Colloids and Surfaces A xxx (xxxx) xxxx

Contents lists available at ScienceDirect

Colloids and Surfaces A

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

Fabrication of super-hydrophobic micro-needle ZnO surface as corrosion

barrier against corrosion in simulated condensation environment
⁎
Shudi Zhanga, Xiangli Zhenga,b,c, Peng Wangb,c,d, , Dun Zhangb,c,d
a
Environmental and Chemical Engineering Institute, Shenyang Ligong University, 6 Nanping Middle Road, Shenyang 110159, China
b
Key Laboratory of Marine Environmental Corrosion and Biofouling, Institute of Oceanology, Chinese Academy of Sciences, 7 Nanhai Road, Qingdao 266071, China
c
Open Studio for Marine Corrosion and Protection, Pilot National Laboratory for Marine Science and Technology (Qingdao), 1 Wenhai Road, Qingdao 266237, China
d
Center for Ocean Mega-Science, Chinese Academy of Sciences, 7 Nanhai Road, Qingdao, 266071, China

G R A P H I C A L A B S T R A C T

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

Keywords: A super-hydrophobic surface (SHS) which facilitates the micro-droplet self-bounce was fabricated over copper
Super-Hydrophobic substrate with hydrothermal synthesis method. It was characterized with FE-SEM, XRD, and so forth, and its
Micro-Needle corrosion protection performance was evaluated with electrochemical measurement. It was demonstrated that
Condensation environment the needle-cone structure of super-hydrophobic surface facilitates the micro-droplets self-bounce behavior. Self-
ZnO
bounce effect of super-hydrophobic surface can help to reduce the contact area between the water droplet and
Atmospheric corrosion
the surface, thereby reducing the corrosion process of substrate under simulated condensation environment. This
research provides a novel direction for the development of corrosion protection methods.

1. Introduction applications. Especially in the environment of the marine atmosphere,

the corrosion of metals is more severe. Since the moisture content in the
Metal materials have a wide range of applications in the chemical marine atmosphere is very high, and the air humidity can reach
and microelectronics industries due to their good electrical and thermal 70%–80%, rich in water vapor and oxygen provides sufficient favorable
conductivity. However, corrosion problems which will cause damage to conditions for electrochemical corrosion. Metal corrosion may cause
materials, even loss of function result in great trouble for metal parts to fail and the equipment to be scrapped. In severe cases, it can

⁎
Corresponding author at: Key Laboratory of Marine Environmental Corrosion and Biofouling, Institute of Oceanology, Chinese Academy of Sciences, 7 Nanhai
Road, Qingdao 266071, China.
E-mail address: [email protected] (P. Wang).

https://doi.org/10.1016/j.colsurfa.2019.124087
Received 17 July 2019; Received in revised form 30 September 2019; Accepted 8 October 2019
Available online 14 October 2019
0927-7757/ © 2019 Published by Elsevier B.V.

Please cite this article as: Shudi Zhang, et al., Colloids and Surfaces A, https://doi.org/10.1016/j.colsurfa.2019.124087
S. Zhang, et al. Colloids and Surfaces A xxx (xxxx) xxxx

cause major safety accidents [1–3]. Therefore, corrosion protection of mixed with 2 M NaOH and 0.25 M Zn(NO3)2・6H2O. A copper sheet
metals has always been an urgent problem to be solved. was polished mechanically and ultrasonic rinsed in ethanol. Then the
Research and development in the area of corrosion protection has as-prepared solution and copper sheet were sealed into a Teflon-lined
led to the identification of various methods for protecting metal ma- stainless-steel autoclave with a capacity of 100 mL for hydrothermal
terials from corrosion. Common methods include alloying, coating and treatment at 60 ℃ for 2 h [20–23]. After hydrothermal process, the
gas phase anti-rust paper coating. Alloys mainly benefit from the pro- copper sample was washed by deionized water and dried by air, sealed
tective films formed by doped metal passivation. Coating is a method of into a lining of Teflon Reactor with 10 μL PFDS, and then heated at
covering the metal surface with a non-metallic material to achieve the 120 ℃ for 2 h. Finally, the copper sheet was heated again at 150 ℃ for
purpose of protecting the base metal. Porcelain and electroplating were 60 min without the cap to remove excess PFDS [24].
commonly used presently. Moreover, gas phase anti-rust paper coating
is one of temporary protections. 2.3. Condensation experiment
Different from the above, super-hydrophobic surface is a potential
corrosion protection method, and it was mostly used in underwater The sample was placed in a plastic box sealed with plastic wrap at
metal corrosion protection in previous reports [4–9]. Super-hydro- room temperature, positioned vertically and temperature-controlled to
phobic surface refers to a kind of surface with a static water contact ～5 °C. Humid air was pumped inward to keep internal humidity
angle greater than 150° and a rolling contact angle less than 10°, and 70 ± 5% [25]. Meanwhile, Real-time shooting of the condensation on
the droplets are in contact with the surface by the Cassie model the surface was taken with an optical microscope system (Digital mi-
[10–12]. Since it is able to insulate water, it can protect the base metal croscope, Hirox RH-2000, Japan). Photos of samples partially sub-
from corrosion quite well in aqueous solution [13,14]. Our team has merged in deionized water were taken to verify the existence state of air
previously confirmed the potential application of super-hydrophobic layer trapped in the micro-structure of super-hydrophobic surface be-
surface in atmospheric corrosion protection caused by salt deliquesce fore and after the condensation experiment.
based on the “lotus” effect [15,16]. However, the “lotus” effect of super- In order to test the lifetime of the superhydrophobic film, the
hydrophobic surface highly relays on the external force, thereby sample was subjected to the same condensation experiment cycle 10
blocking its application in atmospheric corrosion protection. Recently, times. Each cycle lasted 15 min, and the contact angle of the sample was
self-jumping effect of condensation droplet over super-hydrophobic measured after each experimental cycle.
surface has attracted much attention for its potential application in heat
transfer, and so forth [17]. It was reported that the droplets will self- 2.4. Surface characterization
bounce off some super-hydrophobic surfaces with special micro-mor-
phology due to excess energy when two or more droplets with similar Water contact angle was measured with a contact angle measure-
volume merge [18,19]. It was known that there are many factors in- ment (OCA200, dataphysics, Germany) at ambient temperature.
fluencing atmospheric corrosion process, such as condensation beha- Microstructures of the samples were characterized with field emission
vior. Condensation behavior is an important factor in inducing the scanning electron microscopy (FE-SEM, JSM-6700, JEOL Co., Japan).
formation of a liquid film on the surface of the material, which in turn The chemical composition of super-hydrophobic film was acquired by
induces corrosion. X-ray diffraction (XRD, Ultima IV, Rigaku Co., Japan) and X-ray pho-
In theory, the self-bounce effect reduces the coverage and residence toelectron spectrometer (XPS, Escalab 250Xi, Thermo, American).
time of condensation droplets on superhydrophobic surfaces, thereby
reducing the probability of corrosion occurring. Therefore, it might be a 2.5. Electrochemical experiments
new access to reducing condensation-related corrosion over super-hy-
drophobic surfaces. polarization curves were obtained with a computer-controlled
In this research, a super-hydrophobic surface of zinc oxide with electro-chemical system (Zahner Zennium pro, Germany) in 3.5 wt.%
nano-needle cone structure is fabricated on a copper surface with hy- NaCl solution at ambient temperature. The experiments were operated
drothermal synthesis method. It is revealed that the as-fabricated sur- in a three-electrode cell with a platinum electrode as the counter
face facilitates self-bounce of condensed droplets. Based on the com- electrode, and saturated calomel electrode as the reference electrode.
parison of the water layer existing state and electrochemical The scanning rate of polarization curves was 0.5 mV/s. Tests were re-
performance of the super-hydrophobic surface before and after con- peated more than three times to verify the repeatability of the results.
densation, it was suggested that the super-hydrophobic surface presents
high corrosion protection performance under simulated condensation 3. Results and discussion
condition based on the self-bounce effect. This research demonstrated a
novel mechanism of super-hydrophobic surface in corrosion protection. 3.1. Micro-morphology and wettability

2. Experimental Fig. 1 shows the microstructures and contact angles of the filmed
Cu. The filmed Cu is covered with needle-cone structures, which are
2.1. Material and reagents arranged in clusters (Fig. 1a). The nanocolumn has a hexagonal pyr-
amid shape (Fig. 1b). One single nanocolumn is approximately 2.6 μm
Super-hydrophobic films were prepared over Cu ( ≥ 99.9 wt.%) in length and 0.3 μm in bottom diameter. The thickness of zinc oxide
substrate with hydrothermal synthesis. The size of a copper sheet was film can be seen from Fig. 1c to be about 4 μm. There is enough gap for
1.5 cm × 5 cm × 1 mm. The chemical reagents including Zn these needle-cone structures to trap air in it. Due to these needle-cone
(NO3)2・6H2O ( ≥ 99.0%), NaOH ( ≥ 96.0%) and ethanol ( ≥ 99.7%) structures, there top area is quite small. When the droplets are in
were purchased from Sinopharm Chemical Reagent Co., Ltd, China. contact with these nanostructures, the viscous force on the contact
Besides, 1H, 1H, 2H, 2H-perfluorodecyl triethoxysilane (PFDS, surface is small, and the droplets are more likely to bounce on this kind
≥ 96.0%) which was used for modification was obtained from Aladdin of surface. It is obviously that the filmed Cu presents super-hydrophobic
Industrial Co., China. property since the static water contact angle is 157.4 ± 2° (Fig. 1e). In
contrast, the contact angle of the bare surface is 76.1 ± 2°, indicating
2.2. Super-hydrophobic film preparation that it is a hydrophilic surface (Fig. 1d). Hydrophilic surfaces are prone
to corrosion due to long contact with droplets. Owing to the micro-
Hydrothermal synthesis was performed in an aqueous solution structure, the contact area between the superhydrophobic surface and

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S. Zhang, et al. Colloids and Surfaces A xxx (xxxx) xxxx

Fig. 1. FE-SEM front-view imagines (a, b) and side-view imagine (c) of filmed Cu, the contact angle of bare Cu (d) and filmed Cu (e).

water droplet is substantial reduced [26]. At this time, the surface

tension of the droplet increases, and the free energy of the surface of the
material is quite low because of the PFDS. Thus, the wettability of the
material is lowered and the hydrophobicity of the filmed Cu can be
observably strengthened.
Moreover, there are many factors that influence whether a droplet
can bounce from the surface, one of which is the parameter of the na-
nostructure. Generally, the super-hydrophobic surface facilitates the
bounce behavior of micro-droplets, in case that the height of the na-
nocolumn is greater than 0.5 μm, and the spacing of the nanocolumns is
greater than 2 times and less than 10 times of its diameter [27]. If the
spacing between the nanocolumns is too small, the combined droplets
are subjected to excessive resistance during the movement, which re-
sults in difficulty for droplets to bounce off the surface. Conversely, if
the nanocolumn spacing is too large, the condensed droplets will con-
tact the surface with the Wenzel model. From Fig. 1a we can distinguish
that the length and spacing of the nano zinc oxide are suitable, so the
surface has the ability to cause the droplet to self-bounce.

3.2. Film composition Fig. 2. XRD patterns of filmed Cu.

Fig. 2 shows the XRD spectra of the filmed Cu. the peaks located at
32.0°, 34.6°, 36.4°, 47.7°, 56.8° and 62.9° are ascribed to (100), (002),
(101), (102), (110) and (103) planes of ZnO [PDF NO. 79-0206]

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Fig. 3. The XPS results of filmed Cu (a) survey spectrum, (b) O 1s spectrum, (c) C 1s spectrum, (d) F 1s spectrum.

respectively. Meanwhile, the peaks located at 43.5°, 50.5° and 74.2° are or external forces. Without external force, the sudden disappearance of
ascribed to (111), (200) and (220) of Cu [PDF NO. 4-836] respectively. the droplet should be the occurrence of self-bouncing behavior. Also,
The peaks indicate that the sample mainly contains copper and zinc Video 1 shows macroscopically the behavior of droplets bouncing off
oxide. Copper performs as the base material, so the main component of the surface and falling during condensation, which further confirms the
the film is zinc oxide. theory of droplet self-bouncing. Furthermore, droplet coverage in the
Fig. 3 represents the XPS spectra of the copper sample covered with field of vision is much lower than it on bare surface at the ending time
PFDS. The survey spectra prove the existence of Si, Zn, O, F and C (Fig. 4b, c).
elements over the sample (Fig. 3a). Two components with the binding Fig. 5 is a model of the deformation and upward movement of the
energies (Bes) of 531.8 eV and 530.6 eV can be resolved from the O1 s combined droplets. Because the specific surface area of the newly
spectrum (Fig. 3b). They correspond to the O element in -Si-O bond and merged droplet is much larger than it in equilibrium, the droplet has
ZnO matrix, respectively. Moreover, it is easy to identify that the -CF3 excessive surface free energy. Thus, excess free energy will drive dro-
group at 293.7 eV, -CF2- group at 291.6 eV, −CH2-CF2 group at plets to change to the equilibrium state (Fig. 5b). During the transition,
288.9 eV, and CeC bonds at 284.7 eV (Fig. 3c). Also, the C–F bonds at the center of gravity of the droplet deviate from the surface and radius
688.7 eV can be identified from the F 1 s spectrum (Fig. 3d) [28–31]. of the surface of droplet in contact with the surface decreases until
These results demonstrate that the PFDS chemically bonds with the ZnO equilibrium state is reached (Fig. 5c). The driving force of this trans-
layer during the modification process. PFDS is a kind of silane. When it formation process is the difference of surface tension component on
is heated, it volatilizes and adheres to zinc oxide film, thus reducing surface between unstable and equilibrium states [32]. Meanwhile, the
surface energy. Lower surface energy can reduce the resistance of resistance is the adhesion during the base area reduction. After the
droplets during bouncing, which provides the possibility for droplet droplet reaches equilibrium state, due to the effect of inertia, the center
self-bouncing. of gravity of the droplet continues to deviate from the surface and the
liquid radius continues to shrink. At this point, the movement of the
3.3. Condensation behavior on super-hydrophobic surface center of gravity needs to overcome the resistance on the three-phase
line. When the liquid radius is reduced to 0 nm (Fig. 5d), if the center of
Typical time-lapse optical front-views of self-departure instant of gravity of the droplet still has an acceleration deviating from the sur-
condensate micro-drops on the vertical super-hydrophobic surface are face, which means the droplet still has excess kinetic energy to over-
shown in Fig. 4. Droplets are formed by condensation of ambient water come the surface viscous energy, the drop will bounce off the surface
vapor, and growth respectively on the sample surface. Then in-plane and make free fall motion (Fig. 5e).
coalescence of adjacent microdrops which have similar volume con- Moreover, the sample after condensation can still keep the air film
tributes to the self-departure events. As is shown in Fig. 4a, the merged well (Fig. 6). The surface has the ability to cause the droplet to self-
microdrop ejected from the vertical nanosample surface and vanished bounce behavior, and it indicates that most droplets exist on the na-
from sight. Since the droplets around the merged droplets remained nosample surface as Cassie mode during and after condensation because
unchanged, the disappearance of the droplets was not caused by rolling of droplets self-bounce behavior. Therefore, the contact area and time

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S. Zhang, et al. Colloids and Surfaces A xxx (xxxx) xxxx

Fig. 4. (a) Optical front-views showing coalescence-induced condensate microdrop self-departure on the vertical filmed Cu surface. (b) Front-views showing the
ending time of condensation. (c) Front-views showing the ending time of condensation of bare surface.

5
S. Zhang, et al. Colloids and Surfaces A xxx (xxxx) xxxx

Fig. 5. Schematic diagram of deformation and upward movement of droplets after merging: (a) two droplets to coalesce; (b) initial metastable state of the coalesced
drop with apparent contact angle smaller than the equilibrium value;(c) The droplet reduces its base radius to equilibrium value; (d) The droplet continues to reduce
its base radius to 0 mm relying on its transformation inertia; (e) out-of-plane jumping of the droplet.

between droplets and surfaces are greatly reduced.

3.4. Corrosion protection performance

Fig. 7 presents the polarization curves of super-hydrophobic film-

coated sample after condensation (SSAC), deaerated super-hydrophobic
film-coated sample (DS) which was immersed in ethanol, allowing
ethanol to replace the air in the microstructure and bare surface (BS)
[33]. The anodic polarization current density of SSAC is about two
orders of magnitude smaller than the other two samples. This data
means that the SSAC is more resistant to corrosion than the other two
surfaces. It indicates that on this kind of surface, condensed droplets
cannot replace the air in the nanostructures, and the sample still keep
the air film well even after condensation. Therefore, the corrosion re-
sistance of the sample is still very good after condensation. Owing to
super-hydrophobic film contacting with NaCl solution in the Cassie
mode, the solution is not in contact with the base metal [34]. Thus, the
metal dissolution disappeared from the polarization curve. This result Fig. 7. The polarization curves of SSAC, DS and BS in 3.5% NaCl solution.
proves that the super-hydrophobic film which has the ability to cause
the droplet to self-bounce behavior presents a great inhibiting effect on 3.5. The lifetime of the superhydrophobic film
the corrosion of underlying copper which has to experience moisture
condensation hazards [35]. As a result, droplets condensation cannot Fig. 8 shows the results of lifetime testing of the superhydrophobic
destroy the integrity of super-hydrophobic structure with the ability of film. After 10 cycles of condensation experiment, the sample still re-
causing droplets to self-bounce behavior. This kind of surface has good tained superhydrophobic property. After several cycles, the change of
corrosion protection even after condensation. contact angle gradually decreased. This was because droplets contacted

Fig. 6. Images showing SH-Surface partially submerged in deionized water before (a) and after (b) condensation.

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