geopolymers for kaolin

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Journal of Asian Ceramic Societies 3 (2015) 130–138

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Effect of the rate of calcination of kaolin on the properties of metakaolin-based geopolymers

B.B. Kenne Diffo a , b , A. Elimbi a ,∗, M. Cyr b , J. Dika Manga c , H. Tchakoute Kouamo aa Université de Yaoundé 1, Laboratoire de Chimie Inorganique Appliquée,Faculté des Sciences, B.P. 812, Yaoundé, Cameroonb Université de Toulouse, Laboratoire Matériaux et Durabilité des Constructions, INSA/UPS Génie Civil, 31077 Toulouse CEDEX 04, Francec Université de Douala, Laboratoire de Chimie Bio-Inorganique, Analytique et Structurale, Faculté des Sciences, B.P. 24157, Douala, Cameroon

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Article history:Received 7 September 2014Received in revised form18 November 2014Accepted 2 December 2014Available online 20 December 2014

Keywords:RateCalcinationResidual kaolinMetakaolinSetting timeCompressive strength

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Kaolin samples of the same mass were treated at 700 ◦ Cfor the same duration of 30min by varying the rateof calcination (1, 2.5, 5, 10, 15 and 20 ◦ C/min) in order to obtain metakaolins which were used to producegeopolymers. Depending on the nature of each type of material, kaolin, metakaolins and geopolymerswere characterized using thermal analysis, chemical analysis, XRD, FTIR, particle size distribution, specicsurface area, bulk density, setting time and compressive strength. FTIR and XRD analyses showed thatmetakaolins except at 1 ◦ C/min contained residual kaolinite whose quantity increased with the rate of cal-cination of kaolin and which inuenced the characteristics of geopolymers. Thus as the rate of calcinationof kaolin increased, the setting time increased (226 min (rate of 1 ◦ C/min)–773 min (rate of 20 ◦ C/min))while the compressive strength reduced (49.4 MPa (rate of 1 ◦ C/min)–20.8 MPa (rate of 20 ◦ C/min)). Fromthe obtained results the production of geopolymers having high compressive strength along with lowsetting time requires that the calcination of kaolin be carried out ata low rate.

© 2014 The Ceramic Society of Japan and the Korean Ceramic Society. Production and hosting byElsevier B.V. All rights reserved.

1. Introduction

The term geopolymer refers to inorganic aluminosilicatepolymers. These materials nd applications in areas such as con-structionand civil engineering [1–3] , encapsulationof certain toxicwaste [4–7] , removal of certain heavy metal cations from aque-ous solutions [6–8] or the development of biomaterials [9] . Theseinorganic polymers are generallyobtainedby polymerizationreac-tion between aluminosilicate and strongly basic alkaline solution[10] . Aluminosilicate raw materials commonly used for the syn-thesis of geopolymers are y ash, blast furnace slag, volcanic ashor metakaolin [1,4,11,12] . The variability of chemical composi-tion of y ash, blast furnace slag or volcanic ash usually leadsto geopolymers whose physical and mechanical properties varyfromone aluminosilicate raw material to another [7,11] . Regardingmetakaolin, the characteristics of resulting inorganic aluminosili-cate polymers depend on the conditions of calcination of kaolin

∗ Corresponding author. Tel.: +237 677 612 623; fax: +237 222 234 496.E-mail address: [email protected] (A. Elimbi).Peerreview underresponsibility of TheCeramic Society of Japanand theKorean

Ceramic Society.

[11,13,14] . Elimbi et al. [11] studied the effect of temperature of calcination of kaolin on the properties of inorganic aluminosilicatepolymers and found 700 ◦ C as the temperature at which geopoly-mers with optimal characteristics are obtained. Castelein et al. [15]investigated the effect of heating rate of kaolin to reveal its inu-ence on the formation of mullite. Elsewhere, Castelein et al. [16]studied both inuence of temperature and rate of ring of kaolinon the distribution of iron neighboring kaolinite. Ptá ˇ cek et al. [17]studied the effect of the rate of calcination of kaolin to inves-tigate kinetic decomposition of kaolinite under non-isothermalconditions. The obtained results showed that dehydroxylation of kaolinite is controlled by the rate of third-order reaction underapplied condition and the median of overall activation energy andfrequency factor correspond respectively to 227 ± 1kJmol − 1 and(9.4 ± 0.3) × 10 9 s− 1 .

In this study, samples of kaolinof thesame mass were treated at700 ◦ C for the same duration by varying the rate of calcination. Themetakaolins obtained were used for the synthesis of geopolymerswhose characteristics were determined with a view to evaluate theeffect of the rate of calcination of kaolin on their properties. To thatend, kaolin was treated at the following calcination speeds: 1, 2.5,5, 10, 15 and 20 ◦ C/min. Depending on the materials, thermal andchemical analyses, particle size distribution, specic surface area,

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B.B. Kenne Diffo et al./ Journal of Asian Ceramic Societies 3 (2015) 130–138 131

Fig. 1. Particle size distribution of theclay fraction (K).

FTIR, XRD were performed on kaolin, metakaolins and geopoly-mers. The setting time and compressive strength were determinedas well on geopolymers.

2. Materials and methods

2.1. Materials processing

Metakaolins used in this study were obtained from kaolin pro-vided by the NUBRU HOLDING Group which is involved in thevalorization of certain local raw materials in Cameroon. Beforebeing used, the kaolin was enriched with kaolinite by the sedi-mentometry process based on Stokes’s law [18] . The clay fractionobtained labeled as K was rst maintained at ambient laboratorytemperature for a week, cured at 105 ◦ C until its mass became con-stant and then it was ground and sifted through a sieve of mesh90 m. The resulting material was calcinated at 700 ◦ C, the choiceof this temperature being based on the work of Elimbi et al. [11] .Soaking of a mass of 1.5kg of K at 700 ◦ C in an electric mufe fur-nace on ceramic plates (Nabertherm Mod LH 60/14) lasted 30minat the followingrates of calcination: 1 ◦ C/min, 2.5 ◦ C/min, 5 ◦ C/min,10 ◦ C/min, 15 ◦ C/min and 20 ◦ C/min. The obtained metakaolins

were respectively labeled as MK 1 , MK2.5 , MK5 , MK10 , MK15 andMK20 .

The alkaline solution was prepared by mixing sodium silicateand sodium hydroxide solution (12 M) so as to obtain Na 2 O/SiO2molar ratio of 0.7. The sodium hydroxide solution was obtained bydissolving sodium hydroxide pellets witha purity of 99%in distilledwater andsodiumsilicatewas madeupof(mass%)SiO 2 (26.5),Na 2 O(8.0) and H 2 O (65.5).

2.2. Paste and concrete samples preparation and analyticaltechniques

The preparation of geopolymer paste samples consisted of mixing alkaline solution with metakaolin powder according to liq-uid/solidmassratioof 1:1in anautomatic Hobartmixer( Controlab )according to EN 196-1 standard [19] . Setting time of geopolymerpastes was determined using Vicat apparatus according to EN 196-1 standard [19] . For the determination of compressive strength,cubic samples of (2 × 2 × 2 cm 3 ) were made by mixing standard-ized sand [19] and metakaolin powder and alkaline solution inmass ratio of 3:1:1. The molded mortar specimens were curedat 20 ◦ C in a controlled room at 20 ± 2 ◦ C and 98% RH condition.

Demolding was carried out 24h later and the cubic samples werecovered with polyethylene lm and stored at ambient tempera-ture (20 ± 2 ◦ C) under 98% RH condition for 28 days. According tothe rate of calcination of kaolin, the cubic geopolymer specimenswere respectively labeled as GPC 1 , GPC2.5 , GPC5 , GPC10 , GPC15 andGPC20 . The cubic specimens aged of 28 days were subjected tocompressive strength using an automatic electro-hydraulic press(IGM ) operating at an average rate of 0.2 kN/s. Hardened geopoly-mer pastes aged of 28 days were crushed and sifted through asieve of mesh 80 m and powder was subjected to XRD ( SiemensD 5000 diffractometer using CoK ˛ radiation with a rear monochoma-tor ) and FTIR analysis using a BrukerAlpha-p IR spectrophotometeroperating in absorbance mode (interval of wave number rangingwas 4000–400cm − 1 ). The particle size distribution was deter-mined using a granulometer ( CILAS – LIQUID 1090) whose intervalof investigation ranged between 0.04 and 500 m. The thermalanalyses (TG and DSC) of K were performed using a NETZSCH STA-449F3 operating at the rate of 20 ◦ C/min in air. The chemicalanalysesof K andmetakaolinswere performedaccordingto theICP-OES process. Specic surface areas of metakaolins powders were

Fig. 2. Thermal analysis of theclay fraction (K).


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132 B.B. Kenne Diffo et al./ Journal of Asian Ceramic Societies 3 (2015) 130–138

Fig. 3. XRD pattern of theclay fraction (K).

Fig. 4. IR spectrum of theclay fraction (K).

Table 1Bulk density and specic surface area of metakaolins.

Metakaolin

MK1 MK2.5 MK5 MK10 MK15 MK20

Bulk density (g/cm 3 ) 2.54 ± 0.02 2.54 ± 0.02 2.54 ± 0.02 2.56 ± 0.02 2.54 ± 0.02 2.5 6 ± 0.02Specic surface area (cm 2 /g) 128,710 128,200 129,480 125,490 128,720 127,790


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Fig. 5. Particle size distribution of metakaolins.

determined according to Blaine method in a comparative goal andtheir bulk densities were assessed by hydrostatic weighing.

3. Results and discussion

3.1. Characterization of raw materials

3.1.1. Characteristics of the clay fraction

The results of particle size distribution of K are shown in Fig. 1.The curve represents the cumulative distribution of each class of particles. The average particle size ( d50 ) was 14 m and the chem-ical composition (mass%) of K was as follows: SiO 2 (47.2), Al 2 O3(35.1),Na 2 O (


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Table 2Chemical compositions (mass%) of metakaolins.

Chemical composition Metakaolin

MK1 MK2.5 MK5 MK10 MK15 MK20

SiO2 54.60 53.60 52.50 52.10 52.00 51.40Al2 O3 40.60 39.86 39.04 38.74 38.67 38.22CaO 0.12 0.11 0.11 0.11 0.11 0.11MgO 0.22 0.22 0.21 0.21 0.21 0.21Fe2 O3 0.53 0.52 0.51 0.51 0.51 0.50Na2 O 0.12 0.11 0.11 0.11 0.11 0.11K2 O 0.53 0.52 0.51 0.51 0.51 0.50TiO2 0.57 0.56 0.55 0.54 0.54 0.53SO3 0.01 0.01 0.01 0.01 0.01 0.01Loss on ignition 2.26 5.11 6.92 6.93 6.95 7.73Total 99.57 100.64 100.49 99.78 99.62 99.34SiO2 /Al2 O3 (molar ratio) 2.28 ± 0.01 2.28 ± 0.01 2.28 ± 0.01 2.28 ± 0.01 2.28 ± 0.01 2.28 ± 0.01

dehydroxylation of kaolinite and gives rise to the mass percentageof kaolinite to 81%. The crystalline phases revealed by the X-raydiffractogram ( Fig. 3) indicated mainly the presence of kaolinite,quartz, gibbsite and muscovite. Fig. 4 showed the FTIR analysis of

K. The absorption bands at 3688–3619 cm − 1 express the stretchingvibrations of OHgroupsof kaoliniteandgibbsite networks [21,22] .The bands located at 3450 and 1650cm − 1 corresponded respec-tively to stretching vibrations of water molecules [23] w hile those

Fig. 7. IR spectra of metakaolins.


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Fig. 8. XRD patterns of geopolymers.

at 1114 and 1025cm − 1 and then at 998 and 789cm − 1 expressedrespectively the vibrations of Si O Si and Si O Al groups of thenetwork. The bands at 908 and at 789 cm − 1 indicated the presenceof the stretchingvibrationof Al OH withAl in coordinationVI. Theband at 522 cm − 1 indicated the vibrations of Si O Si and Si O Algroups of the network.

3.1.2. Characteristics of metakaolins

Thermal treatment of kaolin generally causes transformationswhich effects are among other things increasing of specic sur-face area and average particle grain size [20] . From Table 1 itwas clear that the variation of the rate of calcination of kaolinhad no signicant effect on the bulk density of metakaolins. Asfor the specic surface area of metakaolins, an outline observa-tion on the different values did not allow to draw meaningfulconclusion on the effect of the rate of calcination of kaolin. Accord-ing to the curves of Figs. 1 and 5 , metakaolins and powder of Kalmost exhibited the same particle size distribution tendency. Thechemical composition ( Table 2 ) showed that the mass percent-ages of SiO 2 and Al 2 O3 decreased contrary to the loss on ignition.This meant that when the rate of calcination of kaolin increased,the minerals in the kaolin (e.g. gibbsite and kaolinite) were less

decomposed and led to a lower production of active compounds

for the geopolymer synthesis. Withregard to kaoliniteparticularly,its transformation into metakaolin fell away with the increase of the rate of calcination ( Fig. 6: increase of intensity of the mainpeak of kaolinite). Consequently loss on ignition became increas-ingly high because of the presence of increasing amount of waterreleased during the dehydroxylation of residual kaolinite. Decreaseof mass percentage of SiO 2 and Al 2 O3 with increase of the rateof calcination correlated well with the increasing of the loss on

ignition since it was taken into account for the determination of mass percentage of oxides present in metakaolins. However, thisdecrease did not affect the molar ratio Al 2 O3 /SiO2 (2.28 ± 0.01)which remained constant because of conservation of matter. TheX-ray diffractograms of metakaolins ( Fig. 6) showed diffuse halopeak with 2 between 18 ◦ and 38 ◦ which is characteristic of amor-phous phase present in metakaolins [24,25] . All minerals initiallypresent in K remained in metakaolins except gibbsite (MK 1 toMK20 ) and kaolinite (MK 1 ). Indeed except for MK 1 where it wasabsent, the main peak (7.15 Å) of kaolinite was observed in alldiffractograms with intensity which increased with the rate of calcination. This behavior was in accordance with the variationof the loss on ignition in metakaolins ( Table 2 ). Thus, the lowerthe rate of calcination, the more complete was the transforma-

tion of kaolin into metakaolin. According to Castelin et al. [15] ,


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Fig. 9. IR spectra of geopolymers.

during the heating of kaolin, kaolinite dehydroxylation, metakaoli-nite structure change, exothermic structural organization alongwith mullite formation are very sensitive to the heating temper-ature rate. In particular, the lower the rate of calcination of kaolin,thelower is thetemperature of commencementof dehydroxylation

of kaolinite [15] . Accordingly, when kaolin was calcined at 700◦

Cfor the same soaking time, kaolinite was more dehydroxylated fora low heating rate. FTIR spectra of metakaolins ( Fig. 7) also con-rmed that exceptfor MK 1 , metakaolins contained kaolinite.In factthe absorption bands assigned to kaolinite (3688–3648, 3619, 908and 788 cm − 1 ) were observed in the spectra of MK 2.5 –MK20 . Con-versely, the FTIR spectrum of MK 1 was mainly characterizedby theband at 1046cm − 1 which corresponded to stretching vibration of Si O Si and Si O Al groups of the metakaolin network [26] .

3.2. Characterization of geopolymers

3.2.1. XRDThe X-ray diffractograms of geopolymer pastes ( Fig. 8) showed

the presence of all the crystalline phases initially encountered

in metakaolins ( Fig. 6). However, the comparison betweenFigs. 6 and 8 revealed certain changes with regard to the halo peakrepresentingthe amorphous phase.The halo peak with 2 between18 ◦ and 38 ◦ for metakaolins ( Fig. 6) was now between 20 ◦ and 45 ◦

for geopolymers ( Fig. 8) which is ngerprint of geopolymerization

[27,28] .

3.2.2. FTIRIn FTIR spectra of geopolymers ( Fig. 9) the absorption bands at

3450–3480 and 1650cm − 1 respectively corresponded to stretch-ing and deformation vibrations of OH and H O H bonds ofwatermolecules [29–31] . Also the absorption band at 1391–1410 cm − 1

referred to stretching vibrations of C O bond of carbonate [32,33]in sodium carbonate which generally induces eforescence withingeopolymers. The absorption band at 1005cm − 1 expressed theasymmetric and symmetric vibrations of Si O Al and Si O Sibonds of SiO 4 and AlO 4 tetrahedrons of the geopolymer network[34,35] . However,contraryto GPC 1 , the FTIR spectra of thegeopoly-mersGPC 2.5 –GPC20 exhibitedabsorptionbands at 3680–3640 cm − 1

which are the ngerprint of the network of kaolinite. Thus, as for


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Fig. 10. Relat ion between sett ing t ime (geopolymers) and loss on ignition(metakaolins).

XRD, FTIR analysis showed that the calcination of kaolin at a highspeed led to geopolymers whichstill contained kaolinite as a result

of incomplete dehydroxylation. In fact geopolymers can be syn-thesized between kaolin and alkali activator solution. However,kaolinite always shows low reactivity [36,37] .

3.2.3. Setting timeThere was increase of setting time of geopolymer pastes with

increase of the rate of calcination of kaolin and it appeared as acorrelation between setting time and loss on ignition ( Fig. 10 ). Theincrease inloss onignitionwiththe rate of calcination ( Table2 ) wasinuenced among other things by the dehydroxylation of residualkaolinite contained in metakaolins. It is well known that amor-phousphasein metakaolin is thephasewhich is reactivein alkalinemedium to produce geopolymers [32,34,38] . Figs. 6 and 10 lead upto consider that during the geopolymer synthesis, increase in set-

ting time with respect to the rate ofcalcination is regulatednotonlyby an amorphous phase but also by the presence of quasi no reac-tive kaolinite. Thus, both amorphous phase and residual kaolinitewere limitingfactors in geopolymerization. The lower was residualkaolinite in metakaolin, the faster was the geopolymer synthesisand this was better accomplished when kaolin was calcined at alow speed.

Fig.11. Relation between compressive strength (geopolymers)and losson ignition

(metakaolins).

3.2.4. Compressive strengthThere was a clear relation between the compressive strength

of geopolymer mortars and the loss on ignition of metakaolins(Fig. 11 ). Unlike the loss on ignition, the compressive strength wasmore and more high when the rate of calcination was low. Accord-ing to the spectra of X-ray diffraction of metakaolins ( Fig. 6), theintensity of the main peak (7.15 Å) of kaolinite was stronger whenthe rate of calcination was higher. In this context, residual kaolin-ite was mainly responsible for the increase of the loss on ignitionwhich was a good indication of the presence of reactive phase: thehigher the losson ignition, the lessermetakaolin contained reactivephase allowed for geopolymer synthesis. The presence of abun-dant reactive phase in aluminosilicate is known to lead to highervalue of compressive strength [11,39] . Thus, compressive strengthof geopolymers was higher for metakaolin which did not containresidual kaolinite and this was achieved when kaolin is calcinatedat a low speed.

4. Conclusion

Metakaolins obtained at 700 ◦ C for the same duration (30 min)by varying therate of calcination (1–20 ◦ C/min)of samples of equal

mass of kaolin were used to produce geopolymers. Chemical anal-ysis of metakaolins revealed that loss on ignition increased withthe rate of calcination of kaolin. This resulted from the presenceof residual kaolinite in metakaolins and whose quantity increasedwith the rate of calcination of kaolin. XRD and FTIR analyses of geopolymers also revealed the presence of residual kaolinite. Thusthe synthesis of geopolymers was affected by both amorphousphase and quasi no residual kaolinite of metakaolins. This simul-taneous effect impacted on the setting time and the compressivestrength: thesettingtime increasedwhilethe compressive strengthfell away. To produce geopolymer having low setting time andhigh mechanical strength, the calcination of kaolin needs to beperformed at a low speed.

Acknowledgments

One of us (B.B. Kenne Diffo) is delighted to acknowledge theFrench Government for granting a scholarship for PhD studiesthrough the “Service de la Coopération et d’Action Culturelle”(SCAC) of the Embassy of France in Cameroon and the staff of the“Laboratoire Matériauxet Durabilité des Constructions”(LMDC)forthe reception and infrastructural support he received during hisstay at INSA–UPS Toulouse (France). Also, nancial supports fromthe“Bureau Afrique Centrale et desGrands Lacs de l’Agence Univer-sitaire de la Francophonie” (BACGL-AUF) under the grant N ◦ S0020*** 10406 and “The World Academy of Sciences” (TWAS) under thegrant N ◦ 13-018 RG/CHE/AF/AC G - UNESCO FR: 3240277723 areacknowledged.

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