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Additive Manufacturing 19 (2018) 29–38

Contents lists available at ScienceDirect

Additive Manufacturing
journal homepage: www.elsevier.com/locate/addma

Full Length Article

Process-structure-property effects on ABS bond strength in fused


filament fabrication
A.C. Abbott a,∗ , G.P. Tandon a , R.L. Bradford a , H. Koerner b , J.W. Baur b
a
University of Dayton Research Institute, Dayton, OH 45469, United States
b
Materials and Manufacturing Directorate, Air Force Research Laboratory, Wright-Patterson AFB, OH 45433, United States

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

Article history: Interlayer bonds pose regions of weakness in structures produced via melt extrusion based polymer addi-
Received 1 March 2017 tive manufacturing. Bond strength was assessed both between layers and within layers as a function of
Received in revised form 25 October 2017 print parameters by performing tensile tests on ABS coupons printed in two orientations. Print param-
Accepted 3 November 2017
eters considered were extruder temperature, print speed, and layer height. An IR camera was used to
Available online 4 November 2017
track thermal history of interlayer bond lines during the printing process. Contact length between roads
was measured from mesostructure optical micrographs. Print speed was found to have a large impact
Keywords:
on tensile strength with high speeds generally yielding lower strength. A plateau in tensile strength of
Fused filament fabrication
IR camera
22 MPa was observed for a normalized contact length greater than 0.6 independent of print orientation.
Road-to-road bond strength © 2017 Elsevier B.V. All rights reserved.
Mesostructure

1. Introduction adjacent roads and between layers in printed parts is measured


while considering two factors: cooling profiles at layer interfaces
Additive manufacturing is an emerging manufacturing tech- and road-to-road contact. These factors are varied by manipulat-
nique in which objects are fabricated in a layer-wise manner. ing print parameters in accordance with a design of experiment.
Material extrusion (ME), also known as fused filament fabrication Tensile strength results are analyzed as a function of road-to-road
(FFF), is an additive manufacturing strategy whereby polymer fila- contact normalized by the road dimensions.
ment is fed through a heated liquefier, is extruded through a nozzle, Print parameters available for user control have a large impact
and is deposited on a build surface or previously printed layers on the mechanical performance of printed parts. While available
where it quickly cools. Structural integrity of AM parts is derived parameters depend on the slicing software used and machine lim-
from bonding between adjacent and stacked extruded roads. Bond- itations, some common parameters include: layer height, infill
ing forms via a polymer coalescence mechanism and is a function orientation, infill density, and extruder temperature (TE ). Several
of thermal history at road interfaces. The cooling profile at road studies have utilized a design of experiment (DoE) approach to
interfaces defines a time window over which molecular diffu- analyze the effects of print parameters on mechanical proper-
sion and randomization of the polymer chains at the interface can ties of parts printed with acrylonitrile-butadiene-styrene (ABS)
occur and is limited at the low end by the polymer glass transi- thermoplastic polymer. Tensile properties have been measured
tion temperature at which polymer dynamics drop by an order in response to build orientation, infill angle, road width, air gap
of magnitude. Additionally, the quality of the bond depends on between adjacent roads [1], extruder temperature, polymer col-
the neck growth which is formed between the adjoining rasters. orants [2], unidirectional infill angle [3,4] and angle-ply laminates
Increasing interfacial contact area between road interfaces offers [5–8]. Flexure properties [9,10] and compression properties [11]
greater potential for strong bond formation as long as thermal con- have also been studied with respect to similar print parameters.
ditions drive polymer coalescence. Analysis that combines thermal Other properties that have been considered include dimensional
history at road interfaces with printed part mesostructure is criti- accuracy [12,13] and elastic flexibility [14]. In general, these stud-
cal as it relates to measured mechanical properties and elucidates ies found infill angle and air gap to have the largest influence on
relationships between the ME process, printed structure, and struc- mechanical properties with infills aligned along the loading direc-
tural performance. In this work, tensile strength of bonds between tion and small air gaps resulting in higher performance. Smaller
layer heights were also found to slightly improve mechanical per-
formance in most cases. Extruder temperature was generally not
observed to have a large impact on mechanical performance. All
∗ Corresponding author.
of these studies varied print parameters and measured changes
E-mail address: andrew.abbott@udri.udayton.edu (A.C. Abbott).

https://doi.org/10.1016/j.addma.2017.11.002
2214-8604/© 2017 Elsevier B.V. All rights reserved.
30 A.C. Abbott et al. / Additive Manufacturing 19 (2018) 29–38

to some performance metric. However, underlying relationships Table 1


Print parameters and levels from which a full-factorial DoE was created.
between print parameters and resulting mesostructure of printed
parts and their impact on mechanical performance have not been Factor Low level High level
explored in detail. Extruder temperature (◦ C) 230 270
In the ME process, extruded roads of material partially coalesce Print Speed (mm/s) 10 50
with adjacent and underlying roads. Road-to-road coalescence is Layer height (mm) 0.1 0.3
the mechanism that drives bond formation between roads. For- Orientation XY ZX

mation of strong bonds is critical to the structural performance


of printed parts. Bond formation involves neck growth, molecular
diffusion between road interfaces, and polymer chain entangle- can be assessed with tensile coupons printed flat (XY orientation).
ment which are strong functions of temperature [15]. Polymer Vertically printed (ZX orientation) tensile coupons have bonds
coalescence has been studied in literature [16–22] and is typi- between layers oriented in the axial direction (Fig. 1a). Mesostruc-
cally expressed as a function of the material properties surface tures are described by measured parameters shown in Fig. 1b and
tension and viscosity. For the ME process, the thermal history at 1c where Lcx and Lcz are the contact lengths over which tensile load
road interfaces influences the dynamics of molecular diffusion and is applied, hx is the height or thickness of a road in the XY orien-
entanglement and defines the processing window over which phys- tation and hz is the road width in the ZX orientation, and Wsx and
ical bonds can form. Thermal history of printed roads in the ME Wsz are referred to as road spacing. Wsx and Wsz are taken as the
process have been analyzed using thermocouples [9], fiber Bragg distance between adjacent contact lengths such that Wsx and Wsz
gratings [23], and IR cameras [24–28], but little work has been done reduce to hx and hz if there is no additional space between adjacent
to couple to printed part mechanical properties. roads.
In this work, a DoE was applied to select print parameters to
observe the effects on extrudate cooling profiles, road-to-road con- 2.2. Printing procedure and design of experiment
tact lengths, and transverse tensile strength. To reduce the number
of parameters in the DoE to a tractable amount, the four most Tensile strength of unidirectional ME coupons printed in the XY
significant parameters were varied: extruder temperature, print and ZX orientations was measured for dog bone shaped coupons.
speed, layer height, and build orientation. Extruder temperature Specimens were 64 mm long, 10 mm wide in the grip section, with a
and print speed were selected as means of varying thermal his- gage section 5 mm wide and 28 mm long, and 2 mm thick. Coupons
tory while layer height was selected to manipulate mesostructure. were fabricated from Makerbot ABS filament using an nScrypt
Build orientation was probed by fabricating tensile specimens in 3Dn-500 system with an nFD pump. While the molecular weight
two orientations shown in Fig. 1a with infill patterns arranged per- of the filament was not measured, common values for number
pendicular to the loading direction such that either road-to-road average molecular weight of polymer filaments used for ME are
bonds (Fig. 1b) or interlayer bonds (Fig. 1c) carried applied load. 100–200 kDa [29,30]. It is recognized that molecular weight plays
Other print parameters not included in this DoE, such as nozzle a vital role in road-to-road diffusion and bond formation [31,32].
size, feeder system, infill pattern, and build plate temperature, are The nScrypt 3Dn-500 system utilizes a 3-axis Aerotech gantry with
expected to have minor effects on thermal history of interlayer support for four tools. One such tool is the nFD pump which features
bonds and mechanical performance. Nozzle size is expected to a worm gear mechanism to advance standard 1.75 mm diameter
affect the number of roads in a layer and thus may impact road- polymer filament into a heated section comprised of a ceramic
to-road contact length and interlayer strength to a small degree. nozzle through which the polymer is extruded and a metal nozzle
Changing feeder systems is expected to have a negligible effect holder. The nozzle holder houses a cartridge heater and thermocou-
on mechanical performance provided the target volumetric flow ples connected to controllers for closed loop feedback temperature
rate out of the extrusion nozzle is satisfied. Infill pattern of spec- control. The gantry system is outfitted with a heated build plate
imens printed in the XY orientation as shown in Fig. 1a will have measuring 330 mm square and capable of heating to 200 ◦ C. Poly-
a large effect on mechanical properties. However, in the ZX ori- imide tape was placed over the build plate to provide a surface
entation, infill pattern will affect the number of roads in a layer, for adhesion to ABS and the plate temperature set points were
but the effect on interlayer bond strength is expected to be minor. 110 ◦ C and 120 ◦ C for XY and ZX oriented coupons respectively. An
Cooling of interlayer bonds was followed with an IR camera dur- increased build plate temperature was required for ZX coupons to
ing the printing process. Printed mesostructures were analyzed by ensure adhesion between the coupons and the polyimide substrate.
optical microscopy and normalized contact lengths were measured. At a set point of 110 ◦ C, the measured temperature at the center of
Tensile specimens were printed in the build orientation described the build plate was 106 ◦ C. At a set point of 120 ◦ C, the measured
because road-to-road and interlayer bonding are identified as per- temperature at the front edge of the build plate was 113 ◦ C. Tem-
formance limiting. Therefore, tensile specimens were loaded to perature variation across the entire build plate was within 10 ◦ C.
assess the performance limiting strengths. A tensile test was seen Slic3r was used to generate G-code machine control code based on
as the most direct way of probing road-to-road and interlayer bond user-selected print parameters.
strength and was therefore selected over other test methods, such A full-factorial DoE procedure was used to measure tensile
as bending, which introduce other modes such as compression and strength as a function of the selected print parameters in Table 1.
shear. Measured tensile strengths were examined relative to nor- These print parameters were selected for their expected influ-
malized contact lengths. ence over road cooling time and adjacent road contact area. Large
contact area and slow cooling are expected to promote diffusion
of polymer across adjacent road boundaries thereby improving
2. Experimental procedures road-to-road tensile strength. The DoE was conducted with four
parameters each with two levels to form an experimental matrix
2.1. Definitions of mesostructure parameters with sixteen unique parameter combinations. These parameter
combinations were applied to each print orientation. Three repli-
Specimens were printed in two orientations to measure road- cates were printed for each combination. For XY oriented coupons,
to-road and interlayer bond strengths. Bond strength between three replicates sharing the same print parameters were printed
adjacent roads within the same layer aligned in the axial direction non-sequentially (one layer for each before printing the next layer)
A.C. Abbott et al. / Additive Manufacturing 19 (2018) 29–38 31

Fig. 1. (a) Printed orientations: XY (flat) and ZX (vertical). Contact length, road height, and road spacing notation is defined for (b) XY and (c) ZX orientations.

during the same build. For the ZX orientation, only one coupon 2.5. Tensile testing procedure
was printed at a time. ZX oriented coupons proved difficult to
print without flaws as overhanging regions in the top grip sections Quasi-static tensile tests were performed on an MTS load frame
were printed without support material. Additionally, the slender at a rate of 1.27 mm/min (0.05 in/min). Strain was measured in both
specimen geometry had small contact areas with the build surface the axial and transverse directions with an MTS advantage video
and some specimens prematurely detached from the build surface extensometer (AVX). This technique operates by the principles of
before print completion. Programming the build plate set point digital image correlation (DIC). DIC is a non-contact strain measure-
to 120 ◦ C mostly alleviated detaching issues. Vertically oriented ment technique that converts from measured pixel displacement to
coupons printed with an extruder temperature of 230 ◦ C resulted local strain by using a correlation algorithm [33]. DIC has a number
in top grip sections that were uneven and rough and therefore were of advantages over contact strain measurement methods (e.g. strain
not tensile tested. gauges or extensometers) including: the ability to detect spatially
variable strains, adaptability to aggressive environments, and suit-
ability for soft materials such as polymers for which adhesive strain
2.3. IR camera temperature calibration gauges would cause local stiffening and inaccurate strain detection
[34]. Software tracked displacement of speckles painted on each
Bond line temperature was observed for coupons printed in the specimen during mechanical loading and used this information to
ZX orientation using a Merlin Indigo IR camera equipped with an calculate axial and transverse strain. Before testing, coupons were
ASIO 3–5 ␮m wavelength microscope lens manufactured by Janos dried at 75 ◦ C for 14 h under vacuum to remove moisture adsorbed
Technologies featuring an adjustable focal length of 75–150 mm. by ABS; a hygroscopic polymer [35]. Although the weight change
The image size captured by the camera using this lens was approx- of dried specimens was insignificant, the drying procedure was
imately 7.5 by 6 mm with a resolution of 320 by 256 pixels. The retained for consistency with other commonly used ME polymers,
integration time, i.e.; the refresh rate of the IR detector, was set to such as Ultem, which readily absorb moisture.
250 ␮s. A LabView program was used to record video from the IR
camera at a rate of 15 frames per second and to record IR counts
at user-defined pixels in each frame. After collecting videos, the
IR counts were converted to temperature following a calibration 3. Results and discussion
curve. The calibrations curve was constructed by printing an ABS
block with two 10 mm long channels on one side located 1 mm from 3.1. Rationale for print parameter selection
the front face and 0.3 mm from the top and bottom faces (Fig. 2a).
Thermocouples were placed in the channels (Fig. 2b) and the block Increasing the extruder temperature was expected to increase
was heated on the build plate. Build plate temperature was held both the initial polymer diffusion rate as well as the amount
at several values between 50 ◦ C and 100 ◦ C in increments of 10 ◦ C of time the polymer was above its glass transition temperature
and allowed to reach approximate steady state at each value. Tem- (Tg). Expanding the time window for diffusion of polymer chains
perature was recorded from embedded thermocouples as well as across road boundaries was expected to increase polymer coa-
with the IR camera on the front face of the block at points A and B lescence, entanglement, and therefore bond strength. Print speed
corresponding to thermocouple locations as shown in the IR image was expected to affect the thermal history of bondlines. As bond
in Fig. 2c. IR counts were plotted against thermocouple tempera- strength is derived from polymer diffusion which is a function of,
ture and fit with a logarithmic function (Fig. 2d). Because the focal among other things, time at temperature, print speeds that maxi-
length of the IR camera lens was short, ZX specimens were printed mize time at temperature are favorable. Depositing molten polymer
close to the front edge of the build plate protecting the camera from was expected to reheat both adjacent and underlying bond lines
the build plate temperature. through radiation and conduction. Reheating would temporarily
accelerate polymer diffusion and entanglement. In this way, bond
formation would intermittently progress in response to reheating
2.4. Optical microscopy for mesostructure analysis from continued road deposition during a print. This bond formation
mechanism is expected to be promoted by slower print speed. At
Mesostructures of printed coupons were examined using optical slower speeds, the heated nozzle is expected to provide local heat-
microscopy with a 2.5 x objective for large field of view. Images ing for longer time through radiation. Once the print progresses
were captured in the gage section of coupons that were not tensile far enough that a specific bond line is no longer heated above Tg by
tested, but rather manufactured using the same print parameters deposition of subsequent roads, bond development is considered to
exclusively for imaging. Three measurements were made for each have ceased. Smaller layer height was expected to increase inter-
unique coupon: contact length, road height, and road spacing as layer bond strength. By decreasing layer height, more layers are
described in Fig. 1b and c. Measurements were made with ImageJ. needed to print any given object. Printing more layers was expected
All values are reported as averages of at least 30 measurements per to create more opportunities for reheating underlying bond lines
specimen. promoting additional polymer diffusion and entanglement.
32 A.C. Abbott et al. / Additive Manufacturing 19 (2018) 29–38

Fig. 2. (a) calibration block for IR counts with (b) thermocouple hole dimensions. (c) IR image of block heated on build plate with thermocouple and IR counts measured at
locations A and B. (d) calibration curve for 250 ␮s integration time.

Fig. 3. Representative cooling curves obtained with an IR camera for coupons printed with (a) TE = 230 ◦ C and (b) TE = 270 ◦ C. The Tg of ABS polymer is given by a horizontal
line. (c) Dashed box represents the IR camera field of view. Build surface not drawn to scale.

3.2. Thermal history of road-to-road bond lines The Tg of ABS was measured as 103.6 ◦ C using differential scanning
calorimetry (DSC) with a heating rate of 10 ◦ C/min. The camera was
Average duration of time that bond lines between layers were focused on the gage section of dog bone coupons. Due to space con-
above Tg was measured with an IR camera for ZX oriented coupons. straints, bond line temperatures of XY oriented coupons were not
A.C. Abbott et al. / Additive Manufacturing 19 (2018) 29–38 33

Table 2
Time at T > Tg from IR thermal history measurments.

TE (◦ C) Speed (mm/s) Layer height (mm) Time at T > Tg (s)

230 10 0.1 50
230 10 0.3 35
230 50 0.1 39
230 50 0.3 32
270 10 0.1 58
270 10 0.3 50
270 50 0.1 50
270 50 0.3 54

measured. Because the IR camera was only capable of measuring


relatively narrow temperature ranges, and because measurement
Fig. 4. Main effects plot of relative effects of print parameters on time above Tg for
fidelity near room temperature was to be maintained, the maxi- ZX printed coupons.
mum measurable temperature was limited. Using a 250 ␮s detector
integration time yielded a measurable temperature range between
160 ◦ C and 65 ◦ C. Therefore, bond line temperature measurement which contact spans the height of the roads. As this ratio approaches
was initiated shortly after road deposition. one, the contact length approaches the maximum equal to the full
Average time at T > Tg was determined for layer-to-layer bond height of the road. Fig. 5c shows a micrograph of a coupon printed
lines at each print parameter combination in the DoE. Fig. 3 shows with low TE , slow speed, and large layer height represented in the
representative cooling curves for each print parameter combina- figure as 230/10/0.3. Effects of extruder temperature on mesostruc-
tion. Bond line temperature was measured for ZX coupons at a ture are seen by comparing Fig. 5c and d. Examining Table 3 reveals
distance from the build plate of about 25 mm. The IR camera field that neither Lc nor Lcx /hx directly trend with TE . At low print speed,
of view is represented by the dashed box in Fig. 3c. IR reflections as contact length decreases with increasing TE. Conversely, contact
described in [24] were considered, but found to only occur for the length increases with increasing TE at high print speed. As seen in
layer directly below the actively printing layer. Because IR counts the main effects plot with error bars indicating standard error in
from this layer saturated the detector while printing, IR reflection Fig. 6a, TE had little effect on Lcx /hx compared to the other print
effects were disregarded. As expected, increasing extruder temper- parameters. The effect of print speed is qualitatively assessed by
ature (TE ) led to longer time above Tg as seen by comparing cooling comparing Fig. 5c–e. A decrease in both Lcx /hx and contact length is
curves at low TE in Fig. 3a and high TE in Fig. 3b. Table 2 gives the observed and confirmed by measured values presented in Table 3.
average amount of time bond lines existed above Tg within the IR This trend of decreasing contact length with increasing speed was
camera field of view. Slower print speeds led to longer time above common to all pairs of coupons printed with the same TE and
Tg contrary to expected results. This phenomenon is suspected to layer height. Fig. 6a captures this trend indicating that Lcx /hx was
be caused by the small cross-sectional area of tensile coupons’ gage larger on average at lower print speeds. Layer height effects are
section (10 mm2 ) which limited required nozzle travel distance. qualitatively assessed by comparing Fig. 5d–f. These coupons were
The nozzle remained in close proximity to deposited roads acting printed with high TE and slow speed. Smaller layer height results
as a radiative heat source. Radiative heating would have been more in oblong roads with small contact lengths perpendicular to the
influential for slower print speeds [24]. Smaller layer heights led to direction of applied load. While increasing layer height resulted
an increase in time above Tg likely due to the combined effects of in adjacent roads with longer Lcx , Lcx /hx only slightly increased on
local heating from the nozzle and improved compaction between average because road height also increased.
layers. Specimen geometry is expected to have a large impact on Micrographs of ZX oriented coupon mesostructures are com-
the cooling profile. Increasing cross-sectional area while holding pared in Fig. 7 in which the build and loading directions are
print speed constant is expected to reduce the time period over collinear. The image in Fig. 7c corresponds to a specimen printed
which bond line temperatures are above Tg. with high TE , large layer height, and slow speed (270/10/0.3). Effects
Fig. 4 captures the main effects of each print parameter on the of TE are seen by comparing Fig. 7c and d. Higher TE resulted in
duration of time above Tg. In a main effects plot, a minus (−) corre- longer Lc and Lcz /hz due to lower polymer viscosity enabling more
sponds to the average measured property for coupons printed with flow and coverage of underlying layers. For all print parameter com-
the low level of the specified print parameter whereas a plus (+) cor- bination, increasing TE increased Lcz /hz which is captured in Table 4
responds to the high value of the print parameter. Main effects plots and the main effects plot in Fig. 6b. Speed effects are assessed
show the relative impact of each print parameter by the absolute by comparing Fig. 7e and f. Both of these coupons were printed
value of the slope of the line connecting the low and high values. with high TE and small layer height. Increasing speed decreased
A high slope indicates that a parameter had a large impact. Lcz , Lcz /hz , and Lc /Wsz in Table 4. When Lcz /Wsz is less than Lcz /hz ,
adjacent roads are not in contact which is expected to interfere
3.3. Analysis of mesostructure features with transfer of applied load and reduce mechanical properties.
Fig. 6b shows that print speed had a large effect on Lcz /hz with
Print parameter settings have significant impact on the resulting slower speed preferred. Effects of layer height on mesostructure are
structure of printed parts as seen by optical microscopy. Mesostruc- seen by comparing Fig. 7c–e. The coupon in Fig. 7e had good com-
tures of select XY oriented coupons are displayed in Fig. 5 where paction between the layers (Z direction) and yielded the largest Lcz
the vertical and horizontal directions are aligned with the build and and highest Lcz /hz . For this print orientation, increasing layer height
applied load directions respectively. The viewing plane for these decreased Lcz and Lcz /hz due to the change in road geometry.
images is the XZ plane as shown in Fig. 5b where Z is the thickness The coupon in Fig. 6c (270/10/0.3) had the second longest
direction. It is important to note that reported contact length only average contact length. The time above Tg for this parameter com-
implies physical contact. It does not necessarily imply molecular bination was 49.5 s, the shortest of any ZX print, but yielded the
diffusion has occurred across road boundaries. The ratio of Lcx /hx highest average tensile strength. This implies that 49.5 s above Tg
is termed the fractional contact length. It indicates the extent to was likely sufficient for polymer diffusion across bond lines and
34 A.C. Abbott et al. / Additive Manufacturing 19 (2018) 29–38

Fig. 5. XY mesostructures. Coupons printed in XY orientation shown in (a), sectioned along the XZ, and imaged at the created surface. Contact length measured perpendicular
to loading direction (b). Select mesostructures (c-f) with print parameters given in format TE /speed/layer height. Scale bar = 1 mm.

Table 3
Contact length from mesostructure analysis and tensile strength for each print parameter combination in XY oriented coupons.

TE (◦ C) Speed (mm/s) Layer height (mm) Lcx (␮m) Lcx /Wsx Lcx /hx

230 10 0.1 87 ± 10 0.8 ± 0.1 0.8± 0.1


230 10 0.3 247 ± 23 0.8 ± 0.1 0.8 ± 0.1
230 50 0.1 52 ± 35 0.5 ± 0.3 0.5 ± 0.3
230 50 0.3 144 ± 24 0.5 ± 0.1 0.5 ± 0.1
270 10 0.1 68 ± 12 0.7 ± 0.1 0.7 ± 0.1
270 10 0.3 233 ± 31 0.8 ± 0.1 0.8 ± 0.1
270 50 0.1 57 ± 12 0.6 ± 0.1 0.6 ± 0.1
270 50 0.3 173 ± 20 0.6 ± 0.1 0.6 ± 0.1

Fig. 6. Main effects plots of relative effects of print parameters on fractional contact length in a) XY and b) ZX orientations.

Fig. 7. Coupons printed in the ZX orientation (a) were sectioned along the YZ plane and rotated. Contact length was measured perpendicular to the loading direction (b).
Select mesostructures (c–e) with print parameters indicated as TE /speed/layer height. Scale bar = 1 mm.
A.C. Abbott et al. / Additive Manufacturing 19 (2018) 29–38 35

Table 4
Contact length from mesostructure analysis and tensile strength for available print parameter combination in ZX oriented coupons.

TE (◦ C) Speed (mm/s) Layer height (mm) Lcz (␮m) Lcz /Wsz Lcz /hz

230 10 0.1 – – –
230 10 0.3 271 ± 18 0.7 ± 0.1 0.7 ± 0.1
230 50 0.1 318 ± 72 0.7 ± 0.3 0.6 ± 0.2
230 50 0.3 134 ± 21 0.2 ± 0.1 0.4 ± 0.1
270 10 0.1 476 ± 27 0.9 ± 0.1 0.9 ± 0.1
270 10 0.3 320 ± 12 0.8 ± 0.1 0.8 ± 0.1
270 50 0.1 312 ± 26 0.7 ± 0.1 0.9 ± 0.1
270 50 0.3 220 ± 42 0.5 ± 0.1 0.6 ± 0.1

formation of interlayer bonds. Above some critical threshold time


at T > Tg for sufficient interlayer polymer diffusion, normalized and
fractional contact length are likely the primary factors driving ten-
sile strength of printed coupons. Below the threshold, polymer
diffusion is the primary factor limiting tensile strength. Polymer
sintering models are sufficient to describe interlayer diffusion in ME
[15–22]. Road interfaces of coupons printed in the ZX orientation
with high extruder temperature are suspected to be above some
critical threshold time at temperature to allow for molecular diffu-
sion across road interfaces and development of higher mechanical
properties. The coupons in Fig. 6c and e printed with small layer
height exhibit substantial compaction between the layers forming
long contact lengths perpendicular to the direction of applied load.
Compaction is expected to aid in bond formation if the polymer is
above the critical temperature for molecular diffusion.

3.4. Analysis of mesostructure effects on tensile strength


Fig. 8. Tensile strength plateaus with normalized contact length where there is
Tensile experiments gave strength results between 10 and contact between adjacent roads.
22 MPa for both orientations. Compiled results are given in Table 5.
It should be noted that one of the specimens printed with the ZX orientation against fractional contact length Lcx /hx and Lcz /hz .
parameter combination ZX 270/10/0.1 yielded the highest mea- A fractional contact length of unity implies that all available area
sured tensile strength value of 27.5 MPa. The large deviation for bond formation has been utilized. Fractional contact length of
(7.19 MPa) in the average value (19.37 MPa) was caused by fail- one along with road spacing equal to road height is equivalent to
ure of some samples at defects induced during printing. Overall, injection molded fully dense polymer. Fig. 8 plots fractional con-
these results are similar to those by Rayegani et al. [1] for parts ori- tact length (Lcx /hx and Lcz /hz ) against tensile strength. A plateau
ented at 90◦ (ZX orientation) and with a 0◦ raster angle. Their results is observed around 22 MPa beginning at Lcx /hx of 0.6. Beyond this
depend highly on air gap, the edge-to-edge spacing between adja- point, neither increasing Lcx /hx nor Lcz /hz led to any significant
cent roads. With a negative air gap, the measured tensile strength improvement in tensile strength. The reduction in tensile strength
is as high as 24 MPa, but a positive air gap yielded strengths up to with fractional contact lengths below 0.6 implies that there is insuf-
only 9 MPa. Although air gap was not directly controlled in results ficient contact for strong bond formation. Of the data points with
presented here, results for high print speed are more similar to fractional contact length below 0.6, three were printed in the XY
Rayegani’s results for positive air gap. Bellini et al. [36] printed orientation. While the average fractional contact length is reported
ZX tensile specimens and obtained an average strength of 7.6 MPa for these specimens, there were some adjacent roads that were not
although the authors used a [0/90/ ± 45] print path. Ahn et al. [2] in contact at all and therefore had no bond strength. Lack of con-
measured tensile strengths of 90◦ raster angle prints in the XY tact between some roads reduces the effective cross-sectional area
orientation with a negative and zero air gaps and obtained approx- to which load was applied contributing to knockdown in tensile
imately 12 and 4 MPa respectively. Rodriguez et al. [7] also printed strength.
specimens with 90◦ raster angle in the XY orientation with a nega-
tive air gap and obtained tensile strength of about 14 MPa. Rezayat 3.5. Print parameter effects on tensile strength
et al. [6] measured tensile strengths of approximately 25 MPa and
18 MPa for negative and zero air gaps respectively for specimens Relative effects of print parameters on tensile strength for XY
printed in the XY orientation. Huang et al. [3] measured the tensile and ZX coupons are shown in Fig. 9a and b respectively. For the
strength of printed ABS rectangular bars with 90◦ infill orientation XY orientation, printing with higher TE , slower speed, and larger
to be 10.08 MPa. For reference, ABS filament tensile strength was layer height increased tensile strength. This parameter combina-
reported as 33–37 MPa [3,6,7]. Literature results are summarized tion yields longer contact lengths between adjacent roads with
in Table 6. Variation in tensile strength among experimenters may increased local heating from the nozzle and increased time for
be attributed to differences in other print parameters, the machine molecular diffusion across road boundaries and hence is preferred
used to manufacture specimens, or differences in ABS material from for increased tensile strength. For the ZX orientation, TE effects
different manufacturers. were not captured because the coupons failed to print at low
Fractional contact length was expected to track with tensile extruder temperature. Slow speed and small layer height were
strength provided that there was sufficient time at temperature favorable in the ZX orientation. Small layer height in the ZX orien-
greater than Tg for molecular diffusion between roads and bond tation allowed for compaction between layers thereby increasing
formation to develop. Fig. 8 plots tensile strength of both XY and the contact length and opportunity for molecular diffusion. For the
36 A.C. Abbott et al. / Additive Manufacturing 19 (2018) 29–38

Table 5
Tensile strength results for coupons printed in both XY and ZX orientations.

TE (◦ C) Speed (mm/s) Layer height (mm) Tensile Strength (MPa)

XY ZX

230 10 0.1 20.2 ± 1.7 –


230 10 0.3 21.5 ± 0.2 –
230 50 0.1 10.2 ± 1.2 –
230 50 0.3 16.8 ± 1.2 –
270 10 0.1 22.4 ± 1.0 19.4 ± 7.2
270 10 0.3 22.0 ± 2.3 22.7 ± 0.8
270 50 0.1 15.1 ± 0.2 22.1 ± 2.1
270 50 0.3 22.8 ± 2.3 10.8 ± 1.1

Table 6
Summary of print parameters and ABS tensile strength from literature.

Author Orientation Infill angle (◦ ) Air gap Tensile strength (MPa)

Rayegani [1] ZX 0 Negative 24


ZX 0 Positive 9
Bellini [36] ZX 0/90/ ± 45 7.6
Ahn [2] XY 90 Negative 12
XY 90 Zero 4
Rodriguez [7] XY 90 Negative 14
Rezayat [6] XY 90 Negative 25
XY 90 Zero 18
Huang [3] XY 90 Negative 10.08

Fig. 9. Main effects plots of tensile strength as a function of print parameters.

XY orientation, low tensile strength was measured for faster print the variance between two or more populations is equal. By com-
speeds and lower TE . The combination of faster print speed and paring the variance, or mean squares, within a population to
smaller layer height also yielded poor mechanical properties. The that between populations, the null hypothesis is either accepted
highest tensile strengths were obtained with three print parame- (parameter has no statistically significant effect on the measure-
ter combinations which had high TE and: slow speed with small ment) or rejected (parameter has a statistically significant effect).
layer height; slow speed with large layer height; and fast speed In addition to examining the significance of individual parameters,
with large layer height. From a manufacturing standpoint, fabri- combining this technique with a full-factorial DoE allows for exam-
cation of mechanically robust products at a fast production rate ination of the significance of parameter interactions [37]. The F
of is most desirable. Aggregate results captured in Fig. 9a show value indicates the ratio of the variance between sample means to
that high TE , slow speed, and large layer height are preferable in the variance among samples [14]. Large F values imply high vari-
the XY orientation. Production rate, currently viewed as one hur- ability among the means. In other words, the higher the F value,
dle to wide adoption of additive manufacturing, is fastest with fast the greater chance that a parameter is significant. A parameter is
print speed and large layer height. For the XY orientation, this print deemed significant if the calculated F value is larger than a criti-
parameter combination along with high TE yielded good tensile cal F value defined by the confidence interval. A p value less than
strength. However, this same parameter combination printed in the significance level indicates that the parameter has a signifi-
the ZX orientation produced the lowest tensile strength. Fig. 9b cant effect on the measurement. The ANOVA approach has been
indicates slow speed and small layer height were favorable in the applied to other DoE studies on ME in literature [10–12]. A sig-
ZX orientation. Slow speed with high TE and large layer height nificance level of ␣ = 0.05, a 95% confidence interval, was used in
produced nearly identical tensile strength regardless of print orien- this study. Considering only XY orientation for which a full tensile
tation. Additionally, these tensile strengths were among the highest strength dataset was collected, all three parameters had significant
recorded in this study and therefore present a possible combination effects based on p < 0.05 as shown in Table 7. There was only one
for production of quality parts while mitigating print orientation degree of freedom (DF) for the XY orientation. Two interactions
concerns. between parameters were found to be significant: speed*TE , and
Analysis of variance (ANOVA) was performed to identify which speed*layer height. Including both XY and ZX orientations in the
print parameters had statistically significant effects on tensile analysis yielded print speed as the only significant parameter as
strength. An ANOVA is performed with the null hypothesis that
A.C. Abbott et al. / Additive Manufacturing 19 (2018) 29–38 37

Table 7
ANOVA table for XY orientation tensile strength.

Source DF Mean Square F Value p

TE 1 0.733 13.06 0.0047


Speed 1 2.234 39.83 0.001
Layer height 1 1.129 20.11 0.0012
TE *Speed 1 0.315 5.62 0.0393
TE *Layer height 1 0.00005 0 0.9767
Speed*Layer height 1 0.694 12.38 0.0056
TE *Speed*Layer height 1 0.125 2.24 0.165

Table 8
ANOVA table factoring both XY and ZX orientations.

Source DF Mean Square F Value p

Orientation 1 10.49 0.48 0.4954


TE 1 59.95 2.72 0.1096
Speed 1 203.07 9.23 0.005
Layer height 1 21.04 0.96 0.3363

shown in Table 8. Interaction effects were not captured in Table 8 Acknowledgements


because the ZX dataset did not include coupons printed at low TE .
The authors would like to acknowledge Ronald Trejo and Dayle
Pearson for their assistance in performing mechanical testing and
digital image correlation. Richard Reibel and Sathish Shamachary
are acknowledged for lending the use of the IR camera.
4. Conclusions

Relationships between print parameters, thermal history


between roads, mesostructure, and tensile strength were studied
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