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Proceedings of the International Conference on Sustainable Materials,
Systems and Structures (SMSS2019)
New Generation of Construction Materials
Edited byMarijana Serdar
Nina ŠtirmerJohn Provis
RILEM Publications S.A.R.L.
ProceedingsPRO 128
International Conference on Sustainable Materials, Systems and Structures
(SMSS 2019) New Generation of Construction Materials
International Conference on Sustainable Materials, Systems and Structures (SMSS 2019)
New Generation of Construction Materials
20-22 March 2019 – Rovinj, Croatia
II
Published by RILEM Publications S.A.R.L.
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ISBN: 978-2-35158-217-6, Vol 1. ISBN: 978-2-35158-223-7
e-ISBN: 978-2-35158-218-3
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International Conference on Sustainable Materials, Systems and Structures – SMSS 2019
New generation of construction materials
Rovinj, Croatia 20-22 March 2019
Edited by Marijana Serdar
Nina Štirmer John Provis
RILEM Publications S.A.R.L.
International Conference on Sustainable Materials, Systems and Structures (SMSS 2019)
New Generation of Construction Materials
20-22 March 2019 – Rovinj, Croatia
XVIII
Mechanical behavior and neutron shielding performances of TiO2-incorporated
cement composites
Jaeyeon Park, Sungwun Her, Heongwon Suh, Seung Min Woo, Keunhong Jeong and
Sungchul Bae
297
Effect of titanate nanotubes on the properties of cement-based composites
Hyeonseok Jee, Jaeyeon Park, Sungwun Her, Erfan Zalnezhad, Keunhong Jeong and
Sungchul Bae
304
Influence of PRAH crystalline admixtures on the durability of concretes
Kosmas K. Sideris, Christos Tassos, Alexandros Chatzopoulos, Panagiota Manita
312
A comparison of graphene oxide, reduced graphene oxide and pure graphene:
early age properties of cement composites
Tanvir S. Qureshi and Daman K. Panesar
318
A new admixture for concrete with clay contaminated sand
O. Mazanec, F. Morati, A. Große-Sommer
326
SESSION 8: Candidates for AAMs 327
Instantaneous activation energy of alkali activated materials
Shiju Joseph, Siva Uppalapati and Özlem Cizer
328
Mechanical parameters of metakaolin-based geopolymer with CRT glass waste
fine aggregate
Natalia Paszek, Marcin Górski
329
Development of alkali-activated magnesium aluminosilicate binders from soap-
stone
Z. Abdollahnejad, T. Luukkonen, M. Mastali, J. Yliniemi J, P. Kinnunen, M. Illi-
kainen
337
Production of alkali-activated binders from iron silicate fines
John L. Provis, Angel L. Muñoz Gomez, Oday H. Hussein, Gaone Koma, Emanuela
Manolova, Vladislav Petrov
345
Mixture proportioning for alkali-activated slag-based concrete
Ning Li, Caijun Shi, Zuhua Zhang, Deju Zhu
353
Alkali activation of high MgO BFS with sodium carbonate added dry vs. wet
Abeer M. Humad, John L. Provis, Andrzej Cwirzen
354
SESSION 9: Alternative binders 362
Hydration of MgO in the presence of hydromagnesite
Frank Winnefeld, Eugenia Epifania, Fabio Montagnaro and Ellis M. Gartner 363
Radioactive waste conditioning using alumina-silicate binary blends
Bastien Planel, David Lambertin and Catherine A. Davy 371
ALKALI ACTIVATION OF HIGH MGO BFS WITH SODIUM
CARBONATE ADDED DRY VS. WET
Abeer M. Humad1,2, John L. Provis3, Andrzej Cwirzen1
1Structural Engineering Division, Luleå University of Technology, Luleå, Sweden.
2Civil Engineering Department, University of Babylon, Iraq.
3Department of Materials Science and Engineering, University of Sheffield, Sheffield, UK.
Abstract
The use of sodium carbonate to alkali activate blast furnace slag has several advantages over
the typically used sodium silicate, including for example easier, safer handling and less negative
environmental impacts. In this study, sodium carbonate (SC)-activated blast furnace slag (BFS)
pastes and concretes were produced using a high MgO content BFS activated with 3, 5, 10 and
14 wt.% (by binder) of SC. The activator was added either as a dry powder or dissolved in water
one hour before mixing. The setting time, workability and compressive strength after 1,7 and
28 days were determined. Concrete cubes were cured in two setups: sealed specimens at 65 ˚C
for 24 hours followed by storage at laboratory conditions (20±2˚C), or simply sealed storage at
laboratory conditions (20±2˚C and 50-55% RH), until testing. The results showed that,
increasing the dosage of SC decreases the initial and the final setting time regardless of whether
the mixing procedure was dry or wet. However, addition of the SC dissolved in water increased
the slump at higher SC dosage, while increasing addition of the dry SC resulted in a lower
slump. A higher dose of SC increased the 28d compressive strength when added as a dry powder
or wet, with higher values in laboratory curing compared with heat curing.
Keywords: Alkali Activated Slag, Blast Furnace Slag, Alkali activation, Sodium carbonate.
1. INTRODUCTION
The contribution of Portland cement manufacture to greenhouse gas emission is estimated
to be at least 6% of total anthropogenic greenhouse gas emissions 1. Alkali activated slag is
indicated as an environmentally friendly alternative to Portland cement, having lower CO2
emissions and energy cost, particularly when near-neutral salt activator are used as these can
be generated with very low carbon footprints. However, sodium carbonate (SC), which was
used in the present research, is less effective as an alkali activator in comparison with, for
example, sodium silicate (SS). Consequently, some SC-activated mixes have a longer initial
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setting time which can span even from 2 to 5 days 2-6. The rate of reaction of sodium carbonate
activated slag is also influenced by factors including the fineness and the chemical composition
of the slag, curing temperature, W/B ratio and SC dosage 6-9 and might be accelerated to a
certain extend by several means, for example higher alkali dosage, addition of additional
activators such as sodium hydroxide or SS or the use of reactive admixtures such as lime or
active MgO 4,10-13. It has been reported that SC-activated slag required around 100-130 h to
reach the reaction peak with variable dosages of SC, when using a slag with moderate MgO
content. The initial formation or precipitation of CaCO3 was indicated as the main reason 7,8.
Increasing the SC content and lowering the water to binder ratio shortened the time required to
reach the reaction peak to 48h or less 9,12, but this is still unacceptably slow for partial
concerting. The pH of the activator solution is playing a significant role in the initial dissolution
and reaction of the precursor followed by the precipitation of the C-S-H gel. The minimum
required pH value was higher than 9.5 14. In spite of the lower initial pH of the SC, it exhibited
better activation results than the NaOH in terms of mechanical properties and durability 6, which
is linked to the reaction kinetics of the SC-activated slag. The dissolution of slag releases Ca2+,
which react with CO32− from the SC activator to form calcite and gaylussite
Na2Ca(CO3)2·5H2O. This occurs earlier than the precipitation of the C–(A)–S–H gel,
consuming the Ca2+ released by the slag at an initial pH below 12. As a result, the dissolution
of silicate species is slow. After consuming CO32− ions, the pH will rise to approximately 13.5
at the later stage of the reaction 6,8.
Concrete produced with SC-activated slag usually showed slower strength development, and
sometimes lower late strength, in comparison with mixes activated by sodium silicate 15. Recent
studies showed significantly higher compressive strength of SC-activated fly ash-slag materials,
reaching up to 80 MPa after 90 days of curing 16. The SC-activated slag showed similar or lower
shrinkage in comparison with PC mortar, while mixes activated with waterglass had 3-6 times
higher shrinkage values 4. The strength development of slags activated with various activators
can be listed in the following order Na2SiO3 > Na2CO3 > Na2SO4 > NaOH 17,18. In a recent
study, the reaction products of SC-activated slag at early age were identified as gaylussite,
calcite and C-(A)-S-H gel 6,9, and the formation of gaylussite tended to occur much earlier in
the binder based on slag with higher fineness 6. Hydrotalcite-group minerals (Mg-Al layered
double hydroxides) are also important reaction products in these binders as they evolve 6,8. SC
or NaOH alkali activated slag with moderate content of MgO in the slag glass showed longer
setting times in comparison with SS activated mixes 7,8, whereas, a high MgO content slag (14.6
wt.%) activated with SC revealed a faster setting in comparison with mixes activated with SS 19. Consequently, the composition of slag has a significant role in defining the kinetics of
reaction SC-activated slag at very high MgO content (16.1wt.% in the slag) had a final setting
time under 21h when activated with 14 wt.% SC, and a rapid loss of workability 9. The MgO
content also affect the microstructure and the strength development of alkali-activated slag,
associated with the availability of Al and the formation of hydrotalcite-type phases 20,21.
In alkali-activation, the alkaline component can be added to slag in different ways, for
example in an aqueous solution, or in the solid state by mixing the dry alkali powder with slag.
The dry alkali powder can be also ground together with the slag 9,13,22,23. Producing a binder
that can be used with only the addition of water, requiring a dry activator, will promote the use
of AAS cements 23. So, the present study is focused on the effect of mixing methods (dry or
wet activator addition) on selected properties of sodium carbonate-activated slag pastes and
International Conference on Sustainable Materials, Systems and Structures (SMSS 2019)
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concretes, using a slag with high MgO content due to its superior compatibility and reaction
with this particular activator type.
2. EXPERIMENTAL WORK
A commercially available ground granulated blast furnace slag (BFS) in Sweden was used
in this study. Table 1 shows the chemical composition, which was determined using a
Pananlytical-Zetium XRF spectrometer. Powdered sodium carbonate (SC) with purity ˃ 99%
was used. The sodium carbonate dosages varied between 3 and 14wt.% Table 2. All concrete
mixes contained 450 kg/m3 of BFS. The water to binder (w/b) ratio was 0.45 for concrete mixes
and 0.36 for pastes. The granite aggregates having a particle size 0-8 mm, with fine aggregate
content of 80 wt.% were used. The total aggregate content for concrete mixes was 1663 kg/m3.
Table 1: Chemical composition of BFS used in this work, measured by X-ray fluorescence and
reported on an oxide basis.
Component CaO SiO2 Al2O3 Fe2O3 MgO Na2O K2O TiO2 MnO SO3 L.O.I
Oxide
wt.%
30.4 35 14.3 0.3 16.1 0.6 0.7 2.8 0.5 0.7 0.9
Physical
data
Specific surface
cm2/g
Particle density kg/m3 Bulk density kg/m3
5000 2950 1100
Table 2: Mix proportions of concrete
Mix ID Binder content
kg/m3
w/b ratio Aggregate content
kg/m3
Sodium carbonate
doses wt.%
3 SC 450 0.45 1663 3%
5 SC 450 0.45 1663 5%
10 SC 450 0.45 1663 10%
14 SC 450 0.45 1663 14%
Note: For all mixes above there were two mixing procedures; dry D and wet W and two
curing types; laboratory curing (20±2˚C and 50-55% RH) and heat curing (65˚C for 24h
then laboratory conditions until testing).
Different mixing procedures were used for dry and wet activators. The dry procedure
included 3 min of mixing of all the dry ingredients (slag + aggregates + powder sodium
carbonate), followed by addition of water and mixing for another 4 minutes. The Hobart mixer
model A200N was used. In the wet procedure, the sodium carbonate was dissolved in the
mixing water and left to stand for one hour before being added to the mixed dry materials (slag
+ aggregate). Specimens for compressive strength testing were casted in alkali-resistant
polymer 100 mm cube moulds. Immediately after casting, all samples were sealed with plastic
film. Curing was carried out following two procedures. In the first procedure, specimens were
sealed and kept at 20±2˚C and 50-55% relative humidity (RH) until testing, whereas in the
second procedure, specimens were sealed and heat cured at 65˚C for 24 hours, then at 20±2˚C
International Conference on Sustainable Materials, Systems and Structures (SMSS 2019)
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and 50-55% RH until testing. Compressive strength values were determined at 1, 7 and 28-days
after casting, following the SS-EN 12390-3 standard (SS-EN 12390-3). The compressive
strength values were determined using an Ele-autotest 3000 instrument. The loading rate was
set to 10 kN/sec. The concrete slump was determined following ASTM C143 (ASTM
International 2015). Initial and final setting times of SC-activated slag pastes were determined
following the IS 4031 process of the Vicat test (IS: 4031-PART 5-1988), measuring the
penetration using a 1-mm diameter needle and a plunger mass of 300 g. The initial setting times
was defined as to occur when the penetration depth was 5-7 mm from the bottom of the material
in its mould, and the final setting time when there was no longer any visible penetration of the
outer circle of the needle plunger.
3. TEST RESULTS AND DISCUSSION
The amount of sodium carbonate and the mixing procedure strongly affected the fresh
concrete properties. Mixes produced with dry SC showed decreasing workability with an
increasing amount of activator, Figure 1. This can be related to the increased water uptake of
the dry activator while it is in the process of dissolving. Conversely, the mixes with SC
dissolved in water prior to the mix showed increasing slump values with an increasing SC
dosage. In that case, no rapid water uptake by the SC was present. The initial setting time
appeared to be slightly shortened for mixes produced with the wet activator. A higher alkali
concentration caused more extensive dissolution of the slag which was followed by more
intense precipitation of the reaction products and thus a shorter setting time 24,25, Figure 2.
Concrete activated with the dry SC activator
showed a longer initial setting time. This could
be related to a slower formation of C-A-S-H due
to the lack of the advanced dissolution as in the
case of the wet SC, Figure 2a. Furthermore, a
high concentration of MgO (16.1 wt.%) in the
blast furnace slag used in this study gives more
extensive formation of hydrotalcite-group phases
at early age, which could also contribute to the
observed short initial setting times 26. The final
setting times were unaffected by the SC
preparation pathway, Figure 2b. Figure 1: Slump test results
International Conference on Sustainable Materials, Systems and Structures (SMSS 2019)
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The compressive strength results are
presented in Figures 3 and 4. Generally, a higher
dosage of sodium carbonate led to increased 1,
7 and 28-day compressive strength values. The
1-day compressive strength was higher for the
heat-cured specimens, Figure 3, due to the
increased dissolution of BFS and acceleration
formation of the reaction products 2. The
laboratory cured specimens activated with less
than 14 wt.% SC did not harden after one day of
curing, Figure 4. After 7-days of laboratory
curing, concrete cube strength values varied
between 22 and 35 MPa, and between 32 and 50
MPa after 28 days. There was not a statistically
significant difference between mixes produced
with dry and wet alkali activators. Longer
curing times are known to stimulate further
strength development of concrete based on blast
furnace slag, which was also observed in the
present research 27. The 28-day old concretes
cubes cured at 20˚C for all mixes showed higher
late (28 day) strength values than the heat-cured
specimens which is similar to the know
behaviour of Portland cement based concrete 28.
Usually, lower curing temperature tends to
promote development of denser and more
homogenous microstructure.
Figure 2: Initial and final setting
times of SC-activated slag pastes.
a)
b)
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The heat curing could decrease the
crystallinity of the C-A-S-H 29. In addition,
it also tends to coarsen the pore structure due
to a higher reaction rate for C-A-S-H, in
comparison with the rate of diffusion. As a
result, the pores formed between denser
precipitates create a barrier inhibiting
additional dissolution and dispersion of ions 15.
4. CONCLUSIONS
The effects of carbonate activator
dosage, mixing procedures and curing
temperatures on sodium carbonate activated
high-MgO blast furnace slag pastes and
concretes were studied. The key findings
include:
Increasing the dosage of the sodium
carbonate reduced the initial and the final
setting time regardless of the mixing
procedure mostly due to the slow reaction
of the sodium carbonate. Addition of the
sodium carbonate dissolved in water one
hour before mixing, enhanced the
workability at higher activator dosage. In
contrast, increasing the amount of dry
sodium carbonate worsened the
workability. Higher amounts of sodium
carbonate increased the 28d compressive
strength when added either as dry or wet
powder. The recorded final compressive
strength values were generally higher for
the laboratory cured samples, however,
early age strength (1 and 7 days) were
higher for the heat cured concretes.
ACKNOWLEDGEMENTS
This research was funded by the Iraqi Ministry of Higher Education and Scientific Research,
Iraq. The authors would like to thank the technical staff of the laboratory at LTU, Sweden, and
Dr Oday Hussein and Dr Xinyuan Ke (University of Sheffield) for conducting the XRF
analysis.
Figure 3: 1, 7 and 28 days compressive
strength results of heat-cured concrete cubes
using the two mixing procedures; dry (D)
and wet(W).
Figure 4: 1, 7 and 28 days compressive
strength results of laboratory-cured concrete
cubes using the two mixing procedures; dry
(D) and wet(W).
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NEW GENERATION OF CONSTRUCTION MATERIALS
SESSION 9: Alternative binders
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International Conference on Sustainable Materials, Systems and Structures (SMSS2019) – 20-22 March 2019 – Rovinj, CroatiaNew Generation of Construction Materials
Edited by Marijana Serdar, Nina Štirmer, John Provis
RILEM Proceedings PRO 128ISBN: 978-2-35158-217-6VOL 1. ISBN: 978-2-35158-223-7 e-ISBN: 978-2-35158-218-32019 Edition
As part of the RILEM International Conference on Sustainable Materials, Systems and Structures (SMSS 2019) the segment New Generation of Construction Materials covers innovation, advances and improvement of construction materials, towards sustainable, intelligent and tailor-made solutions. This volume brings a selection of 100 peer-reviewed papers that were presented within the segment on construction materials. Top-ics include novel advances in raw materials for classical and alternative concretes, innovations in chemistry, application of nanotechnology in construction materials, and requirements for materials to suit the needs of construction automation.
The editors wish to thank the authors for their efforts at producing and delivering papers of a high standard. We are certain that this volume will be a valued reference of research topics in this important field and that it will, together with the other volumes from the SMSS conference, form a suitable base for discussion and suggestions for future develop-ment and research.
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