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Elaboration and study of the functional properties of geopolymer foams
Asmaa [email protected]
Olivier PITOIS, Paméla FAURE
http://navier.enpc.fr/Laboratoire Navier,2 allée Kepler, 77420Champs-sur-Marne, France
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Geopolymerfoams:
Foamconcreteisatypeofalightweightconcretethatconsistsofacementitiousbinderwithahighdegreeofvoidspace.
Airincorporationenablestolighten thematterandtoconferthermalandacousticinsulationproperties.
Geopolymerfoamscanbeusedasacousticandthermalinsulators,filters orlightweightfireproofinsulators.
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Controllingthenature,size anddistribution ofvoidsisthemostcriticalstepintheproductionofthesefoamssincethevoidsdeterminethedensityandstrength ofthefoamconcrete.
Conciliate mechanical resistance of geopolymer foams and their acoustic and thermal insulation
properties
à Morphology optimization
Objective:
ExampleofanaeratedPortlandcementmortar
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0,1
1
10
0 100 200 300 400 500 600 700
Mecha
nicalresistan
ce(M
Pa)
density(kg/m^3)
Hung2013
Sanjayan2015
Skvara2014
Samson2016(40°C)
Samson2016(20°C)
Liu2016
Liu2015
Dembovska2017
Palmero2015
Zhang2014
Verdolotti2015
Kargin2017
Hajimohammadi2017
Bai2017
Bai2016
?
Intheliterature:>ThedensitiesofGeopoymer foamsmadetillnowareover200Kg/m3
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Formulation(Paste&foam)
MixingFreshstate:
aging
Solidstate:Studyoffunctional
properties
Majorissueencounteredduringtheoptimizationprocess:themorphologyevolvesstronglybeforesetting
Issue:
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Formulation(Paste&foam)
MixingFreshstate:
aging
Solidstate:Studyoffunctional
properties
Majorissueencounteredduringthemanufacture:themorphologyevolvesstronglybeforesetting
Destab
ilizatio
nmecha
nism
s
Drainage CoarseningHa
rden
ing
Issue:
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Formulation(Paste&foam)
MixingFreshstate:
aging
Solidstate:Studyoffunctional
properties
Majorproblem incountred during theoptimization process:themorphology evolves strongly before thesetting
Controlthekineticsofsetting
Issue:
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Kineticsofsettingandrheology:
A.Fernandez-Jimenezetal./MicroporousandMesoporousMaterials(2006)
Duxson etal.(2006)
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→Understandingofthetimeevolutionofrheologyofgeopolymerpastesisamajorissuefortheelaborationprocess
Kineticsofsettingandrheology:
A.Favier etal./SoftMatter (2013)
GeopolymerPortlandCement
Rheologicalbehavioroffreshgeopolymer pastes:• Geopolymer pastescanbeassimilatedtosemi-dilutesuspensionsof
non-colloidalparticlesinaNewtonianfluidofhighviscosity.(Roussel &al,2014)
• Freshgeopolymer pasteshaveaverylowyieldstress.
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• Oscillatoryrheology(f=1Hz)
!(#) = !0'()# !(#) = !0'(()#++)
!∗ = $% = !′ + (!′′
G’:elasticmodulusG’’:viscousmodulus
• Ultrasonicrheology(f=100KHz)
! ′ = ! =$12
'(1 + *)2[1 − *]²
R:ReflectioncoefficientZ1:acousticimpedanceofthe
medium1
(Rouyer,2013)
Materials&Methods:• Metakaolin (Argical M1200s)+SodiumSilicatesolution
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- MonitoringofrelaxationtimesT1 andT2whichcharacterizerespectivelythetimesofreturntotheequilibriumofthelongitudinalandtransversalcomponentsofmagneticmoments,
- T1,2 ~V/S,alreadyusedtocharacterizethesettingofPortlandcement.(P.Faureetal./MagneticResonanceImaging(2008))
à ApplicationofProtonNMRtogeopolymerpastes.
Bruker Minispec MQ20
Methods:• ProtonNMR(H1NMR):
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Phase1:formationofanAl-richgelaroundMetakaolin grains(gel1)
Phase2:inductionphase
Phase3:formationofagelofahigherconnectivity(gel2)àsetting
Monitoringoftheelasticmodulususingstandardrheology
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Phase1:formationofanAl-richgelaroundMetakaolin grains(gel1)
Phase2:inductionphase
Phase3:formationofagelofahigherconnectivity(gel2)àsetting
Monitoringoftheelasticmodulususingstandardrheology
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Monitoringoftheelasticmoduluswith:
Ultrasonicrheology(f=100KHz) Calorimetry
ProtonNMR
- ThecurveT1/T2 illustratesthetransitionfromtheliquidphasetothesolidphase.
- ProtonNMRdefinesacharacteristictimeofgeopolymersetting:(d(T1/T2 )/dt)max
LiquidT1/T2̴1,5
SolidT1/T2̴4
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Monitoringoftheelasticmoduluswith:
àProtonNMRisaanindicatorofthesettingtime.
Ultrasonicrheology(f=100KHz) Calorimetry
10
100
1000
10000
100000
0,00
0,50
1,00
1,50
2,00
2,50
3,00
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15
Elasticm
odulusG
'(Pa)
d(T1/T2)/dt
Time(h)
d(T1/T2)/dt
G',oscillatoryrheology
ProtonNMR
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• Allowstomonitorthesettingforlongperiodsoftime
ProtonNMR
?
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• Allowstomonitorthesettingforlongperiodsoftime
ProtonNMR
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Strategyforbubblesstabilization
1
10
100
1000
10000
100000
1000000
0 1 2 3 4 5
G'(Pa)
Temps(h)Time(h)
Bubblesincorporation
Foamstabilization?
Setting
Mixing5min Rest
Blending5min Foamstabilization
TsTr
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Influenceofairincorporationonsettingtime
SequenceforthemeasurementoftheeffectofmixingonthetimeofsettingSecondmixingsimulatesfoamincorporation
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- Gel1reformssystematicallyaftereachblendinginthesameway.- Timeofinductionisasmuchreducedasthetimeofrestbeforemixingis
important
Influenceofairincorporationonsettingtime
Blending5min
Measurementofelasticmodulus
Time(h)
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Influenceoftemperatureonthetimeofsetting
Thedifferencebetweenthetimest(10000Pa)at20°Cand25°Cis2h43min
10
100
1000
10000
100000
1000000
0 1 2 3 4 5 6 7 8
G'(Pa)
Temps(h)
G'(Pa),20°
G'(Pa),25°
G'(Pa),30°
G'(Pa),40°
Time(h)
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EffectofatemperaturesteponthetimeofsettingUnleashthesettingwithatemperaturestepfrom25°Cto40°Cà Gainintimeoffoamstabilization
Time(h)
Elastic
mod
ulusG’(Pa)
Tempe
rature(°C)
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Preliminaryworkforgeopolymerfoaming:
Tween80(Sigma-Aldrich)(M.Strozi Cillaetal./CeramicsInternational40(2014))
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Preliminaryworkforgeopolymerfoaming:
Tween80(Sigma-Aldrich)(M.Strozi Cillaetal./CeramicsInternational40(2014))
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Thankyou!