Results in Physics 12 (2019) 1082–1088

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Results in Physics
journal homepage: www.elsevier.com/locate/rinp

Rapid fabrication of superhydrophobic high-silicon aluminum alloy surfaces T

with corrosion resistance
⁎ ⁎
Yankui Suna, Danyang Zhaoa,b, , Jinlong Songa,b, , Cong Wanga, Zhihao Zhanga, Liu Huanga,
Jiyu Liua, Ziai Liua
a
Key Laboratory for Precision and Non-Traditional Etching Technology of Ministry of Education, Dalian University of Technology, Dalian 116024, PR China
b
Collaborative Innovation Center of Major Machine Manufacturing in Liaoning, Dalian University of Technology, Dalian 116024, PR China

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

Keywords: High-silicon aluminum alloy (high-Si Al alloy) usually used as the electronic packaging materials on the radar on
High-silicon aluminum alloy ships have a susceptibility to corrosion, reducing the life of radar on ships. How to improve the corrosion-
Corrosion resistance resistance ability of high-Si Al alloy is still a challenge. In this paper, we introduced superhydrophobicity on
Superhydrophobic high-Si Al alloy surface by electrochemical etching to improve the corrosion-resistance. The variation of surface
wettability with the etching time was subsequently studied. A better superhydrophobicity with water contact
angle of 163° and roll-off angle of 5° was obtained at 12 min etching time. This superhydrophobicity can ef-
fectively prevent the corrosive solution to corrode the high-Si Al alloy surface and increase the service life.

Introduction on aluminum-silicon alloys with high energy consumption in proces-

High-silicon aluminum alloy (high-Si Al alloy) is often used as the
electronic packaging materials on the radar on ships because of its low
density, suitable thermal expansion coefficient matching with semi-
conductor materials, good heat dissipating performance, and excellent
mechanical property [1–10]. However, as high-Si Al alloy is often long-
term exposed to corrosive atmosphere environment and seawater en-
vironment, it is easily corroded which can reduce the life of radar on
ships. For one thing, the corrosion would waste a lot of high-Si Al alloys
which need more cost than ordinary aluminum alloys [11]. What’s
more, as packaging materials, corrosion in the alloy can easily lead to
some interface defects. This interface defects would cause horrible re-
liability problems of electronic devices under stress concentration and
thermomechanical loading [12]. Therefore, how to improve the cor-
rosion resistance of high-Si Al alloy is one of the urgent problems
needed to be solved in the field of ship radar industry. Till now, only
few methods can be applied to improve the corrosion resistance of high-
Si Al alloy. And these method mainly fall into two kinds: using corro-
sion resistant material as inhibitor and fabricating anti-corrosion oxide
film. Abdallah et al. [13] use animal glues as green inhibitor to improve
the corrosion resistance of high-Si Al alloy. But animal gules are readily
soluble in water so that they are not suitable for seawater environment.
Xue et al. [14] prepared an anti-corrosion film by micro-arc oxidation
sing.
Superhydrophobic surface, with a water contact angle (CA) larger
than 150° and a water roll-off angle (RA) smaller than 10° [15], has
attracted a lot of attention for its potential characteristics, such as
corrosion resistance and self-cleaning [16–18]. There are two elements
to prepare a superhydrophobic surface: rough structure and low surface
energy modification [19]. The voids between rough structures on su-
perhydrophobic surface can easily capture a large amount of air in pits
of the hierarchal rough structures. The corrosive ions cannot migrate in
the captured gas, so the corrosion is inhibited on the superhydrophobic
surface [20]. Obtaining superhydrophobicity on metal substrate has
proven effective in preventing the corrosion of Cu, steel, Mg and Zn
alloys [21–24]. So fabricating superhydrophobic surface on high-Si Al
alloy may be one effective method to prevent its corrosion.
Fig. 1 shows the metallograph of high-Si Al alloy (Al-20%Si), in
which the Si grains uniformly disperse in aluminum matrix. As men-
tioned above, the micro structure is a key element to fabricate super-
hydrophobic surface. If Al was removed partly, silicon particles dis-
tributed in the Al matrix would form the micro-scale structures on the
surface. So a facile electrochemical etching method was applied for
constructing superhydrophobic surface on high-Si Al alloy in this paper,
using a relatively nonpoisonous neutral solium chloride (NaCl) aqueous
solution as electrolyte at room temperature. The rough structures were

⁎
Corresponding authors at: Key Laboratory for Precision and Non-Traditional Etching Technology of Ministry of Education, Dalian University of Technology,
Dalian 116024, PR China.
E-mail addresses: zhaody@dlut.edu.cn (D. Zhao), songjinlong@dlut.edu.cn (J. Song).

https://doi.org/10.1016/j.rinp.2018.12.090
Received 29 November 2018; Received in revised form 30 December 2018; Accepted 30 December 2018
Available online 31 December 2018
2211-3797/ © 2019 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY license
(http://creativecommons.org/licenses/BY/4.0/).
Y. Sun et al.
Fig. 1. The metallograph of high-Si Al alloy.
firstly fabricated on the aluminum-silicon alloy by electrochemically
etching and then modified by low surface energy material.
Experimental section
Fig. 2 shows the process of fabricating superhydrophobic surface on
Al-20Si alloy. High-Si Al alloys (Al-20%Si, 30 mm × 20 mm × 2 mm)
were polished mechanically with 800#, 1200#, 1500# sandpapers to
remove the oxide layer and smoothing the sample substrate surface
before electrochemical etching. Then, the samples were cleaned with
alcohol and deionized water via ultrasonication to remove the oil stains
and residues. In the etching process, the anodic alloy plate and the
cathodic Cu (purity ≥ 99.9%, Hong Wang Die Co., Ltd, Shenzhen,
Guangdong) plate were placed with a distance of 40 mm. The Al-20Si
alloy plates were etched under 100 mA/cm2 current density in the
0.2 mol/L NaCl electrolyte. Then the prepared alloys were immersed in
a 1.0 wt% ethanol solution of Tridecafluoroctyltriethoxysilane
[C8F13H4Si(OCH2CH3)3] (FAS, Degussa Co., Germany) for 1 h and
subsequently heated at 90 °C for 20 min.
The surface morphologies of the obtained samples were character-
ized using a scanning electron microscope (SEM, SUPRA 55 SAPPHIRE,
Germany). The surface roughness was measured using a surface pro-
filometer (ZYGO, NV5000 5022S, America). 5 μL water droplets were
adopted in contact angle and roll-off angle measurement, using an
optical contact angle meter (SL200KS, KINO, USA) and conventional
tilting plate method respectively. 3.5 wt% aqueous solutions of NaCl,
sodium chlorate (NaClO3), and sodium nitrate (NaNO3) were adopted
in electrochemical measurements at ambient temperature using a
computer-controlled potentiostat (Princeton Applied Research,
PARSTAT2273, USA) with external voltage. In these electrochemical
measurements, a three-electrode configuration including a saturated
calomel reference electrode (SCE), a platinum auxiliary electrode and a
Grinding Electrochemical machining
Abrasive paper Ultrasonic
cleaning Anode
Al-20%Si alloy plate Hydrogen ion
Electron
Fig. 2. Schematic representation of fabricating superhydrophobic surface on Al-20%Si alloy.
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Results in Physics 12 (2019) 1082–1088
superhydrophobic high-Si Al alloy sample with an exposure surface of
1 cm × 1 cm as the working electrode, was used. The potentiodynamic
polarization curves were obtained at a scanning rate of 2 mV/s. The
electrochemical impedance spectroscopy (EIS) measurements were
measured in a frequency range from 100 MHz to 2 MHz at a 10 mV
scanning amplitude.
Result and discussion
Wettability of the high-Si Al alloy surfaces
Fig. 3 shows the digital images of water droplets on the different
high-Si Al alloy surfaces. After the FAS modification, the CA of the
original high-Si Al alloy surfaces increased from 31° to 101.4°, de-
monstrating the great effect of FAS on lowing surface energy, as shown
in Fig. 3(a) and (b). When the alloy surfaces were electrochemical
etched for 12 min, it exhibited an excellent superhydrophilicity with a
CA of approximately 0°. After subsequent FAS modification, the alloy
surfaces successfully changed from superhydrophilic to super-
hydrophobic, with a CA of ∼163.2° and a RA of ∼5.5°. The results
clearly indicate that electrochemical etching and low surface energy
material modification are both important in fabricating super-
hydrophobic surfaces on the high-Si Al alloy substrate.
Surface morphologies of the 12 min electrochemically etched high-
Si Al alloy surface were subsequently observed in Fig. 4. The Fig. 4(a)
shows extreme rough microstructure with lots of deep gully and bulges
formed on the alloy surface. From Fig. 4(b), it can be seen that the
shapes of silicon grains in the alloy are various such as bar, plate, ball.
The silicon grains with different shapes and scale combined with each
other by Al matrix form dozens of microns blocks, while the etched and
abscised parts form deep holes and gully. In Fig. 4(c), at the large
magnification, Al matrix has been etched to some small rectangular-
Superhydrophobic
state
Modification
with FAS Droplet
Cathode
Aluminum ion
Silicon Prepared substrate
Y. Sun et al.
Fig. 3. Digital images of water droplets on different high-Si Al alloy surfaces: (a) original alloy surface, (b) original alloy surface with FAS modification, (c) 12 min
electrochemically etched alloy surface, and (d) and (e) 12 min electrochemically etched and FAS-modified alloy surface.
shaped plateaus and grains while the silicon looks like smooth rela-
tively. There are many little holes and pits in dissolved Al matrix closed
to silicon particles. Some attachments on the silicon forms nanoscale
protrusions as shown in Fig. 4(c). Thus, after electrochemical etching,
hierarchical rough structures are formed on the high-Si Al alloy sur-
faces.
A water droplet with a size much larger than the aforementioned
microstructures is suspended on the rough structures instead of pene-
trating into grovels between the structures, forming a Cassie-Baxter
state [25,26]. The contact angles in terms of the Cassie-Baxter equation
is described as follows,
cos θc = rf ·cos θ + f − 1 = f (r·cos θ + 1) − 1
where θc and θ represent the contact angles on the FAS-modified rough
and smooth surfaces, respectively, and f is the fraction of the projected
area of the solid surface that is wet by the liquid, and r is the roughness
ratio of the wet area. Because 0 < f < 1, if 0 < r·cos θ + 1 < 1, the
cos θc < 0. Because θ ≈ 101.4°, that is, cos θ ≈ −0.2, so if
0 < r < 5, under this condition, θc increase with f decreasing.
The chemical composition and organizational structure of high-Si Al
alloy are heterogeneous, including Al, Si and other impurities. In the
alloy, Al matrix acts as the adhesive which entirely encloses and com-
bines the silicon grains. Because of insolubility of Si in the electro-
chemical process, silicon grains gradually emerge with the dissolution
of Al matrix in the process of electrochemical etching. The protruding
silicon grains form microstructures. Meanwhile, larger amount of
Fig. 4. SEM images of the high-Si Al alloy surfaces obtained at 12 min processing time.
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Results in Physics 12 (2019) 1082–1088
plateaus and grains are formed in the Al matrix. Al is one kind of
crystalline metal in which a large number of grain boundaries and
dislocations exist. The grain boundaries dissolve firstly under an ap-
plied electric field, which fabricate the irregular nanometer structures
in the Al matrix. With dissolving of Al matrix, some silicon grains
surrounded by Al begin to loosen and then detach to the electrolyte,
forming the micrometre structure. Finally, the multi-scale micro-
structure was fabricated on the high-Si Al surface.
Effect of the processing time on surface wettability and morphologies
Fig. 5(a, b) shows the variation of the CA, RA and roughness with
the processing time. When the etching time is lower than 12 min, the
CA increase and the RA decrease with the etching time, as shown in
Fig. 5(a). Whereas the roughness always increase with the etching time
increase, as shown in Fig. 5(b). The CA significantly increase to 148° at
4 min etching time, but the RA is so large that the droplet cannot roll
down the surface. As can be seen from the micromorphology [Fig. 5(c)],
there were still a few large island-like blocks with distinct scratches on
the surface, and only few areas was dissolved, exhibiting a low surface
roughness of ∼1.63 μm [Fig. 5(b, d)]. So, at 4 min, the etching depth
and area are not enough to support droplet in Cassie-Baxter state,
droplet beading and pinning on the surface at this time. When the
etching time is at 8 min, large areas are corroded but not uniform, as
shown in Fig. 5(c). The CA is up to 156.2° and the RA is 20°. When the
etching time is at 10 min, the CA is up to 158.1° and the RA is 16.4°.
Y. Sun et al.
Fig. 5. Variation of (a) RA, CA and (b) roughness (Ra) with the etching time; SEM images, CA images (c) and three-dimensional profile (d) of the high-Si Al alloy
surfaces at different etching time.
These indicate the surface cannot achieve superhydrophobicity at 8,
10 min. As can be seen from Fig. 5(a), the TA is always larger than 10°
before 12 min. Compared with the surface topographies at 4, 6, 8,
10 min in Fig. 5(c, d), the surface at 12 min is further etched. At this
time, the superhydrophobicity is obtained with the CA of 163.2° and the
RA of 5.5°. Additionally, the surface roughness also increased to
6.095 μm at 12 min. Moreover, when the etching time prolonged be-
yond 12 min, there was almost no changes in the CA and RA of the
prepared high-Si Al alloy surfaces. Meanwhile, the roughness is in-
creasing, indicating the etching is in process with extra energy con-
sumption beyond 12 min. Therefore, the best superhydrophobicity of
high-Si Al alloy surfaces could be obtained at 12 min etching time.
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Results in Physics 12 (2019) 1082–1088
Corrosion resistance performance of the superhydrophobic high-Si Al alloy
surfaces
Corrosion resistance performance
The corrosion resistance performance of the alloy surface was in-
vestigated by the polarization curves and EIS in different corrosive
solutions. All the superhydrophobic samples were fabricated at 12 min
etching time and the untreated samples were just polished using the
1500# abrasive paper. The Tafel curves were shown in the
Fig. 6(a1–a3). Meanwhile, the corresponding corrosion potential (Ecorr)
and corrosion current density (Icorr) are given in Table 1. The Ecorr of
superhydrophobic high-Si Al alloy surfaces were higher than that of the
untreated ones in all the corrosive solution, indicating that the super-
hydrophobic high-Si Al alloy surface has better corrosion resistance.
Besides, the Icorr of the superhydrophobic high-Si Al alloy surface in the
three measuring corrosive solutions, as shown in Table 1, were less than
Y. Sun et al. Results in Physics 12 (2019) 1082–1088

Fig. 6. Tafel and Nyquist curves of the untreated and superhydrophobic high-Si Al alloy surfaces in different corrosive solution: Tafel curves tested in (a1) 3.5 wt%
NaCl solution, (a2) 3.5% NaClO3 aqueous solution, (a3) 3.5% NaNO3 aqueous solution; Nyquist curves tested in (b1, b4) 3.5 wt% NaCl solution, (b2, b5) 3.5% NaClO3
aqueous solution, (b3, b6) 3.5% NaNO3 aqueous solution.

those of untreated ones respectively. Obviously, the smaller corrosion
current densities of the superhydrophobic samples show better corro-
sion resistance, compared with those of untreated samples, demon-
strating that the superhydrophobicity would slow down the corrosion
process effectively on the high-Si Al alloy surface.
The Nyquist curves of the superhydrophobic and untreated high-Si
Al alloy surfaces are shown in Fig. 6(b1–b6). The impedance of the
superhydrophobic high-Si Al alloy surfaces were much larger than that
of the untreated ones, corresponding to a good corrosion resistance. The
impedance of these two surfaces are very different, so the equivalent
circuits are different either, shown in Fig. 7. The equivalent circuits of
superhydrophobic surface is shown in Fig. 7(a). In these circuits, Rs is
the solution resistance, the Rf is the corrosion layer resistance (super-
hydrophobic layer), and Rt is the charge transfer resistance, C is as-
signed to the capacitance of a surface film and Q is the electrical double
layer capacitance. Fig. 7(b) is the equivalent circuits of untreated sur-
face. As can be seen from Figs. 6 and 7, the superhydrophobicity plays
an important role in improving the anticorrosion of the high-Si Al alloy.
So the superhydrophobic high-Si Al alloy surfaces with higher cor-
rosion potential, lower corrosion current density and larger impedance,
have better electrochemical corrosion resistance performance than the
untreated samples.

Table 1
Corrosion potential (Ecorr) and corrosion current density (Icorr) of the untreated and superhydrophobic high-Si Al alloy surfaces in different corrosive solutions.
Sample NaCl solution NaClO3 solution NaNO3 solution

Ecorr (V) Icorr (A/cm−2) Ecorr (V) Icorr (A/cm−2) Ecorr (V) Icorr (A/cm−2)

Untreated surface −0.625 1.046 × 10−5 −0.717 6.714 × 10−7 −0.613 4.923 × 10−7
Superhydrophobic surface −0.581 1.448 × 10−6 −0.339 1.174 × 10−8 −0.127 1.254 × 10−9

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Fig. 7. Equivalent circuits of the superhydrophobic (a) and untreated (b) high-Si Al alloy surfaces in different corrosive solution.
Corrosive media
Air
Si Si
Al
Fig. 8. Schematic of superhydrophobic surface and prevention of corrosion.
Corrosion resistance mechanism of superhydrophobic high-Si Al alloy
surfaces
From above experiments, it is obvious that superhydrophobic layer
on high-Si Al alloy has great corrosion resistance performance. High-Si
Al alloy as the electronic packaging materials on the radar on ships
usually used in atmospheric environment, rather than in seawater.
However, radar will be flapped by the waves in atrocious weather.
Under this condition, seawater would bead and then roll from the su-
perhydrophobic surface. This way reduces the contact time between
surface and seawater, thus decreasing the possibility of corrosion.
The reason of drops rolling from the superhydrophobic surfaces is
mainly considered on three factors: low surface energy, rough micro-
structure and capillarity [19,27]. First, the spreading of liquid would be
limited on the surface with low surface energy. Furthermore, the air
trapped on the rough structure with low surface energy acts as a
blocking layer as shown in Fig. 8, reducing the contact area between
Fig. 9. Self-cleaning performance test of the superhydrophobic high-Si Al alloy surfaces.
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Results in Physics 12 (2019) 1082–1088
liquid and solid. Moreover, capillarity would keep the water opposing
its own gravity in the rough porous structure of the superhydrophobic
surfaces. Thus, the liquid can be driven out from the gaps of super-
hydrophobic surfaces by the Laplace pressure [24,28]. So the drops can
rolling down easily.
In the contact process, as shown in Fig. 8, the anti-corrosion me-
chanism of the superhydrophobic surfaces is mainly considered on the
following two factors. An important factor is the existence of hydro-
phobic molecules, as modified layer on the superhydrophobic surface
[29,30]. Choosing the suitable low surface energy material would
promote efficiency of corrosion protection properties. Besides, the ac-
tive ions cannot contact the underlying surface due to the existence of
trapped air, and they contact with the protruding silicon particles and a
little Al. Silicon itself has a strong corrosion resistance for common
corrosion solution. So superhydrophobic layer can inhibited the cor-
rosion on the surface.
Self-cleaning performance of the superhydrophobic high-Si Al alloy surfaces
Self-cleaning is one of the most important properties of super-
hydrophobic surfaces, which can be helpful to remove the contaminants
on the surfaces with liquids such as raindrops. Fig. 9 shows the self-
cleaning performance test using the powders mainly composed of cal-
cium sulfate (CaSO4) as contaminants. It could be obviously observed
that drop-by-drop added water droplets could take all the powders
away from the superhydrophobic surface, indicating an excellent self-
cleaning performance of the prepared samples.
Stability of corrosion resistance performance
Since superhydrophobicity is expected to improve the corrosion
resistance of high-Si Al alloy on the radar on ships, the stability of
Y. Sun et al.
Fig. 10. Changes in CAs of superhydrophobic high-Si Al alloys exposed to air (a) and 3.5% NaCl solution (b) for different time.
superhydrophobic high-Si Al alloy is very important for its real appli-
cation. Because the high-Si Al alloys on radar are usually exposed to
atmospheric environment and seawater, so we then tested the influence
of the exposure time in air and immersion time in the 3.5% NaCl so-
lution on the CAs of the samples, as shown in Fig. 10. For the air en-
vironment, the CAs of superhydrophobic high-Si Al alloy surfaces kept
stable for at least 5 months. For the 3.5% NaCl solution, the samples
still showed superhydrophobicity with CAs larger than 150° even im-
mersed for 24 h. All these indicate the superhydrophobic high-Si Al
alloy surfaces have good stability.
Conclusion
The promising superhydrophobic surfaces with water CA of 163.2°
and RA of 5.5° were fabricated on the high-Si Al alloy substrate via an
electrochemical etching method and FAS modification. Corrosion re-
sistance performance of the superhydrophobic high-Si Al alloy were
investigated to illustrate the protective property of super-
hydrophobicity to the substrates. The results of electrochemical mea-
surements indicate that superhydrophobic surface have outstanding
corrosion resistance performance in different electrolyte solutions.
Moreover, superhydrophobic high-Si Al alloy surfaces revealed ex-
cellent self-cleaning performance.
Acknowledgements
This project was financially supported by National Natural Science
Foundation of China (NSFC, 51605078), the Science Fund for Creative
Research Groups of NSFC (51621064), Aviation Science Fund
(2017ZE63012), the Doctoral Scientific Research Foundation of
Liaoning Province (201601058) and the Fundamental Research Funds
for the Central Universities (DUT17JC25).
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://
doi.org/10.1016/j.rinp.2018.12.090.
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