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Mode-1 Interlaminar FT For Additive Manufactured Polymer
Mode-1 Interlaminar FT For Additive Manufactured Polymer
Additive Manufacturing
journal homepage: www.elsevier.com/locate/addma
A R T I C LE I N FO A B S T R A C T
Keywords: This study presents development of a test method for characterization of interlayer, mode-I fracture toughness of
Additive manufacturing fused filament fabrication (FFF) materials using a modified double cantilever beam (DCB) test. This test consists
Interlayer fracture toughness of DCB specimen fabricated from using unidirectional FFF layers, an 8 μm Kapton starter crack inserted in the
Fused filament fabrication midplane during the printing process, and reinforcing glass/epoxy doublers to prevent DCB arm failure during
Fused deposition modeling
loading. DCB specimens are manufactured with a commercially available 3D printer using unreinforced
Acrylonitrile butadiene styrene
Acrylonitrile Butadiene Styrene (ABS) and chopped carbon-fiber-reinforced ABS (CF-ABS) filaments. To examine
the effect of the FFF printing process on fracture toughness, additional ABS and CF-ABS specimens are hot-press
molded using the filament material, and tested with the single end notch bend (SENB) specimen configuration.
The fracture toughness data from DCB and SENB tests reveal that the FFF process significantly lowers the mode-I
fracture toughness of ABS and CF-ABS. For both materials, in situ thermal imaging and post-mortem fractography
shows, respectively, rapid cool-down of the rasters during filament deposition and presence of voids between
adjacent raster roads; both of which serve to reduce fracture toughness. For CF-ABS specimens, fracture
toughness is further reduced by inclusion of poorly wetted chopped carbon fibers. Although this study did not
attempt to optimize the fracture performance of FFF specimens, the results demonstrate that the proposed
methodology is suitable for design and optimization of FFF processes for improved interlayer fracture perfor-
mance.
⁎
Corresponding author.
E-mail address: m.czabaj@utah.edu (M. Czabaj).
1
Fused Filament Fabrication is a material extrusion technology as per ISO/ASTM 52900.
https://doi.org/10.1016/j.addma.2018.02.023
Received 15 November 2017; Received in revised form 7 February 2018; Accepted 21 February 2018
Available online 06 June 2018
2214-8604/ © 2018 Published by Elsevier B.V.
D. Young et al. Additive Manufacturing 22 (2018) 508–515
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D. Young et al. Additive Manufacturing 22 (2018) 508–515
Fig. 3. Schematic of the FFF plaque used for manufacturing of DCB specimens.
during printing. The printing was performed using a Lulzbot TAZ 5 FFF Hysol® (Henkel; Dusseldorf, Germany) structural adhesive mixed with
printer (Aleph Objects, Inc.; Loveland, CO, USA) placed inside of a 0.59 mm dia. glass beads. The cure was performed at room temperature
Plexiglas® (Arkema; King of Prussia, Pennsylvania, USA) enclosure to and 765 KPa pressure for 24 h. The room temperature cure was ne-
minimize cooling due to ambient air currents. Prior to printing, the cessary to avoid buildup of thermal residual stresses caused by differ-
print bed was coated with a thin layer of Avery® Permanent Glue (Avery ential thermal expansion of ABS relative to G10. Note that surface
Products Corporation; Strongsville, OH, USA) to promote adhesion to preparation and adhesive were chosen specifically for ABS-to-G10 ad-
the extruded filament. hesion, and may not apply to other FFF and doubler materials. Also,
To simplify placement of the Kapton insert mid-print, all specimens depending on the flexural stiffness of other FFF materials that may be
were printed at a speed of 35 mm/s. Placement of Kapton between the studied with this method, alternative doubler thicknesses should be
10th and 11th layer was done using a custom U-shaped jig as depicted considered.
in Fig. 4. The Kapton film was stretched taut across the arms of the jig After cure, the resulting sandwich plate was cut to exact specimen
and taped in place using adhesive Kapton tape. Prior to placement, the dimensions given in Fig. 2, using a 1.6 mm thick diamond saw blade.
Kapton film was coated with Avery® glue to promote adhesion to the Aluminum MW2001-6 loading hinges from Genuine Aircraft Hardware
extruded filament. The actual placement was performed without stop- Co. (Paso Robles, CA, USA) were adhered to the doublers using Loctite®
ping the printing process. This was achieved by opening the enclosure 9460TM Hysol® and a custom hinging jig. Prior to adhesion, the hinges
door and quickly butting the jig against the specimen while the nozzle were sandblasted and cleaned with isopropyl alcohol. After hinging, a
was in the final stage of printing the 10th layer. After completion of the band saw was used to cut a notch through the leading 8 mm of material
printing process, all specimens were carefully detached from the print allowing the crack faces to freely open. The final configuration of the
bed and rinsed with water to remove excess Avery® glue. DCB specimen modified for FFF materials is depicted in Fig. 5. In total,
The next step of specimen manufacturing was the adhesion of the 6 ABS and 5 CF-ABS specimens were manufactured. DCB specimens
doubler material. To promote good adhesion between the ABS material were numbered with the designation “material-Y-X”, where “material”
and the doublers, all mating surfaces were textured by surface abrasion. is ABS or CF-ABS, Y is the plaque number, and X is the specimen
The top and bottom surfaces of the FFF specimen were abraded in two number.
steps. First, the surfaces were sand-blasted using 180 grade brown
aluminum oxide grit at 275 KPa. Second, a 240-grit sand paper was
used to manually abrade both surfaces until a consistent texture was 2.2. SENB specimens
achieved on both sides. The G10 doublers were sand-blasted using the
same grit and pressure, but manual abrasion was omitted. After surface The SENB specimens were made in accordance with ASTM D5045-
abrasion, the FFF specimens and doublers were wiped clean with iso- 14 [18] test method for fracture toughness of plastics materials. Resin
propyl alcohol. The adhesion was performed using Loctite® 9460TM plaques with dimensions of 76 mm × 76 mm × 6 mm were made from
both FFF filament feedstock by HPM. Strands of ABS and CF-ABS fila-
ment were chopped into 1–3 mm pieces, arranged in the mold, and
vacuum bagged. Both materials were cured at 230 °C for 105 min, fol-
lowed by a 60-min cool-down to room temperature. To achieve proper
consolidation, 766 kPa and 919 kPa pressures were used for ABS and
CF-ABS plaques, respectively. After cure, both plaques were trimmed
into rectangular beam specimens with dimensions of 44 mm × 10 mm
× 5 mm. Notches were made by first scoring one side of the SENB with
a jeweler’s saw, followed by tapping a razor blade into the notch to
extend the crack. Additional 3-point bend specimens were manu-
factured and left un-notched. These specimens were used to correct the
measured displacement for compliance of the testing apparatus, load-
pin penetration, and specimen compression.
In total, 6 ABS and 3 CF-ABS specimens were hot press molded.
Molded SENB specimens were labeled in the same manner as the DCB
specimens with the letter “M” appended to the end, to represent the
molding process (i.e. “material-Y-XM”).
Fig. 4. Placement of the Kapton insert in-between the midplane of the FFF
specimen.
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D. Young et al. Additive Manufacturing 22 (2018) 508–515
3Pc δc
GIc =
2ba (1)
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D. Young et al. Additive Manufacturing 22 (2018) 508–515
increment of growth. A summary of these data for ABS and CF-ABS The apparent reduction of mode-I fracture toughness in FFF speci-
specimens is presented in Table A1 of the Appendix A. For complete- mens can be linked directly to the manufacturing process. As shown in
ness, Table A1 of the Appendix A includes GIc−NPC calculated based on Fig. 8, extrusion of filament during FFF results in formation of evenly
5%-offset and maximum-load definitions of Pc. The same data are de- spaced inter-raster voids, which decrease the total surface area involved
picted in Fig. 7 as a function of crack extension, Δa. In this figure, in- in the fracture process. However, Eq. (1) assumes that the crack surface
itiation toughness at Δa = 0 (i.e. GIc−NPC) is based on the 5%-offset area is equal to the entire specimen width, b, times the crack length, a.
method. In addition to the DCB data, Fig. 7 includes toughness values of Since the actual width of the fractured material is less than b, Eq. (1)
molded ABS and CF-ABS measured using the SENB test. Given the in- underestimates the actual fracture toughness (i.e. energy per area)
herently unstable nature of crack extension in the SENB tests, only one needed to fracture FFF rasters. To estimate the “true” fracture tough-
value of toughness was recorded per specimen. Also, since all specimens ness of ABS and CF-ABS rasters, GIc-raster, the effective specimen width,
are initially precracked by tapping a sharp razor blade into a pre-ma- b*, involved in the fracture process was measured directly. This was
chined notch, all toughness values from SENB specimens are referred to done by optically imaging fracture surfaces of all tested specimens, and
as PC (i.e. measured from a sharp, naturally occurring crack front). using grayscale thresholding to subtract from the nominal specimen
Consequently, SENB data in Fig. 7 are presented as single points width the cumulative width of the inter-raster voids. This analysis
(hollow symbols) at Δa ≅ 0, with error bars corresponding to plus/ showed that, on average, inter-raster voids corresponded to 38% and
minus one standard deviation in toughness. The summary of toughness 11% of width for ABS and CF-ABS specimens, respectively. Given the
data from SENB tests is presented in Table A2 of the of the Appendix A. corrected width for all specimens, the fracture toughness values for all
Following fracture toughness testing, several FFF specimens were FFF specimens were recalculated using Eq. (1) and plotted in Fig. 9. As
split open and imaged using a scanning electron microscope (SEM). The seen in this figure, for ABS specimens, the width correction resulted in
SEM imaging was performed with magnification of 50x, 300x, and average GIc-raster that was approximately 17% lower than GIc from SENB
1000x. All specimens were imaged within the region of stable crack specimens. The width correction did, however, result in a large scatter
growth, which was determined based on the force versus crack-exten- in the toughness data, which was likely caused by variability in ex-
sion data. Fig. 8 depicts a set of representative SEM images obtained for traction of b* using an optical method. For CF-ABS, GIc-raster increased
each material type, with ABS and CF-ABS shown in the left and right marginally, and remained almost 7 times lower than GIc from SENB
columns, respectively. In all six micrographs, the direction of macro- specimens.
scopic crack growth is from right to left, as indicated. The white square
boxes in the upper four images indicate regions that were examined at a 4.3. Effect of print temperature
higher magnification.
Examining Fig. 8, at 50x the ABS fracture surfaces are textured, The data in Fig. 9 suggests that the presence of inter-raster voids has
clearly showing resin ridgelines and evidence of textured microflow a strong effect on the apparent fracture toughness of FFF parts; how-
that is inherent to mode-I crack growth in polymers [21]. Images of ABS ever, excessive voiding does not fully explain the significant reduction
at 300x and 1000x show that the surface roughness is caused by sig- in toughness, especially for the CF-ABS specimens. To investigate this
nificant plastic deformation during crack growth. The CF-ABS fracture further, a selected number of specimens were imaged using a FLIR 2420
surfaces appear much smoother at 50x, showing little evidence of (FLIR® Systems, Inc.; Wilsonville, OR, USA) thermal camera in situ
ductile deformation during crack growth. At 300x and 1000x, the CF- during the printing process of the midplane layers. An example of this
ABS fracture surfaces reveal a large number of short carbon fibers, imaging is presented in Fig. 10, where the left image shows the full-field
which are either completely separated from, or only partially bonded temperature of the print, and the right plot shows the temperature
to, the surrounding ABS resin. The CF-ABS specimens show very little profile along the newly printed raster. Note that the left image is plotted
evidence of fiber pull-out or fiber bridging across adjacent rasters, on a plateau equalization scale to enhance the contract between the
newly deposited raster and the surrounding material. Examining
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D. Young et al. Additive Manufacturing 22 (2018) 508–515
Fig. 8. Representative fracture surfaces from ABS (left) and CF-ABS (right) specimens. The scale bars on the left apply to both sets of images. The white boxes indicate
magnified regions in subsequent micrographs. Inter-raster voids are indicated with white arrows.
Fig. 10, the ABS raster temperature drops by nearly 100° C in the first
second after deposition, and reaches the glass transition temperature of
105° C in approximately 4 s. The CF-ABS rasters cool much quicker, and
reach 105° C in approximately 1 s. Within 4.5 s, both rasters reach their
respective bed temperatures of 95° C and 60° C. Similar observations
were reported in Ref. [22], suggesting that rapid raster cooldown
during FFF is not specific to this study. By comparison, specimens
created using HPM remain at temperature of 230° C for the entire mold
time of 105 min, allowing polymer chains sufficient time to fully en-
tangle. The quick cool-down of FFF rasters, especially for CF-ABS parts,
leave little time for proper polymer chain entanglement, effectively
reducing the bond strength between adjacent rasters.
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D. Young et al. Additive Manufacturing 22 (2018) 508–515
to pure ABS. This effect, in combination with voiding and processing develop a reproducible test method. In order to more fully understand
temperature, is the likely explanation for a nearly ten-fold reduction in the differences between interlayer toughness of the two FFF materials
mode I fracture toughness of FFF CF-ABS compared to HPM CF-ABS. described herein, a more in depth investigation may be required. It is
possible that careful optimization of the print conditions can sig-
5. Conclusions nificantly improve the interlayer toughness of the CF-ABS materials.
This, however, was not the main focus of this work, and is currently a
This study presents a test methodology for characterization of in- subject of a separate ongoing study. Nevertheless, the above discussion
terlayer fracture toughness of FFF components using a modified version demonstrates that the proposed DCB test can act as an effective tool for
of ASTM D5528 standard. DCB specimens were manufactured with a screening interlayer performance of FFF components and various
commercially available 3D printer using pure ABS, and ABS reinforced manufacturing processes. This method, combined with other material
with short carbon fibers. Novel contributions of this work include: 1) characterization tests developed specifically for polymeric FFF com-
design of unidirectional FFF DCB specimens; 2) insertion of Kapton ponents, may prove critical for their broader acceptance in structural
starter cracks during the printing process; 3) adhesion of reinforcing applications.
glass/epoxy doublers to prevent DCB arm failure during loading; 4) and
data analysis based on fractographic imaging and in situ full-field Funding
monitoring of the print temperature using a thermal camera. The test
data obtained in this study revealed that, if not properly optimized, the This work was supported by NASA Langley Research Center [grant
FFF process can significantly reduce mode I fracture toughness relative number NNX14AQ74A].
to parts manufactured using HPM. Detailed investigation of the FFF
specimens attributed reduction in fracture toughness to the presence of Acknowledgements
inter-raster voids which are inherent to the FFF process, and the rapid
cool-down of rasters during filament deposition. For CF-ABS specimens, This work is funded by NASA Langley Research Center (Grant No.
toughness was further reduced by inclusion, and poor wetting, of the NNX14AQ74A) with Dr. Emilie J. Siochi as the grant monitor. Authors
chopped carbon fibers. would like to thank Dr. Siochi and Dr. James Ratcliffe from NASA LaRC
It must be noted that during the course of this research, no attempts for their invaluable technical support. In addition, the authors would
were made to optimize the FFF processing parameters to improve the like to thank Mr. Jim Baughman from NASA LaRC for help with the
fracture toughness. Rather, processing was optimized to create DCB SEM analysis, and Mr. Jeff Kessler for the Utah Composites Laboratory
specimens with good dimensional quality, which was necessary to for help with fracture toughness testing.
Appendix A
Table A1
Summary of fracture toughness data from ABS and CF-ABS specimens, along with the corresponding averages (AVG), standard deviation (SD), and coefficients of
variation (CV).
Sample 5% offset MAX GIc-PC (kJ/m2) GIc-avg (kJ/m2)
GIc-NPC (kJ/m2) GIc-NPC (kJ/m2)
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D. Young et al. Additive Manufacturing 22 (2018) 508–515
Table A1 (continued)
Table A2
Summary of fracture toughness data from SENB tests.
ABS CF-ABS
2
Sample GIc-NPC (kJ/m ) Sample GIc-NPC (kJ/m2)
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