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Abstract
Surface preparation before adhesive bonding is crucial to improve the resistance and durability of the joint by altering the
surface properties of the adherend. The purpose of surface treatment is to clean the surface from contaminants, activate
the adherend surface and create an optimal surface structure to promote adhesion mechanisms. In that context, this
work aims to investigate the influence of substrate surface texturing on the resistance of adhesive joints. Two bio-inspired
surface textures were investigated, Fish scale (FS) and Tree frog (TF). Polycarbonate (PC) specimens with different surface
patterns were manufactured using the fused deposition modelling process. Surface morphology, such as pattern dimen-
sion (shape and depth), surface roughness (Ra), and wettability, were used to characterise the substrates. The influence of
these texture patterns on the shear strength of adhesively bonded joints was evaluated through the standardised block
shear test method ASTM D4501-01. Moreover, the shear strength of the structured joints was compared to the results
from bonding with polished surfaces (surfaces abraded with 80, 600 and 1000 grit paper), and with as-printed surfaces.
The results revealed that the FS and TF surface textures enhanced the shear strength by 242% and 283% compared to the
adhesive joints with polished surfaces. It was also shown that the variation in depth of the bio-inspired surface texture has
no significant impact on the joint strength. Failure analysis demonstrated that the fracture mode of bonded joints with
polished surfaces was the adhesive failure while mixed failure (cohesive and adhesive) characterises the as-printed, TF
and FS surfaces. Worthy results are obtained rising the effectiveness of surface texture for the PC’s bonded joints.
Graphical Abstract
1
Mechanical Engineering Laboratory, National Engineering School of Monastir, Monastir University, Monastir, Tunisia
2
Faculty of Civil Engineering CVUT, Department of Steel and Timber Structures, Czech Technical University in Prague, Prague, Czech
3
College of Engineering, Jazan University, Jazan, Saudi Arabia
4
Faculdade de Engenharia, Departamento de Engenharia Mecânica, Universidade do Porto, Porto, Portugal
Corresponding author:
N Naat, Mechanical Engineering Laboratory, National Engineering School of Monastir, Monastir University, Monastir, Tunisia.
Email: naatnidhal@yahoo.fr
2 Proc IMechE Part L: J Materials: Design and Applications 0(0)
Keywords
Adhesive bonding, bio-inspired surface texture, additive manufacturing, wettability, shear strength, mechanical
interlocking
Date received: 23 July 2022; accepted: 15 October 2022
cantilever beam joints with bio-inspired 3D-printed surfaces. as transparency, high toughness, biocompatibility and
The authors found that bio-inspired subsurface channels sig- high-temperature resistance. Thereby, PC material is
nificantly increased the total dissipated energy compared to used in optical applications, microfluidic and medical
bulk specimens (i.e. no channels). (e.g. prosthetics, blood filters) devices. PC filament
Various manufacturing methods such as laser, lithog- (Raise3D Premium PC, China) was used to manufacture
raphy and additive manufacturing (AM) have been all the experimental substrates. The characteristics of the
employed to produce structured surface textures. The selected PC are shown in Table 1.
free shape of the 3D-printed parts allows the manufactur- A two-component high-performance, brittle and bio-
ing of various simple and complex structured surfaces to compatible epoxy adhesive (LOCTITE® EA M-121HP
investigate the effect of surface texturing on the resistance from Henkel AG & Co. KGaA, Düsseldorf, Germany)
of bonded joints.22–25 Despite the strong development of was chosen. Table 2 shows the technical specifications,
the AM process, the relationship between structural adhe- as given in the manufacturer’s datasheet.
sives and structured surface texturing of AM components
has not yet been fully understood. Furthermore, the intel-
ligent combination of adhesive bonding and AM technol- Specimens preparation and surface treatment
ogy can be very useful for overcoming one of the major
limitations of AM (the limited bed size of AM machines), Tree frog (Litoria caerulea) toe pads are hierarchically struc-
improving the joint strength by exploiting the capacity of tured with a regular hexagonal pattern of epidermal cells
the AM to tailor a suitable surface texture of a part, and with a diameter of around 10 µm and spaced by 1 µm
manufacturing parts with structured surfaces in one step. wide and deep channels; each epidermal cell consists of
This work aims to investigate the mechanical perfor- thousands of columnar nanopillar peg microstructures
mances of bonded AM specimens with bio-inspired (100–400 nm). The nanopillars have a (mostly) hexagonal
surface textures compared with traditional adhesive outline separated by wide and deep channels of about
bonding on abraded surfaces or with the monolithic 100 nm (Figure 1).5, 6 On the other hand, fish (e.g.
joint (directly printed with an AM machine). The influ- rainbow trout) are covered with oriented scales (diameters
ence of different surface textures on joint strength and of 2–5 mm and height of 200 µm) and arrange into an
adhesion behaviour is investigated using experimental array. The surface of the individual scale consists of micro-
block shear tests. Results show that the bio-inspired papillae with 100–300 µm in length, 30–40 µm in width and
surface textures greatly increased the shear strength of 10 µm in height oriented in the radial direction (Figure 2).7, 8
bonded joints, compared with the abraded surface. Thus, To facilitate the manufacturing of these two hierarchical
the bio-inspired structured surface enhanced the joint bio-inspired textures via a fused deposition modelling
resistance by mechanical interlocking at the macroscopic (FDM) 3D printing machine, multiplier scale factors have
scale. been used to build the geometric models of the two textures,
as shown in Figure 3 (Tree frog) and Figure 4 (Fish scale).
Solidworks software was used to design the PC adher-
ends. Once the STL files were created, they were uploaded
Experimental details into ideaMaker, a 3D slicing software. Then, G-code files
were generated by using ideaMaker. Afterwards, the PC
Materials substrates were manufactured layer by layer via a
Polycarbonate (PC) is an engineering amorphous thermo- Raise3D Pro2 printer with PC filaments in a diameter of
plastic, which is characterised by its specific features, such 1.75 mm, as shown in Figure 5. The process parameters
Polycarbonate
Young’s modulus Tensile strength Elongation at Flexural modulus Flexural strength Glass transition
(MPa) (MPa) break (%) (MPa) (MPa) temperature (°C)
2307 ± 60 (ASTM 62.7 ± 1.3 (ASTM 3.2 ± 0.4 (ASTM 2477 ± 159 (ASTM 100.4 ± 2.7 (ASTM 113 (DSC, 10 °C/min)
D638) D638) D638) D790) D790)
Table 2. Main physical and mechanical properties of the chosen adhesive (manufacturer’s datasheet).
LOCTITE® EA M-121HP
Viscosity (cP) Glass transition Working life (min) at Elastic modulus Tensile strength Elongation at break
at 25 °C temperature (°C) 25 °C (MPa) (MPa) (%)
11,000 (mixed) 90 (ASTM E 228) 120 1490 (ISO 527-2) 40.7 (ISO 527-2) 10 (ISO 527-2)
4 Proc IMechE Part L: J Materials: Design and Applications 0(0)
Figure 1. (A1–A4) Surface texture of Tree frog (Litoria caerulea) toe pads. (B1–B3) Geometrical model of the ventral toe pad texture.
(dp: diameter of ventral pad, dc: diameter of polygonal epidermal cells, CH: channel, wc: channel width, NP: nanopillar, dn: diameter of
polygonal nanopillar, wn: channel width, DI: dimple, Δr: distance between dimple and nanopillar edge).5,6
Figure 2. (a) Optical and (b) scanning electron microscopy (SEM) images of the Fish (Rainbow trout) scales surface texture.7
of PC specimens for the FDM 3D printing machine were Table 3. Fused deposition modelling (FDM) process
listed in Table 3. parameters.
Up to now, there are no standardized testing methods for Parameter Value
polymeric AM adherends. As noted in Forster’s NIST
report,26 current standards are not applicable for AM adher- Nozzle diameter 0.2 mm
ends and specific modifications are needed. Most of the Extrusion temperature 260°C
research works in the literature adopt single lap joints Bed temperature 110°C
(SLJ). For this reason, PC adherends were firstly printed Printing speed 60 mm/s
Layer height 0.1 mm
according to the standards ASTM D3163-01.
Infill density 100%
Unfortunately, the warping effects did not allow the manu-
Enable print cooling No
facturing of the specimens (Flatwise and edgewise orienta-
tions). This effect is due to shrinkage of material and
residual stress because there is a large temperature gradient D4501-01 was adopted. The specimens were printed in
between the formed parts and the surrounding environ- the edgewise orientation and then cooled to room tempera-
ment.27 Therefore, the block shear test method ASTM ture after printing.
Naat et al. 5
Figure 3. Geometric model of Tree frog texture (TF0.75) (all dimensions in mm).
Three test groups were established for the specimens standard. Three measurements were performed at differ-
based on the following surface treatment: ent locations, and then an average was calculated for
each surface texture. Ra was the arithmetic mean devi-
1. Bio-inspired group: 3D-printed TF and FS specimens ation of the profile (µm), Rq was the root mean square
with structured hierarchical surface textures were deviation of the profile (µm) and Rz was the maximum
cleaned using isopropanol. height of the profile (µm).
2. As-printed group: 3D-printed specimens with The static contact angle was measured using the sessile
a structured surface (from the inherent FDM drop method. Thus, a drop shape analyzer DSA25
manufacturing process) were cleaned using (KRÜSS, Germany) was used for measuring the water
isopropanol. contact angle (WCA) under atmospheric conditions using
3. The abrasion treated group (according to ASTM the Young-Laplace method. The 15 μL of distilled water
D2093-03): the as-printed surface was solvent was dispensed onto the surface of the substrate and the
cleaned (isopropanol), then abraded with 80, 600 and droplet contact photograph was captured after stabilization.
1000 grit paper for 1 min along one direction (perpen- For FS texture, there is one measurement position.
dicular to the loading direction), followed by further However, for TF texture, there are three measurement
solvent cleaning (isopropanol). positions (Position1: On a large hexagon, Position 2:
between three large hexagons, Position 3: between two
large hexagons). For each position of FS and TF textures,
a minimum of three measurements were performed in
Surface characterization each of the two directions (transversal and longitudinal).
The surface topography profile and roughness including Then, an average result was obtained for each texture.
Ra, Rq and Rz of as-printed and abraded specimens were Figure 6 shows the measurement positions on TF and
measured using a contact type profilometer (Surtronic FS structured textures using the contact angle goniometer
S-128, Taylor Hobson, UK) according to the ISO 4287 ‘KRÜSS DSA25’.
6 Proc IMechE Part L: J Materials: Design and Applications 0(0)
Figure 4. Geometric model of Fish scale texture (FS0.4) (all dimensions in mm).
To observe the interfacial wetting between adhesive cured for 48 h under a pressure of 0.1 MPa. Finally, a file
and substrates, cross-sections of TF and FS bonded joints is used to remove excess adhesive from the sides of the
were made: firstly, the bonded specimens were cut using joints.
a circular saw. Then, the cut sections were polished with To clamp the specimen in place and minimize the
600 and 1000 grit papers, respectively. After, they were peeling effects that occur during SLJ shear tests, a special
cleaned with isopropanol. Finally, cross-sectional fixture is required for block shear testing. Therefore, it
views of TF and FS bonded joints were taken via was necessary to develop and manufacture this fixture, as
digital photography. shown in Figure 9. One half of the specimen was positioned
in the holding block of the fixture and the shearing tool con-
tains a slot to grip the other half of the specimen. Tension
Test methods was applied to the holding block of the fixture, while the
The block shear test method ASTM D4501-01 was adopted shearing tool remained static. The samples were tensile
for shear strength testing of 3D printed PC bonded joints. tested in a LLOYD 20 kN testing machine. For each case
The full specimen with corresponding dimensions is examined, at least three samples were produced. The
reported schematically in Figure 7. samples were tested under monotonic loading at room tem-
A special mould was designed and manufactured perature with a crosshead speed of 1.3 mm/min. After each
(Figure 8), to ensure the substrates’ alignment, overlap test, the maximum load was registered, and the failure
length and adhesive thickness. Therefore, 3D-printed modes were recorded and visually inspected.
shims made of polylactic acid were used to achieve the On the other hand, full specimens (monolithic joints)
desired thickness (0.2 mm) and overlap length (12.5 mm) with the same geometry as the bonded specimens, printed
of the adhesive with high precision. After the surface treat- as a single part (Figure 10), were also tested to compare
ment, the adhesive was mixed and applied evenly to both the adhesive’s shear strength and the interlayer shear
surfaces to be joined. Then, the bonded substrates were strength of the 3D-printed materials.
Naat et al. 7
Figure 5. Fused deposition modelling (FDM) 3D printing machine and the 3D-printed PC substrates.
Figure 6. (a) Positions of measurements and (b) Contact angle measurements on water drops via a contact angle goniometer ‘KRÜSS
DSA25’.
8 Proc IMechE Part L: J Materials: Design and Applications 0(0)
Figure 7. Geometric parameters of block shear test (ASTM D4501) (all dimensions in mm).
Results and Discussion Rq and Rz, both height parameters. The Ra value of the
abraded sample with P1000 grit paper is the lowest,
Morphology around 260 nm. This reveals that this treatment generates
a flatter and more homogeneous surface, formed by small
Figure 11 illustrates the surface roughness profiles corre-
peaks and valleys.
sponding to as-printed and abrades surfaces. The as-printed
Figure 12 shows digital photographs of the bio-inspired
surface (Figure 11(a)) showed a regular striped pattern,
surface texture of 3D-printed PC substrates. The FS
resulting in a rough surface. The periodicity of the
surface exhibited a regular fish-scale macrostructure
contour surface is governed by the layer height, which
(Figure 12(a)). While the TF surface (Figure 12(b))
has sizes of 100 μm. In addition, the extrusion parameters
showed a regular and hierarchical hexagonal macrostruc-
and cooling conditions of the FDM 3D printing machine
ture (each large hexagon contains 24 small hexagons).
affect the feature sizes. McLouth et al.28 showed that the
Furthermore, the as-printed microstructured texture (with
texture of the lateral surfaces is a kind of micro-curvature.
an ellipsoidal shape) resulting from the intrinsic FDM
Since the material is extruded over the previous layer and
manufacturing process, also exists on the surface of
pushed outwards to form an ellipsoidal shape. On the
bio-inspired textures. On the other hand, it is observed
other hand, the abrading treatment removes the as-printed
that the morphology of 3D-printed bio-inspired surfaces
texture and forms an anisotropic stochastic texture (parallel
is in good agreement with the morphology and the size
grooves).
of the designed ones.
The following conclusions can be drawn from a com-
parison of the data reported in Table 4 and Figure 11.
The as-printed surface showed the highest roughness with
an ellipsoidal shape. For mechanical abrasion treatment,
Wettability
an increase in grain size of the grit paper causes a propor- According to wetting theories, the interfacial wetting of a
tional increase of Ra. Similar behaviour is observed for solid surface through a liquid is influenced by two main
Naat et al. 9
Figure 10. (a) Geometric model (dimensions in mm) and (b) 3D printed full specimen.
Treatment
Figure 11. Surface roughness profiles of polycarbonate substrates: (a) As-printed, (b) abraded with 80 grit paper and (c) abraded with
1000 grit paper.
Figure 12. Photographs of 3D-printed bio-inspired textures, (a) Fish scale, (b) Tree frog.
factors: the texture of the solid surface and the surface Young’s equation,30 the WCA of 90° was identified as
energy of the solid and liquid.3 On the other hand, the θIWT. However, by considering the interphase water mol-
surface texturing decreases the WCA when the measured ecule interactions and structures, a lower θIWT of 65° was
WCA on a flat solid surface is smaller than the intrinsic proposed.31 In this study, only the surface texturing param-
wetting threshold angle of the water (θIWT). Contrarily, eter has been changed.
when the WCA on a flat solid surface is larger than θIWT, WCA measurements were plotted in Figure 13 as a func-
the surface texturing increases WCA.29 Based on tion of surface texture. All tested textures followed similar
Naat et al. 11
Figure 13. The water contact angle of 3D-printed specimens for different surface textures.
Figure 14. Typical force-displacement curves for different configurations of PC/PC joints.
trends; the increase of surface roughness increased WCA. shape, size and distribution on the surface have a great
The WCA of the abraded surface with P1000 (smoother influence on the surface wettability.
surface) is larger than θIWT (65°).31 The as-printed, P80 The increase in WCA is due to a macro and micro-
and bio-inspired textures (rough surfaces) exhibited a geometric barrier effect resulting from the surface textur-
mainly hydrophobic behaviour, as measured WCA ing that prevents the free spreading of the water droplet on
ranged between 93.5° (FS) and 113° (TF). However, the substrate surface.4 The high dispersion of the WCA
P600 and P1000 abraded surfaces (smooth surfaces) measurements is due to the anisotropy of the surface tex-
showed hydrophilic behaviour. Therefore, features’ tures because asymmetric drops with non-circular three-
12 Proc IMechE Part L: J Materials: Design and Applications 0(0)
phase contact lines were obtained. These drops spread more The average shear strength measurements, and corre-
easily in one direction than in the other.32 On the other sponding standard deviations, for bonded joints composed
hand, for the smoothest surface (abraded with P1000), the of different surface textures, are shown in Figure 15. This
roughness isotropy is increasing because the abrading graph shows that the smooth surfaces (abraded with P600
lead to the flattening of the surface asperities (very low and P1000 grit paper) give the worst results. In this case,
barrier effect). Therefore, the droplet spread more easily the joint strength correlates with the wettability and the
and has a more uniform apparent contact angle distribution decrease of WCA from 87° (P600) to 67.6° (P1000)
(circular three-phase contact lines) with low dispersion. increases shear strength by 51%. Thus, the effect of phys-
ical adsorption is more significant than mechanical inter-
locking due to a very low roughness. The as-printed and
Shear strength P80 textures improved the shear strength by 174% and
The surface texture and wettability play a key role in adhe- 162% compared to the P600 specimens, respectively.
sion properties, which is beneficial for enhancing bonding Therefore, both textures showed that the shear strength
strength. Therefore, the influence of surface texturing on increased with increasing surface roughness. For substrates
the shear strength of bonded joints needs to be further with bio-inspired FS and TF textures, the shear strength of
investigated. corresponding bonded joints was 21.05 and 23.59 MPa,
Preliminary shear tests (not reported here) were per- which was increased by 25%, and 40% compared to
formed to see the influence of the depth of the FS and TF as-printed specimens, respectively. As a result, the TF
structured textures. It was found that increasing the depth pattern showed the highest joint strength compared to the
of the bio-inspired surface texture on a macroscopic scale other textures.
does not have a significant influence on the strength of the The enhancement of joint strength after surface texturing
bonded joint. The depths that gave the maximum shear was demonstrated following three aspects: (i) The extended
strength were chosen. Thus, Figures 3 and 4 showed the contact area. (ii) The increase in surface roughness pro-
optimum depths of TF and FS textures, respectively. moted the mechanical locking effect.34–36 (iii) The
Figure 14 illustrates the evolution of the force versus dis- improved wettability allowed the adhesive to better pene-
placement for different types of surface textures. The typical trate the texture. It is known that there is an optimum rough-
curves exhibit the same trend with a similar slope. Two ness range, outside of which the bond strength decreases.
regions can be identified: firstly, the load increases slightly, Indeed, the mechanical interlocking disappears due to inad-
and then it rises to failure. This fact depends mainly on the equate penetration of adhesive on smooth surfaces. For
behaviour at the adherend/adhesive interface. However, the very rough surfaces, insufficient wetting occurs (air can
force-displacement curve for P600 treatment is different be entrapped in the asperity valleys) and then joint resist-
from the others. This behaviour could be explained by the ance decreases.37–39 In this study, TF and FS textures
very low transmitted load through the adhesive along the exhibited poor wettability (Figure 13). However, the
interface because there is no mechanical interlocking, and shear strength was greatly improved (Figure 15).
the physical adsorption is the lowest compared to other treat- Therefore, due to the complexity of surface textures, it is
ments. Therefore, the load rises faster to failure and the crack insufficient to analyse the effect of surface texture on the
propagates faster.33 bond strength from a physical adsorption perspective.17
Naat et al. 13
Figure 16. Failure mode of block shear specimens for (a) P600, (b) P1000, (c) P80, (d) As-printed, (e) TF and (f) FS surface textures.
In this case, the great improvement of joint strength for fracture occurred at the interface between the adher-
bio-inspired textures can be mainly attributed to the end and the adhesive, suggesting little or no mechan-
increased contact area and mechanical interlocking effect. ical interlocking effect, which leads to the lower
bond strength.
(ii) Mixed failure (cohesive and adhesive) with a high per-
Failure analysis centage of adhesive failure, for the specimens as-printed
Figure 16 shows how texturing a surface modifies the and abraded with P80 grit paper. In this case, the crack
failure mode. The fracture surfaces exhibited the follow- runs close to the interface on opposite sides and meets
ing failure modes: roughly in the middle of the overlap.40 Therefore, the
increased contact area and some degree of mechanical
(i) Adhesive failure, for the substrates abraded with locking contribute to the improvement of bond strength,
P600 and P1000 grit paper (smooth surfaces). The compared to smooth surfaces.
14 Proc IMechE Part L: J Materials: Design and Applications 0(0)
Figure 17. Cross-sectional view of adhesive bonded joint for (a) TF and (b) FS textures.
Figure 18. Mechanical models for (a) smooth surfaces (P600 and P1000), (b) P80, (c) As-printed, (d) FS and (e) TF textured surfaces
(Fs: shear force, Fp: physical force, Fm: Mechanical interlocking force, Mb: generated bending moment).
(iii) Mixed failure (cohesive and adhesive), for the speci- observed in the TF grooves and on the FS scales,
mens with bio-inspired textures with wider areas of which proved the effectiveness of mechanical inter-
cohesive failure in the adhesive compared to locking between the textured adherends and the
as-printed and P80 textures. The adhesive was adhesive.
Naat et al. 15
6. Mechanical models are suggested based on different 10. Chen H, Zhang P, Zhang L, et al. Continuous directional
adhesion mechanisms and failure modes. The hexagonal water transport on the peristome surface of Nepenthes alata.
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Declaration of conflicting interests
texturing of hydroxyapatite ceramics: influence on the adhe-
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the research, authorship and/or publication of this article. Funct Biomater 2020; 11: 1–20.
17. Liu X, Zhu H, Xie Y, et al. Optimization of microstructural
Funding morphology via laser processing to enhance the bond strength
The authors received no financial support for the research, author- of Al-CFRP. J Reinf Plast Compos 2021; 40: 463–473.
ship, and/or publication of this article. 18. Salstela J, Suvanto M and Pakkanen TT. Influence of hier-
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ORCID iDs on adhesion between aluminum and epoxy. Int J Adhes
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N Naat https://orcid.org/0000-0002-8274-4796 19. Wan H, Min J, Carlson BE, et al. Spindle-Shaped surface
S Mezlini https://orcid.org/0000-0003-1209-4246 microstructure inspired by directional water collection biosys-
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