Characterisation and reduction by nano-additions of the effect of Ca-leaching in cement pastes
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1 Characterisation and reduction by nano-additions of the effect of Ca-leaching in cement pastes J.J. Gaitero, Y. Saez De Ibarra, E. Erkizia, I. Campillo Unidad Asociada
2 * Ca-leaching Calcium leaching is an ubiquitous process wherever concrete is in contact with water Normal paste Ca-leached paste
3 Calcium leaching of cementitious materials is controlled by the chemical equilibrium of the calcium-silicate-water system Berner leaching curve * Ca-leaching Ca-leaching Equilibrium zone for portlandite [Ca ++ ]>20 mol/m 3 C/S Equilibrium zone for CSH 2 mol/m 3 <[Ca ++ ]<20 mol/m Ca ++ mol/m 3 Ca ++ (mol/m 3 ) licon rich gels: end product of Ca-leaching [Ca ++ ]<2 mol/m 3 U.R. Berner, Radiochimica acta, 44/45, (1988)
![5 2 Ca-leaching Equilibrium zone for portlandite [Ca ++ ]>20 mol/m 3 C/S 1.](/docs-images/43/5492551/images/page_3.jpg "5 1 Equilibrium zone for CSH 2 mol/m 3 <[Ca ++ ]<20 mol/m 3 0.")
4 * Ca-leaching Leaching effects in the C-S-H matrix As leaching goes on, the average C/S-ratio in CSH is reduced The decrease in the C/S-ratio is accompanied by a polymerisation By nanoindentation, Ca leaching has been associated with α-csh from accelerated leaching tests: E(α-CSH) goes from 21,7 to 3,0 GPa E(β-CSH) goes from 29.4 to 12 GPa G. Constantinides, F.J. Ulm, MIT
5 * lica addition Ca() 2 + O 2 C-S-H (1) C-S-H(1) + O 2 C-S-H (2) C/S (1) > C/S (2) MORE GEL Higher Efficiency lica has been usually added in the form of lica Fume ( nm) What happens if we add lower sized silica (nanosilica)?
6 * Objectives To do a systematic study of the phenomenon of calcium leaching in cement pastes To study the influence of nanosilica additions in the calcium leaching process To estimate the validity of this addition as a mean of controlling calcium leaching
7 * Experimental Our experiments have executed over three kind of samples: Plain cement paste with w/c=0.5 Cement paste + colloidal silica (1.8% )(15 nm particle size). Cement paste + agglomerated dry silica (6%)(~1 µm grain size) They have been cured in a saturated solution of Ca() 2 for 28 days. After that, they have been introduced in a 6M solution of ammonium nitrate (NH 4 NO 3 ) Samples have been tested at 0, 10, 20, 40 and 60 days
8 * Experimental
9 Experimental techniques for this work * Experimental X-ray difractometry (XRD), to follow the crystalline phases evolution, and in particular that of portlandite, and the portlandite consumption rate by the nanosilica addition. 29 NMR, to follow the chain growth and redistribution by the addition of nanosilica. EDX-Microanalysis, to follow the Ca/ ratio over time. ESEM, to picture the cement paste at different stages of Ca leaching Hg Porosimetry, to follow the porosity of the paste
10 * Results X-Ray Counts DIAS-comp1.CAF O- Days Plain cement Counts DIAS-comp1.CAF 10 days Plain cement L1-0DIAS_smth.XRDML Colloidal silica L1-9DIAS_smth.XRDML Colloidal silica N1-0DIAS_smth.XRDML Dry silica N1-9DIAS_smth.XRDML Dry silica Position [ 2Theta] Position [ 2Theta] Portlandite has been consumed ~ 10 days
11 60 POROSITY * Results Hg-porosity 50 Plain cement paste Porosity (% ) CP CS ADS Colloidal silica Agglomerated dry silica Leaching time (days) < 10 days: Portlandite consumption > 10 days: no big changes in porosity
12 * Results ESEM O- Days 10 days No Ca-leaching Dissolution front
13 2.5 * Results EDX-microanalysis Ca/ C/S CP CS ADS Plain cement paste Colloidal silica Agglomerated dry silica Leaching time (days) C/S decreases as leaching evolves More moderate for nanosilica modified cement pastes
14 * Results 29 NMR 29 Chemical Shifts for Different Structure Units of licate Species Connectivity Chemical Shift (δ, ppm) Q 0-66 to -74 Q 1-77 to -82 Q 2-85 to -89 Q 3-92 to -100 Q to -115 Q n Tetrahedrally coordinated atom Number of bridging oxygens per tetrahedron Q 0 O O O O O O O Q 2 Q 1 O Q 4 O O Q 3
15 * Results 29 NMR NMR spectra evolution (plain cement paste) Q 1 Q 2 Portland cement with differnet Ca leaching times B3-0days B2-12days B2-20days B2-40days B2-60days Non-degraded Degraded Q 0 Q (ppm)
16 * Results 29 NMR Effect of the nanosilica additions at 40 days Portland cement with different additions at 40 days of Ca leaching Q 2 B2-40days L1-40days N1-40days Colloidal silica Dry silica Plain Cement Q 1 Q 3 Q (ppm)
17 * Results 29 NMR 80 Evolution of Q 3 over time Relative intensity Q Plain cement paste Colloidal silica Dry silica Time (days)
18 * Results 29 NMR Relative intensity Q 3 / Q Relative Intensity of Q 3 to Q Time (days) Plain cement paste Colloidal silica Dry silica Less Ca leaching
19 * Conclusions A coherent set of data from different characterisation techniques has been obtained, confirming that: Portlandite consumption occurs in the early stage of accelerated Ca leaching Pozzolanic reaction induced by dry silica prevents early Ca leaching polymerisation induced by Ca leaching in nanosilica modified cement pastes is less intense than in blank cement pastes Nanosilica addition to cement-based materials can control C-S-H degradation induced by Ca leaching
20 * Acknowledgements The Team Students Juan José Gaitero Yolanda Saez De Ibarra Itsaso Berra Hegoi Manzano Ainara Montero Staff Dr Antonio Porro Dr Igor Campillo Dr Yolanda de Miguel Dr Edurne Erkizia Dr José Antonio Ibáñez Dr. María Moragues Dr Jorge Sánchez Dolado Technicians Eneritz Belasko Raquel Vega Funding: Basque Government under the ETORTEK, SAIOTEK and BIZKAITEK programs
21 THANK YOU VERY MUCH FOR YOUR ATTENTION!!
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