Effect of MK on GGBS based GPCs VelTech Rajamane SRMU 29 Oct 2013 1155 pm 1 EFFECTS OF METAKAOLIN ON...

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.


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


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)


(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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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


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


Figure 1 Fresh Geopolymer Concrete Figure 4.2 Compaction on Vibrating Table

Figure 3 Compression Testing Figure 4 Tested Sample Specimen (Typical)


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


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]

Effect of MK on GGBS based GPCs VelTech Rajamane SRMU 29 Oct 2013 1155 pm 1 EFFECTS OF METAKAOLIN ON...

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