Defect and Diffusion Forum Submitted: 2017-09-15
ISSN: 1662-9507, Vol. 382, pp 104-108 Accepted: 2017-09-25
doi:10.4028/www.scientific.net/DDF.382.104 Online: 2018-01-10
© 2018 Trans Tech Publications Ltd, Switzerland
Extrusion Temperature and Flow Rate Effects on Tensile Properties
of Additively Processed Poly(Ethylene-co-Trimethylene Terephthalate)
Robert Bail
Department of Creative Convergent Manufacturing Engineering (CCME), Dankook University,
Yongin, Gyeonggi 16890, Korea
[email protected]Keywords: Hot melt extrusion, FFF, PETT, ASTM D 638, tensile strength, modulus.
Abstract. This study investigated the effects of the extrusion temperature and volumetric flow rate
settings in a fused filament fabrication (FFF) process on the tensile properties of specimens made of
poly(ethylene-co-trimethylene terephthalate). The tensile strength almost doubled from 13.5 MPa at
230°C to 26.7 MPa at 260°C extrusion temperature, while the elongation at break improved to 5.4%
and the tensile modulus rose to 641.8 MPa at the highest temperature. Similar observations were
made when the extrusion flow rate was augmented to 115% of the initial value, with part strength
greatly improving to 795.9 MPa and part elasticity increasing by 22%. These results illustrate two
effective strategies to enhance the mechanical properties of components made in an engineering
material that is increasingly being utilized in filament-based 3D printing.
Introduction
FFF. Fused filament fabrication (FFF) is an additive manufacturing technique based on the hot
extrusion of a thermoplastic filament in micrometer-thin strands and its selective deposition in fine
layers according to tool path information derived from an STL file [1]. This process is repeatedly
carried out in an automated manner to build up a component layer upon layer. 3D printers based on
this operating principle can be very useful to the rapid materialization of ideas, the verification of
design concepts, or the direct fabrication of functional components with tailored geometries in small
to mid-size batches [2].
Part geometry and the chosen material usually determine the tensile properties of a component.
With FFF, the latter also depend on a set of tool path parameters that can be controlled in the print
preparation software (slicer). The road width (i.e. strand width) and the air gap between two filament
strands are two parameters that heavily influence the porosity of a fabricated component, with low
porosity resulting in increased strength [3]. Furthermore, an increase in the feed rate may enlarge the
cross sectional strand profiles and hence improve part strength [4].
In addition, the tensile properties of a component built by using FFF are affected by the thermal
conditions during material deposition, which in turn affect the bond formation between the material
strands [5]. The resulting neck growth increases when the temperature in the material remains above
the critical sintering temperature [6]. Accordingly, the average pore size in a printed component
decreases with faster print speeds, short motion patterns, increased envelope temperatures, and close
distance of the part to the center of a heated bed, which results in increased strength [7].
Aims and objectives. A wide body of knowledge exists regarding the effects of the FFF process
parameters on the mechanical properties of a part made in one of the well-established filament
materials, like polylactic acid (PLA) and acrylonitrile butadiene styrene (ABS). However, there is a
lack of such data for the recently emerging poly(ethylene-co-trimethylene terephthalate) (PETT),
which is a flame retarded thermoplastic material that can be extruded without releasing potentially
toxic fumes [8]. This study aims at verifying the effects of the extrusion temperature and the extrusion
flow rate on the mechanical properties of a component printed in this material. The insights gained
will be very useful to the development and additive fabrication of PET-based components for a range
of applications where high strength but also some degree of flexibility are required.
All rights reserved. No part of contents of this paper may be reproduced or transmitted in any form or by any means without the written permission of Trans
Tech Publications Ltd, www.scientific.net. (#523796119, Linköpings Universitetsbibliotek, Linköping, Sweden-04/01/20,14:11:20)
Defect and Diffusion Forum Vol. 382 105
Methodology
Specimen design. A tensile test specimen was designed using a parametric computer-aided design
program (FreeCAD, 0.16 stable release) according to ASTM D 638 type IV specifications [9]. The
dogbone-shaped part measured 4 mm in thickness and 6 mm in width at the center. Sets of five
identical specimens were arranged, and 1-mm thin supports were added for lateral support during the
build as shown in figure 1(a). The design files were exported to the STL format using ultra-fine
tesselation settings (max. surface deviation 0.001 mm). The files were then loaded to 3D print
preparation software (Cura Ver. 15.04, Ultimaker, Geldermalsen, NL), where the dogbone set was
placed in a vertical position on the center of the virtual printer bed (figure 1(b)). Each set was built
with an enlarged raft (15-mm margin) for improved adhesion to the printer bed during the fabrication
process.
Fabrication. All sets were fabricated on a FFF-based desktop printer (RexBot3D OC-200,
NTREX Inc., South Korea) featuring a build envelope of 200 x 200 x 200 mm (X, Y, Z). A filament
made of poly(ethylene-co-trimethylene terephthalate) with a 1.75-mm diameter (t-glase, taulman3D,
Saint Peters MO., US) was used as the extrudable material. The following parameters were kept
constant during all print jobs: 0.25 mm layer height, 0.5 mm nozzle diameter, 60°C bed temperature,
and 40 mm/s print speed. During the first experimental series, the nozzle temperature was kept at
240°C but the extrusion rate was varied from 5.00 to 5.75 mm3/s in steps of 0.25 mm3/s (equivalent to
a flow rate of 100 to 115%). During the second set of experiments, the extrusion rate remained steady
at 5.00 mm3/s but the nozzle temperature was augmented from 230°C to 260°C in steps of 10°C. After
completion of each build job, the set was detached from the print bed. The raft and lateral supports
were peeled off the specimens, and the remaining debris at the anchor points was carefully removed
using sandpaper.
Tensile test. The specimens were conditioned for 48 hours at 22±1°C and 40±5% humidity. For
each printed specimen, the actual center thickness (ti) and width (wi) were measured using digital
calipers. They were then examined (n=5) on a universal materials testing instrument (Lloyd LR30K
Plus, Ametek Inc.). The stress was exerted in build direction (Z) of a specimen, i.e. perpendicular to
the layer orientation, to determine the strength and modulus [MPa] in dependence of the extrusion
parameters. The tensile test was carried out at a speed of 2 mm/s using flat jaw grips and a 10-kN load
cell. The testing machine recorded the load vs. extension data automatically, from which the tensile
parameters were calculated.
Fig. 1: (a) CAD model according to ASTM D 638 IV and (b) print simulation in slicer software.
106 Engineering and Innovative Materials VI
Results
The recorded stress-strain curves and mechanical parameters demonstrated that the properties of the
tested samples varied with extrusion temperature (figure 2(a)) as well as flow rate (figure 2(b)). With
an increase in the extrusion temperature from 230°C to 260°C, the test parts condiderably gained in
terms of stiffness and strength. As shown in figure 3(a), the tensile strength increased from an average
of 13.5 MPa at 230°C to 26.7 MPa at 260°C nozzle temperature, while the elongation at break
inclined from 3.4% to 5.4%. The tensile modulus was raised from 490.3 MPa at the lowest to
641.8 MPa at the highest nozzle temperature. This means that an increase in the extrusion temperature
by a mere 13% resulted in specimens with a 98% higher strength, a 59% larger elongation at break,
and a 31% higher stiffness. In addition, the samples extruded at 240°C and higher exhibited similarly
good part quality, whereas the samples extruded at 230°C exhibited a rough surface and were easy to
break. This was confirmed by a drop in the according stiffness and strength data.
Compared to what was observed for the temperature effects, similar observations were made when
the extrusion flow rate was augmented. The increase in strength was even larger and the increase in
stiffness was less pronounced as shown in figure 2(b). The tensile strength went up from 20.9 MPa at
5.00 mm3/s (or 100%) to 32.2 MPa at 5.75 mm3/s (115%) extrusion rate. At the same time, the
elongation at break inclined from 4.1% to 5.0% and the tensile modulus increased from 590.5 MPa to
a remarkable 795.9 MPa at the highest of the tested flow rates, as illustrated in figure 3(b). This
suggested that an increase in flow rate by 15% resulted in a 54% higher strength, a 22% larger
elongation at break, and a 35% higher stiffness. Furthermore, the increase in strength and modulus
with an increase in flow rate was approximately linear for all samples.
It was apparent that the extrusion temperature and the extrusion flow rate had an impact on the
tensile properties of samples extruded in poly(ethylene-co-trimethylene terephthalate). At the lowest
of the tested extrusion temperatures, the actual temperature in the polymer melt was comparatively
low in the moment when it left the extrusion channel. When the deposited filament got in contact with
the printer bed or a previously deposited layer, its actual temperature had already fallen to a value
close to or below the glass temperature of the material. This reduced the ability of the extruded
polymer to build van-der-Waals bonds between adjacent filament strands, resulting in low bond
strength. This explains the drop in stiffness and strength with reduced nozzle temperatures. By
contrast, an increase in the extrusion temperature raised the temperature in the filament in the moment
when it made contact with a previous layer. This resulted in material strands enabled to establish
increasingly strong bonds with the adjacent layer. This was confirmed by the observed increase in
stiffness and strength.
Fig. 2: Stress-strain data (n=5) for tested range of (a) extrusion temperatures and (b) flow rates.
Defect and Diffusion Forum Vol. 382 107
The observed increase in stiffness and strength with an increase in flow rate was not related to bond
strength but to a change in the bonded surface areas. When extruded at 5.00 mm3/s (or 100%), the
filament diameter was equal to the applied path size (0.5mm), and the deposited filament was given
enough space to fit in its “lane”. This also implied that the round cross section of the extruded
filament remained relatively unaltered and the contact area between two adjacent filaments was the
smallest in comparison, leading to relatively low stiffness and strength. By contrast, with an increase
in the extrusion flow rate, the volumetric flow and hence the volume of the filament deposited per
voxel increased but the path width remained constant. This meant that the extruded strands were
squeezed into their “lane”, which gradually turned the initially round cross section of a strand into a
more rectangular shape. As a result, the contact area between two adjacent layers increased with larger
flow rates, which improved stiffness and strength of the deposited structures.
Fig. 3: Effect of extrusion temperature and flow rate on tensile properties of PETT.
108 Engineering and Innovative Materials VI
Conclusions
In this study, the effects of the extrusion temperature and the extrusion flow rate on the tensile
properties of 3D-printed components made of poly(ethylene-co-trimethylene terephthalate) were
investigated. It was demonstrated that an increase in the extrusion temperature from 230 to 260°C
massively improved the mechanical properties, given a 98% higher strength, a 59% larger elongation
at break, and a 31% higher stiffness at the highest temperature setting. An increase in the extrusion
flow rate by 15% resulted in the fabrication of specimens with a 54% higher strength, a 22% larger
elongation at break, and a 35% higher stiffness. These results confirm that augmenting the extrusion
temperature or the extrusion rate are both effective strategies to maximize the tensile properties of
components made in this PET copolyester. This is valuable information for the direct digital
fabrication of components that require a combination of high strength, flexibility, and food safety.
Acknowledgements
This research was supported by the Ministry of Trade, Industry and Energy (MOTIE), KOREA,
through the Education Program for Creative and Industrial Convergence (Grant Number N0000717).
References
[1] I. Gibson: Extrusion-Based Systems, edited by I. Gibson, D. Rosen, B. Stucker, Additive
Manufacturing Technologies, chapter 6, Springer (2010) p.160
[2] Information on: http://www.materialise.com/en/manufacturing (2017)
[3] K.C. Ang, K.F. Leong, C.K. Chua: Rapid Prototyping Journal, Vol 12/2 (2006) p. 100
[4] O. Rishi: Feed Rate Effects In Freeform Filament Extrusion. Rochester Institute of Technology,
MSc thesis (2013)
[5] B.T. Turner, R. Strong, S.A. Gold: Rapid Prototyping Journal, Vol. 20/3 (2014) p. 192
[6] C. Bellehumeur, L. Li, Q. Sun, P. Gu: Journal of Manufacturing Processes, Vol. 6/2 (2004) p.
170
[7] Q. Sun, G. Rizvi, C. Bellehumeur, P. Gu: Rapid Prototyping Journal, Vol. 14/2 (2008) p. 72
[8] L.W. Branscome, U.S. Patent 4,837,254 (1989)
[9] ASTM Standard D 638, Standard Test Method for Tensile Properties of Plastics, ASTM
International, West Conshohocken, USA (PA), 2004.