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PARTIC-636; No. of Pages 16

ARTICLE IN PRESS

Particuology xxx (2014) xxx–xxx

Contents lists available at ScienceDirect

Particuology

journal homepage: www.elsevier.com/locate/partic

**Numerical investigation into the inﬂuence of the punch shape on the
**

mechanical behavior of pharmaceutical powders during compaction

Alexander Krok ∗ , Marián Peciar, Roman Fekete

Slovak University of Technology in Bratislava, Faculty of Mechanical Engineering, Bratislava, Slovak Republic

a r t i c l e

i n f o

Article history:

Received 9 September 2013

Received in revised form

21 November 2013

Accepted 3 December 2013

Keywords:

Powder

Die compaction

FEM

a b s t r a c t

During the production of pharmaceutical tablets using powder compaction, certain common problems

can occur, such as sticking, tearing, cutting, and lamination. In the past, the compressibility of the powder

was calculated only along the axis of the device; consequently, critical areas of the material throughout

the volume could not be identiﬁed. Therefore, ﬁnite element method (FEM) can be used to predict these

defects in conjunction with the use of an appropriate constitutive model. This article summarizes the

current research in the ﬁeld of powder compaction, describes the Drucker–Prager Cap model calibration

procedure and its implementation in FEM, and also examines the mechanical behavior of powder during

compaction. In addition, the mechanical behavior of pharmaceutical powders in relation to changes in

friction at the wall of the system is examined, and the dependence of lubrication effect on the geometry

of the compaction space is also investigated. The inﬂuence of friction on the compaction process for the

ﬂat-face, ﬂat-face radius edge, and standard convex tablets is examined while highlighting how the effects

of friction change depending on the shape of these tablets.

© 2014 Published by Elsevier B.V. on behalf of Chinese Society of Particuology and Institute of Process

Engineering, Chinese Academy of Sciences.

1. Introduction

Tablets are a notably popular form of medicine in the pharmaceutical industry. Tablets have numerous advantages over other

dosage forms, such as their low cost, long storage life, mechanical

and chemical stability, good heat and moisture resistance, accurate dosage, and ease of use for the patient. Tablets are generally

manufactured by compressing a dry powder mixtures; compression may be one of the most signiﬁcant operational processes

in the pharmaceutical industry. Through research, many experimental methods for analyzing the compression process have been

developed. Empirical and regression models (Guyot, Delacourte, &

Marie, 1986; Heckel, 1961; Jetzer, Leuenberger, & Sucker, 1983;

Leuenberger & Rohera, 1986; Rue & Rees, 1978; York, 1979) have

been used for a long time. Although these models provide numerical data that are obtained using the comparison method, they are

not usually appropriate for quantitative forecasting. In most cases,

these methods offer a calculation of compressibility only along the

axis of the equipment; therefore, identifying the critical areas of the

material throughout the entire volume is not possible. In addition,

these experimental methods are often unable to identify the physical nature of the entire compaction process. Later, the process was

**∗ Corresponding author. Tel.: +421 949431543; fax: +421 252962454.
**

E-mail address: alexander.krok@stuba.sk (A. Krok).

**subjected to a more detailed analysis, and the given process was
**

simulated with the constructed models. These phenomenological

constituent models are based on experimental measurements and

the mechanics of particulate materials. Currently, these models can

be applied to FEM (ﬁnite element method) (Cunningham, Sinka, &

Zavaliangos, 2004; Diarra et al., 2012; Kadiri, Michrafy, & Dodds,

2005; Michrafy, Ringenbacher, & Tchoreloff, 2002; Shang, Sinka,

& Pan, 2012; Sinka, Cunningham, & Zavaliangos, 2003; Wu et al.,

2005; Zhang et al., 2010). These works describe the calibration procedure for the constituent model, its application in FEM, and the

investigation into the mechanical behavior of the powder during

compaction. While manufacturing these products, some common

faults, such as sticking, stretching, chipping, restricting or laminating of the product, may occur. Accordingly, FEM in conjunction

with a suitable constituent model is likely to be a very effective

instrument for predicting problems and defects during this process. Numerous publications (Han et al., 2008; Kadiri et al., 2005;

Sinha, Bharadwaj, Curtis, Hancock, & Wassgren, 2010; Sinka, Burch,

Tweed, & Cunningham, 2004; Wu et al., 2008) compared the experimental and calculated data from the FEM simulations, both for

pharmaceutical and cosmetic powders, revealing very good conformity. Microcrystalline cellulose (MCC) Avicel is one of the most

frequently tested powder materials.

Intensive research into powder compaction has revealed that

the elastic properties of a powder signiﬁcantly affect the appearance of cracks (Han et al., 2008; Kadiri & Michrafy, 2013;

1674-2001/$ – see front matter © 2014 Published by Elsevier B.V. on behalf of Chinese Society of Particuology and Institute of Process Engineering, Chinese Academy of Sciences.

http://dx.doi.org/10.1016/j.partic.2013.12.003

Please cite this article in press as: Krok, A., et al. Numerical investigation into the inﬂuence of the punch shape on the mechanical

behavior of pharmaceutical powders during compaction. Particuology (2014), http://dx.doi.org/10.1016/j.partic.2013.12.003

& DiMaggio. For example. 2003) or with micro-identiﬁcation (Han. Coube. The phenomenological Drucker Prager Cap model (DPC model) was originally developed to predict the plastic deformation in soils during compaction. 2000.org/10. and Müller (1995) through nuclear magnetic resonance (NMR) microscopy. In conjunction with this approach. and due to the increasing efﬁciency of computer technology. Cundall & Strack. DPC phenomenological model 2. interesting work regarding the distribution of density in die pressing was carried out by Macleod and Marshall (1977). The law of hardening p pb = f (εv ) determines the relationship of the hydrostatic compression yield stress (pb ) and the corresponding volumetric plastic p strain εv = ln(RD/RD0 ). Schoﬁeld & Wroth.. Hofstetter. The authors also present photographic evidence of the cracked tablets using X-ray tomography. 1972. Krok et al. The results contribute to the research in this ﬁeld because to date. 2013.. 2008. where RD is the relative density and RD0 is the initial relative density of the non-compacted powder.. Particuology (2014). Wu. and Aydin. (1) where ˇ is the internal friction angle. 2007. ﬂat-face radius edge (FFRE) and standard convex (SC) tablets. Sharma. Sinka et al. Michrafy. 2008). p and q. Gakwaya. http://dx. Zhou. 2006. and I is the identity matrix. softening or consolidation. A. the effects of the wall friction may intensify. 2005). p = (1/3) (3/2)(S : S) is the Mises equivis the hydrostatic stress. as expressed by Eq. these models describe the behavior of granular materials or soils. Cocks. ˛ secures the constant ﬂow between Fc and Fs and is designated as the coefﬁcient for the transition curve. DEM (discrete element method) methods are frequently employed (Cleary. The authors of the following references (Cunningham et al. Yang. Tardos. 2008. (iii) and the transition surface (Ft ) that joins the Fs and Fc . Zhu. 2003. 2005) forecast that the DPC areas depend on the density. Lehmann. 2000). & Yu. Sinka et al.doi. is the stress tensor. 2002. & Guillot. & Kadiri. 2. however. depicting the main shear ﬂow of the material during compaction. & Park. Fig. Wu et al. S is the tensor of deviator stress: S = + pI. and q = alent stress. 2003.. 2004. 1979.. Kadiri & Michrafy. and when describing the unloading process. 2002. 2004..partic. are expressed as follows: p= 1 (z + 2r ). testing by X-ray tomography is described. 2000. Kim. 2004. Wu et al. The experiments show that non-linear segments at the end of the compression curves can occur. (3) where z and r are the axial and radial stresses. & Lee.. 1971. 2007).. 1994. 1968. and Henkel (1957). but only the static behavior of a material without addressing the various states of the powder. (4) where R is the cap eccentricity (cap shape parameter). (4): Fc (p. Wu et al. Wood. we will work exclusively with the relative density. 2005). Jonsén & Häggblad. Cunningham et al. Sinka et al.1016/j. 1999.. Haririan. Michrafy et al. 1991). in the articles (Djemai & Sinka. 3 (2) q = |z − r |. Baladi. this parameter reﬂects the changing composition of the powder during compaction more accurately.G Model PARTIC-636. of Pages 16 ARTICLE IN PRESS A. Mazel. The inﬂuence of friction on the process of compaction is identiﬁed for ﬂat-face (FF). Since the ﬁrst presentation by Drucker. The shape of the punch has been investigated by FEM (Eiliazadeh. 2008. Han et al. et al. 1 assumes that the behavior of the material is isotropic. Gurson & McCabe.12.. and these segments become even more apparent in a relatively uncompressed material. & Tweed.. 1996. Pitt. Numerical investigation into the inﬂuence of the punch shape on the mechanical behavior of pharmaceutical powders during compaction. q) = q − p tan ˇ − d = 0. James. 1993). Han et al. The ‘cap’ surface (Fc ) represents an ellipse with a constant eccentricity in the p–q plane. Coube & Riedel. 2002. 2003. Choi. Kadiri & Michrafy. representing a material constant and determining the shape of the ‘cap’ surface. this density distribution was investigated using the indentation-hardness mapping test (Sinka et al. Farber. In the past.. 2013. RD is the ratio Please cite this article in press as: Krok. Drucker & Prager. 2008) indicated that the effects of wall friction can be partially reduced by using a lubrication system.. Busignies. 2003. The shear failure surface (Fs ) in the DPC model provides the criterion for achieving shear ﬂow and depends on the cohesion and the internal friction angle (deﬁned according to the Mohr–Coulomb hypothesis). No. Han et al. Gakwaya. 1976.1.. The distribution of the shear stress depends on the speed of the punch. pa is the evolution parameter that determines the compaction. 1987. but may provide a broader picture of the behavior of the materials beyond the boundaries of practical use. This segment was created to facilitate the numerical application of FEM.. becoming modiﬁed and expanded (Cunningham et al. Some researchers (Aydin et al. 2008.. By changing the shape of the punch. Watson & Wert. Briscoe. this plastic model has changed. Han et al. The experimental measurements of pharmaceutical powders show non-linear behavior during the unloading phase. the change in stress for the powder during compression is not significant. The authors (Coube & Riedel. Wu et al. & Wu. This study was performed to verify whether reducing the friction is a sensible strategy and whether any anomalies in the distribution of the stress and in the density of the tablet appear.. & Tchoreloff. During our calculations and evaluations. depending on the volume of plastic deformation.003 . & Michaels. 2004. (ii) the ‘cap’ surface Fc . One method for retaining the quality of the tablet is to change its shape. and the area of the DPC model is composed of three segments (Chtourou. utilize the law of non-linear elasticity.2013. The previous researchers concluded that by changing the wall friction during the production of ﬂat-faced tablets. Diarra. Gross. commonly causing tablet cracking during compression. et al. DiMaggio & Sandler. Newton. 2000. Korachkin. Furthermore. (1): Fs (p. / Particuology xxx (2014) xxx–xxx 2 Wu et al. 2005) consider the non-linear segments at the end of the curves to be the result of dilation during compaction and therefore dependent on wall friction. The aim of this contribution was to address the real effect of lubrication use and focus on extreme states that have no signiﬁcance from the practical point of view. & Briscoe. Green. as expressed in Eq. The presented article offers results contributing to an investigation into the mechanical behavior of pharmaceutical powders relative to changes in the wall friction of the system and analyses how the effect of lubrication can be observed as a function of the geometry of the compression space. Cocks. Lewis. & Taylor. & Woods. Simo. Background Various phenomenological models that describe geo-materials are available (Chtourou. Gethin. Gilia. & Thompson. no previous simulations have been undertaken to the extent that they have spanned in this study (eight different wall friction coefﬁcients for eight different geometry conﬁgurations). 2004. and Sanhtürk (1996) through auto-radiography or Nebgen. 1992. the changes in the effects of friction relative to the shape of these tablets are also reported. 2004. Frenning. 2005. 2004. 2008. Oh.. Dodds.. 2013. In most cases. 1993): (i) the shear failure surface (Fs ). & Podczeck. 2000. Sandler. Saxena. Kim. depicting the mechanism of non-elastic hardening during plastic compaction. such as hardening. Later.. For the uniaxial cylindrical die compaction test. d is the cohesion. q) = (p − pa )2 + Rq 1 + ˛ − ˛/ cos ˇ 2 − R(d + pa tan ˇ) = 0. Gibson. 1952.

& Cunningham.org/10. Zhang et al. Shang et al. Toussaint. the cohesion (d) and the internal friction angle (ˇ) must be known. 1947. A short description of the situation is included in Fig. Krok et al.2013. the unloading occurs. Accordingly. The situation in which it is possible for the powder to change its stress state throughout the entire process is illustrated in Fig. undergoing plastic deformation to behave according to the non-elastic mechanism of hardening. the material exhibits its elastic properties and attempts to regain its original state. Coube. cracks usually appear in the structure of the material. & Gakwaya. of the bulk density (b ) of the material to the true density of the particles of which the material is composed (T ). precluding it from industrial engineering applications. therefore creating a diagonal load across the tablet. 2008.12.2. 2001. 2001. No. 2. Pavier & Doremus. Frocht. Ft (p. Procopio.. During the second phase. 2008. 2. & Alvain. meaning that the material reduces its stress to a small extent but does not exceed the shear failure curve. During this phase.G Model ARTICLE IN PRESS PARTIC-636. the uniaxial tension (1). When the thickness is larger. such as an experimental investigation in a die compaction test equipped with a sensor for measuring the axial and radial stress (Chtourou. 2002. Numerical investigation into the inﬂuence of the punch shape on the mechanical behavior of pharmaceutical powders during compaction. http://dx.doi. 1. For practical reasons. The unloading continues. these values are obtained experimentally (Brewin. diametrical compression (3) and uniaxial compression (4) (Doremus. This experiment is expensive and requires a long-term and complicated procedure for evaluating the measured data (Koerner. of Pages 16 A. the procedure is partially modiﬁed and the number of measurements is reduced. 1970. This state is expressed by the curve DE. & Tweed.1. such that the material continues to reduce its stress up to the moment when it achieves shear failure (curve Fs ). the behavior is isotropic and linearly elastic. To revert to its original state. Other calibration methods have been developed to identify the material parameters of the DPC model. Coube. as expressed by the curve CD. An illustration of Drucker–Prager Cap model. 2012). & Riedel. q) = (p − pa )2 + q − 1 − − ˛(d + pa tan ˇ) = 0. the slope of this line gives the internal friction angle (ˇ). This process continues up to the moment when the stresses in the radian and axial directions are equal. 1970). a straight line emerges. et al. Rottmann. shear (2). Diametrical compression is a simple test in which two opposing forces (FD ) compress a tablet composed of the material under investigation to reach various volume densities. A diametrical compression test and a uniaxial compression test are undertaken to measure the strength of the product using this equipment. it is assumed that the material is compressed. 1999. ˛ cos ˇ 2 (d + pa tan ˇ) (5) 2. the diameter should be ﬁve times bigger than the thickness.. This phase is characterized by the curve BE. Calibration of DPC model The most effective method for calibrating the DPC model is through an experimental investigation of the compaction of particulate material using a three-axis test. specifically when the material attains its hydrostatic equivalent stress (p > 0) and its von Mises’ equivalent stress is zero (q = 0). Fell & Newton. the material expands. Doremus. During the ﬁrst phase. The transition surface (Ft ) is given by Eq. Depending on the loading size on the material by the punch. As shown in Fig. (5) and the main shape of the DPC area does not depend on the Ft area. 1. 2. using some of the energy gained during compression. The ﬁnal part of the unloading process is the so-called dilation of the material.2. A. Timoshenko & Goodier. 1971. The diametrical compression test (3) is often carried out on a Brazilian compactor. the material is acting in accordance with the elastic mechanism of unloading. Zavaliangos. 2010).003 . and the uniaxial compression (4) is tested such that the shear failure surface retains its linear shape along the total range. and its stress decreases. Han et al. 2003) are used to construct the shear failure curve (Fs ). In this case. time-consuming and expensive. The displacement of this line represents the cohesion (d). Guillot. This procedure is laborious. The process does not end here. After plotting the results of these measurements in the p–q plane. Cohesion and internal friction angle To deﬁne the shear failure surface.partic. The curve BC expresses the ﬁrst stage of unloading. the stress state will only partially widen along Please cite this article in press as: Krok.1016/j. This phase is characterized by the curve AB. In an idealized example. the powder decreases in porosity while increasing its density. / Particuology xxx (2014) xxx–xxx 3 Fig.. After reaching this stage. Particuology (2014)..

No. (7) Uniaxial compression is a common test used to determine the parameters of the material. 2004.1016/j. Eqs. To facilitate these calculations. as does the slope and intercept of the straight line. The force that broke this tablet can be calculated according to the above-stated formulas for stress. [pd .e. qd ] at which the tablet failed the strength-tests can be calculated. et al. A. of Pages 16 ARTICLE IN PRESS A. d and c (i. 2. From the measured forces. √ c d ( 13 − 2) d= . pd . Han et al. 3 d qd = √ 13d . Particuology (2014). The relation h/D is very important. Eq. representing one given density of the tablet. the crack must expand to the center of the tablet. the boundary state will be expressed as follows: 1 pc = − c . radial stress ( r ). and (c) stress state change on the p–q plane.G Model PARTIC-636. These forces are created by pressure. Dh (6) where D is the diameter of the tablet and FD represents the break force of diametrical compression and d is diametrical tensile strength. and thus pc . these values are then plotted onto the p-q plane. resulting in a non-homogeneous stress distribution.doi.partic. After a certain angle.org/10. Shang. the measured value of the forces changes. A cylindrical object is pressed from both sides by FC . This test illustrates the strong inﬂuence of slip forces. A straight line is constructed. From this data.003 . On the p–q plane (pd . 3 qc = −c . D2 (8) where FC represents the uniaxial tensile strength at the yield point. Krok et al. the tested tablet was brought to the breaking point. axial strain (εz ). / Particuology xxx (2014) xxx–xxx 4 Fig. qd – stress state for diametrical compression). The intercept of these lines represents the cohesion (d) and the slope of this straight line represents the internal friction angle (ˇ). Numerical investigation into the inﬂuence of the punch shape on the mechanical behavior of pharmaceutical powders during compaction.2013. (b) axial stress ( z ) vs. the boundary state is expressed as follows: pd = 2 . Subsequently. depending on the h/D ratio. 2012) and the resultant shape of these parameters is described by Eqs. (11) Please cite this article in press as: Krok.. (9) In the previous tests. (10) and (11). qc – stress state for uniaxial compression) plane. qc . (6) and (8)). http://dx.12. affecting the results by 30%. qc ].. Evolution of powder stress state during compaction: (a) axis stress ( z ) vs. the numerous points [pc . (6) is used: d = 2FD . these parameters can be analytically deduced (Cunningham et al. (10) c + 2d ˇ = tan−1 3( + d) c c . including those in other industries. and qd (Eqs. a break-line is formed that continues throughout the entire body and appears in the ﬁnal product. h represents the height of the tablet. During the experiment.. In the p–q (pc . 2008. (7) and (9)) are found. the axial compression strength ( c ) is calculated: c = 4FC . the plane. If a tablet with different geometric dimensions is used.

396 1.238 0.98 25.976 2.706 0.785 0.785 0.662 30. Cap shape and the hardening curve To deﬁne the cap surface.67 0.78 30.729 2. In Fig.8 18.358 18.42 24.4 24.943 20.747 0.061 17.4 1.856 0. the appropriate parameters can be calculated.54 30.G Model ARTICLE IN PRESS PARTIC-636. the hydrostatic yield stress (pb ).808 0.375 1.249 2.308 18.387 1. By using regression analysis.608 11.1016/j.459 1.453 1. From the known mass (mT ).24 25.33 18.415 1. and the transition coefﬁcient (˛) must be known.739 0. No.74 0. http://dx. From the measured break force of diametrical compression (FD ) and break force of uniaxial compression (FC ).809 0.738 0.982 2.837 0.848 0. 3. Table 1 shows that the diametrical test has been carried out for samples with a relative density in the range of RD ∈ 0.679 0.922 2.432 1. the evolution parameter (pa ). (10) and (11). the parameters d and c can be calculated for any selected value of RD with good conformity (R2 > 98%).29 19.78 26.706 23.704 0.404 18.353 2.75 0.707 0.901 20.895 0.081 18.869 11.385 2.677 0.423 2. Particuology (2014).331 2.418 1.206 19.546 18.1 25 25. 4.2. 5.24 25. 3 and 4.853 0. Krok et al.652 0.903 0.8 27.24 24.396 1.836. the values for d and ˇ are thus calculated. / Particuology xxx (2014) xxx–xxx 5 Table 1 Measurement data obtained from the diametrical and uniaxial tests.756 17.708 2. A summary of the measured data from the diametrical and uniaxial tests is depicted in Table 1. Numerical investigation into the inﬂuence of the punch shape on the mechanical behavior of pharmaceutical powders during compaction.835 0.393 17.779 0. while the uniaxial test uses samples with a relative density in the range of RD ∈ 0.366 1.2013.894 0.org/10.029 18. 5 the curves that determine the relationship between z and the volume plastic strain (εv ) are measured.4 1.78 30.2.04 28. ˛ is chosen as a small number (0. By using Eqs.86 30.6 26.675 0.44 25.412 1.747 0.743 2.06 26. the eccentricity (R).807 0. In Fig.857 0.103 18.934 2.398 1.778 2.314 17. height (h) and given the diameter D = 1.408 2. Fig.444 1.5 26.92 28. A.12.837 0.423 2.785 0.894 0.749 0.398 1.003 .236 19. 2.703 0.162 19.419 1.705 0.738 0. Changes of axial stress ( z ) with the axial strain (εv ) obtained experimentally under various values of compaction stress (100–300 MPa).584 2.652.954 18.640 11.737 0. 0.653 0.287 18.16 25. Please cite this article in press as: Krok.4 26.557 2.812 Fig.68 0.675.855 0.836 FC (N) 4659 4787 4999 4827 4840 8192 8106 8157 8208 8336 11.294 2.653 0.392 1.61 2. this step must be carried out to synchronize both tests. of Pages 16 A. the relative density of the tablet (RD) can be calculated.698 19. 0.partic.675 0. The evolution parameter and the eccentricity are calculated by measuring the die compression system.739 2.443 1.65 0.656 18.078 17.860 11.418 1. 6 the Fig.945 18.571 17.124 18.409 2.854 20.903.6 2.598 2.803 0.391 1.982 19. Dependence of cohesion (d) on the relative density (RD) of the tablet.18 mm of the tablet.903 68 61 69 65 63 144 144 148 136 136 244 246 229 236 223 431 421 431 427 442 651 687 656 652 658 18.986 2.25 17.343 2.doi.414 1..853 0.823 17.436 1.805 0.828 18. The dependence of ˇ and d on the relative density of the tablet is illustrated in Figs.84 30.652 0. Dependence of the internal friction angle (ˇ) on the relative density (RD) of the tablet.366 1.749 0.784 0. mT (g) h (mm) RD FD (N) mT (g) h (mm) RD 1.46 30.470 20. et al.01).

G Model ARTICLE IN PRESS PARTIC-636. As mentioned in the introduction. 1976..e. providing pB and qB . 6. the relative density of the tablet corresponding to the ﬁve values of compaction stress... Sandler et al. The hydrostatic equivalent yield stress (pb ) as a function of the volume plastic strain (εv ) – the hardening curve. At this point (B). 2). 2005. 2004. (12). (4). z = r . (2) and (3). / Particuology xxx (2014) xxx–xxx 6 Fig. ˛. prior experiments showed that non-linear segments exist at the end of the unloading curves (Aydin et al... ˇ. The eccentricity (R) vs. the following is valid: ∂Fc p εij = ˙ ∂ij = f d. pa . 2008. Using this assumption has led to an unrealistic simulation of decompression. the law of non-linear elasticity is used to describe the . pa . 2008. ˇ. To avoid this problem. Jonsén & Häggblad. These ﬁgures show that ﬁve curves were measured with varied compaction forces and loading stresses from the punch (100–300 MPa). By using Eqs. qB ) = f (d.. R) = 0. Changes of axial stress ( z ) with radial stress ( r ) obtained experimentally under various values of compaction stress (100–300 MPa). Shang. i. point B is assumed to represent the maximum axial and radial stress during the process (Fig. 2005). where is the wall friction coefﬁcient between the material and the die wall. 2004. the cap line is assumed to run through point B. Han et al. during which the plastic compression almost ceased (Wu et al.qB Fc (pB . these measured points are plotted onto the p–q plane. 8. ( z ) is proportional to the radial stress on the wall. as does the derived cap line. During 2D simulations. R = 0. Krok et al. 1996. 2012) from Eqs. 2005) due to dilation during the die compaction. curves that determine the relationship between the axial and radial stresses during the compaction process are measured.. (13) The required parameters can be analytically derived (Cunningham et al. Cunningham et al. Han et al. Fig. of Pages 16 A. To calculate pa and R. 7. and (13): Fig.. No. ˛. Wu et al. (12) pB .

The shear modulus K and the bulk modulus G may be expressed as follows: K+ 4 B − zC .doi.partic. K and G are calculated. and according to Eqs.org/10. (ii) the gradient of the radial stress is negligible. numerous assumptions must be accepted: (i) the radial stress is proportional to the axial stress. pb = pa (1 + R tan ˇ) + RD. http://dx. 3K + G (19) = 3K − 2G .003 . (16) is the result of the Eq. 9 and 10. Using these equations. the elastic behavior of the materials must be independent of the stress path to avoid hysteresis. r = kz . (14) 2 2(1 + ˛ − ˛/ cos ˇ) (pB − pa ). 2) with the axial strain (εBz and εCz ) and axial stress (zB and zC ). Particuology (2014). Numerical investigation into the inﬂuence of the punch shape on the mechanical behavior of pharmaceutical powders during compaction.1016/j. In the elastic portion. Please cite this article in press as: Krok. These parameters are discovered through experimental measurements.12. (19) and (20).2.. (14)–(16). et al. 3qB (15) p The hardening curve (pb = f(εv )) is calculated using Eqs. Eq. One advantage of this route is that the measuring equipment is a die compression tester. The dependence of the change in these parameters on the relative density of the tablet is illustrated in Figs. (4) when assuming q = 0 and p = pb . 2 pa = − R= [3qB + 4d tan ˇ(1 + ˛ − ˛/ cos ˇ) ] 2 4[(1 + ˛ − ˛/ cos ˇ) ] + 2 9q2B + 24dqB (1 + ˛ − ˛/ cos ˇ) tan ˇ + 8(3pB qB + 2q2B )[(1 + ˛ − ˛/ cos ˇ) tan ˇ] 2 4[(1 + ˛ − ˛/ cos ˇ) ] 2 . The graphical form of the hardening curve depends on the change in eccentricity (R) and on the relative density of the tablet (RD). that is. A. Young’s modulus and the Poisson’s ratio The elastic properties of the powder may be characterized using Young’s modulus (E) and the Poisson’s ratio (). (iii) the tangential stress decompression. where k represents the proportionality coefﬁcient (if a sensor for r is not available). 2(3K + G) (20) where B and C express the position of the stress state of the material (Fig. = B √ − pC p 3K (18) E= 9GK .2013. G = zB 3 εz − εCz (17) 2G qB . (16) 2. as stated in Figs. Young’s modulus (E) and the Poisson’s ratio () can be calculated. 7 and 8.3. To proceed with the measurements.

two methods were developed to measure wall friction with a shear measurement device (ASM Handbook. The role of lubricants during production processes is often a sensitive issue. 2003.. Carr & Walker.. the stresses ( T . 11. B ) are measured with a radial pressure sensor using the following relation (Cunningham et al. 2012). Hölzer & Sjögren. Numerical investigation into the inﬂuence of the punch shape on the mechanical behavior of pharmaceutical powders during compaction. In contrast to simple diffusion mixers (e. 2012. Sommier et al. are used. Jonsén & Häggblad.. The authors who have engaged in research regarding the lubrication of pharmaceutical powders have kept strictly to short mixing times. Han et al. Van Kamp. The negative effects of lubricants on the physicochemical properties of the tablet are often manifested as a defect in the mechanical tensile strength and/or restrict the dissolution of the tablet. Bell. 2004. Yu et al.1–1%) (Celik. and Sjögren (1979). capacity or critical mixing time (Bolhuis. Pingali et al.2013.. Sinka et al. the Turbula mixer ensures rotation. a reduction in the tensile strength of the manufactured tablet occurred. 1995.003 . 1975.. 2004. 1996. A. The change in the wall friction coefﬁcient ( ) with radial pressure during compaction. Please cite this article in press as: Krok. At the interface point.G Model ARTICLE IN PRESS PARTIC-636. = 0. Porion.2. Sommier. Apart from a change of the position (z) of the upper and lower punch.doi. Particuology (2014). Measuring wall friction using a shear device is a sufﬁciently widely investigated issue that will not be presented for any details of its procedure. No.. transmission. et al. and Soininen and Kuusivuori (1980) have shown that by increasing the lubrication content in the tablet mixture.org/10. & Dettmers.1 is used. Shotton & Lewis. of Pages 16 A. Celik.. According to the authors (Kushner. Photograph of micro-crystalline cellulose taken by an electron microscope (Shang et al.5% (w/w). 1968. 2. Beyond a certain position. Mixers with a double wall (Otsuka et al. Wall friction coefﬁcient Previously..4. or by a die compactor (Aydin et al. B (21) To calculate . Otsuka. Fig. the dependence of a change in wall friction on the height of the equipment can be observed. Wu et al. 2004) or planetary. Yamane... Shang et al.1016/j. 1987.. (in the range of 0. Faugère. As observed in Fig. De Jong. V-mixers and Bin mixers) that provide mixing by rotation along a single axis. while using only very small amounts of lubrication. 1964. & Puri. as well as extending the mixing time. MCC Avicel PH 102) (Bolhuis. 9. Zijlstra. 2011). Pingali et al. (in the range of 2–20 min) depending on the type of mixer used. 2013). 2011. 2011). Sandler et al. & Matsuda. Jenike.. 1981.g. / Particuology xxx (2014) xxx–xxx 7 Fig. 2005): = D B 4h r z/H T B ln T . remaining equal throughout the entire process. Hölzer.25% and 0. which differ from each other in terms of rotational speed. 2004. and the reduced tensile Fig.. high-speed mixers (Otsuka Fig. an active material. a more obvious decrease may be observed in crystalline materials. 2001). this parameter does not change. 10. Lerk. Grygo. 1998.partic. the particles bind together. et al. http://dx. & Evesque.12. 1976. and an excipient material (e. The decreasing tensile strength of the tablets due to increased mixing times and increased amounts of lubricant are caused by the creation of a lubrication ﬁlm. Ragnarsson. 2012. & De Boer. The Poisson ratio () as a function of the relative density (RD) of the tablet for four values of compaction stress. Krok et al. 2004. Magnesium stearate (MgSt) is one of the most widely used lubricants. drum. Turbula mixtures have proven to be very suitable.. The mixing can be carried out in mixers with varied geometries and degrees of mixing ﬂexibility. 12. 2005. 2005). and inversion of the powder via Schatz geometry. Duffy. Wu et al.g... The Young’s modulus (E) as a function of the relative density (RD) of the tablet for four values of compaction stress. and cubic mixers. 2008. and its usual concentration ﬂuctuates between 0. 2011). The creation of a suitable compaction mixture from which the tablet is made is a blend of a lubricant (MgSt). 1964) (ﬂat or circular). 11 for this parameter of FEM modeling.

(b) relative density (RD) in the powder during compaction for an FF tablet. and (c) SC tablet. the reader is referred to the web version of the article.) Please cite this article in press as: Krok. 13. 14. http://dx. (b) FFRE tablet. Krok et al.12.G Model PARTIC-636. No. / Particuology xxx (2014) xxx–xxx Fig.003 . Geometry and boundary conditions of the FEM model for (a) FF tablet. et al. A. of Pages 16 8 ARTICLE IN PRESS A. (For interpretation of the references to color in text.doi.2013. Particuology (2014).1016/j. Numerical investigation into the inﬂuence of the punch shape on the mechanical behavior of pharmaceutical powders during compaction.. Distributions of the (a) von Mises stress (q).org/10.partic. Fig.

3.5 mm high for both the 2D axisymmetric model. The particles of this material are very porous and have a large surface area caused by the random grouping of the micro-crystalline ﬁbers. In this case.003 . Therefore. 15. pressure or pH. Hölzer and Sjögren (1981). and the deviation occurred only in the calculation time. where the binding capacity is stronger. The structure of the MCC Avicel PH 102 is illustrated in Fig. Krok et al.partic. 2013. The amount of simulated powder in the die was 13. When modeling the die compaction of powders. as well as the die. the calculations could be completed. the results given by the 3D model are almost identical to the 2D (two-dimensional) axisymmetric model. the 3. The upper and lower punches. 2010). The DPC model was successfully calibrated for the purposes of this work. of Pages 16 ARTICLE IN PRESS A. Therefore. The capillary mechanism between the particles facilitates the transfer of hydrophilic ﬂuids into the pressed material. The 3D simulation of the die compression of the powder was carried out on PC Intel Core i7-CPU 2. & Wassgren. in this article it is used as the model material. & Michrafy. Muliadi. The compacted powder should be a homogenous and isotropic material. 2012). & Zavaliangos. non-adaptive mesh.1. Diarra. In the initial simulations.25 mm. Litster.2 GHz. inducing the rapid dissolution of the tablets.2.. The results verify the measured data on the die compactor. ensuring a prolonged.. the diameter of the die was 5. in this speciﬁc case. After adding excess hydrophobic stearate to the mixture or increasing the mixing time. the shear forces are sufﬁcient to tear off the layers of the molecules from the magnesium stearate particles. delayed or pulsed release of the medicine into the living organism. Microcrystalline cellulose (MCC) Avicel PH 102 is one of the important pharmaceutical materials. Fig. Please cite this article in press as: Krok. 3. forming a thin layer on the particles of the excipient material.12. and the material thus happened to be as a deformable continuum.org/10. Michrafy. Michrafy et al.e. During the mixing process. this material may contain up to 70% of the active medical ingredient.. Comparison of the experimental and calculated data for the axial stress ( z ) vs. The behavior of the powder during compaction will change only along the vertical axis (i. the geometry in the cross-section does not change. the bonding properties and the dissolution speed decreases. if the shape of the compacting geometry is cylindrical (a rotationally symmetric body). MCC’s great compaction potential is used to good effect.. Concurrently. the distribution of the particles is of a different fraction. 2010. if the lubricant is added to the tablet mixture and mixed. The behavior of compression does not depend on the angle of the cross-section because Fig. Modeling powder compaction by FEM 9 the roughness is equal along the entire interior wall of the die. the axial strain (εz ) at ﬁve different loading stresses. were modeled as a solid body without any potential deformation. 3D modeling is required (Cunningham. No. it appears as a layer on the surface of the substrate. and offer complete measurements that may also help while investigating other tasks related to this issue. Numerical investigation into the inﬂuence of the punch shape on the mechanical behavior of pharmaceutical powders during compaction. 2011. Winstead. therefore. this tablet is designed to administer medications requiring regulated release of the medicine. 3D modeling of powder compaction The creation of a 3D (three dimensional) model is necessary only when the geometry is different at each cross-section or the simulated material exhibits anisotropic behavior. and Johansson and Nicklasson (1986) presume that the MgSt is later absorbed into the excipient material particles and is consequently distributed equally across the surface of the substrate. The bulk density of the powder is 300 kg/m3 . 2011. A. After applying the calculation model to ABAQUS. A ‘mapped orphan’.1016/j. 12. http://dx. All the necessary parameters regarding compression and decompression were calculated. while its true density is 1590 kg/m3 . The change of the maximum powder stress on the p–q plane during compaction for ﬁve tablets with different relative densities. the measured data used during the numerical FEM investigation was already published in (Shang et al. height) of the apparatus. Dodds. if the lubricant is prone to deagglomeration and delamination. such as Young’s modulus and the Poisson’s ratio. and for the 3D model. the calculation time was three hours. Sinha et al. was chosen. 4 GB RAM. 2013).doi. 16. Apart from the elastic properties of the material.G Model PARTIC-636. Therefore. the 2D axisymmetric model was more suitable (Diarra et al. Model material At the beginning of this section. For the 2D axisymmertric simulation.2013. et al. the calculation time was 15 s. The difference in the results did not exceed 1%.. / Particuology xxx (2014) xxx–xxx strength can be attributed to the emergence of weaker bonds between lubricant–lubricant compared to the excipient–excipient bond. Particuology (2014). Alternatively. These sophisticated medical forms are also used as sensitive hydrogels that react to changes in temperature. the diffusion or penetration of the solid particles plays a lesser role. the authors concluded that these data are of particular interest. One example is the roll compaction of powder: the walls of the rolls are moving with the model. MCC Avicel PH 102 has an average particle size of 180 m and moisture content below 5%.

the element type was C3D8R (three-dimensional hexahedral element). 14(a) shows the distribution of von Mises stress in the material cross-section.519. Distributions of the stresses for the modiﬁed FFRE tablets: (a) von Mises stress (q) and (b) shear stress (s12 ). representing the distance between the punch and the corner of the tablet. internal friction angle ˇ = 70. 4. http://dx.6423e4.039 GPa. In this study the radius ϕ was set as 1. 2. ‘cap-plasticity’ model was chosen for which input parameters. eccentricity R = 0. 2. et al..5 mm and D = 5. The initial yield surface size is Please cite this article in press as: Krok. and d2 . Numerical investigation into the inﬂuence of the punch shape on the mechanical behavior of pharmaceutical powders during compaction. whose properties for the modeling process are as follows: cohesion d = 0. 14(b) shows the distribution of relative density in the powder throughout the entire process. Young’s modulus E = 12.5 mm for FFRE tablet.org/10. It is assumed that d1 = d2 /2. was set as 1. The USDFL user subroutine was developed to calculate the distribution of the relative density of the powder during the entire process. Master-slave contacts with ﬁnite sliding were chosen to model the interaction between the wall of the apparatus and the powder. where d1 represents the distance between the punch and the center of the tablet. The difference between creating a 2D axisymmetric or a 3D model was as follows: for the 3D task. such as hardening curve. transit coefﬁcient ˛ = 0.partic. For the SC tablet.G Model PARTIC-636. and Fig.003 . similar to the FF tablet. for the FFRE tablet. Besides h and D. the height and width of the tablet also remained the same.1016/j.7119εv .5. the ﬁrst tablet was an FF tablet. and the transition coefﬁcient from calibration were deﬁned. These states are marked with letters A through H.doi. 1. or 3.148 and hardening curve pb = 2. During the FEM simulation.12. Changing the shape of the radius ϕ at the corner of the tablet was also possible. Krok et al. / Particuology xxx (2014) xxx–xxx Fig. the height and width of the tablet could be changed. No. cohesion.25 mm. The following dimensions were retained: h = 13.56◦ . of Pages 16 10 ARTICLE IN PRESS A. internal friction angle. the element type was CAX4R (twodimensional axisymmetric quadrilateral element). 3. additional parameters d2 and d1 were chosen to deﬁne the tablet geometry. while the slip interactions were expressed using the coefﬁcient of friction for the wall. or 2. eccentricity. while in the 2D axisymmetric case. A.5. As observed in Fig. Poisson’s ratio = 0. 13.01. Particuology (2014).2013. Results and discussion Fig. 17.279.

G Model PARTIC-636. Depending on the loading pressure of the punch. Krok et al.003 . et al. the level of the von Mises stress increased slightly. A. In dataset G. eccentricity (R). Figs.0005. the course of compaction can be observed. 4. The radial stress is approximately equal to the axial stress. the correct cohesion (d). / Particuology xxx (2014) xxx–xxx 11 Fig. Distributions of stresses for the modiﬁed SC tablets: (a) von Mises stress (q) and (b) shear stress (s12 ). the coefﬁcient of friction for the wall ( = 0. and the ﬂow stress ratio is zero. when the stress across the entire cross-section is zero. the material reaches the end of its decompression. Young’s modulus (E) and Poisson’s number () must be set according to the measured data from the DPC model calibration. Dataset E shows the course of unloading when the compression stress from the punch no longer acts on the particulate material and elastic behavior occurs more intensively.1. and the punch speed Please cite this article in press as: Krok..2013.1016/j. No.partic.doi. and the wall friction ( ) remain the same. Inﬂuence of punch shape on compaction To demonstrate the inﬂuence of the punch shape. Therefore. The geometry.12. 0. For each selected RD. 2. some properties of the powder have to be changed because relative density is bound to the parameters of the DPC model. the authors began with the assumption that the properties of the powder. 15 and 16 compare the FE analysis from the ABAQUS program with the results from the powder compaction experiment for ﬁve tablet samples with different RD. 18. In datasets B and C. internal friction (ˇ). boundary conditions of the apparatus walls. This state conforms with point C in the DPC model in Fig. Numerical investigation into the inﬂuence of the punch shape on the mechanical behavior of pharmaceutical powders during compaction.org/10. 14(a) dataset A. and in dataset D. Particuology (2014). of Pages 16 ARTICLE IN PRESS A. The red lines in the pictures reveal the shift away from the maximum level of deformation in the material when the von Mises stress achieves its lowest values. In dataset H.1). Compaction begins in Fig. the material is compacted to its maximum value. http://dx. these parameters cannot be selected independently.

The top row represents the distributions of von Mises stress and the bottom row represents the distributions of shear stress in the FF tablet samples.partic. http://dx. the reader is referred to the web version of the article. 17 and 18 show that when changing the shape of the compression space. (For interpretation of the references to color in text.12. the reader is referred to the web version of the article. the distribution of the von Mises stress is homogenous.) Fig.003 .. 13. No. (For interpretation of the references to color in text. The geometry of the model and the boundary conditions are stated in Fig. Figs.2013. as well Fig. for the FF tablet.org/10. the reader is referred to the web version of the article. As observed in Fig. A. the shear surfaces are created only in proximity to the wall of the die because the wall presents the greatest resistance toward the movement of the particles during compaction. 20. et al. Krok et al. while the actual change to the simulation model consists only in a change in the geometry.1016/j. Change of the powder stress on the p–q plane with the change in the geometry of the model (d2 ) and the wall friction coefﬁcient ( ) for the SC tablets.) Please cite this article in press as: Krok. In this case. of Pages 16 12 ARTICLE IN PRESS A. 19.doi. and signiﬁcant changes can be observed only in the corners of this model due to the wall friction. Particuology (2014). / Particuology xxx (2014) xxx–xxx Fig. Dependence of the powder stress on the wall friction coefﬁcient ( ) for the FF tablets. The interaction of the shear stress between the powder and the punch is negligible for the FF tablets. the pressure distribution changes. 14(a). The interaction between the powder and the wall of the die. Numerical investigation into the inﬂuence of the punch shape on the mechanical behavior of pharmaceutical powders during compaction. (For interpretation of the references to color in text.G Model PARTIC-636. Change of the powder stress on the p–q plane with the change in the geometry of the model (R) and the coefﬁcient of wall stress ( ) for the FFRE tablets.7 mm/s) remain the same as for the FF tablet (see the above part of Section 4). 21.) (v = 0.

along with the corresponding hydrostatic stress (p). when increasing ϕ for an FFRE tablet. 2008.003 . The procedure used to test the inﬂuence of the wall friction involved using eight different wall friction coefﬁcients (0. the material must exert part of the energy from compaction to overcome this resistance. the resistance that the punch shows in relation to the movement of the material is also reduced. http://dx. the contact interaction is increased by the contribution of interaction between the powder and the punches. the von Mises stress (q) changes only minimally (Han et al. If the friction coefﬁcient is decreased. Kadiri & Michrafy. In Fig. 19 the reduction of stresses p and q due to lubrication in the range of 0. A. These lines express how the maximum q and p values changed (Fig. In Figs.2. Krok et al. Concurrently.4) for each geometric model.12.org/10.. The inﬂuence of lubrication appears more signiﬁcant after changing the punch geometry. The slope angle of the punch surface is no longer favorable.2013. This result is natural because.05 ≤ ≤ 0. Wu et al. In this case. after an increase in lubrication. the von Mises stress (q) was set to a maximum value on the p–q plane. the sensitivity of the reduction of this stress depends on the geometry of the punches. the results of this investigation are presented on the p–q plane for a clearer interpretation of the results.. Han et al. Therefore.partic. 22 shows that the shear friction is primarily concentrated near the interface between the punch and material.4 for the geometry of the SC tablets (four full black lines marked with colored points) can be observed.doi. 19 and 20. after greasing the punch surface and the walls of the apparatus. Particuology (2014). a more intensive transfer of the stress Please cite this article in press as: Krok. 4. therefore. No. 2.. the impact of the coefﬁcient of the wall friction on the mechanical behavior of the powder was investigated. 19 and 20 four differently colored lines can be observed. 2008. by reducing the wall friction coefﬁcient. the distribution of the von Mises pressure for the SC tablets is shown. 18. change the stresses more signiﬁcantly for the FFRE tablets. of Pages 16 ARTICLE IN PRESS A. capping and lamination faults can be caused by increasing the local concentration of the shear stress. In Fig. Fig. As observed in Fig.. As observed in Figs.05 ≤ ≤ 0. 2008). as well as the interaction with the top and bottom punches. Inﬂuences of friction and punch shape on compaction In this section. the stress on the powder is inﬂuenced by the shear friction from the wall of the die. The result is a non-homogeneous distribution of the von Mises stress in the compacted material. This ﬁgure shows that the effects of the wall friction that originate from the interaction with the top and bottom punches. the total average stress of the SC tablet decreases. / Particuology xxx (2014) xxx–xxx 13 Fig. as the interaction between the powder and the compression punch. in this case.. Numerical investigation into the inﬂuence of the punch shape on the mechanical behavior of pharmaceutical powders during compaction. the stress also increases due to the better transfer of the force in the volume of the sample.1016/j. lubrication has no effect on the distribution of stress in the volume of the tablet. point B) with the wall friction coefﬁcient for the given shape of the model. et al. are signiﬁcant for this shape. 2008) and was found to be acceptable. Wu et al. The effect of lubrication can be observed in the lower right corner (blue area). Concurrently. This range was selected by (Eiliazadeh et al. against which the material is pressed. Dependence of the powder stress on the wall friction coefﬁcient ( ) for the SC tablets. In addition. 2004. The top row represents the distributions of von Mises stress and the bottom row represents the distributions of shear stress in the SC tablet samples. adding lubrication can change the shape of the emerging shear areas. 22. as well as a large shear that also appears due to the radial elasticity of the material. 21. that is.G Model PARTIC-636.. For each calculation. FFRE and SC tablets were used. 2013. for the FF tablets with a ﬂat punch.

No. 2008.5).G Model PARTIC-636.org/10.. 2004. the change in the maximum p and q caused by the lubrication for the geometry of the FFRE tablet (four full black lines marked with colored dots) can be observed. making the tablet more compact. the von Mises stress was concentrated near the wall of the compaction space.4) experimentally. To achieve a higher wall friction coefﬁcient ( = 0.4–0. The principle for obtaining the shear friction coefﬁcient has been presented in Section 2. and the reformation is shifted toward the core of the tablet. In the range of 0. Numerical investigation into the inﬂuence of the punch shape on the mechanical behavior of pharmaceutical powders during compaction. similar to the SC tablet. 20 is interesting. 23). a few minor alterations are necessary. 23).15.g. lubrication yielded a tablet with lower stress than its original value.12. While z dominated initially. Dependence of the powder stress on the wall friction coefﬁcient ( ) for the FFRE tablets..4. http://dx. the effect of r began to appear under reduced friction. the stresses (p and q) increase.) among the particles occurs. while at = 0. when = 0. Consequently. the reader is referred to the web version of the article. and the stress begins to decrease. The top row represents the distributions of von Mises stress and the bottom row represents the distributions of shear stress in the SC tablet samples.. To measure the compaction of the powder in a die with a range of (0. Michrafy et al. If the friction is large ( = 0. which is where the most stress is located.2013.4). After a reduction in friction.15–0.2. the mobility of the particles in contact with the punch surface increases.) The shape of the curves in Fig.4. / Particuology xxx (2014) xxx–xxx Fig. If the wall friction begins to decrease signiﬁcantly due to lubrication. the stresses q are concentrated at this point (Fig.4). When the friction is high ( = 0. Around the circumference of the wall. but the average stress takes up a greater volume.1016/j. during the ﬁnal analysis. A. the stress is minimal. In Fig. After reducing the wall friction coefﬁcient to 0. Particuology (2014). of Pages 16 14 ARTICLE IN PRESS A. the experience of other authors (e. Because the punch has a conical surface.35).05. 23. and in the wall surroundings. et al. the interior surface of the die must be roughened or a different construction material that suits the required properties for the apparatus must be used.05 the emerging area was already distanced from the wall in the direction of the internal volume of the tablet. This change may result in the change in stresses of z and r due to the reduced stress. Wu et al. (For interpretation of the references to color in text.partic.doi.16–0.4. shear areas are formed. 23 for FFRE tablets with a wall friction coefﬁcient = 0. Han et al.05–0. the mobility of the particles at the contact point with the punch surface is restricted. while the core remains only slightly compressed (Fig.. the horizontal component of the force begins to press the powder toward the center of the sample (tablet) due to the disintegration of the forces acting between the punch and the powder. Reaching such a low wall friction coefﬁcient for tablets without Please cite this article in press as: Krok. this trend reverses. the stress is concentrated in the center of the tablet. 20. (See Fig. To acquire a lower wall friction coefﬁcient ( = 0. Krok et al.15 ≤ ≤ 0. 2008) was useful. 23). Consequently. the sample reforms near the wall of the cylinder (see red areas in Fig. Therefore.003 .05 ≤ ≤ 0. the movement of the particles in proximity to the surfaces of the compacting apparatus is freed.

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