Journal of Materials Processing Tech.

259 (2018) 368–379

Contents lists available at ScienceDirect

Journal of Materials Processing Tech.

journal homepage: www.elsevier.com/locate/jmatprotec

Increasing strength and fracture toughness of AA7075-T6 adhesively- T

bonded joints with laser ablation
⁎
Sai Guoa,b, Blair E. Carlsonb, Louis G. Hector Jr.b, Yong Xiaa, , Qing Zhoua
a
State Key Laboratory of Automotive Safety and Energy, Department of Automotive Engineering, Tsinghua University, Beijing, 100084, PR China
b
General Motors Global Research & Development, 30470 Harley Earl Blvd., Warren, MI, 48092, USA

A R T I C LE I N FO A B S T R A C T

Keywords: The effects of surface topography modified by laser ablation on adhesively bonded joint strength and toughness
Laser ablation are quantified. Model joints consisting of AA7075-T6 substrates, a high strength aluminum alloy, and a com-
Surface topography mercial structural adhesive, were investigated with both tensile-shear and double cantilever beam (DCB) spe-
Joint strength cimens. Surface topography was manipulated through varying single crater morphology and crater-to-crater
Fracture toughness
spacing on the substrates with a pulsed Yb-fiber laser. Relationships between single crater morphology and
Adhesive bonding
energy related process parameters were qualitatively established. Three regimes of crater spacing, i.e. over-
AA7075-T6
lapping, tangential and separated, were identified and connected to key process parameters that control
roughness amplitude and spacing. For this purpose, a new energy parameter that links laser pulse energy to
resulting crater geometry and spacing was developed. It was found that both joint strength and toughness in-
crease with Sa , the 3D arithmetic mean roughness height deviation, at low and mild (< 0.31 mJ) laser pulse
energies, but decrease with higher energy input. The reasons for this behavior are considered in detail.
Improvements of 5.9% in tensile-shear strength and 13.5% in the toughness of DCB samples demonstrate that
adhesive joints with optimized topographies via laser ablation can be substantially stronger and tougher than
joints with as-received substrate surfaces.

1. Introduction (Digby and Packham, 1995). Surface contaminants, such as lubricants

Adhesive and cohesive fracture are the two main fracture modes in
adhesively bonded joints of similar or dissimilar materials. Usually
cohesive fracture occurs in well prepared joints while the locus of
fracture tends to the interfacial regions after environmental attack
(Kinloch, 1979). van der Sluis et al. (2014) investigated the competition
between adhesive fracture and cohesive fracture and changed the
fracture locus via surface treatment. Hirsch and Kästner (2017) studied
different effects of fracture modes on the overall interface character-
istics. Based on these findings, cohesive fracture is preferred since en-
ergy dissipation occurs primarily in the adhesive material thereby en-
hancing joint strength and toughness. Furthermore, methods for
increasing adhesively bonded joint strength and toughness involving
aluminum surface pretreatment have received substantial attention in
the literature, since aluminum is considered as a potential material for
lightweight vehicle designs (Hirsch, 2014). The various treatment
methods fall into one of two categories: substrate surface cleaning, in-
cluding changing the surface chemistry of the outer aluminum oxide
layer, or modifying surface topography of the substrate prior to bonding
on as-received aluminum substrates, tend to weaken the aluminum/
adhesive interface strength driving a greater propensity for adhesive
fracture and decreasing the initial bond strength of joints (Zheng et al.,
2015). However, in one example, Saleema et al. (2012) found that
treating AA6061 with sodium hydroxide (NaOH) to improve surface
cleanliness resulted in a 50% improvement of bond strength coupled
with complete cohesive fracture since polymer molecules within the bi-
component epoxy adhesive were strongly bonded with the cleaned
surface. Alternatively, techniques such as etching (Molitor et al., 2001),
anodization (Bjørgum et al., 2003), and plasma treatment (Saleema and
Gallant, 2013) can significantly improve wettability of the adhesive to
the cleaned metal surface since these further alter surface chemistry
leading in some cases to the formation of new oxide or other surface
layers, such as polar groups (Díaz-Benito and Velasco, 2013). Some of
these surface treatments enhance joint durability when exposed to wet
environments (Del Real et al., 2006). Improved adhesive wettability
translates to greater joint strength as demonstrated by Bhattacharya
et al. (2005). These techniques and others can also alter the metal
surface topography (or surface texture) at different length scales, which

⁎
Corresponding author.
E-mail address: xiayong@tsinghua.edu.cn (Y. Xia).

https://doi.org/10.1016/j.jmatprotec.2018.05.010
Received 13 December 2017; Received in revised form 28 March 2018; Accepted 5 May 2018
Available online 06 May 2018
0924-0136/ © 2018 Elsevier B.V. All rights reserved.
S. Guo et al. Journal of Materials Processing Tech. 259 (2018) 368–379

Table 1
Chemical composition AA7075-T6 (wt.%). (ASTM E1251).
Element Si Fe Cu Mn Mg Cr Zn Ti V Zr Other

AA7075-T6 0.08 0.17 1.5 0.03 2.4 0.19 5.8 0.04 0.01 0.02 0.06

Table 2 Table 4
Mechanical properties of the as-received AA7075-T6. (ASTM E8/B557). Intrinsic parameters of the TruMark Station 5020.
Properties Density Elastic Yield Tensile Elongation (%) Laser Pulse energy Wavelength Focal Focal spot
(g/cm3) modulus strength strength medium profile (nm) length diameter (μm)
(GPa) (MPa) (MPa) (mm)

AA7075-T6 2.78 70 521–530 588–594 10.8–11.5 Yb-fiber Nearly 1064 163 67

Gaussian

extends the surface area of contact, providing a greater number of in-

terlocking asperities, thereby leading to a higher probability of cohesive Table 5
versus adhesive fracture and correspondingly greater joint strength. Variable process parameters for laser ablation.
Cordisco et al. (2016) applied sinusoidal surface topographies to Pulse Percentage of Pulse Beam Hatching
AA7075-T6 double cantilever beams (DCB) using wire electrical dis- frequency maximum power duration scanning distance
charge machining. Joint strength and toughness under remote mode I (kHz) density (%) time (ns) speed (mm/s) (μm)
loading using Dow Betamate™ adhesive were directly correlated with η t v
f δh
increasing aspect ratio (i.e. amplitude to wavelength) relative to beams
with the as-rolled surface finish. Xu et al. (2015) rolled unidirectional
and bidirectional surface topography patterns onto AA5052-H32 sub-
strates. Tensile-shear tests of channel arrays and grid patterns showed
noticeable increases in adhesion strength relative to the as-received
condition. Grit-blasting (Harris and Beevers, 1999), sanding (Spaggiari
and Dragoni, 2013) and chemical etching (Liu et al., 2006) have also
been explored as means for manipulating surface topography at dif-
ferent length scales. A key learning from these studies is that even a
nanoscale increase of the mean surface roughness results in greater
bonding energy and hence higher joint strength and toughness as in-
vestigated in (Miki and Spearing, 2003). Surface topography can
change the local deformation and fracture mode in the adhesive,
especially in tests wherein a tensile load predominates, such as the DCB
test (Cordisco et al., 2016). The adhesive tends to deform in shear,
leading to higher energy absorption during joint fracture as discussed
by Maloney and Fleck (2018).
Laser ablation, in which a laser vaporizes/sublimates/or induces
phase change of the substrate surface material directly to a plasma, Fig. 1. W vs. f relationship for the TruMark Station 5020 measured at 16 data
points denoted by the solid black dots. The curve exhibits 2 stages delineated by
depending on the laser flux, can induce both chemical and surface to-
the maximum power density achieved at ∼25 kHz. Red rings around the solid
pography modifications on metal surfaces (Baburaj et al., 2007). The
black dots denote pulse frequencies selected to investigate the resulting surface
design opportunities afforded by adhesive bonding with laser ablation topographies (For interpretation of the references to colour in this figure le-
have received some attention in the literature. It has been demonstrated gend, the reader is referred to the web version of this article).
that laser ablation treatment is an effective way to clean surfaces and
improve adhesive wettability by modifying the oxide layer thus en-
accelerated aging. This further proves that surface topography is an
hancing the bond strength and aging resistance (Rechner et al., 2010).
important aspect in improving joint strength and toughness. The laser
Surface chemistry modification and formation of a new aluminum oxide
intensity is considered to be the main influence on the shape of each
layer were also found to contribute to the improved bond strength over
surface pattern (Wong et al., 1997). The threshold value of laser power
time of AA6022-T4 joints by Wu et al. (2016). X-ray diffraction analysis
after which surface patterning could be induced and surface roughness
was conducted by Rotella et al. (2015) to demonstrate the phase change
could be increased was studied by Alfano et al. (2014). Patterned in-
of surface materials of Ti6Al4V after laser irradiation. Moreover, SEM,
terfaces in copper/epoxy joints (Hernandez et al., 2017) enable an in-
AFM and EDS mapping were reported by Rotella et al. (2017), who
crease in bond toughness by triggering crack initiation, propagation
surveyed surface properties of Ti6Al4V. They found uniform, nanoscale
and arrest. Pan et al. (2017) compared the interlaminar strength of
periodic surface structures, which improve the joint toughness against
CFRP/Mg laminates after grit blasting, micro-arc oxidation and laser

Table 3
Material properties of Dow Betamate™ 1486 adhesive.
Properties Density Viscosity Tensile modulus Tensile strength Tensile Elongation Curing rate
(g/cm3)/(23 ℃) (Pa·s)/(45 ℃) (GPa) (MPa) (%)

Dow Betamate™ 1486 1.22a 40–70 1.9b 38.0b 7.3b 20 min @ 160 °C

a
Tested per ASTM D1875-03.
b
Tested per ASTM D638.

369
S. Guo et al. Journal of Materials Processing Tech. 259 (2018) 368–379

medium was used to generate microscopic crater topographies in which

adjacent crater placement on the AA7075-T6 surfaces was manipulated
with the laser scanning speed and hatching distance. The laser beam
spot is circular with a focal point beam size of 67 μm on the substrates.
The maximum pulse rate frequency is 1000 kHz and processing speed of
0–10,000 mm/s. Individual crater morphologies were controlled with
the laser power density. Relationships between the laser ablation pro-
cess parameters and mechanical performance of adhesive joints were
established via two steps. In the first step, quantitative linkages be-
tween laser ablation process parameters and corresponding substrate
surface topographies were established. In the second step, mechanical
performance of the joints with specific surface topographies was
quantified with tensile-shear and DCB tests. Specific mechanisms that
control joint strength were explained based upon results of steps one
and two. Additional comments regarding application of the laser ab-
lation process to adhesive joints with other materials or treatment
methods are provided.

2. Experimental work

2.1. Materials

As-received AA7075-T6 sheets, with nominal thicknesses of 2.0 mm

and 6.35 mm, were selected as substrates to enable two different me-
chanical tests of adhesively bonded joints. The 2.0 mm sheets were used
in tensile-shear tests, and the 6.35 mm sheets were used to join double
Fig. 2. Adhesively bonded AA70705-T6 joint configurations (all lengths in cantilever beams for DCB tests. The AA7075-T6 chemical composition
mm). (a) tensile-shear, in which a tensile load is applied parallel to the sheets and mechanical properties provided by the supplier are listed in Tables
(top is a side view, bottom is a top-down view); (b) DCB, in which a tensile load
1 and 2, respectively. Dow Betamate™ 1486, an epoxy based, single-
is applied perpendicular to the substrate coupons via hinges affixed to the
component structural adhesive was used in the joints. The properties
coupons. The adhesive is denoted by the gray rectangular regions indicated in
each figure. The blue arrows indicate the loading direction (For interpretation
and curing process parameters of the adhesive from the supplier are
of the references to colour in this figure legend, the reader is referred to the web listed in Table 3.
version of this article).
2.2. Pulsed Yb-fiber laser
ablation under mode I and mode II loading states and correlated the
A pulsed Yb-fiber (1064 nm wavelength) laser, integrated into a
joint strength to surface roughness characteristics. Frenzel et al. (2015)
50 W TruMark Station 5020 marking system produced the AA7075-T6
quantitatively investigated the laser-treated aluminum surface topo-
sheet topographies investigated in this study. The beam is translated
graphies in relation to the applied laser parameters. Similar work was
line-by-line over an AA7075-T6 surface placed within the marking
conducted by Alfano et al. (2012), but no significant surface pattern
system chamber. Properties of the marking system are listed in Table 4.
was provided that led to optimum joint strength and toughness. As
Five marking system process parameters that affect surface topography
revealed by Palmieri et al. (2016), laser pulse energy is critical to the
design are listed in Table 5. These can be classified into the following
formation of a highly uniform faying surface. As a result, there is still a
two categories: 1) those determining nominal total energy ET delivered
significant gap in information that establishes quantitative relationships
in each laser pulse, viz. pulse frequency f , percentage of maximum
between laser ablation process parameters, such as power density,
power density η , and pulse duration time t , 2) those controlling the
scanning speed, and hatching (pitch) distance, and the mechanical
spatial distribution of laser pulse attributes, viz. scanning speed v and
performance of adhesively bonded aluminum alloy sheets, high
hatching distance δh (distance between beam scanning lines). The pulse
strength alloys in particular, under different loading paths. This in-
energy distribution is nearly Gaussian (TEM00) (Steen and Mazumder,
formation can be used to guide development of joint designs that enable
2010). In-plane loading conditions of adhesively bonded joints in ap-
significant manufacturing benefits.
plication (vehicle structures, for example) are complex. To eliminate
The present study aims to address this gap for adhesively bonded
the differences in mechanical behavior of the two orthogonal directions
joints consisting of AA7075-T6 (the substrate material), a high strength
(laser scanning direction and hatching direction) in the plane of the
aluminum alloy. A pulsed, 1064 nm wavelength, 50 W, Yb-fiber laser
adhesive layer, also for the sake of simplicity, δh was set equal to the

Table 6
Surface amplitude parameters. Note that M and N are the number of data points sampled along two directions x and y in the surface plane, and η (x i , yi ) is the height
value at surface point x = x i and y = yi .
Amplitude parameter Description Definition

Sa Arithmetic mean deviation of the surface relative to the mean plane 1

∑
N M
∑ |η (xi , yi )|
MN j = 1 i = 1
Ssk Skewness, or third moment of the roughness height distribution, measures the asymmetry of surface deviations about the mean 1
∑
N M
∑ η3 (xi , yi )
plane, thus describing the shape of the surface height distribution MNSq3 j = 1 i = 1

Sku Kurtosis, or fourth moment of the roughness height distribution, measures peakedness or sharpness of the surface height 1 N M
∑ j = 1 ∑i = 1 η4 (xi , yi )
distribution and characterizes the spread of the height distribution MNSq4

Sq Root-mean-square deviation of the surface roughness heights relative to the mean plane, sensitive to extreme deviations in 1 N M
∑ ∑ η2 (xi , yi )
roughness MN j = 1 i = 1

370
S. Guo et al.
Fig. 3. A single crater morphology on a AA7075-T6 substrate highlighting the
rim and bowl as follows: (a) top-down image from the Keyence VK-9710 laser
microscope; (b) 3D geometry of the crater in (a) redrawn based on the data
from the microscope; (c) cross-sectional profile along the red arrow in (b),
where D, d and H represent nominal crater diameter, bowl depth and rim
height, respectively. See Section 3.1 for detailed definitions (For interpretation
of the references to colour in this figure legend, the reader is referred to the web
version of this article).
center-to-center crater spacing δd , denoted as δ ,
δh = δd = δ
Here, δd is determined by,
Journal of Materials Processing Tech. 259 (2018) 368–379
v
δd =
f (2)
where v is the scanning speed (mm/s) and f is the pulse frequency
(kHz).
The Yb-fiber laser power density W (f ) was measured with an Ophir
Vega laser energy meter and plotted versus f in Fig. 1. The nonlinear
W (f ) curve consists of two stages: the first stage shows the intrinsic
behavior of laser generators at low pulse frequencies (Chesler et al.,
1970). The decrease of power density with pulse frequency in the
second stage results from the limited maximum power that the system
can provide, which is an inverse relation between power density and
pulse frequency in the pulsed mode. The maximum power density is
achieved at ∼25 kHz. The total energy ET contained in each laser pulse
is thus,
ET = ηW (f ) St (3)
Here, S is the area of the beam spot on the substrate during laser ab-
lation.
2.3. Sample preparation and quasi-static tests
Tensile-shear (da Silva, 2012) and DCB tests (Cordisco et al., 2016)
were conducted under room temperature, quasi-static loading condi-
tions to quantify the effects of AA7075-T6 surface topography on ad-
hesive bonding strength, up to fracture, and toughness, i.e. fracture
energy release rate in stable mode I crack propagation.
Joint geometries are shown in Fig. 2. A sheet metal shear was used
to cut all substrate test coupons to size. The substrate surfaces were
cleaned with acetone to remove oil before dispensing the adhesive.
Glass beads, with 0.25 mm diameter, were mixed into the adhesive to
control the adhesive layer thickness upon application. Since the amount
of glass beads may influence joint performance, 5%wt of glass beads
were used in the tests conducted in this study. After making the joints,
any squeezed-out adhesive was removed before curing, and then after
curing, any remaining squeezed-out adhesive was removed by light
sanding to create a straight edge.
Tests were performed by loading each substrate until complete
fracture of the joint (i.e. separation of each joint configuration into two
pieces). Shims were attached to both ends of the substrates to reduce
bending effects during tensile-shear testing. Hinges were attached to
one end of both substrates by adhesive bonding to transfer load in the
DCB tests per Cordisco et al. (2016). The loading speed was set to 10
mm/min for tensile-shear testing per ASTM (2010) and 3 mm/min for
the DCB tests (ASTM, 2012). Load vs. displacement curves were ob-
tained from an Instron 5582 tensile load frame. Each test was replicated
five times.
2.4. Surface characterization
A colour 3D laser-scanning microscope (Keyence VK-9710 genera-
tion II) was applied to measure substrate surface topographies. Four-3D
surface topography amplitude parameters, as detailed by Stout et al.
(1993), were selected to explore potential quantitative relationships
with the spacing parameters in Section 3.2. Each parameter listed in
Table 6 was measured on AA7075-T6 substrate surfaces after laser
ablation with the analyzer module of the Keyence VK-9710 laser mi-
croscope. This was found to have suitable measurement precision.
3. Results and discussion
3.1. Effect of energy-related parameters on crater morphology
(1)
Each Yb-laser pulse produced a crater on an AA7075-T6 surface.
The crater morphology consists of a central “bowl” shape surrounded
by a raised annular “rim”. An example (=60 kHz) is shown in Fig. 3.
371
S. Guo et al.
Fig. 4. Crater morphology vs. ET (see Eq. (3)). (a) D increases with ET , (b) relation between H and ET , suggesting significant non-linearity, and the relation between
d and ET, suggesting that d generally increases with ET, (c) nonlinear relationship between A and ET, (d) aluminum oxide residue on a 6.35 mm thick AA7075-T6
substrate (sample width is 25.4 mm) when a high ET = 0.67 mJ is applied. Dashed lines in (a)–(c) are only for displaying the trends.
Fig. 3a shows a top-down image of a single crater on an AA7075-T6
substrate surface. Fig. 3b shows a 3D perspective of the same crater in
Fig. 3a. Each crater is formed via melting, thermocapillary convection,
and vaporization of surface material as demonstrated by Hector and
Sheu (1993) and Sheu et al. (1998). Surface topographies consist of
crater arrays with the craters positioned at a specific center-to-center
spacing, and hatching spacing relative to each crater. The three energy-
related parameters in Table 5 determine the ET delivered in each pulse
given by Eq. (3). To simplify the test matrix, the power percentage η
was set to 100% and the pulse duration time t was set to 200 ns during
laser ablation. Therefore, the only parameter manipulated to change ET
in each pulse was the pulse frequency. A series of different pulse fre-
quencies f in the 5 kHz to 100 kHz range were selected to manipulate
crater morphology; these are denoted by the red circles in Fig. 1.
Scanning speed and hatching distance were adjusted to initially prevent
crater overlap.
Measured geometric parameters by the laser microscope were:
nominal crater diameter, bowl depth d , and rim height H , as shown in
Fig. 3c, which is a cross-section through a single crater. Note that the
latter two parameters are relative to a substrate surface reference plane.
It can be seen from Fig. 3a and b that the Yb-fiber laser beam inter-
action with the substrate surfaces results in imperfect circular bowls
surrounded by a rim with non-uniform height because of subtleties in
the beam energy or differences in beam absorption of the AA7075-T6
surface in different regions. Thus, the actual diameter and rim height
are functions of the circumferential position around the crater bowl
morphology. Consequently, taking an average value of these quantities
is an effective way to describe crater morphology. Nominal diameter D
determines a circle that has the same area as the projected area of a
372
Journal of Materials Processing Tech. 259 (2018) 368–379
crater on the substrate reference plane, calculated by,
4Spr
D=
π (4)
where, Spr is the projected area of a crater on the substrate reference
plane, which can be obtained from the Keyence VK-9710 microscope.
The rim height H was the average height along the rim circumferen-
tially, given by,
1
H=
L
∮l h (l) dl
(5)
where, L is the circumferential length of the rim, and h (l) is the local
rim height (circumferentially). All three results were measured for five
randomly chosen craters. The amplitude A is defined by,
A=H+d (6)
as denoted in Fig. 3c, and it is the nominal height between the valley
representing the bowl and the peak of the rims.
Crater geometric parameters vs. ET from Eq. (3) are plotted in Fig. 4.
Fig. 4a and b show that D and d both increase as ET increases. A higher
pulse energy level creates a larger molten pool hence increasing D as
shown in Fig. 4a. Fig. 4b suggests that d increases with increasing ET
but appears to gradually approach an asymptotic value at larger ET
values in the range investigated. This is consistent with the results
measured by Vilhena et al. (2009) and predicted by Gilbert et al.
(2014). In Fig. 4b, the relationship between H and ET is nonlinear and
exhibits a maximum averaged crater rim height at ET = 0.36 mJ for f
∼60 kHz. Fig. 4c exhibits a similar nonlinear trend for A vs. ET . We
surmise that when ET < 0.36 mJ, less material is vaporized and ther-
mocapillary convection is the predominant mechanism behind crater
S. Guo et al.
Fig. 5. 3D plot of crater geometries redrawn based on the data from the
Keyence VK-9710 laser microscope, generated by different ET : (a) ET = 0.67 mJ
(f = 25 kHz); (b) ET = 0.36 mJ (f = 60 kHz); (c) ET = 0.18 mJ (f = 100 kHz).
(d) shows the corresponding cross-sectional profiles along the red solid lines in
(a), (b) and (c) (For interpretation of the references to colour in this figure
legend, the reader is referred to the web version of this article).
373
Journal of Materials Processing Tech. 259 (2018) 368–379
formation; hence, A increases with ET . However, when ET > 0.36 mJ,
the molten pool becomes unstable because of the high plasma pressure
resulting from material vaporization. This exerts a downward force
onto the molten pool forcing the molten pool outwards and naturally
splashing upwards; thus, part of the rim is washed away. Evidence of
this is the great amount of condensed aluminum powder remaining on
the surface after application of high power density laser treatment,
shown in Fig. 4d. Fig. 5a–c are scanned images of various crater
morphologies that resulted from different ET values. Fig. 5a is one such
image exhibiting a rough rim geometry resulting from the highest en-
ergy level, i.e. ET = 0.67 mJ ( f = 25 kHz). Some portions of the rim
were washed away leading to discontinuity of the rim. A small amount
of re-solidified surface material can be seen outside the rim. Fig. 5b is
an image representing the lower energy ET = 0.36 mJ ( f = 60 kHz)
and exhibits a relatively smooth and continuous rim. Melting and
thermocapillary convection control rim formation and material vapor-
ization has minimal influence on the rim morphology. Fig. 5c shows the
rim geometry resulting from melting and thermocapillary convection of
surface materials when ET = 0.18 mJ ( f = 100 kHz), which has a
smaller height compared with Fig. 5b (see Fig. 4b for qualitative re-
sults) and is discontinuous at some places.
Notice that crater morphology depends primarily on ET irrespective
of f. See, for example, the comparable results at f = 10 kHz and 30 kHz
in Fig. 4, where both frequencies generate ET ∼0.60 mJ. This further
demonstrates that ET largely determines crater morphology from the
Yb-fiber laser. As shown in Fig. 1, the first stage of the curve covers a
narrow range in terms of f , which leads to difficulty in selecting pulse
frequency with a corresponding ET . Hence, we avoided this narrow
range of f values in Fig. 1, and instead selected values from the second
stage as a means for establishing ET .
3.2. Effect of spacing parameters on surface topographies
Scanning speed, v , and hatching distance, δh , determine the density
of craters on the AA7075-T6 substrate surfaces which are used to form
the adhesive joints. Three different regimes are considered with respect
to the relative positioning of the craters produced by the laser beam
during ablation: overlapping, tangential, and separated. These regimes
correspond to different regimes in Fig. 6a which is a plot of f vs. δ . The
tangential regime, wherein the adjacent crater rims are in close proxi-
mity (see Fig. 6c) occurs for spacings that fall on the solid curve, which
is the relationship between D and f in Section 3.1. The overlapping
regime occurs for crater spacings below the solid curve (see Fig. 6d).
The separated regime occurs for spacings above the solid curve (see
Fig. 6b). For the tangential and separated cases, whole crater patterns
are observed. However, the surface becomes irregular and individual
craters are hard to discern with the advent of the overlapping regime.
To capture the effects of the most important parameters on surface
topographies consisting of crater arrays, we propose a new parameter,
ETU , which is the total energy applied per unit cell. The three unit cells,
which correspond to different values of crater center-to-center spacing,
δ , are defined by the blue dashed squares in the three regimes in Fig. 7.
Hence,
ET S
ETU =
δ2 (7)
since D depends on ET , which is determined by f . To find a general
expression that is independent of f , we introduce an additional spacing
parameter defined as the overlapping or separation coefficient, C . This
coefficient gives a relationship between δ and D ET . Here, D ET denotes
the nominal crater diameter when ET is applied. C is defined as follows,
δ ⎞
C (%) = ⎜⎛1− ⎟ × 100
⎝ D ET ⎠ (8)
The three crater topography regimes detailed in Fig. 6a correspond
S. Guo et al. Journal of Materials Processing Tech. 259 (2018) 368–379

Fig. 6. Three crater topography regimes based upon nominal crater diameter, δ. (a) The solid curve is the tangential regime dividing the overlapping regime (below)
and the separated regime (above), and comes from the relationship between D and f in Section 3.1, the cross marks denote measured data. Typical surface
topographies in the three regimes are displayed in (b), (c) and (d) when f = 60 kHz (ET = 0.36 mJ). The three solid red balls in (a) indicate the chosen crater
spacings: (b) δ = 100 μm (v = 6.0 mm/s) of the separated regime; (c) δ = 70 μm (v = 4.2 mm/s) of the tangential regime and (d) δ = 25 μm (v = 1.5 mm/s) of the
overlapping regime, see Eq. (3) and Table 5 for parameter definitions (For interpretation of the references to colour in this figure legend, the reader is referred to the
web version of this article).

to the following ranges: 0 < C < 100% (overlapping), C < 0% (se-

parated) and C = 0% (tangential). Therefore, substituting Eq. (8) into
Eq. (7) gives,
ET S
ETU = 2
( C
D ET 2 1− 100 ) (9)

The ETU vs. C relationship for three values of ET are plotted in

Fig. 7. Relationship between ET and C based upon Eq. (9), for ET values of
0.67 mJ, 0.36 mJ, and 0.18 mJ. The vertical solid line in the middle, i.e.
C = 0%, represents the tangential regime and divides the graph into the sepa-
rated regime for C < 0% and the overlapping regime for C > 0% as indicated
by the images of the grey filled circles or craters. Blue dashed squares in the
inserted images represent the unit cells defined in the three regimes (For in-
terpretation of the references to colour in this figure legend, the reader is re-
ferred to the web version of this article).
Fig. 7. Note that the area above the red solid line is meaningless in
practice, because the ET = 0.67 mJ of the red solid curve is the max-
imum value that the Yb-fiber laser can provide. The solid vertical line
with C = 0% represents the tangential regime; the maximum value of
ETU = 0.22 mJ is obtained when ET = 0.67 mJ. Thus, any case with ETU
greater than 0.22 mJ only occurs in the overlapping regime, i.e.
C > 0%. The new proposed parameter, ETU , may include other factors
affecting ET that have not been considered in this study. Thus, ETU will
be applied to correlate to surface topography parameters and joint
strength and toughness instead of ET or C.
3.3. Results of 3D surface height characterization
Fig. 8 shows the effects of ETU (see Eq. (9)), which represents the
effect of crater spacing, on the first three surface topography amplitude
parameters in Table 6. Fig. 8a considers Sa vs. ETU . Here, nonlinear
behavior is observed with a local extremum or peak (approximately
2.0 μm) at approximately 0.31 mJ, and a valley at approximately
0.82 mJ based upon polynomial curve fitting. Examination of Fig. 7
reveals that these values of ETU occur only in the overlapping regime.
Hence, to explain the behavior of Sa as a function of ETU , we divide the

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S. Guo et al. Journal of Materials Processing Tech. 259 (2018) 368–379

Fig. 8. Relationships between surface topography amplitude parameters (see Table 6) vs. ETU . (a) Sa vs ETU has three regions divided by two extrema denoted by the
red open triangle at ETU = 0.31 mJ and blue open square at ETU = 0.82 mJ. (b) Ssk vs ETU ; (c) Sku vs ETU . As Ssk and Sku approach 0.5 μm and 3.5 μm, respectively,
under high ETU , the surface height distribution is more Gaussian-like. The surface with the most height value outliers, i.e. asperity peaks, occurs when ETU ∼0.31 mJ.
(d) blue cross marks represent combinations of δ and f selected to generate the experimental data within the tangential, separated (above) and overlapping (below)
regimes (see Fig. 7) (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article).

data plotted in Fig. 8a into 3 regions with each region being delineated
by an extremum. Region I ranges from 0 to 0.31 mJ, where increasing
ETU results in more severe melting and thermocapillary convection
leading to deeper bowls and higher rims, thus increasing Sa . Beyond
0.31 mJ and into region II, an increase of ETU is attributed mainly to an
increase in the overlapping coefficient, C . Because of the overlapping of
individual craters, newly formed rims (or portions thereof) may form
where bowls had just recently formed. In addition, the higher energy
input may cause elevated temperatures thereby softening or even
melting the rims as discussed by Romoli et al. (2017), and consequently
diminishing Sa . For the third region, at values of ETU = 0.82 mJ or
greater, there is at least 50% crater overlapping based upon Fig. 7.
Thus, we surmise that extremely high ETU lead to larger molten pools
with more material melting, convection and even vaporization. More-
over, larger asperities, or asperities that exhibit extreme deviations
from the mean plane and that have a broader spatial footprint result, as
shown in Fig. 9, thereby increasing Sa . Note that the data for Sq vs. ETU
is not shown as the effects of ETU on Sq are nearly the same as Sa . The Sq
(see Table 6) is only used to define and calculate Ssk and Sku .
Fig. 8b and c show the measured relationships between Ssk and ETU
and Sku and ETU , respectively. The Ssk of a Gaussian height distribution
is 0 μm. For Ssk > 0 μm, the surface is flat with a large number of
peaks. For Ssk < 0 μm, the surface has a good bearing area as is the case
for a plateau honed surface with significant troughs (Stout et al., 1993).
In addition, Sku = 3 μm for a Gaussian distribution. For Sku > 3 μm, the
surface has more extreme asperity outliers than does the normal dis-
tribution. For Sku < 3 μm, there are fewer outliers than the normal
distribution. It can be seen in both Fig. 8b and c that maximum values
of Ssk and Sku were obtained when ETU ∼0.31 mJ, as called out by the
vertical, red dashed lines in those figures. This means that many ex-
treme asperity heights remained on the surface after laser ablation at
relatively mild energy inputs (e.g. relative to ETU = 0.82 mJ), which is
consistent with the relationship between H and ET (see Fig. 4b). For
values of ETU > > 0.31 mJ, Ssk and Sku approach 0.5 μm and 3.5 μm
respectively, which indicates that when high energy is applied, as in the
case for the overlapping regime, the crater morphology is largely wa-
shed out and the topography becomes less directionally dependent, i.e.
the height distribution is more Gaussian-like. A small number of outlier
asperity peaks result from the remaining rims on the substrate surface
after laser ablation at high ETU . Similar phenomena were also reported
by Moroni et al. (2018).
ETU values of 0.31 mJ and 0.82 mJ correspond to extrema at the
inflection points in Sa vs ETU , (see Fig. 8a). Fig. 10 shows δ vs. f at these
two points, with the solid line for the tangential the same as that in the
curve of Fig. 6a. The two solid curves with symbols divide δ vs. f ,
which we refer to as a process map since it relates the hatching distance
to laser process parameters via ETU , into the three regions shown in
Fig. 8a. For any value of f , as δ decreases from a large value, Sa will
increase firstly in region I, then decrease in region II, and increase again
in region III. The two solid lines with symbols denote transitions be-
tween regions. The separated and tangential regimes belong to region I
in terms of Sa denoted in Fig. 10. The overlapping regime is divided into
three regions by the two solid lines with symbols, which come from the
two extrema of Sa occur in the overlapping regime. Hence, we select Sa
as the one surface amplitude parameter that we believe is most useful
for quantitative characterization of AA7075-T6 substrate surface

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S. Guo et al.
Fig. 9. Overlapped carter surface topography on an AA7075-T6 substrate sur-
face from ETU = 3.47 mJ ( f = 10 kHz, δ = 25 μm, C = 70%). (a) A digital
image of a AA7075-T6 substrate surface topography taken with the Keyence
VK-9710 laser microscope showing rim and bowl remnants and an asperity
which has an extreme height deviation from the mean plane; (b) 3D topography
redrawn based on the height data within the red rectangular box of (a) (For
interpretation of the references to colour in this figure legend, the reader is
referred to the web version of this article).
topography resulting from laser ablation. Relationships between Sa and
strength and toughness of adhesively bonded joints are therefore con-
sidered in Section 4.
4. Effect of surface topography on adhesive bond strength and
toughness
The tensile-shear and DCB tests discussed in Section 2.3 were con-
ducted to validate the improvement of strength and toughness, re-
spectively, of the adhesively bonded AA7075-T6 joints, with crater-type
surface topographies from laser ablation.
The maximum joint strength, τM , calculated from the tensile-shear
tests is given by,
FM
τM =
Strue (10)
where, FM is the maximum load (N) before joint fracture, and Strue is the
actual cohesive area (mm2) between the two AA7075-T6 substrate
coupons. The latter quantity is determined by measuring the actual
length and width of the applied adhesive, which may be different from
the 12.7 × 25 mm2 area in Fig. 2a because of experimental error.
376
Journal of Materials Processing Tech. 259 (2018) 368–379
Fig. 10. δ vs. f curves (blue for ETU = 0.82 mJ and red for ETU = 0.31 mJ at
the two inflection points in Fig. 8a) that divide the process map into three
regions corresponding to the three regions in Fig. 8a. The solid curve without
symbols denotes the tangential regime, dividing the separated regime above
and overlapping regime below. The separated and tangential regimes belong to
region I, and the overlapping regime is divided into the three regions (For in-
terpretation of the references to colour in this figure legend, the reader is re-
ferred to the web version of this article).
Considering the brittle-like fracture behavior observed in the tensile-
shear tests, it is reasonable to use this averaged maximum strength as a
target to explore process parameters that can provide optimized joint
strength.
For the DCB test, the critical energy release rate of mode I fracture,
GI , is calculated based on the compliance calibration method proposed
by Moura et al. (2009),
P 2 dCp
GI =
2B da (11)
where, P represents the load (N), B is the joint width (mm), Cp is the
compliance (mm/N), a is the crack length (mm).
Given the three regions based on Sa obtained in Section 3.3 (see
Fig. 10), specific combinations of δ and f were selected to produce a
given surface topography followed by mechanical testing as denoted by
the filled symbols in Fig. 11a and b. Three values of f were chosen:
25 kHz with maximum ET inducing a large d but small H (i.e. medium
A ), 60 kHz with medium ET inducing a large d and the maximum H
(i.e. large A ), 100 kHz with small ET inducing a small d and small H
(i.e. small A ). Several different spacing values were chosen for each
frequency aiming to cover a wide range of ETU , i.e. Sa in the three to-
pography regimes (see Fig. 10). In addition, the DCB tests included only
substrate coupons processed at 25 kHz and 60 kHz to investigate the
effects of rim heights on fracture toughness.
Tensile-shear and DCB test results are plotted in Fig. 12a and c as τM
and GI vs. Sa , respectively. In both tests, τM , GI and Sa are positively
correlated when Sa ranges from 0 to ∼2.0 μm and τM and GI show 5.9%
and 13.5% improvements, respectively, compared to the as-received
condition of the AA7075-T6 substrate coupons. It is easy to understand
that joint strength and toughness increase as a function of Sa , because of
a larger contact area and more mechanical (i.e. asperity-asperity) in-
terlocks between the adhesive and substrate coupons. For Sa > 2.0 μm,
τM , GI and Sa are negatively correlated. We surmise that asperities with
extreme height deviations from the mean plane and correspondingly
broad spatial footprints parallel to the mean plane (Fig. 9b) provide
little improvement to both strength and toughness. The data plotted in
Fig. 8a indicates the most improved joint strength and toughness can be
obtained when ETU is ∼0.31 mJ. This is further demonstrated in
Fig. 12b and d, which display the relationships between τM , GI and ETU .
In these figures, the most improved strength and toughness are
S. Guo et al.
Fig. 11. AA7075-T6 substrate surface topographies including as-received sur-
faces were mechanically tested. (a) tensile-shear; (b) DCB. In both figures, the
dashed line represents the tangential regime, and the two solid lines correspond
to the two inflection points in terms of Sa in Fig. 10. The solid diamonds in (a)
and solid balls in (b) correspond to the cases selected from different regions to
conduct mechanical tests.
identified within the shaded areas, representing region II in Fig. 10, and
close to ETU ∼0.31 mJ. Considering experimental errors in collecting
the mechanical test data, measuring surface roughness and other as-
pects, we conclude that combinations of δ and f on or near the red solid
curve with open triangles in Fig. 10, i.e. for ETU = 0.31 mJ, result in the
most improved joint strength and toughness for the Dow Betamate™
1486 adhesive and AA7075-T6 substrate combination.
Joint strength and toughness under remote mode I loading were
found to be positively correlated with increasing aspect ratio (i.e. am-
plitude to wavelength) of the sinusoidal surface topographies by
Cordisco et al. (2016). This conclusion is consistent with results from
the DCB tests in this study. The aspect ratio of the AA7075-T6 laser
ablated substrate coupon surfaces is defined by A / D (amplitude to
nominal crater diameter). Fig. 12c and d show GI vs. Sa and E TU for two
values of f , namely 25 kHz and 60 kHz, with aspect ratios of 0.05 and
0.1 (calculated based on Fig. 4), respectively. The 60 kHz curve is above
that for the 25 kHz, which demonstrates that joint toughness is posi-
tively correlated with aspect ratio.
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Journal of Materials Processing Tech. 259 (2018) 368–379
5. Concluding remarks
The goal of this study was to establish quantitative relationships
between laser ablation parameters and resulting substrate surface to-
pographies that provide insights into enhancing adhesive joint strength
with substrates consisting of high strength aluminum alloys and com-
mercially available adhesives. For this purpose, the study specifically
focused on joints consisting of AA7075-T6 substrates and Dow
Betamate™ 1486, a commercial structural adhesive. A larger adhesion
area and more mechanical interlocks between the adhesive and sub-
strate surface asperities result in improvement of bonding strength and
toughness as denoted by the maximum joint strength in tensile-shear
tests and the critical energy release rate of mode I fracture in double
cantilever beam tests, respectively. Correlations between laser process
parameters and surface height parameters were established first, en-
abling the manipulation of surface topography by varying laser process
parameters. Effects of surface topography on joint strength and
toughness were revealed based upon the 3D arithmetic mean deviation
of the surface relative to the mean plane, Sa . The major conclusions
(relative to as-received substrates with no topography modification),
based upon three types of surface topographies consisting of separated
craters, tangential craters and overlapping craters produced with a
pulsed Yb-fiber laser on AA7075-T6 substrate coupon surfaces are as
follows:
(1) Joint strength can be increased 5.9% in quasi-static, room tem-
perature tensile-shear tests,
(2) Fracture toughness can be increased by 13.5% in quasi-static,
double cantilever beam tests.
(3) To obtain the improvements in [1] and [2], the following roughness
amplitude and spacing conditions are required:
(4) Sa ∼2.0 μm, where Sa is the 3D arithmetic mean deviation of the
surface relative to the mean plane
(5) ETU ∼0.31 mJ, where ETU links energy delivered per laser pulse to
adjacent crater spacing.
The parameters proposed and methods for extracting the most cri-
tical roughness amplitude and spacing information used in this in-
vestigation can be extended to other materials or treatment methods.
This is provided that critical parameters, such as ETU , are properly
calibrated. Chemical effects on adhesion joint strength and toughness
require further investigation since they were not explicitly considered
in this study. As shown in region III of Fig. 10, Sa increases with ETU ,
while mechanical strength and toughness decrease, which may also be a
result of varying ratios of aluminum oxide and hydroxide on the sub-
strate coupon surfaces. Furthermore, only one pulse per crater was
applied in this study. Multiple pulses can generate surfaces with deeper
craters (Kromer et al., 2016), leading to additional asperity interlocking
and contact area. However, entrapment of air bubbles in the craters
may reduce joint strength (Shan et al., 2008). To solve this problem,
viscosity of the adhesive is an important property to be considered as
investigated by Paz et al. (2016), which has an effect on wettability
between adhesive and substrate material. Moreover, time dependent
bonding performance is another aspect of interest in practical appli-
cations.
Declarations of interest
None.
Acknowledgements
The presented work is supported by the Ministry of Science and
Technology of China under Contract No. 2016YFB0101606. Sai Guo
wishes to thank the China Scholarship Council (CSC) for financial
support and General Motors R&D for support during a one-year study as
S. Guo et al. Journal of Materials Processing Tech. 259 (2018) 368–379

Fig. 12. Relationships between the maximum joint strength, τM , and the critical energy release rate of mode I fracture, GI , vs. Sa and ETU are shown. Specifically: (a)
and (b) τM from the lap-shear test; (c) and (d) GI from the DCB test. All dashed lines are suggestive of trends. Shaded areas in (b) and (d) represent region II in Fig. 10.

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