Surface Innovations Pages 49–60 http://dx.doi.org/10.1680/si.14.

00001
Research Article
Volume 3 Issue SI1
Received 07/01/2014 Accepted 02/05/2014
Assessing durability of superhydrophobic Published online 29/05/2014
surfaces Keywords: degradation/superhydrophobicity/surface
characterization/surface durability
Malavasi, Bernagozzi, Antonini and Marengo

ice | science ICE Publishing: All rights reserved

Assessing durability of
superhydrophobic surfaces
1 Ileana Malavasi MSc 4 Marco Marengo PhD*
Department of Engineering, University of Bergamo, Dalmine (BG), Italy Department of Engineering, University of Bergamo, Dalmine (BG), Italy
School of Computing, Engineering and Mathematics, University of
2 Ilaria Bernagozzi MSc Brighton, Brighton, UK
Department of Engineering, University of Bergamo, Dalmine (BG), Italy

3 Carlo Antonini PhD

Department of Engineering, University of Bergamo, Dalmine (BG), Italy
Laboratory of Thermodynamics in Emerging Technologies,
Department of Mechanical and Process Engineering, ETH Zürich,
Zürich, Switzerland

1 2 3 4
                   

Superhydrophobic surfaces (SHS) show remarkable water repellency properties, and their use may have a tremendous
impact for a plethora of applications, where liquid water accumulation needs to be controlled or minimised. However,
the durability of SHS in operational conditions is a severe issue that currently represents a bottleneck for the
technology transfer from laboratory to industrial applications. In the present work, we try to fill in the gap caused by
the absence of a standard for evaluation for SHS durability, by developing a protocol for testing surface durability.
The proposed protocol includes nine tests as follows: water immersion, acidic environment, alkaline environment,
ionic solution, mechanical erosion, ultraviolet exposure, resistance to heating, alcohol immersion and hydrocarbon
immersion. The protocol can serve to give an indication of surface robustness in a variety of potentially harmful
environments, by providing a global figure of merit and ranking for different SHS and thereby allowing for identifying
those surfaces fulfilling requirements for a specific application. To illustrate the protocol, we tested a SHS developed
in-house by grafting of lauric acid molecules on an aluminum substrate. This article contains supporting information
that is available online.

1. Introduction
In the past decade, superhydrophobic surfaces (SHS) have
attracted an increasing interest in both the academic and
industrial  sectors due to their remarkable self-cleaning and
anti-sticking properties1–3 and for the wide range of potential
applications: biomedical applications,4 microfluidics,5 corrosion
resistance,6 drag reduction,7,8 anti-icing,9,10 contamination and
oxidation.4,11
SHS are highly hydrophobic surfaces on which liquid water
adhesion is very low; therefore, they are extremely difficult to wet
by water. SHS cause the water droplet to bead up on the surface
instead of spreading on it. In addition, capillary adhesion forces
are low, so that water drops typically preserve a high mobility on
the surface.
Although SHS possess remarkable non-wetting properties, one
critical issue is represented by surface durability.12 Indeed, SHS
typically suffer from durability issues (i.e. their superhydrophobicity
does not persist for a long time and/or in particular environmental
conditions),13 which result in loss of superhydrophobic properties
and the ability to repel water. As such, the success of a SHS depends
not only on its wetting performances but also on its ability to last
over time and resist to erosion and abrasion.14,15 Nonetheless, only
few papers so far have addressed the durability issues, each of them
using a different method to assess surface durability,16–18 so that a

*Corresponding author e-mail address: m.marengo@brighton.ac.uk

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 Surface Innovations
Volume 3 Issue SI1
systematic approach to the issue of durability is still lacking in the
literature.
Driven by the need to define a standard procedure for testing
SHS durability, we developed a new protocol that can serve
to test resistance of SHS, when exposed to potentially critical
environments, and can also be used to allow comparison of various
SHS, fabricated using different techniques and processes.
1.1 Superhydrophobicity
SHS are solid surfaces characterised by liquid water repellency
and low water adhesion. For this reason, they are also known as
low-wetting or non-wetting surfaces. To characterise the degree of
wetting (or wettability), contact angles are typically used. When
a water drop is deposited on a solid surface, the equilibrium
configuration of the liquid, vapor (i.e. air) and solid phase at the
three-phase contact line is defined by the balance surface tensions
between each pair of the three phases.19 In particular, for an ideally
smooth and homogeneous surface, the equilibrium contact angle θ
is described by the Young’s equation:19
1. γ lg cosθ = γ sg − γ sl
where γlg, γsg and γsl are the surface energies per unit area between
the liquid and the gas, the solid and the gas and the solid and the
liquid, respectively.
On an ideal surface, the equilibrium contact angle is unique. On
a real surface, where chemical and morphological heterogeneities
exist, multiple metastable configurations, and thus multiple contact
angles, can be observed. As such, to better characterise a surface,
it is necessary to provide both the advancing and receding contact
angles, θA and θR, respectively, measured by expanding and
contracting sessile water drops on a horizontal surface; this method
is usually referred to as “sessile drop method”.20 The advancing
contact angle is the maximum stable angle, and receding contact
angle is the minimum stable angle in static conditions. θA and θR
not only provide the range of contact angles at equilibrium but also
provide an indication of the drop mobility, which is related to their
difference, the contact angle hysteresis, Δθ = θA − θR.
In the literature, SHS are traditionally defined as surfaces on
which advancing contact angles exceed 150° and the hysteresis is
less than 10°.9,21,22 However, such criteria are somewhat arbitrary
and should not be taken strictly. As an example, Rioboo et al.23
recently defined a new methodology based on controlled drop
slide on a horizontal surface. The authors found that only when the
receding contact angle is above 135°, the surface can be defined as
superhydrophobic and the drop slides. The proposed limit is also
close to the value 138·6°, which was identified using a theoretical
model by Li and Amirfazli,24 as the minimum receding contact
angle on a pillar-like surface.
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Assessing durability of superhydrophobic
surfaces
Malavasi, Bernagozzi, Antonini and Marengo
As such, in the present paper, we used two conditions for
superhydrophobicity: (a) θR > 135° and (b) Δθ < 10°.
High contact angles and low contact angle hysteresis can be
typically achieved when the drop is in the so-called Cassie–Baxter
state (Figure 1b): in this state, the drop is only partially in contact
with the solid substrate thanks to the presence of gas pockets at the
interface; in contrast, in the Wenzel state, the drop wets the surface
completely (Figure 1a).
1.2 Durability of SHS
The measurement of contact angles, which, as mentioned above,
allows characterising the wettability of a surface, is also a good and
facile method to monitor the superhydrophobicity of the surface
during its ageing.
Li et al.25 reported an approach for preparing SHS by spray
coating of polymerised organosilane/attapulgite nanocomposites,
showing that the coatings were stable after being kept at a water
pressure of 6000 Pa for 5 min, against ultraviolet (UV) irradiation
(200–400 nm for 30 min) and high (200°C for 1 h) and low
(−30°C for 1 h) temperatures, resistant to weak basic solution
(0·1 M NaOH for 1 h) and organic solvents (slight decrease in the
contact angle and a slight increase in sliding angle after immersion
in 0·1 M HCl for 1 h). Cheek et al.26 investigated the loss of
superhydrophobicity only under continuous submersion in water,
which is characterised by the degradation of the trapped air layer,
for various superhydrophobic polymer nanocomposite coatings.
The loss of superhydrophobic performance under continuous
submersion, which is characterised by the degradation of the
trapped air layer, is defined as saturation. The organoclay/MCPU/
PMC nanocomposite resisted not more than 3 h before saturation
was reached. The ZnO/PMC coating resisted more than 12 h before
full saturation was reached. Finally, the organoclay/PUR/PMC
formulation yielded a period, before full saturation, greater than
48 h. Jin et al.27 obtained superhydrophobic and superoleophobic
surfaces from surfactant-modified silica aerogels and evaluated
the wear resistance of the produced surfaces by means of a
mechanical sandpaper abrasion test. Cho et al.28 fabricated SHS
(a) (b)
Figure 1. (a) Representation of the Wenzel state. (b) Representation
of the Cassie–Baxter state
 Surface Innovations
Volume 3 Issue SI1
with nanoscale structures by alkali surface modification method
and self-assembled monolayer coating of fluorinated molecules.
Hierarchical structuring of the surface was achieved by combining
sandblasting techniques for microtexturing and forming an
aluminum hydroxide layer for nanostructuring. Abrasive test was
utilised to evaluate the mechanical durability of the fabricated
surfaces, and the result shows that the superhydrophobicity of
aluminum hydroxide structure becomes more robust by forming
hierarchical roughened structures. Zhou et al.29 investigated
mechanical properties of superhydrophobic fluoropolysiloxane/
TiO2 nanocomposite coatings using pendulum hardness rocker
measurements and nanoindentation measurements. Wang et al.30
prepared superhydrophobic PTFE/PVDF composite surfaces and
tested their mechanical stability with a homemade scratch tester.
Guo et al.8 fabricated SHS with hierarchical flower-like structure
and tested their stability in acidic and basic conditions. Feng
et  al.31 prepared superhydrophobic alumina surfaces and studied
the effect of time and various corrosive solutions on the wettability
of the prepared SHS. Zhu et al.32 evaluated the mechanical
durability of the obtained superhydrophobic fabric by finger
touching and abrasion with sandpaper. Zhang et al.33 checked the
easy-to-clean property and the durability of a superhydrophobic
γ-alumina–coated stainless steel in a paper machine. Steele
et al.34 investigated substrate adhesion for superhydrophobic
coatings fabricated from polyurethane modified with waterborne
perfluoroalkyl methacrylic copolymer and a montmorillonite clay
nanofiller. The authors characterised the adhesion strength with a
90° tape testing method. High contact angles and low contact angle
hysteresis could be preserved under 1750 N/m adhesion strength
tape testing, and significant resistance could be observed as high
as 3850 N/m. Zhu et al.35 prepared a superhydrophobic metal/
polymer composite surface, and the mechanical durability of the
surface was evaluated by scratch and friction tests. The scratch
test was conducted on a homemade scratch tester: 1500 mesh
sandpaper served as an abrasion surface, with the surface to be
tested facing this abrasion material. The friction test was studied
using a ball-on-plate tribometer under reciprocating motion.
Schutzius et al.36 synthesised elastomeric superhydrophobic
nanostructured composite coatings by solution-based processing
of nitrile rubber and two separate particle fillers, nanoscale carbon
black and submicron-scale poly(tetrafluoroethylene). The coatings
were applied on various flexible substrates, which are subsequently
stretched uniaxially. The authors have shown that mechanical
failure of the superhydrophobicity of the composite coating on
silicone rubber occurs at strains at around 30% and that permanent
deformation of the coating on the polyester fabric substrate began
to occur beyond 70% of strain. Amirfazli37 investigated how SHS
change due to wear. The author used an abrasive wear device to
evaluate material durability based on change in surface properties,
such as roughness. He found that advancing and receding contact
angles are not equally susceptible to wear; receding contact angle
is more sensitive to wear than advancing contact angle, with a
consequent increase of contact angle hysteresis and reduction of
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Assessing durability of superhydrophobic
surfaces
Malavasi, Bernagozzi, Antonini and Marengo
drop mobility. Boinovich et al.38 analysed the durability of SHS by
evaluating the contact angle time evolution after soaking the sample
in water for a long time. Larmour et al.39 reported a method for
preparing a new type of superhydrophobic composite material by
compression of superhydrophobic metal particles. Since the entire
material and not only the surface is functionalised, removing outer
layers by abrasion did not result in loss of superhydrophobicity,
since it led to exposure of a fresh portion of the underlying
superhydrophobic material. Jung and Bhushan14 investigated the
durability of their surfaces by conducting waterfall/jet tests and
monitoring the surface degradation by AFM and a ball-on-flat
tribometer. Bayer et al.40 reported fabrication of superhydrophobic
hybrid anaerobic adhesive films, which was capable to resist
exposure to acidic (pH: 2) and basic (pH: 10) aqueous solutions:
no change in superhydrophobicity was measured within 3 days of
observation of liquid blobs placed on the adhesive coatings for both
liquids. Moreover, these films preserved their superhydrophobicity
even if by removal of few microns of the coating by sanding:
gentle surface polishing was performed using a 3M 1000 grit
aluminum oxide sand paper mounted on a rotating disk applying
~0·06 kg/cm2 downward force. Yanagisawa et al.18 evaluated the
abrasion resistance of transparent superhydrophobic coating,
fabricated by combining crater-like silica films with boehmite
powder. Cui et al.41 prepared SHS with multiscale structures on
paint films and tested its durability to the high speed scouring
test and in neutral and basic aqueous solutions and in some
common organic solvents. Cui et al.42 also studied the stability of
four SHS by high-speed current scouring method. Zimmermann
et al.43 studied the long-term environmental durability of a
superhydrophobic silicone nanofilament coating with natural and
artificial weathering tests. Zimmermann et al.44 tested the chemical
stability of a superhydrophobic silicone nanofilament coating by
dipping the surface in various liquid media over a period of 6
months. Wang et al.45 fabricated a superhydrophobic copper fatty
acid carboxylate surface, and they reported that the surface had
stability in observance to organic solvent treatment and exposure
to air. Wang et al.17 studied the stability of the superhydrophobic
polybenzoxazine surface for all the pH environments. Guo et al.46
tested the durability of SHS after a long time immersion in acid
and alkali environments.
The durability of SHS in operational conditions is a severe issue
that currently represents a bottleneck for the technology transfer
from laboratory to industrial applications. Although some efforts
have been done in the direction of assessing surface durability, to
the best of our knowledge, no systematic procedure was developed
so far. With few exceptions (e.g. Li et al.25 and Bayer et al.40), the
majority of articles reported only partial tests, for example, only
mechanical stability or only chemical stability, but not both. In
addition, methods to test mechanical stability can vary significantly,
so that performances of different coatings can be hardly compared.
Indeed, no protocol exists to allow a direct comparison between
the various surfaces with respect to durability. In the present work,
51
 Surface Innovations
Volume 3 Issue SI1
we try to fill in the gap caused by the absence of a regulation for
SHS durability, by developing a standard protocol, which can
serve to this aim. The goal of this research is to define a protocol
for durability assessment, which may also serve as a basis for the
identification of a standard for evaluation of SHS durability. The
protocol allows both for defining a global figure of merit and ranking
for different SHS and for identifying those surfaces that fulfill a set
of durability requirements for a specific application. The idea is to
perform different tests, to evaluate the resistance of the surface in
various environments and to provide a ranking when comparing
different SHS. All tests have been designed on the basis of simple
procedures that can be easily available in research laboratories,
to obviate to the time- and cost-consuming use machineries, for
example, those suggested by the ASTM standards.47,48 In addition,
all the tests can be performed in a reduced time frame (few working
days while evaluating many samples at the same time); as such,
the protocol can be used as facile and standard procedure by
laboratories, companies and other users.
2. Durability test protocols
To monitor surface superhydrophobicity, we measure the values
of advancing and receding contact angles. The contact angle,
θ, is measured automatically from drop images by measuring
the tangent of a circle fitting the drop profile in the vicinity of
the contact point, as shown in Figure 2. Typical drop volume of
analysed drops was ~10 µl. To measure the contact angle, the drop
profile in the vicinity of the contact line is extracted and fitted
with a circle; the contact angle is computed from the slope of the
tangent to the circle.49,50
The durability protocol consists of nine tests, and for each test, five
cycles are performed. For each test, five identical fresh samples
are used, and these five surfaces are tested throughout the five
successive cycles. The suggested test frequencies and/or times are
setting as proposal for a general norm. These tests frequencies and
procedure times allow in fact distinguishing the ageing of many
kinds of SHS. In the present work, we address the absence of a
standard for the evaluation of SHS durability, which appears to
Figure 2. Local fitting of the profile of the drop with the
mathematical expression of the circumference
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Assessing durability of superhydrophobic
surfaces
Malavasi, Bernagozzi, Antonini and Marengo
be the most critical issue for all the applications; the proposed
test timings and repetitions need to be further improved by an
international standardisation process.
Before and after each test cycle, contact angle measurements are
performed to assess the eventual decrease of superhydrophobicity.
Differences in the receding contact angle and in the hysteresis between
two successive cycles correspond to a change of the surface behavior.
In other words, when there is a reduction in the receding contact
angle and/or an increase of hysteresis, so that receding contact angles
becomes lower than 135° and/or hysteresis becomes higher than 10°,
it means the surface loses its superhydrophobicity. The contact angle
test is nondestructive and thus can be used to control and evaluate the
evolution of surface wettability between two test cycles.
2.1 Stability in water
The first test aims at evaluating the resistance of the sample to water
immersion. The sample is dipped in deionised water at a pH of 7, at
room temperature (20°C), for 5 h and then dried in air. Air ambient
conditions were: temperature of 20°C and humidity between 20
and 40%. The contact angle measurements were performed within
few hours from the test.
Water immersion test is useful for evaluating the resistance
to prolonged water exposure. Tests were conducted at room
temperature to avoid the combination of multiple effects (e.g.
exposure to water and heat effects).
2.2 Stability in acidic environment
The second test evaluates the resistance of the sample to acidic
environment. This is recreated in laboratory with a solution of
hydrochloric acid in water, to have a pH of 6 (1 ml of acid at 37%
diluted at 200 ml). The sample is immersed in the solution for 2 h,
then rinsed till neutrality with pure water and finally dried in air. A
pH value equal to 6 is chosen, since this is the pH of the common
rain. Hydrochloric acid is chosen because it is a strong monoprotic
acid, of common use in any research laboratory, and it does not cause
oxidation.
2.3 Stability in alkali environment
The third test determines the resistance of the sample to alkali
environment, that is recreated in laboratory with a solution of sodium
hydroxide in water, to have a pH of 8·5 (1 ml of a 0·1 M NaOH
solution, diluted at 200 ml); the pH of 8·5 is the maximum pH found
in seawater. The sample is immersed in the solution for 2 h, then rinsed
till neutrality with pure water and dried in air. Sodium hydroxide is a
strong alkali of common use in any research laboratory.
2.4 Stability in ionic solutions
The fourth test is designed to test sample resistance in ionic
environment, consisting of a sodium chloride water solution,
3·5% in weight. This concentration is chosen since it corresponds
 Surface Innovations Assessing durability of superhydrophobic
Volume 3 Issue SI1 surfaces
Malavasi, Bernagozzi, Antonini and Marengo

to average sea salt concentration. Water pH is measured equal
to 7, to avoid combined effect of salt and pH. The sample is
immersed in the solution for 2 h, then rinsed till neutrality with
pure water and dried in air. The cycle is repeated five times, as
for the other tests.
2.5 Stability in organic solvents
Supplementary tests are used to evaluate the behavior of the
surfaces in organic environment. The surfaces are tested in two
different kind of solvents, in order to observe the effect of slightly
polar organic solvent (ethylic alcohol) and of a completely apolar
solvent (toluene).
2.5.1 Alcohol immersion
This cycle deals with immersing the samples in ethanol for 30 min
at room temperature, without any stirring. Sigma-Aldrich (St.
Louis, MO) ethanol (absolute alcohol, ≥99·8%) is used.
2.5.2 Hydrocarbon immersion
This cycle deals with immersing the samples in toluene for 30 min,
at room temperature, without any stirring. Sigma-Aldrich toluene
is 352 nm and the density of the exposition dose of irradiation has a
maximum value of ~50 J/cm2.
UV radiation is chosen since this can be potentially harmful for
material; this wavelength is chosen as close as possible to the
common external UV irradiation. Toshiba BLB (Black Light Blue)
lamps (code FL8BLB) and RAYONET photochemical reactor are
used.
3. Taking the durability protocol to test
Despite a plethora of methods have been developed to fabricate
SHS, including fluorosilanes,51,52 silicone silanes,53,54 thiols,55,56
thin polymer layers57,58 and chemical vapor deposition,59,60
to name a few, not all methods can offer the same durability
performances. As a general observation, methods in which
chemical bonding between the functional materials (molecule,
polymer, etc.) and the substrate is achieved, rather than a mere
material deposition on the substrate, have a higher potential in
Etching Grafting
Etched AI

anhydrous 99·8% is used.

AI

2.6 Mechanical integrity Rinsed Rinsed

with with
This test evaluates the SHS resistance to mechanical erosion, pure ethanol
1 l ethanol
caused by a water jet. An air assisted AirMist Lechler nozzle, series HCI at
37%
water
and 100 g
and
and of dried in
136.141.16.11, is used. The sample is placed under a jet of liquid diluted
1:2
dried CH3(CH2)10 air
in air
and air at the distance of 300 mm. Water flow rate of 34·9 l/h with a COOH
Immersion Immersion
relative input nozzle air pressure of 1 bar and a relative input nozzle 2 min 2h
liquid pressure of 0·7 bar. The test is composed of five cycles, with
each cycle lasting 30 s.
Figure 3. Schematic representation of the surfaces fabrication process

Note that multiple tests have been used and developed in the
literature to assess surface durability (such as refs. 34 and 35).
Number of
Here, the abrasion tests by means of sprayed water was used since
Average cycles for
this is a simple test, easily reproducible, with no need for specific
Test type cycles: n each test
equipment to be set up in a common laboratory. In addition, the test
can also be representative of realistic conditions, where surfaces Water immersion 5 5
are exposed to water spray impacts. Acidic environment 4 5
Alkali environment 2·4 5
2.7 Heat resistance Ionic solution 4·6 5
Each round of this test consists of putting the samples in an oven, at Mechanical erosion 1·6 5
100°C, for 2 h, and cooling the samples down to room temperature Heating 5 5
by natural heat exchange with the environment. This test is used
UV resistance 4·6 5
to measure the sample resistance to prolonged thermal stress.
The oven temperature is chosen as it corresponds to water boiling Alcohol immersion 4·6 5
temperature at atmospheric pressure. Hydrocarbon 5 5
immersion

2.8 UV light resistance Total score X = 37·2 Y = 45

The cycle consists in UV irradiation for 16 h, to evaluate the Table 1. Overview of results from protocol tests
damages caused to the surface by UV radiation; peak wavelength

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 Surface Innovations Assessing durability of superhydrophobic
Volume 3 Issue SI1 surfaces
Malavasi, Bernagozzi, Antonini and Marengo

t: h t: h
170 20
5 10 15 20 25 5 10 15 20 25 Sample 1

160 15
Sample 2

∆θ: degree
θR: degree

150 10
Sample 3

140 5
Sample 4
130 0
0 1 0 1 Sample 5
2 3 4 5 2 3 4 5
Cycles, n Cycles, n
(a) (b)

Figure 4. (a) Evolution of receding contact angle against cycles during

water immersion. (b) Evolution of contact angle hysteresis against
cycles during water immersion

t: h t: h
170 20
2 4 6 8 10 2 4 6 8 10 Sample 1

160 15
Sample 2
∆θ: degree
θR: degree

150 10
Sample 3

140 5
Sample 4
0
130
0 1 2 3 4 5 Sample 5
0 1 2 3 4 5
Cycles, n Cycles, n

(a) (b)

Figure 5. (a) Evolution of receding contact angle against cycles as a

result of acid environment. (b) Evolution of hysteresis against cycles as
a result of acid environment

terms of durability. This is one of the main reason why, for the
present paper, we tested fatty acid molecules that are grafted
on the substrate through a two-step wet chemistry approach:
aluminum samples are first etched in hydrochloric acid and then
functionalised by lauric acid (LAU) molecules. Another critical
point is the capability of the hydrophobic material to act as a
barrier layer, for example, to protect the aluminum substrate
from any chemical attack.
The present protocol has been mainly developed for SHS on
hard substrates. Although a test suitable for a metal may not be
a suitable protocol for durability of water-repellent textile, the
majority of tests, such as UV exposure, chemical stability in
acid and alkaline environments, can be potentially used to tests
durability of superhydrophobic textiles, as well. The protocol
for textiles could nonetheless be adapted to introduce specific
requirements. The main reason for defining in the present
work a protocol for SHS on aluminum substrates was driven
by the widespread use of metals in many industrial sectors and
applications.
3.1 SHS preparation
Durability tests were performed on SHS prepared using a
two-step wet chemistry approach on aluminum samples: the
samples are first etched, to enhance surface roughness, and then
functionalised by grafting of fatty acid molecules to impart
hydrophobicity. The use of fatty acid molecules is favourable
due to their reduced cost compared to fluorinated molecules
and has been used in the past, for example, by Sirong et al.61
for hydrophobic functionalisation of steel with myristic acid
(CH3(CH2)12COOH). Aluminum alloy plates (Al 1015), with a
thickness of 0·6 mm and typical dimensions of 30 × 60 mm, are

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 Surface Innovations Assessing durability of superhydrophobic
Volume 3 Issue SI1 surfaces
Malavasi, Bernagozzi, Antonini and Marengo

t: h t: h
170 20 Sample 1
2 4 6 8 10 2 4 6 8 10

160 15 Sample 2

∆θ: degree
θR: degree

150 10 Sample 3

140 5 Sample 4

130 0 Sample 5
0 1 2 3 4 5 0 1 2 3 4 5
Cycles, n Cycles, n
(a) (b)

Figure 6. (a) Evolution of receding contact angle against cycles as a

result of alkali environment. (b) Evolution of hysteresis versus cycles as
a result of alkali environment

t: h t: h
170 20 Sample 1
2 4 6 8 10 2 4 6 8 10

160 15 Sample 2
θR: degree

∆θ: degree

150 10 Sample 3

140 5 Sample 4

130 0 Sample 5
0 1 2 3 4 5 0 1 2 3 4 5
Cycles, n Cycles, n
(a) (b)

Figure 7. (a) Evolution of receding contact angle against cycles as a

result of ionic solution. (b) Evolution of hysteresis against cycles as a
result of ionic solution

purchased from Agnelli Metalli (Lallio Bergamo, Italy). Samples
are initially etched with hydrochloric acid at 37% (Sigma-
Aldrich) diluted 1:2 v/v with water. The samples are inserted in
the acid solution, at room temperature, for 2 min and then rinsed
with pure water and dried in air. Subsequently, the samples are
immersed in an ethanol and LAU (CH3(CH2)10COOH) solution
at room temperature, where LAU concentration is 12·7% by
weight, with respect to ethanol concentration (i.e. 1 litre of
ethanol and 100 g of LAU). Sigma-Aldrich ethanol ≥ 98% and
Sigma-Aldrich LAU ≥ 98% are used. The samples are inserted
into the solution for 2 h to allow LAU molecules grafting on the
substrate, then rinsed with ethanol and dried in air. A schematic
representation of the surfaces fabrication process is shown in
Figure 3. At the end of the second step, the advancing contact
angle of these surfaces is typically 157° ± 2°, the receding
contact angle is 155° ± 2° and the hysteresis is ~ 2° ± 4°.
The process is facile and can be used to functionalise several
aluminum samples in sequence, using the same reaction batch.
In addition, the process can be easily scaled up to large area
treatments, which is an important factor in view of industrial
applications; moreover, it is a low-cost process compared to
other approaches, based on the use of fluorinated molecules.
3.2 Results and discussion
To provide a global index of durability for the surface, results
collected from all tests are inserted in a table (Table 1). Figures
reporting results illustrate the receding contact angle and contact
angle hysteresis for each sequential cycle and for every sample.
In each graph, the thresholds of both receding contact angles (at
135°, on the left) and hysteresis (at 10°, on the right) are also shown
as dotted lines as a guide. To improve the figure readability, the
standard deviation is provided only if greater than 5°. The standard
deviation of the receding contact angle is sufficient to permit an
assessment of the sample degradation degree.

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 Surface Innovations Assessing durability of superhydrophobic
Volume 3 Issue SI1 surfaces
Malavasi, Bernagozzi, Antonini and Marengo

t: s t: s
170 20 Sample 1
30 60 90 120 150 30 60 90 120 150

160 15 Sample 2

∆θ: degree
θR: degree

150 10 Sample 3

140 5 Sample 4

130 0 Sample 5
0 1 2 3 4 5 0 1 2 3 4 5
Cycles, n Cycles, n
(a) (b)

Figure 8. (a) Evolution of receding contact angle against cycles as a

result of mechanical erosion. (b) Evolution of hysteresis against cycles
as a result of mechanical erosion

t: h t: h
170 20 Sample 1
2 4 6 8 10 2 4 6 8 10
160 15 Sample 2
θR: degree

∆θ: degree

150 10
Sample 3

140 5
Sample 4

130 0
Sample 5
0 1 2 3 4 5 0 1 2 3 4 5
Cycles, n Cycles, n
(a) (b)

Figure 9. (a) Evolution of receding contact angle against cycles as a

result of heating test. (b) Evolution of hysteresis against cycles as a
result of heating test

As a general observation, the advancing contact angle is less sensitive
to superhydrophobicity degradation, whereas receding contact angle
can be strongly affected, causing an increase of hysteresis and thus of
drop adhesion.37 This confirms that receding and hysteresis are better
parameters to evaluate surface wettability rather than advancing
contact angle. See Supplementary Data for an example.
Results from water immersion tests are illustrated in Figure 4.
From beginning to end of tests, θR remains, for all tested samples,
well above the threshold of 135°. Also, contact angle hysteresis
remains very low, well below the threshold (10°). As such, it can be
concluded that all five samples maintain superhydrophobicity for
the entire duration of the test.
environment test, four samples resist to all cycles and are still
superhydrophobic.
The results of the alkali environment test are illustrated in
Figure 6. At the end of the five cycles, only two samples remain
superhydrophobic. The other samples lose the characteristics of
SHS, showing the deterioration due to the stress after the tests in
alkali environment.
In Figure 7, the results for the ionic solution test are illustrated.
At the end of the five cycles, four surfaces show resistance to
this test. Sample 1 loses the characteristics of SHS, showing the
deterioration due to the stress after the tests in ionic environment.

Observing Figure 5 and considering the systematic errors due to Organic solvents test results are shown in Figures 8 and 9. It can be
the data acquisition system and the average standard deviation asserted that four samples resist to the alcohol test and that all the
of the receding contact angle, we can assert that for the acid samples resist to the hydrocarbon test.

56

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 Surface Innovations Assessing durability of superhydrophobic
Volume 3 Issue SI1 surfaces
Malavasi, Bernagozzi, Antonini and Marengo

t: h t: h
170 20 Sample 1
16 32 48 64 80 16 32 48 64 80
160 15 Sample 2
θR: degree

∆θ: degree
150 10 Sample 3

140 5 Sample 4

0
130 Sample 5
0 1 2 3 4 5
0 1 2 3 4 5
Cycles, n Cycles, n
(a) (b)

Figure 10. (a) Evolution of receding contact angle against cycles as a

result of ultraviolet test. (b) Evolution of hysteresis against cycles as a
result of ultraviolet test

t: h
170 t: h
20 Sample 1
30 60 90 120 150
30 60 90 120 150
160 Sample 2
15
∆θ: degree
θR: degree

150 10 Sample 3

140 5 Sample 4

130 0 Sample 5
0 1 2 3 4 5 0 1 2 3 4 5
Cycles, n Cycles, n
(a) (b)

Figure 11. (a) Evolution of receding contact angle against cycles as

a result of alcohol test. (b) Evolution of hysteresis against cycles as a
result of alcohol test

In Figure 10, the mechanical erosion test results are reported. Only
one sample resists to five cycles, that is, only one sample is still
superhydrophobic at the end of the fifth cycle.
In Figure 11, the heating test results are illustrated. The receding
contact angles are all higher than 135°, and the hysteresis is
always lower than 10°. All the samples resist to all cycles of the
heating test.
UV test results are shown in Figure 12. Sample 5 is not
superhydrophobic anymore at the end of the third cycle. At the
end of the five cycles, the number of surfaces that resist to this
test is four.
A global overview of test results is given in Table 1, which reports
the average number of cycles before samples showed super-
hydrophobicity degradation. A global assessment of the behavior of
the examined samples is provided by the summation of the average
numbers of cycles over all performed tests. In case of the tested SHS
is 37·2/45: by looking at Table 1 in details, one can notice that this
overall good result is obtained thanks to a good chemical stability
of the samples in different environments, whereas mechanical
resistance is a weak point on which improvement would be needed.
This approach allows thus a general evaluation of the behavior of
the surfaces and can be used to provide a durability ranking between
different surfaces.
4. Conclusions
In the present paper, a durability protocol is presented to test the
robustness and durability of different SHS. Purpose of the protocol
is to assess the durability of various SHS and to provide a figure of
merit to allow comparing different types of SHS. Nine tests have
been included in the protocol: water immersion, acidic environment,
alkali environment, ionic solution, mechanical erosion, heating,

57

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 Surface Innovations
Volume 3 Issue SI1
t: min
170
30 60 90 120 150
160
∆θ: degree
θR: degree
150
140
130
0 1 2 3 4 5
Cycles, n
(a)
Figure 12. (a) Evolution of receding contact angle against cycles as a
result of hydrocarbon test. (b) Evolution of hysteresis against cycles as
a result of hydrocarbon test
UV resistance, alcohol immersion, and hydrocarbon immersion.
For each test, five identical fresh samples are tested throughout
five consecutive cycles to monitor drop wettability and quantify
the eventual loss of superhydrophobicity. Variation in the receding
contact angle and in the hysteresis between two successive cycles
corresponds to a change of the surface behavior. In particular,
decrease of receding contact angle below 135° and an increase of
contact angle hysteresis above 10° were used to mark the surface
as non-superhydrophobic. For each test, the average number of
cycles that the surface can resist before degrading is evaluated in
a systematic way. On the basis of test results, a global figure of
merit is given for providing a general rating of the surface. As a
representative case, the protocol is used in the present study to
test the durability of specifically developed SHS, prepared using
aluminum as substrate and using a two-step wet chemistry approach,
where the aluminum samples are first etched in hydrochloric acid
and then functionalised by LAU molecules. In our study, the global
assessment of the behavior is 37·2/45, an overall good remark given
by the general good chemical stability of the surface, with some
weakness in the mechanical robustness of the surface. Although the
protocol is not exhaustive, specific additional tests can be extended
and tailored for testing durability of surfaces aimed at specific
applications. To conclude, we believe that the systematic approach
used here allows a general assessment of SHS durability and can
serve as the basis for the definition of a standard, which would
allow a comparative ranking between different kinds of SHS from
laboratory investigation to the industrial level.
Acknowledgements
This work is supported by Accordo Quadro - Regione Lombardia
through the project “Strumenti innovativi per il progetto di sistemi
antighiaccio per l’aeronautica” and partially by the European
Cooperation in Science and Technology - MPNS COST Action
MP1106 “Smart and green interfaces - from single bubbles and
58
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Assessing durability of superhydrophobic
surfaces
Malavasi, Bernagozzi, Antonini and Marengo
t: min
20
30 60 90 120 150 Sample 1
15
Sample 2
10
Sample 3
5
Sample 4
0 Sample 5
0 1 2 3 4 5
Cycles, n
(b)
drops to industrial, environmental and biomedical applications”
led by Prof. T. Karapantsios. The authors would also like to thank
Carlotta Ghitti for the help in data analysis and contact angle
measurement. C.A. acknowledges funding by a Marie Curie
Intra-European Fellowship within the 7th European Community
Framework Programme (ICE2, 301174).
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