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Microscopic Observations of Self-Healing Products in Calcareous Fly Ash

Mortars

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DOI: 10.1002/jemt.22440

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 MICROSCOPY RESEARCH AND TECHNIQUE 78:22–29 (2015)

Microscopic Observations of Self-Healing Products in

Calcareous Fly Ash Mortars
 ZWIAK-NIED
DARIA JO  
ZWIEDZKA*
Institute of Fundamental Technological Research, Polish Academy of Sciences, Pawinskiego 5B, 02-106, Warsaw, Poland

KEY WORDS self-healing; cement matrix; stereomicroscope; SEM; EDX analysis

ABSTRACT The results of microstructural characterization of mortars containing fly ash

class C (High Calcium Fly Ash) from combustion of lignite are presented. The evaluation of the
microstructure was performed using scanning electron microscope, optical, and confocal micro-
scope. The tested beams were bent till the crack and microcracks opening, which were healed
during the different curing time. The results showed that the replacement of cement with fly ash
class C influenced the process of crack healing. The addition of HCFA, at both 30% and 60%,
speeds up the self-healing process in cracks and particularly in micro-cracks. In the research,
the completely filling up of the cracks by new phases has not been observed, only the beginning
of such process has been noticed. Microsc. Res. Tech. 78:22–29, 2015. V 2014 Wiley Periodicals, Inc.
C

INTRODUCTION analysis (SEM-EDX), differential scanning calorimetry

The sustainability of concrete outdoor structures is of
primordial importance for countries with climate simi-
lar to that of Central Europe and it is closely related
to the durability of concrete, being a function of its per-
meability to liquids and gases. Structures exposed to
the natural aggressive environment are susceptible to
cracking and that is why cracks and microcracks
are always present during the lifetime of a concrete
structure (Darimont, 1993; Jozwiak-Niedzwiedzka
et al., 2012; Ramachandran, 2001). These discontinu-
ities determine the transport properties across concrete
elements and reduce their durability.
However, there exists a phenomenon known since
many years (Abrams, 1917) that cracked concrete has
the ability to heal itself over time when exposed to
humidity (e.g., Edvardsen, 1999; Herbert and Li,
2013). It has been found that there is a gradual reduc-
tion in permeability of cracked concrete elements
when enough humidity is available, for example when
water is allowed to flow through cracks and micro-
cracks. The decrease in permeability is, among the
others, because of reduction of the crack width as the
healing process advances, and new products develop
between the edges of cracks (Wu et al., 2012). Also, the
reduction in permeability will be dependent on the
materials that are precipitated in the cracks and the
effectiveness of this precipitation to keep moisture out.
In the article, the new products resulting from self-
healing process in the calcerous fly ash mortars are ana-
lyzed as to their nature and composition. The Portland
cement was partially replaced in the mortar elements
with high calcium fly ash (HCFA), and mechanical prop-
erties and durability of such composite material were
examined. Different levels of microscopic observations
including optical microscopy, laser confocal microscopy,
and commonly known scanning electron microscopy
were applied. Microanalysis of the mortar constituents
and self-healing products were also performed by
scanning electron microscope-energy dispersive X-ray
(DSC), and thermogravimetric analysis (TGA) methods.
PRESENT STATE OF KNOWLEDGE
The process of the so-called self-regeneration or
autogenous healing is universally recognized (Herbert
and Li, 2013; Hosoda et al., 2009), but was never
exploited in standardizing neither design procedures.
Different mechanisms for self-healing of cracks in con-
crete were reported (e.g., Edvardsen, 1999; Jozwiak-
Niedzwiedzka et al., 2012; Reinhardt and Jooss, 2003;
Van Tittelboom et al., 2012; Yang et al., 2011). There are
the organic phenomena that help to heal cracks (Bang
et al., 2001) and the systems of incorporated micro-
capsules with monomers, as repair agents, are intelli-
gently applied (Dry, 1996; Van Tittelboom et al., 2012).
However, it seems that the most efficient mechanism is
connected with the autogenous healing of cracks that is
based on the chemo-physical processes occurred in con-
crete microstructure (Ahn and Kishi, 2010; Bang et al.,
2001; Homma et al., 2009). In many studies, it was shown
that the crystallization of calcium carbonate within cracks
and microcracks is the main mechanism for self-healing
in mature concrete elements (Jozwiak-Niedzwiedzka
et al., 2012; Van Tittelboom et al., 2012; Yang et al., 2011).
The research by Jozwiak-Niedzwiedzka et al. (2012),
Edvardsen (1999), Reinhardt and Jooss (2003), and
Homma et al. (2009) revealed also that the self-healing
phenomenon occurs first of all in microcracks below 30
mm. Besides, the low water/binder ratio, in addition to
the large amount of secondary cementitious materi-
als—fly ash—in mixture composition helps to promote
*Correspondence to: Daria Jozwiak-Niedzwiedzka, Institute of Fundamental
Technological Research, Polish Academy of Sciences, Pawinskiego 5B, 02-106
Warsaw, Poland. E-mail: djozwiak@ippt.pan.pl
Received 2 July 2014; accepted in revised form 14 September 2014
REVIEW EDITOR: Dr. Chuanbin Mao
DOI 10.1002/jemt.22440
Published online 25 September 2014 in Wiley Online Library (wileyonlinelibrary.
com).

C
V 2014 WILEY PERIODICALS, INC.
 SELF-HEALING PRODUCTS IN CALCAREOUS FLY ASH MORTARS 23

self-healing via continued hydration and pozzolanic
activities (Schlangen et al., 2010). Lubelli et al. (2011)
observed that the presence of a considerable amount of
free lime was a necessary condition for the occurrence
of the self-healing, and in the mortars with only
cement as a binder no self-healing was observed. The
amount of free Ca(OH)2 produced by hydrolysis of
Portland cement clinker was not sufficient to result in
any effective self-healing. Heide Ter (2005) concluded
that the extent of healing is larger for concrete with
binders with Portland cement without blast furnance
slag.
In high calcium lime mortars, two Ca-bearing com-
pounds are present: Ca(OH)2 and CaCO3; the latter
usually as calcite, though minor amounts of aragonite
and vaterite might be present (Lubelli et al., 2011).
The presence of other components in the matrix may
also influence the solubility of Ca compounds, for
example NaOH and Na2CO3 can strongly decrease cal-
cite solubility, while K2SO4 and CaSO4 decrease it only
slightly. Lubelli et al. (2011) suggested that adding
free lime to cement-based mortars might improve their
self-healing capacity and they concluded that the opti-
mal amount of free lime to be added in order to reach
self-healing needs to be determined.

MATERIALS AND MIXTURE PROPORTIONS

Fig. 1. SEM micrograph showing the morphology of: (a) cement
CEM I and (b) HCFA particles used in the research.
The supplementary cementitious material used in
the research was unprocessed HCFA from Polish lig-
nite burning power plant. This HCFA is mostly in the
form of spherical particles with predominant grain
size between 60 and 20 mm and conglomerates both,
spherical and irregular shape, size from 60 to 80 mm.
These sizes are very large for typical fly ash because
they consist mainly of conglomerates. The surfaces of
the spherical particles differed from each other as to
their morphology. The example of the SEM micro-
graphs of the ordinary Portland cement and HCFA is
shown in Figure 1. HCFA from Polish lignite burning
power plants is a very fine powder, exhibiting not only
the pozzolanic properties but also hydraulic properties,
originating from the presence of highly active constitu-
ents, such as reactive lime, reactive silica, and alu-
mina. HCFA also contains significant amounts of
calcium aluminates glass which is more soluble than
the glass in low-calcium fly ash and may slowly release
calcium and aluminum into solution. The phase com-
position of this kind of fly ash is more complex than
the composition attributed to the commonly used sili-
ceous fly ash. The chemical composition of HCFA used
in research and the fly ash requirements according to
American and European standards are presented in
Table 1. The inconveniences arising from the use of
calcareous fly ash as a component of concrete mix (the
variability of fly ash properties and their composition,
high water demand, concrete mix fluidity deteriora-
tion, the problems of fly ash compatibility with chemi-
cal additives, etc.) were shown in previous research
described by Jozwiak-Niedzwiedzka et al. (2012) and
Jozwiak-Niedzwiedzka et al. (2013), but the results
from the above publications allow to conclude that HCFA
can be a useful addition to mortars and concretes.
Ordinary Portland cement (OPC) and HCFA were
used in all tested mortars. Plain mortar with Type I

TABLE 1. Requirements for fly ash according to ASTM C618-03 and PN-EN 450-1 and chemical composition of HCFA used in research
ASTM C618
PN-EN 450 High Calcium Fly
Constituent Fly ash class F Fly ash class C Type II addition Ash used in research
SiO21Al2O31 Fe2O3, min, % 70 50 —a 58.28
SO3, max, % 5 5 3 4.33
Na2O, max, % 1.5 1.5 —a 0.31
CaO free, max, % —a —a 2.5 3.43
OI 1000oC/1 h, max, % 6b 6 5 2.56
a
Not taken into consideration.
b
The use of Class F pozzolan containing up to 12.0% loss on ignition may be approved by the user if either acceptable performance records or laboratory test results
are made available.

Microscopy Research and Technique

24  ZWIAK-NIED
D. JO  
ZWIEDZKA

TABLE 2. Mineralogical phase composition of high calcium fly ash cement CEMI 42.5R (R-0) and fly ash mortars (R-30
and ordinary Portland cement, in wt%, XRD method, partially from and R-60) in which 30% and 60% respectively by mass
Garbacik (2012)
of cement was replaced by HCFA were prepared in
HCFA OPC
laboratory.
Amorphous 52.8 C3 S 60.5
Quartz SiO2 14.8 C2 S 18.5
Mullite Al6Si2O13 2.8 C3 A 9.0
CaO free 1.5 C4AF 8.0
Anhydrite CaSO4 6.3 TABLE 3. Mortar mixture proportions in (kg/m3)
Larnite CaO2SiO4 4.5 Materials R-0 (control) R-30 R-60
Gehlenite Ca2Al2SiO7 4.7
Anortite CaAl2Si2O8 7.9 Cement CEM I 42.5R 1000 700 400
Ca3Al2O6 2.4 Siliceous sand (0 4 2.0 mm) 600 600 600
Hematite Fe2O3 0.7 High calcium fly ash 0 300 600
Brownmillerite Ca(Al,Fe)2O5 0.9 Water 400 400 400
Sum 99.3 96.0 Fibers, 1% vol. 78.6 78.6 78.6

Fig. 2. Microphotograph of the (a) main crack and microstructure and (b) working fibers in the mortar
specimens without HCFA—R0 after 57 days of healing. [Color figure can be viewed in the online issue,
which is available at wileyonlinelibrary.com.]

Fig. 3. Microphotograph of the crack system in (a) R-0 and (b) R-60. The system of cracks consists of
the microcracks and the main crack. [Color figure can be viewed in the online issue, which is available at
wileyonlinelibrary.com.]

Microscopy Research and Technique

 SELF-HEALING PRODUCTS IN CALCAREOUS FLY ASH MORTARS
Mineralogical phase composition of OPC and HCFA
are presented in Table 2. The density of the OPC was
3.09 g/cm3 and HCFA 2.62 g/cm3. The natural siliceous
sand with nominal maximum size of 2.0 mm, specific
gravity of 2.65, and absorption of 0.3%, was used. The
Fig. 4. Images recorded with the confocal laser scanning micro-
scope, demonstrating the real depth of cracked concrete matrix,
approaching to 200 lm. The color mapping was used to present the
local depression of the surface. [Color figure can be viewed in the
online issue, which is available at wileyonlinelibrary.com.]
Fig. 5. Example of the crack depth measurement on the cross-section from confocal laser scanning
microscope (mm). [Color figure can be viewed in the online issue, which is available at wileyonlinelibrary.
com.]
Microscopy Research and Technique
25
water-to-cementitious (cement 1 HCFA) material ratio
was 0.40. Superplasticiser was not added because of
acceptable workability of the mix. In examined mor-
tars, the volume fraction of binder matrix was higher
than 70%, and the volume fraction of sand was only
slightly above 20%, which was not typical composition
of the mortar contained in a typical concrete. The rea-
son for this specific composition choice was the increas-
ing of the scope of the self-healing process. Steel
microfibres Dramix OL6/0.16, 1% vol, 6 mm long, and
0.16 mm in diameter, made with high-carbon steel
with minimum tensile strength equal to 2,000 N/mm2
were added. Dispersed steel microfibers (1% vol) were
added in order to assess the growth of cracks in a rela-
tively brittle material. The details of mixture propor-
tions are given in Table 3.
Coupon specimens 240 mm 3 320 mm 3 40 mm
were cast and cured for 1 day in the molds under
sealed conditions. Then, the coupons were cured in
water for another 27 days. At the age of 28 days, each
coupon was sawn into six beams with the dimensions
of 220 mm 3 40 mm 3 40 mm. The beams were loaded
in four-point bending test and the support span was
set up for 200 mm with the middle span equal to
66.7 mm. All beams were loaded in Lloyd Ins. EZ 50 up
to maximum deflection equal to 0.3 mm and pre-
cracked. The loading procedure was controlled by
deflection at a constant rate of 0.01 mm/sec, and the
load was varying as it was required by decreasing
beam stiffness after crack opening. This deflection was
arbitrarily selected in order to obtain central crack in
the beam of appropriate width for the self-healing. The
tests were repeated at selected dates (1st, 2nd, and 3rd
loading) to observe and record the advance of the heal-
ing process in time; the detailed test program is
described by Jozwiak-Niedzwiedzka et al. (2012). Addi-
tionally, the acoustic emission events were registered
and recorded in order to monitor crack propagation
(Ranachowski et al., 2012).
RESEARCH PROGRAM
The evaluation of changes in the cracks due to self-
healing was performed using optical microscopy, scan-
ning confocal microscopy, and secondary electron
microscopy. The stereomicroscope Nikon SMZ 800 and
color video camera SONY DXC 950P were used for
determination of the microstructural changes in the
specimens at the micro scale (magnification 363). In
the higher magnification, the specimens were examined
using a combination of SEM with the back scattered
26  ZWIAK-NIED
D. JO 
Fig. 6. Microphotograph from the stereomicroscope, observation of
the beginning of the self-healing process in: (a) reference mortar-R0,
(b) mortar with 30% HCFA-R30, (c) mortar with 60% HCFA-R60
[Jozwiak-Niedzwiedzka et al., 2012]. [Color figure can be viewed in
the online issue, which is available at wileyonlinelibrary.com.]
electrons (BSE), and EDX. Additionally, certain sam-
ples were analyzed using Laser Scanning Confocal
Microscope of LEXT type equipped with a MPALON
object-lens of 320 magnification. Images obtained with
the latter equipment were taken of surfaces polished in
the same way as for the SEM analysis.

ZWIEDZKA
Specimens for stereomicroscope examinations were
dried in an oven at 35 C for three days and then ana-
lyzed with the use of the image analysis software
Image Pro Plus. A sample to be examined in back scat-
tered electron microscope (BSE mode) was dried in an
oven at 50 C for 72 h and then vacuum-impregnated
with a low-viscosity epoxy. The impregnated specimens
were lapped and polished using a special procedure.
The polished face of the specimen which was to be
examined was essentially the region in the beam
approximately 10 mm from the crack for both sides. A
strip of conductive copper tape was attached to each
polished sample, after which they were coated with a
thin layer of palladium for about a minute using a
HummerV R 6.2 sputter coater. Each of the samples
was thoroughly examined using AspexV R LLC personal
SEM in the BSE mode using an acceleration voltage of
15 kV.
The specimens were analyzed after 1st loading in
the SEM-EDX mode on the polished surface and after
3rd loading, and additional 28 days of curing in the
water (total 170 days of curing)—in the stereomicro-
scope. Parallel with microscopic observations after 170
days of curing, the SEM analysis was executed on the
split surface of the specimen.
Apart from the SEM-EDX microanalysis, the TGA
and the DSC were applied also. TGA methods were
used to investigate the thermal characteristics of the
tested mortars. The material for the TGA/DSC analy-
sis was taken from mortar beams after the end of load-
ing process. The prismatic specimens were cut in a
way to avoid the influence of carbonation process. The
obtained material was selected and dried in 140 C for
72 h, then it was preliminary grinded and the steel
fibers were selected with magnet. The rest of the mate-
rial was re-grinded and sieved by 0.063 mm sieve.
RESULTS AND DISCUSSION
In all the tested specimens after the first loading dur-
ing the pre-cracking procedure, a single main crack of
the width about 100 lm appeared (Figs. 2–4). At pre-
cracking, all load–deflection curves showed quasi linear
behavior up to cracking, and then deflection increased
with approximately constant load. All mechanical results
concerning this research are described by Jozwiak-
Niedzwiedzka et al. (2012). The main crack did not con-
tain any new hydration or self-healing products but it
was bridged by fibers (Fig. 2b), which provided correct
application of this kind of reinforcement. Steel fibers tend
to stop or reduce crack propagation (Fig. 2b). It was
observed that in all tested specimens the main crack did
not influence any possible aggregate breaking, cracking,
or debonding. The cracking process was visible only in
the matrix and in the ITZ (Interfacial Transition Zone)
zone.
The image of the observed main crack taken in the
confocal laser scanning microscope (Figs. 4 and 5) con-
firms that crack is present and demonstrated the
depth of the crack propagation which approached to
about 200 mm. The depth of the main crack was meas-
ured in 10 places in the way as shown in the Figure 5.
The process of self-healing was observed in all tested
specimens, despite various matrix components but
with different level of appearance (Fig. 6). This process
was noticeable already after 57 days of curing (SEM
Microscopy Research and Technique
 SELF-HEALING PRODUCTS IN CALCAREOUS FLY ASH MORTARS 27

Fig. 7. Scanning electron micrographs for mortar specimens without replacement of calcareous fly
ash—R0, after 57 days of healing. The presence of the portlandite in the crack is marked.

Fig. 8. Scanning electron micrographs for mortar specimens with 60% replacement of cement by cal-
careous fly ash, R-60. The monosulfate in the crack is formed [J
ozwiak-Niedzwiedzka et al., 2012].

TABLE 4. Differential Scanning Calorimetry results for R-0 mortar without calcerous fly ash and R-60 mortar with 60% of calcareous fly ash
Loss of weight (%)

Specimen 40–100 C 100–400 C 400–500 C 500–600 C 600–700 C 700–1000 C 0–1000 C

R-0 4.2 5.2 3.4 1.2 1.2 1.1 17.0
R-60 6.6 6.0 0.6 2.0 0.7 17.0

analysis), but the visible changes in larger cracks (> nomenon was observed in mortars with 60% of cement
150 mm) in bridging of the microcracks were found replacement by HCFA that apparently stimulated
after 170 days of curing. The more visible healing phe- self-healing of microcracks. Examples of a kind of

Microscopy Research and Technique

28
D. JO 
TABLE 5. Thermogravimetric Analysis results for R-0 mortar with-
out calcareous fly ash and R-60 mortar with 60% of calcareous fly ash
Content of constituents (%)
Bound water
Specimen HI HCH R Portlandite Calcitea
R-0 10.0 3.4 13.4 14.0 5.4
R-60 13.7 0.6 14.3 2.5 4.5
a
Carbonates in terms of calcite content.
“bridges” across microcracks observed additionally in
stereomicroscope are shown in Figures 6a–6c. The
microphotographs from the stereomicroscope are sup-
plement to the SEM-EDS micrographs and analysis.
The stereomicroscopic observation of the beginning of
the self-healing process in larger cracks showed that
this process was still developing. The self-healing
products which were visible in SEM after 56 days of
curing, probably, are also present after 171 days of cur-
ing but in wider cracks.
The more precise analysis of the finer cracks (width
less than 30 lm) which opened near the main crack
revealed that specimens with and without HCFA
replacement differ from each other in the presence of
the new products in cracks (Figs. 7 and 8). In the
smaller cracks in the mortars made without calcareous
fly ash, the portlandite was present (Fig. 7) opposite to
the specimens made with HCFA where the monosul-
fate was present in the cracks (Fig. 8). Monosulfate is
extremely common hydration product in mortars and
concrete. When tricalcium silicate and calcium sulfate
reacts they will produce ettringite and monosulfates
depending on the sulfate levels in solution. Monosul-
fates would be expected to be found in all the tested
mortar specimens, but it was present in one specimen,
with 60% of HCFA. Application of HCFA in concrete
was identified as a potential source of ettringite (Tish-
mack et al., 2001) in Portland cement concrete due to
significant amounts of sulfur, calcium, and aluminum,
but in this case the monosulfate was created, probably
due to the presence of the HCFA (high sulfur content)
in the matrix.
The HCFA mortars generally formed more of the
AFm phases (the monosulfate group, Al-Fe-mono;
mono 5 one mole of CS) than the AFt phases (the
ettringite group, Al-Fe-tri; tri 5 three moles of CS)
(Tishmack et al., 2001). Previous study by Tishmack
et al. (1999) indicated that the addition of HCAF
reduces the SO4/Al2O3 ratio in the system, thus favor-
ing the AFm formation. Monosulfate masses tend to
show its typical structure, according to Diamond
(2004) like the straight “cleavage-like” shrinkage fea-
tures. The EDX spectrum is characteristic for mono-
sulfate where the peak for sulfur is smaller than the
peak for aluminum. The mortar specimens analyzed
after 170 days of curing also indicated the presence of
monosulfate in the microcracks (Fig. 8).
The results of the DSC-TGA mortars analysis con-
firmed the microscopic observations (Tables 4 and 5).
The largest differences were noticeable in mortars
without and with 60% of calcareous fly ash. The
content of portlandite amounted to 14% (R-0) and 2.5%
(R-60). The bound water and carbonates content was
 ZWIAK-NIED

ZWIEDZKA
similar for all the tested mortars. For R-0 amounted to
13.4% and 5.4% consecutively and for R-60 14.3% and
6.1%. In hydrated silicates and calcium aluminum sul-
fates, content of the bound water was equal to 10% for
R-0 and 13.7% for R-60 that could suggest the higher
LOI
1000 C/1 h content of the hydrated calcium silicates in the fly ash
matrix. The replicate specimens were investigated and
17.0 they confirmed the differences in bound water. It may
17.0
be attributed to the reduction of calcium hydroxide
and the subsequent production of calcium silicates or
calcium aluminum silicates in the fly ash specimens.
CONCLUSIONS
The microstructural changes in matrix due to self-
healing phenomenon were analyzed. Complete self-
healing of microcracks was not observed, though ini-
tiation of the process was visible until 24 weeks of cur-
ing in water, but replacement of cement by HCAF
apparently stimulated self-healing of cracks and par-
ticularly of microcracks.
After the microscopic observations and microanaly-
sis of the tested mortar specimens, it can be concluded
that products of the self-healing appeared inside all
tested mortar specimens in microcracks, but the larger
progress of self-healing process was observed in mor-
tars with 60% replacement of Portland cement with
HCFA.
The microscopic analysis showed differences in mor-
phological and chemical composition of self-healing
products in mortar specimens due to different contents
of calcerous fly ash in the matrix. The content of sulfur
in HCFA probably influenced on the composition of the
self-healing products. According to Tishmack et al.
(1999), the replacement of cement by HCFA reduced
the SO4/Al2O3 ratio in the system, so most likely favor-
ing formation of monosulfate instead of ettringite. The
sulfur content, which is relatively high in HCFA, is
decisive in the formation of monosulfate.
It may be supposed that the phenomenon self-
healing in calcareous fly ash mortars occurred mainly
due to the swelling effect, expansion effect, and recrys-
tallization, what corresponds with the results of Ahn
and Kishi (2010).
Probably the HCFA can be considered as a valuable
constituent of cement-based materials when the resist-
ance or even durability to fluid or gaseous media is
required and the future research will focus on this
problem.
ACKNOWLEDGMENTS
The results presented in the paper have been obtained
within the Project “Innovative cement binders and con-
cretes with addition of high calcium fly ash” (Project
no POIG.01.01.02–24-005/09 with the Polish Ministry
of Science and Higher Education) in the framework of
the Operational Programme Innovative Economy
2007–2013.
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