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Journal of the Taiwan Institute of Chemical Engineers

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

A waterproofing textile with robust superhydrophobicity in either air

or oil surroundings
Xiaotao Zhu a,∗, Zhaozhu Zhang b, Yuanming Song a,∗, Jingyong Yan a, Yuyan Wang a,
Guina Ren a,∗
a
School of Environmental and Material Engineering, Yantai University, Yantai 264405, China
b
State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China

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

Article history: Manmade superhydrophobic textiles are mechanically weak, and the current methods to solve this prob-
Received 7 July 2016 lem are usually laborious and cost ineffective. Herein, to address this challenge, we created a robust su-
Revised 10 November 2016
perhydrophobic textile by a one step immersion process that benefited of simplicity and cost efficiency.
Accepted 23 November 2016
The resulting textile remained its superhydrophobicity after finger pressing, knife scratching, twisting
Available online xxx
by hands, and even 10 cycles of abrasion with sandpaper. We also studied the wetting behavior of the
Keywords: resulting superhydrophobic textile when exposed to oily environments. The results showed that the ob-
Superhydrophobic tained textile still displayed superhydrophobic when immersed in oil surrounding, and it kept its water
Oil–water separation repellency even after being contaminated by oil. Moreover, exploiting its superhydrophobicity and super-
Waterproofing oleophilicity, the obtained textile was demonstrated as the separation membrane and oil absorption to
Textiles separate oil from oil–water mixtures efficiently.
Robust
© 2016 Taiwan Institute of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
Mechanical durability

1. Introduction
Surfaces that display contact angles greater than 150° along
with a low contact angle hysteresis for water droplets are known
as superhydrophobic surfaces. On such superhydrophobic surfaces,
water droplets bead up and roll off readily, removing dirt parti-
cles in their path [1–3]. In view of the significant potential of such
surfaces for numerous scientific and industrial applications, many
strategies have been developed to create superhydrophobic sur-
faces till now [4–10]. Among them, the waterproofing of textiles is
considered to be among the primary potential applications for the
superhydrophobic effect. Textiles with superhydrophobic property
would prevent the textiles being wetted even upon full immersion
in water, and thus they could find wide applications as water resis-
tant apparel, self-cleaning textiles, and stain-free clothing [11–13].
However, one big drawback of these manmade superhydrophobic
textiles is that they will lose their self-cleaning property readily
when exposed to physical forces such as abrasion and twisting.
Such critical weakness of superhydrophobic textiles severely hin-
dered their practical utility [14,15]. To solve this problem, differ-
ent strategies including γ -ray induced graft polymerization [16],
in situ growth of silicone nanofilament coating [17,18], the graft-
∗
Corresponding authors.
E-mail addresses: xiaotao.zhu@ytu.edu.cn (X. Zhu), ytusym@126.com (Y. Song),
rgnlicp@126.com (G. Ren).
ing of polyacrylic acid [19], and the direct incorporation of fluori-
nated compound [20,21] have been proposed recently to improve
the mechanical robustness of superhydrophobic textiles. However,
some of the above techniques like γ -ray induced graft polymer-
ization are either time-consuming or laborious [16], while others
require special materials such as fluoro compounds, which are ex-
pensive and environmental unfriendly [20,21]. Thus, additional re-
search is needed to explore a facile, economical, and green strategy
for producing of durable superhydrophobic textiles.
Besides mechanical durability, the wetting behavior of the su-
perhydrophobic textiles when exposed to oil should also be consid-
ered. Till now, the wetting performance of the superhydrophobic
textiles in oil surroundings has not been evaluated, despite the ex-
tensive evaluation of wetting properties of superhydrophobic tex-
tiles in air. Also only few reports have shown water repellency
test of the superhydrophobic textiles upon oil contaminations in
air. Thus, to extend the applications of superhydrophobic textiles,
characterization of these tests is necessary, and it would be highly
desirable that the superhydrophobic textiles can still display wa-
ter repellency and self-cleaning property when contaminated by
oil and even upon immersion in oil.
In this study, we developed a facile, one step immersion ap-
proach to produce a superhydrophobic textile that possessed me-
chanical durability and can still function even when exposed
to oil. The whole process was facile to carry out and did
not require special materials. The resulting textile can keep its

http://dx.doi.org/10.1016/j.jtice.2016.11.029
1876-1070/© 2016 Taiwan Institute of Chemical Engineers. Published by Elsevier B.V. All rights reserved.

Please cite this article as: X. Zhu et al., A waterproofing textile with robust superhydrophobicity in either air or oil surroundings, Journal
of the Taiwan Institute of Chemical Engineers (2016), http://dx.doi.org/10.1016/j.jtice.2016.11.029
JID: JTICE
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2 X. Zhu et al. / Journal of the Taiwan Institute of Chemical Engineers 000 (2016) 1–5

Fig. 1. FESEM images of the polyester fibers before (A) and after (B) coating with H-SiO2 –PFW.

superhydrophobic property after knife scratching, twisting by

hands, finger pressing, and even 10 abrasion cycles with sandpa-
per. Moreover, the superhydrophobic property of the textile can
be regenerated by an easy repair process when loss of superhy-
drophobicity occurred. The wetting behavior of the resulting su-
perhydrophobic textile when exposed to oil was evaluated. It was
found that the obtained textile still displayed superhydrophobic
upon emersion in oil and kept its water repellency when fouled
by oil. We also demonstrated that the superhydrophobic textile can
be used as the separation membrane and oil absorption to separate
oil from oil–water mixtures efficiently.
Fig. 2. (A) and (B) Water droplets can easily wet the native polyester fabric surface,
displaying 0° contact angle on it; (C) and (D) water droplets with spherical shape
2. Experimental display very high contact angles on the superhydrophobic textile. (E) A bright plas-
tron layer is visible when the polyester fabric is submerged in water. The water was
2.1. Materials dyed with methylene blue to aid visualization.

SiO2 nanoparticle (average diameter ∼20 nm) was purchased

from Zhoushan Nanomaterials Co., China. Octadecyltrichlorosilane
was provided by Shanghai Boer Chemical Reagent Co., Ltd., China.
Polyfluorowax (PFW, diameter < 15 μm) was provided by Micro
Power Inc., USA. Commercially available polyester fabric was pur-
chased from a local store and cleaned with acetone and deionized
water sequentially in an ultrasonic cleaner before use. Other chem-
icals were analytical grade reagents and used as received.
2.2. Fabrication of hydrophobic SiO2 particles
0.5 g SiO2 was ultrasonically dispersed in 20 ml toluene, and
0.5 ml octadecyltrichlorosilane was added dropwise under stirring
at ambient temperature. The reaction mixture was stirred at ambi-
ent temperature for 12 h. Finally, the resultant suspension was cen-
trifugation and then placed to dry in an oven for 30 min at 80°C.
3. Results and discussion
3.1. FESEM analysis
The polyester fabric was coated with the mixture of hy-
drophobic silica dioxide and polyfluorowax (hence denoted as H-
SiO2 –PFW) under ambient conditions, to achieve superhydropho-
bic property. Fig. 1 exemplarily shows scanning electron mi-
croscopy images of the textile before and after coating. As shown
in Fig. 1(A), the native polyester fabric presents a highly textured
microscale fiber with a typically smooth surface. After coating, a
rough H-SiO2 –PFW layer is covered on each microscale fibers, as
shown in Fig. 1(B). The textile after coating generates a dual sur-
face texture that resembles the surface morphology of a lotus leaf,
and thus it provides the needed texture to enable the formation of
superhydrophobic surfaces, based on the recent investigation [22].

3.2. Surface wettability of the superhydrophobic textile when exposed

2.3. Fabrication of superhydrophobic textile
0.2 g hydrophobic SiO2 and 0.05 g PFW were dispersed in 20 ml
toluene under stirring at ambient temperature. Polyester fabric was
immersed in this suspension for 1 min and then was placed to dry
in an oven for 30 min at 130°C.
2.4. Characterization
Contact angle (CA) and sliding angle (SA) measurements were
performed on a KRÜSS DSA 100 (KRÜSS Company, Ltd., Germany)
apparatus at ambient temperature. The volume of water and oil
droplet in each measurement was 5 μl. Scanning electron mi-
croscopy measurements were carried out by a JSM-6701F field-
emission scanning electron microscopy (FESEM, JEOL, Japan).
to air
As shown in Fig. 2(A) and (B), the native textile was wetted
by water droplets readily and displayed superhydrophilic with ap-
parent contact angle of 0° for water droplets. After coating with
H-SiO2 –PFW, the textile turned to be superhydrophobic. Water
droplets with spherical shape appeared to float on the coated tex-
tile surface and showed high apparent contact angle (157°) on it
(see Fig. 2(C) and (D)). Moreover, water droplet can roll off the su-
perhydrophobic textile easily at a small titling angle (5°) without
leaving a trace.
When the resulting superhydrophobic textile was immersed in
the water bath, a plastron (air pockets) layer that was indicative
of a robust Cassie–Baxter state was formed (see Fig. 2(E)) [23].
The plastron layer was stable and remained unchanged even upon

Please cite this article as: X. Zhu et al., A waterproofing textile with robust superhydrophobicity in either air or oil surroundings, Journal
of the Taiwan Institute of Chemical Engineers (2016), http://dx.doi.org/10.1016/j.jtice.2016.11.029
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X. Zhu et al. / Journal of the Taiwan Institute of Chemical Engineers 000 (2016) 1–5
Fig. 3. Wetting tests when exposed to oil. (A) Water droplets were repelled by the
resulting textile when immersed in silicon oil; (B) water droplet displayed spherical
shape with a contact angle of 163° on the textile immersed in oil; (C) water droplet
can wet the original textile immersed in oil completely; (D) the obtained textile
retained its water-repellent property even after being contaminated by silicon oil,
and water droplet can slide on the silicon oil contaminated textile surface easily.
The sample supported on a glass slide was tilted at 10°.
extending the periods of immersion time. After 1 day of full im-
mersion, the textile surface was completely dry to touch and still
displayed superhydrophobic property with contact angle of 157°
for water droplets. Additionally, the surface texture of the obtained
textile did not exhibit observable changes after the immersion test.
These results indicated that the resulting textile was able to ef-
fectively retain its superhydrophobic property underwater for ex-
tended periods of time.
3.3. Surface wettability of the superhydrophobic textile when exposed
to oil
We next studied the wetting behavior of the resulting super-
hydrophobic textile when exposed to oil. When immersed in sil-
icon oil, water droplets (colored with methylene blue) displayed
a sphere shape at the oil–solid interface without wetting the re-
sulting textile (see Fig. 3(A)), and they can slide off the textile
surface readily. The contact angle value of water droplets placed
on the resulting textile that was immersed in silicon oil is 163°,
as shown in Fig. 3(B). These results meant that the resulting tex-
tile still displayed superhydrophobic property even upon being im-
mersed in oil. However, water droplet spread and wet the native
textile surface completely, leading to the contact angle of 0°, as
shown in Fig. 3(C). When the resulting superhydrophobic textile
was immersed in silicon oil, silicon oil gradually penetrated into
the textile, and thus the water droplets were supported by both
oil and the surface structures. In this condition, the wetting be-
havior under oil is similar to that in air [24,25]. For these reasons,
the resulting superhydrophobic textile retained its water repellency
when immersed in oil.
We further investigated the wetting behavior of the resulting
superhydrophobic textile after being contaminated by oil. Actually,
the resulting textile can be wetted and thus contaminated by oil
liquids with much lower surface tension than water (such as sili-
con oil) easily, due to its superoleophilicity; however, the oil con-
taminated textile still preserved its water repellency. As shown in
Fig. 3(D), water droplet slipped off from the superhydrophobic tex-
tile that was fully contaminated by silicon oil readily, with the slid-
ing speed of about 1.17 cm/s. On the contrary, Water droplet pinned
on the original textile contaminated by silicon oil and permeated
into the textile eventually, as shown in Fig. S3. When the silicon
oil penetrated into the textile, it covered the surface texture and
formed an oil layer on the surface, which can serves as lubricating
film to repel water [26]. Thus, a slipper state was achieved on this
oil contaminated textile.
Please cite this article as: X. Zhu et al., A waterproofing textile with robust superhydrophobicity in either air or oil surroundings, Journal
of the Taiwan Institute of Chemical Engineers (2016), http://dx.doi.org/10.1016/j.jtice.2016.11.029
[m5G;December 1, 2016;13:10]
3
Fig. 4. Relevant manual tests for evaluating the robustness of the superhydrophobic
textile, including finger pressing, knife scratching, and twisting by hands (A1), (B1),
and (C1); the textile can keep its self-cleaning property after the relevant tests (A2),
(B2), and (C2).
3.4. Mechanical robustness of the superhydrophobic textile
The mechanical durability of superhydrophobic surfaces is cru-
cial for their use in practical applications [15]. Here, the mechani-
cal robustness of the resulting superhydrophobic textile was firstly
assessed by finger pressing. For superhydrophobic surfaces, the
force exerted by touching would damage their fragile surface tex-
tures, and finger contact could also cause salt and oil contamina-
tions to them. Both processes can make the superhydrophobic sur-
faces lose their self-cleaning property. However, our created tex-
tile remained superhydrophobic after being pressed with a finger
(see Fig. 4(A1) and (A2)). Water droplets still maintained a spheri-
cal shape on the touched surface with the apparent contact angle
more than 150°. Moreover, water droplets can roll off the touched
textile surface at a small titling readily. Similar water repellency
behaviors were also observed after other qualitative tests includ-
ing knife scratching and twisting by hands, as shown in Fig. 4(B)
and (C).
We next conducted linear abrasion test to fully study the me-
chanical durability of the superhydrophobic textile. The methodol-
ogy of the linear abrasion test was illustrated in Fig. S3. Sandpaper
(1500 mesh) served as the abradant, with the superhydrophobic
textile weighting 80 g to be tested facing this abrasion material.
The superhydrophobic textile was dragged in one direction with
the speed and abrasion length of 3 cm/s and 10 cm, respectively.
The water contact angles and sliding angles after each abrasion test
were shown in Fig. 5. It was observed that CAs for water droplets
placed on the fabric surface varied from 157° in the initial state
to 152° after 10 cycles of abrasion, whereas the corresponding SA
ranged from 5° to 19°. These results indicated that our created su-
perhydrophobic textile possessed mechanical durability.
3.5. Easy reparability of the superhydrophobic textile
The resulting textile lost its superhydrophobic property after a
long abrasion, leading to much lower CAs with water droplets (see
Fig. 6(A)). However, as the fabrication approach is facile to carry
out, it provides an opportunity to construct a regenerative super-
hydrophobic surface. After repeating the dip coating process, the
damaged textile was rendered with superhydrophobicity again, al-
lowing the textile to display high CAs with water droplets placed
on at any location on it (Fig. 6(B)). Moreover, the regenerative tex-
tile also exhibited robust superhydrophobicity evidenced by the
above mentioned manual tests as well as linear abrasion test.
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4 X. Zhu et al. / Journal of the Taiwan Institute of Chemical Engineers 000 (2016) 1–5
Fig. 5. The value of CA and SA as a function of the number of abrasion cycles for
the obtained superhydrophobic textile.
Fig. 6. Photographs of water droplets (dyed with methylene blue) on the damaged
textile surface (A) and repaired textile surface (B).
Fig. 7. The superhydrophobic textile used for oil–water separation. Hexadecane
droplets (colored with oil red) easily pass through the membrane, whereas water
droplets (dyed with methylene blue) bead up on the surface.
3.6. Superhydrophobic textile for the separation of oil–water mixtures
Removing organic contaminants and oil spills from oil–water
mixtures has recently generated immense commercial and aca-
demic interest due to the increasing amount of industrial oily
wastewater, as well as the frequent oil spill accidents [27–31].
The resulting textile was both superhydrophobicity and super-
oleophilicity, which enabled it to be a good ideal for separation
oils from mixtures of oil liquids and water. The oil–water separa-
tion experiment was firstly performed using the textile as a sepa-
ration membrane, as shown in Fig. 7. When the mixture of 0.05 M
Please cite this article as: X. Zhu et al., A waterproofing textile with robust superhydrophobicity in either air or oil surroundings, Journal
of the Taiwan Institute of Chemical Engineers (2016), http://dx.doi.org/10.1016/j.jtice.2016.11.029
[m5G;December 1, 2016;13:10]
Fig. 8. Removal of oils with density lower (hexadecane) and higher (chloroform)
than water from oil–water mixtures using the superhydrophobic textile. For easy
observation, the oils, namely hexadecane (A) and chloroform (B), were dyed with
oil red.
AgNO3 aqueous solution and hexadecane was poured onto the re-
sulting superhydrophobic textile suspended over a beaker, hexade-
cane passed through the beaker underneath whereas the water
droplets remained on the top surface. As a result, oil–water sep-
aration was easily achieved.
It is well known that that Ag+ is very sensitive to Cl− . Even if a
tiny amount of Ag+ was contact with the Cl− , a white precipitate
would be generated. It was found that no white precipitate was
observed, when NaCl aqueous solution (0.1 M) was poured into the
beaker containing hexadecane, indicating the high oil–water sep-
aration efficiency of the textile. Furthermore, the obtained textile
can keep its enhanced separation efficiency even after ten cycles
of oil–water separation.
In addition to serving as the separation membrane, the result-
ing superhydrophobic textile can also be used as an oil absorbent
to absorb oil selectively from oil–water mixtures. When brought
into contact with a hexadecane film spreading on a water surface,
the superhydrophobic textile can absorb the hexadecane selectively
and completely within a few seconds, as shown in Fig. 8(A). More-
over, the resulting textile can be used to absorb heavy oils such as
chloroform under water. As shown in Fig. 8(B), when immersed in
water to contact with the chloroform droplet, the resulting textile
can absorb the chloroform from water completely and rapidly, and
the chloroform absorbed can be taken out of water with the tex-
tile. Importantly, the absorbed oils were collected easily by squeez-
ing the textile, and the residual oil can be extracted by immersing
the oil-soaked textile into acetone or other organic solvents. In this
way, the superhydrophobic textile was reused to absorb oil liquids
once more.
Other types of oil compounds such as motor oil, rapeseed oil,
and silicone oil can also be absorbed selectively from oil–water
mixtures by the same process. Moreover, the oil absorption capac-
ity of the superhydrophobic textile differed slightly even after 10
cycles of oil absorption (see Fig. S5), demonstrating the stability
of this oil absorbent material. Thus, our created superhydrophobic
textile is a good candidate in industrial oil-polluted water treat-
ment and oil spill cleanup.
4. Conclusions
A superhydrophobic textile was produced by modifying the
native textile with polyfluorowax–hydrophobic SiO2 through a
JID: JTICE
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X. Zhu et al. / Journal of the Taiwan Institute of Chemical Engineers 000 (2016) 1–5
dip coating process. The resulting textile possessed mechanically
durable superhydrophobicity, and it can retain its superhydropho-
bic property after immersion test, finger pressing, knife scratching,
twisting by hands, and even 10 cycles of abrasion with sandpa-
per. The textile was endowed with superhydrophobicity by an eas-
ily regeneration process when loss of self-cleaning occurred. The
resulting textile still displayed superhydrophobic upon emersion in
oil and exhibited water repellency after being contaminated by oil.
The resulting superhydrophobic textile can be applied as the sepa-
ration membrane and oil sorbent scaffold to separate oil from oil–
water mixtures efficiently. This superhydrophobic textile is hoped
to be implemented in air and oil surroundings where robustness is
needed, and it is also hoped to be a promising candidate for sepa-
ration oils from oil–water mixtures.
Acknowledgments
This work was supported by the Doctoral Starting up Founda-
tion of Yantai University (HJ15B36), the Nature Science Foundation
of Shandong Province (Grant no. ZR2016EEB02), and the National
Nature Science Foundation of China (Grant no. 51272222).
Supplementary materials
Supplementary material associated with this article can be
found, in the online version, at doi:10.1016/j.jtice.2016.11.029.
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