Optics and Laser Technology 102 (2018) 25–31

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Optics and Laser Technology

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

Full length article

Controllable superhydrophobic aluminum surfaces with tunable

adhesion fabricated by femtosecond laser
Yuxin Song, Cong Wang ⇑, Xinran Dong, Kai Yin, Fan Zhang, Zheng Xie, Dongkai Chu, Ji’an Duan
State Key Laboratory of High Performance and Complex Manufacturing, College of Mechanical and Electrical Engineering, Central South University, Changsha 410083, China

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

Article history: In this study, a facile and detailed strategy to fabricate superhydrophobic aluminum surfaces with con-
Received 22 June 2017 trollable adhesion by femtosecond laser ablation is presented. The influences of key femtosecond laser
Received in revised form 28 August 2017 processing parameters including the scanning speed, laser power and interval on the wetting properties
Accepted 13 December 2017
of the laser-ablated surfaces are investigated. It is demonstrated that the adhesion between water and
Available online 20 December 2017
superhydrophobic surface can be effectively tuned from extremely low adhesion to high adhesion by
adjusting laser processing parameters. At the same time, the mechanism is discussed for the changes
Keywords:
of the wetting behaviors of the laser-ablated surfaces. These superhydrophobic surfaces with tunable
Aluminum
Superhydrophobic surfaces
adhesion have many potential applications, such as self-cleaning surface, oil–water separation, anti-
Tunable adhesion icing surface and liquid transportation.
Femtosecond laser Ó 2017 Elsevier Ltd. All rights reserved.

1. Introduction was a little complicated and required a long processing time. In

2015, Yu et al. constructed the submillimeter-scale V-shaped
Superhydrophobic surfaces with an apparent water contact groove arrays on the 5083 Al alloy substrates by the high speed
angle (WCA) above 150° are fairly common in the nature. The electrical discharge machining technology [16]. After a solution
leaves of certain plants, such as lotus, exhibit extreme water- immersion, the structures presented good superhydrophobicity
repellent because the microscopic structures of their surfaces pro- and low adhesion, but the adhesive property could not be regu-
vide them with extremely low adhesion, known as ‘lotus effect’ [1]. lated on large scale. However, among these proposed methods, it
This kind of surface allows water easily roll off and take away dust is difficult to control the structures precisely and regulate the
particles on the surface. Comparatively, the petals of rose, with adhesion. Besides, some methods are sophisticated and hazardous
high adhesion to water, can tightly grasp water droplets even for the environments.
when the surface is put upside down, which is called ‘petal effect’ Femtosecond (fs) laser micromachining is an effective tech-
[2]. nique to create micro-structures on surfaces for industrial applica-
In the past few years, superhydrophobic surfaces have attracted tions [17–22]. And the structures can be easily regulated by
extensive interests due to their potential applications, such as self- adjusting the laser processing parameters, such as laser power,
cleaning surface, oil–water separation, anti-icing surface and liquid laser scanning speed and scanning overlap. Recently, the wettabil-
transportation [3–8]. To achieve these functions, it is critical to ity of some laser-patterned surfaces has been reported [23–29].
control the adhesion of the surface. Generally, different surface However, most of these works only focused on the superhydropho-
microstructures, which affect the wetting states of water droplets bicity of surfaces. Little is known about the effects of different fs
on the surfaces, play a significant role in regulating adhesions on laser parameters on the surface water adhesion. Only one paper
the superhydrophobic surfaces [2]. Nowadays, various methods just demonstrated how the scanning speed affected the adhesion
have been applied so far to fabricate a variety of hierarchical struc- [30].
tures, such as the colloidal template technique, immersion method Due to their superior mechanical properties, Al and its alloys are
and electrochemical machining [9–14]. Xu et al. fabricated multi- widely used in automotive, aerospace, aviation, shipbuilding and
functional Al surface which showed stable superamphiphobicity, construction industries. Superhydrophobic Al surfaces can be sim-
anti-corrosion, and self-cleaning properties [15]. But the process ply fabricated, but the methods for adjusting adhesion and super-
hydrophobicity on the Al surfaces are few. In this study, the effect
⇑ Corresponding author. of laser power, scanning speed and scanning interval on the fs laser
E-mail address: [email protected] (C. Wang). irradiated Al surface structures and surface wetting behaviors are

https://doi.org/10.1016/j.optlastec.2017.12.024
0030-3992/Ó 2017 Elsevier Ltd. All rights reserved.
26 Y. Song et al. / Optics and Laser Technology 102 (2018) 25–31

investigated. Also, the influence of different laser parameters on The as-prepared samples were irradiated with a linearly polar-
the surface water adhesions has been demonstrated. Different ized fs laser (Pharos from Light Conversion) with a wavelength of
hierarchical structures consisting of micro/nano-scale features 1030 nm, repetition rate of 75 kHz, and pulse width 1000 fs. The
are fabricated by simply adjusting the laser processing parameters, output laser power was adjusted from 1000 mW to 10,000 mW.
which lead to different surface wetting abilities. The present paper A two mirror galvanometric scanner (Scanlab, Germany) with an
is sub-divided into two parts. In the first part, fs laser is applied F-Theta objective lens (f = 100 mm) was used and scanned the
with a wide range of laser power, scanning speed and interval to laser beam in x-y direction. The focused diameter of the
investigate their effects on the generated structures on the Al sur- Gaussian-profile laser at 1/e2 of its maximum intensity was
face. In the second part, the influence of surface morphology on the approximately 30 lm. The laser scanning was performed line-by-
surface wettability and the high-adhesive and low-adhesive super- line in the horizontal direction (x direction) and then in the vertical
hydrophobic surfaces for on-demand droplet transportation are direction (y direction). The interval of adjacent laser scanning lines
studied. was changed from 10 lm to 200 lm, which mean there were two
conditions including overlap and no overlap. In the experiments,
2. Materials and methods we changed the scanning speed of the laser beam from 50 to
1000 mm/s.
The commercial flat Al (30 mm
2 mm
1 mm) was mechan- The residual debris on the laser-ablated samples were removed
ical polished and cleaned with deionized water, acetone and anhy- by being cleaned ultrasonically with ethanol and dried in air. Then
drous ethanol in an ultra-sonic bath before laser treatment. the samples were immersed into a 0.015 mol/L aqueous PFOA

Fig. 1. (a–h) SEM images of the Al surfaces’ structures by fs laser at different scanning speeds: (a, b) 50 mm/s, (c, d) 100 mm/s, (e, f) 200 mm/s and (g, h) 400 mm/s. The laser
power is 8 W and scanning interval 50 lm.

Fig. 2. (a–f) Scanning interval dependence of SEM images of the Al surfaces structures by fs laser: (a, b) 10 lm; (c, d) 50 lm; (e, f) 200 lm. The laser power is 8 W, and
scanning speeds 100 mm/s.
 Y. Song et al. / Optics and Laser Technology 102 (2018) 25–31 27

Fig. 3. (a–d) SEM images of the Al surfaces structures as a function of the laser
power with a scanning speed100 mm/sand scanning interval 50 lm: (a) 10 W; (b)
8 W; (c) 4 W; and (d) 1 W.

(Pentadecafluorooctanoic acid from Aladdin, China) solution for 3 h

to reduce the surface energy and dried in an oven at 150 °C for 1
hour. The various samples were analyzed by SEM before and after
immersion in aqueous PFOA solution. Due to the thin layer coated
by PFOA, the surface morphology did not change after the chemical
treatment.
The morphologies of the samples were analyzed using a MIRA3
LMU scanning electron microscope (SEM, TESCAN, Czech) and a
laser confocal microscopy (LCM, Zeiss, Germany) whose built-in
software can calculate the average roughness Ra from the mor-
phology image. The wettability of the samples was evaluated by
measuring the apparent WCA (water contact angle) and WSA
(water sliding angle). The WCA and WSA of 8 lL water droplets
were measured in air at room temperature by an optical contact
angle meter (HARKE, China), using a sessile method. The WSA
was measured when a water droplet is about to slide down the
sample surface which gradually tilts from horizontals.

3. Results and discussions

SEM images of fs laser irradiated Al samples show that the

changes in surface morphologies which strongly depend on the
laser parameters, including the scanning speed, laser power and
scanning interval. As shown in Fig. 1(a)–(h), the topography of
the ablated Al surfaces changes greatly with different scanning
speeds while the laser power and the interval is 8 W and 50 lm.
When the scanning speed is low, the elongated pillared pattern
emerges which is decorated by plenty of laser induced sophisti-
cated nanostructures covered by the microstructures, such as some
nano-folds and nanoscale extrusions, according to Fig. 1(a) and (b).
The coarse nanostructures and elongated micro-pillars construct
double roughness patterns. As exhibited in Fig. 1(c), (e) and (g),
with the increase of scanning speed, the micrometer scale struc-
tures become flat and shallow. When the speed is 100 mm/s, the
surfaces are mainly consisted of the micro-pillars and some
nanoparticles (Fig. 1(c) and (d)). As the speed is further raised,
the comparatively flat pillars are covered by nano-scaled ripples,
and the period of ripple is around 600–800 nm, as presented in Fig. 4. Surface morphology and surface roughness of laser treated surfaces at
different laser parameters. (a) 3D profile of a typical surface, fabricated with the
Fig. 1(f) and (h). Therefore, the morphology of the surface can be
laser power of 8 W, a scanning speed of 50 mm/s and scanning interval of 50 lm;
tuned by simply adjusting the scanning speed. surface roughness of textured surface with different laser parameters: (b) laser
By increasing or decreasing the scanning interval at a constant power 8 W, interval 50 lm and scanning speed from 50 to 1000 mm/s; (c) interval
scanning speed 100 mm/s and laser power 8 W, two additional dif- 50 lm, scanning speed 100 mm/s and laser power from 1 to 10 W; (d) scanning
ferent micro/nano-patterns are obtained. Fig. 2 shows SEM images speed 100 mm/s, laser power 8 W and interval from 10 to 200 lm.
28 Y. Song et al. / Optics and Laser Technology 102 (2018) 25–31

Fig. 5. Water contact angle of laser treated surface (laser power 8 W, interval 50
lm and scanning speed from 50 to 1000 mm/s) with different surface roughness.

of the ablated pillared-like structures manufactures with changing

scanning interval from 10 lm to 200 lm. When the interval is so
small that the adjacent scanning paths overlap each other, the
microgrooves disappear and the parabolic-pillared pattern turns
up. Fig. 2(b) is a magnification of the sample depicted in Fig. 2(a),
which reveals that the laser induced irregular surface parabolic-
pillared structures are consisted of coarse micro-asperities of irreg-
ular shape covered by small spheres with a diameter of 0.5–2 lm.
With the increase of the scanning interval, the microgrooves and
micro-pillars are gradually distinct firstly. The surface is just like
the structure with some micro-pillars and nanoparticles men-
tioned above. As the scanning interval is continually enlarged,
the surface is divided into several neat squares by microgrooves
along the scanning paths, as shown in Fig. 2(e). The groove walls
of the microgrooves are covered by colloidal-like structures and
the areas of the squares, which is near to the microgrooves, are
covered with nano-scaled ripples (Fig. 2(f)). The period of ripples
is also about 600–800 nm. Hence, the laser treated surfaces gradu-
ally vary from irregular to regular with the increase of the scanning
interval
Besides, the changes of laser power also affect the microstruc-
tures of the laser treated surfaces if the scanning speed and interval
are fixed, such as 100 mm/s and 50 lm respectively. When the
laser power is far beyond the material ablation threshold, the
micro-pillars are obvious and covered by plenty of nano-scale
structures, such as some nanoparticles and nano-folds (Fig. 3
(a) and (b)). By decreasing laser power, the microstructures on
Fig. 6. Contact angles and sliding angles of a water droplet on the laser treated
the ablated surface gradually become flat and shallow and are cov-
surfaces at different laser parameters: (a) laser power 8 W, interval 50 lm and
ered with some nano-scale ripples (Fig. 3(c)). Moreover, there are scanning speed from 50 to 1000 mm/s; (b) interval 50 lm, scanning speed 100 mm/
only a few shallow traces of ripples on the laser-treated surface s and laser power from 1 to 10 W; (c) scanning speed 100 mm/s, laser power 8 W
while the laser power is reduced to 1 W (Fig. 3(d)). Obviously, and interval from 10 to 200 lm.
the higher the laser power is, the more complicated the structures
on the surface are. Besides the results mentioned above, more dif- 300 mm/s. This roughness reduction coincides with the phe-
ferent laser-patterned structures can be obtained with different nomenon discussed above, that the surface morphologies become
laser parameters [31]. more plain and shallow with the increasing scanning speed. Fur-
In order to study the relationship between laser parameters and thermore, Fig. 4(c) and (d) also exhibit the dependence of surface
surface morphologies better, the samples have been characterized roughness on laser power and scanning interval. With the increase
with LCM to get the 3D profile images of surface structures. And of laser power, surface roughness value increases while enlarging
LCM includes a built-in data processing program which provides scanning interval reduce surface roughness instead. It is because
the arithmetic mean of surface roughness based on the 3D profile increased laser power and decreased scanning intervals could also
images. Fig. 4(a) shows the 3D profile of a typical surface, fabri- lead to more complicated and coarser structures. Therefore, surface
cated by the laser power of 8 W, a scanning speed of 50 mm/s roughness can be well-controlled by laser parameters.
and scanning interval of 50 lm. The structure has the roughness Fig. 5 shows the relationships between surface roughness and
value of 4.99 lm, which is higher than all other samples with dif- WCA. Obviously, WCA increases from 134.3° ± 0.2° to 163.6° ±
ferent scanning speeds. With the increase of scanning speed, the 1.3° with the surface roughness value growing from 1.34 lm to
roughness value is gradually reduced, as shown in Fig. 4(b), and 4.99 lm. These results cater to the equation established by Cassie
it remained stable at about 1.35 lm when the speed is beyond and Baxter as follow [29].
 Y. Song et al. / Optics and Laser Technology 102 (2018) 25–31 29

Fig. 7. Sequential snapshots of a water droplet of 2 lL suspended on a syringe contacting a laser-ablated surface with (a) low adhesion, (b) high adhesion and then moving
away from it. (c) A water droplet easily rolls off from the laser-ablated surface (with a scanning speed of 50 mm/s, laser power of 8 W and interval of 50 lm). (d) Shape of a
water droplet on the ablated surface (with a scanning speed of 200 mm/s, laser power of 8 W and interval of 50 lm).

cos hr ¼ f 1 cos h  f 2 ð1Þ at the laser power of 1 W. This is mainly because the laser cannot
fabricate enough coarse surfaces, which contributes to superhy-
Here hr and h are WCA on Al samples with rough and flat struc-
drophibicity, if the power is too low. This indicates that the laser
tures respectively; f1 and f2 are the fractional interface areas of Al
power has little influence on the surface wetting properties as long
surfaces and air in surface structures, respectively. And f1 + f2 = 1.
as the laser power does not exceed a certain threshold. At last, as
From this equation, it is easy to find that the increase of f2, for
illustrated in Fig. 6(c), the interval plays the same role as the scan-
example, the more air fractional interface areas, will result in the
ning speed in wetting properties of surfaces when the other
increase of hr. Thus, rougher surface owns higher WCA because
parameters are unchanged (100 mm/s and 8 W). When the interval
the higher roughness value means more air trapped in surface
is below 150 lm, fs laser ablated surfaces’ WCAs are beyond 150°
structures, which leads to more air–water interface areas.
and the WSAs are below 10° just when the width of two adjacent
To investigate the effect of the scanning speed on the wetting
scanning paths is lower than 50 lm. According to the expansion of
property, the other two parameters are fixed as 8 W and 50 lm
the interval, the WSA of the surface adds to 11.5° ± 2.7° while the
firstly, and the WCAs as well as WSAs of the laser ablated surfaces
interval is 100 lm and still rises until the WSA equal to 90°.There-
are illustrated in Fig. 6 (a). When the scanning speed is lower than
fore, there are three effective ways to adjust the surface wetting
300 mm/s, the WCAs of the laser-ablated surfaces are over 150°. As
properties including the regulation of scanning speed and interval.
the scanning speed is 50 mm/s, the WCA of the surface reach to the
In addition to measure the WCAs and WSAs of the laser ablated
maximum, which is 163.5° ± 1.5°. Besides, the WCAs of the sur-
surfaces, a water droplet bouncing experiment was also carried out
faces decrease from 152° to 125° if the scanning speed varies from
by making a water droplet free-falling from a certain height onto
300 mm/s to 1000 mm/s. As for the adhesion of the surfaces, when
the object surface in order to further characterize superhydropho-
the scanning speed is lower than 150 mm/s, the WSAs of the sur-
bic surfaces [33,34]. Snapshots in Fig. 8 show the rebound behavior
faces are below 10° and the minim is 5.1° ± 1.2° as the scanning
of 2 lL water droplets on the laser-ablated surface with scanning
speed is 50 mm/s, which means that they are superhydrophobic
speed of 50, 75, 100, 200 mm/s, respectively. It is shown that the
surfaces and show very low adhesion between water and the trea-
rebound behavior is significantly influenced by the scanning speed,
ted surfaces. As shown in Fig. 7(a) and (c), we put a water droplet
which directly affects the microstructures on the surface. When
by a syringe on the low-adhesive surfaces and found that the dro-
the speed is 50 mm/s, the water droplet can rebound from the sur-
plet was easily moved away without any loss. As displayed in Fig. 7
face twice due to the extremely low adhesion of the surface and
(b) and (d), the WSAs also gradually increase to 90°as the scanning
the times of rebound decreases to one as the speed rise to 75
speed rises. However, the WSAs remain unchanged when the scan-
mm/s. Then, the water droplet cannot leave the surface as the
ning speed is beyond 200 mm/s. Compared with low-adhesive sur-
scanning speed reaches to 100 mm/s or higher and it sticks to
face, the high-adhesive surface can easily catch water droplet, and
the surface. This indicates a high adhesion to water. These results
it sticks to the surface firmly even when the surface is put upside-
further demonstrate that, by adjusting the scanning speed, the
down. In terms of the wetting properties influenced by the laser
water adhesion of the surfaces can be apparently tuned.
power, the trend of WCAs changing is completely different, as
To further understand the wetting behaviors of the laser-
depicted in Fig. 6 (b). If the laser power is beyond 1 W when the
ablated surfaces, the wetting mechanism is analyzed. At first, when
scanning speed and interval is 100 mm/s and 50 lm, the WCAs
the energy is high or the scanning speed is quite low, the surfaces
of laser-ablated surfaces are all beyond 155°. And WSAs are grad-
exhibit superhydrophobic and low adhesion, which can be
ually reduced from 90° with the increase of power and below 10°
explained by Cassie state [32] as shown in Fig. 9 (a). The surfaces
just as the power exceeds 8 W. However, WCA decreases to 135°
30 Y. Song et al. / Optics and Laser Technology 102 (2018) 25–31

Fig. 8. Snapshots of a water droplet free-falling on the fs laser treated surfaces with different scanning speeds: (a) 50 mm/s; (b) 75 mm/s; (c) 100 mm/s; and (d) 200 mm/s.

consist of microstructures covered by plenty of nanostructures, microstructures, which lead to Cassie state, can be formed on parts
which can trap large fraction of air between the water droplet of the surface ablated by fs laser. With the increase of interval, the
and the hierarchical structures. Therefore, the solid-water-air portion of Cassie state is reduced while it increases for the Wenzel
interface is formed and the air can be considered as perfectly state. Therefore, the WCA of surface decreases and the WSA of the
non-wetting [35]. Thus, it leads to extremely low adhesion. Then, surface increases.
if the laser power is diminished or the scanning speed decreases, These superhydrophobic surfaces with controllable adhesion
the microstructures become flat and shallow. Meanwhile, the are potential in many fields. For example, they can be used as a
coarse nanostructures, which are formed on the top of microstruc- kind of water transference equipment for the transfer of small
tures, gradually disappeared and the ripples were emerging. water droplets without any loss or contamination, and oil/water
Hence, the water can partly enter into the structures, as displayed separation [39–44]. As exhibited in Fig. 10, an 8 lL water droplet
in Fig. 9(b). The transitional state can be called Cassie-Wenzel state is first placed on the low adhesive superhydrophobic surface with
or Metastable state [36,37]. In this state, the WCA comparatively a WCA of 163° and a WSA of 1°. Then the middle adhesive super-
goes down and WSA increases, which results in superhydrophobic hydrophibic surface with WCA of 156° to touch the droplet. The
surface with high adhesion. With further decrease of laser power droplet is simply attached to the middle adhesive superhydropho-
or increase of scanning speed, there are just some ripples on the bic surface and the first-step transference is successful. Later on,
surfaces and water fills up the structures, as illustrated in Fig. 9 the middle superhydrophobic surface which carried the water dro-
(c). The third state is called Wenzel state [38]. Through modulating plet is moved to contact with a high adhesive superhydrophobic
scanning speed and laser power, the surface structures can be surface with a WCA of 150°, and the droplet is released on it. More-
tuned so as to change the contact state from Wenzel state to Cassie over, it can be observed that the transference from a low adhesive
state. As for the interval, the phenomenon is a little different. As surface to a high adhesive surface without any loss.
presented in Fig. 9(d), there is Cassie state and Wenzel state simul-
taneously, which is called mixed state. The nanostructures and

Fig. 9. Schematic illustration of four kinds of Al surfaces with various liquid–solid Fig. 10. Photographs for a water droplet (8 lL) during no lost transport from the
contact states: (a) the Cassie state; (b) the Metastable state; (c) the Wenzel state; low adhesive superhydrophobic surface to the high adhesive superhydrophobic
and (d) the Mixed state. surface. The black arrow represents the moving direction of the above sample.
 Y. Song et al. / Optics and Laser Technology 102 (2018) 25–31 31

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China (Grant No. 2017YFB1104300), National Natural Science assisted femtosecond laser irradiation, RSC Adv. 6 (44) (2016) 37463–37471.
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