Influence of Raw Material Surface Roughening On TH
Influence of Raw Material Surface Roughening On TH
Influence of Raw Material Surface Roughening On TH
https://doi.org/10.1007/s00170-022-09590-6
ORIGINAL ARTICLE
Received: 9 January 2022 / Accepted: 21 June 2022 / Published online: 30 June 2022
© The Author(s), under exclusive licence to Springer-Verlag London Ltd., part of Springer Nature 2022
Abstract
Surface roughening of the substrates before bonding plays a significant effect on improving the mechanical performance
of the adhesively bonded joints, which are prevalently used for light-weighting vehicle bodies. In this study, the influence
of surface roughening on the lap shearing strength and failure behavior of adhesively bonded aluminum sheet joints was
investigated. Sandpaper grinding was employed for surface roughening; methods such as tensile testing and microstructure
observation were employed for evaluating the performance of the joints. The results showed that the lap shearing strength of
adhesively bonded joints increased and then decreased with the surface roughness of the aluminum substrate. The maximum
shearing strength of the joint bonded with grinded substrates was 30.4 MPa which was improved by 57.5% compared to that
produced with un-grinded substrates. However, over-roughening is harmful. When the surface roughness was too large, the
failure mode of the joint turned from the mixed failure mode to the interfacial failure mode, which decreased the strength
of the joints. Related mechanisms were demonstrated. When the substrate surface was coarsened, the bonding area and the
wettability of the adhesive on the surface were both increased, which promoted the beneficial mechanical interlock effect
between the adhesive and the substrate. However, when the substrate surface was over-roughened, defects such as voids and
insufficient infiltrating of the adhesive were induced, which apparently increased the proportion of the interfacial failure area.
Keywords Bonded aluminum joints · Surface roughness · Interfacial adhesion · Lap shearing strength · Failure behavior
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has a monotonic relationship with the surface roughness the increase in strength of adhesively bonded joints by surface
of the raw materials [6]. However, the results were exam- roughening, but they did not point out the failure behavior and
ined in a small surface roughness range. Several reports the strengthening mechanisms.
pointed out that there exists a most suitable surface rough- Different treatment types of adhesively bonded joints
ness for the raw materials which bring about the maximum exhibited different failure modes under tensile or shear load
tensile strength of the adhesively bonded aluminum joints conditions. Pietro Maressa et al. studied failure mechanisms
[7–11]. Tezcan studied the influence of surface roughness of the adhesively bonded Ti6Al4V sheets with laser processed
on the adhesively bonded joint strength under impact load- patterns on the surface and discovered partial cohesive failure,
ing with different strain rates. It was demonstrated that the fully cohesive failure, and textured substrates failure in vari-
lap shearing strength of the adhesively bonded joints will ous laser treatments [17]. Chen et al. investigated the damage
be a minimum value when the surface roughness Ra of the characteristics and failure behavior of hybrid materials joints
substrate was less than 0.1 μm or higher than 2.5 μm [12]. and reported that the adhesive joints showed a combined
Ghumatkar et al. treated the surface of adherend materials mode of fiber-tear failure, adhesive failure, and cohesive fail-
with sandpapers of different mesh numbers to obtain the ure [18]. The failure of the bonding surface can be prevented
most appropriate surface roughness and found that when by roughening the substrate surface. Surface roughening
the surface roughness Ra of the aluminum substrate and provides the beneficial mechanical interlocking between the
the steel substrate were 2.05 μm and 1.98 μm, respectively. aluminum substrate and adhesive, but over-roughening would
The maximum strength of the adhesively bonded joints reduce the wettability of the substrates; thus, the strength of
was 4.97 MPa and 6.78 MPa [13]. These studies help engi- the joints was weakened. Voids possibly occur at the bonding
neers to realize that the relevance between the lap shearing interface in this condition, which accelerates the crack propa-
strength of the adhesively bonded joints and the surface gation and lowers the strength of the interfacial force [19–21].
roughness of the raw materials is not linear. Nevertheless, For example, the influence of surface characteristics on the
the related mechanism of this phenomenon is still indistinct. strength of adhesively bonded aluminum joints was investi-
Using sandpapers with different mesh numbers, Ghumatkar gated by Boutar and found that the bonding quality decreases
et al. found that the surface roughness for aluminum substrates with increasing surface roughness [22]. In the study carried
could be achieved in a wide range by the various grinding direc- out by Yang et al. [23], it found that non-permeable zones, an
tion and duration [13]. Da Silva et al. verified the influence of alternation of solid–liquid-gas interfaces, were produced if
grooves and scratches on the joint strength with brittle adhe- the substrate was over-roughened which were both harmful
sives and ductile adhesives comparatively. The results showed to the bonding quality.
that scratches or grooves produced by grinded aluminum sub- Although engineers have realized the significance of
strate were harmless and even increase interface force [14]. the mechanical strength and failure behavior in designing
Mechanical technology, sandpaper grinding, for example, is adhesively bonded joints, investigation related to the rela-
still considered to be optimal for large-scale industrial produc- tionship between them is still few. The purpose of our cur-
tion in view of the operability, efficiency, and economic cost. rent work is to obtain a comprehensive understanding about
Clarifying the mechanisms for the strengthening of the the influence of the aluminum surface roughness on the lap
interface of the bonded metal joints through surface treatment shearing strength of adhesively bonded joints. Meanwhile,
of the raw material is crucial for the processing parameters failure behavior and the related mechanism of joints with
designing. In the study carried out by Ghumatkar et al., they different surface roughness were discussed systematically.
hold the opinion that the improved adhesion quality resulted In this research, the surface of aluminum sheets was treated
from mechanical interlocking between the adhesive layer and using sandpaper with different mesh numbers, and then the
metal surface [13]. Dong-Jun Kwon et al. investigated the samples were bonded with structural adhesive. The surface
influence of the surface roughness on the interfacial adhe- morphology, contact angles, surface free energy, and interfa-
sion strength of joints. Experimental results showed that the cial failure area of the samples were compared and analyzed
mechanical anchoring effect of the joints was enhanced by for reasoning the related mechanisms.
increasing the roughness of the aluminum surface [15]. J.P.B.
van Dam et al. investigated the influence of surface roughness
on the interfacial adhesion of adhesively bonded steel joints 2 Materials and methods
with epoxy through different surface treatments. They revealed
that the improved shear strength was mainly resulted from the 2.1 Raw materials
increased interfacial bond area [16]. Even though, regarding
the mechanisms, the consensus has not been reached. The rea- A commercial 6063 aluminum alloy in the state of the
son is that the adhesive layer itself and the bonding surface are extruded sheet was used as the raw material, which has
always the weakest part. The above studies showed results of excellent mechanical performance and is widely used in the
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field of automobile manufacturing. Specimens with sizes of 2 μm and a measuring force is 0.75 mN. Before the test,
of 100 mm in length, 3.8 mm in thickness, and 25 mm in the samples were placed on the testing platform and fixed
width were used for adhesive bonding. A structural adhesive with a clamping device. For each sample, five points, as
for the automobile industry, Dow BETAMATE 1840C, a shown in Fig. 1, were selected for testing, and each point was
single component, heat-cured epoxy, was employed for the tested for three times. Three specimens of each parameter
adhesion. Its density is 1.24 g/ml at 23 ℃, and its viscosity group, as shown in Table 1, were measured, and the aver-
is 46 Pa.S at 45 ℃. Its tensile strength is 37.1 MPa. age value was regarded as the ultimate result. The surface
morphology characteristics and micro-surface area of sam-
2.2 Surface treatment of the aluminum substrates ples were obtained using a VHX-2000C testing machine and
scanning electron microscope (SEM) device.
Sandpaper grinding was adopted as the surface treatment of To accurately obtain the failure pattern and the interface
the aluminum sheets, which were subdivided into six groups failure area, the failure surface of the adhesively bonded
to investigate the mechanical behaviors of the adhesively joints was recorded and the failure area was measured using
bonded joints for tensile testing, as shown in Table 1. Sand- a DXT-45 single-cylinder stereomicroscope. The percentage
paper mesh numbers of P80, P180, P320, P600, and P800 of interfacial failure is equal to the proportion of interfa-
were used. The sheets were grinded in a single direction that cial failure area to the whole overlap area in the adhesively
vertical to the tensile load direction of the adhesive joints bonded joints.
for tensile testing, as shown in Fig. 1. The grinding time
for each sheet was 10 min. In Table 1, sixteen sheets were 2.4 Contact angle testing and surface free energy
prepared for each group, and six sheets were used for the test calculating
microcosmic surface area, surface free energy, and surface
roughness, respectively, and the remaining ten sheets were Ordinarily, the considerable level of wettability of the alu-
bonded into five single lap joints. The surface characteristics minum substrate surface is a precondition for good adhe-
were measured at ambient humidity of 42 ± 3% and room sion. It is generally determined by the surface free energy
temperature of 25 ± 1 ℃. of the substrates to be bonded. The contact angle meas-
urement methods were adopted to compare the change of
2.3 Surface characterization surface free energy of the aluminum sheets after grinding.
The contact angles of testing liquids were performed on a
Two roughness parameters for the substrate are Ra and Rz. JC-2000D4F analyzer. The measured values were employed
Ra represents the arithmetic mean of the absolute values of to estimate the surface free energy which was very strongly
the longitudinal coordinates of the roughness profiles, and associated with wettability. The picture of the droplet was
Rz represents the arithmetic mean value of the individual captured by a digital camera located in a contact angle meas-
roughness depth of successive sampling lengths [24]. Rz urement instrument, and the images were analyzed using the
was applied to assess the surface roughness of the samples JC2000DB software. The surface free energies were counted
throughout this study. Surface roughness values, Ra and Rz, by the Owens–Wendt equation, as shown by Eq. (1). Dis-
were measured parallel to the load direction using a pro- tilled water and diiodomethane, typical polar and liquid, and
filometer (MarSurf PS 10, Germany), and the test device nonpolar liquid were used, which were selected for contact
accuracy is 0.001. The measuring principle is based on prob- angles measurement. In the test process, three points were
ing the surface with an inductive stylus with a tip of a radius tested on each specimen. The test liquid drop volume was
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3.36 μl, and each drop was measured three times by the samples, respectively; γd and γw represent the surface free
JC2000DB software. Furthermore, their average values were energy of the diiodomethane and water, respectively; γd w
used as the ultimate results. Surface tension measurement of and γp w represent the dispersive component and polar com-
liquid at room temperature and its component are shown in ponent of the surface free energy of water, respectively; γp
Table 2. Taking the surface tension of the liquid–solid-gas d and γd d represent the polar component and dispersive
triangular points into account in the equilibrium equation component of the surface free energy of diiodomethane,
Eq. (2), the surface free energy γs with its dispersive com- respectively; θw and θd represent the contact angle of water
ponent γd s and polar component γp s of the substrates were and diiodomethane, respectively. According to Eq. (2), the
counted [25] as below: surface free energy of joints with different surface treatments
√ √ can be calculated.
Wa =𝛾L (1 + cos 𝜃) = 2 𝛾Sd 𝛾Ld + 2 𝛾S 𝛾L
p p
(1) In order to completely comprehend the wetting status of
the adhesive on the aluminum surface and to validate the test
results for the test liquids, the contact angles of the 1840C
𝛾s =𝛾sp + 𝛾sd (2) structural adhesive on the aluminum substrate surface at 180
℃, which was beyond its melting point, were also tested for
where θ represents the contact angle, and Wa represents the
comparison. The same testing and calculating methods as
work of adhesion, the total surface energy, and γs represents
described above were adopted. The only difference was that
the sum of the polar component γp s and dispersive com-
the testing platform was constantly heated and kept at the
ponent γd s.
testing temperature.
For the liquid–solid interaction system through dispersion
forces, Eq. (2) can be derived by considering the geometrical
average of two liquid dispersion components, and Eq. (3)
2.5 Joint preparation and lap shearing strength
can be introduced:
testing
𝛾sl = 𝛾s + 𝛾L − 2(𝛾sd 𝛾Ls )1∕2 (3)
After surface treating with different sandpapers, the alu-
or Eq. (4) minum sheets were cleaned with acetone with an ultrasonic
cleaner for 20 min. Then the sheets were dried in the air
𝛾L (1 + cos 𝜃) = 2(𝛾sd 𝛾Ls )1∕2 (4) at room temperature for 4 h. The adhesive was uniformly
daubed on the aluminum surface. In order to control the
While the diiodomethane and the water contact angles
adhesive thickness, two copper wires with Φ 0.3 mm are
on the samples were tested at the room temperature, the
inserted into the adhesive layer. The adhesive area was
components γp s and γd s of the aluminum substrates can
25 mm in width and 12.5 mm in length. A C-type flat-mouth
be counted according to the Owens–Wendt equations Eqs.
fixture was used to clamp the aluminum substrates and adhe-
(5) and (6):
sive together at a pressure of 0.2 MPa [26]. After assem-
bly, the redundant adhesive beyond the bonding area was
√ √
p p
𝛾w 𝛾d (1 + cos 𝜃w ) − 𝛾d 𝛾d (1 + cos 𝜃d )
d 0.5 removed. Finally, the adhesively bonded joints were cured
(𝛾S ) = (5)
for half a minute in a drying oven at 180 ± 0.2 ℃.
√ √
p p
2( 𝛾wd 𝛾d − 𝛾dd 𝛾w )
The lap shearing test, which is a widely used joint test
for automobile parts [27], was conducted to investigate the
effect of the different surface roughness of the aluminum
�
𝛾w (1 + cos 𝜃w ) − 2 𝛾sd 𝛾wd
p
(𝛾S )0.5 = (6) substrates on the shear strength of the adhesively bonded
joints. The parameters setting referred to the standard ASTM
√ p
2 𝛾w
D1002-2001. Detailed parameters of the adhesively bonded
where γd s and γp s represent the dispersive component and joints for lap shearing strength testing are shown in Fig. 2.
polar component of the surface free energy of the tested The testing was carried out using an Instron 3369 tensile
testing equipment, and the load–displacement curves were
acquired, and the loading speed is 5 mm·min−1. The maxi-
Table 2 The components and its surface free energy of the measured mum load in the load–displacement curve was applied to
liquids at room temperature, in mJ·m−2 estimate the lap shearing strength. Tensile tests were per-
Testing liquids γL γp L γd L formed on three joints for each parameter in Table 1, and
the average strength was considered as the ultimate result.
Diiodomethane 50.8 0 50.8
Lap shearing strength of the joints was calculated on the
Distilled water 72.8 51.0 21.8
basis of Eq. (7):
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16
(a) 2.06 Sandpaper grinding (b) 13.74
2.0 Sandpaper grinding
Non-grinded 14
Non-grinded
Surface roughness Rz (m)
Surface roughness Ra (m)
12
1.5
10
1.19 7.84
8
1.0 0.85 6.08
0.68 6 4.69
0.52 3.93
0.5 4 2.88
0.29
2
0.0 0
P80 P180 P320 P600 P800 Non-grinded P80 P180 P320 P600 P800 Non-grinded
Mesh number of sandpaper Mesh number of sandpaper
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33
30.4 thus, the surface has minimal surface roughness. The
sandpaper-treated surface is covered with parallel ridges
30 28.7
27.7 27.5 and grooves. The coarser the particles of the sandpaper, the
26.7 rougher the surface is. During the sandpaper grinding pro-
27 cess, when the particles grinded of the sheet surface, the
metal was pushed and folded to form multiple cavities with
24 different sizes. This morphology increases the actual contact
area between and the liquid and the surface, thus increasing
21 the lap shearing strength.
19.3
As shown in Fig. 4, the picture shows that surface rough-
ness significantly affects the lap shearing strength of the
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2.88 3.93 4.69 6.08 7.84 13.74 adhesive bonded joints. When the surface roughness of
Surface roughness Rz (m) the grinded aluminum substrates is 6.08 μm, the lap shear-
ing strength is 57.5% higher than that of the joint made of
Fig. 4 Lap shearing strength changes with surface roughness the sheets, whose surface roughness is 2.88 μm. The rea-
son is that when the aluminum substrates were grinded by
sandpaper, grooves, ridges, and other uneven flats were
which is about 37.1 MPa. Lap shearing strength decreases produced on the substrate surface, as shown in Figs. 5d or
when the joints of surface roughness exceed 6.08 μm. For 6d. It prevents the adhesive from detaching the aluminum
example, the lap shearing strength of the joints that were substrates. When the aluminum surface roughness increases
made of sheets with a surface roughness of 13.74 μm is 26.7 from 2.88 to 3.93 μm, the lap shear strength increased by
Mpa, which is 12.2% lower than that of the joints made of 8.4 MPa (from 19.3 to 27.7 MPa). When the aluminum sur-
the sheets whose surface roughness is 6.08 μm. face roughness increases from 2.88 to 6.08 μm, the lap shear
strength increased by 11.1 MPa (from 19.3 to 30.4 MPa). It
is related to the wettability of the aluminum surface before
3.3 The effect of surface roughening on the lap measurement. In this way, surface roughening improves
shearing strength of the joints the lap shearing strength of joints greatly. The roughening
grade also significantly affects the lap shearing strength of
3.3.1 Influence of grinding on the surface morphology the joints. When the aluminum substrate surface roughness
of the raw materials made of the sheet is 6.08 μm, the lap shearing strength is
30.4 MPa, which is 9.7% higher than that of the joints made
The surface roughness affects the lap shearing strength of of the sheet, whose surface roughness is 3.93 μm. The rea-
adhesively bonded aluminum joints through surface mor- son is that when the aluminum substrates were grinded by
phologies modification. To explore the inherent mecha- the coarse sandpaper so that several hollows were formed
nism, the surface morphology of the aluminum substrates on the aluminum substrates’ surface. The grooves become
treated with sandpapers of different mesh numbers was wider and deeper, and the ridges become wider and higher
observed and compared. The surface morphology images (illustrated in Fig. 5b, d). The greater the height difference
are presented in Fig. 5, and the SEM images of the surface between the grooves and the ridges is, the more difficult
morphology are shown in Fig. 6. Many parallel valleys are to separate the adhesive from the aluminum substrates will
recorded on the surface of the grinded aluminum substrates, be [23]. It was found that the grinded surface exhibit uni-
and width and depth of these valleys decrease with the form grooves and ridges surface pattern, as shown in Figs. 5
increase of the sandpaper number mesh. The surface mor- and 6. Grooves and ridges offer more micro-surface area for
phology of the un-grinded sheets is also shown in Fig. 5, in bonding and increase the opportunities for the adhesive to
which the color of surface images is lighter compared to the permeate into the grooves. However, it weakens the inter-
grinded sheets. It means that the un-grinded specimen has a locking effect of the surface features when the raw sheets
flat surface and exhibits a small surface roughness value. For were grinded by P800 and un-grinded samples. As shown
the surface characteristics of the grinded sample, as shown above by the experimental results, it can be seen that when
in Fig. 5, the morphology color brightens dramatically and the surface of the substrate was over-roughened, ridges will
the scratches depth increases with the surface roughness of form. It will weaken the interlocking effect of the surface
sheets increases. features. This is due to that the over-roughened surface and
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Fig. 5 Surface morphology images of aluminum sheets before and after grinding with different mesh numbers of sandpaper: a un-grinded, b
P800, c P600, d P320, e P180, and f P80
ridge will store more gas. When the adhesive gradually infil- increases the interfacial area ratio. As a result, the number
trates the metal surface, it is not easy for the gas to escape of bonding points at the contact area between the adhesive
from the interface because of the high viscosity of the adhe- and aluminum substrates increases remarkably. In addition,
sive. As a result, air bubbles were formed at the interface a large number of anchors allow the adhesive to permeate
between the adhesive and the metal surface, which prevented the surface of the aluminum substrate, and then the adhe-
the adhesive integrating the metal surface further and caused sive is interlocked with the substrate in the groove during
the wettability decreased. In this way, the interlocking effect curing. Because the grinding process modifies the amount
is also weakened [28, 29]. Therefore, to a certain extent, of interaction between the substrates and adhesive, surface
roughening the aluminum substrate surface enhances the lap roughening increases the mechanical interlocking effect.
shearing strength of the joints. In Fig. 7, the fluctuation of the un-grinded samples’ pro-
The anchor behavior mechanisms between the substrates file curve is lower than that of the grinded samples. In the
and the adhesive indicate that the grinding surface morphol- cases when the surface roughness values are 2.88 μm and
ogies have a significant effect on the shearing strength. As 6.08 μm, the mean depth of the grooves of aluminum sub-
demonstrated in Figs. 7 and 8, surface roughening obviously strates are approximately 0.02 μm and 4 μm, respectively.
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Moreover, the rougher the aluminum substrate is, the of the bonded samples was examined. Figure 8 lists the
stronger the fluctuation of the surface profile becomes. When cross-section morphology of the adhesively bonded joints
the surface was not grinded, the surface profile is nearly a made of the sheet without grinding (a), smaller roughness
straight line. However, as seen from Fig. 7b-f, the surface (b), moderate roughness (c), and larger roughness (d), which
profiles are dramatically fluctuant curves when the samples has a higher magnification compared to the surface profiles
were grinded by sandpapers. To better clarify the influence in Fig. 7. It is obvious to see that the cross-section of Fig. 8a
of anchoring of adhesively bonded joints, the cross-section shows a nearly straight line, and the cross-section of Fig. 8d
Fig. 7 The surface roughness profile of aluminum substrates with various surface treatment: a un-grinded, b P800, c P600, d P320, e P180, and
f P80
13
15
10
8
5
5 4
3
0
0
2.88 3.93 4.69 6.08 7.84 13.74
Surface roughness Rz (m)
Fig. 8 Optics microscope (OM) images of the adhesively bonded
joints cross-section with various surface treatments: a un-grinded, b
P800, c P600, and d P320 Fig. 9 The increment of microcosmic surface area for grinded sheets
compared to un-grinded sheets
shows a sawtooth shape. The difference of the two types of there is more micro-surface area for bonding. Therefore, the
cross-sections leads to different surface roughness. Com- larger the effective contact area is, the weaker the stress con-
bined with Fig. 4, the lap shearing strength of the bonded centration will form, and the adhesively bonded joints are
joints made of grinded sheets is higher than that of joints difficult to be damaged [14]. Similar trends were observed in
made of un-grinded sheets. This is related to the stronger average roughness and microcosmic surface area when the
anchor effect of the surface morphologies originated from Rz is between 2.88 and 13.74 μm, which proves the enhanced
larger contact areas [14]. With larger anchor sizes, it is adhesion caused by mechanical grinding resulting from the
much more difficult for the adhesive to separate from the increasement of surface area. However, the lap shearing
aluminum substrates. Analyzing the other samples that were strength of the joint is not in a linear relationship with the
grinded with sandpaper, the same effect can be summarized microcosmic surface area.
when the surface roughness values are below 6.08 μm.
3.3.3 Influence of grinding on the surface free energy
3.3.2 Influence of grinding on the surface area of the raw of the raw materials
materials
In order to find out the reasons why the lap shearing strength
Figure 9 shows the change of microcosmic surface area for of the joint does not increase monotonically with the surface
grinded sheets compared to un-grinded sheets. It is obvi- roughness increasing, the interfacial adhesion situations of
ously examined that the microcosmic surface area value the joints with grinded aluminum substrates surface were
of samples grinded by sandpaper is apparently higher than investigated. Wettability is an important indicator to evaluate
that of un-grinded samples. The microcosmic surface area interfacial adhesion situations, which can help engineers to
of un-grinded sheets is 3.2 × 105 μm2. The higher the sur- comprehend the interaction mechanism between the adhe-
face roughness of aluminum substrates is, the larger the sive and substrate. The wetting behavior of the adhesive on
microcosmic surface area will be. Besides, when the surface the aluminum sheets with different surface morphology and
roughness is 3.93 μm and 13.74 μm, its microcosmic surface roughness was analyzed based on the method reported in the
area increment is 3 × 105 μm2 and 19 × 105 μm2, respectively. literature [30]. Figure 10 shows the average water and diio-
These results indicate that surface roughening can increase domethane contact angles on the aluminum substrate surface
the microcosmic area of the aluminum substrate. Further- after grinding with the different number of mesh sandpapers,
more, combined with Fig. 4, it is clear that the lap shearing respectively. As the surface roughness of the aluminum sub-
strength of grinded samples with a rougher surface is greater strate increases, the surface contact angle decreases firstly
than that of un-grinded samples when the Rz is between and then increases gradually in the test liquid. Furthermore,
2.88 and 6.08 μm. This is related to that surface roughening when the surface roughness of the aluminum substrate
improves effective contact areas in grinded samples. Due to is 2.88 μm, the water contact angle is 67.21°, and then it
the existence of grooves and ridges on the substrate surface, decreases dramatically when the surface roughness turns
13
70 50
(a) 67.12 Non-grinded (b) 47.18 Non-grinded
Diiodomethane contact angles (Deg)
45
59.23
60
40
53.94
55 52.32 35.61 35.78
35 33.52
50 47.17 30.64
45 30 27.97
42.25
40 25
2.88 3.93 4.69 6.08 7.84 13.74 2.88 3.93 4.69 6.08 7.84 13.74
Surface roughness Rz (m) Surface roughness Rz (m)
Fig. 10 The contact angle of testing liquid with different surface roughness: a water and b diiodomethane
13
energy of the aluminum substrate has the opposite change increases from 2.88 to 6.08 μm. In all cases, the aluminum
trend compared to the contact angle with the increase of substrate surface was grinded by a different number of mesh
surface roughness. However, the surface free energy of alu- of sandpaper, and the percentage of the polar component of
minum substrates and the lap shearing strength of the adhe- surface free energy is greater than that of the dispersive com-
sively bonded joints have the same change trend with the ponent. These results are consistent with the previous studies
surface roughness increase. The dispersion component (dii- [24, 33]. The surface free energy values of the sample with
odomethane) and polar component (water) of surface free a surface roughness of 2.88 μm are 45.89 mJ·m−2 which are
energy of various samples are apparently different from each 14.8% and 29.5% lower than those when the surface rough-
other. The polar components (water) surface free energy is ness is 3.93 μm and 6.08 μm, respectively. Meanwhile, the
generally lower than that of the dispersion components (dii- surface free energy of the sample with a surface roughness
odomethane). Although there is no obvious relationship of 13.74 μm is 56.69 mJ·m−2, which is 12.9% lower than that
between the surface free energy and surface roughness, the of the sample when the surface roughness is 6.08 μm. Thus,
surface free energy of the dispersion component (water) is when the surface roughness of aluminum sheets is 6.08 μm,
much closer to the total surface free energy. One reason is it has the highest surface free energy. As pointed out by
that polar elector-donor interactions decrease with the sur- Harris and Beevers [34], smoother sandblasting surfaces
face roughness and the nonpolar dispersion interactions do have higher surface-free energy. Furthermore, Hitchcock
not rely on the surface morphology. The adhesive adsorption et al. [35] examined that the surface roughness of the sub-
theory holds the opinion that bonding is the use of mechan- strate usually leads to the decrease of wettability in a certain
ical bonding force, chemical bonding force, and physical range, too. Some researchers found out that the asperities,
adsorption force between the interfacial connecting mate- ridges, and peaks on the surface of the substrates produce
rials. Because the electronic polarity of the adhesive and obstacles to prevent droplet diffusion [36, 37]. Thus, an over-
aluminum substrate attracts each other to produce a bonding roughening surface greatly decreases the surface free energy
force, the adhesively bonded joints become stronger, which of the aluminum substrates and reduces the lap shearing
leads to less interfacial failure area. As a result, the failure strength of adhesively bonded joints.
percentage of the interfacial contact area initially decreases According to Eqs. (3) and (4), the adhesion energy of
and then increases with the surface roughness, as shown in adhesive/aluminum substrate is calculated by combining
Fig. 14. Similarly, the lap shearing strength of the adhesively the surface free energy of the adhesive and the test contact
bonded joints firstly increases and then gradually decreases angle. The results are shown in Table 3 and Fig. 12. The sim-
as the surface roughness increases, according to the theory. plified zero diffusion pressure is the premise for calculating
Generally, with the increase of surface roughness of the the adhesion work in ambient air using Eq. (3). Because the
sheets, the surface free energy calculated by the water con- work of adhesion, Wa, determines the status of that adhesive
tact angle decreases. Moreover, the polar component of the penetrating into the substrate, the bonding work has a sig-
surface free energy increases from 35.83 to 45.03 mJ·m−2 nificant impact on the diffusion of the adhesive. The bonding
when the surface roughness of the aluminum substrate joints are heated to 180 ℃, which is the curing temperature
of the adhesive. The adhesive will form a specific contact
angle on the surface of the aluminum plate to wet the alu-
minum substrate. The contact angle of the adhesive on the
SFE = ps + ds
60 ps aluminum substrate is 55.4° ± 0.8°. According to the refer-
SFE and its components (mJ·m-2)
13
Table 3 Surface free energy and Rz (μm) 2.88 3.93 4.69 6.08 7.84 13.74
its components for substrates
with different surface roughness −2
γp s (mJ·m ) 35.83 41.74 43.95 45.03 42.71 41.66
γd s (mJ·m−2) 10.06 12.14 17.86 20.03 15.53 15.03
SFE (mJ·m−2) 45.89 53.88 61.81 65.06 58.24 56.69
adhesive interfacial adsorption that can improve the mechan- joint made of un-grinded sheets has the biggest interfa-
ical interlock effect. Another significant factor is satisfied cial failure area among all the different treatment param-
adhesion work, which promotes the bonding strength, eters joints. Moreover, the interface failure area initially
although the value is much lower than that of the actual decreases and then increases with the surface roughness
separation work. Because of the tested value of the adhesion increases. When the surface roughness of the aluminum
work Wa = 102.14 mJ·m−2 in the adhesive/aluminum bond- sheet is 6.08 μm, the interface failure area rarely exists in
ing system is higher than 65.06 mJ·m−2, it is sufficient to the failure pattern. Compared to the failure pattern of other
produce a mechanical interlocking. Under this condition, the treatment parameters joints, the number of bare regions in
adhesive can completely flow into all corners of the micro the fractured surface is the least.
roughened aluminum substrate. The interface failure area percentages of the adhesively
bonded joints are demonstrated in Fig. 14. With the surface
3.4 Failure behavior of the adhesively bonded roughness of the aluminum substrates increases, the per-
joints centage of interface failure area of adhesively bonded joints
initially decreases drastically and then increases slightly.
The failure mode of adhesively bonded joints after the The percentage of interface failure area of the joint made by
tensile test usually includes three types, namely the cohe- the substrates with a surface roughness of 9.8 μm drops by
sive failure, interfacial failure, and mixed failure modes 76.4% approximately, compared to the adhesively bonded
[39]. Cohesion failure is a fracture of the adhesive itself. joints made of un-grinded substrates. It indicates that the
The interfacial failure mode is defined as the adhesive is surface roughening reduces the percentage of interface fail-
completely separated from the substrate surface. However, ure significantly and enhances the lap shearing strength.
the mixed failure mode refers to some cohesive failure and In addition, the smaller the interface failure percentage is,
some interface failure. In practical application, most of the stronger the adhesively bonded joint strength will be.
them are mixed failure modes. In this way, the engineers When the surface roughness is 6.08 μm, the adhesively
try to make the most of the mechanical performance of bonded joints have the smallest interface failure area, which
the structural adhesive. The failure patterns of adhesively decreases by 92.5% and 68.3% for those bonded joints with
bonded joints after the test are shown in Fig. 13. The the surface roughness of 2.88 μm and 13.74 μm, respectively.
Fig. 13 The macro-morphology
of fractured surface with differ-
ent mesh number of sandpaper:
a un-grinded, b P800, c P600, d
P320, e P180, and f P80
13
The percentage of interface failure (%) 45 (roughened by P80 and P180), whose surface roughness is
41.6
Non-grinded greater than that of the other three treatment methods and
40
Sandpaper grinding un-grinded, but their mechanical interlocking effect is very
35 terrible. Some reasons are concluded as follows: (i) The
profiles were disorder and nonuniform on the micro-scale
30
aluminum substrate surface, as shown in Fig. 7. It will cause
25 the adhesive to be irregularly distributed on the aluminum
substrate surface. (ii) Air gas is trapped in the valleys; thus,
20
over-roughening substrate surface prevents the adhesive from
15 wetting the coarse surface of the aluminum substrate com-
8.5
9.8 pletely. (iii) Because of insufficient wettability and residual
10 7.7
6.1 air between the aluminum substrate and the adhesive, the cor-
5 3.1 ners and grooves on the substrate surface cannot be entirely
0
saturated with adhesive before solidification. Those factors
2.88 3.93 4.69 6.08 7.84 13.74 reduce the valid bond area and create stress concentration in
Surface roughness Rz (m) the interfacial region. As a result, when the aluminum sub-
strate surface is grinded by P80 or P180, the surface is coarse,
Fig. 14 The bare area on the fracture surface and a lot of underfill areas of the joints will be formed, and
an alternating solid–liquid and gas–liquid interface will also
gradually appear, as shown in Figs. 15 and 16a.
3.5 Influence of over‑roughening on the failure It can be seen from Fig. 16 that the penetration of the
behavior of the joints epoxy on the grinded aluminum surface has two different
modes. Figure 16a illustrates the distribution of the epoxy
As illustrated in Fig. 4, the lap shearing strength decreases on the coarse substrate with surface roughness, for exam-
apparently when the surface roughness turns from 6.08 to ple, the sheets grinded by P80 and P180, while Fig. 16b, c
13.74 μm. In another word, the over-roughening surface of depicts the distribution of epoxy on the sheet with moder-
raw materials is harmful to the interfacial adhesion state of ate and fine roughness, representing the cross-section of
the joint cross-section. Figure 15 depicts the OM images of adhesive joints made of sheets which were grinded by P320,
the adhesively bonded joints cross-section with coarse sur- P600, and P800 and un-grinded sheets surface, respec-
face treatments (grinded by P80 and P180). It can be seen tively. The capillary wettability mechanism of the grooves
that over-roughening produces micro-cracks in the interfacial is applied to explain the observed penetration process of
region, which is consistent with the previous studies [23, 40]. epoxy [37]. The adhesive flows into the grooves driven by
These defects will lower the effective contact area so that lap the capillary force. The capillary wettability of the uneven
shearing strength decreases. Moreover, the extremely uneven surface can be influenced by two key factors: the percentage
surface prohibits the adhesive in freely spreading on the sub- of the groove depth to groove diameter and the percent-
strate surface. Based on the information mentioned above, age of the groove diameter to the groove space. When the
taking adhesively bonded joints as examples, Fig. 16 depicts percentages are at appreciate values, the substrates have
a mechanism diagrammatic of the cross-section of the joints excellent wetting. Moreover, the epoxy wetting mechanism
with different surface roughness. Figure 16a shows the mech- changes with the different surface microstructures of alu-
anism diagram of the bonding status of the coarse interface minum substrates. To verify the hypothesis, it is obvious
13
Fig. 17 Failure pattern a
grinded by P180 and b grinded
by P80
to see that many voids in the failure pattern of adhesively related mechanisms were systematically investigated. The
bonded joints after the shearing test, as shown in Fig. 17. main conclusions can be drawn as follows.
It means that the adhesive is not entirely contacted with
the aluminum sheets. The lap shearing strength of adhesive 1. The lap shearing strength of the adhesively bonded
joints with over-roughening surfaces is very low because of joints was obviously influenced by the surface rough-
many internal voids and other defects in the joints. ness of the aluminum substrate. With the surface rough-
ness of the aluminum substrate increased, the lap shear-
ing strength of the joints initially increased and then
4 Conclusions decreased. When the surface roughness of the aluminum
substrate reached to 6.08 μm after roughening with sand-
In this research, the influence of surface roughness on the lap paper, a maximum lap shearing strength of 30.4 MPa
shearing strength and the failure behavior of the adhesively was obtained for the joint, improved by 57.5% compared
bonded aluminum joints were experimentally studied. The with that of the joint made by sheets with a surface
13
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