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Effect of Fly Ash/Alkaline Activator Ratio and Sodium Silicate/NaOH Ratio on

Fly Ash Geopolymer Coating Strength

Article  in  Key Engineering Materials · January 2014

DOI: 10.4028/www.scientific.net/KEM.594-595.146

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Key Engineering Materials Vols. 594-595 (2014) pp 146-150
Online available since 2013/Dec/05 at www.scientific.net
© (2014) Trans Tech Publications, Switzerland
doi:10.4028/www.scientific.net/KEM.594-595.146

Effect of Fly Ash/Alkaline Activator Ratio and Sodium Silicate/NaOH

Ratio on Fly Ash Geopolymer Coating Strength

J. Liyana1,a, A.M. Mustafa Al Bakri2,b, H. Kamarudin3,c, C.M. Ruzaidi4,d

and A.R. Azura5,e
1,2,3,4
Centre of Excellence Geopolymer & Green Technology (CEGeoGTech), School of Materials
Engineering, Universiti Malaysia Perlis (UniMAP), 01000, P.O. Box, D/A Pejabat Pos Besar,
Kangar, Perlis, Malaysia
5
School of Materials and Minerals Resources Engineering, Universiti Sains Malaysia, Malaysia
a
liyanajamaludin@unimap.edu.my, bmustafa_albakri@unimap.edu.my, cvc@unimap.edu.my,
d
ruzaidi@unimap.edu.my and eazura@eng.usm.my

Keywords: geopolymer, ratio, fly ash, coating, strength.

Abstract Fly ash geopolymer coating material potential used to protect surface used in exposure
conditions. Ratio of fly ash/alkaline activator and Na2SiO3/NaOH play important parameter on
determining the best flexural strength of geopolymer coating material. Fly ash and alkali activator
(Al2O3/Na2SiO3) were mixed with the solids-to-liquid ratios in range of 1.0-3.0 and different ratios
of Na2SiO3/NaOH (1.0-3.0) to prepare geopolymer coating material at constant NaOH
concentration of 10 M. Effect of fly ash/alkaline activator ratio and Na2SiO3/NaOH on geopolymer
coating was determined with respect to the highest flexural strength of the 1200ºC sintering
temperature of geopolymer coating substrates. The results concluded that the highest strength for fly
ash geopolymer coating material is achieved 42 MPa when the solid/liquid ratio is 2.0 and the
Na SiO /NaOH ratio is 2.5.

Introduction

Surface deteriorations become major problem for wear of ceramic products. In the pottery industry,
lead glazes are still implemented to color, decorate and smooth the surface of ceramic products. As
long as the clay and glazes are compatible and these glazes are properly fired at a high enough
temperature for an appropriate amount of time, the lead is not likely to leach through the surface.
However, with constant use and scrubbing, ceramic products can wear down over time, and may
cause lead to leach through. In order to curb this problem, geopolymeric application is used to
replace traditional method of ceramic glaze processing by possessing several better characteristics.

Geopolymers are formed when alumino-silicates dissolve in a strong alkaline solution, reorganize,
and precipitate in a hardened state [1,2]. The term “geopolymer” was coined by Davidovits during
his research into inorganic-polymer technologies for industrial applications [3]. Geopolymer is a
material that exhibits many exceptional properties such as high compressive strength, low shrinkage
plus acid and fire resistance [3]. Geopolymer give the potentional possibilities to prepare inorganic
bonds and building materials from the waste as slag, fly ash, kaolinitic substances, etc. [4]. Fly ash
is a finely solid waste generated from coal-fired thermal power stations during the combustion of
coal. At present, about 80% of total power generation in the world based on thermal power plants
which consume CO2 to atmosphere which effect the greenhouse emissions. Due to environmental
concern, new ways of utilizing fly ash being explored in order to protect the environment and
provide useful ways for its utilization and disposal.
This paper summarizes the effect of solid-to-liquid ratio and Na2SiO3/NaOH ratio on the
flexural strength of geopolymer coating substrates at constant sintering temperature (1200ºC).

All rights reserved. No part of contents of this paper may be reproduced or transmitted in any form or by any means without the written permission of TTP,
www.ttp.net. (ID: 175.145.188.10, Universiti Malaysia Perlis (UniMAP), Kangar, Malaysia-26/03/14,04:35:40)
 Key Engineering Materials Vols. 594-595 147

Materials and Method

Raw Materials. Fly ash used as aluminosilicate source to produce geopolymer coating material by
using various geopolymer compositions sodium hydroxide added to sodium aluminate or sodium
silicate solutions. Fly ash is removed from the combustion gases by the dust collection system,
either mechanically or by using electrostatic precipitators, before they are discharged to the
atmosphere. The fly ash was supplied by YTL Cement Corporation, Malaysia. The chemical
composition of the fly ash was determined by X-ray Fluorescence (XRF) and listed in Table 1. The
composition analysis indicated that Al2O3, SiO2 and Fe2O3 content was higher than 70% which
conforming that the fly of Class F type according to ASTM C618-12a.

Table 1: Chemical compositions of fly ash

_______________________________________________
Chemical wt (%)
_______________________________________________
Al2O3 15.4
SiO2 35.7
CaO 20.8
Fe2O3 19.91
SO3 3.55
K 2O 1.85
LOI 0.2
______________________________________________

Mix Design. The ratio of fly ash/alkaline activator were synthesized by four different ratios which
is 1.0, 1.5, 2.0 and 2.5 and ratio of Na2SiO3/NaOH solution which is 1.0, 1.5, 2.0 and 2.5. The
NaOH solution was prepared by dissolving sodium hydroxide pellets in deionised water, the
concentration of the NaOH was kept constant at 10 M [5]. The sodium silicate was added to
enhance the process of geopolymerization [6]. Geopolymer coating materials were activate by
adding the alkaline activator gradually with several ratios into fly ash in process at ambient
temperature. Table 2 shows mix design formulations of molar compositions to obtain geopolymer
fly ash pastes coating material.

Table 2: Mix Design Formulation of Geopolymer Coating Materials

Fly ash/alkaline activator Sodium Silicate/ Fly ash Sodium Silicate NaOH (g)
(FA/AA) NaOH (g) (g)

FAAa-1.0 SSa-1.0 421.88 210.94 210.94

FAAa-1.0 SSa-1.5 421.88 253.13 168.75
FAAa-1.0 SSa-2.0 421.88 281.25 140.63
FAAb-1.0 SSa-2.5 421.88 301.34 120.54
_____________________________________________________________________________________________
FAAb-1.5 SSb-1.0 506.25 168.75 168.75
FAAb-1.5 SSb-1.5 506.25 202.50 135.00
FAAb-1.5 SSb-2.0 506.25 225.00 112.50
FAAb-1.5 SSb-2.5 506.25 241.07 96.43
_____________________________________________________________________________________________
FAAc-2.0 SSc-1.0 562.50 140.63 140.63
FAAc-2.0 SSc-1.5 562.50 168.75 112.50
FAAc-2.0 SSc-2.0 562.50 187.50 93.75
FAAc-2.0 SSc-2.5 562.50 200.89 80.36
_____________________________________________________________________________________________
FAAd-2.5 SSd-1.0 602.68 120.54 120.54
FAAd-2.5 SSd-1.5 602.68 144.64 96.43
FAAd-2.5 SSd-2.0 602.68 160.71 80.36
FAAd-2.5 SSd-2.5 602.68 172.19 68.88
148 Advanced Materials Engineering and Technology II

Sample Preparation. Geopolymer coating material was prepared by mixing alkaline activator with
fly ash powder. The mixture was applied at ceramic substrates by brushing method. After coating,
samples were placed at room temperature for drying process for 24 hours before sintering in the
furnace at 1200 °C for 3 hours soaking time with heating and cooling rates at 5°C/min to evaluate
the performance of thermal properties [7].

Testing and Analyzing. The characterization of this material was analyzed by using X-ray
Flourescence (XRF). The scanning electron microscope (SEM) with JSM-6460L model (JEOL) was
performed to reveal the microstructure of the various degrees of reaction at different solid-to-liquid
ratios of geopolymer coating material. The flexural strength was measured according to ASTM C
1161 by using the Instron machine series 5569 Mechanical Tester. A minimum of three specimens
were tested to evaluate the strength gain for the specimens

Results and Discussion

Effect of fly ash/alkaline activator ratios and on flexural strength.

Figure 4.1 shows the influence of fly ash/alkaline activator ratios on mean flexural strength values
for the ratios 1.0, 1.5, 2.0 and 2.5 after sintering at 1200 °C. It is summarized that highest flexural
strength was obtained when the ratios of fly ash/alkaline activator and Na2SiO3/NaOH were 2.0 and
2.5 with compressive strength 43.5 MPa. Fly ash/Alkaline Activator ratio and Na SiO /NaOH ratio
influence the workability of the mixture. Less workable mixture causes difficulty in flexural testing
where failure in providing good flexural properties may severely reduce the flexural strength of the
geopolymer paste [8]. An increasing in Na O concentration will improve the solubility of the
alumino-silicates source.The results proved by research from Mustafa et. al [9,10] that the optimum
mix design for geopolymer material of fly ash.

Flexural Strength versus Solid Liquid/Alkaline Activator Ratio

60

50
Flexural Strength (MPa)

40
Na2SiO3/NaOH-1.0

30 Na2SiO3/NaOH-1.5

Na2SiO3/NaOH-2.0
20
Na2SiO3/NaOH-2.5
10

0
1 1,5 2 2,5
Solid liquid/alkaline activator ratio

Fig.1. Flexural Strength of Mix Design Proportion

 Key Engineering Materials Vols. 594-595 149

Stereo Microscopy Analysis.

The coating surface microstructures studied using stereo microscope show the presence of
difference phases and crystallize structure of coating materials after sintering at temperature
1200 °C. Fig. 2 shows the microstructure of geopolymer coating at solid/liquid ratio with different
ratio at constant ratio Na SiO /NaOH at 2.5. Fig. 2 (a) shows the morphology of the coating reveals
regions of fully molten ceramic particles [11]. The geopolymer coating showed the existence of
pores as shown in Fig. 2(d). The porosity sizes were in the range of 5-20 µm. Figure 2 (d) shows an
increase in porosity would be expected to lead of reducing flexural strength. No sizable cracks are
noted on the coating surface. Fig 2(c) shows crystalline structure after sintering with optimum ratio
solid/liquid 2.0.

Fig. 2.Stereo micrograph for geopolymer coating after sintering 1200 °C at different FA/AA ratios
(a) 1.0; (b) 1.5; (c) 2.0 and; (d) 2.5.

Conclusion

The ratio of the alkaline activator/Fly ash, found to have a great influence on the flexural strength of
the fly ash-based geopolymer coating material. It can be concluded the alkaline activator/fly ash
ratio of 2.0 and Na2Si03/NaOH ratio of 2.5 has the optimum amount of alkaline liquid, which could
activate the fly ash in highest rate of geopolymerization comparing to other ratio. There was less
research made on the effect of solid/liquid ratio and Na SiO /NaOH ratio on the geopolymer
synthesis for coating implementations.
150 Advanced Materials Engineering and Technology II

References

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[2] J. Davidovits, Geopolymer: Inorganic polymeric new materials.: Journal of Thermal Analysis
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 Advanced Materials Engineering and Technology II
10.4028/www.scientific.net/KEM.594-595

Effect of Fly Ash/Alkaline Activator Ratio and Sodium Silicate/NaOH Ratio on Fly Ash Geopolymer
Coating Strength
10.4028/www.scientific.net/KEM.594-595.146

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