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Facile Spray-Coating for Fabrication of

Superhydrophobic SiO2/PVDF Nanocomposite Coating
on Paper Surface
a a
Yinlong Shi & Xinyan Xiao
a
College of Chemistry and Chemical Engineering, South China University of Technology,
Guangzhou, PR China
Accepted author version posted online: 29 Jul 2015.

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To cite this article: Yinlong Shi & Xinyan Xiao (2015): Facile Spray-Coating for Fabrication of Superhydrophobic SiO2/PVDF
Nanocomposite Coating on Paper Surface, Journal of Dispersion Science and Technology, DOI: 10.1080/01932691.2015.1053145

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 Facile Spray-Coating for Fabrication of Superhydrophobic SiO2/PVDF
Nanocomposite Coating on Paper Surface

Yinlong Shi1, Xinyan Xiao1

1
College of Chemistry and Chemical Engineering, South China University of Technology,
Guangzhou, PR China

Abstract

A facile and low-cost superhydrophobic nanocomposite coating on paper surface was

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fabricated through one-step simply spraying dispersion, using hydrophobic silica

nanoparticles as a filter and polyvinylidene fluoride (PVDF) as a film-forming material.

Hydrophobic silica nanoparticles (SiNPs) were fabricated via co-hydropholysis and

condensation of TEOS and long-chain alkyl silane based on a simple sol-gel process, and

the surface chemical structure of silica nanoparticles was characterized by Fourier

transform infrared (FTIR) spectra. The wettability and morphology of the coating surface

were measured by contact angle (CA) measurement and scanning electron microscope

(SEM), respectively. The influence of the mass ratio of hydrophobic silica nanoparticles

to PVDF (M(SiNPs:PVDF) ) on the superhydrophobicity of paper surface was studied.

The results showed that when M(SiNPs:PVDF) was 3:1, the water CA was 156.0±1.0° for

the nanocomposite coating with micro/nano- hierarchical structure on paper surface.

Further, such superhydrophobic nanocomposite coatings on paper surface showed little

adhesive property with water. In addition, the prepared superhydrophobic nanocomposite

1
 coating could be applied in other substrates, such as wood, aluminum sheet, stainless steel

and PTFE, etc.

KEYWORDS: Superhydrophobicity; Silica; Polyvinylidene fluoride; Spray; Wettability

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1. INTRODUCTION

Inspired by the self-cleaning effect of lotus surface, superhydrophobic surface, having

water CA higher than 150° and slide angle (SA) less than 10°, has recently received

extensive attention from academic and practical points of view. In general, the water

repellency of surface is attributed to the synergistic effect of surface roughness and

low-surface-energy materials 1,2 . The surfaces with this special wetting property exhibit

some important applications, such as anti-icing 3 , drag reduction 4 , liquid

transportation 5 , oil-water separation 6 , anti-corrosion 7 and other fields. Based on

such broad application perspectives, therefore, lots of techniques including plasma

treatment 8 , lithography 9 , phase separation 10 , chemical vapor deposition (CVD)

11 , electrochemical deposition 12,13 , layer-by-layer (LBL) assembly 14 , template

15 , solution immersion 16 and spray 17,18 , were exploited to fabricate

superhydrophobic surfaces. These routes can develop superhydrophobic surfaces through

2
 constructing the rough structure on the inherent hydrophobic surface or coating

low-surface-energy materials on a rough surface. However, many techniques involve strict

conditions, expensive materials, complicated steps and time-consuming processes, making

it impossible to fabricate superhydrophobic with effective cost. In addition, the durability

of superhydrophobic surface is one of the greatest challenges for the practical application.
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Paper products have been widely used in both work and daily life because of its cheap,

nontoxic, degradable and good mechanical properties. As a cellulose-based material, paper

contains amounts of hydroxyl groups on its surface, which can absorb water from the air,

resulting in its surface being easily affected with damp. The key point to solve this

challenge is to endow paper surface with the superhydrophobicity[19-22]. Yang et al. [23]

fabricated superhydrophobic surfaces on paper by multi-layer deposition of

polydiallyldimethylammonium chloride (PDADMAC) and silica particles, after which the

samples were modified by 1H,1H,2H,2H-perfluorooctyltriethoxysilane (PFOTS). Water

CA on the hydrophobic paper was greater than 150° and SA was less than 5°. Further, the

superhydrophobic paper products possessed a high tensile strength at high relative

humidity condition, and also showed excellent bacterial resistance. Wang et al. 24

prepared a superhydrophobic coating solution via co-hydrolysis and condensation of

TEOS and a fluorinated alkylsilane under the alkaline condition on various substrates such

as cotton and filter paper. The superhydrophobic coatings exhibited good transparency,

which the water CA is 170° and SA is no more than 10°. It should be noted that this is a
3
 one-step, simple and universal generation of superhydrophobic surface on paper. Tang et al.

25 fabricated a transparent superhydrophobic coating on paper by dip coating paper

samples in silica ethanol sol through co-hydrolysis of TEOS and

hexadecyltrimethoxysilane (HDTMS), followed by curing coating overnight at indoor

temperature. Huang et al. 26 developed a superhydrophobic paper via mixing

MPS-modified TiO2 nanoparticles modified by silane coupling agent, 3-(trimethoxysilyl)

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propylmethacrylate (MPS), into cellulose pulp, after which the pulp mixture was diluted

with distilled water to prepare hand sheets through a series of basic operation including

vacuum filtration, dehydration and curing. Water CA on the modified paper was measured

to be 154.2°, and 5 μL water droplets instantly dripped off the paper when the substrate was

tilted lower to 3°.

In this study, a facile fabrication process of superhydrophobic paper was reported, in

which superhydrophobic nanocomposite coating was fabricated simply by spraying

nanocomposite dispersion containing hydrophobic silica nanoparticle and PVDF on paper

surface. The influence of the mass ratio of hydrophobic silica nanoparticles to PVDF on

the wettability on paper surface was investigated. Further the adhesive property of the

superhydrophobic nanocomposite coatings also was discussed. In addition, the prepared

superhydrophobic nanocomposite coating could be applied in other substrates, such as

wood, aluminum sheet, stainless steel and PTFE, etc.

4
 2. EXPERIMENTAL

2.1. Materials

Printing paper was purchased from a local store. Tetraethylorthosilicate (TEOS, 98.0%),

ethanol (99.7%) and ammonia hydroxide (NH3·H2O, 25.0%) were supplied by Guangzhou

Chemical Reagent Factory, and n-dodecyltrimethoxysilane (DTMS) was obtained from

Huangshan KBR Chemical Co., Ltd. Poly(vinylidene fluoride) (PVDF) powder was
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purchased from Shanghai 3F New Material Co., Ltd. N,N-dimethylacetamide (DMAc)

were obtained from Tianjin Kemiou Chemical Reagent Co., Ltd. All of the chemical

reagents were used as received without further purification.

2.2. Preparation of Superhydrophobic Coating on Paper

The schematic diagram for fabrication of superhydrophobic SiO2/PVDF nanocomposite

coating on paper surface was shown in Fig. 1. The whole process can be divided into two

steps.

Step a: Hydrophobic silica nanoparticles（SiNPs）were prepared according to the previous

method 25 . In a typical process, 5 mL TEOS, mixed with an appropriate amount of

DTMS, was dissolved in 25 mL ethanol. The solution was added into ethanol-NH3·H2O

solution (25% NH3·H2O in 25 mL ethanol), and stirred intensively at room temperature for

12 h. Hydrophobic silica nanoparticles (SiNPs) with the size close to 85 nm were obtained

5
 after the resulting silica sol was successively centrifuged three times and rinsed with

ethanol, dried at 80 ℃ and ground into fine powders using a mortar.

Step b: The PVDF powders (0.1 g) were ultrasonic dispersed in mixed solvents

(DMAc/ethanol in a volume fraction of 1:5) for 30 minutes, so that PVDF powders can be

completely dissolved to form transparent solution. Then, the dispersion solution based on
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the mixture of silica nanoparticles and PVDF powders was prepared by the addition of 0.3

g silica nanoparticles to the above solution under moderate magnetic stirring until there

was hardly any precipitate. Finally, the obtained dispersion with different mass ratio of

PVDF to SiNPs (M(PVDF: SiNPs)) was manually sprayed on paper surface, keeping a

distant of 20 cm from paper surface to the airbrush. As soon as air was supplied into the

vaporizer by a pneumatic pump, pressure in the vaporizer was suddenly and

instantaneously increased, leading to spraying the mist of the sol. The process of spray

coating was performed 5 times till appropriate thickness of superhydrophobic

nanocomposite coating on paper surface was obtained. The papers with sprayed coating

were placed horizontally and dried overnight at room temperature.

2.3. Characterization

To determine surface composition change of silica nanoparticles, Fourier transform

infrared (FTIR) spectrum was recorded with a Bruker Tensor 27 spectrometer in the range

4000~400 cm-1. The morphological structure of the as-prepared paper was observed using
6
 a Hitachi S-3700 SEM. Apparent CA was measured with 6 μL water droplet using a CA

measurement apparatus (OCA-40, Data Physics). The average CA value was determined

by measuring the CA of the same sample at five different positions.

3. RESULTS AND DISCUSSION

3.1. Facile Preparation of the Nanocomposite Coating on Paper Surface

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Hydrophobic silica nanoparticles was fabricated via co-hydrolysis and condensation based

on a sol-gel process using TEOS and DTMS as co-precursors in ethanol with NH3·H2O as

catalyst. Compared with the speed of DTMS hydropholysis, TEOS in the ethanol solution

hydrolyzed more quickly to form hydrophilic silica nanoparticles and turned the sol milky

via successive hydrolysis and condensation 27 . Following the formation of silica

nanoparticles (SiNPs), DTMS gradually hydrolyzed into dodecyltrihydroxysilane (DTHS),

which could react with reactive silanol groups presented on the surface of silica

nanoparticles. Due to the presence of long hydrophobic dodecyl chain, therefore, silica

nanoparticles were endowed with the hydrophobicity. It is worth noting that PVDF, as a

commercially available fluoropolymer with extremely low surface energy, has high

mechanical strength, good film forming property, excellent thermal and chemical

stabilities. The superhydrophobic coating on paper surface was prepared by spraying the

nanocomposite dispersion with the addition of hydrophobic silica nanoparticles to PVDF

in ethanol-DMAc solution. The addition of hydrophobic silica nanoparticles (SiNPs)

could contribute to enhancing the surface roughness and decreasing the surface free
7
 energy, while PVDF can be employed as a film-forming material to improve the adhesion

between silica particles and the surface of paper. It can be demonstrated that incorporating

hydrophobic silica nanoparticles as the filler into PVDF polymer results in the

superhydrophobicity on paper surface because of the combination of surface

microstructure and low surface free energy.

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3.2 FT-IR Characterization of Silica Nanoparticles

FT-IR was carried out to analyze the interaction between DTMS and silica nanoparticles.

Fig. 2 showed the FTIR spectra of DTMS, DTMS-modified and unmodified silica

nanoparticles. As shown in Fig. 2(c), the peaks appearing at 2923 and 2854cm-1 were

attributed to the stretching vibrations of –CH3 and –CH2, respectively, which were in

consistence with that of DTMS (Fig. 2(b)). In addition to these peaks, the strength the

broad peak in the range of 3700 to 3000 cm-1, which was assigned to –OH heavily

presented on the surface of silica particles, appeared to be weakened markedly as

compared to that of Fig. 2(a). It was mainly because the coverage of dodecyl groups on

silica nanoparticles played an important role so that the content of resulting hydroxyl

groups on silica particle surface significantly decreased. The results confirmed evidently

that the DTMS molecules have been self-assembled onto the surface of silica nanoparticles

so that they showed hydrophobic property.

3.3 The Morphology of the Superhydrophobic Paper Surface

8
 The surface morphologies of pristine paper surface, paper surface with only PVDF coating

and superhydrophobic paper surface were examined by using scanning electron

microscopy (SEM) at different magnifications, respectively. As shown in Fig. 3(a1), it

could be clearly seen that the surface of the pristine paper with subtle textures consisted of

a large number of hydrophilic cellulose by tightly intertwining and stacking each other, and

fabric surface was relatively smooth (Fig. 3(a2)), which resulted in the low water CA close
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to 76.6° on the paper surface (Fig. 4(a)). After coated with inherently hydrophobic PVDF,

a continuous film with microscale streak protuberances could be observed, and fabric

surface distributed uniformly many bare nanoprotrusions (Fig. 3(b1) and (b2)), making

water CA greatly increase up to about 129.0° (Fig. 4(b)). When the surface of paper was

covered with hydrophobic SiO2/PVDF composite coating, as provided in Fig. 3(c1), it

could be clearly seen that microscale aggregates distributed thickly and uniformly on the

paper surface because of silica agglomeration. Additionally, Fig. 3(c2) was the

magnification image of Fig. 3(c1), which showed that fabric surface distributed many

nanoscale pores and protrusions, leading more air to being trapped into these pores on the

nanocomposite coating and minimizing dramatically the actual contact area. It was worth

noting that the evaporation of solvents was vital to the formation of nanoscale structure of

coating surface. Due to hierarchical structure with binary roughness on the surface, paper

surface covered with the nanocomposite coating was rendered superhydrophobic, which

resulted in a maximum water CA of 156.0° (Fig. 4(c)). Accordingly, the above results

9
 demonstrated convincingly that surface microstructure morphology played a significant

role in the enhancement of surface superhydrophobicity.

3.4 The Influence of M(PVDF: Sinps) on Wettability

However, due to the poor adhesion of inorganic particles, hydrophobic SiO2 coating on

paper surface was easily destroyed even by finger touching. The best way to solve that
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problem was to introduce film-forming materials for improving the interaction of

inorganic particles with substrates. Therefore, in order to improve the coating performance,

the present study used PVDF as the binder to improve the adhesion between hydrophobic

SiO2 nanoparticles (SiNPs) with paper surface. Extensive research about the preparation

of inorganic nanoparticles/polymer composite materials has recently been reported [28-30],

and the role of polymer as film-forming materials was greatly vital for improving the

adhesion between inorganic nanoparticles and substrates, which was highly superior to the

single inorganic coating.

In order to investigate the influence of the mass ratio of PVDF to hydrophobic silica

nanoparticles (M(PVDF: SiNPs)) on wettability of the paper surface, a series of

nanocomposite coatings on paper surface were fabricated under different M(PVDF: SiNPs)

ranging from 0:1 to 5:1. As shown in Fig. 5, it can be seen that the water CA of

nanocomposite coating on paper surface increased significantly from 129.0° to 149.0°

with the increase of M(PVDF: SiNPs) from 0:1 to 2:1 and reached a maximum value of
10
 156.0°, which occurred at the mass ratio of 3:1. Thereafter, the water CA on

nanocomposite coatings decreased slightly but were kept above 150.0° as M(PVDF:

SiNPs) was further increased to 5:1. This could be mainly attributed to the formation of

hierarchical roughness constructed by hydrophobic silica nanoparticles and the decrease

of surface energy. In general, increasing the amount of the hydrophobic silica

nanoparticles was much conducive to the enhancement of the hydrophobicity of the paper
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surface. Additionally, as mentioned above, PVDF also played an important role in the

improvement of the hydrophobic behavior of coating through making the nanocomposite

coatings adhere tightly to the paper surface.

3. 5 Ultralow Adhesion Property And Application of Nanocomposite Coating

Fig. 6 showed the approach and departure processes of a water droplet suspending on a

syringe with respect to the superhydrophobic coating on paper surface. It could be seen

that the resulting SiO2/PVDF nanocomposite on paper surface was so extremely

hydrophobic that the water droplet had almost no possibility to sit on and even completely

separated with the coating surface. Meanwhile, there was nearly no water residue left after

the water droplet departed from the paper surface, which illustrated that there was

exceedingly less adhesion force between water droplet and coating surface compared with

the capillary force between water droplet and the syringe. It was convincingly suggested

that the as-prepared superhydrophobic nanocomposite coating on paper surface possessed

good non-sticking characteristic.

11
 Furthermore, the nanocomposite coating was not substrate-limited. It could be fabricated

on various substrates, such as stainless steel, aluminum sheet, wood and polymer

membrane (PTFE) through one-step spray-coating. Fig. 7 showed the optical images of

water droplets floating on the surface of the nanocomposite coating on different

substrates. It was clear that the coating surface was so extremely hydrophobic that the
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water droplets deposited on the surface could remain almost perfect spheres. The water

droplet could be moved easily when the surface is slightly tilted.

4. CONCLUSIONS

In summary, superhydrophobic coating on paper surface was fabricated through facile

spraying the nanocomposite dispersion. The surface wettability could be adjusted by

varying the mass ratio of PVDF to SiNPs. The adhesion test demonstrated that the

superhydrophobic nanocomposite coating on paper surface showed ultralow adhesion

with de-ioned water. The approach to fabricate superhydrophobic coatings on paper

surface may have potential application in the fields of anti-contamination and protection

against moisture.

ACKNOWLEDGEMENTS

We gratefully thank the financial support from the National Natural Science Foundation

of China (No. 21076092, 21376099).

12
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 Fig. 1. Schematic diagram of the fabrication of super hydrophobic nanocomposite coating

on paper surface.
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16
 Fig. 2. FT-IR spectra of (a) unmodified SiO2, (b) DTMS, and (c) DTMS modified SiO2.
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17
 Fig. 3. SEM images of the pristine paper surface at low (a1) and high (a2) magnification,

the paper surface with PVDF coating at low (b1) and high (b2) magnification, the paper

surface covered with SiO2/PVDF composite coating at low (c1) and high (c2)

magnification.
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18
 Fig. 4. The CA images of 6 μL water droplet on (a) the pristine paper surface, (b) paper

surface with only PVDF coating, and(c) paper surface covered with SiO2/PVDF

nanocomposite coating.
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19
 Fig. 5. Effect of M(PVDF:SiO2) on water CA of the super hydrophobic paper surface.
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20
 Fig. 6. Sequential photographs (a-e) show the approach, contact, deformation, and

departure processes of a 6μL water droplet suspending on a syringe with respect to the

coating on paper surface, in which the arrows represent the moving direction of the

substrate.
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21
 Fig. 7. Optical images of water droplets (dyed blue) floating on the nanocomposite coating

surface on different substrates such as (a) stainless steel, (b) aluminum, (c) wood, and (d)

PTFE.
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22