Ain Shams Engineering Journal: T. Chandra Sekhara Reddy, A. Ravitheja

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Ain Shams Engineering Journal 10 (2019) 23–32

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Ain Shams Engineering Journal


journal homepage: www.sciencedirect.com

Macro mechanical properties of self healing concrete with crystalline


admixture under different environments
T. Chandra Sekhara Reddy ⇑, A. Ravitheja
GPR Engineering College, Kurnool, Andhra Pradesh, India

a r t i c l e i n f o a b s t r a c t

Article history: The civil research community has been attracted to concrete with self-healing properties since they are
Received 8 May 2017 an intelligent solution for sustainable infrastructures with long duration. The present study is analyzing
Revised 27 September 2017 the self- healing capability of early age and structural cracks in concrete by using crystalline admixture as
Accepted 10 January 2018
self-healing agent under four different exposure conditions by assessing the regained mechanical prop-
Available online 26 December 2018
erties of concrete. Physical (morphological) and chemical composition of the hardened pastes, were stud-
ied using Fourier transform infrared spectroscopy (FTIR) and energy-dispersive spectroscopy (EDS). The
Keywords:
analysis showed that for all exposure conditions the compressive strength and split tensile strength of
Self-healing concrete
Early age cracks
the tested concrete with crystalline admixture (CCA) samples regains after early age and structural
Structural cracks cracks. This is due to substantial increase in the calcite content which is evident from SEM-EDS and
Crystalline admixture FTIR analysis.
Ó 2018 The Authors. Published by Elsevier B.V. on behalf of Faculty of Engineering, Ain Shams University.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-
nd/4.0/).

1. Introduction tanks storing highly toxic waste and radioactive waste disposal
facilities. The ability of a material to repair itself with only a little
Cracking in concrete structures not only reduces designed ser- or almost no external help to regain its desirable mechanical prop-
vice life but also causes corrosion of steel bar due to weathering erties after it has incurred damage or degradation is attributed as
action. Some kind of human intervention is required to inspect its self-healing property [1]. Biological entities like bones, muscles
and repair the cracks in concrete. In some cases, however, it is dif- and trees, have the ability of self-healing [2].
ficult for engineers to access damaged sites for repair work because The use of self-healing materials undoubtedly represents an
of their location and/or environmental conditions. Examples of innovative and cutting edge issue for sustainable civil engineering
above scenario are underground structural members, walls of industry. The requirement of unexpected maintenance and repair
can be eliminated for a standard prolonged duration of time result-
Abbreviations: WI2, Specimen pre cracked at 2nd day and cured in water
ing in creation of better and more sustainable civil infrastructure
immersion; WC2, Specimen pre cracked at 2nd day and cured in water contract; by using building materials with self-healing properties [3]. Most
WD2, Specimen pre cracked at 2nd day and cured in wet-dry; AE2, Specimen pre of the research work for self-healing materials have been concen-
cracked at 2nd day and cured in air exposure; WI28, Specimen pre cracked at 28th trated on cracks closing and regaining their durability and strength
day and cured in water immersion; WC28, Specimen pre cracked at 28th day and
based mechanical properties.
cured in water contract; WD28, Specimen pre cracked at 28th day and cured in wet-
dry; AE28, Specimen pre cracked at 28th day and cured in air exposure; CCA, Autogenous healing and autonomous/engineered healing are the
Concrete with Crystalline admixture; CA, Crystalline admixture; SEM-EDS, Scanning two self-healing modes of concrete. The natural and intrinsic ability
electron microscopy with Energy Dispersive X-Ray Spectroscopy; FTIR, Fourier to self-heal the small cracks in concrete owing to its composition is
transform infrared spectroscopy. termed as autogenous healing. Hydration of cement and calcium
⇑ Corresponding author at: Civil Engineering Department, GPR Engineering
College, Kurnool 518007, Andhra Pradesh, India.
carbonate precipitation is the dominant cause for autogenous heal-
E-mail address: tcsreddy61.ce@gprec.ac.in (T. Chandra Sekhara Reddy). ing. There are other modes for execution of this process too. An engi-
Peer review under responsibility of Ain Shams University. neered healing process developed for enhancing the self-healing
properties of a concrete element is termed as autonomous healing.
Autonomous/engineered healing divided as ’passive’ and ’active’
modes. Activating the mechanism by human intervention is active
Production and hosting by Elsevier mode and without human intervention is passive mode [4–10].

https://doi.org/10.1016/j.asej.2018.01.005
2090-4479/Ó 2018 The Authors. Published by Elsevier B.V. on behalf of Faculty of Engineering, Ain Shams University.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
24 T. Chandra Sekhara Reddy, A. Ravitheja / Ain Shams Engineering Journal 10 (2019) 23–32

It is observed that a lot of work has been done on to improve the cylinder of size 150 mm  300 mm. In the first 24 h the samples
self-healing capability in concrete, i.e. the use of microencapsu- were allowed to be in the steel mould at ambient condition.
lated healing agents, super absorbent polymers (SAPS), sealing Total 10 group of specimens were cast. Two groups are used for
materials in brittle tubes, shape memory alloys, bacterial concrete improvement of strength characteristics without CA and with CA,
and the use of crystalline admixtures [11–30]. Crystalline admix- four groups are used for early age cracks self-healing study and
tures (CA) is permeability decreasing mixture which have hydro- remaining four groups are used for structural cracks self-healing
philic properties. The behavior of these products is still partially study under four exposure conditions respectively.
unknown: in fact, the ACI TC 212 report states that the concrete
compounds reacting with CA are tricalcium silicates, while other 2.2. Materials and mix proportions
authors [31] indicate calcium hydroxide as the reactive. The quan-
titative assessment of crack sealing/healing on the recovery of In this present work fiber reinforced concrete has been used.
engineering properties of concrete still needs a much deeper inves- Fibers can be an excellent counter action against crack causing
tigation. Most of the surveyed studies focused on the variation of forces during both the pre-cracking period and post-cracking per-
water permeability and only very few among them analyzed the iod [47,48]. This can be done since the emphasis of this study is
effects on recovery of mechanical properties, in case evaluated by to improve the healing properties of the specimens. To suppress
means of non-destructive techniques. It was anyway pointed out the cracks from branching excessively the quantity of steel fiber
that recovery in signal transmission was not as spectacular as that was fixed at 40 kg/m3. This is with adherence to the criterion of
in permeability [32–36]. In recent studies, it is reported that controlling crack openings. The materials used in the CCA as shown
delayed hydration was the main process in young concrete and in Table 1.
carbonation was more relevant for older concrete. Still with refer-
ence to the autogenous healing process, the use of different addi- 2.3. Experimental methodology
tions such as fly ash or blast furnace slag and their increase of
the delayed hydration enhances self-healing capacity of concrete Four stages of methodology adopted for studying the effects of
[37–42]. The presence of crystalline additive in concrete improves self-healing of concrete samples:
its self-healing properties. Immersion in water improves the higher
self-healing properties, for higher crack widths especially, as 1. Determination of mechanical properties of normal concrete and
expected. [31,43–46]. concrete with crystalline admixture (CA) at 28 days.
2. Creation of control damage in the specimens
1.1. Research significance (a) Early age cracks
(b) Structural cracks
The mechanical parameters and crack closing ability are taken 3. Exposure simulation
as healing properties for analyzing the influence of crystalline 4. Evaluation of the regained mechanical properties
admixture as a self-healing property enhancer. The results of this
analysis is obtained as the performance parameters of healing of 2.3.1. Creation of control damage in the specimens
early age and structural cracks. Exposure to four different environ- Cube and Cylindrical specimens were pre cracked at the age of
mental conditions are done and comparative study is done by 2 days for early age cracks and 28 days for structural cracks [49],
investigating them. inducing a controlled damage by means of a compression test
The range of widths of the cracks were between 0.10 and and splitting test (Fig. 1). The crack width measurement employing
0.40 mm for all the four cases. By varying the combination of the calibration ruler of optical micrometer while conducting the
experimental parameters, the healing property’s efficiency limits compression and splitting test obtains crack dimensions accurately
were analyzed. New perspectives on the use of crystalline admix- with the range of 0.2–0.4 mm.
tures as self healing agents in engineering applications where Four environmental exposures created for early age and struc-
water tightness is a key factor. tural after pre cracking of specimens were studied in order to
determine the effect of humidity on the self-healing capability of
the cracked specimens.
2. Experimental program and methodology
1. Water immersion (WI): Immersion in tap water continuously
2.1. Experimental program 2. Wet-dry cycles (WD): Immersion in tap water for 3.5 days and
air exposure for others 3.5 days.
Self-healing capability of the concrete is assessed by elevated 3. Water contact (WC): A layer of water about 2 cm on one sur-
strength regain capability of cracked specimens after healing. The face, Additional water was supplied to maintain the water layer.
crack width between 0.2 and 0.4 mm is maintained. 4. Air exposure at laboratory conditions (AE): Storage of the spec-
As the most shrinkage cracks occurs few days after casting, pre imens in normal atmospheric air conditions.
cracking is fixed at 2 days for early age cracks. Most of the struc-
tural cracks occur in the service life hence pre cracking is fixed at 2.3.2. Evaluation of the regained mechanical properties
28 days for structural cracks. The strength healing capability of Since the self-healing properties are projected to increase, a cor-
concrete with 1.1% of CA is studied under different environmental responding increase in the value of stiffness and cracking loads are
exposures like water immersion (WI), water contact (WC), wet-dry expected from the stage of initial loading to reloading. First crack-
(WD) and air exposure (AE) by assessing regained mechanical ing load lapsing recovery (R) was employed to calculate the
properties. improvement in self-healing strength using Eq. (1) given below.
This study includes assessment of regained mechanical proper-
ties due to self healing specimens under different exposures and P healed
R¼ C
 100 ð1Þ
strength properties of control concrete and crystalline admixture P Virgin
C
concrete specimens. Concrete cubical moulds of size 150mm3w-
erecast for the determination of compressive strength of concrete where Phealed
C and P Virgin
C are the critical loads at fracture for the
and split tensile strength of concrete is determined by casting healed and virgin specimen respectively.
T. Chandra Sekhara Reddy, A. Ravitheja / Ain Shams Engineering Journal 10 (2019) 23–32 25

Table 1
Mix proportions of CCA concrete.

Material Cement(Kg) W/C Gravel (Kg) Gravel (Kg) Sand (Kg) Steel fibers (Kg) Crystalline admixture (Kg)
(20–12.5 mm) (12.5–4.75 mm)
CCA 425.5 0.45 599 599 656.5 40 4.68

Fig. 1. Pre-cracking process of concrete specimen.

3. Results and discussion cured for 42 days in WI28 and WC28 has increased by 13.98%
and 7.72% compared with compressive strength of CCA after
3.1. Compressive strength 28 days and WD28 and AE28 has decreased by 9.79% and 23.82%
compared with compressive strength of CCA after 28 days shown
Compressive strength was used to evaluate whether the mate- in Fig. 3. Results of the recovery of compressive strength can be
rial was able to recover some of its strength after acquiring some attributed to the self-healing of these pre existing micro cracks,
minor damage. The samples were then left to heal for 42 days. due to hydration of anhydrous particles of cement and especially
Compressive strength of concrete with CCA shows an 11.457% by the activating effect of the crystalline admixture, on the sur-
increase in strength compared to normal concrete which is attrib- faces of these micro cracks. This is determined as a percentage
uted to the filling of voids by CASAH and calcite content. Com- of gain of mechanical properties for WI28 and WC28. Compressive
pressive strength of concrete with early age cracks cured for strength recovery of CCA after healing of early age and structural
42 days in WI2, WC2, WD2 and AE2 has decreased by 7.18%, cracks with respect to compressive strength of CCA in WI, WC,
4.47%, 15.29% and 36.07% compared with compressive strength WD, AE is 90–115%,85–110%,75–95% and 55–80% respectively
of CCA after 28 days curing due to insufficient calcite formed are shown in Fig. 4. It could be noted that CA in the concrete
inside the crack. The strength between the crack surface and should be added in optimum proportions, considering their reac-
new calcite is most likely weaker compared CCA matrix as shown tivity and filling of cracks s desired for improving the autogenous
in Fig. 2. Compressive strength of CCA with structural cracks self-healing capacity.

Fig. 2. Compressive strength of CCA after early age cracks healing under different exposures.
26 T. Chandra Sekhara Reddy, A. Ravitheja / Ain Shams Engineering Journal 10 (2019) 23–32

Fig. 3. Compressive strength of CCA after structural cracks healing under different exposures.

Fig. 4. Percentage compressive strength recovery of CCA after early age and structural cracks healing under different exposures.

3.2. Split tensile strength analysis 3.3. Load displacement curve

Split tensile strength with CA after 28 days curing in water is High deformation capacity and energy dissipation capacity are a
increased 35% when compared to normal concrete. Split tensile paramount requirement for concrete materials used in structural
strength of concrete with early age cracks cured for 42 days in WI2- application as shown in Figs. 8 and 9. It is observed that the incor-
WC2, WD2 and AE2 has decreased by 14.43%, 25.98%, 26.50% and poration of CA in concrete results increased in deformation capac-
50.13% compared with Split tensile strength of CCA after 28 days ity of concrete which is due to the formation of hydrated products
curing. Split tensile strength of CCA structural cracks cured for at larger scale. It can be observed that the healed concrete under
42 days in WI28 has increased by 2.88% compared with split tensile exposure for 2 days and 28 days pre crack has regained its defor-
strength of CCA after 28 days and WD28, WC28 and AE28 has mation capacity.
decreased by 3.67%, 16.83% and 26.02% compared with Split tensile It is therefore, deduced that crystalline admixture inclusion
strength of CCA after 28 days Figs. 5 and 6. Split tensile strength results formation of hydrated products at larger scale. These
recovery CCA after healing of early age and structural cracks with hydrated products heal the shrinkage cracks and pores in concrete
respect to split tensile strength of CCA in WI, WC, WD, AE is 80– matrix. The hydrated products also enhance the load carrying
105%, 70–100%,70–90% and 45–80% respectively are shown in Fig. 7. capacity and strain capacity of concrete.
T. Chandra Sekhara Reddy, A. Ravitheja / Ain Shams Engineering Journal 10 (2019) 23–32 27

Fig. 5. Split tensile strength of CCA after early age cracks healing under different exposures.

Fig. 6. Split strength of CCA after structural cracks healing under different exposures.

Fig. 7. Percentage split tensile strength recovery of CCA after early age and structural cracks healing under different exposures.
28 T. Chandra Sekhara Reddy, A. Ravitheja / Ain Shams Engineering Journal 10 (2019) 23–32

Fig. 10. Stress-strain curves of CCA after healing of early age cracks under different
exposures.

Fig. 8. Load-displacement curves of CCA after healing of early age cracks under
different exposures.

Fig. 11. Stress-strain curves of CCA after healing of structural cracks under different
exposures.

Fig. 9. Load-displacement curves of CCA after healing of Structural cracks under was observed that the healing of cracks increased the stain capac-
different exposures.
ity of concrete in water immersed (WI) conditions.

4. Morphology of healing vicinity


3.4. Stress-strain behaviour
Based on FT-IR and SEM-EDX the characterization of self-
Compression test was conducted by measuring the cylindrical healing material’s microstructure is presented. As clearly pre-
specimen’s stress strain behavior. The cylindrical specimens of var- sented in Fig. 12, the initially observable feature of the crack heal-
ious compositions that were cured for duration of 28 days were ing phenomenon was the formation of white crack sealing in
subjected to compression till they failed. Figs. 10 and 11 show concrete specimens with CCA immersion in water for a period of
the stress strain curve of each specimen at various exposure condi- 42 days. It was observed that WI and WC subjected specimens
tions. The test proved that adding of CA to concrete has improved have superior healing properties compared to specimens that were
the strain capacity which is principally attributed to its ductile subjected to WD and AE. The closing of cracks was observed even
behavior. in WC and AE subjected specimens but to a lesser level compared
It is therefore, crystalline admixture in water immersed (WI) to WI and WC specimens. The importance of water for healing pro-
inclusion results in formation of hydrated products at large scale. cess is ascertained by the results of this experimental study. Pre
The hydrated products also enhance the load carrying and strain cracked specimens healed by cracks filling with calcium silicate
capacity. This proves the increased ductility of crystalline admix- hydrates and a calcite precipitate. The concrete specimens before
ture in water immersed (WI). In other exposures show low peak healing and after healing as shown are Fig. 12.
strain values to their corresponding WC, WD, AE due to the fact Fig. 14 shows the FT-IR spectra graph. Here infrared bands of
that increased local compressive stresses under loading point similar nature were observed irrespective of different specimen
results in overall low compressive strength compared to WI.it types. The presence of portlandite Ca(OH)2 was indicated by
T. Chandra Sekhara Reddy, A. Ravitheja / Ain Shams Engineering Journal 10 (2019) 23–32 29

Fig. 12. Self healing of early age and structural cracks under four different exposures.

shallow wide transmittances that followed around the characteris- Where Ca2+ are the calcium ions, (CO2 + H2O) represent the
tic stretching of H-O-H bond. The presence of carbonate phases external environment, entering in reaction and forming the cal-
(CO2
3 ) were confirmed in all samples, similar to the study in cium carbonate (CaCO3).
[50,51] by the sharp bands around 1424–1430 cm1 and
870 cm1. The 900 and 1418 cm1 stretching vibration confirmed Ca2þ + CO2 + H2 O $ CaCO3 + 2Hþ
the presence of sulfate (SO) and hence the existence of ettringite Calcium hydroxide (Ca(OH)2) in the area of the crack can dis-
in the specimen. Such results were similar to that of [52,53]. The solve in the water inside the crack and precipitate calcium ions
980 cm1 deep banding registered the presence of SiAO bonding at the crack surface.
further inferring the possibility of CASAH presence. The
830 cm1 bending is seen as a possibility of CA’s reaction and Ca(OH)2 $ Ca2þ + 2OH
adherence to the CASAH as noted by researchers [53,54]. This is
also supported by the observation of high noise effect presence On the crack surface of concrete some calcium carbonate will be
at low range web number’s signal. In spite of FT-IR based identifi- formed due to the reaction of CO2 present in the crack with Port-
cation of inherent self-healing constituents, the role played by CA landite (calcium hydroxide) present in the concrete matrix accord-
as a healing agent was distinctively identified. The complexity ing to the following reaction:
involved in the self-healing properties as a result of CA addition
CO2 + Ca(OH)2 $ CaCO3 + H2 O
to cement is obvious from FT-IR analysis. The SEM imaging of sur-
face and results of EDX quantification describes the varying self- To completely quantify the self-healing properties at elemen-
healing properties corresponding to the quantities of CA in the con- tary level composition, SEM-EDX elemental detection was per-
crete mix. Fig. 13 shows the typical microstructural surface mor- formed of the different spots of the specimen. The cracked
phology of self-healing materials. Only water immersion leads to vicinity’s morphology by SEM and newly formed crystals by crys-
Ca rich products on the surface of self-healing specimens like cal- talline admixture is shown in Fig. 14. The crack is completely
cite and C-S-H. Below mentioned reactions may be the cause for closed by the white crystals indicating formation of new chemical
self-healing mechanisms: compounds. Further observation on the vicinity of the crack under
30 T. Chandra Sekhara Reddy, A. Ravitheja / Ain Shams Engineering Journal 10 (2019) 23–32

Fig. 13. Morphology of the cracked vicinity by SEM with EDS.

a higher magnification exhibits dense and good crystallization of Crystalline admixture is a suitable material for self healing con-
the new products. Energy spectrum demonstrates that the new crete. Form the results strength is regained remarkably in the self
products are mostly composed of calcite. Mechanical properties healing concrete by using crystalline admixture.
restoration by healing are not as effective as the other curing con-
ditions when compared with WI. The new crystals are observed 5. Conclusions
with a much bigger size in WI compared to that by the other curing
conditions. The mechanism of healing by crystalline admixture is An experimental investigation on the self-healing properties of
the expansion by volume of the products, i.e., calcite and CASAH the concrete with CA under the different environments was carried
in hydration. The self-healing properties of concrete is accom- out and the following conclusions are drawn:
plished also by the role of secondary hydration of cement where
Ca2+ ions play an active role. The increase in the expansion prop-  Crystalline admixtures are able to catalyse the aforementioned
erty of cement during its rehydration stage is attributed to CA self-healing capacity recovery and is more systematic and reli-
added to the cement. The enhancement in the durability is because able due to their hydrophilic nature. They are also able to
of rehydration product’s densification that is accomplished by trig- absorb moisture from the atmosphere thus results in a not neg-
gering more self-healing materials formation. ligible healing also in air exposures. The early age and structural
The primary aim of this study is to use Fourier transform infra- cracks in concrete with CA are completely healed under the
red (FTIR) spectroscopy to examine the CaCo3 and CASAH of crys- water and dry-wet exposures and partially healed at water con-
talline admixture concrete in different environment conditions. tact and air exposures .
T. Chandra Sekhara Reddy, A. Ravitheja / Ain Shams Engineering Journal 10 (2019) 23–32 31

Fig. 14. FTIR Patterns of CCA.

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composites reinforced with flax and cottonised flax, and compared with year of 2013-2015.
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