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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
Institute of Agrophysics, Polish Academy of Sciences, P.O. Box 201, 20-290 Lublin 27, Poland
Otto-von-Guericke University, Magdeburg, P.O. Box 4120, 39106 Magdeburg, Germany
a r t i c l e
i n f o
Article history:
Received 4 February 2010
Received in revised form 19 May 2010
Accepted 14 June 2010
Available online 21 June 2010
Keywords:
Compression test
Powder compaction
Modulus of elasticity
Tablet density
Tablet strength
a b s t r a c t
The compression and compaction behaviour of bentonite, limestone and microcrystalline cellulose (MCC)
three cohesive powders widely used in industry were studied. Uniaxial compression was performed in a
cylindrical die, 40 mm in diameter and 70 mm high, for three selected cohesive powder samples. The initial
density, instantaneous density and tablet density were determined. The inuence of maximum pressure and
deformation rate was examined. The secant modulus of elasticity Esec was calculated as a function of
deformation rate v, maximum pressure p and powder sample. After compaction experiments in hydraulic
press at three pressures p = 30, 45 and 60 MPa and two different deformation rates, the strength of the
produced tablets was examined in a material strength testing machine.
From uniaxial compression tests performed on the universal testing machine for loading and unloading, the
modulus of elasticity E was calculated on the basis of the rst linear phase of unloading. The total elastic
recovery of tablets was also obtained.
2010 Elsevier B.V. All rights reserved.
1. Introduction
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 efcient
equipment requires more precise information about physical properties 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).
0032-5910/$ see front matter 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.powtec.2010.06.010
grains or particles, adhesion and friction between particles, interparticle contact geometry and prior history of loading [20].
Compressibility and compactability of a powder are inuenced by
the ow 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 sufcient 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 inuenced by feed
properties such as particle size and shape distribution, modulus of
elasticity, moisture content, ow properties and temperature
[6,12,24,27].
Most frequently the design of efcient processing equipment
requires the data of tablet density , angle of internal friction ,
coefcient of wall friction between powders and apparatus or
machine wall , 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 experimental values of this parameter that depends on moisture, pressure,
load history, density, porosity, internal structure and kind of material
Table 1
Granulometric characteristics of powder samples.
Material
d50
in m
Xw
in %
Sm in m2/g
(BET)
Sm in m2/g
(Blaine)
s in
kg/m3
Limestone
Bentonite
MCC
20
7.4
70.2
0.56
4.65
5.09
2.28
16.51
4.84
0.45
0.8
0.434
2590
2640
1551
483
484
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 0, the compacted density and the instantaneous density i
during powder compression. The inuence 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. 5. Inuence 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 condence
interval.
485
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: z = ez + pz . Two phases of unloading
can be observed (see Fig. 2). The rst 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 rst phase of unloading,
the sample shows linear response which is characteristic for
reversible elastic deformation. Thus z may be expressed as [21]:
z =
z
E
!
2
2
:
1
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
486
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 tted by linear
approximation. Coefcient 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 ts 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 nal part of the experiments was to determine the
initial density 0, the instantaneous density 0 and density of powders
during the process of compaction 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 (Fig. 7).
The highest values of density 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 were
obtained for MCC in a range from 860 kg/m3 for p = 30 MPa to
Fig. 9. Compression forcedisplacement tests of bentonite, limestone and MCC
agglomerates obtained for three maximum compaction pressures at v = 3.5 mm/s.
Fig. 11. Typical experimental data obtained for loading and unloading cycle of bentonite
powder in universal testing machine for two maximum compression pressures p = 10
and 20 MPa. Straight lines represent tangents of the rst parts of unloading curves.
487
Fig. 12. Sequence of micro-processes and deformation mechanism during press agglomeration.
=
0
p n
1+
:
0
2FB
:
dh
The highest values of B, 1.14 and 3.95 MPa for respectively 30 and
60 MPa of maximum pressure, were obtained for MCC tablets while the
lowest, B = 0.012 and 0.027 MPa, for limestone tablets. Values of B 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 B increased only of nearly 120%. No signicant
inuence of the deformation rate was observed on tablet strength B.
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 z and the relative displacement z 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 rst part of the loading curve reects
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 h of the tablets are presented in Table 2.
Tested parameters E and h 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 h determined in uniaxial compaction tests at universal testing machine.
Powder
material
Maximum pressure
p in MPa
Modulus of
elasticity E in MPa
Elastic recovery of
tablets h in mm
Bentonite
10
20
10
20
10
20
48.4 2.5
71.4 2.8
55.6 3.1
81.2 3.0
30.4 3.5
56.5 7.2
1.66 0.08
2.10 0.54
2.05 0.07
4.02 0.08
2.60 0.05
2.79 0.09
Limestone
MCC
488
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