Physics of tablet compression

Properties of powders
Physicotechnical properties of pharmaceutical solids dictate
the performance and processing of solid dosage forms,
including their compressibility.
These properties are inter-related and a change in one
property is likely to affect the other.
1.Surface Properties
2.Porosity
3.Flow property
Surface Property: Surface properties of a powder
material have a major influence on their flow and
intermolecular attraction.
Atoms or ions located at a surface have a different
distribution of intermolecular and intramolecular
bonding forces than those present within a particle.
This is caused by the unsatisfied attractive
molecular forces that extend out to some small
distance beyond the solid surface.
This gives rise to free surface energy of solids, which
plays a major role in interparticulate interaction.
Particulate attractive forces include those between like
particles called cohesion, and those between un-like
particles called adhesion.
 The attractive forces resist the differential movement of
constituent particles when subjected to an external force.
Other types of resistance to relative movement of particles
include:
the electrostatic forces,
adsorbed moisture, and
residual solvent on the surface of solid particles.
Porosity: The porosity of powder (E) is defined as the ratio
of total void volume (Vv ) to the bulk volume (Vb) of the
material.
total void volume, Vv = Vb - Vt
where, Vt is the true volume.
E = Vb - Vt / Vb = 1 - Vt / Vb
One of the methods used to determine the compressibility
of a powder bed is the degree of volume reduction owing to
applied pressure, which is related to porosity and is
assumed to be a first-order reaction.
Flow Properties:
Good flow property of a pharmaceutical powder is essential to ensure
proper die fill during compression, especially in direct compaction
process.
Reasons such as, high percentage of fines, excess moisture, lubricants,
and electrostatic charge may contribute to poor flow of powders.
The increase in bulk density of a powder is related to its cohesivity.
Indices such as the Hausner Ratio (H) and Carr’s Index (CI) are based
on tapped and bulk densities.
Hausner ratio is the ratio of tapped density to bulk density and varies
from about 1.2 for a free-flowing powder to 1.6 for cohesive powders.
Carr’s Compressibility Index: Tapped density – bulk density
X 100
Tapped density
Values of Carr’s index of about 5–12% indicate free-flowing powder,
23–35% indicate poor flow,
>40% an extremely poor flow
Flow rate :It is used to determine the resistance to movement of
particles especially for granular powder with poor cohesiveness.

An indication of the ease with which a material can be induced to flow

is given by compressibility index, I.
 I = [1 - Vt / V0] × 100
Vt is the tap volume and V0 is the volume before tapping.
Value of I below 15% indicate good flow properties but values above
25% mean poor flow.
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In pharmaceutical tabletting an appropriate volume of granules in a die
cavity is compressed b/w an upper & lower punch to consolidate the
material into a single solid matrix, which is subsequently ejected from
the die cavity as an intact tablet.
The subsequent events that occur in the process are:
1.Packing Rearrangement and volume reduction
2.Deformation at the point of contact.
3.Fragmentation .
4.Bonding.
5.Deformation of the solid body.
6.Decompression.
7.Ejection.
Compaction: It can be defined as the compression and
consolidation of a particulate solid–gas system as a result of
an applied force.
Compression: It involves a reduction in bulk volume as a
result of reduced gaseous phase.
A closer packing of the powder particles as a result of
rearrangement is the main mechanism for initial volume
reduction.
As the force is further increased, rearrangement becomes
difficult and particle deformation sets in.
Consolidation, which is a subsequent process, involves
increase in the mechanical strength resulting from particle–
particle interactions.
As the particles move into closer proximity to each other
during the volume reduction process, bonds are established
between the particles.
The nature of bonds formed is similar to those of the
molecular structure of the interior of the particles, but
because of the roughness of the particles surface, the actual
surface area involved is small.
Consolidation is the major reason for increase in
mechanical strength of a powder bed, when subjected to
rising compressive forces.
The various steps involved in powder compaction
The compaction process mainly includes:
 particle rearrangement,
deformation under pressure,
 smaller particles formed as a result of fracture of larger
particles may undergo further rearrangement
Compressibility is the ability of a material to undergo a
reduction in volume as a result of an applied pressure and is
represented by a plot of tablet porosity against compaction
pressure.
Compactibility is the ability of a material to produce tablets
with sufficient strength under the effect of densification and
is represented by a plot of tablet tensile strength against
tablet porosity.
Tabletability is the capacity of a powdered material to be
transformed into a tablet of specified strength under the
effect of compaction pressure and is represented by a plot
of tablet tensile strength against compaction pressure.
1. Particle Rearrangement and Volume Reduction

The first thing that happens when a powder is compressed is that the particles
are rearranged under low compaction pressures to form a closer packing
structure.

The finer particles enter the voids between the larger ones and give a closer
packing arrangement.

In this process, the energy is evolved as a result of interparticulate friction and

there is an increase in the amount of particle surface area capable of forming
interparticulate bonds.

As the pressure increases, further rearrangement is prevented and subsequent

volume reduction is accomplished by plastic and elastic deformation and/or
fragmentation of the particles
The number of contact points known as potential bonding areas
(inter- and intraparticulate) of the particles, are dependent on:
particle size
size distribution
density
surface properties
interparticulate voids
 process variables: moisture content, rate of flow, and the
relationship between die-cavity diameter and particle diameter.
Brittle particles are likely to undergo fragmentation, i.e., breakage of
the original particles into smaller units resulting in increase in contact
points.
Plastic substances deform in an irreversible manner, resulting in a
permanent change of the particle shape (irreversible process),
Elastic substances when deformed resume their original shape.
(reversible process).
The degree of volume reduction that a pharmaceutical powder bed
undergoes depends on the mechanical properties of the powder and the
type of volume reduction mechanisms involved.
Particle size and speed of compression influences the mechanical
properties of the material.
Reduction in particle size has been related to a decreased tendency to
fragment.
Some materials appear to have a critical particle size at which a transition
from brittle to ductile behavior occurs as the particles become smaller.
Brittle materials that undergo extensive fragmentation generally result in
tablets of relatively high porosity because of the large number of bonding
points that are created, which prevent further volume reduction.
A ductile material often results in tablets of low porosity because the
high degree of plastic deformation enables the particles to move very
close to each other.
Similarly, different crystal habits such as spherical, cubical, and acicular,
have different tendencies to pack in a close structure.
Particles having regular shape appear to undergo rearrangement more
easily as compared to irregular particles.
Deformation of Particles:
As the upper punch penetrates the die containing the powder bed, initially
there are essentially only points of contact between the particles.
Application of the external forces to the bed results in force being
transmitted in through these interparticulate points of contact, leading to
development of stress and local deformation of the particles.
Energy is lost at this stage as a result of interparticulate and the die-wall
friction, as well as deformation.
Particles, either whole or a part, can change their shape temporarily by
elastic deformation and permanently by plastic deformation Particles can
also fracture into a number of smaller, discrete particles, i.e. particle
fragmentation
 Based on their mechanical
properties, powders are classified
as plastic, elastic, and viscoelastic.
However, under the influence of
an applied pressure, the particles
not only deform plastically or
elastically, but also fragment to
form smaller particles.
The type of deformation depends not only on the physical properties
of the material but also on the rate and magnitude of the applied
force and the duration of locally induced stress.
As a result of the resistance of a material against deformation (strain),
the stress inside the particles increases.
If the applied stress is released before the deformation reaches a
specific critical value, the particles deform elastically, i.e., the
deformation is reversible and the particles inside the powder bed
regain their original shapes.
The force required to initiate plastic deformation is known as yield
stress.
Elastic deformation is a reversible process, whereas plastic
deformation results in a permanent change in the particle shape.
Elastic and plastic deformation of particles are a time-independent
processes, i.e. the degree of deformation is related to the applied
stress and not the time of loading.
Both plastic and elastic deformation may occur although
one type predominates for a given material.
Deformation increases the area of true contact and formation
of potential bonding areas.
 Fragmentation
As the compressional load increases, the deformed particle starts
undergoing fragmentation.
Because of the high load, the particle breaks into smaller fragments
leading to the formation of new bonding areas.
The fragments undergo densification with infiltration of small
fragments into voids.
In some materials where the shear stress is greater than the tensile
strength, the particles undergo structural break down. This is called
brittle fracture.
Example: sucrose – shear strength is greater than the tensile strength.
With some materials fragmentation does not occur because the stresses
are relieved by plastic deformation.
Irrespective of behavior of large particles, small particles may deform
plastically, a process known as microsquashing, and the proportion of
fine powder in a sample may therefore be significant.
because this product requires gradual application 13 Electronic Data
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force to minimize elastic recovery and allow stress relaxation. Similar
sizes for main and precompression rollers to apply similar forces are
reported to result in optimal tablet formation.
The majority of powders handled in pharmaceutical production consist not
of non-porous primary particles but rather of granules; porous secondary
particles formed from small dense primary particles.
For granules, a larger number of processes are involved in their
compression. These can be classified into two groups:
These can be classified into two groups:
Physical changes in the granules, i.e. the secondary particles;
 Physical changes in the primary particles from which the granules are
formed.
Granules can be broken down into smaller units by
different mechanisms:
1. Primary particles might be removed from the surface of
granules when they slide against each other or against the
die wall. This can be described as erosion or attrition, rather
than fracturing. This mechanism occurs primarily for
granules with a rough surface texture.
2. Granules can fracture into a number of smaller ones i.e.
granule fragmentation
 Time Dependency of Compaction Process

Some deformation processes (plastic deformation) are time

dependent and occur at various rates during the compaction
sequence.
This means that the rate at which load is applied and removed
may be a critical factor.
More specifically, if a plastically deforming solid is loaded (or
unloaded) too rapidly for this purpose to take place, the solid may
exhibit brittle fracture.
This is a contributing factor to structural failure of tableting as the
machine speed is raised.
Conversely, if the dwell time under the compression load is
prolonged, then plastic deformation may continue, leading to
more consolidation
Hence, the compact formation is determined by the time
dependant viscoelastic behavior.
 Speed of the process (dwell time) can have marked effect on
compactibility and on tendencies such as lamination, capping,
and picking, which can occur during and/or after ejection.
 Extended dwell time involves application of compression
force for a longer period of time. This further allows plastic
flow.
Coupling of these processes results in viscoelastic behavior
being observed during the compression of the tablets at normal
production speed and often at slower speeds.
 Models for mechanical strength of tablets
Bonding Mechanisms:

 The mechanical strength of a tablet depends on the dominating

bonding mechanism between the particles and the surface area
over which these bonds act.
 When the surfaces of two particles approach each other closely
enough, their surface energies result in a strong attractive force,
a process called cold welding.
 This hypothesis is favored as a major reason for the increasing
mechanical strength of a powder bed when subjected to
compression force.
On the macro scale, most particles have an irregular shape, so
that there are many points of contact in the bed of powder.
As the force is applied to the powder bed, this transmission may
result in generation of considerable frictional heat.
If this heat is not lost, the local rise in temperature could be
sufficient to cause melting of contact area of the particles, which
would relieve the stress in that particular region.
In that case, the melt solidifies giving rise to fusion bonding.
“Rumpf bond summation concept” is based on the following types
of bonding mechanism, where the agglomerate strength is considered
to dependent on the interparticulate bond structure.

a)Solid bridges (as a result of melting, crystallization, sintering,

chemical reaction, and binder hardening)
b) Bonding as a result of movable liquids (capillary and surface
tension forces)
c) Non freely movable binder bridges (viscous binder and adsorption
layers)
d) Attraction between solid particles (molecular and electrostatic
forces)
e) Mechanical interlocking (irregular particle size and size
distribution)
Dominating bond types for dry powders are solid bridges,
mechanical interlocking and intermolecular forces.
Intermolecular forces include Van der Wall’s forces, hydrogen
bonding, and electrostatic forces.
 These bonds are of a special importance for directly
compressible binders such as microcrystalline cellulose (MCC),
polyvinyl pyrrolidone (PVP), and lactose.
Bonding Surface Area
Bonding surface area is often used to define the effective
surface area taking part in the intermolecular attraction
area, whereas for intermolecular forces the term is difficult
to define.
Considering the importance of the bonding surface area for
the mechanical strength, it is desirable to measure the
actual surface area participating in bonding.
Hiestand described that the mixing of elastic drug with
plastic deforming material (e.g., MCC), resulted in a harder
compact as a result of plastic deformation increasing the
bonding surface area.
Particle size, shape, fragmentation, deformation, and bond
formation determine the bonding surface area in tablets
COMPRESSION CYCLE AND EFFECT OF APPLIED
FORCES
Compression is important for molding a drug-
excipient blend into tablets.
The compression cycle on a rotary tablet press
includes precompression, main compression,
decompression, and ejection phases.
I
Precompression: Precompression is the stage where the
tablets are partially formed and the precompression roller is
usually smaller than the compression roller,
Optimal compression efficiency is achieved on a machine
that offers multistage compression with high
precompression and a desirable main compression force.
Precompression plays a major role especially at high
compression speeds.
For products that undergo brittle fracture, the application of
precompression at a higher force than main compression
results in higher tablet hardness.
.
Main Compression:
 Main compression is the phase in which
compression and consolidation of powder bed
occurs at high force.
During main compression, the applied energy is
transformed into formation of interparticulate
bonds.
When a force is applied in a die, the particles first
undergo rearrangement to form a less porous
structure at very low forces.
Subsequently, the particles reach a state where
further relative movement is impossible, and an
increase in the applied force induces either particle
fragmentation or deformation (or both).
 Decompression
As the applied force is removed, a new set of stresses
within the tablet gets generated as a result of elastic
recovery.
The tablet must be mechanically strong enough to
accommodate these stress, otherwise the structure failures
occur.
The degree and rate of relaxation within the tablet is the
characteristic of a particular blend. Recording of this phase
provides insights into tableting problems. For example, if
the degree and rate of elastic recovery are high, the tablet
may cap or laminate.
 If the tablet undergoes brittle fracture during
decompression, the compact may form failure planes as a
result of fracturing of surfaces.
Tablets that do not cap or laminate are able to relieve the
stresses by plastic deformation.
The tablet failure is affected by rate of decompression
(machine speed).
 Addition of a plastically deforming agent (e.g., PVP,
MCC) is advisable to reduce the risk of such structure
failures.
Ejection
Ejection phase also requires force to break the adhesion between die wall
and compact surface and other forces needed to complete ejection of
tablet.
Radial die wall forces and die wall friction also affect the ease with
which the compressed tablet can be removed from the die.
The force necessary to eject a tablet involves the distinctive peak force
required to initiate ejection, by breaking of die wall–tablet adhesion
The second stage involves the force required to push the tablet up the die
wall, and the last force is required for ejection.
Variation in this process are sometimes found when lubrication is
inadequate and a slip-stick condition occurs between the tablets and die
wall, with continuing formation and breakage of tablet die–wall
adhesion.
Heat is generated during ejection as a result of friction from shear
between the compact and the die wall, and absorption of this heat can aid
in bond formation.
Lubrication usually assists in reducing the ejection
forces, The unequal stress exerted on the compact
during ejection can cause capping or laminating.
 Lubricants minimize stress patterns so, they reduce
the tendency for materials to cap or laminate.
The particle size of the powdered material also has an
effect on ejection forces and shear.
As particle size decreases, more of its surface may be
in contact with the die wall.This adds to increased
friction forces and the generation of heat. If more
particle surface is available for contact with the die
wall, larger forces may be required to remove the
compact.
 Effect of friction
•Interparticulate friction: :Arises at particle- particle contact
• :More significant at low applied loads
• :Glidants used to reduce this

Die-wall Friction: Results from materials being pushed against the die wall
and moved down it
 : More dominant at high applied forces when particle
rearrangement stops
 : lubricants added to reduce this friction
 Distribution of
forces
When force is being applied to top
of a cylindric powder mass, the
following basic relationship applies,
since there must be an axial
(vertical) balance of forces.
the system is represented
diagrammatically.
FA= FL + FD
Where, FA = force applied to upper
punch
FL = proportion of FA force
transmitted to lower punch
Cross section of simple die FD =reaction at the die wall due to
and punch assembly friction at the surface
Inherent difference b/w the force applied at the upper
punch & that affecting material close to the lower punch, a
mean compression force applied is given by:

 FM= FL + FD
2

FM gives practically friction independent measure of compaction load

which is more relevant than FA .
In single station press applied force transmission decays exponentially
(i.e. FL= FA .e – KH/D)
To over come this, appropriate geometric force FG might be used,
FG= (FA x FL)0.5
Ejection force: Radial die wall forces and die wall friction
affect the ejection of tablet.
Force required to eject a tablet follows 3 stages:
1. A peak required to ejection by breaking of tablet and die
wall adhesions.
2. A smaller force required to push the tablet up the die wall.
3.Declining force of ejection as the tablet emerges from the
die.
 DIE WALL LUBRICATION
Die wall lubricants function by interposing a film of low
shear strength at interface between tableting mass and
die wall.
Best lubricants
are those with
low shear
strength but
strong cohesive
tendencies in
direction at right
angles to plane of
shear
Force volume relationship
In many tablets processes , when appreciable force has been
applied, the relationship btw applied pressure (p) & volume
parameters such as porosity E becomes linear over the range
of commonly used pressure. –

It can be expressed by shapiro equation

Log E =Log E0 -K.P.
E0=porosity when pressure is zero
K=constant
P= pressure –
Walker expressed similarly 1/1-E=K1 -K2 .Log P
i initial repacking of
particles
ii. Elastic deformation
until elastic limit is
reached.
iii. Plastic deformation
or brittle fracture
dominates.
iv. Compression of solid
crystal lattice formation.
 Compaction Profiles

Compaction data obtained from instrumented tableting machine
are basically of two types—force-time and force-displacement
profiles
Force-Time Profile

Compression force-time profiles are used to characterize
compression behavior of active ingredients, excipients, and
formulations with respect to their plastic and elastic deformation
On a rotary tablet press, the force-time curves are segmented into
three phases—
A.Compression phase
B. Dwell phase
C. Decompression phase
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 which maximum displacement occurs
Contact time is the time for compression and decompression

(a) compression
(b) dwell
(c) decompression-both punches moving away from upper and lower surfaces, initial
relaxation of the tablet.
Force-Displacement Profile
Stress relaxation is observed to be minimal in case of
plastic deformation
Materials that undergoes elastic deformation tend to relax
to a greater extent during and/or after decompression.
However, it has been observed that most of the materials
undergo both plastic and elastic deformation at different
stages of compression, hence the work required for
compression is the sum of work necessary to rearrange the
particles, deform, and finally to fragment them
In a typical instrumented tablet machine, net work of compaction
(NWC) is calculated by subtracting the work of elastic relaxation
(WER) from the gross work of compaction (GWC).
So NWC includes work against frictional forces and work required for
deformation and/or fragmentation.
NWC = GWC – WER
GWC = Wf + Wp + We + Wfr
where, Wf is work against friction, Wp is work of plastic
deformation, We is work of elastic deformation, Wfr is work of
fragmentation, with We ≈ WER.
At a given fmax, the displacement area of plastic deformation is more when
compared to the displacement area of elastic deformation
Compaction Equations
A compaction equation relates some measure of the state of
consolidation of a powder, such as porosity, volume (or relative
volume), density, or void ratio, as a function of the compaction
pressure.
1. Kawakita Equation
2. Heckel Equation
3. Walker Equation
 Heckel’s plot
The Heckel equation is based on the assumption that
densification of the bulk powder under force follows first-order
kinetics.
The Heckel equation is expressed as
ln [1/1–D] = KP + A
where, D is the relative density of the tablet (the ratio of tablet
density to true density of powder) at applied pressure P, and K is
the slope of straight line portion of 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. *
Although Heckel plots are mostly used to characterize single materials,
they can also be used for powder mixtures.
Hersey & Rees and York & Pilpel classified
powders into three types A, B and C.
The classification is based on Heckel plots and the
compaction behavior of the material.

With type A materials, a linear relationship is

observed, with the plots remaining parallel as the
applied pressure is increased indicating
deformation apparently only by plastic
deformation.
An example of materials that exhibit type A
behavior is sodium chloride.
Type A materials are usually comparatively soft
and readily undergo plastic deformation retaining
different degrees of porosity depending on the
initial packing of the powder in the die.
This is in turn influenced by the size distribution,
shape etc. of the original particles.
For type B materials, there is an initial curved region followed
by a straight line.

This indicates that the particles are fragmenting at the early

stages of the compression process i.e., brittle fracture precedes
plastic flow.
Type B Heckel plots usually occur with harder materials with
higher yield pressures which usually undergo compression by
fragmentation first, to provide a denser packing.
Lactose is a typical example of such materials.
For type C materials, there is
an initial steep linear region
which become superimposed
and flattens
out as the applied pressure is
increased.

York and Pilpel ascribed this

behavior to the absence of a
rearrangement stage and
densification is due to plastic
deformation
 Factors affecting compaction
1.Moisture content: Moisture affects the flow, mixing rheology,
compaction, true density, and mechanical properties of granules as well
as tablets.
Water plays a key role in all manufacturing steps, therefore, water–
powder interaction is a major factor in the formulation, processing, and
performance of solid dosage forms.
 The amount of water associated with a solid at a particular RH and
temperature depends on its chemical affinity, surface area, and
available sites of interaction
Moisture plays an important role in interparticulate bond formation by
enhancing the tensile strength of the powder bed and decreasing the
density variation within the tablet.
MCC is an important excipient upon which, the role of
moisture has been extensively investigated.
Tablets containing MCC became harder as the moisture
content increased, whereas a lack of moisture was
responsible for tablet lamination because of increased yield
force and elastic recovery.
2.Compression Force Profile
Altering the method of force application is beneficial for
tablet production in order to increase tablet strength and
prevent the incidence of capping and lamination.
3.Solid-State Properties:
Drugs and excipients used in tablet manufacture exist in a
variety of solid state forms. These forms often show
difference in their physico-technical behavior, therefore, it is
important to know their influence on compaction.
A. Hydration/Solvate State: The need for optimal moisture
content in the formation of strong tablets is indicated by
crystal hydrates that compress well, but fail to form strong
tablets when water of crystallization is removed .
B. Crystal Habit: Isomorphic forms of drugs differ only in their crystal
habit. Tableting behavior flowability, and the tendency to stick to the
punches can be affected by the crystal habit of the drug(s). Crystal
engineering and particle design can be effectively used to improve
compactibility.
C.Polymorphism: In a study on compression behavior of pure
orthorhombic or monoclinic paracetamol, ortho-rhombic crystals
exhibited better technical properties due to presence of sliding planes
for crystal plasticity, greater fragmentation at low pressure, increased
plastic deformation at higher pressure, and lower elastic recovery, thus
avoiding capping even at high compression pressures
Particle Size and Particle Size Distribution: The particle size and particle
size distribution can affect both the particle rearrangement and
compaction phases.
Correlations between average particle size and tablet tensile strength
are important to select and design appropriately sized particles.
It was concluded that the distribution in size of free flowing particles is
not critical for the tablet porosity, but may give significant effects on
tablet tensile strength as a result of post-compaction hardening.
4.Salt Form:These are rarely affecting the compaction profile.

5. Granulation Method and Binder: The compactabilities of granules

varied with the granulation method used In the wet granulation
methods.
The tensile strength was in the order of wet massing granulation > wet
fluidized bed granulation > wet tumbling fluidized bed granulation >
wet highspeed mixer granulation; and melt high-speed mixer
granulation > melt fluidized bed granulation > melt tumbling fluidized
bed granulation in melt granulation.