Revista de Ciencias Tecnológicas (RECIT). Universidad Autónoma de Baja California ISSN 2594-1925
Volumen 5 (1): e190. Enero-Marzo 2022 https://doi.org/10.37636/recit.v5n1e190.
ISSN: 2594-1925
1
Research article
Statistical influence of NH4OH, number of layers and droplet
volume in the development of ultra-hydrophobic coatings based
on SiO2 nanoparticles
Influencia estadística del NH4OH, número de capas y volumen de gota en el
desarrollo de recubrimientos ultra-hidrofóbicos basados en nanopartículas de
SiO2
José Felix Magdaleon Loredo , Delfino Cornejo Monroy
Instituto de Ingeniería y Tecnología, Universidad Autónoma de Ciudad Juárez. Av. Del Charro 450 Norte, Col. Partido
Romero 32310, Ciudad Juárez, Chihuahua, México
Corresponding author: Jose Felix Magdaleon Loredo, Instituto de Ingeniería y Tecnología, Universidad Autónoma de Ciudad Juárez. Av.
Del Charro 450 Norte, Col. Partido Romero 32310, Ciudad Juárez, Chihuahua, México. E-mail: al198636@alumnos.uacj.mx. ORCID: 0000-
0002-2043-2842
Recibido: 18 de Septiembre del 2021 Aceptado: 22 de Diciembre del 2021 Publicado: 13 de Enero del 2022
Abstract. – Ultra-hydrophobic coatings are of interest in automotive, aeronautical and construction applications and in
general in any area or surface where the use of highly water-repellent surfaces, with self-cleaning, anti-icing, and anti-
corrosion properties is favorable. In recent years, various researchers have proposed different physical and chemical methods
to obtain high-hydrophobic condition. In this article, the manufacture of a colloid based on SiO2 nanoparticles is described to
manufacture hydrophobic coatings with contact angles greater than 140º. With the help of a design of experiments and the
manufacture of a colloid based on SiO2 by the colloidal method, three factors were analyzed with their corresponding levels
and their influence to maximize the contact angle. The fabricated colloid was sprayed and layered onto glass. In all the
materials where the coating was applied, static contact angles (SCA) between 120º and 160º were obtained. Results by UV-
Vis’s spectroscopy indicate that the transparency is greater than 68% and that this depends directly on the layers applied by
spraying and on the quality of the film formed. The FT-IR spectra support the formation of SiO2 nanoparticles, the presence of
-OH groups in the different stages of the colloid manufacturing process, and C-F bonds. The composition and morphology
were analyzed by field emission scanning electron microscopy (FESEM). FESEM micrographs were analyzed for the ultra-
hydrophobic solutions and showed agglomeration of nanoparticles. As work in the future, it is proposed to analyze the wear
resistance of coatings, their durability, and sliding angle, improving their hydrophobic properties.
Keywords: Ultra-hydrophobic coatings; Design of experiments; SiO2 nanoparticles; Sol-gel method; Transparency.
Resumen. – Los recubrimientos ultra-hidrofóbicos son de interés en aplicaciones de automoción, aeronáutica y construcción
y en general en cualquier zona o superficie donde sea favorable el uso de superficies altamente hidrofugantes, con propiedades
autolimpiantes, antihielo y anticorrosión. En los últimos años, varios investigadores han propuesto diferentes métodos físicos
y químicos para obtener una condición altamente hidrofóbica. En este artículo se describe la fabricación de un coloide a base
de nanopartículas de SiO2 para fabricar recubrimientos hidrofóbicos con ángulos de contacto superiores a 140º. Con la ayuda
de un diseño de experimentos y la fabricación de un coloide a base de SiO2 por el método coloidal, se analizaron tres factores
con sus correspondientes niveles y su influencia para maximizar el ángulo de contacto. El coloide fabricado se pulverizó y se
colocó en capas sobre el vidrio. En todos los materiales donde se aplicó el recubrimiento se obtuvieron ángulos de contacto
estático (SCA) entre 120º y 160º. Los resultados por espectroscopía UV-Vis indican que la transparencia es superior al 68%
y que esto depende directamente de las capas aplicadas por proyección y de la calidad de la película formada. Los espectros
FT-IR respaldan la formación de nanopartículas de SiO2, la presencia de grupos -OH en las diferentes etapas del proceso de
fabricación de coloides y enlaces C-F. La composición y morfología se analizaron mediante microscopía electrónica de
barrido por emisión de campo (FESEM). Las micrografías FESEM se analizaron en busca de soluciones ultra hidrofóbicas y
mostraron aglomeración de nanopartículas. Como trabajo a futuro se propone analizar la resistencia al desgaste de los
recubrimientos, su durabilidad y ángulo de deslizamiento, mejorando sus propiedades hidrofóbicas.
Palabras clave: Recubrimientos ultra-hidrofóbicos; Diseño de experimentos; Nanopartículas de SiO2; Método sol-gel;
Transparencia
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1. Introduction
Material surfaces are highly exposed to
environmental conditions [1], contamination, dirt
[2-3], dust [4], sand [5], acidic water, oily
substances [6], etc. In general, many of these
conditions are undesirable since they negatively
influence the useful life of the material and its
performance [7-8]. Some surfaces are more often
faced with certain substances and are therefore
more prone to damage [7]. That is why, for some
years now, scientists have tried to create surfaces
that meet certain needs [8], starting from knowing
the characteristics and abilities of some plants and
animals.
One of the most studied conditions in recent times
is high-hydrophobic condition. Ultra-hydrophobic
(UH) surfaces show values of SCA between 120-
1500 [9], while in superhydrophobic (SH) surfaces
are above of 1500 [2][6][12-19] between the solid
phase and the liquid phase. This characteristic
allows a wide number of applications, including
self-cleaning [8][10-16], drag reduction
[8][12][17], anti-corrosion [8][10][18-21],
transparency [8][22-23], anti-icing [16][18-20],
oil-water separation [17-18] and so on. This type
of surface influences the reduction of maintenance
costs [24] and increases the useful life of the
materials [25].
There are two approaches to achieve high-
hydrophobic conditions: (i) increase surface
roughness [26-29], (ii) decrease surface tension
[20][30-33]. The first approach is related to the
idea of reducing, as much as possible, the contact
area between liquid and solid, and in turn, being
able to create spaces in which air bubbles can be
located [20] [31][34-36] that serve as a barrier
(protects the drop from morphological
irregularities that can undo them). The second
approach is closer to the chemical composition,
which determines the adhesion forces present in
the contact area [37-40].
There are compounds that make it possible to
achieve superhydrophobic characteristics
through the application of the aforementioned
approaches, specifically the use of silanes.
Vouvoudi et al. [1] manufactured a
superhydrophobic coating for the protection of
the stone-built cultural heritage. They reported
SCA of 1700 approximately. To do this, they
mixed tetraethyl orthosilicate (TEOS) and 1H,
1H, 2H, 2H-perfluorooctyl tri-ethoxy silane
(FAS). Finally, the versatility of the solution
allowed excellent results on at least 3 more
substrates [1]. Zhu et al. [26] created a
transparent SH coating with good mechanical
properties. The silane used was
polydimethylsiloxane (PDMS), which is not
contaminating like those containing fluorine.
The modification achieved by this compound
allowed reaching values of SCA higher than
1600 and transparency levels higher than 76%
[26].
In this article, we report the development of UH
and transparent coatings through SCA
optimization based on a general full factorial
design. The coatings show SCA values greater
than 1400 and transparency values greater than
65%. The corresponding characterizations were
carried out.
2. Methodology
The Figure 1 illustrates the steps to follow in
the present investigation.
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Figure 1. Methodology
2.1 Materials
The following materials were used for the
preparation of the coatings: tetraethyl orthosilicate
(TEOS), (98% from Sigma-Aldrich) as a precursor
for SiO2 nanoparticles; Ammonium hydroxide
(NH4OH), (NH3 content 28-30% from Sigma
Aldrich®) that influences the size of the
nanoparticles; 1H, 1H, 2H, 2H-
perfluorodecyltriethoxysilane (AC-FAS) (97%
from Matrix Scientific®) is applied as a surface
modifier; isopropyl alcohol (IPA) and deionized
water (DIW).
2.2 Equipments
Stirring hot plate (model PC-420D, CORNING®.
Ultrasonic cleaning bath (model TS-2.5L),
truSonik ®.
2.3 Design of experiment (DOE)
The DOE chosen was a general full factorial
design. The Figure 2 illustrates a general analysis
for our investigation.
Figure 2. General model of the investigation process
The inputs for this design were the drying time
of coatings and deposition time between layers.
The controllable factors were the NH4OH
concentration, the number of layers and the
applied droplet volume to measure the static
contact angle. As an uncontrollable factor, it
was only defined at room temperature. The
output variable was established as the SCA. All
prepared samples were made up to a volume of
50 ml. Table 1 shows the agent volumes in each
sample.
Table 1. Agent volumes
Samples
IPA
(ml)
DIW
(ml)
TEOS
(ml)
AC FAS
(ml)
NH4OH
(ml)
M1
36.8
11.71
1
0.15
0.5
M2
37.04
11.71
1
0.15
0.25
M3
37.24
11.71
1
0.15
0.05
M4
37.265
11.71
1
0.15
0.025
The only difference between samples is the
NH4OH content. This difference made it
possible to assess the influence of NH4OH on
SCA.
2.4 Preparation of samples
The preparation procedure proposed by Ge et
al. [41]. Prior to the preparation, a deep wash
of all the necessary elements (glass Erlenmeyer
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flasks, pipette tips, magnetic stirrers) was carried
out to develop the preparation of the samples. The
washing was carried out with DIW and alconox®
detergent, and subsequently they were rinsed with
DIW and IPA. The preparation of the solutions
was started by stirring a mixture of IPA and DIW
at 500 rpm, in a 100 ml glass Erlenmeyer flask, for
10 min. Then NH4OH and TEOS were added in the
order mentioned and kept at the same angular
stirring speed for 24 h. After the planned time, the
AC-FAS was added and 48 h were waited to turn
off the stirring hot plate machine, in this way the
preparation process was concluded. The entire
process was carried out at room temperature.
2.5 Spray Deposition
Prior depositing the solution on the substrate (26 x
76 x ± 1-1.2 mm glass slides, from Lauka®), it was
placed in the ultrasonic cleaning bath machine in
order to achieve a greater degree of homogeneity
of the solution. The spray gun was also washed as
an essential element of the selected method. The
spray method was carried out at 15 cm from the
substrate placed horizontally, the firing pressure
was 0.2 MPa at room temperature. The deposition
time between coats was set at 10 min, while the
final drying time (time in which the SCAs were
measured was 24 h). The drying was carried out
naturally (air).
2.6 Characterization
The chemical composition and morphology of the
surface, and NPs size analysis were carried out
with the use of the field emission scanning electron
microscope (FESEM) (JEOL® brand, model JSM-
7000F) and energy dispersive spectrometer (EDS).
The volume ratio between IPA and samples was
10: 1, and it was deposited on a carbon adhesive
tape. Fourier transform infrared (FT-IR)
spectrophotometer (BUCK Scientific®, model
530), it was used to identify the functional groups
in a wavenumber interval of 600-4000 cm-1, and a
resolution of 0.8 cm-1; the samples had to be
prepared with potassium bromide (KBr).
Ultraviolet visible light (UV-vis)
spectrophotometer (series AF1311015) was
used to determine the light transmittance in a
range of 380-760 nm with intervals of 1 nm.
SCA measurement was achieved with a Profile
Projector (Mitutoyo Corporation®, model PH-
A14).
3 Results and Discussion
3.1 Statistical analysis
Images for SCA measurement were obtained
using a profile projector and analyzed with the
ImageJ software. Table 2 shows the SCA
values.
Table 2. Static contact angles
Samples
SCA-10 µl ( 0)
M1 (2 layers)
M1 (4 layers)
146.2±3
150.6±2
M2 (2 layers)
M2 (4 layers)
148.2±2
150.3±2
M3 (2 layers)
M3 (4 layers)
M4 (2 layers)
M4 (4 layers)
143.3±2
151±1
144.1±3
151.7±1
Table 2 presents all the values in a range of 141-
1530 when the highest value was 152.55 ± 10
and it was reached in M1. Table 2 shows that,
as the number of layers increases, the SCA
increases. The number of layers is a factor that
can be directly related to the thickness of the
coating, because, as the number of layers
increases, the thickness increases. Ge et al. [41]
investigated the influence of thickness on SCA
for a coating obtained from the mixture of two
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silanes, TEOS and (heptadecafluoro-1,1,2,2-
tetrahydrodecyl)triethoxysilane (HDFTES), with a
stringed SiO2 NPs. The result shows that when
increasing the thickness of 2-8 µm, the SCA
increased from 160.5-165.50 approximately [41].
This result coincides with the result obtained in
this investigation. Purcar et al. [42] reported the
influence of thickness on the SCA of SiO2-based
coatings obtained from TEOS and modified with
alkoxysilane mixtures using the sol-gel method.
The alkoxysilanes used were methyl
triethoxysilane (MTES), octyltriethoxysilane
(OTES), vinyltrimethoxysilane (VTMES), and
hexadecyltrimethoxysilane (HDTMES). The
thicknesses for TEOS/MTES/OTES,
TEOS/MTES/VTMES and
TEOS/MTES/HDTMES were 3522.8, 1288.0 and
1584.9 nm respectively; their respective SCAs for
the thicknesses obtained were 104, 88 and 1060
[42]. The presence of a second factor included in
the analysis caused a change in the results. This
time the study included, in addition to thickness,
the type of alkoxysilane, which led to the loss of
the relationship obtained in the present study and
increases in SCA were not achieved with
increasing thickness.
Using the Minitab® 17 software, it performed the
general full factorial design to determine if the
factors taken into account significantly influence
the response variable. The experiment was
randomized and replicated to ensure a more
reliable test. Figure 3 presents the results of the
analysis.
Figure 3. P-Value analysis
Taking into account a confidence level of 95%,
the significant factors will be those that do not
exceed the level of significance (0.05). As can
be seen, the three factors proposed in the
experiment showed p-values lower than the
reference value mentioned above. Similarly,
double and triple interactions have p-values
lower than the reference value. All this
information allows us to declare that all the
factors and their interactions will be significant
for the response variable. It also generated the
main effects plot for SCA to more easily
observe the influence of each factor on the
response variable. Figure 4 presents the
directions we can choose from each factor to
increase SCA.
Figure 4. Main effects plot for SCA (fitted means)
Figure 4 presents the behavior of each factor in
this investigation. The NH4OH factor showed
better SCA values at the levels with the highest
concentration of NH3; the number of layers
confirmed that as it increased, the values of the
response variable increased too; while an
increase in drop volume tends to decrease SCA.
These SCA results make it possible to ensure
that the three factors influence the achievement
of ultrahydrophobicity (120 <SCA≤1500); in
addition, in the particular case of number of
layers, 4 layers allowed achieving
superhydrophobicity (SCA> 1500). Figure 5
allows a double interaction analysis of the
factors.
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Figure 5. Interaction plot for SCA (fitted means)
This figure shows the interactions between factors,
and it is evidenced that the least interaction is
established between NH4OH and number of
layers. On the other hand, between number of
layers and drop volume a certain closeness and
similar direction is perceived, which allows to
ensure that it is the interaction that has the most
effect on SCA; the highest SCA values were
reached for this interaction.
The response variable was maximized to
determine the 5 best combinations of factors.
Figure 6 shows the response optimizer.
Figure 6. Response optimizer.
Fig. 6 allows determining the combinations of
factors with the highest SCA values. The response
optimizer presented the 5 highest SCA values in
the study. All combinations met the maximum
number of layers deposited (4 layers), this
confirms the idea that to achieve
superhydrophobic surfaces it was necessary to
apply 4 layers of coatings. The highest value
obtained was 152,550.
3.2 Functional groups analysis
The analysis of the functional groups was
carried out with a FT-IR. In Figure 7 the
spectrum generated by the SiO2 NPs is
observed.
Figure 7. FT-IR spectrum (sample M3)
In the FT-IR spectrum of glass substrate, a
broad band were identified from 2750-3800 cm-
1 with center at approximately 3400 cm-1,
corresponding to the hydroxyl stretching (-OH
stretching vibrations) [1][37-39], then another
-OH group was observed around 1630 cm-1.
The C-F stretching vibrations peak at 1204 cm-
1 was easily recognized in the spectrum
[41][43]; these groups are characterized by
having low energy, they are attributed a
decrease in the surface energy of the coating.
The peak at 1100 cm-1 was attributed to the most
characteristic peak of the SiO2 nanoparticles
[1][37-38], which is assigned to the asymmetric
stretching, symmetric stretching and bending
vibration. Finally, two more peaks were located
below 1000 cm-1: (i) at 950 cm-1 (Si-O bond)
[42] and (ii) at 793 cm-1 belong to vibrations Si-
O-Si bonds [1][26][41][44] attributed to the
bending vibrations.
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3.3 Chemical composition
The chemical composition was evaluated with the
use of FESEM-EDS. The solution was analyzed
before adding the AC-FAS and another with all the
reagents that make up the coating. In addition,
images of the distribution of each chemical
element in each sample were obtained, as shown
in Figure 8.
Figure 8. FESEM (EDS mapping) images (sample M3): (a)
Solución sin AC-FAS, (b) solución con AC-FAS, (c) Oxygen map,
(d) Silicon map, and (e) Fluorine map.
In Figure 10 (a, b), the presence of Si, O and C is
observed, while F only appears in Figure 10b due
to the addition of AC-FAS. All chemicals were
evenly distributed over the entire surface,
suggesting that the preparation method used was
appropriate to achieve a uniform coating.
3.4 Surface morphological study
The morphological analysis was carried out in
FESEM. Figure 9 showed the surface
morphology of the sample M3.
Figure 9. FESEM (secondary electrons) images (sample M3)
The images obtained in SEM showed a large
agglomeration of particles. This agglomeration
can be a consequence of the addition of AC-
FAS. This agglomeration can also decrease the
degree of hydrophobicity, and can be the cause
of a decrease in the percentage of light
transmittance. Finally, particle agglomeration
made particle size determination impossible.
3.5 Transparency analysis
The transparency of all samples (2 and 4 layers)
was determined by using the UV-vis
spectrophotometer; all analysis was performed
in the wavelength interval 380-760 nm. Figure
10 shows the transmittance spectra of the
coatings.
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Figure 10. Transmittance spectra UV-vis: (a) 2 layers, (b) 4 layers.
As shown in Figure 10a, the M2 lost 11% of the
transmittance compared to an uncoated glass
(100%), for 89% of transmittance, approximately.
The other samples presented average values in a
range of 68-80%. When the number of layers was
increased to 4 (Figure 10b), there was a loss of
transmittance of 23% (sample 2), while the others
were less than 60%. These results suggested that
by increasing the number of layers there was an
increase in surface roughness, which led to an
increased light scattering, thus decreasing the light
transmittance. In this case, the number of layers is
analogous to the number of cycles, which
increases the thickness of the coating as it
increases. H. Teisala et al. [45] transparency was
investigated using UV-vis spectrophotometer for
different Si/Ti ratios. The results were obtained by
applying 1 and 5 coating cycles on the
substrate. For 1 cycle, all transmittance values
were greater than 98% for wavelengths greater
than 500 nm. For 5 cycles, 97% were obtained
in Si-100% and 79% with Si-1%, which
indicated a decrease in transmittance as the
concentration of Si in the coatings decreased
[45]. It can be noted that this result agrees with
the result obtained in our study, the increase in
the number of cycles has a negative effect on
the level of transparency [45]. Ge et al. [41]
investigated the influence of thickness on the
transparency results of coatings made with a
TEOS/HDFTES solution with stringed SiO2
nanoparticles. The range in which the
measurements were made was 3-8 µm and it
was observed that as the thickness increased
there was a decrease in transmittance; the
transmittance obtained was approximately
91.5% at 550 nm for a thickness of 5 µm [41].
This result also confirms our result.
4 Conclusions
Ultra-hydrophobic coatings based on SiO2
nanoparticles were developed using the sol-gel
method. The SCA obtained exceeded 1400,
reaching values above 1500 (super-
hydrophobicity). The influence of three factors
(NH4OH, number of layers and droplet volume)
on the ACS was analyzed using a general full
factorial design with a 95% confidence level.
All the factors were statistically significant for
the output variable. By increasing NH4OH there
was an increase in SCA; when the number of
layers increased, the SCA also increased; while
with increasing droplet volume, SCA
decreased. Other studies show similar results
for the number of layers because it is related to
the increase in surface roughness; This factor is
also the main responsible for achieving SCA
values higher than 1500.
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The FESEM images showed an excessive
agglomeration of particles, an aspect that must
have had a negative impact on the results of
contact angles and that prevented the
determination of the particle size; agglomeration
was attributed to AC-FAS.
The analysis of functional groups permitted to
identify SiO2 nanoparticles, which shows that the
sol-gel method is appropriate for this objective; It
was possible to verify the presence of C-F groups,
to which the decrease in the surface energy of the
coating and the high degree of hydrophobicity due
to its low energy are attributed.
Transparency levels of 68-89% were achieved.
The number of layers negatively influenced the
level of transparency, reducing the transmittance
of sample M2 from 89 to 77 for 2 and 4 layers
respectively. This result was consistent with
studies conducted by other researchers.
In this study, we managed to include a factor not
widely studied: droplet volume. In addition, the
coatings developed can be implemented in
applications such as self-cleaning, anti-reflection,
anti-corrosion, among others.
5. Acknowledgements
To Universidad Autónoma de Ciudad
Juarez/Instituto de Ingenieria y Tecnología, and
CONACyT.
6. Authorship and Contribution
Jose Felix Magdaleon Loredo: Conceptualization,
methodology, validation, formal analysis,
research, original draft, revision-edition,
visualization, project supervision-administration,
data analysis. Delfino Cornejo Monroy:
Conceptualization, methodology, research,
revision-edition, project supervision-
administration.
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