Civil Engineering Seminar Topics_ Geopolymeric Building Materials by Synergetic Utilisation of...

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WEDNESDAY,NOVEMBER30,2011

GEOPOLYMERICBUILDINGMATERIALSBYSYNERGETICUTILISATIONOFINDUSTRIALWASTES

ABSTRACT

Solidwastemanagement isoneamongthebasicessentialservicesprovidedbymunicipalauthorities in thecountry tokeepurbancentresclean.

Duetorapidurbanizationandindustrializationtheproductionofvarioustypesofsolidwasteswhichposeseriousproblemtotheenvironmenthave

been generated. So the disposal and reuse of solid industrial wastes like phosphogypsum, flurogypsum, flyash, slag and lime sludge, etc. is

significantinviewoftheiravailabilityandpotentialapplication.

It isestimatedthatabout300million tonnesof inorganicwaste fromindustrialandminingsectorsaregeneratedeveryyear in India.Advances in

solidwastemanagementresulted inalternativeconstructionmaterialsasasubstitute to traditionalbuildingmaterials likebricks,blocks, tilesetc.

Theeffortsarebeingmadeforrecyclingdifferentwastesandutilizetheminvalueaddedapplications.

Sincealmosteverynaturalresourcesareoverexploitedandareatthevergeofextinctionitisthehightimeforallofustoliveasideourtraditional

conservative approaches and to move forward with new alternatives which are ecofriendly and techniques that leads towards a sustainable

development.

SynergisticutilisationofmajorindustrialwastesgeneratedinIndia,namelyflyash,blastfurnaceslagandredmud,hasbeenexploredtodevelop

novelbuildingcomponentsusinggeopolymerisation.Theseinclude:(a)highstrengthcements(b)selfglazedwalltiles,and(c)pavementtiles.Fly

ashwasusedasmainsourceofsilicoaluminateforgeopolymerisation.Granulatedblastfurnaceslag(GBFS)andredmudwereusedindividuallyor

incombinationwithflyashtotailorpropertiesofthedevelopedcomponents.Chemicalandmechanicalactivationhavebeenjudiciouslyincorporated

in the processing schemes through an understanding of processingstructureproperty relationships. Improvement in the reactivity of fly ash by

mechanicalactivationusinghighenergymillswasfoundtoresultsintheformationofacompactmicrostructureduringgeopolymerisationleadingto

highcompressivestrength(above100MPa) ingeopolymercements.Thecementsalsoexhibited improvedsetting timeandavery lowautoclave

expansion.Inselfglazedwalltiles,thehardimperviousglazedsurfacewasobtainedattemperaturelowerthan150Cbycontrollingtheparticlesize

distribution of solid reactants, viscosity of slurry and reaction atmosphere. The selfglazed surface showed the presence of gismodine (Na

plagioclase)phasewhichwasabsent in themainbodyof thetiles. Inpavementtiles, flyashandgranulatedblast furnaceslagwereusedtogive

structural framework,whereas redmudwasused tosupplement the ironoxide for colouringeffectandalkalis.Thesettingandhardeningoccurred

duetoformationofcementitiousASHandCSHgel(A=Al2O3,S=SiO2,C=CaO,H=H2O).Thetechnologieshavebeendevelopedatbench

scaleandeffortsareunderwayforscalinguptopilotplantlevel.

Thisreportaimsatstudyingtherecyclingandutilisationofindustrialwastesinmakingvalueaddedbuildingmaterials.

CHAPTER1

INTRODUCTION

Theconceptofindustrialecologyisbasedonintegrationofbyproductandwastesteamsacrossindustriesleadingtoproductionofusefulproducts

with near zero flow of material to the environment. Building industry is one of the most dynamic sectors with enormous potential of industrial

symbiosisandsynergisticutilisationof industrialwastes.With increasingenvironmentawareness, there isgrowingconcernworldwide forupdating

production processes, as well as development of green building materials. The green material can be defined as products made from waste,

recycled or byproductsto conserve natural resources, circumvent toxic and other emissions, saves energy, and contribute towards a safe and

healthyenvironment. Geopolymers, silicoaluminatematerials formed throughmimicking natural rock forming process, are fast

emergingasnewclassofgreenbuildingconstructionmaterials.Intheprocessofgeosynthesis,silicon(Si)andaluminium(Al)atomsreacttoform

moleculesthatarechemicallyandstructurallycomparabletothosebindingnaturalrockandallowsfornovelproductssynthesisthatexhibitthemost

idealpropertiesofrockformingelements,i.e.,hardness,chemicalstabilityandlongevity.Flyash,blastfurnaceslagandredmudarethethreemajor

industrialwastesinIndia.Presentlyover100milliontonnesofflyash,12milliontonnesofblastfurnaceslagandnearly4milliontonnesofredmud

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aregenerated.It isestimatedthatproductionof thesewasteswilldouble inforeseeablefutureduetorapidexpansioncoalbasedpowergeneration,

andincreaseintheproductionofiron&steelandaluminiumthroughprimaryprocessing.ThesewastematerialscontainSiO2andAl2O3,alongwith

Fe2O3,CaO,MgO,MnO,etc,andhaveimmensepotentialasmanmaderawmaterialsforgeopolymers.

During geopolymerisation process, the aluminosilicate fraction reactswith alkaline media and transform into a solid geopolymer product, via a

dissolutionpolycondensationstructural reorganisation mechanism, to developstrength. Blast furnace slag behaves differently during

geopolymerisationas compared to fly ashand clay.This is attributed to its higher reactivity duetomostly glassy structurewhich, leads to faster

dissolution ofSi andAlduringgeopolymerisation. TheCaO portion of the slag particles does not necessarilyparticipate in polycondensation, but

reactswithwaterandmayundergohydrationreaction.Ithasalsobeenreportedthatadditionofblastfurnaceslagintheconventionalsilicoaluminate

geopolymercementandconcreteimprovessettingcharacteristics.Useof redmud ingeopolymersappearstobeanattractiveproposition fromthe

pointofviewofitshighalkalinecontent.However,therehaveverylimitedattemptsinthisdirection.

Thispaperisbasedonrecentresearchonthedevelopmentofawidevarietyofgeopolymericproductsusingflyashasthemainrawmaterialalong

with granulated blast furnace slag (GBFS) and redmud. The focus is on: (a) high strength cement, (b) selfglazed tiles, and (c) pavementtiles.

Processing,structureandpropertiesoftheproductsarehighlighted.Thecommercialisationprospectsoftheproductsarealsodiscussed.

CHAPTER2

MATERIALSANDMETHODS

TheflyashandGBFSusedinthestudywereobtainedfromacementgrindingunitatChattisgarhState,India.Theredmudwasobtainedfroma

AluminiumPlantatOrissaState,India.Thechemicalanalysisandphysicalpropertiesoftheflyash,GBFSandredmudaregiveninTable2.1.

Table2.1.ChemicalanalysisandphysicalpropertiesofFlyash,GBFS,Redmud

TheSiO2+Al2O3+Fe2O3contentoftheflyashwas>70%anditwasaClassFfly

ashasperASTM.Thebasicityoftheslag(CaO/SiO2ratio)was1.06.Thebatchcompositionoftheeachproductwasselectedbasedonchemical,

physicalandmineralogicalcharacteristicandreactivity.Thecompositionoftheproducts,intermsoftheamountsofflyash,blastfurnaceslagand

redmudusedareindicatedintheternarydiagramshowninFig2.1.

Figure2.1.Compositionofgeopolymercement,selfglazedtilesandpavementtiles

The geopolymer cements were prepared using the raw as well as preprocessedfly ash. The techniques used for preprocessing include air

classification andmechanical activation. Air classification was carried out using an air classifier 50 ATP.Mechanical activation of fly ash was

carriedoutusinganattritionmillandavibratorymill.Sodiumhydroxidewasdissolvedinwateratleast24hoursbeforeuse.Incaseofgeopolymer

cement,geopolymerisationwascarriedoutbykeepingthesamplesincontrolledhumidityfor24hoursat27Cfollowedbythermalcuringat60Cfor

24hours.

For self glazed tile, fly ash and a ball milled granulated blast furnace slag (GBFS) were used as main materials. The batch composition was

thoroughlymixedwithalkalineactivatorandthencastedintilemould.Colourpigmentswereaddedintotheslurrybeforecastingtogetthedesired

colouringeffects.Thecastedtileswerethenedgedfor24hoursat27Cfollowedbyheattreatmentintherangeof150300Cusingdifferentthermal

cycle.

Inpavement tiles, redmudwas intimatelymixedwith flyashandballmilledGBFS.Thebatchwaspreparedbyaddingcoarse,mediumand fine

aggregatesandalkalineactivator. The slurrywas casted in rubbermouldsandallowed to set at ambient temperature. In all the cases, physical

properties were tested as per standard procedures discussed elsewhere. The heat evolution during reactions was monitored using an

isothermalconductioncalorimeter.XRDpatternsofsampleswererecordedonaSiemensDiffractometerusingCoKradiation.Themorphologyof

thesampleswasexaminedusingScanningElectronMicroscope(SEM)withEDSattachmentformicroanalysis.

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CHAPTER3

GEOPOLYMERISATIONOFWASTE

Mostproposedmechanismsofgeopolymerisationconsistofdissolutionofaluminosilicatephase,polymerisationandreprecipitationofgelphase,

and transformation of the gel phase into geopolymer of varying crystallinity and structure.Depending upon experimental conditions, the different

stages of geopolymer formation may overlap and even merge with each other. Isothermal conduction calorimetry was used to study the

geopolymerisation of fly ash,mixture of (GBFS+fly ash), and themixture containing (fly ash+GBFS+redmud). The calorimetry was carried out

underfollowingconditions:

(i)27Cfor24h(Fig.3.1)

(ii)60Cfor24hafterkeepingthesampleat27Cfor24h(Fig.3.2)

Figure.3.1IsothermalConductionCalorimetrycurveshowingdissolutionofsamplesat27C

Figure.3.2IsothermalConductionCalorimetrycurveshowinggeopolymerisationat60Cafter24hourdissolutionat27C

Thecalorimetric response inFig.3.1 for thealkali flyashmixtureat27C isexpected to representdissolutionpolymerizationand initiationofgel

formation. Response in Fig.3.2 signifies the conversion into geopolymer via gel formation step. Based on conduction calorimetric results, the

followingobservationsweremade:

(i)at27C (Fig.3.1), the initialexothermicpeak I inall thecases indicates that reactionstartedassoonas thestartingpowderswasmixedwith

NaOHsolution.Inthecaseof(flyash+GBFS+redmud)mixture,aminorpeakwasobservedatthestart,whichafterashortinductionperiodof

30minacceleratedtostrongerexothermicpeak.Nosuchinductionandacceleratoryperiodwasobservedinothersamples.In

termsofmaximumreactionrate,(flyash+GBFS+redmud)mixturehasshownmaximumreactionratefollowedby(flyash+GBFS)andflyash.

(ii)at60C,afteredgingthesampleat27Cfor24h(Fig.3.2),twopeakswereobservedinallthesamples.Firstendothermicpeak,observedduring

0250 min, corresponds mainly to dehydration that occurred owing to the evaporation of water formed or water remained unused during gel

formation.Theareaundertheendothermicpeakfor(flyash+GBFS)sampleshowedahigherarea,indicatinggreateramountofgelformation.After

the endothermic peak, the broad flat exothermic peak, observed during 2401200min, corresponds to polycondensation. This peak started and

flattens earlier in fly ash.Whereas in other cases, the peak took longer time to flattens possibly due to presence of GBFS,which resulted into

formationofCSHgel.



Figure3.3Conceptualmodelforgeopolymerisation

CHAPTER4

DEVELOPMENTOFNOVELBUILDINGMATERIALS

4.1.GEOPOLYMERCEMENT

Lowreactivityofflyashhasoftenrestrictedtheuseofflyashforgeopolymercementsduetoslowstrengthdevelopment.Thereactivityofflyash

dependsonitsvitreousphasecontent,whichparticipatesingeopolymerisationreaction.Theremainingconstituentstakeslongertimeforreaction

due to poor reactivity and leads to slow setting and strength development in geopolymers. Various methods such as chemical activation,

mechanicalactivationandsizeclassificationofflyashhasbeensuggestedasameanstoimprovethereactivity.Recentlyobservationsweremade

bythepresentauthorsthatuseofmechanicallyactivatedflyashleadstohighcompressivestrengthingeopolymers.Twodifferentapproachwere

adoptedtoenhancereactivityofflyash:(a)airclassificationtoseparatefinerfractions,and(b)mechanicalactivationinattritionandvibratorymills.

Smallsizecenospherecoolsfasterduringtheirformationincoalcombustionprocessandseparationoffinerfractionbyairclassificationresultsin

increase in theglasscontentsvisvis raw flyash.Mechanicalactivation resultsdue tocombinedeffectofparticlebreakage (surfacearea)and

otherbulkandsurfacephysicochemicalchangesinducedbytheprocessofmilling.

Thechange in reactivityof flyashdue to increasedglasscontentandmechanicalactivationwasassessedvisvis raw flyash.Fig.4.1shows

typicalparticlesizedistributionof rawflyash(RFA),classified flyash(CFA),attritionmilled flyash(AMFA)andvibratorymilled flyash(VMFA).

Basedonmedianparticlesize(X50),thesamplescanbearrangedinfollowingdescendingorder:RFA(36.2m)>VMFA(5.99m)>AMFA(4.85

m)>CFA(2.79m).

Figure.4.1particlesizedistributionofRFA,CFA,AMFAandVMFA



Figure.4.2XRDpatternofRFA,CFA,AMFAandVMFAbasedgeopolymersshowingformationofaluminasilicategelandhydroxysodalite

Figure.4.3SEMmicrographshowingcompactstructureobservedinVMFAbasedgeopolymers

Figure.4.4Geopolymercementandconcretecubes

Figure.4.2 showsXRDpattern ofRFA,CFA,AMFAandVMFAbased geopolymers.Similar nature of XRDpatterns suggests formation of same

phasesinallthesamples.TheXRDpatternsshowabroadpeakintherangeof1016correspondingtoaluminosilicategel.Inaddition,presenceof

hydroxyl sodalitephase is observed indicatinggeopolymerisation.Themost compactmicrostructurewasobtained inVMFAbasedgeopolymers

withhighproportionofreactionproduct(Fig.4.3).Basedontherelativeamountofgeopolymerproductformedandcompactnessofmicrostructure,

thereactivityofflyashsamplesdecreasesinfollowingorder:VMFA>AMFA>CFA>RFA.InspiteofhigherparticlesizeofVMFAandAMFA(5

6m)ascomparedtoCFA(~3m),higherreactivityofmechanicallyactivatedsampleswasinteresting.

ThephysicalpropertiesofthegeopolymercementaregiveninTable2.ThehigherstrengthinAMFAandVMFAisattributedtohigherreactivitydue

to mechanical activation that leads to enhanced geopolymerisation and more compact microstructure. Significantly higher strength of samples

preparedusingVMFAovercorrespondingAMFAsampleshighlightsthe importanceofmechanicalactivationdevice.Theotherproperties,suchas

setting time,autoclaveexpansion,etc. indicate that thedevelopedgeopolymercementsmeet thespecificationsdrawn forhydrauliccements like

ordinaryPortlandcement,PortlandslagcementandPortlandpozzolanacement.

Table4.1Propertiesofgeopolymercement

4.2.SELFGLAZEDTILE

Conventionallyceramic tilesareproducedbyhigh temperaturesintering/vitrificationofaluminosilicateandsilicatemineralssuchasclay,quartz,

feldspar,etc.Thestrengthandotherpropertiesof tilesaredevelopeddue to formationofceramicbonds.Developmentofstoneware tilesat250

400C by geopolymerisation of aluminosilicate minerals has been reported. The processing involved reaction between aluminosilicate mineral

kaoliniteandNaOHat100C150Cresultingintotheformationofhydrosodalite

Si2O5,Al2(OH)4+NaOHNa(SiOAlO)n

kaolinitehydrosodalite

Inthealkaliactivationofflyashandslagmixtureatambienttemperature,flyash/slagratioisthemostrelevantfactoronthestrengthdevelopment.

Themainreactionproduct isahydratedcalciumsilicatewithhighamountoftetracoordinatedAl in itsstructure.Theadditionsofcalciumcontent

increase the degree of geopolymerisation at elevated temperature and results into higher strength. Beneficial effect of slag on fly ash

geopolymerisationwasexploitedinthedevelopmentofselfglazedwalltiles.

TheglazedsurfaceandthebodyoftilesshoweddistinctlydifferentmicrostructureasrevealedbySEMmicrographsshowninFig4.5aandFig4.5b,

respectively.

Theglazedsurfaceischaracterizedbywellknittedgrainsgivingrisetocompactmicrostructurewithverylowporosity(Fig.4.5a).Themorphology

ofthetilebodyshowsthewellreactedporousbody.XRDstudiesindicatedthepresenceofgismodine(Naplagioclase)phaseintheglazedsurface



(Fig.4.5c).

Figure4.5a.Closelyknittedmicrostructureofglazedsurface,b.wellreactedmicrostructureoftilebody,c.XRDpatternofglazedandbodyoftile,

andd.tilesofdifferentcolour

TwotypeofbulkreactionproductswereidentifiedbyEDXstudies:(a)alowcrystallinecalciumsilicatehydraterichinAl,whichincludesNaintoits

structureandresultsfromthealkaliactivationofslag,and(b)anamorphousalkalinealuminosilicatehydrateresultingfromthealkaliactivationoffly

ash.Criticalcontrolonparticlesizedistribution,chemicalcomposition,rheologyofslurryandreactionenvironmentisnecessaryfortheformationof

requiredphasesintheglazedsurface.

ThepropertiesofglazedgeopolymertilearesummarisedinTable4.2.

Table4.2Propertiesofgeopolymertile

ThetilesdevelopedconformtotheEuropeanNation(EN)specificationforwalltiles.Thenaturalcolourofthetileswaslightgreybutdifferentcolour

anddesignswereproducedusingcolourpigments.Unlike thefiredceramic tiles,nocrazingandotherglazedefectswereobserved.Althoughthe

surfaceofthetilewasimpervious,theporosityofbodywas1317%,whichisgoodforbondingwithcement.

4.3PAVEMENTTILES

Pavementtilesaresmallcementstructuresingeometricalshapesthatareusuallylaidonpathwaysoronanyopengroundasasolidplatform.As

these tilesarenot cementedandonly laid closelyover abedof loose sand, they canbeeasily removed, storedand reusedasmany timesas

possible.InIndia,thepavementtilesaremostlyvibrocastand/orpressedcementmortarorconcretehydratedfor28days.Thestrengthisobtained

due to hardening of cement. Earlier research on alkalislagredmudcement (ASRC) has indicated high early and ultimate strength togetherwith

excellent resistanceagainst chemical attacks. This was achieved by introduction of solidcomposite alkali activator into slagred mud mixture

systeminsteadofliquidwaterglass.ThehydrationproductsofASRCcementweremostlyCSHgelwithlowCa/Siratiointherangeof0.8to1.2.

Inthepresentworkflyash,GBFSandredmudwasusedtodevelopcementitiousphasesbyalkaliactivationatambienttemperature.Redmudwas

usedtogivecolouringeffecttothetilesfrompresenceof ironoxides,andalsopartlysupplementalkaliesforreaction.Similartoselfglazedtiles,

twomajorreactionproductswereidentifiedinXRD(Fig4.6)andEDXstudies.CSHgelwithNainitsstructurefromtheactivationofGBFS,and

amorphousalkalinealuminosilicatehydrateresultedfromtheactivationofflyash.Alsopresenceofironoxideandhydroxideresultedfromaddition

ofredmud.

Figure4.6XRDpatternofpavementtiles



The SEM studies (Fig4.7) have shown a dense microstructure including numerous fibrous structures corresponding to CSH gel with Na in

structure.

Figure4.7Densemicrostructurewithnumerousfibers

Figure4.8Pavementtiles

Table4.3Propertiesofpavementtile

Thetiles,althoughproducedatambienttemperature(2735C),exhibitsgoodcompressiveandflexuralstrength.

CHAPTER5

SYNERGETICUSEOFINDUSTRIALWASTE

Synergisticuseof industrialwaste isanemergingconceptwherebycombinationof twoormorewastes isused todevelopausefulproduct.The

mainadvantageof thesynergy is thedeficiencyofconstituents fromonewaste iscompensatedbyusingsecondor thirdwaste,which is rich in

deficient constituent. Synergistic use also includes industrial symbiosis where physical exchange of waste/byproducts between geographically

close industries is exploited. In the present work, waste from three industries, fly ash from thermal power plants, fly ash and granulated blast

furnaceslagfromSteelPlants,andflyashandredmudfromAluminiumplants,hasbeenused.

Flyashwasusedforthedevelopmentofgeopolymerscement,combinationofflyashandblastfurnaceslagwasusedforselfglazedtilesandall

three wastes fly ash, GBFS and red mud was used for pavement tiles. From the point of view of zero or minimum flow into environment,

geopolymer cement is best suited for thermal power plant, where fly ash is themain byproduct. Selfglazed tiles and pavement tiles aremore

suitableforiron&steelandaluminiumindustryrespectively.Fig.5.1showsthesynergymapofthesewastes.

Figure.5.1SynergymapfortheUtilisationofdifferenttypeofIndustrialwastes

CHAPTER6

ECONOMICSANDCOMMERCIALPOTENTIAL



PostedbyPremMohanat9:42PM

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Thecostofmost industrialproduction is increasingly influencedbytheoperationsrequiredfortheadequatedisposalofbyproducts.Thedisposal

costasperregulationsmayadd510%oftheproductioncostdependingonvolumeandnatureofwastegenerated.Themajorbenefitofsynergistic

useof industrialwaste is reduction inproduct cost.Thegeopolymerisationprocess is low temperatureprocessand thus thepotential forenergy

savings issubstantial.Cementclinker isnormallyproducedat~1400Candceramic tilesareproducedat9501200C.Whereasthegeopolymers

cementandselfglazedtilesrequire60150Ctemperature.Thissignificantreductionintemperatureisexpectedtosaveupto70%inenergycost.In

addition,therewillbeenormoussavingincapitalcostasnohightemperatureprocessingkilnsarerequired.

Producersofgeopolymersproductsmayalsobenefit fromrawmaterialcostsbecausethemainreagentsarewastematerial. In India, flyashand

redmudarefreeofcostandonlytransportationcostisinvolved.ThecostofgranulatedblastfurnaceslagisaroundRs.400500pertonne.Based

onthevariousinputs,atechnoeconomiccalculationwascarriedoutasfollows(Table.6.1):

Table.6.1Technoeconomicsfortheproductionofgeopolymerproducts

Thetechnoeconomicsbasedonlaboratoryresultsindicatehighcommercialization

potential.Effortsareunderway in thisdirection throughsettingupofapilotplant tooptimizemanufacturingparametersandpropertiesona larger

scale.

CHAPTER7

CONCLUSION

DuetotheirabilitytopolycondenseSiliconandAluminiumintosolidmonolithicceramiclikestructureduringalkaliactivation,geopolymershavethe

potential of utilization of industrial wastes rich in silicoaluminates such as fly ash,GBFS, redmud, etc. Novel buildingmaterials such as high

strengthgeopolymerscementcanbedevelopedbyadditionalprocessingsuchasmechanicalactivation,andselfglazedtileandpavementtilescan

be developed by synergistic use of industrial waste namely fly ash, GBFS and red mud. The developed geopolymer products qualify as new

membersinthespectrumofecofriendlyconstructionmaterialsduetoeasyandsimpleprocessing,lowenergyrequirementandnoCO2emission.

Theproductshavegoodcommercialisationpotentialwithsignificantreturns.

REFERENCES

1.SanjayKumar,RakeshKumaar,A.Bandopadhyay,S.PMehrotra(2007)Novelgeopolymericbuildingmaterialsthroughsynergeticutilisationof

industrialwaste,NationalMetallurgicallaboratory,Jamshedpur,India.

2.S.D.Muduli,P.K.Rout,S.Pany,S.M.Mustakim,B.DNayak,B.KMishra(2010) InnovativeProcess inManufactureofColdSettingBuilding

brickfromMiningandIndustrialwastes,IMMT(CSIR),Bhubaneswar.

3.C.Casco,A.Alvarez,N.Navarro,L.Yague,AdvantageanddisadvantagesofusingPhosphogysumasbuildingmaterialRadiologicalaspects,

CSIC,Madrid,Spain.

4.P.Duxson,A.Fernandez,J.CProvis,G.CLukey(2006)Geopolymertechnology:thecurrentstateofart,ARC,Australia

5.www.wikipedia.com

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4comments:

ShaswatSwain August16,2013at7:15AM

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AbhishekKumar May24,2014at9:03PM

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