AN EXPERIMENTAL INVESTIGATION ON SUPERHYDROPHOBIC COATING USING NANO-GGBS ON CEMENT … · 2019-05-04 · for cement mortar. The super hydrophobic coating is prepared by sonicating

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International Journal of Civil Engineering and Technology (IJCIET)

Volume 10, Issue 03, March 2019, pp. 3137–3148, Article ID: IJCIET_10_03_316

Available online at http://www.iaeme.com/ijmet/issues.asp?JType=IJCIET&VType=10&IType=3

ISSN Print: 0976-6308 and ISSN Online: 0976-6316

© IAEME Publication Scopus Indexed

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 Nano-

scaled 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(3), 2019, pp. 3137–3148.

http://www.iaeme.com/IJCIET/issues.asp?JType=IJCIET&VType=10&IType=3

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

Jeya Sheema J and Prabavathy S


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 water-

borne chloride (Cl-) and sulphate (SO4

2-) 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

An Experimental Investigation on Superhydrophobic Coating Using Nano-GGBS on Cement Mortar


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 Description

C-1 Conventional cement mortar

B-1 Brush coated mortar specimen

S-1 Spray coated mortar specimen

I-1 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.



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 CaO SiO2 MnO2 Fe2O3

Composition 83.3% 6.6% 6.4% 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-1

indicates 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

.



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.



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 W0(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/mm

3) 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



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.



Table 3 Water absorption test results

Sample

Dry

weight W0

(g)

Saturated

weight W1

(g)

Rate of

Absorption

(%)

Average (%)

C-1

750 838 11.74

11.75 747 835 11.79

752 840 11.71

B-1

776 792 2.07

2.01 785 802 2.17

793 807 1.77

S-1

785 799 1.79

1.75 783 796 1.67

791 805 1.77

I-1

806 815 1.12

1.09 798 808 1.26

805 812 0.87

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 Length

(xo) mm

Time

travel (µs)

Sample

velocity, ʋ

(km/s)

Average

velocity, ʋs

(km/s)

C-1

70.6 21.6 3.27

3.17 70.6 20.4 3.46

70.6 25.5 2.76

B-1

70.6 18.3 3.85

3.95 70.6 17.2 4.10

70.6 18.1 3.90

S-1

70.6 15.6 4.52

4.38 70.6 16.4 4.30

70.6 16.3 4.33

I-1

70.6 13.9 5.08

5.11 70.6 13.3 5.31

70.6 14.3 4.94



Figure 7 Graph representing the rate of water absorption of the samples after 48hrs of immersion in water.

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 Roughness

Material Method Ɵ

Ref.

Ilaria Alfieri et

al

Fuoroalkyl-functional

water-borne oligosiloxane SiO2 hybrid sols

Coating by

deposition

147° ±

3° [14]

Guo Li et al Silane coupling agent

KH-570

TiO2

nanoparticles

Organic film

coating 87.3° [34]

C. Esposito

Corcione et al Silane & siloxane

Silica nano-

particles Brush coating

127.1° ±

2.1° [35]

M.U.M. Junaidi

et al

1H,1H,2H,2H

perfluorodecyltriethoxysilan

e

Rice husk ash Spray coating 144.2° [36]

Chao Peng et al Silane coupling agent - Impregnated

for 30mins

107°±

0.2° [37]

Shashi B. Atla

et al Sodium stearate CaCO3 particles

Via

carbonation 129° [38]

Rosa Di Mundo

et al Tyre rubber Tyre rubber

Replacement

of sand ~125° [39]

Irene Izarra et al Tetraethyl orthosilicate and

Methyltriethoxysilane

SiO2-CH3

submicron-sized

particles

Cast in

impregnated

mould

>145° [40]

Jeya Sheema et

al Isobutyltriethoxysilane GGBS particles Spray coating 152.2°

Present

study

11.75

4.51

1.75 1.09

0

2

4

6

8

10

12

14

C-1 B-1 S-1 I-1

Ab

sorp

tio

n %

Water absorption

0

0.05

0.1

0.15

0.2

0.25

0 60 120 180 240 300 360 420 480 540 600

Wa

ter

up

tak

e, I

(m

m)

Time0.5 (√s)

Sorptivity

C-1

B-1

S-1

I-1



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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Documents

AN EXPERIMENTAL INVESTIGATION ON SUPERHYDROPHOBIC COATING USING NANO-GGBS ON CEMENT … · 2019-05-04 · for cement mortar. The super hydrophobic coating is prepared by sonicating