Bachelor of Pharmacy program

Third year B Pharm program

PM 3125:Pharmaceutical technology I
Compression and compaction
of powder solids
Physics of the compression and decompression

Dr. HMAJ Halahakoon BPharm (Specialist) MSc; PhD (Pharmaceutical Science)

Generally, the tabletting process (compression/compaction)
is influenced by several factors including :
 formulation properties,
 process parameters such as compaction speed,
 geometrical factors including punch shape and tooling
dimensions,
 lubrication,
 and ambient conditions such as temperature and relative
humidity.
 COMPACTION PROFILES
• The powder particles during compression is governed by factors
such as pressure (or stress), the amount of deformation (or
strain), and the rate of deformation (or strain rate) at the
particulate level.
• The stress-strain behavior of the particles during compression can
be affected by factors like:
The nature of the equipment used,
The physicochemical properties of the solid,
 The ambient conditions of temperature and humidity
- Two important mechanisms by which materials may deform
under stress are elastic deformation and viscous flow.
 Elastic, viscous and viscoelastic stress-strain behavior
1.The theory of elasticity, according to which the stress in elastic
solids is always directly proportional to strain but is independent of
the rate of strain.
This is the basis of the Hooke’s law of elasticity, which can be
expressed as:

where, = stress, = elastic strain and E is the modulus of elasticity,

or the Young’s Modulus, of the solid assuming an isotropic nature.
 The elastic strain is completely recoverable upon the removal of
stress.
 Elastic, viscous and viscoelastic stress-strain behavior

Change over from elastic state to plastic state is

characterized by the yield strength (σ0) of the
material.
2. The theory of hydrodynamics, according to which the
stress in viscous materials (fluids) is always directly
proportional to the rate of strain but is independent of the
strain itself.
This is described by Newton’s law of flow of viscous fluids:

where, = rate of strain, and is the coefficient of viscosity.

• The strain in viscous materials is non-recoverable upon the
removal of stress.
Elastic, viscous and viscoelastic stress-strain behavior
The phenomenon of gradually increasing strain under
constant stress is called creep, while the phenomenon of
gradually diminishing stress under a constant strain is called
stress relaxation.
Materials which show these deviations from ideality may
not be able to recover their deformation instantaneously
and/or completely upon the removal of stress and are called
viscoelastic materials.
- Viscoelasticity is the property of materials that exhibit both
viscous and elastic characteristics when undergoing
deformation.
 Compression Cycle
Powder compression can be divided to
few phases accordingly to the time of
the compression.
These are:
(i) Consolidation time: time to reach
maximum force.
(ii) Dwell time: time at maximum force.
(iii) Contact time: time for compression
and decompression excluding ejection
time.
(iv) Ejection time: time during which
ejection occurs.
(v) Residence time: time during which
the formed compact is within the die.
 Compression Cycle
The force-time profile gives
information about these phases as
well as various characteristic
parameters of the compression cycle.
Consolidation time is the time to
reach maximum force.
dwell time is the time at puncher
no longer experience vertical
displacement .
contact time is the time for
compression and decompression.
 Compression Cycle

Schematics showing tableting punch head

designs with different head flat (HF) dimensions
(a) and the graphical representation of
Some researchers have defined dwell time as an interval compaction profiles associated with change in
during which maximum compaction pressure is head flat dimensions
maintained by the punches during the compaction cycle
 Compression Cycle

In Figure the shown compression force-time curve is divided into compression, dwell-time, and
decompression phases. The area under the curve A1 represents compression phase. Areas A5
and A6 are obtained by drawing a parallel line to x-axis from starting to the end point of dwell
phase. Plastic materials show a decrease in force over dwell time, in contrast a plateau is
observed for brittle materials (DCP, crystalline lactose), and therefore the dwell-time coefficient
(A6/A5) can be used to measure the plasticity of a substance mixture.
 Compression Cycle
Most compression theories and their related
equations describe only the compression stage of the
tabletting process, whereas a complete tabletting
cycle involves compression, decompression and
ejection stages.
 These theories have in effect proved inadequate to
explain some of the compression problems often
encountered in routine tablet production.
 The compression process consists of several stages, it may
seem unrealistic to look for one relatively simple formula
with few parameters covering the entire compression
process.
 It is therefore, generally agreed that the mathematical
models fit the data in either the initial or the final stage of
the densification process.
As the density must be expected that the different stages of
the process overlap each other. This makes it difficult or
impossible to point out distinct regions where only one type
of deformation — plastic, elastic or brittle — is dominating.
 Compression Cycle
The decompression stage is as important as (but not
independent of) the compression stage in determining
whether or not a tablet formulation will form
satisfactory tablets.
Some deformation processes are time-dependent and
occur at various rates during the compaction
sequence, so that the tablet mass is never in a state of
stress/strain equilibrium during the actual tabletting
process.
 Compression Cycle
The rate at which load is applied and removed may be a critical
factor in materials for which dependence time is significant.
More specifically, if a plastically deforming solid is loaded (or
unloaded) too rapidly for the process to take place, the solid may
exhibit brittle fracture.
In view of this, research investigations in recent years have shifted
to relating the capping and lamination tendencies of tablet
formulations to their plastic and elastic behavior during the
compression/ decompression/ ejection cycle.
The same deformation characteristics that come into play during
compression and play a role during decompression.
FORCE-VOLUME RELATIONSHIPS IN THE COMPRESSION
- The end of the compressional process may be recognized as being the point
at which all air spaces have been eliminated, i.e. vb = vt and therefore E = 0.
The decreasing porosity resulted from a two-step process:
1. The filling of large spaces
2. The filling of small voids by deformation or fragmentation at higher loads.
This process can be expressed mathematically:

where Eo is the initial porosity, E is the porosity at pressure P, and K1, K2, K3
and K4 are constants. The two terms on the right side of the equation refer to
steps (1) and (2) respectively.
 COOPER-EATON EQUATION
- Cooper-Eaton equation assumes that the compression of powders follows a two-
step process.
- The first step is the rearrangement of particles so that the particles fill those voids
that are larger than or of the same size as that of the particles.
- In the second stage there occurs deformation(elastic, plastic, fragmentation),
whereby the voids that are smaller than that of the particles are filled due to applied
pressure.
- This process can be expressed mathematically:

- Where, D0 is the relative density of the powder at zero pressure, D is the relative
density at pressure P, a1, a2 indicate the proportion of the total compaction achieved
by filling those voids larger or of the same size (a1) and smaller (a2) than the actual
particles. Constants k1 and k2 describe the pressures at which this two-stage
densification is thought to occur.
FORCE-VOLUME RELATIONSHIPS IN THE COMPRESSION
(Stage i) represents the initial
repacking of the particles, followed by
elastic deformation.
 (stage ii) until the elastic limit is
reached. Plastic deformation and/or
brittle fracture then dominates.
(stage iii) until all voids are virtually
eliminated.
At this point, the onset of stage iv,
compression of the solid crystal lattice,
occurs.
 FORCE-VOLUME RELATIONSHIPS IN THE COMPRESSION
- The relationship between applied
pressure (P) and some volume
parameter such as porosity (E) does
become linear over the range of
pressure commonly used in
tabletting (region iii ).
• an equation first suggested by
Shapiro has been shown to fit data
obtained from several
pharmaceutical materials: Where Eo is the porosity when the
Log E = Log Eo – K P pressure is zero, and К is a
constant.
 FORCE-VOLUME RELATIONSHIPS IN THE COMPRESSION
The Walker equation
= K1-K2

- In the area of pharmaceutical

powder technology, the global
models of Heckel and Kawakita have
typically been the most frequently where E is the porosity when the
used model to describe the F-V-P pressure applied, and К1,K2 is a
constant.
relationship during the compression.
 THE HECKEL EQUATION
- Shapiro and Konopicky published data based on powder
compression, where the natural logarithm of the tablet porosity as
a function of the applied pressure was used to describe the process.
- The Shapiro-Konopicky-Heckel equation, but for the sake of
simplicity it will be referred to as the Heckel equation.
- The equation is based on the assumption that compression of
powders is analogous to a first-order chemical reaction, the pores
being the reactant and densification of the bulk being the product.
- The equation was first developed and applied on compression of
metals, materials known to deform predominately plastically.
R = – d[A]/dt = k [A] =ke
On integrating and putting e equal to e0 at P equal to 0 gives;

ln [A] = ln [A]o – kt

ln = ln +kP
 THE HECKEL EQUATION

where E is the porosity of the powder bed and P the applied compression pressure,
A and k are materials dependent parameters.
For a cylindric tablet, P is given by：

where D is the tablet diameter, F - force.

D
Similarly, values of E can be calculated for any stage from： H
w

where w is the weight of the tabletting mass, is its true density, and H is the thickness of
the tablet at that point (obtained from the relative punch displacement measurements).
 THE HECKEL EQUATION
; Like linear function y =mx + C
Relative density ρR
ρR = Powder density at P pressure
True density of the powder
Porosity E = (1- ρR )

ρR
 THE HECKEL EQUATION
In 1961, Heckel proposed a relationship between
the constant K and the yield strength for a range
of metal powders.
K = 1/3 σ
where, σ is the yield strength of the material. K is
inversely related to the ability of the material to
deform plastically.
the intercept of linear portion A gives
densification of the powder as a result of initial
particle rearrangement (Da):
A = ln [1/1–D0] + B
Yield strength is defined in engineering as the amount of stress
(Yield point) that a material can undergo before moving from elastic
deformation into plastic deformation.
Yielding - a material deforms permanently
 THE HECKEL PLOT
A Heckel profile is normally distinguished by
three different regions,
an initial nonlinear part (Region I),
followed by a linear part where the data
obey the expression (Region II),
finally, a non-linear region (Region III) .
Heckel parameters have been shown to be
more dependent on the compression–
decompression cycle than on the size of die.
A typical Heckel plot
 THE HECKEL PLOT

- Curves i, ii, and iii represent decreasing particle size fractions of the same
material. Type a curves are typical of plastically deforming materials, while
those in which fragmentation occurs initially tend to show type b behavior.
- Type a Heckel plots usually exhibit a higher final slope (Ky) than type b.
- The two regions of the Heckel plot are thought to represent the initial
repacking stage and the subsequent deformation process, the point of
intersection corresponding to the lowest force at which a coherent tablet is
formed.
THE HECKEL PLOT
 THE HECKEL PLOT
 The crushing strength of tablets can be correlated with the value of Ky
of the Heckel plot; larger values of Ky usually indicate harder tablets.
 Such information can be used as a means of binder selection when
designing tablet formulations.
Note that Heckel plots can be influenced by the overall time of
compression, the degree of lubrication, and even the size of the die, so
that the effect of these variables should be considered.
Another important factor in the use of all force-porosity relationships is
that for many formulations, there is a relatively narrow optimum
residual porosity range that provides adequate mechanical strength,
rapid water uptake, and hence, good disintegration characteristics.
The initial porosity can affect the course of the entire compressional
sequence, and that in general, slow force application leads to a low
porosity for a given applied load.
 THE HECKEL PLOT
 Kuentz and Leuenberger postulated a modified Heckel
equation which allows the description of the transition
between the states of a powder to the state of a tablet.

Where, σ is the pressure, ρ is the relative density, ρc is the critical

density, and C is a constant similar to the constant K in the Heckel
equation, the constant C in the modified Heckel equation shows high
values for plastic behavior and low values for brittle powder
behavior.
- The effect of varying particle size of a material on the constants
derived from the Heckel equation has been investigated by
researchers.
- For plastically deforming materials (sodium chloride and potassium
chloride) Hersey et al and Humbert-Droz et al reported that measured
yield pressures, Py were independent of particle size.
- However, for materials that are thought to deform by particle
fragmentation (lactose and calcium carbonate), Hersey et al and York
found that yield pressures increased with a reduction in particle size.
- Roberts & Rowe extended the concept by investigating the effect of
punch velocity on the mean yield pressure of a wide variety of
materials and have shown that each material can be characterized by a
strain rate sensitivity index.
 The Shapiro General Compression Equation
- The Shapiro General Compression Equation can be seen as a
refined Heckel equation, where an exponential term is added to
describe the first curved part of the compression profile.
= - kP – fP0.5
- where E is the porosity of the powder bed, E0 the initial porosity of
the powder bed, P the applied compression pressure and k and f are
parameters.
- The k parameter is in theory equal to the Heckel parameter, and the
f parameter is an indication of the initial curvature in Region I.
 THE KAWAKITA EQUATION
- Another way of representing compression data is to relate the volume
reduction (engineering strain) of a powder bed to the applied pressure, and
the most familiar expression in this class is the Kawakita equation.

C= 𝟎
𝟎
Where C is the degree of volume reduction, (where V0 is the initial volume of
the powder bed and V is the volume under applied pressure), P is the applied
Axial pressure, and a and b are parameters.
The Kawakita equation is often considered to be best suited for analysis of soft,
fluffy powders compressed under low pressures.
 THE KAWAKITA EQUATION
- The linear relationship between C and P
makes it possible to derive values of the
parameters a and b.
- The parameter a represents the maximal
engineering strain, Cmax of the powder
bed,
- and mathematically the parameter b is
equal to the reciprocal of the pressure
when the value, C, reaches one-half of
the limiting value (C=Cmax/2), as
illustrated in Figure.
 THE KAWAKITA EQUATION
- The physical interpretation of the Kawakita parameters has been discussed
in the literature, and the inverted b-parameter is claimed to reflect the
agglomerate strength, fracture strength of single particles or the plasticity
of a granule.
- The physical interpretation of the b-parameter in terms of bulk powders
have been more complicated to address, represent a resistant towards
compression.
- The Kawakita equation may also be applied to tapping of bulk powders, as a
measure of fluidity and cohesion, replacing the pressure term (P) in Eq by N
– the tapping number.

-
 Leuenberger Equation
• The Leuenberger equation was introduced in the early 1980s by Leuenberger.
• It is based on the assumption that the crosssectional area A of a cylindrical
tablet contains a number N+ of bonding contact points and a number N− of
nonbonding contact points.
• The following equation describes the contact points over the cross-sectional
area :

Where, A is the cross-sectional area and a is the unit area per bonding point.
• With the postulation of the hardness proportionality to the number of bonding
points N+ (λ, proportionality factor),
 Leuenberger Equation
• By taking into consideration that the relative decrease in the number of
nonbonding points dN-/N− has been assumed to change proportionally to the
applied compression force and in connection with the relative density dρc, the
following equation can be proposed (γ, proportionality factor),

• After numerous mathematical steps and introduction of additional

physicochemical powder technology rules, the Leuenberger equation is
reached.
• In a first phase, the Brinell hardness was used for this equation, but numerous
authors, such as Blattner, suggest the application with the tensile strength σt,
the relative density ρr, and the compaction pressure σ.
 Leuenberger Equation
• This fitting allowed the determination of the maximum possible tensile
strength σtmax at zero porosity and the pressure susceptibility γt.

• where σtmax is the tensile strength (kg/cm2) when P (compression pressure) →

∞, ρr → 1, and γ is compression susceptibility.
• Tensile strength ( σt of the compacts was calculated using
where, x is hardness (in kg/cm2), and d and t are the diameter and
thickness of the compacts (in mm), respectively.

• A main focus has been set to the factor γ because it expresses the
compressibility of the powder formulation.
 Drucker-Prager Cap (DPC) models
Recently, Drucker-Prager Cap models have been used for the compaction
analyses of pharmaceutical powders .
- Drucker–Prager Cap (DPC) is the constitutive model that is often used to study
tablet compaction. It is able to describe the complex events taking place
during compression, namely: volume reduction, shear flow, nonlinear
densification due to frictional forces, stress hardening, and elastic recovery
occurring during decompression and ejection.
- The model is pressure-dependent and assumes isotropic powder behaviour.
- The Drucker–Prager Cap (DPC) model is one of the continuum mechanical
models in which the powder is considered a porous medium.
- The DPC model is therefore frequently used to analyse the strain, relative
density changes, and stress distribution of tablets during the tableting
process.
*Isotropy is uniformity in all orientations
 Drucker-Prager Cap (DPC) models
• The DPC model is characterized by parameters such as cohesion, internal
friction angle, Young’s modulus, Poisson ratio, parameters related to volume
change and hardening mechanisms, and so on.
• In general, full calibration of the DPC model requires triaxial and hyodrostatic
compressions, and proportional loading tests.
Assumes that the behavior of the material is isotropic, and the area of the DPC model is
composed of three segments.
 (a) The Drucker–Prager Cap (DPC) model and its parameters and (b) family of DPC models for different levels
of relative density over a range of compaction.

• Figure depicts a 2D projection of DPC model at a fixed solid fraction.

• The Y-axis corresponds to the von Mises equivalent or effective stress, q, and the X-axis
corresponds to the hydrostatic pressure, P.
 • The two yield surfaces represent two types of
deformation under compression.
• At high hydrostatic pressures (advanced
compaction), the material densifies when the
pressure exceeds a certain value, Pa, as
represented in Figure a (right) by the “cap” line
(Fc).
• At low hydrostatic pressures, the material
exhibits shear failure, as represented in Figure a
(left) by the failure line (Fs).
• Therefore, at the beginning of compaction, the
DPC is a shear failure model reflecting the
dependence of strength on the intrinsic cohesion
and angle of internal friction of the powder.

Effective stress can be defined as the stress that keeps particles together or Von Mises stress is an equivalent stress value
based on distortion energy to decide if a ductile material will fail (yield or fracture) under a given loading condition.
• The shear failure surface (Fs) which describe the main shear flow of
the powder under low mean stresses and depends on the cohesion
and the internal friction angle, as expressed in;
= q – p tanβ – d = 0
Where, β is the internal friction angle,
d is the cohesion, p and q are the
hydrostatic pressure and the Mises
equivalent stresses, respectively.

(The Von Mises failure theory indicates that a

material will fail if the Von Mises stress or effective
stress of that material under load is equal or greater
than the yield limit of the same material under a
simple uniaxial tension test)
• In tablet compaction, p and q are given by Equations respectively.

Where, is the axial stress and is the radial stress.

• The “cap” surface Fc which depicts the strain-hardening plastic

behavior of the powder under high mean stresses induced during
the compaction process.
• The FC surface is represented by an elliptical shape with a constant
eccentricity, as shown in,
Where, R is a cap shape parameter that controls the shape of the cap, a is a
transition surface radius that takes a small value (typically 0.01–0.05), and pa is
an evolution parameter.
• The transition surface (Ft), the purple line in Figure, does not have any
physical meaning.
• This surface, i.e., Ft, only used to allow for a smooth transition between the
cap (Fc) and the shear (Ft) which is a numerical requirement to facilitate the
application of FEM.
• The full description of DPC model requires knowledge of flow rule.
• The DPC model uses an associated flow potential (Gc) for the cap
region and non-associated flow potential (GS) for the shear line and
transition segment.
• The Gc and Gs flow potentials are expressed as follows in Equations.
• Since the powders exhibit a strain hardening behavior during the
compaction where the volume reduces and the material becomes
harder, DPC uses a hardening rule to define the dependence of
hydrostatic compression yield stress ( ) on volumetric plastic strain
( ), as shown in Equation.

• The volumetric plastic strain is given by

Where, RD and RDo are the final and initial relative densities, respectively.
• The last powder behavior which should be included in the constitutive
model is elasticity.
• Considering the elastic behavior is of critical importance for successful
modeling of the tablet compaction process particularly during
decompression and ejection stages where most strains are elastic.
• Experimental investigations on the pharmaceutical powders have
revealed that powders offered nonlinear elastic behaviour during
unloading phase of the compaction process because of the powder
dilation phenomena.
• The elastic properties of the powder can be expressed by Young’s
modulus (E) and Poisson’s ratio (ν).
• A nonlinear elasticity law should be used to calculate the elastic
properties which should be independent of the stress path to avoid
hysteresis.
 DPC model calibration
• Calibration of DPC model means determination of model
parameters, i.e., d, β, R, , , E, and ν, which can be used in finite
element code.
Experimental procedure for calibrating Drucker–Prager Cap (DPC) model

The cohesion and internal friction angle can be obtained by conducting

diametrical compression and uniaxial compression.
From the diametrical compression test, the diametrical strength (σD), also
known as tensile strength, can be determined using
Where, FD is the maximum crush force, D and t are the diameter of and thickness of the
tablet, respectively.
The uniaxial compression test allows for calculating the uniaxial strength as
follows:

Where, Fc is the uniaxial breaking force and D is the diameter of the tablet.
Subsequently, after calculating the uniaxial and diametrical strength, the
cohesion (d) and internal friction angle can be calculated as follows:

An instrumented die compaction test is normally used to deduce the cap line
parameters, i.e., pa and R. The stress state (pB, qB) at maximum compaction,
Point B in Figure, is calculated in terms of radial and axial pressure as follows:
The Pa and R are defined as follows:

The parameter α is a small value (typically 0.01–0.05) . Lastly, the pb can be

determined as follows:
The elastic parameters, Young’s modulus (E) and Poisson’s
ratio ( ), are calculated from the unloading curve of the
instrumented die compaction test as follows in Equations.

Where, dσrr is the normal radial stress increment during unloading, dσzz is the axial strain
increment during unloading, and dεzz is the axial strain increment during unloading.

• For modeling of tabletting, DPC model’s parameters should be calculated as

a function of the relative density to take into account the changes in
powder’s properties during the process.
 Modeling applications
Typically, the finite element modelling of tabletting process can be used to:
Estimate and analyse the stress and density distributions within the tablet where
these distributions may influence the mechanical properties, dissolution, drug
release, and the potential damage during coating, and transport.
Investigate the effect of punch shape and optimize the compaction tools.
Explore the tablet failure mechanism and assess the origin of defect or crack
formation.
Estimate the break force of the tablet which can replace the empirical methods
currently used in design and the development process of pharmaceutical product.
Estimate the temperature evolution during compaction that has a direct effect on
compressibility and strength, lubricant efficiency, friction between tools, and ejection
force.
Investigate the effect of interaction (i.e., friction) between the powder and
compaction tools on the process and tablet structure.
Axial stress distribution at the end of decompression for CF Shear stress distribution within CF tablets with different
tablets with different geometric parameters. geometric parameters as they emerge from the die
 Comparison of flat- and optimal convex-faced tablets:
(a) relative density (RD) distribution, (b) shear stress distribution within the tablets as they eject from the die
Reference Article - https://doi.org/10.1016/j.partic.2018.11.002
Plot of radial pressure vs. compaction pressure
• Figure shows, flat-faced tablets (FT) exhibited lower density variation than
the Convex face tablet. The relative shear stress of the FT was 47% smaller
than that obtained for the optimal CT tablet.
• Furthermore, larger residual die press evolved during the production of FT
tablets than during that of CT tablets, and it was concluded that, if there is no
occurrence of capping or chipping, a better performance is expected from CT
than FT tablets during down-processing (coating, packaging, transportation).
 DECOMPRESSION
- If the stress relaxation process involves
plastic flow, it may continue after all
compressional force has been removed, and
the residual radial pressure will decay with
time.
The plastic flow can be interpreted in terms
of a viscous and elastic parameter in series.
This interpretation leads to a relationship of
the form：
Log Ft = Log Fm - Kt
where Ft is the force left in the viscoelastic
region at a time t, and Fm is the total
magnitude of this force at time t = 0 (i.e.,
when decompression begins). К is the
viscoelastic slope and a measure of the
degree of plastic flow.
Density distribution of powder compacted by flat-face punches:
(a) at maximum compaction; (b) after decompression.
 DECOMPRESSION

Density distribution of powder compacted by concave-face R20 punches:

(a) at maximum compaction; (b) after decompression.
Density distribution of powder compacted by concave-face R10 punches:
(a) at maximum compaction; (b) after decompression.
 DECOMPRESSION
- The materials with higher К values undergo more plastic flow; such materials often
form strong tablets.
- Alternatively, the changing at relatively low compaction forces thickness of the
tabletting mass due to the compactional force, and subsequently due to elastic
recovery during unloading, can be used to obtain a measure of plastoelasticity ϒ：

ϒ=
where Ho, Hm, and Hr are the thickness of the tablet mass at the onset of loading, at
the point of maximum applied force, and on ejection from the die, respectively.
A linear relationship between у and log reciprocal of the tensile strength of the
tablets has been demonstrated.
 In general, values of ϒ above 9 tend to produce tablets that are laminated or
capped.
 Compaction Profile
-When the powder mass undergo compression force , that the
radial die-wall force arises as a result of the tabletting mass
attempting to expand in the horizontal plane in response to the
vertical compression.
The ratio of these two-dimensional changes, the Poisson ratio, is
an important material-dependent property affecting the
compressional process.
 when the elastic limit of the material is high, elastic deformation
may make the major contribution, and on removal of the applied
load, the extent of the elastic relaxation depends upon the value
of the material modulus of elasticity (Young’s Modulus).
 Compaction Profile
The value of the material modulus of elasticity (Young’s Modulus)
value is low, there is the danger of structural failure.
Maximum compressional force level are particularly important in
such case, since most of the stored energy is released on removal
of the applied load.
If modulus of elasticity is high, there is a small dimensional
change on decompression and less risk of failure.
 Compaction Profile

Examples of compaction profiles. Dotted line 0 to A represents a highly variable response due to repacking, while at A,
elastic deformation becomes dominant and continues until the elastic limit В is reached. From В to the point of maximum
compression C, deformation is predominantly plastic, or brittle fracture is taking place. The decompression process C to D
is accompanied by elastic; recovery, and if a second yield point (D) is reached, by plastic deformation or brittle fracture D
to E. The decompression line В to C' represents the behavior of a largely elastic material.
 Compaction Profile
• In many tabletting operations, the applied force exceeds
the elastic limit (point B), and brittle fracture and/or
plastic deformation is then a major mechanism.
• For example, if the material readily undergoes plastic
deformation with a constant yield stress as the material is
sheared, then the region В to C should obey the equation
：
PR = PA - 2S
where S is the yield strength of the material.
• Note that the slope of BC line plot is unity, so that marked
deviation from this value may indicate a more complex
behavior.
• Deviation could also be due to the fact that the material is
still significantly porous
 • Perhaps the residual radial pressure (intercept
EO when all the compressional force has been
removed, is more significant, since this
pressure is an indication of the force being
transmitted by the die wall to the tablet.
• As such, it provides a measure of possible
ejection force level ( ) and likely lubricant
requirements； if pronounced, it suggests a
strong tablet capable of at least withstanding
such a compressive pressure.
• Conversely, a low value of residual radial pressure, or more significantly, a
sharp change in slope (DE) is sometimes indicative of at least incipient failure
of the tablet structure.
• In practical terms, this may mean introducing a plastically deforming component (e.g., PVP
[polyvinyl pyrrolidone] as binder, starch as diluent) to facilitate dissipation of these stresses,
and hence a more gradual change in slope of the decompression plot, a preferred feature.
 ENERGY INVOLVED IN COMPACTION
• Tablet machines, roll compactors, extruders, and similar types of
equipment require a high input of mechanical work.
The work involved in various phases of a tablet or granule compaction
operation includes
(1)that necessary to overcome friction between particles,
(2) that necessary to overcome friction between particles and machine
parts,
(3) that required to induce elastic and/or plastic deformation of the
material,
(4) that required to cause brittle fracture within the material,
(5) that associated with the mechanical operation of various machine
parts.
 WORK OF COMPACTION
• The three main deformation mechanisms that can occur to particles
within the powder bed are elastic deformation, plastic deformation
and fragmentation.
• Elastic deformation is reversible, i.e. the work stored during loading is
recovered during unloading.
• However, a material with time-dependent properties can store elastic
energy and may relax only after a period of time or after ejection from
the die.
• The energy required to cause plastic deformation or fragmentation
cannot be recovered, as these are permanent changes to the structure
of the particle.
 • A typical plot of the force exerted by the
upper punch against the displacement of
the upper punch is shown in Figure.
• The compaction process can be split into
two sections.
• The first section involves increasing the
compaction pressure to a set amount:
this is shown by the curve between A and
B.
• The area under this curve, shown by E2 +
E3, represents the total work of
compaction (WT).
Plot of upper punch force vs. upper punch displacement
during compression and decompression. • Some of the work required to compact
E1- energy for friction. E2- energy accumulated by the the tablet will be recovered in the second
tablet after compression. E3 - energy of decompression section: represented by the curve
between points B and D.
• The material usually expands to relax at
this stage. The area under this curve (E3)
corresponds to the recovered or elastic
work.
• The deduction of the elastic work from
the total work represents the
unrecoverable work (plastic work): this is
represented by the area E2.
 ENERGY INVOLVED IN COMPACTION
• The estimation of the total work involved, WT, was obtained by monitoring
punch force and the distance D through which it acted, so that:
= 𝒎𝒂𝒙
𝑭 𝟎

Example of force-displacement (F-D) curve. (▲) upper punch force; (▲) leaver punch force. The area WF represents the
work done in (overcoming friction, while that of area WD is the elastic deformation energy stored in the tablet during
compression. Thus, is the net mechanical energy actually used to form the tablet.
 ENERGY INVOLVED IN COMPACTION
• Normally, an appreciable amount of the energy supplied is converted to heat,
which of course does not contribute toward the main objective of the process.
• Energy expended in compression of 400mg Sulfathiazole Granulation
Compression Process Energy Expended (J)
Unlubricated Lubricated
Compression 6.28 6.28
Over coming the die wall friction 3.35 Negligible
Upper punch withdrawal 5.02 Negligible
Tablet ejection 21.35 2.09
Total Energy 36.00 8.37
• Note that lubrication has no apparent effect on the actual amount of energy
required to compress the material, that is overcome resistance to relative
interparticulate movement.
 STRENGTH OF TABLETS
- The mechanical strength of tablets has been described in a
variety of ways, including hardness, bending strength, fracture
resistance, friability, and crushing strength.
- The most popular estimate of tablet strength has been crushing
strength, Sc, which may be defined as “that compressional force
(Fc) which, when applied diametrically to a tablet, just fractures
it.

where ST is the tensile strength, and D and H are the diameter and
thickness of the tablet, respectively.
 STRENGTH OF TABLETS

The work Wf required to cause tablet failure correlates better

with other mechanical strength tests and is a more sensitive
parameter for comparison with other tabletting parameters.
Wf is obtained from the equation:

where F is the force applied to the tablet and z, the

deformation resulting from it, is represented by the relative
displacement of the anvil and plunger.
 STRENGTH OF TABLETS

The work Wf required to cause tablet failure correlates better

with other mechanical strength tests and is a more sensitive
parameter for comparison with other tabletting parameters.
Wf is obtained from the equation:

where F is the force applied to the tablet and z, the

deformation resulting from it, is represented by the relative
displacement of the anvil and plunger.
 Determination of brittle fracture index (BFI)
Crack theory can be used to develop a quantitative expression
for the measurement of the brittle fracture tendency;

Where, To and T are the tensile strengths of tablets with and

without a central hole, respectively.
• The BFI value thus has a range of 0 (no fracture tendency) to
1 (maximal fracture tendency).
Summary of compaction properties