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Self-Healing in Fiber-Reinforced
Self-Healing in Fiber-Reinforced
h i g h l i g h t s
a r t i c l e i n f o a b s t r a c t
Article history: Despite that considerable research has explored self-healing of portland cement-based materials, poten-
Received 23 March 2020 tial self-healing in alkali-activated binders remains largely unexplored. Therefore, this paper deploys a
Received in revised form 20 June 2020 wide array of experimental techniques to investigate the self-healing properties of PVA fibre-
Accepted 23 June 2020
reinforced alkali-activated slag-based composites incorporating crystalline additives (CA) and bentonite
Available online 4 July 2020
minerals (BN). X-ray microcomputed tomography (lCT) with three-dimensional image segmentation and
analysis, scanning electron microscopy with energy dispersive X-ray (SEM-EDS) analysis, inductively
Keywords:
coupled plasma optical emission spectroscopy (ICP-OES), optical microscopy, and water sorptivity mea-
Crack
Self-healing
surements were used to visualize, quantify, and identify the nature of healing compounds. While speci-
Alkali-activated mens incorporating CA exhibited significant self-healing, less self-healing was observed in specimens
Slag incorporating bentonite. X-ray lCT results indicated that the healing mechanism mainly occurred at sur-
Composite face cracks and calcium carbonate was the prevalent self-healing product formed. It was found that rising
Crystalline additive the pH and concentration of calcium ions of the curing medium and using polyvinyl alcohol (PVA) fibers
Bentonite in the mixture acted synergistically to accelerate crack self-healing in alkali-activated slag composites.
Calcium carbonate Ó 2020 Elsevier Ltd. All rights reserved.
Computed tomography
Microscopy
https://doi.org/10.1016/j.conbuildmat.2020.120059
0950-0618/Ó 2020 Elsevier Ltd. All rights reserved.
2 L.V. Zhang et al. / Construction and Building Materials 262 (2020) 120059
divided into autogenous healing and autonomic healing [10]. Auto- revealed that the risk of early-age cracking caused by drying
genous healing can be defined as an inherent ability to seal cracks shrinkage in AAMs was considerably higher than that in OPC con-
automatically without any intervention, for instance via carbona- crete [39–40]. This shortcoming could jeopardize wider implemen-
tion of Ca(OH)2 and formation of CaCO3, hydration of unreacted tation of AAM in various construction applications. Thus, exploring
cement and other cementitious materials, and swelling of hydrated the ability to endow AAM with crack self-healing ability has para-
cementitious products (C-S-H) [11]. For instance, Suleiman and mount importance.
Nehdi [12] investigated the self-healing of cracks in cement- While there is abundant research on self-healing of OPC-based
based composites under different environmental exposures and materials, there are few studies devoted to the self-healing behav-
found that the main self-healing product was calcium carbonate. ior of AAMs, despite their use in full-scale construction projects
By contrast, autonomic healing refers to the mechanism that is [28]. While the efficacy of CA and BN as self-healing additives in
triggered by artificial healing substances, which can be achieved OPC-based materials has been well documented, there are no stud-
for instance via microcapsules containing polymeric adhesive ies devoted to the self-healing of AAMs incorporating CA and BN.
agents such as epoxy, or microbially induced calcium carbonate Thus, the present study explores, for the first time, the effective-
precipitation (MICP) [13]. ness of CA and BN in fiber-reinforced alkali-activated slag compos-
Several techniques have been explored to improve the self- ites using various techniques including microscopy, inductively
healing capacity of cementitious materials [14]. For example, Jiang coupled plasma optical emission spectroscopy (ICP-OES), and X-
et al. [15] investigated the feasibility of enhancing the self-healing ray micro-computed tomography (l-CT) coupled with 3D image
in cementitious materials by incorporating various mineral addi- segmentation and analysis. Moreover, the recovery of transport
tives. They observed an improved healing efficiency using a combi- property was investigated using a water absorption test. The self-
nation of minerals. Nguyen et al. [16] used Bacillus subtilis as a healing products were characterized via scanning electron micro-
microbial adjuvant to improve crack self-healing and found that scopy (SEM) coupled with energy-dispersive X-ray spectroscopy
cracks of up to 400 lm in width were completely sealed. Du (EDS) analysis.
et al. [17] used microcapsules with toluene-di-isocyanate (TDI) as
a healing agent and paraffin as shell material. Compressive
2. Experimental procedures
strength could be restored and enhanced by 28.2%, while surface
cracks below 400 lm in width were filled within 6 h.
2.1. Materials
Crystalline additive (CA), a hydrophilic admixture containing
reactive silica and crystalline catalysts, has potential for reducing
Ground granulated blast furnace slag (GGBFS) was used as the
the permeability of concrete by reacting with some of its com-
AAM precursor. Sodium hydroxide pellets were used as alkali acti-
pounds [18]. Using CA for enhancing the self-healing efficiency of
vator. The CA and BN self-healing admixtures were obtained from
concrete has been widely investigated. The reaction products of
industrial suppliers. The chemical composition and physical prop-
CA deposit in cracks, thereby contributing to sealing [19]. For
erties of the slag, as determined by X-ray fluorescence, are given in
instance, Sisomphon et al. [20] explored the self-healing of surface
Table 1. The particle size distribution of the GGBFS was measured
cracks in mortars that incorporate CA. They found that more Ca2+
using a Malvern laser diffraction particle analyzer (Fig. 1). The
leached out from mortars incorporating CA, which enhanced pre-
GGBFS was activated using a 5 M sodium hydroxide solution. Poly-
cipitation of calcium carbonate as a self-healing product. Roig-
vinyl alcohol (PVA) fibers, with mechanical properties shown in
Flores et al. [21] found that specimens with 4% by-weigh-of-
Table 2, were used to control cracks and improve self-healing as
cement of CA and cured by water submersion exhibited best self-
recommended by Feng et al. [41] who observed that the presence
healing capability. Azarsa et al. [22] investigated the effect of CA
of PVA fibers contributed to calcium carbonate nucleation. A super-
on mechanical strength, self-healing, and durability properties of
plasticizer (SP) was used to achieve good workability. Two differ-
concrete. Their results showed that water permeability decreased
ent additives, namely CA and Na-bentonite in powder form, were
by three times, and the self-healing efficiency increased consider-
added to the mixture. The mixture proportions are shown in
ably by adding CA into the concrete mixture.
Table 3.
Bentonite (BN) has been also employed as a self-healing pro-
moter owing to its swelling properties in contact with water,
thereby sealing cracks [23]. Another mechanism reported by Eka- 2.2. Mixing procedure and specimen preparation
putri et al. [24] suggests that BN promoted precipitation of calcite
crystals by providing additional calcium ions. Previous studies All solid ingredients were first dry-mixed using a 10L-Hobart
showed that crack healing could be achieved either by embedding mixer for two minutes. A 5 M sodium hydroxide solution was
capsules containing BN or incorporating BN powders in mortars
[23,25]. Qureshi et al. [26] confirmed that the cement mixture with
Table 1
BN exhibited limited improvement in crack sealing compared to a
Physical and chemical properties of GGBFS and silica sand.
combination of expansive minerals.
Recently, Alkali-Activated Materials (AAM) have emerged as a Components/property GGBFS Silica sand
strong contender to replace Ordinary Portland cement (OPC) con- Silicon oxide (SiO2) (%) 33.70 99.70
crete in diverse applications. This binder system is derived from Aluminum oxide (Al2O3) (%) 12.80 0.14
Ferric oxide (Fe2O3) (%) 0.96 0.016
the reaction of a solid aluminosilicate precursor with a concen-
Calcium oxide (CaO) (%) 45.40 0.01
trated alkaline aqueous solution that encompasses alkali hydrox- Magnesium oxide (MgO) (%) 1.00 0.01
ide, carbonates, silicate, sulfate, etc. [27–29]. The solid precursor Sulfur trioxide (SO3) (%) – –
containing aluminosilicate can be a beneficiated industrial or a Tricalcium silicate (C3S) (%) – –
mining by-product, such as fly ash from coal combustion or metal- Dicalcium silicate (C2S) (%) – –
Tricalcium aluminate (C3A) (%) – –
lurgical slag from iron production [30]. Apart from the reduction of Tetracalcium aluminoferrite (C4AF) (%) – –
CO2 emissions from OPC production [1], AAM have shown Specific gravity 2.90 2.65
enhanced resistance to chemical attack [31–33] and high- Blaine fineness (m2/kg) 399 –
temperature [34–36], and to better immobilize toxic substances Loss on ignition (LOI) at 1000 °C 2.72 –
Time of setting (min) Vicat Initial – –
such as nuclear waste [37–38]. However, numerous studies have
L.V. Zhang et al. / Construction and Building Materials 262 (2020) 120059 3
Table 2
Mechanical properties of PVA fibres.
Mechanical properties Ultimate tensile strength (MPa) Diameter (mm) Density (kg/m3) Length (mm) Young’s modulus (GPa) Elongation (%)
PVA 1620 0.039 1300 12 43 6
4 L.V. Zhang et al. / Construction and Building Materials 262 (2020) 120059
Table 3
Mixture design of the mortars.
Fig. 2. Cracking specimens using a screw jack. Fig. 4. Vista-Pro ICP-OES system.
130 lm in CA-AAS specimens submerged in water could be com- self-healing efficiency. To quantitatively compare the self-healing
pletely sealed in 30 days. However, 0-AAS and BN-AAS specimens capability of the three specimen groups, the crack sealing ratio
exhibited less self-healing. The crack sealing ratio was used as an was estimated using nonlinear curve fitting. Fig. 10 (b) shows the
indicator to evaluate self-healing efficiency. Fig. 10 (a) plots a typ- crack sealing ratio of different specimen groups having initial crack
ical relationship between the crack sealing ratio and the initial width of 50 lm, 100 lm, and 150 lm, respectively. CA-AAS spec-
crack width. It can be observed that CA-AAS specimens achieved imens had the highest potential of crack width reduction, while BN
the highest efficiency of crack width reduction among the three reduced the self-healing efficiency compared to the control speci-
types of specimens. In addition, smaller cracks showed higher men 0-AAS. This result is consistent with Suleiman et al. [4] who
6 L.V. Zhang et al. / Construction and Building Materials 262 (2020) 120059
Fig. 10. Relationship between initial crack width and crack sealing ratio for the three mixtures: (a) non-linear fitting of the typical relationship between crack sealing ratio
and initial crack width; (b) effect of original crack width on crack sealing ratio determined from Fig. 10 (a).
Table 4
Calcium concentrations in water after 16 days submersion.
crack mouth in the 0-AAS and BN-AAS specimens, as shown in
Mix Ca2+ concentration (mg/L) Fig. 13 (b) and (c).
CA-AAS 4.22 To further confirm the chemical composition of self-healing
0-AAS 1.27 products, elemental EDS analysis was conducted. The healing prod-
BN-AAS 1.22 ucts at the surface cracks of all specimens were mainly dominated
by Ca, O, and C according to the spectrum maps, confirming that
the self-healing materials were primarily composed of CaCO3.
Noticeably, a small amount of silicon and aluminum was also
found, which suggests the presence of calcium-alumino-silicate-
hydrate (C-A-S-H) as a hydration product of alkali-activated slag.
This finding is in agreement with Nguyn’s study [62], which con-
cluded that the dominant healing material of sodium activator-
based alkali-activated slag composites was CaCO3. The observed
magnesium content could arise from the raw GGBFS or is possibly
from magnesite (MgCO3), or brucite (Mg(OH)2) [62].
Fig. 14 shows the morphology of self-healing materials covering
PVA fibers. In the CA-AAS and the BN-AAS specimens, irregular
polyhedron-like crystals were packed more densely than in the
0-AAS specimens. Interestingly, small needle-like crystal clusters
were scattered on the surface of PVA fibers in the CA-AAS and
the 0-AAS specimens, as shown in Fig. 14 (a) and (b). The self-
healing products on the boundary of the crack were attracted by
the PVA fiber and grew towards it (Fig. 14 (b)), suggesting a trend
to bridge the gap. It can be hypothesized that PVA fibers induced
precipitation of self-healing products by acting as nucleation sites.
According to this hypothesis, the PVA fiber-induced bridging of
cracks could promote self-healing efficiency of alkali-activated
slag-based composites, indicating that self-healing was deter-
mined by coupled factors through synergistic action [50].
Fig. 12. Change in water absorption of cracked specimens exposed to water (a) before cracking, (b) upon cracking, (c) after curing, and (d) sorptivity coefficient reduction
ratio of the specimen groups.
Fig. 13. SEM images with EDS pattern of self-healing products within the cracks of (a) CA-AAS, (b) 0-AAS, and (c) BN-AAS.
L.V. Zhang et al. / Construction and Building Materials 262 (2020) 120059 9
3.6. Synergistic effect of calcium ions, pH, and PVA fiber on self-healing
Fig. 15. X-ray lCT scanning images of the CA-AAS specimen with modified binary images demonstrating interior cracks: (a) upon cracking and (b) after healing.
Fig. 16. Electrical conductivity vs. pH of curing water for the submerged specimens. Fig. 18. Schematic illustration of the self-healing mechanism of PVA fiber-
reinforced alkali-activated slag-based composites incorporating CA.
4. Conclusions
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