) and standard deviation . All
the results are presented in micrometers.

1.8
1.6
1.4
1.2
14

16

18

20

22

24

d(0,1) [m]
Fig. 15. Evolution of the parameters obtained with the GranuPaQ instrument (the initial
0 and nal packing fractions, the Hausner ratio Hr and the compaction characteristic
time n1/2) as a function of d(0, 1) obtained with the ve samples of our.

26

G. Lumay et al. / Powder Technology 224 (2012) 1927

60

Table 4
Geometrical characteristics of the grains of rice used to perform the macroscopic property measurements. The grains have been tted by ellipses to obtain the major a and
the minor b axes. The standard deviations obtained on the measurement of a and b
are indicated. The ratios a/b give the elongation of the grains.

58
56

54
52
50
4 RPM
6 RPM
10 RPM

48
46
50

Rice

a [mm]

b [mm]

a/b

Risotti
Long rice No 1
Bosto Wok
Thai
Basmati

6.1 1.1
6.0 1.5
6.7 1.0
6.7 1.4
7.3 1.1

2.8 0.6
2.2 0.3
2.4 0.3
2.2 0.3
1.9 0.1

2.2
2.7
2.8
3.0
3.8

35
30
25
14

16

18

20

22

24

d(0,1) [m]
Fig. 16. Evolution of the owing angle f and of the deviation f from the steady ow as
a function of d(0, 1) obtained with the ve samples of our. 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 conrm that the owability is enhanced for larger
values of d(0, 1). This conclusion is conrmed 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. Inuence of grain shape
For small grains, i.e. for grain diameters inferior to 50 m, the macroscopic 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 inuence of the particle
shape on the macroscopic parameters obtained from the analysis of
the ow 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, ve samples of approximately one hundred grains has been scanned with a classical ofce scanner
(see Fig. 17). Afterward, the images have been binarized and the black
shapes corresponding to the grains have been tted with ellipses. This
simple method allows to obtain the major a and the minor b axes for
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
and 3.8. The Long rice No 1 is particular because it contains a lot of
broken grains. Therefore, the standard deviation of the long axis a is
much larger than the other types of rice.

Fig. 18 shows that the elongation a/b inuences the packing fraction
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 owing angle f and the uctuations of the
owing interface f increase with the grain elongation a/b. In this case,
the uctuations of the ow f is related the elongation of the grains, not
to cohesive forces. Indeed, grain elongations are known to induce intermittencies in ows [49]. The owing angle f is found to increase with
the drum rotating speed . This is a classical behavior with non cohesive
granular materials. This tendency has not been observed with the abrasives and with the ours probably due to an effect of rheouidization.
4. Conclusion
Three well known powder characterization tests have been optimized 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, ours 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 diameter is inferior to 50 m. Moreover, the cohesion modies the static, the
quasi-static and the dynamic properties of the pile. Indeed, the cohesion
0.60
0.56

40

0.52
0.48

Hr

45

500
0

1.19
1.18
1.17
1.16
1.15

n1/2

42

38
34
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
ofce scanner. (middle) The image is binarized to obtain black shapes corresponding to
the grains. (left) The black spots are tted by ellipses to obtain the major a and the
minor b axes for each grain.

Fig. 18. Evolution of the parameters obtained with the GranuPaQ instrument (the initial
0 and nal packing fractions, the Hausner ratio Hr and the compaction characteristic
time n1/2) as a function of the grain elongation a/b for ve samples of rice.

G. Lumay et al. / Powder Technology 224 (2012) 1927

60
57

4 RPM
6 RPM
10 RPM

54
51
48
45
42
13

12
11
10
9
8
1.6

2.0

2.4

2.8

3.2

3.6

4.0

a/b
Fig. 19. Evolution of the owing angle f and of the deviation f from the steady ow as
a function of the grain elongation a/b for ve 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 r and the owing angles f are also increased by
the cohesion. In addition, the cohesion induces some uctuations of
the ow and some irregularities at the surface of a pile. Concerning
the polydisperse powders, the analysis of different ours has shown
that the smallest grains inuence the macroscopic properties of the
powder. For larger grains d > 50 m, the particle shape becomes an
important parameter. In particular, the elongation of the grain inuences
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 nancial support. This work has also been supported by INANOMAT project (IAP P6/17) of the Belgian Science Policy. Thanks to Cat
(microscopy center of the University of Lige) for the SEM micrographs.
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