Effect of MK on GGBS based GPCs VelTech Rajamane SRMU 29 Oct 2013 1155 pm 1
EFFECTS OF METAKAOLIN ON GGBS BASED GEOPOLYMER CONCRETES
Harsha Vardhan K.,1 Dhinesh M., Dr Jeyalakshmi R.
3, and Dr Rajamane N. P.
4
1MTech (Str) 3
rd Semester,
2 Scientific Officer, CACR, 3 Professor, Department of Chemistry,
4 Head, CACR, SRM University, Kattankulathur, 603203, India
SYNOPSIS
Geopolymer Concretes (GPCs) have potential to become alternate to Portland
cement based concretes. GGBS based GPCs produce generally high strengths even when
they are cured at ambient conditions. Metakaolin (MK) is clay based pure alumino-silicate
and consists of mostly silica and alumina. Hence, MK is reported to produce pure
geopolymers. Effect of addition of MK to GGBS based GPCs are discussed in this paper.
1.0 INTRODUCTION
The development of new binders from alumino silicate sources, as an alternative to
Ordinary Portland Cement (OPC), by alkaline activation, is the current interest in various
R&D related activities in engineering laboratories. This paper describes experimental work
on use of Granulated Blast Furnace Slag (GGBS) and Metakaolin as active fillers in the
making of geopolymers. Alkali-activated metakaolin (AAMK) belongs to prospective
materials in the field of Civil Engineering. Metakaolin is an alumino-silicate which can form
pure geopolymer. The most common alkaline liquid used in geopolymerisation is a
combination of sodium hydroxide (NaOH) or potassium hydroxide (KOH) and sodium
silicate or potassium silicate
Geopolymers are members of the family of inorganic polymers. The chemical
composition of the geopolymer material is similar to natural zeolitic materials, but the
microstructure is amorphous instead of crystalline. The polymerization process involves a
substantially fast chemical reaction under alkaline condition on Si-Al minerals that results in
a three dimensional polymeric chain and ring structure consisting of Si-O-Al-O bonds. The
reactions in geopolymerisation can be separated into three main mechanistic steps, i.e.
dissolution/hydrolysis, restructuring, and polycondensation /gelation. These three
mechanisms may occur concomitantly, and are reversible to some extent. The kinetics of
each step vary depending on the type of aluminosilicate solid, the solid to solution ratio, the
concentration of silicate, alkali, water content, and the reaction condition.
The ingredients of GPCs can be broadly divided into (i) geopolymeric source
materials (ii) alkali activators, and (iii) filler materials. The geopolymeric source materials
are aluminosilicate source materials i.e. material containing SiO2 & Al2O3. The GSMs used
in the work are GGBS and Metakaolin. Activator solution is prepared by mixing the
commercially available Sodium Hydroxide solution (Caustic Lye), Sodium Silicate solution
(Water Glass), and Distilled Water to obtain desired oxide composition. The filler materials
used for the experiment are normal fine aggregate and coarse aggregate which are also used
for ordinary cement concrete.
Effect of MK on GGBS based GPCs VelTech Rajamane SRMU 29 Oct 2013 1155 pm 2
Unlike ordinary Portland/pozzolanic cements, geopolymers do not form
calciumsilicate-hydrates (CSHs) for matrix formation and strength, but utilize the
polycondensation of silica and alumina precursors and a high alkali content to attain
structural strength. It may be noted here that Geopolymer is a relatively new binder having
potential to use in production of concretes for any practical application in place of
conventional Portland based concretes [Rajamane, 2005-2012]. Important publications on
Geopolymer Concrete Technology are listed in Appendix A of this paper. Apart from the
term ‘Geopolymer Concrete’, many other names are used in the literature to describe the
same or similar material as listed in Appendix B of this paper [Rajamane, 2013]
3.0 GEOPOLYMERIC SOURCE MATERIALS (GSMs)
(a) Metakaolinite or Metakaolin (MK): It is obtained from the calcination of kaolinitic clay
at temperatures ranging from 500-750 ᴼC. The further calcination of kaolinite at higher
temperatures leads to the formation of more ordered crystalline phases, such as spinnel,
mullite and cristobalite. It is suggested that firing kaolinite at lower temperatures (< 500 ᴼC)
does not give sufficient energy to break the crystalline structure of kaolinite. As a result,
amorphous metakaolinite is not formed. However, calcination at higher temperatures, i.e.
higher than a threshold temperature turns the metastable phase, metakaolinite, into more
ordered crystalline phases, which are non-reactive upon alkali-activation. The high
amorphicity of metakaolinite leads to the high reactivity when it is activated in alkali
solutions. MK has the smallest particle size in comparison to FA or GGBS. The fine and
irregular particle shape of MK often mean that MK generally requires more solution for
wetting and reaction to take place appropriately.
(b) Granulated Blast Furnace Slag (GGBS) : Blast furnace slag is formed in processes
such as pig iron manufacture from iron ore, combustion residue of coke, and fluxes such as
limestone or serpentine and other materials. If the molten slag is fast-cooled by high-pressure
water, a vitreous Ca–Al–Mg silicate fine grain glass is formed. Blast furnace slag is a non-
metallic by-product. It consists primarily of silicates, aluminosilicates, and calcium-
aluminosilicates. There are different types of slag products depending on the methods used to
cool the molten slag, namely air-cooled blast furnace slag (ACBFS), expanded or foamed
slag, pelletized slag, and granulated blast furnace slag (GGBS). Only GGBS is used as a
replacement material for OPC. GGBS has also been used to synthesize alkali-activated
cement and geopolymers. The process of cooling and solidification of molten slag results in
glassy-state materials, which take the form of frit-like fragments. Before being used in
cement or geopolymer application, GGBS is usually crushed, and milled to a finer size. The
GGBS consists mainly of calcium aluminosilicate glass with crystal inclusions of larnite and
melilite.
3.0 SCOPE AND OBJECTIVES OF PRESENT WORK
Effect of MK on GGBS based GPCs VelTech Rajamane SRMU 29 Oct 2013 1155 pm 3
The study presented here aims to use MK and GGBS material for production of
structurally useful geopolymer concretes through identification of suitable Alkaline
Activator Solution (AAS) system for initiating geopolymerisation reactions.
The introduction of new products in the construction industry is controlled by the
understandably conservative nature of the engineering profession and the need to meet
existing industry specifications. The scope of present work is to understand the chemistry and
structural characteristics of Metakaolin and GGBS based geopolymers. Key issues needed to
be addressed in the development of practical applications of Geopolymer Technology are:
i. Absence of GPC mix formulation guidelines.
ii. Practical constraints (e.g. controlling workability, setting time and strength
development rate of GPCs.
iii. Uncertainty over long-term performance of GPCs
iv. Urgent need to identify appropriate test methods and limits to control
properties but avoid unacceptably high rates of noncompliance in GPCs
3.0 MATERIALS USED IN EXPERIMENTAL WORKS (Tables 1 to 4)
The locally available river sand was used as fine aggregate in the present
investigation. The sand used conforms to grading zone II of IS 383: 1970. The Specific
Gravity and Fineness Modulus of sand were 2.76 and 2.49 respectively. Sand is sieved
through IS 4.75 mm Sieve.
Crushed angular granite metal of 10 mm size from local quarry was used as Coarse
Aggregate (CA). The cleaned coarse aggregate was tested for properties such as specific
gravity. The Specific Gravity of CA is 2.75
Physical and chemical properties of GGBS used are in conformation with IS: 12089-
1987. MK is whitish in colour and it is a manufactured amorphous alumino-silicate.
The Alkaline activator Solution (AAS) was prepared by mixing the commercially
available Sodium Hydroxide Solution (Caustic Lye), Sodium Silicate Solution (Water Glass),
and Distilled Water (DW) in the required proportions.
4.0 PREPARATION OF TEST SPECIMENS (Figs 1 to 4)
The fresh mix was prepared by hand mixing as the quantity used for each batch of
mix was small The use of trowel was sufficient to get a uniform mix as the mix had good
cohesiveness and workable. The fresh mix was poured into plastic cylindrical moulds in three
layers and then kept on vibrating table for 5 minutes to ensure proper compaction. The
moulds are kept for 24 hrs at ambient condition and then demoulded by cutting the plastic
moulds. The demoulded specimens are kept for further curing by storing at ambient
condition. Specimens are tested after 1 day, 7 and 28 days of curing period.
5.0 DISCUSSION OF TEST RESULTS (TABLE 5)
Effect of MK on GGBS based GPCs VelTech Rajamane SRMU 29 Oct 2013 1155 pm 4
(i) GPC mixes with 100% GGBS as GSM can be demoulded after 24 hours of casting.
The compressive strength at 1 day is 23.2 MPa for AAS/GSM ratio of 0.55 which
increases to 33.0 MPa at 7 days and to 39 MPa at the end of 28 days.
(ii) When the AAS/GSM ratio is increased to 0.60, there is only very marginal increase of
1 day strength as compared to GPC with AAS/GSM ratio of 0.55. But, for 7 days and
28 days strength for AAS/GSM ratio of 0.60 was 37.4 MPa and 47 MPa respectively
which is about 10% more than that of GPC with 0.55. Thus increased quantity of
AAS generates more geopolymeric reactions and thus increases the mechanism of
GPC.
(iii)When 25% of GGBS in GPC was replaced by MK, at AAS/GSM ratios of both 0.55
& 0.60, there was high retardation of setting and thereby strength development. This
resulted in postponement of the demoulding operation to 3rd
day. However, the
strength recorded was very low, the actual value being about 1.5 MPa only for 4th
day. Even after 14 days of curing period, the strength increase was not substantial.
The strength recorded was only about 2.5 MPa.
6.0 CONCLUDING REMARKS
The test data show that addition of MK affects very adversely the strength
development in GGBS based GPCs. This may be due to the high temperature required by
MK to initiate chemical reactions. Presence of MK seem to affect the geopolymerisation of
GGBS also since the strengths of MK containing GPCs were very low in spite of presence of
as much as 75% of GGBS in GSM of the mix. Thus, careful formulations of GPC is
necessary so that GPCs perform similar and if possible better than conventional concretes in
terms of strength level achieved and its rate of development, beside time required for
demoulding.
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Effect of MK on GGBS based GPCs VelTech Rajamane SRMU 29 Oct 2013 1155 pm 8
Table 1 Physical Properties of MK & GGBS
Property Metakaolin (MK) GGBS
Specific Gravity 2.52 2.89
Physical Form Powder Powder
Colour Off-White(Light Pink) Light Grey
Fineness (m2/kg) 15000 (BET) 425
BET 15M2/gram NA
D10 <2.0μm NA
D50 <4.5μm NA
D90 <25μm NA
Bulk Density (kg/m3) NA 1360
Table 2 Chemical Properties of MK & GGBS
Chemical Composition Metakaolin (MK) (% Wt.) GGBS (% Wt.)
SiO2 51-53 43.4
Al2O3 42-44 12.5
Fe2O3 <2.20 0.3
TiO2 <3.0 NA
SO4 <0.5 NA
P2O5 <0.20 NA
CaO <0.20 40.3
MgO <0.10 1.5
Na2O <0.05 0.9
K2O <0.40 0.6
L.O.I. <0.50 2.1
Table 3 Properties of Caustic Lye
% NaOH content 50 % (by mass)
Density 1.6 kg/l
Nature Hygroscopic
Table 4 Properties of Sodium Silicate
% Na2O 12
% SiO2 25
% H2O -
PH 12.49
Density 1490 kg/m3
Nature Transparent Viscous Liquid
Effect of MK on GGBS based GPCs VelTech Rajamane SRMU 29 Oct 2013 1155 pm 9
Table 5 Details of GPC mixes and experimental data
Mix No 1 2 3 4
Type GPCG GPCG GPCMK GPCMK
ID G 0.55 G 0.60
GK
0.55
GK
0.60
GSM MK % 0 0 25 25
GGBS % 100 100 75 75
AAS Type A mixture of SHS and SSS
SiO2/Na2O w/w 0.512 0.512 0.512 0.512
Na2O/GSM
% 5.64 6.15 5.64 6.15
SiO2/GSM % 2.89 3.15 2.89 3.15
AAS/GSM w/w w/w 0.55 0.6 0.55 0.6
Quantity MK kg 0 0 0.25 0.25
per batch GGBS kg 3 3 2.75 2.75
AAS kg 1.65 1.8 1.65 1.8
Sand kg 4.5 4.5 4.5 4.5
CA kg 7.5 7.5 7.5 7.5
Fresh Slump mm 20 to 30
mix Nature Cohesive mix, no bleeding
Density kg/m3 1726 1735 1715 1705
Specimen Dia mm 75 75 75 75
size High mm 150 150 150 150
Compressive 1 Day MPa 23.2 24.5 CND CND
Strength 7 Day MPa 33.0 37.4 1.5 1.9
fc28d 14 Day MPa 35.0 40.0 2.3 2.5
28 Day MPa 38.9 46.9 2.6 2.7
Change due to GSM/AAS % - 20.3 NA NA
Change in fc28d due to MK % - - -93 -94
fc28d of GPCG / GPCMK NA NA 7 6
Note: NA=Not Applicable, CND=Could Not be Demoulded
SHS = Sodium Hydroxide Solution, SSS = Sodium Silicate Solution
Effect of MK on GGBS based GPCs VelTech Rajamane SRMU 29 Oct 2013 1155 pm 10
Figure 1 Fresh Geopolymer Concrete Figure 4.2 Compaction on Vibrating Table
Figure 3 Compression Testing Figure 4 Tested Sample Specimen (Typical)
Effect of MK on GGBS based GPCs VelTech Rajamane SRMU 29 Oct 2013 1155 pm 11
Appendix A
Important publications on Geopolymer Concrete Technology
[1] Davidovits J., [2011]. “Geopolymer Chemistry and Applications”, 3rd Edition, Institut
Géopolymère, Saint-Quentin, France, 632 pages.
[2] Hardjito, D. and Rangan, B. V., [2005]. “Development and Properties of Low Calcium
Fly Ash Based Geopolymer Concrete”, Research Report GC1, Faculty of Engineering,
Curtin University of Technology.
[3] Provis J L and J S J van Deventer (Ed). [2009]. “Geopolymers: Structures, processing,
properties and industrial applications,” ISBN-13: 978 1 84569 449 4
June, 464 pages.
[4] Shi Caijun, Della Roy, Pavel Krivenko, [2006]. “Alkali-Activated Cements and
Concretes”, Taylor & Francis, 392 pages.
[5] Sindhunata [2006]. “A conceptual model of geopolymerisation”. PhD Thesis of
Chemical & Biomolecular Engineering Department. Melbourne: The University of
Melbourne
[6] Sumajouw, M.D.J. and Rangan, B.V. [2006]. “Low-Calcium Fly Ash-Based
Geopolymer Concrete: Reinforced Beams and Columns”, Research Report GC3, Faculty
of Engineering, Curtin University of Technology, Perth
[7] Torgal Fernando Pacheco, Joa˜o Castro-Gomes, Said Jalali [2008a]. “Review Alkali-
activated binders: A review Part 1. Historical background, terminology, reaction
mechanisms and hydration products”, Construction and Building Materials, Vol 22, pp
1305–1314.
[8] Torgal Fernando Pacheco, Joa˜o Castro-Gomes, Said Jalali [2008b]. “Review Alkali-
activated binders: A review Part 2. About materials and binders manufacture”,
Construction and Building Materials, Vol 22, pp 1315–1322
[9] Wallah, S.E. and Rangan, B.V. (2006). Low-Calcium fly ash-based geopolymer concrete:
Long-term properties. Curtin University of Technology. Research Report GC 2, 107 p
Effect of MK on GGBS based GPCs VelTech Rajamane SRMU 29 Oct 2013 1155 pm 12
Appendix B
DIFFERENT NOMENCLATURES OF GEOPOLYMERS
Though the term, ‘geopolymer’ has become now more common to represent the synthetic
alkali aluminosilicate material (produced by reaction of a solid aluminosilicate with a highly
concentrated aqueous alkali hydroxide or silicate solution), it is worthwhile to note that the
following nomenclatures are also reported to describe similar materials:
(i) Inorganic polymer [van Wazer, 1970; Barbosa, 2003]
(ii) Low-temperature aluminosilicate glass [Rahier, 1996a, 1996b & 1997]
(iii) Alkali-activated cement [Roy, 1999; Palomo, 2003]
(iv) Alkali-activated binders [Torgal, 2008a, 2008b]
(v) Geocement [Krivenko, 1994]
(vi) Alkali-bonded ceramic [Mallicoat, 2005]
(vii) Inorganic polymer concrete [Sofi, 2007a and 2007b; Duxson, 2007b]
(viii) Hydroceramic [Bao, 2005]
(ix) Mineral Polymers[Davidovits, 1980]
(x) Inorganic polymer glasses [Rahier, 2003]
(xi) Alkali ash material [Rostami, 2003]
(xii) Soil cements [Glukhovsky, 1965]
(xiii) Alkali Activated Aluminosilicate [Provis and Deventer, 2009]
(xiv) Chemically Bonded Ceramics [Allahverdi Ali & František Škvára, 2005]
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