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Evaluation of essential powder properties through complementary particle

size analysis methods for laser powder bed fusion of polymers

Article  in  Procedia CIRP · September 2020

DOI: 10.1016/j.procir.2020.09.023

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 Available online at www.sciencedirect.com
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11th CIRP Conference on Photonic Technologies [LANE 2020] on September 7-10, 2020
11th CIRP Conference on Photonic Technologies [LANE 2020] on September 7-10, 2020
Evaluation of essential powder properties through complementary particle
Evaluation of essential
size analysis CIRPpowder
28thmethods Design properties
forConference,
laser powder Maythrough bed
2018, complementary
fusion
Nantes, France of polymers particle
size analysis methods for laser powder bed fusion of polymers
A new methodology
A. Sommereynsa,b, to*,analyze
T. Hupfeldthe c
, B.functional and physical
Gökcec, S. Barcikowski c
architecture
, M. Schmidt a,b
of
a,b, c c c a,b
existing
a
products
Institute ofA. Sommereyns
Photonic
b
for
Technologies (LPT),an T.assembly
Hupfeld , B.oriented
*,Friedrich-Alexander-Universität
Gökce , S.product
Barcikowski
Erlangen-Nürnberg, family, M.
Konrad-Zuse-Str. identification
3-5,Schmidt
91052 Erlangen, Germany
a
Erlangen Graduate School in Advanced Optical Technologies (SAOT), Paul Gordan Straße 6, 91052 Erlangen, Germany
c InstituteChemistry
Technical of Photonic Technologies
I and Center for (LPT), Friedrich-Alexander-Universität
Nanointegration Erlangen-Nürnberg,
Duisburg-Essen (CENIDE), Konrad-Zuse-Str.
University of Duisburg-Essen, 3-5, 91052 Erlangen,
Universitaetsstrasse Germany
7, 45141 Essen,
c
b
Paul Stief *, Jean-Yves Dantan, Alain Etienne, Ali Siadat
Erlangen Graduate School in Advanced Optical Technologies
Germany(SAOT), Paul Gordan Straße 6, 91052 Erlangen, Germany
Technical Chemistry I and Center for Nanointegration Duisburg-Essen (CENIDE), University of Duisburg-Essen, Universitaetsstrasse 7, 45141 Essen,
* Corresponding
Écoleauthor. Tel.:Supérieure
Nationale +49-913-185-64102; fax: +49-913-185-23234.
d’Arts et Métiers, E-mail address:
Germany
Arts et Métiers ParisTech, LCFC [email protected]
4495, 4 Rue Augustin Fresnel, Metz 57078, France
* Corresponding author. Tel.: +49-913-185-64102; fax: +49-913-185-23234. E-mail address: [email protected]
* Corresponding author. Tel.: +33 3 87 37 54 30; E-mail address: [email protected]
Abstract
Abstract
The resolution of complex parts produced by laser powder bed fusion of polymers (PBF-LB/P) is defined significantly by the shape and size
Abstract
distribution of the feedstock powder. Its analysis is usually performed by optical measurement systems such as laser diffraction or image
The resolution of complex parts produced by laser powder bed fusion of polymers (PBF-LB/P) is defined significantly by the shape and size
analysis. In this study, the most relevant particle size parameters will be extracted from a set of different measuring methods, as well as the
Indistribution
today’s ratio
Hausner
of the environment,
business feedstock powder.
and finally discussed
Its towards
trend analysis more
the regarding is usually
product
safe and successful
performed
variety by optical
and measurement
customization
processability. Extracted isdata
systems such
unbroken.
include Due
as laser
to this diffraction
development,
the sphericity, theorvolume-
fine fraction,
image
need of
analysis.
agile and In this study, the
reconfigurable most relevant
production systemsparticle
emergedsizetoparameters
cope with will be extracted
various products from
and a set offamilies.
product differentTo measuring
design methods,
and optimizeas production
well as the
and number-weighted diameter distributions, and statistical significance analysis, including comparison of PA12 and carbon-black-additivated
Hausnerasratio
systems and finally discussed regarding safematches,
and successful processability. Extracted data include the sphericity, fine fraction, volume-
PA12. Thewell as to
presented choose
resultsthe optimal
should giveproduct
researchers product
a first analysis
impression methods
about are needed.
the suitability of Indeed,
polymermost of thefor
powders known methods
PBF-LB/P, aim on
based to
and number-weighted
analyze a product or one diameter
product distributions,
family on the and statistical
physical level. significance
Different analysis,
product including
families, comparison
however, may of PA12
differ largelyand
in carbon-black-additivated
terms of the number and
powder feedstock characterization.
PA12.ofThe
nature presented This
components. results should
fact impedesgiveanresearchers a first impression
efficient comparison and choiceaboutof the suitabilityproduct
appropriate of polymer
familypowders for PBF-LB/P,
combinations based on
for the production
powder feedstock characterization.
system. A new methodology is proposed to analyze existing products in view of their functional and physical architecture. The aim is to cluster
© 2020 The Authors. Published by Elsevier B.V.
these
© products
2020 The in new assembly
Authors. oriented product
B.V.families license
for the optimization of existing assembly lines and the creation of future reconfigurable
This is an open accessPublished by Elsevier
article under the CC BY-NC-ND (http://creativecommons.org/licenses/by-nc-nd/4.0/)
© 2020
assembly
This The Authors.
systems. BasedPublished
on Datumby Elsevier
Flow B.V.
Chain, the physical structure of the products is analyzed. Functional subassemblies are identified, and
Peer is an open
review access article
statement: under the
Peer-review CCresponsibility
under BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/)
of the Bayerisches Laserzentrum GmbH
This is an open
aPeer-review
functional access
analysis
under is article under
performed.
responsibility the Bayerisches
CC BY-NC-ND
ofMoreover,
the a hybrid license (http://creativecommons.org/licenses/by-nc-nd/4.0/)
functional
Laserzentrum and physical architecture graph (HyFPAG) is the output which depicts the
GmbH
Peer review
similarity statement: Peer-review under responsibility ofsupport
the Bayerisches Laserzentrum GmbH
Keywords:between product
polymer powders; families
laser beamby providing
melting; designparticle
PBF-LB/P; sizeto both, production
distribution; system
flowability; image planners and diffraction,
analysis; laser product designers. An sintering
selective laser illustrative
example of a nail-clipper is used to explain the proposed methodology. An industrial case study on two product families of steering columns of
Keywords: polymer
thyssenkrupp Prestapowders;
France islaser beam
then melting;
carried out PBF-LB/P; particle
to give a first size distribution;
industrial evaluation flowability; image analysis;
of the proposed laser diffraction, selective laser sintering
approach.
© 2017 The Authors. Published by Elsevier B.V.
Peer-review
1. Introductionunder responsibility of the scientific committee of the 28th CIRP theDesign Conference
cumulative 2018.
volume-weighted size distribution (Q ). In this
3

1. Introduction arrangement,
the cumulativelarger particles havesize
volume-weighted a more significant
distribution (Q3). impact
In this
Keywords: Assembly; Design method; Family identification
The ability to create fine structures and precise geometries on
arrangement, larger particles have a more significant aimpact
the distribution than small ones [9]. However, high
with a resolution close to the feedstock powder
The ability to create fine structures and precise geometries particle sizes amount of finer particles increases the
on the distribution than small ones [9]. However, a high cohesion among the
is one of the advantages of laser powder
with a resolution close to the feedstock powder particle sizes bed fusion of powder particles [6,10], which impairs the
amount of finer particles increases the cohesion among the powder flowability
1.polymers
one of (PBF-LB/P)
isIntroduction the advantages [1,2]. Through
of laser a layer
powder by layer
bed fusion and
of of thethus
powder the powder
product
particles range and
[6,10], application during
characteristics
which impairs PBF-LB/P
manufactured
the [11–13].
and/or
powder flowability
principle, three-dimensional structures can
polymers (PBF-LB/P) [1,2]. Through a layer by layer assembledbe created without Consequently,
and thus the in this the cumulative
system.
powder number-weighted
In this context,
application duringthe particle
main challenge
PBF-LB/P size
[11–13]. in
the need of subtractive
Due tothree-dimensional
principle, machining
the fast development [3].
structures canin beBesides
thecreated important
domain withoutof distribution
modelling
Consequently, (Q ) needs
and 0analysis to be addressed
is now number-weighted
the cumulative as well, where
not only to cope particle every
with singlesize
thermal
the needandofoptical
communication and material
an ongoing
subtractive properties,
machining trend the
[3]. particle
ofBesides
digitizationshape and
important particle
and products, isa limited
distribution equally
(Q0) needs weighted
product relative
range
to be to as
or existing
addressed thewell,
totalwhere
product number
families,
everyof
its distribution
digitalization,
thermal and optical affects the
manufacturing powder
material properties, processability,
enterprises the are particle specifically
facing important
shape and but particles [14,15].
also toisbeequally
particle able to weighted
analyze and to compare
relative to theproducts to define
total number of
the recoating
challenges
its distribution process
in today’s
affects theduring
market
powderpowder application,
environments:
processability, and thus new
a specifically
continuing Being
product
particles able to evaluate
families.
[14,15]. It can besmall particles
observed also allows
that classical existingthe
influence
tendency
the recoating the quality
towards process and
reduction performance
of product
during of the produced
powderdevelopment
application, and parts
times and examination
thus product
Being ableof are
families particle
to sizessmall
regrouped
evaluate smaller
in functionthan 10also
µm,or
of clients
particles which
features.
allows are
the
[4–8].
shortened
influence product lifecycles.
the quality In addition, of
and performance there
theisproduced
an increasing inhalable
parts However,
examination and thus
assembly can
oriented
of particle affect the
product
sizes circulatory
families
smaller than 10 system
areµm,
hardly of heart
to find.
which are
As a of
demand
[4–8]. first estimation ofbeing
customization, the provided powder
at the same timequality (VDI
in a global and
Onlungs of thus
the product
inhalable and thefamily
human
can body
level,
affect [16–19].
products
the However,
differ
circulatory mainlyofinround
system two
heart
3405As Part
competition 1.1),
a firstwith datasheets
competitors
estimation of all
of the powder manufacturer
over the
provided Thistypically
world.quality
powder trend,
(VDI mainparticles canofbe the
and characteristics:
lungs morehuman
(i)easily removed
the number ofby alveolar
components
body [16–19]. macrophages
and (ii)
However, the
round
provide
which
3405 Part the quantile
is inducing particle diameters
the development
1.1), datasheets of powder from x , x
10,3 macro
manufacturer
50,3, and x
totypically
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90,3 of through
type phagocytosis
of components
particles can be more (e.g.than fibrous
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by alveolarelectronical).
macrophages
markets,
provide the results in diminished
quantile lot sizesx10,3
particle diameters due, xto50,3,augmenting
and x90,3 of Classical
through methodologies
phagocytosis than considering mainlywhich
fibrous particles singleexhibit
products an
product varieties (high-volume to low-volume production) [1]. or solitary, already existing product families analyze the
2212-8271 © 2020 The Authors. Published by Elsevier B.V.
To
Thiscope
is an with this augmenting
open access article under thevariety as welllicense
CC BY-NC-ND as to(http://creativecommons.org/licenses/by-nc-nd/4.0/)
be able to product structure on a physical level (components level) which
2212-8271
identify © 2020
possible The Authors. Published
optimization by Elsevier
potentials B.V.
in the existing
Peer review statement: Peer-review under responsibility of the Bayerisches Laserzentrum causesGmbH difficulties regarding an efficient definition and
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/)
production system, it is important to have a precise knowledge comparison of different product families. Addressing this
Peer review statement: Peer-review under responsibility of the Bayerisches Laserzentrum GmbH
2212-8271 © 2020 The Authors. Published by Elsevier B.V.
This is an©open
2212-8271 2017access article Published
The Authors. under theby CC BY-NC-ND
Elsevier B.V. license (http://creativecommons.org/licenses/by-nc-nd/4.0/)
Peer-review
Peer-review under
under responsibility
responsibility of scientific
of the the Bayerisches Laserzentrum
committee GmbH
of the 28th CIRP Design Conference 2018.
10.1016/j.procir.2020.09.023
 A. Sommereyns et al. / Procedia CIRP 94 (2020) 116–121 117
2 A. Sommereyns / Procedia CIRP 00 (2020) 000–000

increased length in one dimension [20,21]. These conditions 2. Materials and methods
of particle size and shape also apply for polymer particles
[22,23]. Polyamide 12 powders (PA12; Evonik Vestosint 1115)
The particle morphology is not only relevant regarding were used for the particle analyses. To evaluate the effect of
human health but also important for the spreadability of the adhesion of additives on the particle morphology and size,
powder by the coater in a PBF-LB/P machine. Typically, 1 wt% Carbon Black (CB; Origin “Lamp Black”) were added
spherical or potato shapes are considered the most suitable to the surface of the PA12 powders through mechanical
forms for PBF-LB/P powders due to their achievable high mixing (milling with 50 g steel balls at a rotation speed of
powder density and good flowability [6,14,24–28]. Up to now, 60 rpm for 2 h).
there is still a lack of measuring systems to accurately Automated analyses via static laser diffraction were
examine the spreadability of PBF-LB/P powders in such a conducted in air and in a wet state (Sympatec HELOS
way to emulate the recoating mechanisms under realistic equipped with RODOS and SUCELL), based on 𝑥𝑥���� . In the
process conditions [12,29]. Currently, most instruments rely wet state, 20 mg of polymer particles were dispersed in water
on measuring the flowability of loose powders at room by ultrasonic treatment. In air, the analysis required at least
temperature (e.g. angle of repose, powder rheometer, 200 g of powder for measurements. The range of detectable
revolution powder analyzer, bulk and tapped volume particles was between 0.5/0.9 µm and 175 µm.
[6,12,30]). Despite its simplicity, one of the most commonly For the dynamic image analysis, a few grams of PA12
used technique is the empirical calculation of a flow index via powder, which corresponds to approximately 500,000
the Hausner ratio 𝐻𝐻� . The main advantages are the fast detectable particles, were analyzed via the Camsizer X2 with
procedure and its high reproducibility for thermoplastic compressed air of 50 kPa through the X-Jet extension to get
powders even among different work spaces and operators rid of possible agglomerations. The range of detection went
[6,31,32]. Modified annular ring shear cells, which can from 0.8 µm to 8 mm. The system allowed the simultaneous
determine the flowability under high temperatures, show the measurement of number- and volume-weighted particle size
potential to replace the Hausner ratio measurement [33–35]. distributions using a two-camera system. Respectively, the
However, ring shear test measurements are more time particle diameter 𝑥𝑥���� and the longest Feret diameter 𝑥𝑥�� ���
consuming and the powder is not recyclable afterwards due to have been recorded for comparison between the different
thermal aging. The spreading process of the ring shear cell particle analysis methods. The sphericity (ISO 9276-6) was
still doesn’t replicate the recoating process of PBF-LB/P, but calculated by using volume-weighted data and was based on
comes closer to it than any other method so far. the measurements of 𝑥𝑥���� .
Frequently used methods for particle analysis are laser Approximately 1000 PA12 powder particles were analyzed
diffraction measurements (ISO 8130-13) [36–40] as well as by light microscopy at 20-fold magnification (one pixel
static (ISO 13322-1) [41–45] and dynamic image analysis corresponds to 0.33 µm) by applying a single powder layer on
(ISO 13322-2) [45–48]. Depending on the utilized particle a microscope slide. The ImageJ plugin ParticleSizer [50,51]
size analysis method, the obtained results may show large has been used for the semi-automatized particle size (𝑥𝑥�� ��� )
discrepancies due to different physical measuring principles measurements and all images were checked manually on
and mathematical calculations [49]. misinterpretation of agglomerated particles.
Among the vast amount of available particle analysis SEM images were taken after applying a powder layer on
techniques, this study aims to provide an overview of the an adhesive carbon tape and removing loose powder particles.
effect of different measuring principles on the results of A 3 nm layer of platinum was sputtered on the powder layer.
examined powder particles and which parameters are Images (one pixel corresponds to 9.93 µm) of about 100
important for a first assessment of the suitability of polymer PA12 powder particles were analyzed manually ( 𝑥𝑥�� ��� ),
powders for PBF-LB/P. since the contrast was not suitable for automated analysis.
In order to get an impression of the general flowability of
Nomenclature the powder, the Hausner ratio 𝐻𝐻� was measured according to
VDI 3405 Part 1.1 with a 100 mL plastic measuring cylinder.
CB carbon black The procedure was repeated five times for the same powder
LM light microscopy for statistical analysis. For maintaining the same prerequisites,
PA12 polyamide 12 the powders have been analyzed as received within a short
PBF-LB/P laser powder bed fusion of polymers time span by the same operator.
Q0/3 cumulative particle distribution, weighted by For the statistical evaluation of available datasets, analyses
number (0) or volume (3) of particles of significance (𝑝𝑝 ≤ 0.05) have been conducted.
rpm rounds per minute
SEM scanning electron microscopy
𝑥𝑥���� particle diameter calculated by the area of a
particle, assuming a spherical shape
𝑥𝑥�� ��� longest Feret diameter of a particle
118 A. Sommereyns et al. / Procedia CIRP 94 (2020) 116–121
A. Sommereyns / Procedia CIRP 00 (2020) 000–000 3

3. Results and discussion Meanwhile, laser diffraction measurements in air result in an

x50,3 of 58 µm and an x90,3 of 89 µm. Surprisingly,
When considering a typical powder layer in PBF-LB/P of measurements in water deliver larger particle sizes with an
100 µm, firstly, the median value (x50,3) should be represented x50,3 of 61 µm and an x90,3 of 108 µm, even though particles
by at least two particles [52]. Assuming perfectly spherical were dispersed in water by ultrasound. The particles seem to
particles, an x50,3 value of around 50 – 59 µm should be ideal be less dispersed in water than in air due to a possible lack of
considering stacking two particles on each other (worst case) wetting of smaller particles, resulting in agglomerations.
and an optimal dense powder layer (best case) in z-direction Measurements in Ethanol instead of water could improve the
of the powder bed (Fig. 1). The radius of the best case was accuracy of the results. Only the Camsizer and laser
calculated by (1): diffraction measurements in air would declare the analyzed
powder as suitable for PBF-LB/P, when considering the
2𝑟𝑟 + 𝑠𝑠𝑠𝑠𝑠𝑠 45° ∙ 2𝑟𝑟 = 100 µm (1) aforementioned two criteria. While there is a certain
agreement at x50,3, the cumulative distribution curve measured
Secondly, at least 90 % of the particles (x90,3) should with dynamic image analysis has a steeper slope than the one
measure less than 100 µm in size to ensure that one particle of static laser diffraction (Fig. 2 a, c), which increases the
doesn’t exceed the typical layer height and thus parts with total range of measured particle sizes with static laser
lower accuracy and resolution are produced [6]. diffraction.
The cumulative distribution curves of each method show
overall similar characteristics in their slope and course. A
closer look reveals that the dynamic image analysis seems to
measure a higher amount of smaller particles than the laser
diffraction and the microscopic methods below 5 % due to
their different measuring principles (Fig. 2 b, c).
Fig. 1. A layer of 100 µm, achieved by (a) stacking two 50 µm particles onto Furthermore, the curves of 𝑥𝑥���� and 𝑥𝑥�� ��� of the
each other and (b) by close-packing of equal spheres, but with larger dynamic image analysis match below 32 µm, providing useful
diameter; displayed as two-dimensional images. data on the ratio of length to width of the powder particles. An
overlap of 𝑥𝑥���� and 𝑥𝑥�� ��� data would refer to spherical
For all particle measurements it is important to know particles, while larger 𝑥𝑥�� ��� values would indicate irregular,
which kind of particle diameter they are based on. The elongated shapes. In our study, this becomes especially
differences between particle diameters measured by laser apparent for particles > 32 µm, where 𝑥𝑥�� ��� displays an up
diffraction and image analysis can be clearly distinguished for to 13 µm shift to higher values than 𝑥𝑥���� . This difference
PA12 in Fig. 2 a. indicates the potato-shape of the PA12 powders over 32 µm,
Despite the wider availability of static image analysis while smaller particles have a more spherical character.
systems, the amount of analyzable particles is much smaller Analyzing both 𝑥𝑥���� and 𝑥𝑥�� ��� can be useful to estimate
than with dynamic image analysis and thus comes with the overall shape of the particles, depending on how well the
weaker statistics. LM and SEM would declare the analyzed 𝑥𝑥���� and 𝑥𝑥�� ��� values coincide.
powder as suitable for PBF-LB/P when considering only the
second criterion, as they show an x50,3 value of 72 µm with 100
x90,3
LM and 74 µm with SEM, while their x90,3 values are at a)
92 µm. Accordingly, dynamic image analysis of 𝑥𝑥�� ��� 80 PA12 Vestosint
Laser diffraction dry (xarea)
display an x50,3 value of 67 µm and an x90,3 value of 91 µm. Laser difftraction wet (xarea)
60
SEM, LM and Camsizer measurements coincide, among a x50,3
Camsizer (xarea)
few outliers, at the important particle quantiles. The 40 Light microscopy (xFe max)
overestimation of certain particle sizes can be explained by SEM (xFe max)
Camsizer (xFe max)
existing agglomerated particles, which cannot be completely 20
x10,3
avoided in the microscopic setups. Especially small polymer
particles below 40 µm are underestimated due to
Q3 / %

0
0 50 100 150 200
agglomeration and adhesion on larger particles. Nevertheless,
b) c)
the relatively large overlap between the results of the 8 8

automatic dynamic image analysis and the microscopic

methods proves that the manual or semi-automatized 4 4

measurement is feasible to represent our powder batch. 0 0

However, determining only the Feret diameter would not be 0 20 40 0 20 40

sufficient to define the shape of particles, since it only depicts Particle diameter / µm
one size.
Automatic analysis methods (dynamic image analysis and Fig. 2. Comparison of PA12 Vestosint 1115 between the different particle
diameters (Q3) through various methodologies with (a) the complete particle
laser diffraction), which base their calculations of particle size distribution of every method and their values below x10,3 (b) for 𝑥𝑥�� ���
sizes on 𝑥𝑥���� can examine higher amounts of powder in a and (c) for 𝑥𝑥���� .
short time, leading to better statistics. In this regard, Camsizer
measurements exhibit an x50,3 of 59 µm and an x90,3 of 77 µm.
 A. Sommereyns et al. / Procedia CIRP 94 (2020) 116–121 119
4 A. Sommereyns / Procedia CIRP 00 (2020) 000–000

In order to avoid misinterpretations, the particles must On the other hand, when considering the number-weighted
have a chance to deagglomerate during the analyzing process. distribution, 94 % of PA12 particles and 95 % of
Applying a powder layer on a microscopic slide or letting PA12 + 1 wt% CB particles are smaller than 10 µm (Fig. 3 a).
particles fall down a shaft by gravity are not suitable At the same time, the values of PA12 significantly decrease
approaches to adequately represent the distribution of for x10,0 from 2.45 ± 0.10 to 2.10 ± 0.06, for x50,0 from
powders for PBF-LB/P. Analysis methods which base their 4.28 ± 0.05 to 3.80 ± 0.06 and for x90,0 from 8.15 ± 0.19 to
calculations on 𝑥𝑥���� should be used preferably as first 7.57 ± 0.15 due to the additivation process of CB through
estimation. This diameter depicts particles as close to a sphere mechanical forces during milling (Fig. 4 a). The sphericity
as possible, including their length and width, while others below 10 µm for PA12 is between 0.82 and 0.91, while it lies
measure only one size [53]. This way, particles with different between 0.79 and 0.89 for PA12 + 1 wt% CB. These values
morphologies can be compared more easily with a perfect correlate to ellipsoidal particles that can be removed from the
sphere, which is an optimal geometrical shape for PBF-LB/P respiratory system by alveolar macrophages [22,23].
[5,13,54]. Even when the particle diameter is the same by Next to this, the average sphericity of particles represents
definition, each method uses its own mathematical an important parameter for the spreadability in PBF-LB/P.
calculations and assumptions based on different physical The values should be between 0.79 (potato shape) and 0.99
processes. Despite similar tendencies and characteristics, (spherical shape) [57,58], while a perfect sphericity of 1 can
results of different particle size analysis methods can have hardly be achieved during powder manufacturing. This
significant differences, even when the same methodology has parameter becomes especially relevant if the good flowability
been applied. of already optimally shaped particles has to be maintained by
Accordingly, further investigations of important particle adhesion of additives to their surface. In our study, the
parameters were carried out for this study with dynamic particles retained their average sphericity of 0.80 by adding
image analysis (Camsizer X2) and repeated three times for 1 wt% of CB onto the PA12 particles.
statistical analysis. The relevant findings can be transferred to The particle size evaluations on a microscopic level may
other methods analogously. also macroscopically affect the powder spreadability during
To understand how many fine particles (< 10µm) are the recoating process. When combining the resulting data of
within the powder batch, the typically displayed x10,3 values Q0 with the 𝐻𝐻� , it becomes apparent that the ball milling
don’t give conclusive results due to the overall particle process reduces the particle sizes of PA12 significantly (**;
volume outweighing individual particle sizes (Fig. 2 b, c). 𝑝𝑝 𝑝 𝑝𝑝𝑝𝑝 ) by up to 0.5 µm, increasing the 𝐻𝐻� value from
Instead, the analysis of fine particles should be done via the 1.10 ± 0.03 to 1.18 ± 0.02 (Fig. 4). This means that the
number-weighted distribution Q0. A certain amount of fine flowability worsened due to an increase in inter-particle
particles may even be useful for PBF-LB/P, as they fill the cohesion of more available smaller particles, which were
gaps between bigger particles and thus lead to denser parts formed through impact and attrition during the ball milling
[11,28,55,56]. The difference between the volume- and process. Note that Hausner ratio can only be a first indication
number-weighted distributions of the used polymer powders of flowability, but is often considered to be inappropriate to
can be seen in Fig. 3 a. predict an accurate PBF-LB/P processing behavior [12,59,60].
In this study, based on the volume-weighted distribution, Nevertheless, the overall good flowability (< 1.25) is still
only 3 % of the PA12 particle diameters are below 10 µm maintained. Smaller particles don’t per se worsen the
(Fig. 3 a). The additivation of 1 wt% CB shows a small effect flowability in such a way that they are not spreadable
on the volume-weighted particle size distribution with an anymore during the recoating process. First PBF-LB/P runs
increase of x90,3 from 74.90 ± 1.20 to 78.10 ± 1.31, while the under elevated temperatures showed that the recoating process
other quantile diameters remain within the range of the was not affected by the addition of 1 wt% CB to the PA12
standard deviations (Fig. 3 b). surface.

a) b) a) b)

Fig. 3. (a) Distribution curves depicting the difference between the Fig. 4. (a) The particle diameters (𝑥𝑥���� ) of PA12 powders based on the
cumulative number- and volume-weighted particle size distribution of PA12 number-weighted Q0 and (b) the powder flowability. The significance levels
and its additivation with 1 wt% CB, resulting in (b) averaged volume- (𝑝𝑝 𝑝 𝑝𝑝𝑝𝑝) are depicted with an asterisk (*); the higher the significant
weighted particle sizes. The significance levels (𝑝𝑝 𝑝 𝑝𝑝𝑝𝑝) are depicted with difference to the reference, the more asterisks are appointed.
an asterisk (*); a declaration of “n.s.” will be used in case of no significant
differences.
120 A. Sommereyns et al. / Procedia CIRP 94 (2020) 116–121
A. Sommereyns / Procedia CIRP 00 (2020) 000–000 5

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