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The Flowability of Powders

an empirical approach
Reg Freeman
Freeman Technology

Presented at:

International Conference on Powder and Bulk Solids Handling


13-15 June 2000, IMechE HQ, London

This paper is the copyright of the IMechE and may not be reproduced without
permission.

SYNOPSIS

Powder flowability is inherently complex due to the many physical and environmental
variables that determine how it responds to being moved. Investigating flowability requires a
high specification powder rheometer having exceptional sensitivity and repeatability of
measurement. The FT3 Powder Rheometer, designed and manufactured by Freeman
Technology, measures the forces required to cause deformation and flow and uses these
profiles to characterise flowability. The paper presents a number of application studies
supported by graphical results and video film of testing. These studies show how powders
may be classified regarding flowability in relation to flow rate, compaction and other factors.

1. INTRODUCTION

The subject of this paper is the flowability of powders a complex, challenging subject of
relevance to many industries, researchers, academics and others like myself who design
instrumentation.

Investigating and understanding powder flow is difficult and time consuming and not helped
by the absence of the supportive mathematics nor quick and easy to use instrumentation that
would allow a thorough and structured empirical enquiry. Shear testing of powders is a
complicated topic, and it requires both technical knowledge and (in most cases), hands on
skill to perform successfully. (1) Many traditional techniques have poor repeatability and do
not simulate a dynamic flow condition. In addition, flowability of powders is affected by
many physical, chemical and environmental variables. Some of the more obvious ones are
listed below.

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Powder or Particle variables External Factors influencing
Powder Behaviour
Particle size
Size distribution Flow rate
Shape Compaction condition
Surface texture Vibration
Cohesivity Temperature
Surface coating Humidity
Particle interaction Electro-static charge
Wear or attrition characteristic Aeration
Propensity to electro-static charge Transportation experience
Ability to recover from compaction Container surface effects

Flowability of a powder is not an inherent function of the physical powder but a consequence
of the combined effects of many variables including those above. There are no reliable
quantitative relationships between primary properties like particle size and distribution,
particle shape, etc. and secondary properties such as failure properties or bulk density (2).
Ideally the impact and the interaction of all these variables need to be understood if flow
performance is to be reliably predictable. In reality, the task is enormous and the pragmatic
solution is to identify the key variables and evaluate them as part of a practical research
programme. Some of the questions that commonly arise concerning powder flowability are:

How does the flowability of this powder compare with standard production powders?
Is segregation significant and how does it affect flowability?
How does the rate of powder flow affect flowability?
What is the optimum amount of additive eg lubricant?
How durable is this powder and does attrition affect flowability?
How does the packing condition of the powder affect flowability?
How does temperature and humidity affect flowability?
How do particle surface conditions such as texture, surface coating, and electro- static
charge etc affect flow parameters?
How does the material and surface condition of containing surfaces affect flowability?
Is flowability of this production sample the same as the formulated product?
What is the instantaneous flowability of the powder in this storage container?

Answering these questions would require a high specification powder rheometer capable of
allowing one variable to be evaluated whilst all others are maintained constant. The key
specification needs would be as follows:

1. Flowability indices derived from measurements of the forces causing deformation and
flow of the powder.
2. Exceptional repeatability from test to test and between different instruments.
3. Exceptional sensitivity to allow small rheological changes to be detected and
quantified. For example, the testing of say 10 samples over a given temperature range,
or a series of tests to evaluate the affect of different amount of additive.
4. Long-term stability and accuracy of measurement.
5. Range of flow modes varying from gentle aeration to aggressive compaction.
6. Quick and automated testing and analysis with little dependence on operator skill.

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2. THE FT3 POWDER RHEOMETER

Freeman Technology (3) completed a feasibility study in 1996 that led to new design concepts
and the patenting of an innovative displacement principle that became the basis of the FT3
Powder Rheometer. Aided by SMART and SPUR innovation awards from the UK
Department of Trade & Industry, the instrument was subsequently developed to meet a
detailed specification based upon the above requirements.

The FT3 operating principle is to force a twisted blade along a helical path through a column
of powder or other material contained in a circular vessel having a closed bottom. The forces
causing the deformation and flow of the powder are those imposed by the moving blade and
these are measured continuously and used as the basis of the flowability assessment.

The helical path along which the blade


moves is determined by the
combination of axial and rotational
speeds. Thus a downward helical path
may be a small or steep helix and it
may be left or right handed depending
on which direction the blade rotates.

A blade with a right handed twist,


when moved along a right-handed
helical path, would produce relatively
low compaction and low displacement
because of the slicing action. When the
helix and blade angles coincide, the
action would be a slicing action in the
way that a knife slices through a solid.

Movement along a left handed helical


path produces more compaction and
higher flows, because the angle of
approach to the blade face may be close
to perpendicular. A bulldozing type of
action is then established.
FT3 Powder Rheometer showing
50mm bore vessel in foreground.

This angle of approach may be pre-set simply by setting the polarity and magnitude of the
helix angle. Hence, a 5 negative upward helix would establish a gentle lifting action that
would allow the displaced powder to fall to rest behind the moving blade, the normal
conditioning mode to be described later, (Fig1c). Conversely a 10 negative downward helix
produces high compaction and high flow, commonly used for testing. Hence a wide range of
flow modes is available simply by defining the helical path angle. The rate of displacement
or flow rate is dependent only upon the blade tipspeed, and this is the other set parameter
needed to fully define blade movement.

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Fig1 Three of the many displacement modes available

Because the powder column has a free surface, but is contained in a vessel with a closed base,
displacement of the powder upwards is unhindered, whereas displacement downwards is only
possible if compaction and circular flow occurs, i.e. flow downward causing neighbouring
particles to flow upwards. For most displacement modes the flow is predominantly up and
over the blade. Each particle within the powder mass lies at a state of rest until forced to
move, coming to rest again as the blade moves on. The pattern of powder displacement is
virtually steady state, allowing flow to be observed and generally resulting in smooth, linear
or logarithmic profiles of the measured forces. These forces are those required to initiate
shearing and breakdown of interparticulate bonding of the powder in the zone immediately
around the blade, a process that is continuous.

Force and torque measurements are sampled continuously whilst the blade traverses
downwards and then upwards through the test material. Energy consumed is calculated from
this data so that an energy gradient profile for each traverse is available as shown in Fig2.
The shape and magnitude of these profiles are therefore representative of the combined forces
required to deform and displace the sample at the prevailing test conditions. Various
flowability indices may be calculated using this data such as the energy gradient intercept
value, Ce and the total energy consumed, E, as shown in Fig2.

Fig2 Typical energy gradient profile Fig3 Typical set of energy gradient
profiles (Talcum powder)

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The instrument can produce variable flow rates and stresses that may vary from gentle and
aerating to aggressive downward compaction. The helix angle determines the type of
displacement and the blade tip speed sets the rate of flow. Fig 3 shows a typical set of results
for a range of flow rates. This versatility allows the FT3 to test virtually any material through
which a blade may be passed and for a suitable test condition to be devised, whether testing
sub-micron cohesive powders, 5mm granules, dough or other semi-solids.

In addition to flowability testing, the FT3 is able to condition powders prior to test and also to
blend powders with powders or with liquids. All programmes may be saved and reused so
that testing or blending may be precisely reproduced.

3. APPLICATIONS

The FT3 rheometer is a versatile instrument that will test powders and semi-solids. It is
capable of:
Conditioning materials in preparation for test.
Testing and assessing flowability values in terms of energy and flowability indices.
Blending powders with liquids or other powders.
The first independent research (4), on seven types of microcrystalline cellulose, demonstrated
the high sensitivity of the instrument and provided correlation between the FT3 measurements
and actual capsule filling experience.

This paper includes four application studies that involve the conditioning and testing of
powders. They describe methods of investigating flowability in relation to packing condition,
flow rate, attrition and segregation.

Flowability is a term used widely to describe the flow properties of powders. The basis of the
FT3 flowability assessment is the energy required to cause a particular flow pattern and flow
rate. In a broader sense, flowability indicates the degree of difficulty that may be expected in
trying to transport powders under practical conditions of varying rates of flow, changing
levels of compaction and other factors. It is suggested that this difficulty is closely linked to
the variability of the energy required to maintain flow throughout any powder handling
process.

3.1 How the Packing Condition Affects Flowability


The flowability of powder is very dependent on its packed condition. Therefore a powder
cannot be assigned an intrinsic flowability value, in the way, for example, that its particle
size range may be described.

To demonstrate the variation of flowability at different levels of powder compaction, a series


of tests were done on a powder coating sample having a particle size in the range of 20 to 35
microns. In each case the test was a single downward traverse along a negative 10 helix at a
blade tipspeed of 100mm/s. The sample was initially sieved, poured into the test vessel and
tested without conditioning (Test1). The low energy figures and high volume reflect the loose
packing density and the presence of entrapped air. The as tested sample was then subjected
to 3 conditioning cycles to gently aerate and rearrange the particles to form a layered, very
consistent, bed of powder. The test was then repeated (Test2). Further preparation and testing

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was done using various methods of compacting the sample including the use of dead weights,
programmed compaction and repeated tapping. The following points of interest are apparent
from the results represented in Fig4.

The energy consumed in displacing the powder, varied from 30mJ, max air entrainment,
to 920mJ, the 100 taps case that caused maximum consolidation of the powder.
Conditioning was effective in removing the excess air from the initial sample and in
removing the high compaction imposed by tapping. Conditioning, prior to Test2 and
Test7, produced the same volume and the subsequent tests showed similar consumed
energy requirements of 125 and 103mJ.
Dead weight compaction used prior to Test3 and Test4 shows that incrementally
applying the weights almost doubled the consumed energy during the subsequent tests.
This probably indicates the significance of the vessel wall friction effects and no doubt
this would constitute a useful study in itself.

Fig4 Results of flowability testing on powder coating sample,


showing the affect of different packing methods.

The large difference of energy measurements shows clearly that any flowability assessment
would be of limited value unless the initial packing condition was known. Therefore as a
preliminary to testing, a method of pre-conditioning powders is needed that is reliable and
very repeatable. This should produce gentle aeration and rearrangement of all particles to
form a layered, consistent, bed of powder. The FT3 Powder Rheometer allows conditioning
cycles to be built into the start of each test programme. The programme may be saved and
used repeatedly so that conditioning is guaranteed and is precisely defined and controlled.

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If conditioned packing is regarded as the standard and is used prior to all standard
flowability testing, then the affect of compaction state on flowability could be expressed as:
energy consumed during test on compacted sample
Compaction Flowabilit y Index =
energy consumed during test on conditione d sample
For example, the powder coating sample in relation to the tapped compaction test would give:
Compaction Flowability Index = 920/125 = 7.36

3.2 Testing at Various Flow Rates


The FT3 Powder Rheometer displaces powder during testing by moving a twisted blade along
a helical path through the powder bulk. Each particle is initially at rest and is caused to flow
along with its neighbours when the blade approaches it. For a downward helical path, the
displacement is mostly up and over the blade, coming to rest behind it as the blade moves on.
The forces needed to promote this flow depend primarily upon three factors:

the resistance of the powder to flow


the angle at which the blade approaches the powder
the speed of the blade, (expressed as tipspeed, mm/s)

The flow rate of the powder is therefore proportional to blade tip speed and it is a simple task
to evaluate flowability at different flow rates. Fig 5 shows how the consumed energy for a
standard test condition, varies with flow rate for a range of materials.

Fig 5 Energy required to maintain flow as a function of


Flow Rate for a range of materials

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Fine cohesive powders usually have high sensitivity to flow rate and highlight the need to
avoid intermittent flow conditions during processing. The shape of the energy vs flow rate
curve is an important indicator of whether or not a powder will flow consistently. The syrup
data, included as a reference, shows the expected linear relationship for a Newtonian material.

Fig 6 shows the results of testing at blade tip speeds starting at 100mm/s, reducing to 10mm/s
and then increasing again in order that the hysteresis could be measured. Each test cycle was
preceded by a conditioning cycle to remove the compaction of the previous test cycle. These
two powders are opposites in that the powder paint becomes less free flowing at lower speeds.
Another difference is the large hysteresis in the case of the cooking salt that became freer
flowing as a result of the testing. The powder coating sample however was unaffected,
showing the same energy consumption at the start as at the finish.

Fig 6 Energy requirement as function of flow rate showing hysteresis

A Flow Rate Flowability index may be derived from the above set of data, as follows:

energy required for the test trav erse at 10mm/s


Flow Rate Flowabilit y Index =
energy required for standard test trav erse at 100mm/s

For powder coating sample- Flow Rate Flowability Index = 2023/1029 = 1.97
For cooking salt sample- Flow Rate Flowability Index = 1164/1608 = 0.72

An idealised powder would require the same energy to maintain flow whatever the flow rate,
i.e. the Flow Rate Flowability Index would be 1.

All powders could be assessed and classified in this way. This Compaction Flowability Index
and the Flow Rate Flowability Index, introduced above, are arguably the two most important
indicators of whether or not a powder will flow consistently when processed.

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3.3 Flowability changes due to Segregation and Wear
The results shown in Fig 6 show an improvement in the flowability of the salt as a result of
testing. Why was this? In what ways did the salt change between the first test and the last?
One explanation could be segregation promoted by the conditioning cycle that preceded each
test cycle. A second factor could be the physical changes to particles due to wear. Attrition
and segregation effects were investigated separately as described below.

3.4 Powder Attrition Study


Most particles will change physically due to wear caused by abrasion, compression and
shearing that occurs whenever powder flows. The consequences may be the generation of
smaller angular particles or more rounded ones and in most cases, a bi-product is a
considerable number of very fine wear particles. Surface coatings when present, may also be
degraded. The affect of these changes on the flow properties of the powder is usually
significant.

Fig 7 Effect of repeated attrition on the Flowability index of cooking salt

Fig 7 shows the results of stressing 270g of cooking salt repeatedly and measuring the effect
on flowability. 10 compacting cycles were applied to promote wear. The sample was then
sieved onto a tray to assist size redistribution and then retested. This was repeated 7 times.
The results show a steady reduction throughout the test series, in the energy required to
maintain the flow condition. The most likely explanation is that the particles became more
rounded and as a result freer flowing. This trend correlates with the decrease in the energy
imparted during the compacting cycles between each test as shown in Fig 7.
An Attrition Flowability Index could be derived from the test data as follows:

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energy required for standard test trav erse after 200J of work done on powder
Attrition FI =
energy required for standard test trav erse using new powder

For cooking salt, Attrition Flowability Index = 1182/1722 = 0.69

Tests similar to those described above will indicate whether flowability is improved or not
and provide more understanding of the robustness and durability of a powder.

3.5 Segregation Study


The flowability of a powder containing a wide range of particle size is likely to change if
segregation occurs. Agitation of the powder may result in migration of the smaller particles
downward and the larger ones upward. Mixtures of different powders may also become
segregated.

Fig 8 Effect of segregation on the Flowability index of granulated sugar

Fig 8 shows the results of tests on a 160g granulated sugar sample, designed to investigate
segregation. The sample had been repeatedly compacted earlier to promote attrition, a process
that consumed 183 joules. It was then sieved onto a tray in an attempt to uniformly distribute
the particles by size before pouring into the test vessel.

Each segregation test was preceded by 3 aeration cycles that gently rearranged the particles
and promoted segregation without imposing significant stresses. Each test phase was followed
by the next without removing the sample from the vessel so that the segregation effect was
cumulative. The results show a steady increase of the energy requirement, eventually
levelling off when segregation stabilised. The final test followed sieving and reconditioning
and shows that the energy requirement was then reduced to less that the starting figure.

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For this granulated sugar sample, the energy requirement levelled off after a total of 30
aeration cycles had been applied. If 30 aeration cycles is taken as the standard then we may
calculate:

energy required after 30 aeration cycles


Segregatio n Flowabilit y Index = = 1518 / 1309 = 1.16
energy required during initial test trav erse

Segregation may significantly affect flowability. This test method provides a quick and
sensitive way of quantifying and classifying this.

3.6 Other Applications


Some possible applications have been reviewed above. Others might include:

Formulation development repeated testing to assess key components e.g. glidants.


Temperature dependence flowability of samples at different temperatures.
Humidity dependence humidity cabinet soak prior to sealing, removal and test.
Electro-static studies flowability testing of differently charged powder samples.
Powder blending programmed blending of powders and flowability assessments.
Granulation studies granulation with programmed binder addition.
Fluid bed studies testing with fluid bed at vessel base.
Shear strength measurements.
Wall affect studies.

4. CONCLUSIONS

Measurement of powder flowability is inherently difficult because of the many factors such as
humidity, vibration and flow rate that may affect the flow properties. The FT3 Powder
Rheometer offers a unique, dynamic displacement principle that is exceptionally sensitive,
easy and quick to use and operator independent. The instrument provides a new approach to
assessing flowability that enables this complex subject to be investigated in a systematic way
as exemplified in the four application studies.

The basis of all FT3 flowability assessments used in the studies is the energy required to
maintain a certain pattern of flow and flow rate. The focus is on the change of this energy
requirement because it is suggested that high energy gradients in any transportation system
will probably result in inconsistent flow.

The first application study, section 3.1, showed that flowability measurements that did not
take account of the powder packing condition would be of little value. The FT3 rheometer
overcomes this complication by creating a standardised packing state the process of
conditioning the powder. This makes it possible to evaluate flowability in terms of the key
variables, because each test starts from a standardised packing condition that can easily be
reproduced. Classification of powder flowability then becomes practicable.

Whilst a single number classification would be ideal, the reality is that each powder needs to
be classified for flowability in relation to each of its key variables. Flowability indices have

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been derived for packing condition, flow rate and other variables, based upon the use of a
standardised set of testing conditions.

In the case of the powder coating tests, a Compaction Flowability Index of 7.36 showed that
compared with a conditioned state, a consolidated packing state induced by tapping,
required a sevenfold increase in energy needed to maintain flow. The Flow Rate Flowability
Index for this powder was 1.97, indicating that almost twice as much energy is needed to
maintain flow at low rates of flow.

Such variability of energy requirement is likely to cause inconsistent flow performance at the
very least. If in addition, there are other significant factors such as attrition, electrostatics or
humidity to compound the problem, then processing and the control of quality become
increasingly difficult, if not impossible.

Powder classification in terms of the key variables affecting flowability, would improve the
understanding and prediction of powder flowability performance. Classifying existing
powders and correlating this information with processing experience could provide benefits at
all stages of future powder development, production and quality control. An example is the
inclusion of flowability criteria in powder specifications and the ability to measure this in a
matter of minutes.

REFERENCES

(1) T.A.Bell, Industrial Needs in Solids Flow for the 21st Century powder handling &
processing, Vol.11 (1999) No1, pp 10.

(2) L.Svarovsky, Principles of Powder Technology, edited by M.J.Rhodes, (1990), Ch3,


pp35.

(3) Freeman Technology, Boulters Farm Centre, Castlemorton Common, Welland, Malvern,
Worcs, WR13 6LE, UK
Tel 01684 310860, Fax 01684 310236
Email info@freemantech.co.uk Website www.freemantech.co.uk

(4) F. Podczeck, Rheological Studies of the Physical Properties of Powders Used in Capsule
Filling, by, The School of Pharmacy, University of London. Published with the kind
permission of Pharmaceutical Technology Europe.

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