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1. Background ...................................................................................................................... 3
Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 2
1. Background
Powders are at the core of numerous applications in the pharmaceutical, additive manufacturing,
chemicals and other process manufacturing industries. The Discrete Element Method (DEM)
has proven to be a great predictive tool for simulating processes in these powder handling
industries. One important aspect in powder simulations is the formation of suitable virtual
materials that reflect a realistic performance. This can be achieved by calibrating the input
parameters and it is an important step towards accurate DEM simulations. However, it is also a
genuine barrier for DEM applications.
At EDEM we are keen to support our customers and bring together the experience and know-
how on powder calibration techniques for various powder applications. This document aims to
discuss the latest challenges and advances in powders as well as providing guidelines for
calibration. Future user meetings and research advances will be used as source of information
to update this document.
Due to the complex nature of powders several topics are considered crucial when calibrating.
Some of the common topics asked include:
The following sections will discuss some of these areas in more detail.
Specifically, the first step towards a meaningful calibration process is to identify the critical
mechanisms that occur in the real applications and then design simple experimental tests that
will be able to capture these mechanisms. To achieve this, the flow conditions and stress state
Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 3
of the powder should be comparable between the smaller-scale measurement test and the real
process.
The basic criteria that need to be considered for designing suitable calibration tests follow what
we will refer to as the SANFE rule and include the following:
3. Calibration procedure
The calibration procedure is designed to work with several DEM models and response values
simultaneously and needs to follow a certain logic:
1. Simple experimental test needs to be performed replicating the conditions of the real
applications (e.g material is being transported with 10m/sec velocity. Suitable calibration
test could be the static angle of repose test where the material is generated with 10m/sec
velocity – Appendix I).
2. Starter DEM material parameters for calibration are either measured or taken from
literature. Very often, only ranges of parameters are available, due to the discrepancies in
the measurement data. Inputs such as Shear Modulus and particle size are typically set
prior to any calibration runs and are set based on predicted simulation run times.
3. Model particle shape and size. In principle, non-spherical shapes provide improved realism
of material flow due to particle interlocking and geometric constraint to particle rotation.
However, a balance needs to be achieved between the real shape and a virtual
representation allowing for feasible computational performance and accurate results. For
powders the analysis focusses around bulk behavior rather than individual particle behavior.
4. Select appropriate particle size distribution (systems in DEM often need to be scaled to
achieve feasible run times). The density of the virtual assembly needs to be calibrated
against the bulk density of the real powder. A simple experimental test can include the filling
of a tube (see section 7.1).
5. Next, the particle-to-particle contact parameters need to be calibrated by running a number
of small-scale DEM simulations. The chosen parameter sets are used to gain insight into
which combination of parameters influences the material behavior the most (see Appendix
II). The combination of parameters that provides results closer to the real ones are the
chosen ones.
Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 4
6. Once the particle-to-particle parameters have been selected (step 5) the bulk density (step
4) needs to be measured again to make sure that it has not been affected. In case of
different bulk density measurement then step 6 needs to be repeated.
7. Next, the particle-to-equipment contact parameters need to be calibrated by performing
small scale DEM simulations and comparing the results against experimental data.
8. Once the relationship between calibration parameters and response values has been
established, the values of the calibration parameters are adjusted until the responses match
the experimental values within an acceptable tolerance.
9. Incorporating data derived from additional independent experiments will increase the
validity of the calibrated DEM parameter set.
Currently, the calibration procedure includes the measurement phase (parameters, test and
repeatability) and the modelling phase (physics model, link to the measured data, scale). It has
been observed that there is a consistent deviation of the experimental measurements using
industrial equipment and the DEM simulation results, and this is another challenge that DEM
users are currently facing. The need for better accuracy and minimization of the number of DEM
calibration parameters requires a framework to be established. This framework will enable the
scalability of parameters from a single scale to input values up to relevant particle scale without
compromising the results. At the same time, simplification of the industrial design needs to be
considered allowing for replication of real industrial applications by DEM in a user-friendly
manner while capturing the critical DEM parameters.
Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 5
Furthermore, particle’s size has a direct impact on the behavior of the powder especially in
applications where the powder is under consolidation (storage in Hoppers/silos/bins). A strong
example is the various mixing applications in which the powder’s initial state is already under
consolidation since it has been previously stored inside a container. This means that the yield
strength of the material when stored is increased which is likely to affect its flowability in the
mixing application. In these cases, caking is often observed as an unwanted by-product. Caking
is a phenomenon that results when the magnitude of the inter-particle forces increases over
time. Due to their size, powders are subjective to adhesive forces and those primarily are van
der Waals forces, polar interactions, and those associated with liquid bridges (when moisture is
present). So, in storage structures, such as hoppers, the consolidation stress can result in
increase of the adhesion forces and significant caking can be developed. As these forces are
proportional to particle size, the likelihood of caking generally decreases with increasing particle
size. The best way to address this problem is by choosing appropriate calibration tests which
will be able to simulate the consolidation pressures that are expected when a powder is stored.
Results then can be confidently applied as the DEM simulated tests will replicate the conditions
in larger-scale storage vessels. The most suitable calibration tests are considered the Uniaxial
Unconfined Test and Shear cell testing, such as the Jenike Shear Tester (described by ASTM
D-6128) and the Schulze Ring Shear Tester (described by ASTM D-6773). Through these tests
the flowability of the material is assessed as the Flow Function and the Time Flow Function are
calculated (see Chapter 6.7 and 6.8). The criteria for choosing the best test will be the expected
stress state of the real application. For example, if the mixing is generally a low stress application
then the Shear testers are going to be a better option compared with the Uniaxial test, as the
latter is considered inadequate at very low stresses (<10 kPa).
Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 6
results as the bulk friction of the material is no longer achieved. This is because on the particle
level not all particles can be in contact and not every contact can achieve the maximum values
of friction, hence there will always be a deviation between the bulk friction and the particle
friction.
Furthermore, it is important to note that the chosen timestep can directly affect the results.
Cohesive and in general complex systems require smaller timesteps to provide numerical
stability and capture the higher stiffness and loading/unloading paths. Therefore, it is common
practice to use 15-20% of the critical timestep, where the critical timestep would be the minimum
of the Rayleigh timestep and the timestep related to the maximum spring stiffness and the
maximum bond stiffness. Since the timestep varies with different particle materials, for an
assembly consisting of different material type particles, the critical timestep should be the
smallest among those determined for different material properties. More information can be
found in Otsubo et.al. (2017). As a rule of thumb a suitable range of timesteps for numerical
stability is found to be around 5 -20% of the Rayleigh timestep.
Specifically, when using the EEPA contact model is suggested to use the following equation
𝑡𝑡 = 0.17�𝑚𝑚�𝑘𝑘 (1)
2
Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 7
2𝐸𝐸 ∗ 𝑅𝑅 ∗ if n=1 (2)
𝑘𝑘1 = �
4/3√𝐸𝐸 ∗ 𝑅𝑅 ∗ if n > 1
where 𝜆𝜆𝑝𝑝 is the contact plasticity ratio. For detailed information please refer to Morrissey (2013).
Regarding the DEM-CFD coupled simulations the correct calculation of the drag force and heat
flux is critical when using scaled-up particles. The latest version of the EDEM-Fluent coupling
uses the parcel approach (scale factor approach), where the drag force and heat flux are initially
calculated on a single particle that has a diameter multiplied by the reciprocal of the scale factor
(i.e. a scale factor of 10 results in forces and fluxes calculated based on a particle diameter 10%
of the original value). The forces and fluxes of this scaled particle are than multiplied by the ratio
of the original particle volume to the scaled particle volume, which represents the number of
scaled particles contained in the original particle. This accounts for the summation of the scaled
drag forces and fluxes within the original particle (Fig.1 – work from A. Hobbs of Astec Inc.)
providing increased accuracy. More information regarding this can be found in the EDEM User
Forum (available to EDEM users only).
It is important to note that the scaling effects depend on the scale, the size distribution and the
shape of the DEM particles. Therefore, the contact model used will only be able to quantitatively
capture the bulk powder behavior by using upscaled particles only if the scaling laws (geometry
dimensions, stress levels, loading conditions, etc) are applied correctly [14, 15]. Finally, this
approach must be employed with caution when combined with physics that is important for small
Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 8
time-scales (e.g radiation). The outcome of this method is meaningful when it is related to the
bulk powder behavior and not with the behavior of the individual particles.
Figure 1
Drag force calculation based on the scaling factor (a) Drag force is calculated at real scale with no scaling
factor (scale factor=1) (b) Particles are scaled up 10 times with no scaling factor (scale
factor=1). (c) Particles are scaled up 10 times with a scaling factor (scale factor=10) –
work by A. Hobbs from Astec Inc.
Some basic guidelines on how to scale up specific contact models can be found below:
EEPA is valid for two types of systems, cohesive and non-cohesive. The non-cohesive systems
include only the loading and unloading stiffness. Stiffness is a function of the shear modulus and
is proportional to the particle’s radius:
• Loading stiffness: k1 ∝ d
• Unloading/reloading stiffness: k2 ∝ d
Therefore, the stiffness is automatically scaled with the change of particle size without the need
of any other consideration by the user. This is valid for both linear and non-linear modes.
Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 9
The cohesive systems require the use of the pull-off force and the adhesion which is load
dependent. These parameters are not scaled automatically, and the user needs to scale them
based on the particle size:
• Constant pull-off force: f0 ∝ d2
• Load dependent adhesion: kadh ∝ d
𝐸𝐸 2�
𝛾𝛾 = 𝛾𝛾𝑚𝑚𝑚𝑚𝑚𝑚 ( ) 5 (1)
𝐸𝐸𝑚𝑚𝑚𝑚𝑚𝑚
where 𝛾𝛾𝑚𝑚𝑚𝑚𝑚𝑚 and 𝐸𝐸𝑚𝑚𝑚𝑚𝑚𝑚 are the modified surface energy and Young’s modulus, respectively.
Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 10
Figure 2 Example of a simple DEM bulk density simulation using EDEM – measurement of material
mass used for the calculation of density and comparison with real bulk density.
Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 11
Figure 3 Experimental Static Angle of Repose test (left) and virtual representation with EDEM (right).
The use of the standard slump (tube) test has been controversial. It has been reported that for
calibration of cohesive and wet materials, the standard slump (tube) test is inadequate as it
cannot capture the effect of various moisture contents on the angle of repose or pile height. An
alternative method would be the drained angle of repose test (Fig.4), where the material is
drained from a box to examine the quasi-static and dynamic behavior when the pile forms. When
used as a highly automated process it provides more accuracy and better describes the behavior
of the material.
As a rule of thumb measurements of the resulting angle need to be taken following the free
surface of the material and not the corner of the test equipment. Also, it is important that when
setting up the DEM simulation it contains enough particles so that the results are not misleading.
A general rule for having enough particles is to keep the simulation time in a reasonable
timeframe.
Figure 4 Drained angle of Repose test. Hopper discharge for measurement of the angle of repose and
height of pile.
Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 12
between the range of 1-70rpm. A camera is used that monitors the flow and takes snapshots for
each angular velocity. The powder-air interface is detected by using different colors, usually air
is shown as white and powder as black. Then for each rotating velocity, the average avalanche
angle (or DAoR) is calculated, which corresponds to the angle where the powder was at
maximum position before the start of the avalanche (Fig.5 (right)).
Figure 5 Schematic of a drum with glass side-walls used for the rotating drum test (left) and virtual
representation of the test using EDEM (right) [1, 2].
Finally, from the interface fluctuations in this position the standard deviation is measured, which
is directly related with the cohesive index of the material. The rotating drum process needs to
be replicated by the DEM tool and both the average avalanche angle and the standard
deviations need to be derived and compared with the experimental values.
This calibration test provides information relating the static part and the frictional part of the flow.
Therefore, the DAoR is influenced by several DEM parameters such as friction coefficients,
shape of particles and cohesive forces. The dynamic cohesive index is only related to the
cohesive forces between the particles. Dynamic cohesive index close to zero corresponds to
non-cohesive powders, whereas when the powder cohesiveness increases, the cohesive index
increases accordingly. Therefore, the Cohesive Index can also quantify powders spreadability.
Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 13
a
Slices
Figure 6 Virtual replication of the rotating drum experimental test and calculation of the average
avalanche angle with the use of slices.
Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 14
The instrument calculates the total energy required to mix a powder using Eq.(2)
𝑡𝑡
where ∆𝑡𝑡 is the data write out interval, 𝑣𝑣𝑣𝑣 is the blade vertical velocity, 𝜃𝜃𝑟𝑟 is the blade rotational
velocity and 𝐹𝐹(𝑡𝑡) and 𝑇𝑇(𝑡𝑡) are the instantaneous vertical force and torque on the blade at time
t, respectively.
Figure 8 shows the virtual replication of this test, using the DEM tool, in terms of dynamics and
test conditions. This type of simulation is highly influenced by the chosen timestep and the hence
the shear modulus of the material (see Chapter3.3). Apart from the shear modulus it has been
reported that the solid density has a large influence on the simulation results while the poison’s
ratio is the least influencing factor. Finally, the particle size and shape for this calibration test is
critical and has to be carefully chosen. Based on research, bi-sphered particles with specific
aspect ratios can usually capture the behavior of the real material. For more information and
relevant references please refer to Chapter 3.
Figure 8 Simulation of the FT4 test at different times using EDEM [5].
Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 15
paused for 2 s to allow the material to settle and the bulk density measurement taken. When the
bulk density variation between measurements was negligible the tapped density was recorded.
A time-step of 5e-6 s was used for the tap tests.
(a)
(b)
Figure 9 DEM simulation of the tapped density test with the use of EDEM (a) and schematic of the
apparatus used for experimental measurements (b) [4].
Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 16
6.6 Untapped bulk density test
The untapped density follows the same logic as the tapped density test. Figure 10 shows a DEM
example in which a 100 ml cylinder is created with 16 mm radius and 185 mm height. 0.05 kg
of powder material is added via a funnel at the top of the cylinder at a rate of 0.2 kg/s and an
initial velocity of -0.25 m/s.
Figure 10 DEM simulation of the untapped bulk density test at different times using EDEM.
The material was allowed to settle and the bulk density was calculated from the height of the
material in the cylinder following a standard experimental [4]. A time-step of 2e-6 s was used for
bulk density tests.
The measurements taken from the tapped and untapped density tests are used for the
calculation of the Carr index and the Hausner ratio, that characterize the flowability and
compressibility of a powder:
Compressibility or Carr index: 100 × (tapped density – untapped density)/tapped density
Hausner ratio: tapped density/untapped density
Research has shown that values of Carr Index below 15% indicate very good flow character but
values above 25% indicate poor flow. Also, Hausner ratio values of around 1.00–1.25 indicate
free-flowing powder, values between 1.26–1.45 indicate poor flow, and above 1.46 are related
to extremely poor flow [19, 20] Marshall (1986).
Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 17
pressure is removed and the consolidated sample is removed from the cylindrical cell so it is
free standing. This is referred to as an unconfined sample as no walls are confining it to a fixed
shape. Then increasing pressure is slowly applied to the top of the sample until the sample
breaks or yields (Figure 11). The maximum pressure before the sample yields is referred to as
the Unconfined Yield Strength σc. The σc is the strength of the powder mass after it has been
compressed by the σ1. This means that the material will flow only if the force acting on it is
greater than its unconfined yield strength.
To have meaning, the unconfined yield strength must be expressed in combination with the
major consolidation stress. This is because granular materials and especially powders gain
strength when consolidated with more pressure. A flow factor can be calculated by dividing the
major consolidation strength by the unconfined yield strength. The greater the value of the flow
factor the better the material will flow at any given pressure.
Table 1 presents generally accepted classification of powders and granular materials with
different flow factors. This test is often chosen for characterizing the flowability of powders but
only if the stress state of the application is high enough (>10kPa).
Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 18
6.8 Ring Shear cell test
This test is suitable for mixing applications, especially when the powder is pressurized during
mixing or while kept inside a container, as well as for predicting the conditions under which
caking is likely to occur. Figure 12 shows the apparatus that is used for this type of test. A
sample of powder is contained in an annulus, restricted by co-axial cylindrical walls, and is
rested on a stationary bottom disk, covered with a top lid. Both the top lid and the bottom surface
have geometric spaces (teeth) oriented radially and uniformly spaced around the annulus. The
top lid rotates with a controlled angular speed and applies a normal load to the powder. The
powder is pre-sheared which means that it is consolidated by applying a normal stress and then
sheared (by lid rotation) until the measured shear stress reaches a quasi-static condition. The
purpose of the pre-shear step is to establish a consolidation state that replicates the pressures
that would be experienced at a container. Next, the normal load is reduced, and another shear
step is applied until the material fails. From the test results, the major consolidation stress and
unconfined yield strength are determined [21].
The major consolidation stress describes the state of stress that was used to consolidate the
sample during the pre-shear step, which includes contributions of the normal and shear stresses
present in the cell during the pre-shear step. The unconfined yield strength is a measure of the
cohesive strength that the powder gained due to its consolidation during the pre-shear step.
The test is then repeated over a range of consolidation states to establish the Flow Function
relationship, the Flow Function coefficient and the Time Flow Function relationship of the
material.
The Flow Function is the relationship between consolidation pressure and the cohesive strength
(unconfined yield strength) of the material, while the Time Flow Function is the relationship
between consolidation pressure and the material’s cohesive strength after it has been stored at
rest. Specifically, when conducting a time test, the sample is kept in a consolidated state after
the pre-shear step for the time of interest and then sheared until failure. When the measured
cohesive strength of a powder is greater after storage at rest than during continuous flow, this
is an indication that caking is likely to occur in the real application. Therefore, this type of
calibration test can predict the conditions under which caking is likely to occur and hence give
room for improvements and alterations of the operating conditions.
In real life there are cases where even though powders have very similar flow functions they
have very different flow behavior. This is likely to happen due to their differences in weight,
hence by integrating the effect of density against its own strength, the analysis can provide
meaningful results. The Normalized Flow Function (NFF) analysis offers this type of analysis
and provides valuable insight as to why powders fail to flow. The NFF is produced by plotting
the arching dimension (D) of the outlet versus the consolidation stress.
Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 19
Figure 12 Schematic of a Ring Shear Tester (left) and top view of the particles as simulated inside the
ring shear tester (right) [3].
Shear cell testers can also be used to measure the material’s wall friction, which is required if
the solids stress in a rigid container must be calculated. Wall friction is measured by following
the method described in ASTM D-6128. The friction coefficient is the ratio of the shear stress to
the normal stress. Because it is a function of normal pressure, the test needs to be repeated
over a range of normal loads.
More specifically, DOE/Opt methods explore a design space to identify the behavioral trends
and influences of possible input parameters. In a DEM calibration simulation, a typical DOE
search will involve running a series of simulations with different combinations of input parameter
values and monitoring of performance output. A typical analysis of the results will identify those
parameters that have the most influence on the performance output; to what extent; and the
interdependencies that exist between parameters.
The automated nature of the DOE/Opt methods is critical as parameter spaces for powder
applications are complex and human-based decision making may not be the most effective way
of reaching a solution. In addition, manual intervention increases the time required to perform
such analysis. Automating the process means that parameter space exploration is performed in
a mathematical, objective way without constant human intervention. However, designing a full
calibration procedure through DOE methods will always have a level of uncertainty and difficulty
Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 20
as the parameter responses are often non-linear and there is high inter-dependency (e.g. static
friction, rolling friction, cohesion, particle shape etc.). Therefore, it should be expected that the
calibration can be a time-consuming, and challenging process.
Nevertheless, the way forward appears to be the integration of DEM with DOE/Opt methods and
EDEM is aligned with this vision. Part of the future developments include collaborations with
different DOE packages aiming to an automated/faster calibration process, removal of the
dependency on human judgement on parameterization and to a greater insight on the
identification of the critical parameters.
Another important requirement in the powder handling processes is the ability to model real size
particles, and hence vast numbers. Modelling industrial processes based on laboratory or pilot
scale devices without any scaling up is still a big challenge and the use of GPU and multi-GPU
technology appears to be the way forward. EDEM is actively supporting its customers as well
as research by implementing important features and capabilities, such as the double precision
GPU solver engine for increased accuracy, the Application Programming Interface (API) that
enables users to customize physics and development of multi-GPU technology for even faster
and larger simulations. This will allow direct comparison with pilot-scale experimentation and
optimization of the production.
Finally, a topic that seems to gain more ground in the latest research is the use of the Bond
number (Bo) in the calibration process. Very recently researchers from the University of Leeds
have been investigating Bo as an alternative/new method to scale-up and predict the flowability
of multi-component blends. This is an ongoing work from Leeds University as part of the Virtual
Formulation Laboratory project and it is due for publication in September 2018.
For more information and/or questions please contact EDEM support team at
support@edemsimulation.com
Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 21
Appendix I: Suggested Calibration tests per application
Industrial Suggested
Measured bulk properties
applications calibration tests
• Unconfined yield strength
Hopper
Uniaxial Unconfined Test • Flow factor
applications
* not applicable to low stresses (<10kPa)
• Flow energy
• Particle- particle friction
FT4 Freeman Rheometer • Particle-wall friction
* insensitive to Coef. of Restitution thus unsuitable for systems
vary cohesion and static friction. Materials with low P-P cohesion should have low P-G
cohesion, materials with high P-P cohesion should have high P-G cohesion. Following
that rule the P-G static friction can then be varied to check influence of results.
High speed video • P-P restitution (ratio of the velocities before and after impact gives
recording camera test the coefficient of restitution)
Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 23
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Calibrating DEM Models for Powder Simulation: challenges, advances and guidelines 25
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