Characterization of Damage and Healing of Cement

Matrices Based on Fly Ash under Repeated Loading

Zhen-Yu Chen 1; Wenting Li 2; and Qian-Qian Yu, A.M.ASCE 3

Abstract: This paper investigates damage and healing of cementitious materials based on fly ash (FA) with a special focus on the effect of
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repeated loading on the self-healing performance. In total, 90 prism specimens and 33 cylinder specimens were prepared and tested. Variables
including the FA replacement ratio and preloading level were considered. Different methods were adopted to evaluate the self-healing per-
formance, i.e., mechanical tests, acoustic emission (AE) analysis, water absorption measurement, and scanning electron microscope (SEM)
observation. Test results revealed that an appropriate amount of cement replaced by FA was beneficial to the self-healing performance of the
specimens subjected to a high level of repeated preloading, where the strength increased by 11% and the water absorption rate decreased by
12%, in comparison with that of the undamaged specimens. This was attributed to the active hydration of FA, which was confirmed by an
energy dispersive X-ray spectroscopy (EDS) analysis. This study extends understanding of the self-healing performance when subjected to
repeated loading and provides some useful suggestions for the self-healing technique based on mineral additives. DOI: 10.1061/(ASCE)
MT.1943-5533.0003516. © 2020 American Society of Civil Engineers.
Author keywords: Self-healing; Fly ash; Repeated loading; Acoustic emission analysis.

Introduction concrete particles. The chemical effect is composed of continuous

Concrete structures are susceptible to cracking due to service loads
and environmental attacks. Through open paths created by cracks,
aggressive agents ingress into concrete and consequently reduce
durability of the structures (Mohammed et al. 2001). In recent years,
self-healing cement matrices based on different approaches have
attracted much attention. These methods include autogenous self-
healing (Granger et al. 2007; Şahmaran et al. 2008; Yang et al. 2009;
Snoeck et al. 2014; Zhang et al. 2014; Yildirim et al. 2015a; Keskin
et al. 2016), chemical encapsulation (Blaiszik et al. 2009; Liu et al.
2009; Thao et al. 2009; Van Tittelboom et al. 2011; Souradeep and
Kua 2016; Dong et al. 2017; Li et al. 2020), and bacteria application
(Van Der Zwaag 2007; Wang et al. 2012, 2014). Among them,
the autogenic self-healing mechanism is generally distinguished
into three parts, i.e., physical, mechanical, and chemical effects
(Edvardsen 1999; De Rooij et al. 2011; Yildirim et al. 2015b).
Invasion of water promotes swelling of hydrated cement paste
(HCP), leading to reduced space between the constituents of HCP,
which is called the physical effect. The mechanical effect indicates
plugging of cracks by impurities from water and fracture of small
1 increase of the FA content, cracks became denser and tighter.
Graduate Student, Key Laboratory of Performance Evolution and
Control for Engineering Structures, Ministry of Education, Tongji Univ.,
Shanghai 200092, China; Dept. of Structural Engineering, Tongji Univ.,
Shanghai 200092, China. Email: czy1996824@tongji.edu.cn
2
Associate Researcher, Key Laboratory of Advanced Civil Engineering
Materials, Ministry of Education, Tongji Univ., Shanghai 201804, China.
Email: lwt@tongji.edu.cn
3
Associate Professor, Key Laboratory of Performance Evolution and
Control for Engineering Structures, Ministry of Education, Tongji Univ.,
Shanghai 200092, China; Dept. of Structural Engineering, Tongji Univ.,
Shanghai 200092, China (corresponding author). ORCID: https://orcid
.org/0000-0003-1772-3195. Email: qianqian.yu@tongji.edu.cn
Note. This manuscript was submitted on February 10, 2020; approved
on June 24, 2020; published online on October 21, 2020. Discussion period
open until March 21, 2021; separate discussions must be submitted for in-
dividual papers. This paper is part of the Journal of Materials in Civil
Engineering, © ASCE, ISSN 0899-1561.
hydration of unhydrated cement and formation of calcium car-
bonate. In terms of these three items, the physical and mechanical
effects reduce fluid flow and consequently are beneficial to the
resistance against water penetration, whereas the chemical effect
generates chemical products to fill cracks and therefore provides
mechanical strength.
Normally, to activate the chemical effect, mineral additives
are adopted such as fly ash (FA), silica fume, and furnace slag
(Şahmaran et al. 2008; Qian et al. 2009; Van Tittelboom et al. 2012;
Zhang et al. 2014). Qian et al. (2009) investigated the performance
of strain-hardening cementitious composites (SHCC) containing
blast-furnace slag (BFS) and limestone powder (LP). It was found
that addition of BFS and LP not only increased the ductility of
SHCC but also promoted noticeable self-healing performance be-
cause of the pozzolanic reaction of supplementary materials. Ahn
and Kishi (2010) selected expansive agents consisting of calcium
sulfoaluminate, free lime, anhydrite, and geomaterials. Concrete
with such additives successfully healed cracks with an initial width
of 0.2 mm after 28 days. Zhang et al. (2014) conducted an exper-
imental study on the self-healing behavior of engineered cementi-
tious composites (ECC) with different volumes of FA. With the
Roig-Flores et al. (2015) made use of crystalline additives con-
taining reactive silica and some crystalline catalysts, which led to a
remarkable improvement in the water resistance of tested concrete.
Siad et al. (2017) investigated the possible use of glass powder (GP)
in ECC. The flexural strength and deformation were assessed on
beams precracked at 28 days and healed in water up to 28 þ
90 days. Although the self-healing efficiency was slightly more
evident in samples without GP, a higher level of deformation recov-
ery was witnessed in ECC incorporating a GP replacement ratio of
25%. Yildirim et al. (2018) compared the autogenous self-healing
capability of one-year-old ECC with different mineral admixtures.
It was shown that self-healing performance of ECC with Class F
fly ash (ECC-FA) was pronounced, in which case the cracks with
different widths were fully repaired after 90 days of CO2 -water
curing.

© ASCE 04020408-1 J. Mater. Civ. Eng.

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Fig. 1. Specimen geometry and mechanical test setup: (a) four-point bending test for prism specimens; and (b) uniaxial compression test for cylinder
specimens (units in millimeters, not to scale).

Based on the aforementioned research, self-healing techniques the performance between the first and second self-healing. The self-
show a great promise in repair of cracks for concrete structures. To healing performance was carefully evaluated through mechanical
the best of the authors’ knowledge, most previous studies investi- tests, acoustic emission (AE) analysis, water absorption measure-
gated the self-healing behavior of damaged cementitious materials. ment, and scanning electron microscope (SEM) observation. Var-
Specimens were firstly loaded (monotonic or cyclic) and then a rest iables including the FA replacement ratio and preloading level were
period was interposed before another loading, which was used to considered. Test results showed that the self-healing capability can
evaluate the self-healing behavior. However, performance of the be maintained after repeated loading, especially for the samples
self-healed structures under repeated loading has not been fully with a moderate FA replacement ratio subjected to a high level of
understood, although concrete structures are inevitably subjected predamage.
to cyclic loads and multiple environmental attacks during their ser-
vice life.
Yildirim et al. (2015c) and Şahmaran et al. (2015) performed a Experimental Program
series of experimental studies on ECC with FA or slag additives.
The specimens were repeatedly preloaded to 70% of their splitting Prism and cylinder specimens were designed in this experiment to
tensile deformation capacities and subjected to cyclic wet/dry con- investigate the self-healing behavior in terms of strength restoration
ditions between each preloading interval. Resonant frequency test and water absorption, respectively. A total of 123 specimens were
results showed a remarkable self-healing effect for the specimens prepared and tested, among which 90 were prisms and the other 33
cured for 28 days during the first three cycles; however, perfor- were cylinders.
mance of the specimens became weaker in the following six cycles.
Sneock and De Belie (2016) applied two cycles of preloading to Specimens and Materials
strain-hardening cementitious composites with superabsorbent
polymers. The strain in the preloading process was limited to 1%. Fig. 1 gives the geometry and dimensions of the specimens. The
The self-healing effect was verified, but its effectiveness decreased prism specimen had a cross section of 40 × 40 mm and a length
after the second preloading. of 160 mm. The cylinder specimen had a diameter of 100 mm
This paper presents an investigation of the damage and healing and a height of 200 mm.
of cementitious material based on FA with a focus on the effect Mortar specimens were prepared using ordinary portland ce-
of repeated loading. Specimens were preloaded and cured twice ment (PC) type 52.5R [GB 175 (General Administration of Quality
in a lime-saturated solution. Special attention was paid to compare Supervision, Inspection, and Quarantine of the People’s Republic
of China 2007)]. The chemical composition and physical properties
of the FA according to the datasheet provided by the manufacturer
are presented in Table 1. Three mix proportions were adopted for
Table 1. Chemical composition and physical properties of the FA the preparation of mortar, as listed in Table 2. FA0 denotes samples
Composition/property Value without FA as control specimens. FA35 and FA55 represent spec-
CaO (%) 12.06
imens with the FA replacement ratios of 35% and 55% by mass
SiO2 (%) 55.80
Al2 O3 (%) 14.33
Fe2 O3 (%) 4.14 Table 2. Mixture proportion of the mortar by mass ratio
TiO2 (%) 0.72 FA
(%) Standard
SO3 (%) 0.0083
Mortar FA þ PC Cement Fly ash Water sand
K2 O (%) 2.12
Na2 O (%) 2.72 FA0 0 100 0 45 200
Loss on ignition 0.74 FA35 35 65 35 45 200
Specific gravity (g=cm3 ) 2.70 FA55 55 45 55 45 200

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 of binder (PC þ FA), respectively. For all the mixtures, the water/
binder ratio and sand/binder ratio were fixed at 0.45 and 2, respec-
tively. After casting, the specimens were cured under standard
conditions [20°C  2°C and relative humidity (RH) of 95%] for
28 days before preloading.
Test Setup
Nine prism and nine cylinder specimens were monotonically loaded
to determine the load-bearing capacity [GB/T 50081 (Ministry of
Housing and Urban-Rural Development of the People’s Republic
of China 2002)], which was used to provide a reference for the fol-
lowing preloading procedure. The prism specimens were tested un-
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were mounted at each end of the specimens with a thin layer of
vacuum silicone grease. The transducers had a brand character-
istic ranging from 60 to 400 kHz with a maximum sensitivity of
150 kHz. The threshold value for this mode was set at 40 dB to
exclude the influence of noise (Pour-Ghaz and Weiss 2010; Li et al.
2017). The position and direction of the specimens as well as the
AE instruments during preloading and reloading were carefully
kept consistent to minimize the test error. The acoustic hits as well
as corresponding amplitude and cumulative energy were collected
during the loading process. In addition to the specimens listed in
Table 5, extra nine prisms without a healing procedure, identified as
FA0-B-30-H0, FA0-B-60-H0, and FA0-B-80-H0 (three specimens
for each scenario), were tested to get the accumulative energy as a

der a four-point bending test rig with a loading rate of 0.1 mm=min. benchmark.
The beam span between two supports was 120 mm, and the load Water absorption measurement was adopted according to
applied by the actuator was evenly distributed between two loading ASTM C1585 (ASTM 2013) to assess the crack characterization
points through a spreader beam with a span of 40 mm [Fig. 1(a)]. (Şahmaran and Li 2009; Zhang et al. 2014). There are two spec-
The cylinder specimens were loaded under axial compression with a imens for each scenario as listed in Table 6. The two specimens
loading rate of 1 mm=min, as displayed in Fig. 1(b). There are three (dimeter of 100 mm and height of 50 mm) were made from one
samples for each scenario, as listed in Tables 3 and 4, and the aver- cylinder (dimeter of 100 mm and height of 200 mm) after preload-
age value of the results was taken as the ultimate strength of the ing and immersion, as shown in Fig. 2 (Castro et al. 2011). The
specimens. specimens were placed in an environmental chamber with a temper-
Preloading was applied to both prism and cylinder specimens to ature of 50°C  2°C and RH of 80%  3% for 3 days. Afterward,
simulate initial damage. Different preloading levels, defined as the they were left in a sealed plastic bag for 15 days for the redistrib-
ratio of the applied load to the load-bearing capacity of the speci- ution of the internal water. During the water absorption test, it is
men, were selected in this study, i.e., 30%, 60%, and 80%. After important to guarantee the directional water flow through the speci-
preloading, the specimens were stored in lime-saturated water at men. Therefore, the lateral surface of the sample was sealed by ep-
23°C  2°C for 30 days. Afterward, one batch of the specimens oxy and only the bottom surface of the specimen was exposed to
were loaded until failure while the other batch was again preloaded water with a level 1–3 mm higher than the support (Fig. 3). Before
to the same preloading level and subsequently immersed for an- each test, the initial mass of the sample was first measured. After
other 30 days. Finally, they were tested to failure to examine the that, the mass gain in contact with water was recorded at given time
effect of repeated loading on the self-healing behavior in terms of intervals of 1, 5, 10, 20, 30, and 60 min, and then at hourly intervals
strength restoration. There were three specimens for each scenario, for the next six hours.
and the average results are listed in Table 5.
An AE system was installed on the prism specimens [Fig. 1(a)]
to capture the damage and healing evolution of the mortar when
Table 5. Experimental program and results of the prism specimens
subjected to bending. Two highly sensitive broadband transducers
FA Ultimate
replacement Preloading Healing load
Table 3. Ultimate load-bearing capacity of prism specimens under bending Specimen ratio (%) Preloading level (%) times (kN)
Specimen No. Mixture Ultimate load (kN) Average (kN) FA0-B-0-H1 0 Bending 0 1 2.89
FA0-B-0-H2 0 Bending 0 2 2.68
1 FA0 3.16 3.03
FA0-B-30-H1 0 Bending 30 1 3.25
2 2.87
FA0-B-30-H2 0 Bending 30 2 2.46
3 3.06
FA0-B-60-H1 0 Bending 60 1 3.10
4 FA35 1.99 2.38
FA0-B-60-H2 0 Bending 60 2 2.33
5 2.82
FA0-B-80-H1 0 Bending 80 1 2.44
6 2.33 a
FA0-B-80-H2 0 Bending 80 2
7 FA55 1.98 1.99
FA35-B-0-H1 35 Bending 0 1 2.11
8 2.02
FA35-B-0-H2 35 Bending 0 2 2.19
9 1.97
FA35-B-30-H1 35 Bending 30 1 2.57
FA35-B-30-H2 35 Bending 30 2 2.00
FA35-B-60-H1 35 Bending 60 1 2.47
Table 4. Ultimate load-bearing capacity of cylinder specimens under FA35-B-60-H2 35 Bending 60 2 1.86
compression FA35-B-80-H1 35 Bending 80 1 2.35
FA35-B-80-H2 35 Bending 80 2 2.43
Specimen No. Mixture Ultimate load (kN) Average (kN)
FA55-B-0-H1 55 Bending 0 1 1.91
1 FA0 316.9 321.3 FA55-B-0-H2 55 Bending 0 2 2.63
2 318.6 FA55-B-30-H1 55 Bending 30 1 1.83
3 328.3 FA55-B-30-H2 55 Bending 30 2 1.97
4 FA35 290.4 288.6 FA55-B-60-H1 55 Bending 60 1 2.38
5 295.8 FA55-B-60-H2 55 Bending 60 2 1.97
6 279.6 FA55-B-80-H1 55 Bending 80 1 2.05
7 FA55 177.2 186.4 FA55-B-80-H2 55 Bending 80 2 2.25
8 187.0 a
Specimens prematurely failed during the second preloading of 80%, and
9 226.7
the corresponding data is missed.

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 Table 6. Experimental program and results of the cylinder specimens The rate of absorption is expressed by
Water mt
FA absorption I¼ ð1Þ
Aρ
replacement Preloading Healing rate
Specimen ratio (%) Preloading level (%) times (10−3 ) where I = water absorption; mt = change in the specimen’s mass at
FA0-C-0-H1 0 Compression 0 1 4.08 the time t; A = exposed area of the specimen; and ρ = water density.
FA0-C-0-H2 0 Compression 0 2 2.31 To have an insight into the healing products, the secondary elec-
FA0-C-30-H1 0 Compression 30 1 2.70 tron images of the specimens after failure were observed by using
FA0-C-30-H2 0 Compression 30 2 1.95 SEM. Samples were cut into small cubes and coated with gold.
FA0-C-60-H1 0 Compression 60 1 2.87 Energy dispersive X-ray spectroscopy (EDS) analysis was also per-
FA0-C-60-H2 0 Compression 60 2 2.08
formed at certain locations of the samples to examine the potential
FA0-C-80-H1 0 Compression 80 1 3.70
FA0-C-80-H2 0 Compression 80 2 2.74
self-healing products.
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FA35-C-0-H1 35 Compression 0 1 1.36

FA35-C-0-H2 35 Compression 0 2 1.51
FA35-C-30-H1 35 Compression 30 1 2.01 Results and Discussions
FA35-C-30-H2 35 Compression 30 2 1.65
FA35-C-60-H1 35 Compression 60 1 1.63 Tables 3 and 4 list the ultimate load of prism and cylinder speci-
FA35-C-60-H2 35 Compression 60 2 1.18 mens after 28 days’ curing, respectively, which decreased with
FA35-C-80-H1 35 Compression 80 1 1.22 the increase of the FA replacement ratio. The decline in the flexu-
FA35-C-80-H2 35 Compression 80 2 1.32 ral strength was 23% and 35% when the FA replacement ratio
FA55-C-0-H1 55 Compression 0 1 3.92 was 35% and 55%, respectively. The compressive strength re-
FA55-C-0-H2 55 Compression 0 2 3.08
duced by 10% and 42% simultaneously. Calcium silicate hydrate
FA55-C-30-H1 55 Compression 30 1 4.73
FA55-C-30-H2 55 Compression 30 2 3.62 (CaH2 SiO4 · H2 O), abbreviated as C-S-H, is recognized as one of
FA55-C-60-H1 55 Compression 60 1 3.79 the main sources of mechanical strength of cementitious materials
FA55-C-60-H2 55 Compression 60 2 4.07 (Fan and Li 2014; Siad et al. 2018; Öztürk et al. 2020), and it is
FA55-C-80-H1 55 Compression 80 1 4.52 generated by hydration of cement and FA (Maltais and Marchand
FA55-C-80-H2 55 Compression 80 2 4.55 1997; Termkhajornkit et al. 2006, 2009; Martin et al. 2017). During
the first 28 days, the hydration degree of cement is much higher
than that of FA. Therefore, the specimens with more cement ob-
tained a relatively higher ultimate load at 28 days. Similar results
were reported by Swamy et al. (1983), Malhotra et al. (2000), and
Termkhajornkit et al. (2009).
Tables 5 and 6 present summaries of the test program and results
of the prism and cylinder specimens, respectively. In terms of the
specimen nomenclature, FA0, FA35, and FA55 represent the FA
replacement ratios of 0%, 35%, and 55%, respectively. The letter
200

after the first hyphen stands for the load type, i.e., B for bending
and C for compression. The number after the second hyphen means
the preloading level. The last symbol indicates times of the healing
process.
50

100 100 Strength Restoration

Fig. 4(a) plots the normalized strength of the unhealed specimens,
Fig. 2. Preparation of specimens for water absorption tests (units in
which were immediately loaded to failure after preloading without
millimeters, not to scale).
any immersion process involved. In comparison with the specimens
without preloading, the residual strength decreased by 15%, 19%,
and 22% when preloaded by 30%, 60%, and 80%, respectively.
The failure load of all the specimens after the first and second
healing process was normalized by that of the specimen without
FA after 28 days’ curing in standard conditions and is shown in
Figs. 4(b and c), respectively. The normalization here was intended
to exclude the influence of strength variation with time. Most spec-
imens showed apparent strength growth in comparison with the
undamaged ones, denoted as blank columns. Although the strength
of Specimens FA0-B-80-H1 and FA55-B-30-H1 witnessed a de-
cline of 15% and 4%, respectively, the drop percentage was lower
than the effect induced by preloading as identified in Fig. 4(a). It
was, therefore, demonstrated that considerable strength recovery
was gained after the first immersion procedure. In Fig. 4(b), the
specimens with the FA replacement ratio of 35% showed the best
performance, where the flexural strength subjected to preloading
levels of 30%, 60%, and 80% increased by 22%, 17%, and 11%,
Fig. 3. Water absorption test setup.
respectively. The noticeable healing performance in the first healing

© ASCE 04020408-4 J. Mater. Civ. Eng.

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 period was related to the early precracking age adopted in the cur-
rent experimental program. All the specimens here were preloaded
after 28 days’ curing when there was plenty of unhydrated cement in
the mortar specimens.
Continuous hydration of the unhydrated cement contributed to
the apparent self-healing behavior, which was also boosted by the
addition of FA (Termkhajornkit et al. 2009; Van Tittelboom and
De Belie 2013). The experimental findings are in conformance
with those reported by Ter Heide and Schlangen (2007) and Qian
et al. (2010). Although all the specimens were preloaded after
28 days’ curing, those with the FA replacement ratio of 55%
did not show a prominent self-healing performance. In compari-
son with the respective specimens without preloading, strength of
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Specimen FA35-B-30-H1 grew by 22%, whereas that of Specimen
FA55-B-30-H1 decreased by 4%. This phenomenon suggested that
an appropriate replacement ratio of FA was beneficial to hydration
Fig. 4. Strength restoration: (a) unhealed specimens; (b) specimens
after the first healing; and (c) specimens after the second healing.
© ASCE 04020408-5
J. Mater. Civ. Eng., 2021, 33(1): 04020408
of unhydrated cement. However, when excessive cement was re-
placed by FA, the amount of unhydrated cement was reduced, lead-
ing to a declined quantity of hydration products.
The mechanical performance of the specimens after the second
healing process is presented in Fig. 4(c). The specimens without FA
prematurely failed during the second preloading of 80%f max , and
the corresponding data is missed. However, the specimens with FA
replacement ratios of 35% and 55% survived under two preloadings
of 80%f max , which demonstrates that the replacement of cement by
FA was beneficial for the long-term behavior of concrete structures
subjected to high levels of repeated loading.
Most specimens in Fig. 4(c), contrary to those in Fig. 4(b), show
a strength reduction in comparison with those without preloading.
However, the drop degrees were all lower than that in Fig. 4(a) ex-
cept for Specimens FA55-B-30-H2 and FA55-B-60-H2, which
Fig. 5. Amplitude of acoustic hits of the unhealed specimens during
the first preloading and reloading phases: (a) Specimen FA0-B-30-H0;
(b) Specimen FA0-B-60-H0; and (c) Specimen FA0-B-80-H0.
J. Mater. Civ. Eng.
 implies an apparent self-healing performance after repeated load-
ing. Generally, the efficiency of the second healing declined in
comparison with that of the first healing, although this trend
was not followed by Specimen FA35-B-80-H2.
The bending strength gained an increase of 11%, which was the
same as that after the first healing. This phenomenon could be ex-
plained by the pozzolanic reaction of FA, which plays a key role in
the late stage of strength development of mortar (Termkhajornkit
et al. 2009; Şahmaran et al. 2013; Zhang et al. 2014). FA reacts
with calcium hydroxide from the cement hydration to produce
C-S-H gels to fill the cracks. The reaction mainly depends on two
key factors, i.e., available space, and amount of anhydrate FA and
calcium hydroxide (Termkhajornkit et al. 2009; Şahmaran et al.
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AE Analysis
Strength variation is a comparatively rough evaluation to judge
the performance of self-healing because mechanical behavior is
normally insensitive to healing on a micro or even mesoscale level
until the event accumulates to a certain level (Li et al. 2017). There-
fore, an AE test with acoustic hits and energy recorded was further
adopted to characterize the self-healing process. For the unhealed
specimens and the specimens with one healing process, there were
two phases involved in the AE analysis, i.e., the first preloading and
reloading. In terms of the specimens experiencing two healing
processes, there were three stages, i.e., the first preloading, second
preloading, and reloading stages.

2013). During the second healing period, the anhydrous FA became
active and, more importantly, sufficient space for reaction was gen-
erated by a high preloading level of 80%. Therefore, remarkable
self-healing performance was observed in Specimen FA35-B-
80-H2. Nevertheless, for Specimen FA55-B-80-H2, which did not
show a pronounced self-healing effect, the possible reason was
that, in the mixture of FA55, excessive cement was replaced by FA,
leading to a limited amount of calcium hydroxide during the first
healing period. Consequently, although the space for reaction and
sufficient FA were supplied, no active pozzolanic reaction occurred.
The amplitude of acoustic hits versus load of the unhealed spec-
imens without FA is displayed in Fig. 5. The stars represent the
acoustic hits recorded in the first preloading stage, and the dots
stand for those obtained from the reloading phase. The preloading
level is marked by a dashed line. The larger preloading brought
about more serious damage to the specimens, so more stars were
observed before the dashed line. It is interesting to see that fewer
acoustic hits were recorded in the reloading phase in comparison
with that in the preloading stage before the predamage load-
ing. However, the number of acoustic hits in the reloading phase

Fig. 6. Amplitude of acoustic hits versus load of the specimens after the first healing: (a) Specimen FA0-B-30-H1; (b) Specimen FA0-B-60-H1;
(c) Specimen FA0-B-80-H1; (d) Specimen FA35-B-30-H1; (e) Specimen FA35-B-60-H1; (f) Specimen FA35-B-80-H1; (g) Specimen FA55-B-30-H1;
(h) Specimen FA55-B-60-H1; and (i) Specimen FA55-B-80-H1.

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 considerably increased after the dashed line. This phenomenon is
known as the Kaiser effect (Kaiser 1950). The applied load resulted
in cracking of the microstructure, which produced acoustic signals.
Because these specimens experienced no healing process, the bro-
ken matrix remained the same during the reloading phase. Addi-
tional cracking as well as extra acoustic hits were not expected
until the previous damage was exceeded.
Fig. 6 presents results of acoustic hits against load of the spec-
imens after the first healing. For the specimens without FA, slight
self-healing was observed for Specimens FA0-B-30-H1 and
FA0-B-60-H1. The number of circle acoustic hits increased before
the dashed line, which was attributed to the continuous hydration of
cement during the immersion procedure. For Specimen FA0-B-80-
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However, an adverse influence was induced by excessive cement
replaced by FA. Specimens FA55-B-30-H1 and FA55-B-60-H1 fol-
lowed the Kaiser law like the unhealed specimens did, and no ap-
parent self-healing effect was observed. It should be pointed that
the experimental findings of Specimen FA55-B-60-H1 here was
not in compliance with that displayed in the “Strength Restoration”
section, where the strength increased by 25% in comparison with
the undamaged ones. It was found that the number of stars for Speci-
men FA55-B-60-H1 was much more than expected because the pre-
loading level was between that of Specimens FA55-B-30-H1 and
FA55-B-80-H1. It may be the possible reason for the unreasonable
comparison of the acoustic hits between the first preloading and re-
loading stage. However, the reason for the unexpected number of

H1, the performance was similar to that of the specimens without
the immersion procedure. In contrast, regardless of the preloading
levels, the specimens with an FA replacement ratio of 35% pre-
sented a considerably increased number of circle acoustic hits be-
fore the dashed line, which were originally from the damage of
healing products formed by unhydrated cement (Jiang et al. 2019).
The addition of FA slowed the hydration speed during the casting
procedure, contributing to more hydration in the service period
(Termkhajornkit et al. 2009). Therefore, the specimens with the
mixture of FA35 proved a pronounced self-healing behavior.
stars needs future research.
The acoustic hits versus load after the second preloading and
healing are illustrated in Fig. 7. Specimen FA0-B-80-H2 prema-
turely failed during the second preloading and consequently, the cor-
responding figure was missed. When the specimens were repeatedly
loaded by 30%f max and 60%fmax , the Kaiser effect was clearly
observed in the specimens with the mixtures of FA0 and FA35, in-
dicating the detrimental effect induced by the repeated loading.
However, Specimen FA35-B-80-H2 behaved differently where
more intensive hits were obtained in the reloading phase before

Fig. 7. Amplitude of acoustic hits versus load of the specimens after the second healing: (a) Specimen FA0-B-30-H2; (b) Specimen FA0-B-60-H2;
(c) Specimen FA35-B-30-H2; (d) Specimen FA35-B-60-H2; (e) Specimen FA35-B-80-H2; (f) Specimen FA55-B-30-H2; (g) Specimen FA55-B-60-H2;
and (h) Specimen FA55-B-80-H2.

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J. Mater. Civ. Eng., 2021, 33(1): 04020408

 the dashed line. This remarkable performance was consistent with
the pronounced recovery of 11% in the mechanical property. This
interesting behavior was related to the pozzolanic reaction of FA,
which was more easily activated by a high preloading. The perfor-
mance of Specimen FA55-B-30-H2 was similar to that of Specimen
FA55-B-30-H1, again indicating the negative effect due to an ex-
cessive amount of FA.
In terms of the remaining specimens in Figs. 6 and 7, such as
FA55-B-80-H1 and FA55-B-60-H2, it is difficult to compare the
number of acoustic hits between the reloading stage and first pre-
loading stage with the naked eye, which implies a limitation when
evaluating the self-healing effect by using the acoustic hits.
Accumulative energy was analyzed to give a further index on
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the healing mechanism. Fig. 8 presents the accumulative energy

of the unhealed specimens during the preloading and reloading

Fig. 8. Accumulative energy versus load of the unhealed specimens Fig. 9. Energy ratios of the specimens under various preloading
during two loading phases: (a) Specimen FA0-B-30-H0; (b) Specimen levels: (a) preloading level of 30%; (b) preloading level of 60%;
FA0-B-60-H0; and (c) Specimen FA0-B-80-H0. and (c) preloading level of 80%.

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J. Mater. Civ. Eng., 2021, 33(1): 04020408

 phases. The dashed line represents the predamage level. For sce-
narios with various preloading levels, a common phenomenon was
found whereby before the dashed line, the accumulative energy
during the reloading stage was much lower than that in the preload-
ing period. That was attributed to the fact that little new damage and
cracking occurred in the latter stage, which was consistent with the
observation of acoustic hits.
To quantitatively manifest this characterization, the ratio of the
energy during reloading to that in preloading at the dashed line was
extracted and is diagrammed in Fig. 9. The average energy ratios
of the unhealed specimens were considered as the benchmark,
i.e., 0.09, 0.22, and 0.18 under the preloading levels of 30%, 60%,
and 80%, respectively. For the scenarios where the value was higher
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Fig. 10 shows the water absorption property of Specimen FA0-
C-0-H0. According to ASTM C1585 (ASTM 2013), the initial rate
of water absorption is defined as the slope of the line best fit to
water absorption I plotted against the square root of time t (s1=2 ).
The initial water absorption rate of the specimen was 0.00335.
The water absorption rates of all the specimens are normalized
by that of the specimen without FA after 28 days’ curing, as illus-
trated in Fig. 11. For the unhealed specimens shown in Fig. 11(a),
the water absorption rate decreased by 7% and 6% and increased by
9%, corresponding to the preloading levels of 30%, 60%, and 80%,
respectively, in comparison with the undamaged ones. Different
levels of preloading induced various numbers of cracks into mor-
tars. Under a low stress level, cracks had relatively small size and

than the reference, it was assumed that more energy was emitted were restricted to the aggregate–paste interface, which slightly
before the dashed line during the reloading phase, indicating that influenced the water absorption rate (Samaha and Hover 1992). In
additional damage from healing products occurred. addition, the compression load compacted the microstructure of
The average energy ratios of all the specimens after the first
healing were higher than the benchmark, except for Specimens
FA55-B-30-H1 and FA0-B-80-H1 with the ratios of 0.08 and
0.16, respectively. The best performance was found in the speci-
mens with the mixture of FA35, where the energy ratios were about
21, 5, and 9 times larger than that of the unhealed specimens when
subjected to preloading of 30%, 60%, and 80%, respectively.
In terms of the solid columns denoting the specimens after the
second preloading and healing, self-healing behavior was witnessed
in Specimens FA35-B-30-H2, FA35-B-80-H2, and FA55-B-80-H2,
with an increased energy ratio compared with the dashed line. The
energy ratio of Specimen FA35-B-80-H2 increased from 1.76 to
17.47 in comparison with that after the first healing. This remark-
able feature was attributed to the combined effects of the proper
addition of FA and sufficient reaction space induced by a high load
level. Nevertheless, Specimen FA55-B-80-H2 did not perform as
well as Specimen FA35-B-80-H2, where the ratio slightly increased
from 0.26 to 0.27. Although the presence of unhydrated FA was
favorable for the self-healing of the specimens after 28 days’ curing,
excessive FA additives reduced the amount of cement and resulted
in the decrease of calcium hydroxide generated by the hydration
of cement. Therefore, it was detrimental to the pozzolanic reaction
of FA.

Water Absorption Test

To investigate the self-healing effect on permeation, which is very
important to the durability of concrete, water absorption tests were
also performed in this study. A lower water absorption rate repre-
sents a better resistance against water penetration and vice versa.

Fig. 11. Normalized water absorption rate: (a) unhealed specimens;

(b) specimens after the first healing; and (c) specimens after the second
Fig. 10. Water absorption test results for Specimen FA0-C-0-H0. healing.

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J. Mater. Civ. Eng., 2021, 33(1): 04020408

 mortar, resulting in a declined water absorption rate. As the load
approached to the peak value, more cracks were generated and
the coalescence of cracks prior to failure rapidly increased the water
permeability. The threshold stress level that influenced the water
absorption rate was around 80% based on the limited test results
in this study, which was in line with experimental findings reported
by Hearn (1996), Sugiyama et al. (1996), and Hearn and Lok
(1998).
Regardless of the predamage level and healing time, the water
absorption rate pronouncedly decreased when the FA replacement
ratio was improved from 0% to 35%. However, the water absorp-
tion rate dramatically increased with the FA replacement ratio of
55%, especially for the specimens after two times of preloading.
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The results clearly showed that a proper addition of FA (35%)
was effective to resist water invasion, which is in compliance with
the experimental findings reported by Şahmaran et al. (2008) and
Chahal et al. (2012).
In Fig. 11(b), the water absorption rate of the undamaged speci-
men with the mixture of FA0 is higher than that in Fig. 11(a). This
result was inconsistent with the findings observed by Şahmaran
et al. (2008), wherein generated hydration products blocked the
penetration path of water over time and reduced the initial rate of
water absorption. The possible reason may be the scatter results as
indicated by a large coefficient of variation as shown in Fig. 11(a).
The water absorption ratio of the undamaged specimens after
the second healing gave a much reasonable result, as depicted in
Fig. 11(c), which is much lower than that in Fig. 11(a).
Fig. 12. Typical results for Specimen FA35-B-80-H1: (a) SEM observation; and (b) EDS analysis.
© ASCE 04020408-10
J. Mater. Civ. Eng., 2021, 33(1): 04020408
When compared with the undamaged specimens, the water ab-
sorption rates of the mortar without FA in Fig. 11(b) witnessed a
decline of 34%, 30%, and 9% under the preloading levels of 30%,
60%, and 80%, respectively. The reduction percentage is larger
than that induced by preloading as shown in Fig. 11(a), implying
good self-healing behavior in the mortar without FA, which was
mainly attributed to the filling effect of the hydration products.
In addition, the water absorption rate increased with the damage
level because more cracks were generated by a higher preloading
level.
However, the water absorption rate dropped with the increase
of the damage level for the specimens with the mixture of FA35.
A pronounced self-healing effect was observed in Specimen FA35-
C-80-H1, where the water absorption rate decreased by 11% in
comparison with the specimens without preloading. One potential
reason was that a high preloading led to an adequate reaction
space, which is fundamental to the pozzolanic reaction of FA
(Termkhajornkit et al. 2009). For the specimens with the mixture
of FA55, only a slight decrease of the water absorption rate was
found when the preloading level was 60%, in comparison with the
undamaged ones, indicating a detrimental influence on the self-
healing behavior when a high FA replacement ratio was used.
Fig. 11(c) exhibits the normalized water absorption rates of the
specimens after the second preloading and healing. The water ab-
sorption rate of the specimens without FA declined by 16% and 10%
under the preloading levels of 30% and 60% in comparison with
the undamaged specimens, respectively. The reduction percentages
J. Mater. Civ. Eng.
 are slightly higher than those presented in Fig. 11(a), indicating the
presence of self-healing. However, this effect was weakened after
repeated loading, as suggested by the comparison with Fig. 11(b).
It should be pointed out that the water absorption rate of Specimen
FA35-C-80-H2 decreased by 12% in comparison with the undam-
aged ones, which was higher than the corresponding change of
Specimen FA35-C-80-H1. This was attributed to the pozzolanic re-
action of FA.
As mentioned previously, the activity of FA increased over time,
and sufficient calcium hydroxide was generated in the first healing
period. More importantly, a high predamage level provided ad-
equate space for the pozzolanic reaction. The combination of these
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features contributed to the apparent self-healing behavior under the
high repeated loading. For the specimens with the mixture of FA55,
the water absorption rate noticeably increased when a high predam-
age level was adopted, which again confirmed that the replacement
ratio with an excessive FA content had a detrimental effect on the
mortar.
SEM Observation
The morphology and composition of healing products are important
indexes of self-healing mechanism. SEM and EDS were adopted to
observe the morphology and analyze the composition of the healing
products, respectively. Taking Specimens FA35-B-80-H1 and FA35-
B-80-H2 as examples, typical results are given in Figs. 12 and 13,
Fig. 13. Typical results for Specimen FA35-B-80-H2: (a) SEM observation; and (b) EDS analysis.
© ASCE 04020408-11
J. Mater. Civ. Eng., 2021, 33(1): 04020408
respectively. The dashed lines represent the crack paths, and the rec-
tangles mark the area for EDS analysis.
In Fig. 12(a), two cracks intersect with each other at the cement
particle (circle area). This resulted in an easy invasion of water
and consequently promoted hydration of unhydrated cement. The
healing products help to fill the microcracks (Edvardsen 1999;
Şahmaran et al. 2008; De Rooij et al. 2011). In Fig. 13(a), few ce-
ment particles are observed, which implied that after two times of
the healing process, most unhydrated cements had been consumed,
and the pozzolanic reaction of FA took effect in healing cracks
(Termkhajornkit et al. 2009; Şahmaran et al. 2013; Zhang et al.
2014).
EDS analysis was conducted on the areas around microcracks to
further clarify the healing mechanism. Results revealed that cal-
cium (Ca), silica (Si), and oxygen (O) were the primary elements
of the healing products for both specimens. The high existence of
calcium and silica indicated that the main healing products were
composed of calcium silicate hydrate (CaH2 SiO4 · 2H2 O) as well
as calcium carbonate (CaCO3 ). For the first healing process, the
unhydrated cement reacted with water, generating calcium silicate
hydrate and calcium hydroxide. The dissolution and carbonation
of calcium hydroxide on the surface promoted the formation of
calcium carbonate (Hearn 1998; Edvardsen 1999; Sahmaran et al.
2017). The calcium hydroxide inside reacts with FA with the pres-
ence of water, called pozzolanic reaction, where calcium silicate
hydrate (C-S-H) is produced. However, the pozzolanic reaction
was not active until 28 days (Termkhajornkit et al. 2009).
J. Mater. Civ. Eng.
 Regarding the second healing process, little unhydrated cement
was left, and the pozzolanic reaction played a dominant role in heal-
ing of cracks. Consequently, more C-S-H gels occur in Fig. 13(a).
This was supported by the Ca/Si ratio in Specimen FA35-B-80-H2,
i.e., 1.52, which was lower than that of Specimen FA35-B-80-H1
(3.80). A lower Ca/Si ratio represents a higher amount of C-S-H,
which is the main source of mechanical strength of cementitious
materials (Fan and Li 2014; Siad et al. 2018; Öztürk et al. 2020).
Furthermore, the stiffness of C-S-H was directly influenced by the
Ca/Si ratio. The low Ca/Si ratio in Specimen FA35-B-80-H2 pro-
moted a higher stiffness than that in Specimen FA35-B-80-H1.
Therefore, a better self-healing performance was found in Specimen
FA35-B-80-H2, in which a higher recovery strength and more ac-
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cumulative energy were obtained, as mentioned previously.
Conclusions
This paper presents an investigation of the self-healing behavior of
cement matrices based on FA with a special focus on the effect of
repeated loading. Mechanical tests, AE analysis, water absorption
measurements, and SEM were used to monitor the existence of self-
healing and evaluate its efficiency. Variables including the FA
replacement ratio and preloading level were considered. Based on
current test results, the following observations can be made and
conclusions drawn:
• The recovery strength of the damaged specimens after the
immersion process was one of the indexes to evaluate the self-
healing behavior. However, this approach was insensitive to heal-
ing on a microscale or even on a mesoscale level until the event
accumulated to a certain level. AE analysis and SEM observa-
tion proved helpful to comprehensively assess the self-healing
performance.
• An appropriate amount of cement replaced by FA was beneficial
for the self-healing performance of mortar, leading to a better
strength recovery and resistance to water invasion. Based on
the mixture of FA35 adopted in this study, the strength increased
by 11% and the water absorption rate dropped by 12% in com-
parison with the undamaged specimens when subjected to a
high level of repeated loading.
• Self-healing behavior was witnessed in the specimens after re-
peated loadings, especially for those with a moderate FA replace-
ment ratio under a high level of predamage.
• SEM results demonstrated that the healing mechanism was
originally from the hydration of unhydrated cement and the poz-
zolanic reaction of FA. Furthermore, EDS analysis suggested
that the pozzolanic reaction was a domain effect in the second
healing process.
Data Availability Statement
All data, models, and code generated or used during the study
appear in the published article.
Acknowledgments
The authors gratefully acknowledge the financial supports provided
by the National Natural Science Foundation of China (Nos.
51878485 and 51938013) and the Top Interdisciplinary Funds
of Civil Engineering for Tongji University. Thanks also go to
Professor Xiang-Lin Gu for his guidance. Furthermore, the help
from undergraduate students Lian-Zhi Zhang and Rui-Qi Deng
is appreciated.
© ASCE 04020408-12
J. Mater. Civ. Eng., 2021, 33(1): 04020408
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