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The carbonation resistance of LVFA and HVFA based SCC made with coarse RCA have been investigated.
Compressive strength for all the SCC mixes has been reported for reference.
The microstructural investigation of LVFA and HVFA based SCC has been done by SEM and TGA tests.
Electrical resistivity has also been calculated for all the mixes.
The effect of replacement of NA with RCA has been evaluated in binary and ternary blended SCC mixes.
a r t i c l e i n f o a b s t r a c t
Article history: The present study investigates the carbonation resistance of Low Volume Fly Ash (LVFA) and High
Received 30 June 2016 Volume Fly Ash (HVFA) based Self Compacting Concrete (SCC) made with Coarse Recycled Concrete
Received in revised form 7 October 2016 Aggregates (RCA). In order to study the carbonation resistance of LVFA and HVFA based SCC mixes made
Accepted 9 October 2016
with RCA, accelerated carbonation tests were conducted for an exposure period of 4, 12 and 16 weeks.
Available online 14 October 2016
The results indicate that with the increase in RCA content as replacement of Coarse Natural Aggregates
(NA), decrease in the carbonation resistance of SCC mixes has been observed. The inclusion of metakaolin
Keywords:
(MK) as a mineral admixture has been found to compensate the loss in the carbonation resistance on
Low Volume Fly Ash
High Volume Fly Ash
account of substitution of NA with RCA to some extent. The current investigation also emphasises on
Self Compacting Concrete the microstructural study performed by Scanning Electron Microscopy (SEM) and Thermogravimetric
Coarse Recycled Concrete Aggregates Analysis (TGA) for validation of observed results.
Accelerated carbonation Ó 2016 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.conbuildmat.2016.10.067
0950-0618/Ó 2016 Elsevier Ltd. All rights reserved.
N. Singh, S.P. Singh / Construction and Building Materials 127 (2016) 828–842 829
and cost effectiveness and other long term performance aspects coefficients (CC) have been noticed respectively [40,41]. Since car-
[6–9]. The sustainability can also be achieved to some extent by bonation phenomenon is complex in nature as conflicting results
reducing the quantity of clinker in concrete and this can be possi- have been mentioned by many researchers.
ble only by adding different cement additions like FA, Silica Fume However, to the best of knowledge of the authors, no informa-
(SF), Metakaolin (MK) etc., which are having inherent pozzolanic tion on the carbonation resistance of LVFA and HVFA based SCC
and binding properties [5,7]. Hence, the use of cement additions mixes made with RCA is available. Thus, the main objective of this
has increased in cement industry to minimise the Portland Cement paper is to evaluate the carbonation resistance of LVFA and HVFA
(PC) content [9]. For achieving sustainability, adoption of FA in cur- based SCC mixes made with different replacement levels of NA
rent concrete manufacturing system has become necessary while with RCA. The emphasis here is to achieve a most sustainable
maintaining top priority for the durability aspect. SCC that can be used in civil engineering construction which com-
The production of Self Compacting Concrete (SCC) was initiated prises alternative materials both in the form of binders and RCA.
in Japan in the late eighties to compensate the shortcomings of The current investigation includes, in total ten number of SCC
Normally Vibrated Concrete (NVC). Due to numerous advantages mixes differentiated according to content of FA (LVFA and HVFA
in terms of improved mechanical and durability properties, the based mixes) and replacement levels of RCA. Herein, the study
SCC has gained world-wide recognition in very short time [10– examines the carbonation depth as main parameter of LVFA and
14]. As the trend of using SCC has increased, the researchers also HVFA based binary and ternary blends (PC, FA and MK) of SCC
put some efforts to make SCC more durable and sustainable by mixes made with varying quantities RCA. The performance of all
using different cement additions. The previous studies have the SCC mixes has been judged on the basis of their observed car-
reported that, addition of cement admixtures helps in enhancing bonation depths. Also, in present study an effort has been made to
the overall performance of the concretes e.g. the use of SF, MK, characterise those compounds which are key parameters for car-
Blast Furnace Slag (BFS) has been found to improve its mechanical bonation phenomenon, like Calcium Silicate Hydrates (CSH),
and long term properties [12,15]. However, the use of RCA in con- CaCO3, Ca(OH)2 etc., as all the mixes have been tested for micro
struction industry has been initiated in the last decade but its structural characterization. Specifically, Scanning Electron Micro-
implementation has been constricted in only few categories due scopy (SEM) and Thermogravimetric Analyses (TGA) have been
to its poor physical and mechanical properties [16–20]. The kind used to explore the carbonation mechanism at the microscopic
of inert material obtained from C&D waste in the form of RCA level. In addition to this, the compressive strength and electrical
has been employed in NVC and SCC and the influence of these resistivity of all the LVFA and HVFA based SCC mixes have also
materials has been examined in terms of physical, mechanical, rhe- been evaluated.
ological and durability properties [21–25]. The literature con-
firmed that replacing Coarse Natural Aggregates (NA) with RCA
degrades the performance of all types of concretes i.e. reduction 2. Experimental programme
in workability, compressive and tensile strengths etc. [26–31].
The reason behind the poor performance of using RCA lies in weak 2.1. Materials and mix proportions
Interfacial Transition Zone (ITZ), micro and macro cracks, pores in
adhered mortar, generation of fissures during its processing. Car- Portland Cement (PC) of grade 43 was used throughout the
bonation is a major risk for reinforced concrete structures because experimental programme. Locally available natural fine aggregates
it lowers alkalinity of concrete which results in enabling the exter- and NA of maximum size 10 mm were used. The RCA were pre-
nal aggressive agents to act [1,32]. Carbonation is a reaction of gas- pared in the laboratory by crushing and the maximum size of
eous atmospheric Carbon Dioxide (CO2) with the calcium-bearing RCA was also kept as 10 mm. Two basic SCC mixes containing
phases of concrete and is known to cause lowering of alkalinity low and high volume FA content and 100% NA were prepared as
leading to the corrosion of steel bars embedded in concrete [7,9]. shown in Table 1.
It depends on various factors like permeability of concrete, mois- These mixes were designated as LVFA and HVFA based mixes
ture content, concentration of environment’s CO2 and relative respectively. In each of these mixes, the replacement levels of NA
humidity. with RCA were kept at 0%, 50% and 100%. Fly ash was also replaced
A lot of research has been carried out to evaluate the carbona- approximately by 10% of MK in the mixes containing 50% and 100%
tion resistance of NVC made with NA and RCA and SCC made with RCA to obtain ternary blended mixes. Appropriate doses of poly
NA using low and moderate volumes of FA [21–22,33–42]. In addi- carboxylic-ether based superplasticizer and viscosity modifying
tion to this, direct influence of FA on carbonation depth for various agent were used to obtain adequate workability and viscosity
types of concretes has also been studied by numerous researchers respectively. The particle size distribution of PC, FA and MK is pre-
[31,33]. An increase of the order of 1.3–2.5 times in carbonation sented in Fig. 1. The grading curve of RCA was purposely kept com-
depths of NVC made with RCA has been observed compared to parable to the grading curve of NA used in present study. The
NVC made with NA [24,31]. The exceptional effects of FA was noted grading curves of NA and RCA used in the present study are shown
in another study in which carbonation depths of NVC made with in Fig. 2.
RCA were found to be lower in comparison to NVC made with A total number of 10 SCC mixes were developed with a water/
NA [33,35]. Another similar research was conducted in order to binder (w/b) ratio of 0.45 and total binder content of 615 kg/m3.
evaluate the effect of FA in NVC made with RCA. The results The binary control SCC mix of LVFA based mixes has been desig-
showed that, addition of FA affects the carbonation resistance. It nated as CFL-R0, whereas the rest of the mixes are designated as
has also been found that addition of FA decreased the carbonation CFL-R50, CFL-R100 containing 50% and 100% of RCA respectively.
resistance of NVC made with RCA for longer exposure periods Similarly, the ternary blended mixes containing MK are designated
[31,35]. Few of the investigations done on SCC indicated its higher as ‘CFLM-R50’ and ‘CFLM-R100’. Similar to LVFA based SCC mixes,
durability performance over NVC [21,36–37], with the presence of the binary mixes of HVFA based SCC mixes has been designated as
cement additions which supports in enhancing the microstructure CFH-R0, CFH-R50 and CFH-R100, whereas the ternary mixes are
and carbonation resistance [22,38]. In addition to this, the carbon- designated as CFHM-R50 and CFHM-R100. For details of the vari-
ation depths for RCA concrete depends mainly on water/cement ous mixes, their designations and description, reference may be
(w/c) ratio and curing periods, as higher and lower carbonation made to Table 2.
830 N. Singh, S.P. Singh / Construction and Building Materials 127 (2016) 828–842
Table 1
Mix proportioning for LVFA and HVFA SCC mixes.
100 results of the workability tests for all the mixes tested in this inves-
tigation are given in Table 2.
Table 2
Workability properties of LVFA and HVFA based SCC mixes.
Mix designation Mix description Slump flow V-funnel (s) Whether conforms to EFNARC guidelines
T50 D (mm)
(s)
LVFA based mixes
CFL-R0 PC + LVFA + 0%RCA 2.0 685 6.0 Yes
CFL-R50 PC + LVFA + 50%RCA 2.2 688 5.8 Yes
CFL-R100 PC + LVFA + 100%RCA 2.0 680 7.0 Yes
CFLM-R50 PC + LVFA + MK + 50%RCA 2.1 685 8.0 Yes
CFLM-R100 PC + LVFA + MK + 100%RCA 2.5 680 6.5 Yes
HVFA based mixes
CFH-R0 PC + HVFA + 0%RCA 3.3 695 5.5 Yes
CFH-R50 PC + HVFA + 50%RCA 3.5 690 5.8 Yes
CFH-R100 PC + HVFA + 100%RCA 3.6 680 6.7 Yes
CFHM-R50 PC + HVFA + MK + 50%RCA 4.0 670 9.0 Yes
CFHM-R100 PC + HVFA + MK + 100%RCA 4.1 670 9.5 Yes
20
2.3.4. Electrical resistivity test
The test was performed on surface dried specimens of size 10
100 mm 100 mm 100 mm after curing periods of 28 and
90 days. Electrical resistivity was measured by using ‘Four-Probe
0
Method’ commonly known as Wenner’s Array Four-Probe Method.
Mix combinations
In the current study, the combined or synergetic effects of PC,
FA and MK have been discussed mainly in reference to carbonation 7 Days curing 28 Days curing 90 Days curing
resistance and microstructural changes. An improved behaviour in
Fig. 3. Compressive strength test results for LVFA based SCC mixes.
carbonation resistance with incorporation of MK along with PC and
FA has been observed in both LVFA and HVFA based SCC mixes
(binary and ternary) made with RCA. Similarly, the improvement
40
Compressive strength (N/mm²)
3.2.1. LVFA based SCC mixes mance. The presence of MK as partial replacement FA has not been
The accelerated carbonation test results for an exposure period found to overcome the dominant nature of RCA for CFLM-R100
of 4, 12 and 16 weeks, after curing period of 28 days are presented mix. The observed increase in carbonation depths approaches to
in Fig. 6. In whole, an outstanding reduction in carbonation resis- 50%, 59% and 52% relative to CFL-R0 for the same exposure periods.
tance has been observed for mixes made with intermediate (50% The observed behaviour has been validated from the weak pore
RCA) and complete (100%) replacement of NA with RCA at both structure of RCA which is entirely different from that of NCA (as
low and high exposure periods w.r.t. the control mix. The recom- discussed in previous section). The presence of weak ITZ, high
pensing effect of MK has been noticeable from the observed fig- porosity (Fig. 5a, Fig. 5b), and low density became responsible in
ures, as lower carbonation depths have been attained. deteriorating the carbonation resistance in concrete mixes
The results presented in Fig. 6 revealed that carbonation depths [70,71]. However, the remedial effect of addition of MK can also
for CFL-R50 and CFL-R100 mixes have been found to increase by be seen, when CFL-R100 mix has been compared with CFLM-
35% and 60% respectively w.r.t. CFL-R0 mix for an exposure period R100 mix, as improvement in carbonation resistance has been
of 4 weeks. Correspondingly, as projected the carbonation depth in noticed. The shrinkage in carbonation figures has also been noticed
both cases increases, with increase in exposure period. The after both exposure periods when CFLM mixes are mutually com-
observed behaviour has been found to show similarity with previ- pared with CFL based mixes. The much anticipated improvement
ous literature available on NVC, in which higher carbonation in carbonation resistance has been obvious due to inherent action
depths have been noted with higher percentage replacements of of MK as discussed above.
NA with RCA when compared to control mix (CFL-R0) [68,69]. An
increment of around 1.4 and 1.6 times in carbonation depths has
3.2.2. HVFA based SCC mixes
been observed for CFL-R50 and CFL-R100 mixes after an exposure
The results for the carbonation depths for an exposure period of
period of 12 and 16 weeks relative to control mix (CFL-R0). The
4, 12 and16 weeks are compiled in Fig. 7. The increase in the car-
experimental investigation also demonstrated that development
bonation depth viz. a viz CFH-R0 mix has been found to be quite
of increment, in decreasing carbonation resistance appears to be
substantial on account of substitution of NA with RCA in HVFA
less prominent in CFL-R50 mix rather than CFL-R100 mix. The rea-
based SCC mixes, after curing period of 28 days and 4 weeks of
son behind this behaviour is the presence of remained alkalinity
exposure. The maximum increment of 53% and 29% in carbonation
due to higher percentage replacements of RCA. Moreover, the
depth has been noted for CFH-R100 mix followed by CFH-R50 mix
non-completion of pozzolanic reactions between PC and FA and
in association with the CFH-R0 mix. Similarly, the increase has
faster consumption of calcium hydrates (CH) during hydration
been restricted to 34%, 21% and 34%, 24% when observed after 12
reactions probably seemed to be responsible for higher increase
and 16 weeks of exposure period respectively. Previous literature
in carbonation depths.
reported that, higher replacements of FA with PC have decreased
the carbonation resistance [44]. On examining carefully, it can be
seen that the increase in percentage in carbonation depths for
3.2.1.1. Effect of MK in LVFA based SCC mixes. The inclusion of MK in
HVFA based SCC mixes follows roughly the identical trend as in
SCC mixes made with RCA has been found to recover the loss in
case of LVFA mixes. The FA particles are unable to provide their
carbonation resistance due to presence of RCA. The advantageous
contribution at the initial ages rather than higher ages due to lesser
effect of MK has evidently been observed in case of CFLM-R50
production of CSH and other hydration products. Moreover, the
mix after exposure period of 4 weeks (and at the end of 28 days
probable formation of excess of ettringite due to non-completion
curing), since an increment in the carbonation depth by 20% has
of pozzolanic reactions leads to further decrease in carbonation
been observed. This increase in carbonation depth restricts to
resistance.
merely 13% for 12 and 16 weeks of exposure for the same curing
period. Higher reactivity of MK with pozzolanic products (like Ca
(OH)2 etc.) at early ages appeared to be responsible for lowering 3.2.2.1. Effect of MK in HVFA based SCC mixes. Fig. 7 also represents
the carbonation depths [66]. However, the development of CSH the impact of incorporation of MK in HVFA based SCC mixes. The
gel at higher ages helped in attaining quite satisfactory perfor- observed increase in carbonation depths has been found to be
35
30
Carbonation depth (mm)
25
20 4 Weeks
12 Weeks 28 days
curing
15 16 Weeks
4 Weeks
10 12 Weeks 90 days
curing
16 Weeks
5
0
CFL-R0 CFL-R50 CFL-R100 CFLM-R50 CFLM-R100
(Control)
Mix combinations
Fig. 6. Accelerated carbonation test results for LVFA based SCC mixes at different exposure periods after curing period of 28 days and 90 days.
834 N. Singh, S.P. Singh / Construction and Building Materials 127 (2016) 828–842
60
50
4 Weeks
28 days
30 12 Weeks curing
16 Weeks
4 Weeks
20 90 days
12 Weeks curing
16 Weeks
10
0
CFH-R0 CFH-R50 CFH-R100 CFHM-R50 CFHM-R100
(Control)
Mix combinations
Fig. 7. Accelerated carbonation test results for HVFA based SCC mixes at different exposure periods after curing period of 28 days and 90 days.
lower than in mixes made without incorporation of MK when com- 16 weeks of exposure. Likewise, for HVFA based SCC mixes, an
pared to CFH-R0 mix. For example, incorporation of MK in CFHM- increase to an extent of around 17% and 27% has been noticed
R50 mix, the reduction in the carbonation resistance after 4 weeks, for CFH-R50 and CFH-R100 mixes respectively after 4 weeks of
12 weeks and 16 weeks of exposure has been observed to be 22% exposure period. For the same mixes, the increase in carbonation
against 29%, 20% in contrast to 14% and 21% to 17% respectively depth approaches to 12%, 29% and 30%, 45% for 12 weeks and
for SCC mix made with 50% RCA (CFH-R50 mix) only. For similar 16 weeks of exposure period. The anti-carbonation ability has
conditions, the increase in carbonation depth drops approximately improved significantly after curing period of 90 days. For e.g. in
from 53% to 43%, 34% to 18% and 34% to 26% for CFHM-R100 mix case of CFHM-R100 mix, the percentage increase in carbonation
relative to CFH-R100 mix respectively. It can be seen from Fig. 1 depth which was initially 43% after curing period of 28 days has
that MK used as blending material has better fineness than FA been reduced to 17% after curing period of 90 days for an exposure
which helps in making concrete mixes denser, consequently resist- period of 4 weeks respectively. Similar performances have been
ing the ingression of CO2. In addition to this, the rate of increase of seen for CFHM-R50 mix for both exposure periods. The enhanced
carbonation depth indirectly depends on content of Ca(OH)2 and performance can be seen from the reduction in percentage increase
the earlier consumption of Ca(OH)2 due to presence of highly reac- for all the mixes.
tive MK particles leads to improve the comprehensive performance The most probable reason for the improvement of carbonation
of the concrete mixes. resistance in all SCC mixes is the condensing of CSH gel during
development of time with enhanced quantity. This dense phase
3.2.3. Effect of curing of CSH gel supports in filling the micro and macro pores, cracks
The long duration performance in terms of carbonation resis- and loose joints in SCC mixes, which results in resisting the further
tance of the LVFA and HVFA based SCC mixes can be judged after ingression of CO2. Congruently, the variation also occurred due to
higher curing period (90 days). The pozzolanic reactions occurred reduction in the quantity of CaCO3 in concrete mixes which tran-
between blending materials in concrete mixes has been incapable spires due to completion of pozzolanic reactions of the hydrated
to compensate the dilution and micro filler effect at 28 days of cur- products. The overall performance of any concrete depends on
ing [72]. Under same conditions, the carbonation depths have been two main factors (1) the completion of hydration process and (2)
calculated after curing period of 90 days for an exposure period of prolonged water curing, which helps in improving the short as well
4 weeks, 12 weeks and 16 weeks. The detected values are pre- as long term properties. The steadiness of curing phenomenon sup-
sented in Figs. 6, 7. This trend of variation in carbonation resistance ports in dipping the porosity of concrete by many previous litera-
is fairly alike to that noted for 28 days curing as carbonation depth ture studies [41,73]. Based on the achieved results, the prolonged
changes significantly. The results of carbonation depths have been water curing adopted in this investigation absolutely backs in nul-
found to be quite low in comparison to values found for early age lifying the negative effects of poor RCA based mixes to some
curing of 28 days. extent, as the carbonation depths have been reduced to significant
In case of LVFA based SCC mixes, the maximum increase in car- levels.
bonation depths limits around 44% and 63% for CFL-R50 and CFL-
R100 mix relative to control concrete (CFL-R0) after 4 weeks of 3.2.4. Relation between compressive strength and carbonation
exposure respectively. The carbonation resistance has decreased coefficient
with 12 weeks and 16 weeks of exposure for CFL-R100 mix by The rate of carbonation is defined by the following expression
42% and 36% whereas lower increment of 17% and 14% has been [41]:
observed for CFL-R50 mix. The best performance has been wit- p
C ¼ k ðTÞ ð1Þ
nessed in case of CFLM-R50 mix in which carbonation depth have
been reduced to an extent of 25% after 4 weeks of exposure, where C = depth of carbonation (in mm); k = coefficient of carbona-
whereas lower variations have been noted after 12 weeks and tion; T = time (in weeks/days). Using the above relation, the values
N. Singh, S.P. Singh / Construction and Building Materials 127 (2016) 828–842 835
exposure)
9
2.0
25 30 35 40
8
Compressive strenth (N/mm²)
7 12 Weeks exposure
Fig. 9b. Relation between carbonation coefficients with compressive strength for
R² = 0.9651 4 Weeks exposure HVFA based SCC mixes after 90 days of curing period.
6
3.3.1. Scanning electron microscopic analysis completion of reactions of hydrated products deteriorates the per-
Scanning electron microscopic imaging was carried out on the formance of concrete matrix.
fracture surfaces of all SCC mixes after compression tests. The
images for LVFA and HVFA based SCC mixes are presented in
Figs. 10A, 10B, 10C, 11A, 11B, and 11C after curing periods of
3.3.1.2. HVFA based SCC mixes. The higher values of carbonation
28 days and 90 days respectively.
depths obtained for HVFA based SCC mixes has clearly been attrib-
uted to the high content of Ca(OH)2, ettringite and weak formation
of CSH gel crystals. Figs. 11A(a) and 11A(b) show the SEM images
3.3.1.1. LVFA based SCC mixes. From Figs. 10A(a) and 10A(b), it can for CFH-R0 mix.
be noticed that the CSH gel obtained in the case of control mix The presence of platy, hexagonal shaped Ca(OH)2 and irregular
(CFL-R0) has found to be highly dense in nature at both the ages. fibrous growths of CSH crystals has been observed after 28 days of
An array of irregular blocks/sheets has been observed after 28 days curing whereas, with development of curing period of 90 days the
of curing whereas with development of curing period the dense overlapping of these compounds has been attained. At later ages,
rocky shaped CSH gel crystals have been observed. The observed FA reduces the amount of Ca(OH)2 produced during hydration pro-
dense and perfect nature of CSH gel is mainly responsible for filling cess and transforms the Ca(OH)2 into blocky C-S-H gel. The pres-
the micro and macro flaws of concrete matrix more efficiently. The ence of micro and macro pores in CFH-R50 mix has also been
change in shape of crystals has been observed for CFL-R50 mix for confirmed with the observation of ettringite. The ettringite is a sec-
both curing periods when compared to control mix (CFL-R0). ondary product of the hydration chemistry and it is commonly
Figs. 10B(a) and 10B(b) present layered CSH gel in hollow and found in voids and cracks [76]. The formation of highly porous
thin cloud form with needle shaped ettringite after 28 days. The CSH gel and non-completion of hydration products is responsible
presence of hollow/weak shapes of CSH gel proved the lag in rate for the further ingression of CO2 in concrete matrix. The presence
of hydration compared to control mix. After 90 days of curing per- of ettringite in fissures and in form of web can be noticed from
iod the thick blocks of CSH have been found to appear along with Figs. 11B(a), 11B(b). The worst behaviour for CFH-R100 mix can
presence of continuous fissures and gaps. The loose structure of the be noticed from Figs. 11B(c), 11B(d) in which presence of only
hydration products has been observed quite prominent in CFL- ettringite and very weak and foam shaped of CSH gel. The presence
R100 mix compared to control mix (CFL-R0). The presence of of significantly porous CSH, Ca(OH)2 and ettringite at later ages
voids/thick gaps and highly porous CSH gel can be seen from confirms the poor resistance against carbonation.
Fig. 10B(c) and uneven, irregular grains/ semi-circular shape has Figs. 11C(a) and 11C(b) show a compact formation of hydration
been seen from Fig. 10B(d), after 28 days and 90 days of curing per- products and quite reduced content of Ca(OH)2 crystals due to
iod respectively. The non fusion of these CSH gel crystals leads to occurrence of additional reactions. SEM images demonstrated a
an increase in the probability of easy sequestration of CO2 in con- more compact microstructure, which indicates rapid formation of
crete mixes. The presence of MK and FA particles along with ettrin- CSH gel in presence of MK and additional FA. The absence of cracks
gite (needle shaped structures) has been observed clearly from and voids at micro and macro levels made the CFHM-R50 mix com-
Fig. 10C(a) in case of CFLM-R50 mix. The change in shape of CSH parable resistant to carbonation. The observed decrease in carbon-
crystals has been evident from the occurrence of additional reac- ation depth as compared to mixes without inclusion of MK in
tions of hydrated products with MK, as thick clouds of CSH gel preceding section has clearly justified from the noticed behaviour.
can be clearly observed. Meanwhile, the presence of insignificant In parallel way relatively loose, scattered and flabellate shape of
content of ettringite validated the advantageous effect of MK. After CSH gel has been observed for CFHM-R100 mix after 28 days in
90 days of curing in Fig. 10C(b), the CSH gel has overlapped with Fig. 11C(c). The presence of unreacted spherical shaped MK and
each other making highly condensed state in concrete matrix, FA particles has also observed in voids of CSH gel, which indicates
which hampers the probability of further ingression of CO2, leading the slight improvement in carbonation resistance. The slight
to an increase in the carbonation resistance. The highly improved improvement in properties of SCC mixes comprised of MK is due
dense microstructure upon addition of MK has also proved to be to the faster consumption of Ca(OH)2. The existence of unreacted
the major cause for the increased compressive strength and ettringite in Fig. 11C(d) confirms the expected slight change in car-
decreased carbonation depths. Figs. 10C(c) and 10C(d) depicts bonation depths at curing periods. These types of flaky crystals are
the completely irregular and distorted flabellate, beaded and cune- unable to make a condensed/viscous concrete mix due to brittle
ate shape of CSH gel for CFLM-R100 mix. The observed change nature, consequently resulting in creation of immature microstruc-
seemed to be obvious due to complete replacement of NCA with tures. This seems to be attributing to generation of additional pores
RCA. Most of the cracks remain unfilled due to less quantity of after evaporation of water from the surface of RCA which leads to
CSH gel. Moreover, extremely porous nature of CSH gel and non- easy assessment of CO2.
Dense rocky
shaped CSH
Densely layered
irregular shape CSH (a) (b)
Fig. 10A. SEM images for CFL-R0 (a) 28 days (b) 90 days of curing.
N. Singh, S.P. Singh / Construction and Building Materials 127 (2016) 828–842 837
Cloud Blocks of
form CSH CSH
(a) (b)
(c) (d)
Uneven shape
Highly Porous CSH with pores
CSH
Fig. 10B. SEM images for CFL-R50 (a) 28 days (b) 90 days and CFL-R100 mix (c) 28 days (d) 90 days of curing.
FA and MK
particles with Dense rocky
ettringite shaped CSH
(a) (b)
(c) (d)
Fig. 10C. SEM images for CFLM-R50 (a) 28 days (b) 90 days and CFLM-R100 mix (c) 28 days (d) 90 days of curing.
3.3.2. Thermogravimetric analysis 3.3.2.1. LVFA based SCC mixes. Fig. 12a presents the TGA curves for
Thermal gravimetric analysis (TGA) determines the change in LVFA based SCC after curing period of 28 days. The relative differ-
weight of powdered samples w.r.t. change in temperature. The ence in weight loss between the CFL-R50 and the control mix CFL-
method provides an excellent estimation of the compounds quan- R0 is marginal as indicated by the percentage weight loss of 0.83%
titatively which are chiefly responsible for carbonation process. and 0.63% attributed to Ca(OH)2 respectively. Similar observation
The obtained TGA curves are divided as: 38–125 °C: dehydration has been witnessed in the case of CFLR-100, which shows the cor-
of pore water; 125–425 °C: dehydration of CSH, 425–475 °C: de- responding weight loss of about 0.89%. This is again minimal when
hydroxylation of Ca(OH)2 and 475–765 °C: and de-carbonation of compared to the control mix CFL-R0. Weights lost by the samples
CaCO3 [77,78]. Since carbonation process is directly related to con- were found to be very less relative to control mix (CFL-R0). The
tent of Ca(OH)2 and CaCO3, therefore, herein the stress is given only weight loss reduction for MK based LVFA mixes shifts to 0.67%
given on the third and fourth stage of the obtained TGA curves. and 0.76% for CFLM-R50 and CFLM-R100 mixes respectively, at
838 N. Singh, S.P. Singh / Construction and Building Materials 127 (2016) 828–842
Hexagonal or Overlapping of
Platy shape Platy shape
Ca(OH)2 Ca(OH)2 and CSH
(a) (b)
Fig. 11A. SEM images for CFH-R0 (a) 28 days (b) 90 days of curing.
Ettringite web
(a) (b)
Ettringite web
Fig. 11B. SEM images for CFH-R50 (a) 28 days (b) 90 days and CFH-R100 mix (c) 28 days (d) 90 days of curing.
same cuing period. The significant differences of 0.54%, 0.86% and The results clearly show that the percentage weight loss
1.16% in weight loss corresponding to CaCO3 for CFL-R0, CFL-R50 corresponding to Ca(OH)2 and CaCO3 was lower in the SCC mixes
and CFL-R100 mixes have been noticed respectively. Likewise, for containing PC + FA + MK based mixes compared to that of SCC
CFLM-R50 and CFLM-R100 mixes the loss has been limited to mixes made with PC + FA. The generation of additional CSH (as
0.65% and 0.99%. Similarly, quite low percentage reductions for discussed in preceding section in detail) probably the sole cause
weight loss for all the mixes have been observed in Fig. 12b after for this positive change. The observed reductions in weights for
90 days of curing. carbonated products (Ca(OH)2 and CaCO3) has also been evident
from the change in nature of aggregates (replacement of NA with
3.3.2.2. HVFA based SCC mixes. Congruently, Figs. 13a and 13b RCA) and the incorporation of higher content of FA. The
demonstrations the TGA curves after curing period of 28 and experimental behaviour from TGA results justified the trends
90 days. The results for all HVFA based SCC mixes revealed in for change in carbonation resistance as reported in preceding
accordance of percentage loss of Ca(OH)2 and CaCO3. The weight sections.
loss reduction for CFH-R0, CFH-R50 and CFH-R100 varied as
0.45%, 0.5% and 0.66%, whereas for CFHM-R50 and CFHM-R100 3.4. Electrical resistivity test result
the loss for Ca(OH)2 limits to 0.57% and 0.65% respectively. The
weight lost for CFH-R0, CFH-R50 and CFH-R100 matching to CaCO3 Electrical resistivity is also related to corrosion of concrete. It
ranges as 0.42%, 0.52% and 0.54% respectively. Similarly, for CFHM- provides a good indication regarding the resistance offered to the
R50 and CFHM-R100 mixes, the loss constricted up to 0.42% and moving ions during development of concrete. Higher will be the
0.43% accordingly. The significant changes in trends for TGA curves resistivity lesser will be the chances of corrosion and vice versa.
can be seen after 90 days of curing as much flatter curves have The electrical resistivity test results are compiled in Figs. 14a,
been obtained corresponding to the similar temperature change. 14b. The presence of higher moisture content of RCA creates a
N. Singh, S.P. Singh / Construction and Building Materials 127 (2016) 828–842 839
(a) (b)
Merging of
FA and MK platy shape
particles in CSH
porous CSH
Fig. 11C. SEM images for CFHM-R50 (a) 28 days (b) 90 days and CFHM-R100 mix (c) 28 days (d) 90 days of curing.
Fig. 12b. TGA curves for LVFA based SCC mixes after 90 days of curing.
Fig. 12a. TGA curves for LVFA based SCC mixes after 28 days of curing.
Table 3
Electrical resistivity range corresponding to
corrosion risk [79].
4. Conclusions
25 90 Days curing
based SCC mixes. Similarly, an increase in carbonation depth
20 reaches nearly to 53% for HVFA based SCC mixes after 4 weeks of
exposure period. Likewise in case of compressive strength, the car-
15 bonation resistance has been influenced with addition of MK.
A highly agreeable linear relationship between carbonation
10 depth and compressive strength was observed for both curing peri-
ods in cases of LVFA and HVFA based mixes as all R2 values have
5 found to be more than 0.80 (>80%). Prolonged curing for all the
SCC mixes has proved to be highly beneficial as satisfactory perfor-
0 mance in terms of compressive strength and carbonation resis-
tance has been achieved.
The microscopic analysis performed by SEM and TGA confirms
the attained results of the experimental study w.r.t. carbonation
behaviour quite adequately. The quantitative and qualitative anal-
Mix combinations
ysis performed by SEM and TGA also provides a good estimation of
Fig. 14a. Electrical resistivity test results for LVFA based SCC mixes. the hydration and carbonated materials generated during develop-
ment of concrete mixes.
In the case of electrical resistivity results, a maximum reduction
of around 49% and 52% was observed for LVFA and HVFA mixes
30 28 Days curing made with 100% of RCA after 28 days of curing. The electrical resis-
tance has found to increase with increase in curing period in all the
Resistivity (K Ohm-cm)
25 90 Days curing
SCC mixes, whereas an increase of about 24% and 15% has been
20 noticed after 28 days of curing for LVFA and HVFA based mixes
respectively.
15
Acknowledgements
10
The financial assistance in the form of fellowship to the first
5
author from the Ministry of Human Resource Development
0 (MHRD), Government of India is appreciatively acknowledged.
The authors also acknowledge the support of the staff of Structures
Testing Laboratory at Dr B R Ambedkar National Institute of Tech-
nology, Jalandhar, India during the experimentation work reported
in the paper.
Mix combinations
Fig. 14b. Electrical resistivity test results for HVFA based SCC mixes. References
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