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ppap.201700141

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Received: 20 July 2017
|
Revised: 25 September 2017
DOI: 10.1002/ppap.201700141
|
Accepted: 26 September 2017
FULL PAPER
Enhancing the mechanical performance of additive
manufactured polymer components using atmospheric
plasma pre-treatments
Hisham Abourayana
School of Mechanical and Materials
Engineering, University College Dublin,
Belfield, Dublin 4, Ireland
Correspondence
School of Mechanical and Materials
Engineering, University College Dublin,
Belfield, Dublin 4, Ireland.
Email: denis.dowling@ucd.ie
| Peter Dobbyn | Denis Dowling
This study evaluates the use of a barrel atmospheric plasma system for the treatment
of acrylonitrile butadiene styrene and polylactic acid polymer particles. Treatments
were carried out in a helium discharge with either oxygen or nitrogen addition.
The plasma activated polymer particles were then used to prepare filaments, which
in-turn were then used to fabricated parts by additive manufacturing. The resultant
dog bone polymer parts
exhibited up to a 22% increase
in tensile strength, compared to
parts fabricated using unactivated polymer particles. The
explanation for the increased
mechanical strength is the
enhanced activation of the
treated polymer particles, as
well as the removal of contaminations from the polymer
surface.
KEYWORDS
additive manufacturing, plasma treatment, tensile strength, water contact angle
1 | INTRODUCTION
Additive manufacturing (AM) also known as threedimensional (3D) printing, is a process where parts are
generated layer by layer.[1,2] It has increasingly been used
for advanced applications including the printing of adaptive
structures utilizing shape memory polymer and even
printing cell structures in a granular gel medium.[3,4] One
approach to AM is called fused deposition modeling
(FDM).[5] In this approach the polymer is extruded through
a nozzle that traces the part's cross sectional geometry layer
Plasma Process Polym. 2017;e1700141.
https://doi.org/10.1002/ppap.201700141
www.plasma-polymers.com
by layer.[6,7] The nozzle contains resistive heaters that
keep the polymer at a temperature just above its melting
point so that it flows easily through the nozzle and forms
the layer. The polymer hardens immediately after flowing
from the nozzle and bonds to the layer below. Once a layer
is built, the platform lowered, and the next layer is
deposited. The most commonly used polymers for AM are
acrylonitrile butadiene styrene (ABS) and polylactic acid
(PLA).[8,9]
Plasma treatments have previously been applied to
modify surface properties of polymer particles by cleaning
© 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
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ABOURAYANA
the surface, by altering crystallinity or by cross-linking and
the introduction of polar groups on the surface, without
changing the bulk composition.[10,11] This study reports the
performance of barrel atmospheric plasma system for the pretreatment of both ABS and PLA polymer particles prior to
filament formation. The effectiveness of the barrel plasmas
for the pre-treatment of powders has previously been
reported.[12,13] In this study the effect of systematically
altering the atmospheric plasma treatment conditions on the
level of polymer particle activation is investigated. The
activated particles were used in the fabrication of filaments
and the performance of these in the AM fabrication of
polymer parts was investigated. Several studies have reported
on the understanding of the mechanical behavior of parts
fabricated by AM and the development of analytical tools
and design guidelines for engineers.[14,15] To the authors
knowledge however, there have been no reports to-date which
have investigated the effect of plasma pre-treatment of
polymer particles on the mechanical properties of the AM
fabricated parts.
2 | EXPERIMENTAL SECTION
ET AL.
to two aluminium rods which act as the biased and earthed
electrodes, these are also used to rotate the plasma chamber
during treatment.
The atmospheric plasma treatment of acrylonitrile
butadiene styrene (ABS) and polylactic acid (PLA) polymer
particles was investigated. The ABS granules were obtained
from LG Chem and the PLA was supplied from Ingeo. Both
polymer types have a mean particle size in the range of 3 to
4 mm. Helium, helium/oxygen and helium/nitrogen gas
mixtures were investigated as the process gases. Their flow
rate was controlled using rotameters (Bronkhorst). To remove
the residual air, the plasma chamber was purged using helium
for 2 min at a flow rate of 10 slm, prior to plasma ignition.
2.2 | Optical emision spectroscopy (OES)
OES is widely used to obtain information on the concentration
of the species formed in the plasma.[16] In this study,spectra
from the plasma discharge were obtained in the 200–850 nm
region using an Ocean Optics USB4000 UV/VIS spectrometer. This system has a resolution of about 1.2 nm full width at
half maximum (FWHM).
2.1 | Atmospheric plasma treatment of
polymer particles
2.3 | Water contact angle measurements
(WCA)
The barrel reactor which has previously been described,[12] is
shown schematically in Figure 1. It consists of a quartz
chamber with effective treatment dimensions of 10 cm length
and 10 cm diameter. The system is driven by a 100 W high
voltage power source (Plasma Technics Inc.) operating at
20 kHz. The high voltage power source is directly connected
WCA measurements were performed using the sessile drop
method using an OCA 20 Video capture apparatus from
Dataphysics Instruments. Measurements were obtained using
deionized water droplets of volume of 0.5 µL at room
temperature.WCA measurements were obtained both immediately and at varying times after plasma treatment, in order to
FIGURE 1
Schematic diagram of the plasma barrel reactor (left) and images of the polymer particles used in this study
ABOURAYANA
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ET AL.
determine the rate of hydrophobic recovery. At least 25
measurements of contact angles for each batch (one
measurement per particle) were performed and average
values were calculated.
2.4 | X-ray photoelectron spectroscopy (XPS)
XPS analysis was carried out to investigate the surface
chemistry of polymer particles before and after plasma
treatment by using an Axis Ultra spectrometer system (Kratos
Analytical) set-up with a monochromated Al Kα X-ray
source. The measurements were obtained within 2 hrs of
plasma treatment of the polymer particles.
2.5 | Filament extrusion and three-dimensional
printing
The printing filaments used for this study were ABS and PLA.
A Filabot extrusion machine was used to produce these
filaments from both un-activated and plasma activated polymer
pellets. The pellets are manually introduced into the hopper and
heated up to approximately 220 and 180 °C for ABS and PLA
respectively. The filament produced with the diameter of 3 mm
using an appropriate die mounted with the extruder.
An Ultimaker three-dimensional printer was used to
produce the tensile test specimens with the standard
dimensions according to the ASTM D1708-13. The printing
parameters used to produce these samples are listed in Table 1.
2.6 | Tensile test
Hounsfield universal testing machine equipped with a 10 kN
load cell was used for tensile test. Load values were recorded
by QMat software. The specimens were tested at a rate of
50 mm min−1. A minimum of five measurements for each
material were used to calculate the average values of Young's
modulus, yield strength and max stress.
3 | RESULTS AND DISCUSSION
This section firstly considers the evaluation of the barrel's
effectiveness for the plasma activation of polymer particles
and then as to how this treatment influences the mechanical
performance of AM parts fabricated from the resulting
polymer filaments.
3 of 8
3.1 | Optical emission spectroscopy analysis
A qualitative overview of the plasma chemistry is obtained
from data obtained by analysing the observed line and band
emission intensities in the OES spectral range 200–850 nm.
The OES measurements were obtained with and without
polymer particles in the barrel chamber. As shown in Figure 2,
The emission spectra obtained in the absence of particles
were similar to those previously reported for this type of
discharge.[17] The second positive system of molecular
nitrogen N2 [C3Π+u − B3Π+g] are located at the wavelengths,
λ = 337, 358, and 380 nm.[18] At λ = 391 and 427 nm the
first negative system of molecular nitrogen ions N2+
[B2Σ+u − X2Σ+g] is recorded. Two lines from atomic species
are found in the near-infrared region, He I transition
3s3S1 → 2p3P0 at 706 nm and O I transition 3p5P → 3s5S0
at 777 nm.[19] While in the UV emission band, OH radicals
OH [A2Σ+ − X2Π] around 307 nm are observed.[20] The
observed emission lines from the non-helium species is
induced mainly by the back diffusion of humid air into the
plasma chamber [21].
Addition of oxygen to the helium plasma leads to the
absent of nitric oxide (NO) emission bands in the region of
200–300 nm. A probable explanation is that the quenching
effect of molecular oxygen on the helium plasma results in a
very low level of NO being formed.[22]
OES spectra obtained during polymer particle treatment
in the helium discharge did not exhibit any additional lines for
carbon species such as CN, CH, or CO species at 419, 431, and
519 nm respectively. This would indicate the absence of
significant levels of polymer etching by the discharge
(Figure 2).
To get an indication of the relative sensitivity of specific
species to plasma processing conditions, the spectral intensity
of several OES peaks were integrated. Five wavelengths were
selected for this investigation; 307 nm (OH), 337 nm (N2),
391 (N2+), 706 nm (He), and 777 nm (O). It is convenient to
normalise the entire spectrum to the intensity of the N2+ peak
at 391 nm. This allows the intensity ratios of various peaks to
be examined which can give a better insight into the generated
plasmas.[22] As shown in Figure 3, the normalised data
indicates that, addition of oxygen to the helium plasma as
expected yields an increase in the intensity of the oxygen
emission line at 777 nm, while the intensity of the other
emission lines decrease. This is partly attributable to the
reduction of electron density due to attachment to oxygen.[23]
TABLE 1 Parameters used to print Samples for tensile test
Materials
Print temp. ºC
Layer height mm
Fill density %
Print speed mm/sec
Nozzle size mm
Raft
ABS
240
0.1
100
40
0.4
No
PLA
200
0.1
100
50
0.4
No
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ABOURAYANA
ET AL.
FIGURE 4
FIGURE 2
Typical OES spectrum of He (with and without
particles in the plasma chamber), He/O2 and He/N2 plasma
In contrast addition of nitrogen to the helium plasma will have
a considerably more intense of N2 and N2+ emission lines than
either a He or a He/O2 plasma.
3.2 | Plasma treatment of polymer particles
A study was undertaken to evaluate the effect of plasma
processing conditions on ABS and PLA particle activation.
The effect of treatment time and addition of either oxygen or
nitrogen (0.02 slm) to the helium discharge (10 slm) on the
resultant water contact angle of the polymer particles were
investigated. Figure 4 shows the effect of treatment time on
the water contact angle of PLA and ABS polymer particles
after using a He only discharge. It was found that, the water
contact angle decreased with increasing treatment time. After
30 min the decrease obtained was from 120 to 65° and 95–41°
for PLA and ABS respectively.
Addition of 0.02 slm oxygen or nitrogen to the He
discharge (10 slm) were also investigated. As shown in
Figure 5, it was found that after 15 min treatment using He/O2
Effect of plasma treatment time on the water contact
angle of PLA and ABS polymers. (He flow rate 10 slm)
or He/N2 plasma that a further decrease in water contact angle
was obtained for the polymer particles compared with that
observed for the He only discharge. The higher degree of
plasma activation obtained for ABS compared with PLA may
be due to the enhanced lability of the CC bond in the
butadiene unit and the nitrile group in the acrylonitrile unit.[24]
The rate of hydrophobic recovery of the treated polymer
particles was investigated for the He plasma activated
(30 min) polymer particles, which were stored in plastic
vials and wrapped in aluminium foil to minimise surface
contamination.[25] The rate of hydrophobic recovery was
examined at intervals for up to 15 days. In the case of PLA,
the water contact angle recovered slightly from 65 to 71° at
the first day and then increased to 80° after 15 days. In
contrast the water contact angle values of ABS polymer
only increased to 55° after 15 days. This is significantly
below the 95° obtained for the untreated polymer. The
ageing of plasma treated polymer surfaces has been
described as a combination of processes including reorientation of polar functional groups at the surface layer as
governed by thermodynamics, diffusion of unpolar groups
from the sub-surface to the surface layer and the reaction of
FIGURE 5
FIGURE 3
Intensity ratios of the He, He/O2, and He/N2 plasma
species. Each spectrum is normalized to the N2+ peak at 391 nm
Water contact angle obtained after treating polymer
particles in a He, He/O2, and He/N2 plasma (He flow rate 10 slm, O2
flow rate 0.02 slm, and N2 flow rate 0.02 slm. treatment time 15 min)
ABOURAYANA
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ET AL.
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TABLE 2 C:O, C:N ratios, and C1s components on ABS polymer particles surface before and after plasma treatment
C1s Components %
C:O
C:N
C-H/C-C
C-O-C
-C=O
O-C=O
Before treatment
33.4
24.5
83.1
7.9
6.7
2.3
He plasma
7.5
21.9
80.2
11.2
7.3
1.3
He/O2 plasma
6.7
18.1
73.1
7.5
10.5
8.9
He/N2 plasma
6.6
12.2
75.2
11.1
5.7
5.3
free radicals at the surface.[26] Thus, metastable polar
species are removed during aging.
3.3 | X-Ray photoelectron spectroscopy
analysis
To evaluate the influence of the plasma treatment on surface
chemistry, XPS analysis was performed on the ABS particles.
This analysis was obtained before and after treatment with a
He, He/O2 and He/N2 plasmas. The elemental composition of
carbon, oxygen, and nitrogen determined from these spectra is
tabulated in Table 2. The surface of ABS polymers is mainly
composed elementally of carbon and a small amount of
oxygen and nitrogen. It is evident that the plasma treatment
produces a notable reduction in the carbon contents and an
increase in the ratio of oxygen and nitrogen atoms on the
polymer surfaces. The C 1s spectrum revealed the significant
change in the polar species percentages on polymer surfaces
after plasma treatment. It was observed that; a decrease of
concentration occurs for C─C/C─H bonds (285 eV) after
treatment with a He, He/O2 and He/N2 plasmas. For particles
treated with He/O2 plasma there is an increase in the
concentration of −CO carbonyl groups (287.6 eV) and
CO carbonyl or amid group (288.1 eV). In contrast using
He/N2 leads to create a new species correspond to imide or
urethane group N─CO (289 eV). Table 2 shows the C:O
and C:N ratios and the percentage of species on ABS polymer
particles before and after plasma treatment.
In the case of PLA, the C:O atomic ratio was decreased
after treatment with a He, He/O2, and He/N2 plasmas. The
components of C1s indicates a decrease in the concentration
of C─C/C─H bonds (285 eV), with an increase in the
N-C=O
2.7
concentration of both C─O (286.5 eV) and CO (288.1 eV)
after treatment with a He, He/O2, and He/N2 plasmas. For
particles treated with He/N2, a new polar N─CO group
(289 eV) formed. Table 3 shows the C:O ratios and the
percentage of species on PLA polymer particles before and
after plasma treatment.
The results of this XPS study correlate well with the OES
results detailed in Figure 4 and the water contact angle data
given in Figure 6. He/N2 plasma treatment leads to a higher
concentration of oxygen and nitrogen species on the ABS
surface. This correlates with the larger decrease in water
contact angle obtained after this treatment. This observation is
consistent with reports in the literature that the most probable
mechanism of surface modification of ABS polymer involves
an increase in the surface concentration of functional groups
such as N–CO, CO, C─OH, and R─COO−.[24] In the case
of PLA, functional groups such as C─O, CO, and −COOH
are most frequently introduced by plasma treatment.[27–28]
3.4 | Tensile testing
To establish if the atmospheric plasma treatments of either/
both the polymer particles and the resultant filaments
influenced the tensile performance of the resultant AM
polymer parts, was investigated. Measurements were obtained on three types of dog-bone samples as follows:
– Control samples for which no plasma treatment was used.
– From filaments prepared from activated polymer particles.
– From filaments prepared from both activated polymer
particles and the resultant filaments were also plasma
treated.
TABLE 3 C:O ratio and C1s components on PLA polymer particles surface before and after plasma treatment
C1s Components %
Before treatment
C:O
C─H/C─C
C─O
CO or ─COOH
9.9
86.6
11.3
2.1
He plasma
7.8
79.9
16.3
3.8
He/O2 plasma
3.5
74.4
17.4
8.2
He/N2 plasma
6.2
79.9
15.1
3.3
N─CO
1.7
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ABOURAYANA
FIGURE 6
Change in water contact angle due to hydrophobic
recovery of the PLA and ABS polymer particles
The tension measurements were obtained from batches
of at least five dog-bones printed for each filament type
and the results averaged to find the properties in each batch.
The results of this study are presented in Table 4. The
extension at failure results are not included because many
specimens broke outside of the gage length, probably due
to assumed stress concentrations in the regions changing
geometry.[29]
After plasma treatment of polymer particles, the maximum tensile strength increased by 17% for ABS and 10% for
PLA. While plasma treatment of both particles and filament
leads to an increase in the maximum tensile strength by 22 and
16% for ABS and PLA respectively. The results also showed
the increase in Young's modulus after plasma treatment and
there is no significant increase in the yield strength. From
Table 4 it is shown that the plasma activation of the polymer
particles is shown to have a much more significant impact on
increasing the mechanical strength of the dog-bone samples,
compared with plasma activating the beads and filaments
used to fabricate these samples.
It is important to consider the failure mechanisms of
specimen before and after plasma treatment in addition to the
tensile test data. For the majority of ABS and PLA specimen
fractures followed gaps formed between polymer deposition
ET AL.
lines. This highlights that these gaps are weaknesses in the
polymer structure. Many untreated specimens also experienced total separation of the peripheral wall layers during
tensile testing. Both these features demonstrate relatively
poor bonding between the deposited layers of polymer during
printing.
For the dog-bone specimens printed using polymers
which had been plasma pre-treated, the failure mechanism
was found to be cohesive in all cases, fractures occurred at 90°
to the direction of load (Figure 7). Print lines did not visibly
affect the direction or location of failures. This type of failure
demonstrates the increased structural homogeneity obtained
for the plasma pre-treated polymer structures.
In addition to its effect in activating the polymer surface,
and potentially altering its crystallinity, the plasma also cleans
the surface by removing moisture or organic
contaminations.[30,31]
It is reported that contaminants can adversely disrupting
interfacial bonds and forming a weak boundary layer.[32] In
order to investigate if polymer cleaning, as opposed to plasma
activation is the major contributor to the enhanced mechanical
performance of the plasma treated polymer particles, a
solvent cleaning study was carried out. This involved treating
the PLA polymer particles in an ultrasonic bath while
immersed in propanol for 5 min, followed by ultrasonic
cleaning with deionized water for a further 15 min. The
particles were then dried in an oven at 90 °C for 15 min.
Propanol was selected for this cleaning procedure due to its
use previously for polymer cleaning.[33] XPS analysis of the
cleaned PLA polymer particles, demonstrated an increase in
oxygen concentration, which resulted in a decrease of the C:O
ratio to 4.9, compared with the 9.9 value obtained for the
untreated polymer (Table 3). The solvent cleaned PLA
particles were then extruded as before, to fabricate filaments,
these in-turn was used to produce tensile test specimens. The
tensile strength of dog-bone samples obtained for particles
subject to propanol and water washing was found to be 6%
higher, than obtained for test samples fabricated using the
as-received particles (Table 5). This increase however is
TABLE 4 Tensile strength measurements of ABS and PLA dog-bone samples
Yield strength MPa
Young's modulus MPa
Max. tensile strength MPa
Without treatment
16.8 ± 1.5
1725 ± 83.2
31.0 ± 1.0
Only beads treated
17.9 ± 1.1
1744 ± 59.4
36.4 ± 2.0
Beads and filament treated
18.0 ± 1.7
1759 ± 80.2
38.1 ± 2.2
Without treatment
18.9 ± 0.5
2405 ± 108
42.7 ± 1.2
Only beads treated
20.5 ± 0.4
2403 ± 105
47.2 ± 1.5
Beads and filament treated
21.5 ± 0.9
2498 ± 101
49.5 ± 2.4
ABS
PLA
ABOURAYANA
FIGURE 7
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ET AL.
7 of 8
Photograph of the tensile test fractures obtained for the ABS and PLA polymers
TABLE 5 Tension properties of PLA printed specimens obtained after washing of both beads and filament
Yield strength MPa
Young's modulus MPa
Max. tensile strength MPa
Before treatment
18.9 ± 0.5
2405 ± 108
42.7 ± 1.2
Beads and filament washed
19.76 ± 1.3
2407 ± 88
45.3 ± 1.2
significantly lower than the 16% increase obtained for the
particles/filaments, which had been plasma treated. It is
therefore concluded that the solvent cleaning of the polymer
particles by removing the contamination does enhance the
mechanical strength of the AM fabricated parts, however to a
significantly lower extent than achieved using the atmospheric plasma particle treatment.
4 | CONCLUSIONS
This study investigated the use of barrel atmospheric plasma
system for the activation of ABS and PLA polymer particles.
The influence of processing parameters including; plasma
treatment time and addition of either oxygen or nitrogen to the
helium plasma on the level of plasma surface activation,
based on WCA measurements were investigated. A large
decrease in water contact angle was observed during the first
5 min of He plasma treatment, however the polymer particles
were not found to be significantly affected by longer
treatment times. Addition of oxygen or nitrogen into the
He plasma led as expected to a further decrease in water
contact angle associated with increased oxygen functionality
on the PLA polymer surfaces and increased oxygen and
nitrogen functionality on the ABS polymer surface. Associated with the addition of oxygen to the helium plasma, there is
an increase in the intensity of the OES singlet oxygen lines,
while the corresponding intensity of the other emission lines
were decreased, due to partial quenching of the discharge. In
contrast addition of small amount of nitrogen results to an
increase the intense of N2 and N2+ emission lines. XPS
analysis indicated that, the decrease in WCA of ABS polymer
is largely associated with the formation of C─O and C─N
functional species. The tensile strength of AM printed
samples fabricated from ABS and PLA, were found to
increase after plasma pre-treatment of the polymer particles.
The plasma pre-treated samples also exhibited increased
structural cohesivity during testing, with the three-dimensional structure remaining intact until the moment of failure.
In contrast the untreated samples experienced failure between
printed layers and between walls and the printed layers,
resulting in multiple fracture zones. The use of the plasma
pre-treatment of both the polymer particles and filaments
yielded an increase in the maximum tensile strength of 22 and
16% for AM fabricated ABS and PLA dog bone samples
respectively. Based on ultrasonic solvent cleaning study
carried on PLA particles, it was concluded that plasma
activation as opposed to contaminant removal, was the most
significant contributory factor to achieving the enhanced
mechanical strength of the AM tensile test samples.
ACKNOWLEDGEMENTS
This work is partially supported by the Irish Centre for
Composite Research (IComp) and the I-Form Advanced
Manufacturing Research Centre.
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ORCID
Hisham Abourayana
4005
http://orcid.org/0000-0003-2817-
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How to cite this article: Abourayana H, Dobbyn P,
Dowling D. Enhancing the mechanical performance
of additive manufactured polymer components
using atmospheric plasma pre-treatments.
Plasma Process Polym. 2017;e1700141,
https://doi.org/10.1002/ppap.201700141
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