International Journal of Civil Engineering and Technology (IJCIET)
Volume 10, Issue 04, April 2019, pp. 1971–1982, Article ID: IJCIET_10_04_206
Available online at http://www.iaeme.com/ijmet/issues.asp?JType=IJCIET&VType=10&IType=4
ISSN Print: 0976-6308 and ISSN Online: 0976-6316
© IAEME Publication
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AN EXPERIMENTAL INVESTIGATION ON
SUPERHYDROPHOBIC COATING USING
NANO-GGBS ON CEMENT MORTAR
Jeya Sheema J
PG Student, Department of Civil Engineering,
Mepco Schlenk Engineering College, Sivakasi, Tamilnadu, India
Prabavathy S
Senior Professor & Head, Department of Civil Engineering,
Mepco Schlenk Engineering College, Sivakasi, Tamilnadu, India
ABSTRACT
A novel method to achieve water-repelling character upon a cement paste has
been investigated. GGBS (Ground Granulated Blast furnace Slag) is a by-product
from steel industry which is preferred to produce a superhydrophobic surface coating
for cement mortar. The super hydrophobic coating is prepared by sonicating Nanoscaled GGBS powder into a mixture of silane/siloxane. Different methods of
application of coating, such as brushing, spraying and impregnation are used. In this
paper, the super hydrophobic performance and durability of the coated cement mortar
cubes has been reported based on water contact angle, water absorption and
sorptivity. Also the reduction of surface porosity has been studied by using Ultrasonic
pulse velocity test. As a result, The spray coated surfaces exhibited
superhydrophobicity with a water contact angle of 152.2°. The performance of the
impregnated samples are notably higher in water absorption, sorptivity and ultrasonic
pulse velocity.
Key words: Hydrophobicity, Silane, Contact angle (CA), Water-repellency,
Nanoparticles
Cite this Article: Jeya Sheema J and Prabavathy S, An Experimental Investigation on
Superhydrophobic Coating Using Nano-GGBS on Cement Mortar, International
Journal of Civil Engineering and Technology 10(4), 2019, pp. 1971–1982.
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1. INTRODUCTION
Reinforced concrete is the often used construction material in buildings, roads and bridges, in
any case, steel corrosion poses an incredible threat to the strength and stability of these
concrete structures [1]. Ingression of water is the major cause for all the physical and
chemical degradation in concrete structures [2]. Generally, the hydrophilic behavior of the
concrete is induced by the micro-pores, micro-voids and micro-cracks on its surface [3]. The
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water droplets entering into the concrete through these defects carries dissolved aggressive
substances like chloride ions, carbon dioxide, sulphur dioxide and sulphates [3-6]. Also, the
capillary uptake of water into these micro-cracks deteriorate the concrete during freeze-thaw
cycles [7]. The steel reinforcement embedded into the concrete is endangered by the waterborne chloride (Cl-) and sulphate (SO42-) ions [8]. The rust formation around the
reinforcement will induce expansion and tensile stresses on the surface of the encompassing
concrete [9]. Cracking, spalling and delamination of concrete are led by these stresses [9,10].
Recent developments in this field of research, have found an alternative solution for
protecting the concrete by super hydrophobic impregnation [11-13]. The leaves of Lotus,
exhibit super hydrophobicity with a water contact angle greater than 150° [14]. This concept
of recreating the effect of Lotus leaf on the surface of cement paste is called Biomimetics or
biomimicry [14-16]. Silanes/siloxanes are the most commonly relied material for inducing
hydrophobicity upon concrete surface [12]. The low surface energy materials in hierarchical
scale of micro/ nanometer will enhance the hydrophobic surface to produce super
hydrophobicity [17-20]. Initiation of corrosion is postponed by super hydrophobic
impregnation, since it arrests the penetration of water and chloride ion into concrete [13].
The objective of this paper is to apply a super hydrophobic surface treatment using GGBS
(Ground Granulated Blast furnace Slag) and silane on cement mortar. Inorder to manipulate
the adequate roughness and super-hydrophobicity required by the coating on cement mortar,
GGBS was synthesized to Nano scale. The air captured on this rough surface will reduce the
contact between mortar and water, thereby producing water-repelling and self-cleaning
characteristics. The influence of this surface treatment on super hydrophobicity and durability
are studied by adopting different methods of application.
2. MECHANISM OF HYDROPHOBICITY
2.1. Theory of wettability [21,23]
Owing to the electrical dipole behavior of water molecules, upon a high surface energy
surface they get attracted to charged ions and wet the surface [24]. On a surface with low
surface energy, the water molecules will bead-up forming a spherical droplet and gets roll-off
without wetting the surface. The minimum contact angle exhibited by the water loving surface
is 0° and the maximum contact angle exhibited by the water repelling surface is 180°.
2.2. Water contact angle [25-27]
Figure 1 Theory of Hydrophobicity
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The water contact angle is usually measured using WCA Goniometer. The surfaces
exhibiting contact angle <90° are said to be hydrophilic. For over-hydrophobic surfaces, water
contact angle ranges between 120° to 150°. Surfaces showing contact angle >150° are called
as Ultra hydrophobic. Generally the concrete surface exhibit contact angle <30°. Also, the
mortar surface would exhibit absolute wetting with 0° contact angle.
3. EXPERIMENTAL WORK
3.1. Materials
Ground Granulated Blast furnace Slag (GGBS), a major by-product from the steel
manufacturing industries is bought. The average particle size varies from 1000 to 1300nm. It
appears to be light grey with a specific gravity of 2.93.
Isobutyltriethoxysilane (C10H24O3Si) [28] with a molecular weight of 220.38 g/mol and
97-98% purity purchased from the Aldrich was used as the hydrophobizing agent in this
paper. The Isobutyltriethoxysilane has a dual character from hydrophilic to hydrophobic
phase. Also it penetrates deeply into the cementitious substrate [29]. Commercially available
Epoxy resin and hardener are used as adhesive to bind the nanoparticles to the mortar surface.
The Ordinary Portland Cement (OPC) of grade 53 with a specific gravity of 3.16 was used
as the binding material. River sand passing through zone II grading with a specific gravity of
2.66 was used as the fine aggregate.
3.2. Sample preparation
The cement pastes of CM 1:3 with a water/cement (w/c) ratio of 0.5 was adopted. Cement
composites of 70.6 mm x 70.6 mm x 70.6 mm size were cast. These cubes are subjected to 28
days curing.
Table 1. Description of samples in this work
Sample
C-1
B-1
S-1
I-1
Description
Conventional cement mortar
Brush coated mortar specimen
Spray coated mortar specimen
Hydrophobic impregnated mortar
Figure 2. Methods of application adopted a) Brush coating, b) Spray coating and c) Hydrophobic
impregnation.
Three types of samples were cast by varying the method of application of the super
hydrophobic surface coat. Case I consist of samples, surface coated by brushing technique.
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Case II consist of samples, surface coated by spraying. Case III consist of samples, surface
treated by super hydrophobic impregnation [3]. The impregnated samples are prepared by
immersing the mortar cubes for 60s into the prepared super hydrophobic mixture.
3.3. Synthesis of Nano-GGBS and characterization
The GGBS was synthesized to nano-scale by Ball mill technique, which works on the
principle of impact and attrition. The wet milling of 20g of GGBS was done using ethanol for
a duration of 5 hours by employing 50 balls of tungsten carbide. This ground GGBS will
stimulate the adequate roughness required by the surface to produce super hydrophobicity.
3.3.1. X-Ray Fluorescence spectroscopy (XRF)
The X-Ray Fluorescence (XRF) spectroscopy is a technique for analyzing the elemental
composition of the material. The results are obtained from Central Electro Chemical Research
Institute (CECRI) at Karaikudy, Table. 2 indicates the mass percentage of metallic oxide
composition present in GGBS powder. From Fig. 3(a) it can be interpreted that CaO is the
major composition present in the GGBS. Also the elements present in this powder is similar
to the elemental composition of cement.
Table 2. XRF elemental analysis
Metal Oxide
Composition
CaO
83.3%
SiO2
6.6%
MnO2
6.4%
Fe2O3
3.6%
3.3.2. Fourier Transform Infra-Red spectroscopy (FTIR)
The FTIR is usually done to study the presence of chemical bonds present in the sample. The
results of the IR spectrum are plotted for %transmittance vs. wavenumber. The peak at
675.88cm-1 indicates the presence of silica or Si–O bond. The carbonate peak obtained at
910.46 cm-1indicates the presence of C–O stretching bond. Also the presence of C=O
bending bond or carboxylic bond was indicated by the peak value at 1477.62 cm-1.
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An Experimental Investigation on Superhydrophobic Coating Using Nano-GGBS on Cement Mortar
Figure 3 Characterization results of GGBS a) XRD results showing the elemental oxide content b)
FTIR image of GGBS indicating the presence of metallic oxides c) SEM image of ground GGBS
showing agglomeration of particle.
3.3.3. Scanning Electron Microscopy (SEM)
The Scanning Electron Microscopy has been done to investigate the topography of the
surface. The SEM image of GGBS indicates that all the particles are varying in size and are
agglomerated. Fig. 3(c) shows the SEM image of GGBS after ball milling captured at a
working distance of 10.6mm by applying 10.0kV with 6.00k magnification in a scale of
5.00µm. The SEM image of nano-ground GGBS also indicated agglomeration of particles
with size ranging around 529nm.
3.4. Preparation of super-hydrophobic surface coating
Initially the hydrophilic Isobutyltriethoxysilane was diluted in distilled water in the ratio of
1:25. This ratio for Isobutyltriethoxysilane was adopted based on its molecular ratio.
Meanwhile, 1g of nano-GGBS was added to this mixture. Inorder to uniformly disperse the
agglomerated nanoparticle into this silane solution, ultrasonication was done for about 30
min. Then the prepared mixture was left undisturbed for a period of 12 hours. Hydrolysis of
the mixture was initiated by heating the solution at 60°C for about 45 minutes. As a result of
hydrolysis, a highly reactive compound called silanol was formed by elimination of ethanol.
Then the prepared coating was permitted to cool for a while and applied evenly on all the
faces of the mortar surface following an adhesive coating. Epoxy resin was the adhesive used.
The coated substrates were allowed to dry in sunlight. After condensation, the silanol
compounds react with each other and gets converted into a compound called polysiloxane.
This component will induce super hydrophobicity on concrete surface. Thus the dual nature of
silane from hydrophilic state to hydrophobic state was exhibited using the above process.
3.5. Preparation of adhesive [30]
The adhesive is generally used for sticking the nano/micro particles to the coated surface for
longer life of the coating. The epoxy resin and hardener is a two-part system. It is an
extremely strong material that can be used as a sealant and an adhesive on concrete surfaces.
They are blended consistently in the ratio 10:1. One troublesome thing about this substance is
that it is very thick and viscous, which implies that it is hard to apply. Inorder to overcome
this, Ethyl alcohol was added to it as an epoxy thinner in the ratio of 5:1 and ultrasonicated
for 10 minutes. Then the prepared adhesive was applied uniformly on all the faces of the
specimen.
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Figure 4 General equation exhibiting the process of conversion of the hydrophilic silane to
hydrophobic nature by hydrolysis and subsequent condensation.
3.6. Measurement of hydrophobicity [34]
The degree of hydrophobicity is estimated in terms of water contact angle by using WCA
Goniometer. A dosage of 2.5µl of water droplet was dispensed by the needle of goniometer
over the coated and uncoated surface of cement paste and the contact angle is measured after
5s. Similarly, three trials are done for each type of sample. When the coated substrates are
tilted, the droplet rolls-off.
3.7. Water absorption test
Water absorption test was done affirming to ASTM C_642 13 [31]. Initially the mortar
specimens were dried absolutely to expel dampness by using Hot air oven for a duration of 24
hours. The samples were taken out from the oven and their initial weights are noted as W 0(g).
The samples were immersed into water not less than a period of 48 hours. The final weight of
the samples W1(g) was recorded after taking out the immersed samples from water. The rate
of water absorption is calculated by using the following expression.
Rate of water absorption =
x 100 %
(1)
3.8. Sorptivity test [8]
This test is done to record the capillary uptake of water as a function of time. The mortar
samples were sealed at its sides with epoxy resin to allow unidirectional uptake of water. The
top of the samples were secured with plastic sheet to avoid evaporation. The initial weight of
the resin coated mortar samples were measured. Then these samples were placed in a pan
upon supporting devices. The water level was maintained at 1-3mm above the support device.
Eventually, the weight readings were noted at interims as per ASTM C_1585 [32]. The water
uptake rate (I) is determined by the following expression.
Absorption, I =
mm
(2)
Where, ‘mt’ is the change in specimen mass (g); ‘a’ is the surface area of the specimen
(mm2); ‘d’ represents the density of water (g/mm3) and ‘I’ is the rate of vertical uptake or
sorptivity of water (mm).
3.9. Ultrasonic Pulse Velocity (UPV) test [9]
The UPV is a non-destructive test conducted to determine the defects in a sample. Initially
zero was set by placing the two electro-acoustical transducer together. Then a reference
velocity was set by using Quartz crystal whose travel speed of pulse velocity is known as
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An Experimental Investigation on Superhydrophobic Coating Using Nano-GGBS on Cement Mortar
25.4µs. The probes were placed on any two faces of the specimen and speed of the passed
ultrasonic pulse velocity was recorded from the digital display. The direct measurement
method was adopted, since it is more convenient for mortar cubes. The UPV test was done
confirming to Indian Standard IS: 13311 (Part 1) – 1992 [33].
4. RESULTS AND DISCUSSION
4.1. Measurement of hydrophobicity
Fig. 5 demonstrates the measurement of hydrophobicity by visual assessment. On placing
water droplets over a sample treated with spray coating without adhesive, the surface of the
substrate exhibited superhydrophobicity. Fig. 6 shows the water contact angle measured in
Goniometer apparatus for each method of application of super hydrophobic coating. From the
acquired results, it was revealed that the spray coating produced super hydrophobicity with a
contact angle of 152.2° due to the uniform distribution of nanoparticles on the concrete
surface. Also, the impregnated samples produced only 122.7° contact angle due to less
deposition of nanoparticles on the substrate. The brush coated samples exhibited near super
hydrophobic behavior with 146.3° contact angle.
Figure 5. Super-hydrophobicity of a spray coated sample without applying adhesive.
Figure 6 Water contact angle obtained for a) Brush coating b) Spray coating and c) Hydrophobic
impregnated specimen.
4.2. Water absorption test
The rate of penetration of water into the mortar specimens were tested and the result outcomes
are tabulated in Table. 3. From the graph shown in Fig. 7, it is deciphered that the
impregnated samples showed reduced water absorption comparing to other samples. The I-1
samples had a least of 1.09% of water absorption rate. On comparing the water absorbed by
conventional mortar specimens, the brush coated, spray coated and the impregnated
specimens absorbed only 17.1%, 14.9% and 9.3% respectively.
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Table 3 Water absorption test results
Sample
C-1
B-1
S-1
I-1
Dry
weight W0
(g)
750
747
752
776
785
793
785
783
791
806
798
805
Saturated
weight W1
(g)
838
835
840
792
802
807
799
796
805
815
808
812
Rate of
Absorption
(%)
11.74
11.79
11.71
2.07
2.17
1.77
1.79
1.67
1.77
1.12
1.26
0.87
Average (%)
11.75
2.01
1.75
1.09
4.3. Sorptivity test
The capillary uptake of water in uncoated and coated samples were measured at intervals like
60s, 5min, 10min, 20min, 30min, 1hr, 2hr, 3hr, 4hr, 5hr, 6hr, 1day, 2days and 3 days. The
results are plotted for rate of capillary uptake of water vs. square root of time in Fig. 8. It
could be inferred from the graph that the capillary uptake of water was greatly resisted by the
spray coated and impregnated specimens. Both S-1 and I-1 samples showed similar
performance till 6hrs, after which the I-1 samples resisted better than S-1 samples. The other
samples which were brushed and impregnated also showed reduced vertical water uptake than
conventional samples.
4.4. Ultrasonic Pulse Velocity (UPV) test
The Ultrasonic Pulse Velocity test is usually done to find the imperfections or pores in the
specimen by passing ultrasonic pulses through the two probes of the instrument. From Table.
4 it is perceived that the ultrasonic pulse velocity travels faster through coated specimens than
through the conventional mortar. This proves that the applied super hydrophobic coating
reduces the surface porosity of the specimens. Also among the three types of coating, the
samples subjected to hydrophobic impregnation showed excellently reduced surface porosity.
Table 4. UPV test results
Sample
C-1
B-1
S-1
I-1
Length
(xo) mm
Time
travel (µs)
70.6
70.6
70.6
70.6
70.6
70.6
70.6
70.6
70.6
70.6
70.6
70.6
21.6
20.4
25.5
18.3
17.2
18.1
15.6
16.4
16.3
13.9
13.3
14.3
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Sample
velocity, ʋ
(km/s)
3.27
3.46
2.76
3.85
4.10
3.90
4.52
4.30
4.33
5.08
5.31
4.94
Average
velocity, ʋs
(km/s)
3.17
3.95
4.38
5.11
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An Experimental Investigation on Superhydrophobic Coating Using Nano-GGBS on Cement Mortar
Water absorption
14
11.75
Absorption %
12
10
8
6
4.51
4
1.75
2
1.09
0
C-1
B-1
S-1
I-1
Figure 7 Graph representing the rate of water absorption of the samples after 48hrs of immersion in water.
Sorptivity
Water uptake, I (mm)
0.25
0.2
0.15
C-1
B-1
0.1
S-1
I-1
0.05
0
0
60
120
180
240
300
Time0.5
360
420
480
540
600
(√s)
Figure 8. Rate of capillary uptake of water plotted against square root of time.
Table 5. Methods of Fabrication and WCA reported in literatures
Author
Repellent Material
Ilaria Alfieri et
al
Fuoroalkyl-functional
water-borne oligosiloxane
Silane coupling agent
KH-570
Guo Li et al
Roughness
Material
SiO2 hybrid sols
TiO2
nanoparticles
Silica nanoparticles
Method
Ɵ
Ref.
Coating by
deposition
Organic film
coating
147° ±
3°
[14]
87.3°
[34]
Brush coating
127.1° ±
2.1°
[35]
Spray coating
144.2°
[36]
107°±
0.2°
[37]
129°
[38]
~125°
[39]
>145°
[40]
152.2°
Present
study
C. Esposito
Corcione et al
Silane & siloxane
M.U.M. Junaidi
et al
1H,1H,2H,2H
perfluorodecyltriethoxysilan
e
Rice husk ash
Chao Peng et al
Silane coupling agent
-
Sodium stearate
CaCO3 particles
Tyre rubber
Tyre rubber
Irene Izarra et al
Tetraethyl orthosilicate and
Methyltriethoxysilane
SiO2-CH3
submicron-sized
particles
Impregnated
for 30mins
Via
carbonation
Replacement
of sand
Cast in
impregnated
mould
Jeya Sheema et
al
Isobutyltriethoxysilane
GGBS particles
Spray coating
Shashi B. Atla
et al
Rosa Di Mundo
et al
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5. CONCLUSIONS
The superhydrophobic coating for cement composite surfaces was created effectively utilizing
GGBS powder and isobutyltriethoxysilane. The spray coated surfaces exhibited
superhydrophobic nature comparing with the other samples with a water contact angle of
152.2° and when tilted the droplets rolled off. Comparing to the conventional mortar the
coated mortar specimens showed up to 90% of reduced water absorption. All the coated
samples produced good resistance towards vertical uptake of water. Among them the
impregnated and spray coated samples were found to produce least capillary uptake of water.
A reduced surface porosity of the coated specimens was proved from the faster travelling
ultrasonic waves through these samples.
The overall performance of the impregnated samples are notably higher in water
absorption and ultrasonic pulse velocity tests with 1.09% and 5.11 km/s respectively, though
it had lesser contact angle of 122.7°. Since the depth of penetration of the silane coating was
greater in case of impregnated specimens, they produced enhanced results compared to other
surface treated specimens.
ACKNOWLEDGEMENT
I sincerely thank the Principal and Department of Civil Engineering at Mepco Schlenk
Engineering College for the support and guidance throughout this work.
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