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Marchetti, L., Hulme-Smith, C. (2021)

Flowability of steel and tool steel powders: A comparison between testing methods
Powder Technology, 384: 402-413
https://doi.org/10.1016/j.powtec.2021.01.074

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 Powder Technology 384 (2021) 402–413

Contents lists available at ScienceDirect

Powder Technology

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

Flowability of steel and tool steel powders: A comparison between

testing methods
Lorenzo Marchetti ⁎, Christopher Hulme-Smith
Department of Material Science and Engineering, KTH Royal Institute of Technology, Brinellvägen 23, 11324 Stockholm, Sweden

a r t i c l e i n f o a b s t r a c t

Article history: The flow behaviour of a powder is critical to its performance in many industrial applications and manufacturing
Received 24 September 2020 processes. Operations such as powder transfer, die filling and powder spreading all rely on powder flowability.
Received in revised form 29 January 2021 Multiple testing methods can help in assessing flowability, but it is not always clear which may better represent
Accepted 30 January 2021
specific flow conditions or how different metrics correlate. This study compares 8 different flowability testing
Available online 16 February 2021
methods using 11 steel powders varying in chemistries and size fractions. Regression analysis was used to test
Keywords:
the relationship between each flowability metric obtained. Some metrics, such as the conditioned bulk density, re-
Powder flowability late to many flowability indicators. Others, such as the basic flowability energy, show poor correlations to other
Steel powders variables, likely describing different aspects of the powder flow behaviour. When two metrics show a strong cor-
Comparative flowability testing relation, as between conditioned bulk density and Hausner ratio, a numerical relationship is derived: CBD =
Flowability correlation − (5.65 ± 0.86)HR g cm−3.
Powder rheometer © 2021 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY license (http://
creativecommons.org/licenses/by/4.0/).

1. Introduction
The flow of a powder is a complex phenomenon to understand or
model. It is sensitive to properties of the powder itself and external fac-
tors such as humidity [1,2], geometrical impediments [3], or applied
stresses [4]. Within the powder, many factors affect flow properties,
such as the size distribution and shape of the particles, their surface
roughness and oxidation state, the material density, and electrostatic
and magnetic characteristics [5,6]. Powder handling also affects flow
by altering the packing of particles and the ratio of solid to other phases
in the ensemble. This complexity has significant consequences for many
fields that rely on powder and its propensity to flow or remain cohesive,
such as powder metallurgy, soil mechanics, civil engineering, the phar-
maceutical industry, paint production and food processing. If the pow-
ders are more cohesive than predicted, this could limit the materials
stream in a process or affect the final product quality [7]. Therefore, it
is crucial to provide an accurate description of the flow of a powder
for a specific process. When the same powder is used in different appli-
cations, it may be important to provide a description that is relevant for
a general process [6].
The growing focus on metal powder-based additive manufacturing
technologies increasingly highlights the need to deliver components
that comply with industry standards and operate under demanding
conditions. The powder plays a key role in the final component quality
[8–11]. For example, to produce low defects components in a powder-
⁎ Corresponding author.
E-mail addresses: lormar@kth.se (L. Marchetti), chrihs@kth.se (C. Hulme-Smith).
bed based additive manufacturing process, the metallic powder should
be spread in a thin, compact, and even layer [12–14]. Similarly, in press
and sinter and hot isostatic pressing a good powder flowability can
avoid cavities and improve the die filling [15], while in cold spray depo-
sition the flow rate of powder and gas can directly affect the coating de-
position rate [16]. There are many viable techniques to measure flow in
a powder, but no agreement as to which is the best testing method for a
given application [6,17–21]. Furthermore, there is no agreement on
what flow behaviour is required for a powder to be considered suitable
for any specific manufacturing process.
The flow behaviour depends on the balance between forces that
drive the motion of particles and those that prevent it. Forces promot-
ing flow are gravity and applied external forces, while the ones oppos-
ing it include frictional forces between the powder particles and the
external surfaces, as well as forces between neighbouring particles.
Such inter-particular forces include mechanical friction, the mechani-
cal interlocking of particles, van deer Waals forces, capillary forces,
electrostatic force, and magnetic force [22–24]. The magnitude of
these resistive forces is determined by an array of properties arising
from the powder, such as powder particle size and particle size distri-
bution, particle shape, material density, particles roughness, surface
chemistry, oxidation, and water content [18,25]. In addition, the ma-
terial of the testing equipment, its surface conditions, geometry, and
operating conditions (e.g., if the test uses stationary or moving pow-
der, stress state, temperature, gas flow) can also have a significant ef-
fect on the flow behaviour. For example, when a stress is applied to a
powder column of irregular particles, its density increases, locking the
particles in position. Hence, mechanical forces will propagate across

https://doi.org/10.1016/j.powtec.2021.01.074
0032-5910/© 2021 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
L. Marchetti and C. Hulme-Smith Powder Technology 384 (2021) 402–413

particles more easily, strongly affecting the flow behaviour and over- Table 1
coming the effect of the weaker cohesive forces. This web of proper- Overview of the powders used in the experimental trials.

ties and mechanisms that compete and act concurrently makes Material classification Particle size distribution
powder flow a complex multivariate problem [17], where is not fully Production process Alloy Designation D10 / μm D50 / μm D90 / μm
clear exactly how properties of the powder itself affects flowability
Water atomization 17–4 PH 1 7.4 19.9 44.6
[17,19].
316L 2 8.2 20.7 42.3
Due to the complexity of the powder flow, there is no single tech- Gas atomization 17–4 PH 3 5.7 10.7 15.4
nique to characterise flowability for a specific application [26] and stud- 4 7.5 17.0 37.2
ies do not always agree on the best one to use for any specific case 5 59.8 75.1 95.6
[18,21,27]. Furthermore, many common methods found in the literature 316L 6 16.5 35.4 50.4
7 14.5 26.4 46.2
are not standardised, such as the rotating drum angle of repose, powder 420 8 11.5 28.3 45.4
rheometry and spreading devices [18,21,28]. Others, such as tap density Tool steel 1 9 25.0 37.8 57.0
testing, static angle of repose and shear cell testing are standardised Tool steel 2 10 23.9 35.8 55.4
[29–32], but not included in the recommended standards when Tool steel 3 11 18.4 30.9 55.7
characterising the flowability for additive manufacturing metallic pow-
ders [26]. ASTM F3049-14 suggests instead to characterise powders for
additive manufacturing with a Hall funnel, Carney funnel or Arnold
2. Materials and method
meter [26]. However cohesive powders might not be suited for these
methods as they B. Spierings, M. Voegtlin, T. Bauer, K. Wegener, Powder
2.1. Sample preparation
flowability characterisation methodology for powder-bed-based and
give non-quantitative results [21]. When ranking the flowability of sev-
Flowability tests were performed on 11 steel powders with various
eral powders, it will not be possible to differentiate between the non-
chemistries, atomization routes and particle size ranges (Table 1). The
flowing ones, making a comparison difficult. Also, characterising
particle size distribution of each powder was measured using a
flowability with different methodologies may lead to contrasting results
Camsizer XT particle analyser with compressed air dispersion. Addi-
[33,34]. To avoid this, it is often recommended that testing should be
tional data regarding particle shape and particle size distribution are in-
performed under conditions that reproduce the specific case of interest
cluded in the supplementary files (Supplementary Fig. 1 and
as far as possible [17,26].
Supplementary Table 1). Each powder batch was sampled with a rotat-
A holistic evaluation of the flow behaviour of a powder based on
ing sampler divider (spinning riffler) to obtain 5 individual specimens,
multiple testing would solve the limitations of using a single
prepared according to the relevant industrial standard (ASTM B215)
flowability test for powders intended for applications with different
[38]. Three specimens with a mass of 50 g were prepared to test the
parameters or where it is not clear which test is the most suited [6].
flow rate and tap density [39–41]. Two further specimens were pre-
However, a comprehensive model describing flowability has proven
pared with a volume of 25 ml for testing in a powder rheometer
problematic to obtain. This is due to the complexity the high number
[29,42] and a fixed height funnel angle of repose meter [43]. The speci-
of inter-dependent variables that must be accounted for in powder
mens were dried for 30 min at 105 °C to remove moisture immediately
flow [10]. Some models are published in literature, mostly restricted
before testing. Adsorbed water layers and liquid bridging between par-
to specific flow conditions and without explicit physical variables
ticles are known to deteriorate the flow properties of metallic powders,
[21,35]. Comparative testing can complement existing models and
especially at higher relative humidity [44–46]. While it is reasonable
give a more complete description of the problem [6,8,17,19]. Numer-
that during testing powders adsorbs some moisture from the environ-
ical modelling simulations such as the direct element method (DEM)
ment, it is unlikely that such uptake within the short time between dry-
are also a powerful tool to link interactions between particles to
ing and testing will have a large impact on the results [47].
their flow and the behaviour of the ensemble. In the case of fine metal-
lic particles, such modelling techniques may have some limitations.
2.2. Flowability measurements
This is partly due to increased computational demands of modelling
micrometre-scale particles and the need to consider several factors,
Flowability was evaluated with multiple measuring techniques,
such as the particle size distribution, shape, roughness, van deer
which can be divided into separate categories (Fig. 1). The difference
Waals forces, liquid bridging and eventual electromagnetic forces
within these techniques can be important, as a testing method affects
that are known to affect the flow. It may be possible to simplify the
the stress state, velocity of the powder particles, packing density and
force models used in the simulations, but more research is required
other factors in a powder. The ambient conditions and the history of
before such solutions may be applied with confidence and be realistic
the powder are also well known to influence its flow behaviour
for industrial applications [36,37].
[42,48,49].
In the present work we compare a range of flowability measuring
techniques available using a range of metal powder size fractions and
2.2.1. Flow rate measurements
chemistries. The results are used to evaluate the relationships between
When in a funnel, a powder may flow out due to gravity. A way to
the metrics from the different flowability measuring techniques using
quantify the phenomenon is the time required for a fixed mass (or vol-
statistical analysis. By including a range of powder chemistries and
ume) of powder to flow entirely out of the funnel. This metric is com-
size distributions, it is intended that relationships should not be specific
monly referred to as the flow rate.1 A lower flow rate is an indicator of
to individual alloys or powder production conditions. The common
a better flowability. When frictional forces are low, the powder flows
flowability measurement techniques are assigned to categories, where
out of the funnel and the powder remaining in the funnel forms a sur-
one representative method is selected from each. Every powder is
face that is approximately horizontal and gradually descends. When
then measured using each selected technique and statistical analysis is
frictional forces dominate, powders may form an arch near to the outlet
performed on pairs of metrics to derive any correlations. From these
of the funnel, which leads to the presence of stable vertical cavities
evaluations, it may be understood which techniques are equivalent of
each other and which techniques do not correlate. These are likely to 1
There is a contradiction that a “rate” measures how much or how often something
be measuring different responses in the powder to flow. Multiple tech- happens per unit time, but the flow rate is the time required for a fixed mass (or volume)
niques would be needed to describe all aspects of the powder flow of powder to leave the funnel. More correctly, this is a specific (or volumetric) time, not a
behaviour. rate, but the term flow rate is common.

403
L. Marchetti and C. Hulme-Smith Powder Technology 384 (2021) 402–413

Fig. 1. Flowability testing methods overview. For every testing method class, some of the common testing methods applicable are listed below. The highlighted methods have been chosen
for this work [19,21,29,39,40,42,43,50–57].

(ratholes) or jamming, where the powder does not flow at all. These ef- can be overcome by shaking the powder and allowing particles to rear-
fects are well studied in the literature and can be observed when range through tapping. Similarly, in the first stages of the particle mo-
powders are cohesive, when the ratio of the orifice diameter to the par- tion, powders will locally vary in their densities when particles start to
ticle diameter is too low or when the particle size distribution is too move one past each other. In the current work, the apparent density is
wide [58]. replaced by the conditioned bulk density (CBD, ρc) [42], which is a similar
Such techniques have been common for a century and are currently quantity measured in the Freeman FT4 powder rheometer from Free-
recommended for additive manufacturing [21], with several funnel ge- man Technology Ltd. (Tewkesbury, U. K.) (Eq. (1)). Conditioned bulk
ometries described in the active standards. The best-known experimen- density is measured after the powder sample has been gently stirred
tal setup is the Hall flowmeter (ASTM B213–17) [39], which works well by an upwards-moving blade and reduced to a fixed volume.
for non-cohesive powders. Cohesive powders may be tested using the
Carney funnel (ASTM B964−16) [40], with a wider bottom opening, RH ¼ ρt=ρc ð1Þ
and the Gustavsson funnel [56], with a steeper conical surface. In the
current study, Hall, and Carney funnels from Qualtech Products Ltd.
(Manchester, U. K.). were used.
2.2.3. Angle of repose
The angle of repose is the angle of a pile of powder at which it stops
2.2.2. Density ratios flowing. It is the complementary property to avalanche angle, which is
The ability of a powder to pack can be taken as an indicator for its the angle at which a stationary powder will begin to flow. A well-
flowability, as particles must move past each other (i.e., flow must flowing powder will not stop flowing when the powder pile has high
occur) to increase packing density [54]. In general, the packing of a pow- angles. However, lowering the pile angle, the gravitational component
der is quantified through its bulk density (defined as the mass of a sam- moving the powder will diminish. At the point where the powder
ple divided by the total occupied volume, inclusive of particles and air stops flowing, the gravitational component driving the flow is balanced
gaps). Santomaso et al. [54] make a distinction between measuring by the attractive and frictional forces within the powder (Fig. 2). Previ-
the bulk density of a powder in a loose or a dense packing condition. ous research has used the angle of repose to qualitatively classify the
For example, a loose random packing condition is achieved through flowability powders [65, Table 1].This angle can be measured in several
test as aerated, poured, or apparent density [57,59–61]. Other tests pro- alternative methodologies: by allowing a powder to fall through a
mote a denser random packing through different methods, allowing
air to exit the bulk volume. The most well-known example is the tap
or tapped density, which is achieved after the powder is gently shaken
and allowed to settle to a constant volume [41]. In this study, 3 samples
of 50 g were tapped using an Autotap tap density tester from
Quantachrome (Boynton Beach, Florida, U. S. A) for twice as many
taps as was necessary for the volume to stop changing, in accordance
with ASTM B527-15.
When comparing different powders, the ratio between high and low
packing densities, or Hausner Ratio, RH is commonly used. This is often
expressed as the ratio between the tapped density ρt is and the apparent
density ρa. However, some authors replaced the apparent density with
other alternative metrics, such as aerated density [35,62], poured den-
sity [63], apparent density determined with the Scott volumeter [64].
A high value of Hausner ratio indicates a high variation between the
starting loose packing density and the final dense packing density. Fig. 2. Forces acting on a single particle in a powder pile. Fg is the gravitational force, Fa is
the sum of the frictional forces, Fc the sum of the cohesive forces, FN is the normal force. F is
This is usually due to weak forces, such as mechanical contact forces the gravitational component promoting the flow. (a) With a steeper pile, F > Fa and the
or cohesive interparticle forces, which prevent the powder from particle will move down the inclined surface; (b) when the powder pile is flatter, F < Fa
reaching an optimal loose packing density. The effect of these forces so the particle slows down, and eventually stop.

404
L. Marchetti and C. Hulme-Smith
funnel onto a flat surface and form a pile (fixed funnel method), by filling
a hollow cone with powder and removing the cone, allowing the pow-
der to settle into a pile (hollow cylinder method), or by causing powder
to run along a planar surface tilted at some angle and finding the tilt
angle at which the powder stops moving (tilting box method) [43].
While this final method measures the avalanche angle, it is commonly
referred to as a technique to measure angle of repose. In all these
cases the cone angle of the pile of powder is measured statically. It
should be noted that there is evidence that the angle of repose depends
strongly on the method chosen to measure it. For example, the proce-
dure outlined in the standard ASTM C1444 (a variant of the fixed funnel
method) gives a higher angle of repose than the cone lifting technique
[65]. In the current study, a fixed funnel method was used, with a pro-
tractor fitted to the funnel stand to measure the angle of the side of
the pile directly. The funnel has a cone angle of 60°, an orifice diameter
of 5 mm and a distance between the orifice and the tray where the angle
forms of 80 mm (Qualtech Products Ltd., Manchester, U. K). When pos-
sible, two samples of 25 ml were measured three times for each powder,
where every measurement consisted of three angles observations at an-
gles from the same pile, as suggested in the instrument operating man-
ual. The angle of repose was taken as the average angle of the pile.
Measuring the angle with a protractor mounted on the funnel assembly,
it was possible to exclude the effect of possible distortions on the pile,
such as the presence of a small flat cone tip, or a wide base, by taking
the angle in the remaining part of the pile edge. Other methods, which
calculate the angle based only on the diameter and the height of the
pile, could be more prone to these errors.
These methods are inexpensive and traditionally used to character-
ise powder flow, but none of them are described in the current stan-
dards for the characterisation of metallic powders [30–32,51]. A
related technique, which is mostly automated and not standardised, is
the dynamic angle of repose or rotating powder analyser, in which pow-
ders are placed in a drum and rotated for a pre-programmed speed
cycle, during which pictures are taken and evaluated automatically.
Powders rise the drum until some critical angle is reached (avalanche
angle), at which it begins to flow. It then stops at some lower angle
(rest angle). Based on these angles and the irregularity of the powder
profile, several parameters are automatically calculated and can be
used to indicate flow behaviour.
2.2.4. Shear cell
In a shear cell, a powder sample is confined between two flanges,
which subject the powder to a pre-set cycle of normal and shear
stresses. First, the powder sample is consolidated to a set pre-
compaction normal stress (σ1c). It is then sheared at different compres-
sive stresses below σ1c. Some powder particles move coherently with
one moving flange, while some other adopt the velocity of the second
flange, which is usually fixed. There is a region where particles will tran-
sition from following one flange to following the other. In this region,
particles move past to each other under a shear stress. The shear stress
necessary to initiate the flow is recorded at different compressive
stresses. The normal and shear stresses are then used in a Mohr's circle
to plot the stress state at which flow first began in at each compressive
stress, known as the locus of incipient flow. Several parameters can be
derived from this diagram, such as cohesion (C), unconfined yield
strength (UYS), major principal stress (MPS), angle of internal friction
(AIF) and the flow function coefficient (ffc or FF) [42,66]. In general, a
good flowability leads to lower shear values of these metrics, except
for the flow function coefficient, where a higher value should indicate
a better flow behaviour transitioning from static to dynamic friction.
In this work, a shear cell supplied with the FT4 powder rheometer
was used following ASTM D7891–15 [29]. Pre-compaction stresses of
3 kPa and 9 kPa were chosen. To increase the data reliability, two sam-
ples were tested for each powder. The pre-compacted volume of the
tested sample was of 10 ml, while the vessel diameter 25 mm.
405
Powder Technology 384 (2021) 402–413
2.2.5. Rheometry
Powder rheometry is becoming increasingly popular also for metal-
lic powders [6,8,67,68]. In addition to the shear cell unit, other test
methodologies are available to characterise the powder behaviour
under different conditions. The testing is mostly automated, while the
interaction with the operator very limited. To homogenise the sample,
a pre-mixing (conditioning) is performed prior testing. Two standard
programs of the FT4 powder rheometer were used with a 25 ml sample
and a vessel diameter of 25 mm. Each test was performed on two
samples.
The first program was the stability and variable flow rate test, in
which an impeller moves in a set path through the powder (Fig. 3a).
For each sample, the test automatically runs 11 times: seven tests run
at a fixed vertical blade tip speed and then four runs at increasing verti-
cal blade speeds. The resistance met from the impeller is recorded and
converted into synthetic indices. The basic flowability energy (BFE) is
the energy spent from the blades moving downwards, where the pow-
der is compressed and confined to a fixed volume by the blade and the
walls of the test vessel. The specific energy (SE) represents the energy
spent when the blades move upwards, when the powder is free to oc-
cupy more volume (unconfined flow) [42].
The second method performed was the compressibility test, where
the powder is confined in a vessel and slowly subjected to uniaxial com-
pression (Fig. 3b). At the same time, the variation in height is recorded.
The compressibility (CPS) is then calculated as change in volume before
and after the powder is compacted with a 15 kPa applied compressive
stress [42].
3. Calculation
3.1. Parameters
In this study a broad overview of the relationships between several
flowability measurements is presented. For every flow test performed,
one or more metric can be recorded to evaluate the behaviour of a pow-
der (Table 2). Each of these metrics was then compared with all the
other, as well as conditioned bulk density. To focus on the relationship
between testing methods, no distinction was made between different
powders and all the eleven tests were taken as a dataset. The mean of
all repeats was reported for each powder. All results are supplied as a
supplementary file in the online version of the article.
Fig. 3. (a) Sketch of the FT4 vessel and impeller in the Stability and Variable flow rate,
(b) sketch of the vessel and the flange for the Compressibility test.
L. Marchetti and C. Hulme-Smith Powder Technology 384 (2021) 402–413

Table 2
Samples, devices, test performed and flowability indicators considered. N
∑ðxi −xÞðyi −yÞ
i¼1 σ xy
Sample Test Device Test Flowability Unit β11 ¼ ¼ ð4Þ
class indicator N σ 2x
∑ ðxi −xÞ2
50 g Flow Hall funnel Hall flow rate [31] Flow rate s (50 g)−1 i¼1
(3×) rate Carney Carney flow rate [32] Flow rate s (150 g)−1
funnel β10 ¼ y−β11 x ð5Þ
Packing Tap-meter, Tapped density [33], Hausner
density Rheometer Conditioned bulk ratio
density [34] β11 determines the steepness of the correlation between two vari-
25 ml Other Rheometer Flowability [34] BFE mJ ables (Fig. 4b). However, this does not measure the dispersion of the
(2×) SE mJ (g)−1 data. For this, the Pearson correlation coefficient, r, is used (Eq. (6)).
Other Rheometer Compressibility CPS (%)
For this reason, it can give an indication of the strength of the correlation
@ 15 kPa [34]
Shear Rheometer Shear test Cohesion kPa and its direction. As the Pearson correlation coefficient is scaled for each
cell with shear @ 3 kPa [23] UYS kPa variable, it oscillates between −1 (inverse perfect correlation) and +1
cell MPS kPa (direct perfect correlation), while 0 implies no correlation.
FF
AIF degrees N
Shear Rheometer Shear test Cohesion kPa ∑ðxi −xÞðyi −yÞ
cell with shear @ 9 kPa [23] UYS kPa i¼1 σ xy σx
r ¼ sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
ffisffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi ¼ ¼ β11 ð6Þ
cell MPS kPa N N σ xσ y σy
FF ∑ ðxi −xÞ2 ∑ ðyi −yÞ2
AIF degrees i¼1 i¼1
Angle of Fixed Fixed funnel angle of Angle of degrees
repose funnel repose repose
angle of
repose
3.3. Non-linear correlation

It is possible that pairs of metrics may be correlated in a non-linear

way [35]. To assess the non-linear data trend between flowability pa-
rameters, a multiple linear regression was performed. In addition to f1
3.2. Linear correlation
(xi), the data have been fitted to polynomial (Eqs. (7) and (8)) logarith-
mic (Eq. (9)) or mixed (Eq. (10)) functions. The polynomial expressions
As a first evaluation step, the correlation across each pair of param-
are a natural extension to the linear correlation. The logarithmic depen-
eters (X and Y) was investigated using the programming language R.
dence was tested in the eventuality that a correlation could gradually
To analyse the data, the generic equation for a straight line was used
decrease in strength.
(Eq. (2)). The intercept β10 and the slope coefficient β11 were deter-
mined performing a linear regression with the ordinary least square
f 2 ðxi Þ ¼ β20 þ β21 xi þ β22 x2i ð7Þ
method, where the sum of the squares of the residual ϵi (Eq. (3),
Fig. 4a) is minimized.
f 3 ðxi Þ ¼ β30 þ β31 xi þ β32 x2i þ β33 x3i ð8Þ
f 1 ðxi Þ ¼ β10 þ β11 xi ð2Þ
f 4 ðxi Þ ¼ β40 þ β41 log ðxi Þ ð9Þ

yi ¼ f ðxi Þ þ ϵi ð3Þ f 5 ðxi Þ ¼ β50 þ β51 xi þ β52 log ðxi Þ ð10Þ

The solution of a system between Eqs. (2) and (3) leads to the deter- Multiple linear regression is similar to the linear regression, where
mination of β10 and β11 (Eqs. (4) and (5)). linear coefficients (βk0, βk1, βk2, βk3) are found minimizing the matrix

Fig. 4. Graphical description of the correlation between the Angle of repose and the Hausner ratio. (a) shows the straight line fitted to the data, the predicted values of the Hausner ratio as a
function of angle of repose, f(xi), (red diamonds) and the actual Hausner ratio, yi, (black dots). The vertical lines highlight the residuals, ϵi; (b) the uncertainty σ11 around the slope
coefficient of the gradient β11.

406
L. Marchetti and C. Hulme-Smith
of the square residuals [ϵ], obtained subtracting the fitted values [fk(x)]
from the observed values [y]. The adjusted coefficient of determination
R2adj was used to test the suitability of the model. As R2, R2adj explains how
much of the total variation from of the data from the average value is
expressed through the model (Eq. (11)). If the data had a similar disper-
sion to the model, then R2 will tend to 1, meaning that the model fits the
data well. Otherwise, if there are additional sources of variance in the
data, such as random scatter, R2 will fall to 0. In this case the model
does not explain any variance of the data. However, R2 increases with
many coefficients, leading eventually to overfitting. R2adj adjusts for the
number of coefficients in the model (k) relative to its data points (N)
(Eq. (12)).
N
2
∑ ð f k ðxi Þ−yÞ  2
σ xy
2
R ¼ i¼1
¼ ð11Þ
N σ xσ y
∑ ðyi −yÞ2
i¼1
  N−1
R2adj ¼ 1− 1−R2
N−k−1
3.4. Statistical significance
Although the linear coefficients βk (or the regression coefficient r)
are obtained minimizing the sum of residuals ϵi, there is always some fi-
nite probability that the fit is simply due to random scatter in the data
(i.e., there is not enough evidence to confirm the relationship between
variables). This probability is given from the p-value. When a p-value
is smaller than a pre-set significance level, there is enough evidence to
consider the relationship statistically significant. In this work the re-
quired significance level for all the p-values was set at 0.05, thus mean-
ing that there is 95% probability that the calculated fits are genuine
trends. The p-values were calculated with a Student's t-test, based on
a Student t distribution. This is preferred in regression analysis when a
small data set with unknown variance is used [69,70].
Fig. 5. Linear relationships across flowability indicators: (a) correlation matrix, where the size of the circles represents the modulus of the Pearson coefficients (from 0 to 1). The colour
describes the sign of the Pearson coefficients (white for a positive coefficient, black for a negative one); (b) map of the most important correlations between metrics.
Powder Technology 384 (2021) 402–413
4. Results and discussion
4.1. Linear correlation
While most of the flowability parameters reveal a positive linear cor-
relation, the conditioned bulk density (CBD) and the flow function coeffi-
cient (FF) clearly show an inverse one (Fig. 5a).
Hall and Carney flow rate exhibits a strong correlation with several
variables (e.g., positive with Hausner ratio and negative with compress-
ibility, CPS), while showing a weak dependence with most others. How-
ever, a powder with a good flowability would be expected to have a
lower flow rate, as well as a lower Hausner ratio and compressibility. It
is useful to note that, due to the cohesiveness of many of the powders
used in this study, few could give quantitative results in flow rate test-
ing: jamming or ratholing were observed on many samples, in agree-
ment with what was stated from Marnani et al. for fine and ultra-fine
particles [71] and Muñiz-Lerma et al. for fine metallic powders [73].
The low number of flow rate data available prevents us from drawing
conclusions on possible correlations (Figs. 2–4 in the Supplementary
file).
ð12Þ Conversely, Hausner ratio, angle of repose (AOR) compressibility and
specific energy (SE) all show a strong positive correlation between
them (Fig. 5 and Figs. 8–11 in the Supplementary file). These variables
also exhibit strong interactions with other shear test parameters. For in-
stance, Angle of repose and compressibility are strongly correlated with
cohesion, unconfined yield strength (UYS), major principal stress (MPS)
and flow function coefficient (FF), correlated with the conditioned bulk
density and weakly correlated with the angle of internal friction (AIF).
Conversely, Hausner ratio and Specific energy are weakly correlated
with cohesion, unconfined yield strength and flow function coefficients,
while strongly correlated with the major principal stress, angle of internal
friction and conditioned bulk density (Fig. 5). Many interactions between
shear test variables were similarly found in a study from Li et al. [73],
where 11 powders were tested with different Freeman FT4 setups. Co-
hesion was found positively correlated with unconfined yield strength
and major principal stress, while negatively correlated with the flow
function coefficient, indicating that a more cohesive has a lower
flowability.
407
L. Marchetti and C. Hulme-Smith
Basic flowability energy (BFE) shows weak between most of the var-
iables (Fig. 5 and Fig. 5 in the Supplementary file) and only some corre-
lation with the angle of internal friction and the flow function coefficients.
It is worth noting that basic flowability energy is one of the few parame-
ters to be poorly related to the conditioned bulk density (Fig. 6 in the Sup-
plementary file). This disagrees from what was found by Li et al. [74],
where the basic flowability energy clearly correlates with the condi-
tioned bulk density. In this study the powders tested had a significant
difference in density. In our study instead, all powders used are iron
based steels, with a relatively similar size fraction and density, so that
the effect of the density on the basic flowability energy goes unseen.
Other parameters poorly related to the conditioned bulk density are
shear cell metrics. Cohesion, unconfined yield strength and flow function
coefficients show a strong correlation between each other, but a poor
correlation with the conditioned bulk density. Conversely, the angle of in-
ternal friction is correlated with the conditioned bulk density. The Major
principal stress always showed a strong correlation with the conditioned
bulk density (Fig. 5).
Fig. 5b further summarizes some of the correlations analysed. Pa-
rameters showing ambiguous relationships with other variables, such
as Hall flow rate, Carney flow rate or the major principal stress (MPS) in
relationship to some shear cell parameters, were not included.
All the Pearson correlation coefficients obtained (Fig. 5a) were sub-
sequently filtered according to their significance level. The matrix of
the statistically significant correlation coefficients (with a confidence
of 95% or more) is shown in Fig. 6a. Despite the data filtering, 51 of
these relationships proved to be statistically significant, while the re-
maining 102 did not. For example, almost all the correlation coefficients
related to Hall and Carney flow rate are found to be not significant
(Fig. 6a). The only exception is the correlation between Carney flow
rate and the flow function coefficient with pre-compaction at 3 kPa. Al-
though this proved to be statistically significant, the data suggests that
the correlation is due to the lack of data available and not due to under-
lying physical causes (Fig. 4 in the Supplementary info).
Angle of repose, specific energy, compressibility and Hausner ratio con-
firmed most of their mutual strong positive correlation (Fig. 6a,
Figs. 8–11 in the Supplementary file). The correlation between the
angle of repose and Hausner ratio is often found in the literature
Fig. 6. Significant linear relationships across flowability indicators. a) Correlation matrix showing only the Pearson correlation coefficients with p a p-value < 0.05 (or with a 95% probability
of being representative). The size of the circles represents the modulus of the Pearson coefficients (from 0 to 1). The colour describes the sign of the Pearson coefficients (white for a pos-
itive coefficient, black for a negative one). b) Scheme of the most important and statistically significant (p<0.05) correlations.
408
Powder Technology 384 (2021) 402–413
[35,54], while there is less information available for the other variables.
These variables still exhibit some correlation with shear cell parame-
ters: while all except for compressibility are correlated with the major
principal stress, only the angle of repose and compressibility are correlated
with the unconfined yield strength. Finally, only compressibility is corre-
lated with both cohesion and the flow function coefficients. The correla-
tions can be summarised in the map shown in Fig. 6b, where only
variables correlating both to shear variables with pre-compaction at
3 kPa and 9 kPa are included.
Across the shear cell results, the strong correlation between cohe-
sion, the ultimate yield strength and the flow function coefficient can be
confirmed. The uncertain correlation the major principal stress with
other variables from shear cell testing is also confirmed, as well as its
strong correlation with other variables (Hausner ratio, specific energy,
angle of repose) and the conditioned bulk density (Fig. 6a). Finally, the
Conditioned bulk density shows a strong negative correlation with the
specific energy, Hausner ratio (Fig. 7 in the Supplementary file), Angle
of repose, major principal stress, while none with compressibility.
The diagram in Fig. 6b shows only the significant relationships pre-
viously reported in Fig. 5b. Parameters showing ambiguity, such as
Hall flow rate, Carney flow rate or major principal stress in relationship
to some shear cell parameters (cohesion, ultimate yield strength, flow
function coefficient, angle of internal friction) were not included.
4.2. Non-linear correlation
Along with the linear correlations, Fig. 7 shows the statistically sig-
nificant non-linear relationships obtained through the multiple linear
regression analysis (where all the individual coefficients were found
to be significant). Quadratic (Eq. (7)), cubic (Eq. (8)), logarithmic
(Eq. (9)) and mixed (Eq. (10)) relationships were all evaluated, but
only quadratic or cubic were found to be significant in any case. All
the non-linear relationships found are like the ones reported in Figs. 9
and 12 in the Supplementary file. While it is clear there is a statistically
significant variation from linearity, it is also difficult to explain the data
trend shown.
In some cases, non-linear relationships were found to fit the data
slightly better than some linear ones (for example the flow function
L. Marchetti and C. Hulme-Smith Powder Technology 384 (2021) 402–413

Fig. 8. Scheme of the correlations statistically significant (p < 0.05) and representative
(R2adj > 0.7).

Fig. 7. Correlation matrix summarizing the significant relationships between flowability

indicators. The chart includes both linear and non-linear relationships. All the
correlations and correlation coefficients shown have p < 0.05.
coefficient with pre-compaction at 9 kPa and compressibility), with the
latter having already a significance level above the pre-set 95% value.
For this reason, considering a non-linear relationship between these
variables could lead to overfitting.
The correlation between Carney flow rate and flow function coefficient
with pre-compaction at 3 kPa was instead excluded from Fig. 7 as there
are few data available from the Carney flow rate trials (Fig. 4 in the Sup-
plementary file). Taking this into account, the total number of statisti-
cally significant relationships increased from 51 to 59. The angle of
repose was confirmed to correlate linearly to the Hausner ratio, as also
observed from Geldart et al. [35] and Santomaso et al. [54].
In this study, only the correlations explaining the data to a good degree
should be considered. Table 4 in the Appendix reports all the statistically
significant regression coefficients βk along with their confidence inter-
val and the coefficient of determination R2 for the model considered,
which can be used to evaluate the goodness of fit for each correlation.
Table 3 instead reports only the correlations coefficients having a
R2adj > 0.7 (meaning that 70% of the variation observed in the data can
explained through the proposed model). A visual explanation of these
results is shown in in Fig. 8. Out of the 59 statistically significant rela-
tionships, only 15 are shown to fit well the data. Many of the correla-
tions previously found between specific energy, Hausner ratio, angle of
repose and compressibility are not found to be explanatory. However,
these metrics are still found to be important, relating either to shear
cell parameters or to conditioned bulk density.

4.3. Significant and representative quantitative relationships between
metrics
Although the relationships from in Fig. 7 are considered statistically
significant, this does not explain how well the coefficients βk fit the data.
Table 3
Statistically significant (p < 0.05) and representative (R2adj > 0.7) correlations across
flowability indicators.
4.4. Physical explanation
Many of the powders tested in this work showed a cohesive behav-
iour during the flow rate trials. When the powders obstructed the Hall
and Carney funnels, no flow rate could be recorded. Table 4 compares
the flow rates and the powder size in relationship to the funnel outlet
diameter, showing how for powders of similar chemistry and produc-
tion technique, the finer fractions have a greater tendency to jam
the funnels (sample 3 and 4, 7 and 11), while the coarsest powder

Variables Function β1 ± σβ1 R2adj

[β2] [± σβ2] Table 4

Measured Hall and Carney flow rates and ratio D50 (Doutlet)−1 for each sample.
MPS9 = ƒ(HR) Linear 10.1 ± 1.2 0.86
CBD = ƒ(HR) Linear −5.65 ± 0.86 0.81 Powder Hall funnel flow test Carney funnel flow test
SE = ƒ(AOR) Linear 0.083 ± 0.01 0.78 −1
D50 (Doutlet) Flow rate / s D50 (Doutlet)−1 Flow rate / s
MPS3 = ƒ(AOR) Linear 0.033 ± 0.006 0.74
MPS9 = ƒ(SE) Linear 0.337 ± 0.16 0.74 1 8.0 Jamming 4.0 Jamming
AIF9 = ƒ(SE) Polynomial,2 −34.9 ± 7.2 0.80 2 8.3 Rathole 4.1 Rathole
[6.52] [± 1.3] 3 4.3 Jamming 2.1 Jamming
FF3 = ƒ(CPS) Linear −0.895 ± 0.16 0.74 4 6.8 Jamming 3.4 Jamming
UYS3 = ƒ(C3) Linear 2.7 ± 0.1 0.98 5 30 21 15 4.7
FF3 = ƒ(C3) Linear −14 ±3 0.74 6 11 11 5.7 2.8
UYS9 = ƒ(UYS3) Linear 1.3 ± 0.3 0.70 7 11 Jamming 5.3 Jamming
UYS9 = ƒ(C9) Linear 2.5 ± 0.2 0.96 8 11 12 5.7 2.4
FF9 = ƒ(UYS9) Linear −6.8 ±1 0.82 9 15 12 7.6 4.4
FF9 = ƒ(C9) Linear −20 ±3 0.81 10 14 11 7.2 2.6
CBD = ƒ(MPS9) Linear −0.502 ± 0.096 0.72 11 12 11 6.2 Jamming

409
L. Marchetti and C. Hulme-Smith
(sample 5) is always able to flow through the funnels (table). This is op-
posite from what found from Janda et al. [74], where bulk solids jam
when their particle size is too coarse in relationship to the funnel orifice.
While in this case the interlocking mechanisms, affecting coarser parti-
cles, can explain the jamming, in our work the fractions that are finer in
relationship to the funnel diameter are more prone to the jamming phe-
nomenon due to their higher cohesive forces. This can be seen very
clearly with sample 11, where the same powder was able to flow
through the Hall funnel, but not through the Carney funnel. Our findings
agree with other results in the literature [75]. With less data available,
any outlier can have a significant impact on any data trend observed
for the flow rate trials. This can explain why flow rate shows little corre-
lation with other variables (Figs. 10–12 in the Supplementary file).
Basic flowability energy measures flowability dynamically in pow-
ders confined under a compressive load. These conditions are unique
amongst the techniques used in the current study and it explains why
basic flowability energy shows no correlations with other parameters
(Figs. 5–6 and Figs. 5–6 in the Supplementary file). This suggests that
powders subjected to a dynamic flow and confined under the blade
stress behave very differently than other cases and highlights the need
to test flowability under conditions that are representative of the pro-
cess for which the powders are intended.
In our study the conditioned bulk density was found to be clearly con-
nected with multiple flowability metrics (Figs. 6,8 and Fig. 7 in the Sup-
plementary file), but a weak correlation between conditioned bulk
density and basic flowability energy (Fig. 6 in the Supplementary file).
The correlation between flowability and powder density in generally
known in the literature: Santomaso et al. brings evidence of a correla-
tion between the density ratios and the angle of repose [54], while Ab-
dullah and Geldart find an important contribution of the particle shape
distribution to both bulk density and flowability for fluid-cracking cata-
lyst and fire-retardant filler powders [76]. Hou and Sun note that higher
particle density corresponds to a better flow behaviour for pharmaceu-
tical powders tested with a powder shear cell [77]. The reason to this
could be that in many flowability testing techniques, only mild forces
are applied to the powder, limiting the influence of mechanisms such
as mechanical friction, or the propagation of forces through particle
interlocking. These mechanisms are more pronounced when stronger
forces are applied to the powder and with an increased particle packing.
For this reason, in flow tests with cohesive powders, weaker forces be-
tween neighbouring particles may predominate. Similarly, these
weaker forces are important when determining the conditioned bulk
density of these powders. Conversely, when a stress is applied to the
powder, the mechanical friction and interlocking are more important,
and the flow is therefore determined by other powder properties. This
could explain why the basic flowability energy does not correlated with
the conditioned bulk density (Fig. 6 in the Supplementary file).
Specific energy, Hausner ratio, compressibility, and angle of repose
(Fig. 6 and Figs. 7–11 in the Supplementary file) seem to be strongly re-
lated and are all correlated to the conditioned bulk density, suggesting
that the effect of weak cohesive forces is limiting in these flowability
tests. However, there is variation between these flowability indicators.
From the current data, specific energy and Hausner ratio are more corre-
lated to each other than to other metrics (Fig. 8 in the Supplementary
file) and with the major principal stress (Table 3 and Fig. 8). The correla-
tion observed between Hausner ratio and angle of repose agrees with
what was found from Riley and Mann for glass particles of different
shapes [78]. Similarly, Geldart et al. found a clear correlation between
the angle of repose and the Hausner ratio for different non-metallic
powders [35]. The reason may be that Hausner ratio considers both
weak cohesive forces and the rearrangement of particles, as powders
are shaken in the tapped density measurement. It is reasonable that
both these phenomena are also affecting the specific energy and major
principal stress measurements, where the powder resistance to an ap-
plied stress is recorded under conditions of low stress. Similarly, during
the angle of repose measurement powders are forced to fall from a
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Powder Technology 384 (2021) 402–413
funnel and come to rest in a pile: the cohesive and frictional forces act
to oppose a motion that is imposed on the powder, which are partly
allowed to rearrange (Fig. 10 in the Supplementary file). Conversely,
in the compressibility test, powders are slowly compressed up to a pre-
set stress, overcoming weak cohesive forces. However, the pre-set low
level of stress and the single action movement prevent powders to rear-
range with a higher packing fraction. For this reason, this test does not
correlate well with other metrics, such as Hausner ratio, for all the pow-
ders measured (Fig. 9 in the Supplementary file). Instead, compressibility
correlates with cohesion and ultimate yield strength, where the powder
resistance to flow is driven by weak applied forces and in static condi-
tions (Table 3 and Fig. 8). In these tests, the mechanism of particle rear-
rangement is inhibited, allowing results to be compared to the
compressibility test. Zegzulka et al. found that flow function coefficient,
angle of internal friction and angle of repose vary all similarly across dif-
ferent metallic powders, and the particle shape has a prominent effect
on their flowability. This result is somewhat different from what we
found in our study, but it highlights the existence of a similar trend be-
tween the angle of repose and some rheometry variable [79].
In the stability and variable flow rate test, specific energy is mostly de-
termined by interactions due to attractive forces between particles, such
as electrostatic forces or polar attractions due to the presence of water.
Since these forces generally weak, the inertia of the powder due to the
work done by the impeller strongly affects the results. For this reason,
specific energy is normalized by the sample mass (hence the use of the
word “specific” in the name of the metric). However, the current data
still shown a strong and statistically significant correlation between
the specific energy and the conditioned bulk density. While normalizing
the force recorded from the impeller for the sample mass removes the
effect of different powder densities, it is also true that the conditioned
bulk density, as well as the specific energy, can be an indicator of the at-
tractive forces between particles in the powder (Fig. 6).
4.5. Testing strategy
Flow rate metrics proved unsuitable to evaluate flowability with our
samples. For this reason, in disagreement with current standards [26],
these metrics are not recommended to measure flowability for cohesive
steel powders.
Many single metrics proved to offer meaningful results, however not
always in agreement. For example, when evaluating flowability,
Hausner ratio, specific energy, and angle of repose showed an agreement.
However, a funnel flow device to measure angle of repose like the one
used in this study is not indicated with cohesive powders as the results
reading heavily relies on the operator as the funnel could get blocked
with cohesive powders. Compressibility behaves similarly but
underestimating the effect due to particle rearrangement compared to
Hausner ratio and specific energy. Conversely, basic flowability energy
gives unique results, strongly enhancing the effect of frictional mecha-
nisms and particle interlocking. Flowability results that, similarly to
our case, are not in agreement were found also from Mellin et al.
when comparing the Basic flowability energy and the specific energy
with the Hall and Gustavsson flow rates [80]. These differences suggest
that when powder flowability is needed to be evaluated comprehen-
sively, a multiple tests strategy is needed, in agreement with similar
considerations made from Leturia et al. [6] and Prescott [17]. For exam-
ple, basic flowability energy, compressibility and one metric between
Hausner ratio andspecific energy can measure the flow behaviour in dif-
ferent conditions. Instead, when the flow characterisation is needed for
a specific application, it is recommended to select a flow test that can
replicate adequately the powder condition. However, Ghadiri et al. [7]
observe that this could not always be possible, as when evaluating the
spreading of powders for additive manufacturing.
Shear cell testing records accurately the powder stress state and can
offers several metrics to evaluate flowability. The major principal stress
was found correlated to other metrics (Hausner ratio, specific energy,
L. Marchetti and C. Hulme-Smith
and angle of repose), while cohesion and ultimate yield strength were
found linked to the compressibility (Table 3 and Fig. 8). This means
that it is possible to reliably express all the shear cell metrics with
other metrics (and vice-versa) for the powders in our possession. How-
ever, as it was experienced that all shear cell metrics are sensitive to in-
terferences, including a correct sample preparation, these values can be
reliably obtained from other metrics (Hausner ratio, specific energy,
angle of repose, compressibility), as shown in Table 3 and Fig. 8.
5. Conclusions
• A testing strategy using multiple techniques is necessary when
characterising the flow behaviour of a powder in a comprehensive
way: different metrics depend on different properties of the powder
and, so, give different results. Basic flowability energy, compressibility
and at least one of Hausner ratio and specific energy revealed to repre-
sent different aspects of the flow behaviour of cohesive steel powders.
• Hall and Carney flow rate methods were found not suitable for
assessing the flowability for cohesive steel powders. The funnel
method is not suitable for the cohesive powders because the jamming
does not allow to record a flow rate, useful to compare different pow-
ders. For this reason, it is not possible to determine any significant and
representative correlations between either Hall or Carney flow rate
and any other flowability metric.
• The conditioned bulk density (CBD) showed a strong correlation with
most metrics. Many of these correlations were found to be statistically
significant, while 2 (CBD with Hausner ratio (HR) and major principal
stress with pre-compaction at 9 kPa (MPS9), Eq. (13) and (14) were
also found to be representative of the data.


CBD ¼ −ð5:65  0:9Þ∙HR R2adj ¼ 0:81 ð13Þ
 023.

CBD ¼ −ð0:502  0:22Þ∙MPS9 R2adj ¼ 0:72 ð14Þ
• The basic flowability energy (BFE) showed a weak correlation with
most flowability metrics, consistent with the fact that powders were
confined and compressed during testing. It is reasonable that this
stress state heavily promoted mechanical interlocking and inter-
particle mechanical friction.
• Specific energy (SE), Hausner ratio (HR), compressibility (CPS) and
angle of repose (AOR) were found to be inter-correlated. Specific en-
ergy, Hausner ratio and angle of repose were found to behave very sim-
ilarly and the results from Hausner ratio and angle of repose, being
statistically significant and representative of the data, can be reliably
converted between them (Eq. (15)). Compressibility was found to
lead to some different results, probably because the test conditions
lead to underestimate the effect of particle rearrangement compared
to other techniques.
 [10] J. Clayton, Optimising metal powders for additive manufacturing, Metal Powder

SE ¼ ð0:083  0:03Þ∙AOR R2adj ¼ 0:78 ð15Þ
• Other metrics were found strongly correlated. For example, the major
principal stress (MPS) was found to be more correlated to Hausner
ratio, specific energy, and angle of repose. Conversely, cohesion and ulti-
mate yield strength were found to be more strongly correlated to com-
pressibility and angle of repose (Table 3). This means that is possible to
reliably express all the shear cell metrics with other metrics (and vice-
versa) for the powders in our possession, making the shear cell test
flexible in representing different flow behaviours.
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Powder Technology 384 (2021) 402–413
6. Future work
In this work, we focused on the comparison between several
flowability testing methods. However, this will be completed when
we will establish a procedure to characterise the spreadability of steel
powders. In addition, the influence of some relevant powder properties
on flowability should be determined. For example, the effects of the par-
ticle size distribution, morphology, and environmental moisture. Fi-
nally, is could be useful to expand this work to a wider range of
powder chemistries, such as titanium or aluminium alloys and non-
metal powders.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influ-
ence the work reported in this paper.
Acknowledgments
This work was made possible by financial support from the Swedish
Governmental Agency for Innovation Systems (Vinnova), project num-
ber 2019-01087.
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://doi.
org/10.1016/j.powtec.2021.01.074.
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