Powder Technology 203 (2010) 482–488

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

Uniaxial compaction behaviour and elasticity of cohesive powders

M. Stasiak a,⁎, J. Tomas b, M. Molenda a, R. Rusinek a, P. Mueller b
a
Institute of Agrophysics, Polish Academy of Sciences, P.O. Box 201, 20-290 Lublin 27, Poland
b
Otto-von-Guericke University, Magdeburg, P.O. Box 4120, 39106 Magdeburg, Germany

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

Article history: The compression and compaction behaviour of bentonite, limestone and microcrystalline cellulose (MCC) —
Received 4 February 2010 three cohesive powders widely used in industry were studied. Uniaxial compression was performed in a
Received in revised form 19 May 2010 cylindrical die, 40 mm in diameter and 70 mm high, for three selected cohesive powder samples. The initial
Accepted 14 June 2010
density, instantaneous density and tablet density were determined. The influence of maximum pressure and
Available online 21 June 2010
deformation rate was examined. The secant modulus of elasticity Esec was calculated as a function of
Keywords:
deformation rate v, maximum pressure p and powder sample. After compaction experiments in hydraulic
Compression test press at three pressures – p = 30, 45 and 60 MPa – and two different deformation rates, the strength of the
Powder compaction produced tablets was examined in a material strength testing machine.
Modulus of elasticity From uniaxial compression tests performed on the universal testing machine for loading and unloading, the
Tablet density modulus of elasticity E was calculated on the basis of the first linear phase of unloading. The total elastic
Tablet strength recovery of tablets was also obtained.
© 2010 Elsevier B.V. All rights reserved.

1. Introduction grains or particles, adhesion and friction between particles, interpar-

Powders and bulk solids are produced, handled and applied in
food, pharmaceutical, chemical and building material industries. The
volume and range of bulk solids used in industry are still increasing,
and simultaneously powder handling remains one of the least
understood areas associated with solid processing plants. Predictable
processing, increase of quality and reduction of losses of products are
still the main issues [4]. Process design and optimisation determine
the properties and quality of products. With increasing scale of
industrial operations, the design of reliable processes and efficient
equipment requires more precise information about physical proper-
ties and on how different process conditions change them [25]. The
most important technologies of process engineering involving
powders and bulk solids, as listed in handbooks, are e.g.: pneumatic
conveying, transport, size reduction, screening, coating, mixing,
segregation, dust collection, feeding, weighing, metering, packaging
and bagging, storage, instrumentation and quality control. Predictable
processing, increase of quality and reduction of product losses are the
main issues addressed in last few decades [9]. Process design and
optimisation generate the need to determine properties and quality
parameters measures of powders and bulk solids. Mechanical
properties that serve as design parameters for storage systems or
processing plants usually depend on the properties of individual
⁎ Corresponding author.
E-mail address: mstasiak@ipan.lublin.pl (M. Stasiak).
ticle contact geometry and prior history of loading [20].
Compressibility and compactability of a powder are influenced by
the flow properties, and in the microscale, by the adhesion and
friction forces between the particles. Compressibility is the ability to
reduce the volume under pressure and compactability is the ability to
build a solid tablet under pressure, with sufficient mechanical
strength and stability. Powders are often compacted to make them
easier to handle and transport and also to reduce dust problems. One
of the most important processes is press agglomeration. The press
agglomeration process of powders is also influenced by feed
properties such as particle size and shape distribution, modulus of
elasticity, moisture content, flow properties and temperature
[6,12,24,27].
Most frequently the design of efficient processing equipment
requires the data of tablet density ρ, angle of internal friction φ,
coefficient of wall friction between powders and apparatus or
machine wall μ, modulus of elasticity E and lateral stress ratio k.
Modulus of elasticity E characterises the elastic deformation of
powder under compression load and is one of the parameters
required for numerical modelling of uniaxial compression using the
discrete element method (DEM) [5]. For structural engineer it
determines how much a bar will sag under its own weight or under
a loading when used as a beam within its limit of proportionality [17].
These parameters are in particular interest of professionals using
computer aided design that recently has become very common tool
[3]. Equipment design for handling and processing requires experi-
mental values of this parameter that depends on moisture, pressure,
load history, density, porosity, internal structure and kind of material

0032-5910/$ – see front matter © 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.powtec.2010.06.010
 M. Stasiak et al. / Powder Technology 203 (2010) 482–488 483

test with additional measurement of lateral stress. Eurocode 1 [7]

recommends the uniaxial compression test under loads similar to
those occurring in the full-scale process.
The modulus of elasticity E was found to be strongly influenced by
moisture content, compacted density and porosity. Liu [15] measured
the modulus of elasticity E of sand and found approximately threefold
change in the values with varying experimental parameters. Investiga-
tions on agricultural bulk solids by Moya et al. [18,19] confirmed very
strong influence of moisture content and pressure level on the value of
modulus of elasticity E.
The objective of this study was to determine essential process
parameters of three cohesive powders during compaction: the
compacted ρ and instantaneous density ρi, the modulus of elasticity
E and strength of the press agglomerate σB. These parameters are
useful to design effective and reliable processes with granular
materials as well as for numerical modelling of mechanical behaviour
Fig. 1. Particle size distributions of bentonite, limestone and microcrystalline cellulose.
of granular materials.

[15,18,22,27]. Eurocode 1 part 4 [7] recommends to determine two 2. Powder samples

values of effective modulus of elasticity. One, denoted Eload, is
measured during loading of the sample and the second, Eunload, Reported project was performed for bentonite, limestone and
during unloading. Calculation of values require two ratios of change in microcrystalline cellulose (MCC). Powder particle size distributions are
lateral stress to change in the vertical stress Kload and Kunload that are presented in Fig. 1 [11]. The particle size distribution was determined
determined during loading and unloading using uniaxial compression by Mastersizer 2000 (Malvern).
The mean diameter d50, moisture content XW specific surface Sm by
gas adsorption (BET) and air permeation methods (Blaine) as well as
Table 1
true particle density ρs are listed in Table 1 [11]. The large differences
Granulometric characteristics of powder samples.
in surface areas of both test methods, especially at bentonite and MCC,
Material d50 Xw Sm in m2/g Sm in m2/g ρs in show the large influence of internal pores and asperities of the
in μm in % (BET) (Blaine) kg/m3 particles. Only materials at equilibrium moisture content were
Limestone 20 0.56 2.28 0.45 2590 investigated because the main interest of the project was to
Bentonite 7.4 4.65 16.51 0.8 2640 characterize parameters of powders useful industrial conditions of
MCC 70.2 5.09 4.84 0.434 1551
operation, namely roller press agglomeration.

Fig. 2. Hydraulic press and uniaxial compression chamber.

484 M. Stasiak et al. / Powder Technology 203 (2010) 482–488
Fig. 3. Universal testing machine (TIRAtest) with equipment to determine the tensile strength of tablets applying diametrical compression force.
3. Methods
3.1. Uniaxial compression in hydraulic press
First, the compaction behaviour of cohesive powders during
compression in hydraulic press was analysed to determine the initial
density ρ0, the compacted density ρ and the instantaneous density ρi
during powder compression. The influence of maximum pressure and
deformation rate was examined. Experiments address the problem of
agglomerate quality obtained in compaction tests. The secant modulus
of elasticity Esec was calculated as dependant on deformation rate v and
maximum pressure p.
The uniaxial compression tests of bentonite, limestone and MCC
were performed in a hydraulic press, in a 40 mm in diameter chamber,
70 mm high (Fig. 2). All experiments were conducted for the initial
height of powder sample of 60 mm. The displacement was measured
by an inductive sensor having accuracy of 0.01 mm. The sensor was
mounted with a rubber coupling to avoid moments generated by
eccentric forces occurring during the experiments.
The tests were performed at two deformation rates v = 3.5 and
9.5 mm/s for maximum pressure p in a range from 30 to 60 MPa with
the step of increase of 5 MPa. Speed v = 3.5 mm/s is the minimal
which could be obtained in hydraulic press and comparable with
Fig. 4. Typical pressure–displacement relationship from hydraulic compression tests
and method to determine secant modulus Esec during loading.
speed v = 2 mm/s in universal testing machine while v = 9.5 mm/min
is characteristic for speed of deformation in roller press during
production of agglomerates. All experiments were performed in three
replications and the results were statistically elaborated.
3.2. Testing the agglomerate strength
After compaction experiments, the tablet strength was tested by a
universal testing machine. The strength of agglomerates was obtained
for tablets compacted at pressures of p = 30, 45 and 60 MPa and for two
deformation rates v of 3.5 and 9.5 mm/s. The tablets were diametrically
compressed between circular plate and stamp as shown in Fig. 3.
During the experiments, the stamp was moving down with
constant deformation rate v of 0.033 mm/s. The real time, compres-
sion force in N and displacement in mm of the moving stamp were
recorded continuously.
3.3. Uniaxial compression in universal testing machine
The uniaxial compression tests of powder samples for loading and
unloading were performed using the same universal testing machine
to determine the strength of agglomerates. From these tests the
Fig. 5. Influence of powder sample on the modulus of elasticity Esec calculated on the
basis of loading. Points denote mean values and vertical bars the 0.95 confidence
interval.
 M. Stasiak et al. / Powder Technology 203 (2010) 482–488 485

Fig. 7. Compacted density of powder agglomerates versus compression pressure.

of 0.01 mm. Next, the sample was unloaded at the same deformation
rate until zero stress level was reached. The tests were conducted in
three replications.
For data evaluation the model, equation of Sawicki [21] was used.
During the loading both reversible (elastic) and irreversible (plastic)
strains develop in the sample: εz = εez + εpz . Two phases of unloading
can be observed (see Fig. 2). The first phase is characterised by a
purely elastic deformation and was used to determine the modulus of
elasticity E. The second stage of unloading is characterised by both
elastic and plastic deformations. During the first phase of unloading,
the sample shows linear response which is characteristic for
reversible elastic deformation. Thus εz may be expressed as [21]:

!
2
σz 2ν
εz = 1− : ð1Þ
E 1−ν

4. Results

4.1. Secant modulus of elasticity by uniaxial compression in hydraulic

press

Based on the experimental curves (pressure versus relative

displacement) the secant modulus of elasticity Esec was determined
as recommended by European Standard Eurocode 1 [7] (Fig. 4).
Fig. 5 presents the secant modulus of elasticity Esec calculated for
each maximum pressure and for the two deformation rates. Variance

Fig. 6. Influence of maximum compaction pressure on the modulus of elasticity Esec.

Points denote mean values and vertical bars the 0.95 confidence intervals.

modulus of elasticity E of powders was calculated based on the first

linear part of unloading curve (see Fig. 2). At this phase of unloading
only elastic response of the material takes place [21,22]. The method is
also recommended by European Standard [7]. These tests were also
performed to determine the elastic recovery Δh of tablets after
unloading. The powder was filled into the test chamber without
vibrations or another compression effects. The sample was 60 mm
high and 40 mm in diameter. The bed was loaded to the reference
vertical stress σz of 10 and 20 MPa. The top cover of the apparatus was
moving down at a constant deformation rate of 2 mm/s, while the Fig. 8. Density of powder agglomerates versus deformation rate obtained in uniaxial
displacement was measured with an inductive sensor having accuracy compression tests on hydraulic press.
486 M. Stasiak et al. / Powder Technology 203 (2010) 482–488

Fig. 10. Breakage strength of bentonite, limestone and MCC agglomerates obtained for
three maximum compaction pressures at v = 9.5 mm/s.

for bentonite Esec were obtained in the range from 75 to 106 MPa, and
low values — from 47 to 62 MPa for MCC, while for limestone
Esec = 209 to 276 MPa. Relationships between secant modulus of
elasticity Esec and compression pressure p were fitted by linear
approximation. Coefficient of determination of R2 = 0.68 for bentonite
and MCC was higher than that R2 = 0.12 obtained for limestone.
In Fig. 6 results of calculated Esec from experiments on universal
testing machine at 10 and 20 MPa of maximum pressure are
presented for comparison. These values are lower than linear fits of
values of secant modulus obtained by uniaxial compression in
hydraulic press at the pressures ranging from 30 to 60 MPa.

4.2. Compression function by hydraulic press

Li and Puri [14] presented an empirical relationship between the

compression behaviour and the initial bulk density. The authors found
that limestone had the highest bulk density for loose packing (approx.
900 kg/m3). The microcrystalline cellulose had the lowest initial bulk
density (approx. 300 kg/m3) but its compressibility index was the highest.
The aim of the final part of the experiments was to determine the
initial density ρ0, the instantaneous density ρ0 and density of powders
during the process of compaction ρ in hydraulic press. For all
experiments the relationships between instantaneous densities and
vertical deformation were determined, but the most important
parameter in tablet production is the agglomerate density ρ (Fig. 7).
The highest values of density ρ in the range of maximum pressure
from 30 to 60 MPa and at the two constant deformation rates of v 3.5
and 9.5 mm/s were found for limestone. The lowest values of ρ were
obtained for MCC in a range from 860 kg/m3 for p = 30 MPa to

Fig. 9. Compression force–displacement tests of bentonite, limestone and MCC

agglomerates obtained for three maximum compaction pressures at v = 3.5 mm/s.

analysis was performed to estimate the influence of deformation rate

on modulus of elasticity Esec. No significant effect of deformation rate
(F-ratio = 0.33) was observed for three experimental materials.
Significant differences were found in modulus of elasticity Esec
between powders (see Fig. 5). The highest value of modulus of
elasticity Esec = 255 MPa was obtained for limestone, the lowest for
MCC. For bentonite the modulus of elasticity Esec = 90 MPa was found
to be nearly two times higher than for MCC. The elongated fibre-like
shape of the largest MCC particles could be the reason for higher
deformability of this powder bed. The limestone powder consists of
crushed particles with rough surface and shows lower deformability.
From all considered factors influence of compression pressure was
the strongest. The results are presented in Fig. 6. For bentonite and Fig. 11. Typical experimental data obtained for loading and unloading cycle of bentonite
MCC an increase in pressure from 30 to 60 MPa resulted in significant powder in universal testing machine for two maximum compression pressures p = 10
increase of modulus of elasticity Esec. Values of modulus of elasticity and 20 MPa. Straight lines represent tangents of the first parts of unloading curves.
 M. Stasiak et al. / Powder Technology 203 (2010) 482–488 487

Fig. 12. Sequence of micro-processes and deformation mechanism during press agglomeration.

1100 kg/m3 for p = 60 MPa and were strongly affected by maximum
compaction pressure. For limestone and bentonite an increase in
pressure resulted in a small increase of ρ from 1820 to 1880 kg/m3
and from 1700 to 1840 kg/m3, respectively. Practically no influence of
deformation rate on density ρ was noted (Fig. 8). Using the
compression function on physical basis, [26], defined the compress-
ibility index n, as:
 
ρ p n
= 1+ : ð2Þ
ρ0 σ0
In current investigations its values of 0.092 (for limestone), 0.175 (for
bentonite) and 0.650 for MCC was found higher than those obtained by
[10,11]. Tablet density was analyzed in detail by Sinka et al. [23] and by
Wu et al. [27]. Sinka et al. [23] examined compaction of microcrystalline
cellulose and concluded that that non-uniform density distribution was
mainly caused by wall friction within the die. Factors such as friction,
geometry, loading schedule and method of filling the die all influence
compaction but conclusions regarding density distribution cannot be
generalized. Each practical situation requires individual analysis. Wu et al.
[27] analyzed compaction of lactose powder and pointed out to
localization of intensive shear stresses during unloading that caused
breaking of tablets upon ejection. A set of reported effects was a probable
reason of discrepancies in our results and those obtained by other authors.
Obtaining of coherent results in different laboratories require similarity of
equipment as well as precise control of condition of compaction.
4.3. Strength and compaction function of agglomerates
During the experiments different types of deformation were
observed, Fig. 9. MCC was reported as a mainly plastic deforming
powder by Inghelbrecht and Remon [13] who analysed roller
compaction and tabletting of MCC.
Using the maximum compression force at breakage point B the
tensile or breakage strength of agglomerates σB was calculated as in Fell
and Newton [8] (FB — breakage force, d — tablet diameter, and h —
height of tablet), Fig. 10:
lowest, σB = 0.012 and 0.027 MPa, for limestone tablets. Values of σB for
MCC were higher than those estimated by [10]. The largest increase of
breakage strength approximately 200% with increasing compaction
pressure was observed for bentonite and MCC tablets. In the case of
limestone tablets σB increased only of nearly 120%. No significant
influence of the deformation rate was observed on tablet strength σB.
4.4. Modulus of elasticity by uniaxial compression in universal testing
machine
Elastic constants were determined using experimental results from
linear phase of unloading. Fig. 11 shows the relationships between the
compression stress σz and the relative displacement εz for loading–
unloading cycles of bentonite powder at maximum compression
pressures of 10 and 20 MPa. In Fig. 12 schematic of change modes of
deformation is illustrated. The first part of the loading curve reflects
compaction of the sample with translation and rotation movements of
particles, at relatively small contact deformations, Fig. 12b) and c). The
second, steeper part of the curve shows a sharp increase in the elastic–
plastic contact stresses associated with deformations of entire particles
and their breakage, Fig. 12d) and e) [1,2]. During loading, deformation
takes place in contacts as well as volume deformations of particles.
Controlling the elastic recovery is very important in the processing of
powders compacts because defects, such as cracks and fractures of
powder compacts may occur as an effect of faster elastic recovery or
spring back. According to Wu et al. [27] the phenomenon requires
further research. Obtained values of modulus of elasticity E and elastic
recovery Δh of the tablets are presented in Table 2.
Tested parameters E and Δh were found to be dependent on the
powder and on the maximum stress. For all samples tested, the
modulus of elasticity E increased with increasing maximum pressure
Table 2
Modulus of elasticity E calculated on the basis of linear part of unloading and elastic
recovery Δh determined in uniaxial compaction tests at universal testing machine.
Powder Maximum pressure Modulus of Elastic recovery of
material p in MPa elasticity E in MPa tablets Δh in mm

Bentonite 10 48.4 ± 2.5 1.66 ± 0.08

2⋅FB
σB = : ð3Þ 20 71.4 ± 2.8 2.10 ± 0.54
π⋅d⋅h Limestone 10 55.6 ± 3.1 2.05 ± 0.07
20 81.2 ± 3.0 4.02 ± 0.08
The highest values of σB, 1.14 and 3.95 MPa for respectively 30 and MCC 10 30.4 ± 3.5 2.60 ± 0.05
20 56.5 ± 7.2 2.79 ± 0.09
60 MPa of maximum pressure, were obtained for MCC tablets while the
488 M. Stasiak et al. / Powder Technology 203 (2010) 482–488
p. The highest values of modulus of elasticity E = 55.6 MPa for 10 MPa
of compression pressure and E = 81.2 MPa for p = 20 MPa, were
obtained in the case of limestone, while the lowest values were
obtained for MCC. Modulus of elasticity E of MCC ranged from
30.4 MPa to 56.5 MPa and that of bentonite ranged from 48.4 MPa to
71.4 MPa. Modulus of elasticity of MCC was also determined by
Michrafy et al. [16] by a four-point beam bending test at different
densities. The authors obtained modulus of elasticity E = 90 MPa for
pressure of 60 MPa, in good agreement with our results.
Experiments performed on the universal testing machine allowed to
obtain elastic recovery Δh of tablets after uniaxial compression [Fig. 11].
Values of this parameter are presented in Table 2. The lowest value of
elastic recovery Δh =1.66 mm was obtained for bentonite at p =10 MPa,
and the largest, Δh =4.02 mm, for limestone at p =20 MPa.
5. Summary and conclusions
The highest value of secant modulus of elasticity Esec = 255 MPa
determined at hydraulic press was obtained for limestone and the
lowest Esec = 55 MPa for MCC. No influence of deformation rate on
modulus of elasticity Esec was found. For bentonite and MCC an
increase in pressure from 30 to 60 MPa resulted in significant increase
of secant modulus of elasticity Esec even for 41% and 32% adequately.
The highest compressibility index n = 0.350 was obtained for MCC
while the lowest n = 0.092 for limestone.
The highest value of tablet density ρ from 1820 to 1880 kg/m3 was
obtained in the case of limestone. Lower for 45% for MCC, and for this
material it was strongly affected (increase 28%) by maximum
compaction pressure. No influence of deformation rate on this
parameter was observed.
Values of σB were found to increase with an increase in
compaction pressure p more than two times. The highest values of
breakage strength σB = 1.14 and 3.95 MPa for p = 30 and 60 MPa
were obtained for MCC tablets, and the lowest adequately 0.012 and
0.027 MPa for limestone tablets. Deformation rate during compaction
had no significant influence on tablets breakage strength.
The largest values of modulus of elasticity E = 55.6 MPa for 10 MPa
of compression pressure and E = 81.2 MPa for p = 20 MPa calculated
on the basis of the first phase of unloading were obtained in the case
of limestone, while the lowest ranged from 30.4 MPa to 56.5 MPa
were values obtained for MCC.
The lowest value of elastic recovery Δh = 1.66 mm was obtained
for bentonite and more than 200% higher for limestone.
Acknowledgment
This project was supported by DFG in the frame of project DFG
project (TO 156/18–2): Modeling of cohesive powder compaction in
the roller press.
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