Fabrication and characterization of post fire self-healing of

concrete
Abstract
In this study, self-healing of cracks by using novel immobilization and encapsulated methods
in cement based composites is investigated. Particularly, bacteria (bacillus subtilis) is used
with calcium lactate inside carbon fibre balls and inside gelatine capsules in two different
experiments. Cement coating is provided over gelatine capsules. These capsules and balls
are mixed with cement, coarse aggregate, and fine aggregate to form cement based
composites. These composites are heated at high temperature (around 650 degree Celsius)
until crack is appeared in these samples. These samples are water cured for 28 days and it is
observed that crack is self-healed. The main advantage of using bacteria (bacillus subtilis) is
that this bacteria precipitates carbonate ion which fills the gap. It becomes active when it
gets contact of calcium lactate. When samples are heated, both carbon fiber balls and
gelatine capsules are bursted and bacteria (bacillus subtilis) comes out. SEM testing is
performed to observe crack filling and porosity at micro level.

1. Introduction
Concrete emerged as the most used construction materials around the world after the
invention of Portland cement in the early 19th century. Cement is the binding component in
the concrete mix, along with water and aggregates – rock, sand, or gravel. The presence of
cracks in concrete increases its permeability and provides access to moisture, oxygen,
carbon dioxide and detrimental chemicals (e.g., chloride, sulphate), which eventually causes
rebar corrosion and compromises the structural integrity. Common repair techniques
involve the use of sealant agents or utilization of biotechnology methods that can self-heal
the cracks [24]. The compressive strength of concrete increases and varies from 27.4 MPa to
68 MPa made crushed limestone sand and concrete made with 50 % of river sand plus 50 %
of recycle aggregate respectively. Also, the strength tensile increases and varies from 3.9
MPa to 8.75 MPa for the concrete made with river sand plus crushed limestone and
concrete made with river sand, respectively [30]. Researchers investigated supplementary
cementitious material which improves the workability and self-healing characteristic of
cement based composites. So cement based composites came into picture to improve
workability and healing of crack. A. Kanellopoulos et al. [23] encapsulated of mineral
compounds as healing materials for cement-based composites. Three liquid (sodium silicate,
colloidal silica and tetraethyl ortho silicate) and one powdered (magnesium oxide) minerals
were encapsulated in thin walled soda glass capsules. Water immersion resulted in crack
area closure that ranged from 85% to 100% for all mineral treated samples.
Mohammadhossein Zamani et al. [24] used a polyurea polymer because of its adaptable
mechanical properties needed for encapsulation (e.g. moisture barrier and spore
immobilisation) and its fast curing reaction is proposed as a potential suitable shield and
carrier for Bacillus pseudofirmus to produce calcium carbonate (CaCO 3) crystal. Besides fly
ash (FA) could be utilized as a supplementary cementitious material (SCM), for its pozzolanic
reactivity, in ordinary concrete [9,10] such that it enhances mechanical characteristics as
well as workability and at the same time it decreases heat of hydration. Fire disasters draw
attention of researchers towards the cement based composites which helps to self-heal the
crack with the help healing agent at high temperature which is better known as post fire
self-healing. At higher temperatures, cracking in cement composites occurs mainly due to
the internal pore pressure and thermal stresses [14]. There are several healing agents which
have been used in concrete. Some of them are recycled glass cullets, glass in powder form,
recycled carbon fiber, bacteria etc. These cementitious composites shows post fire self-
healing characteristics. In the event of fire, the high temperatures usually causes
dehydration of the portlandite and C-S-H gel, which generates water steam thus increase
the pore pressure inside the concrete. The generated pore pressure causes splitting of
concrete cover or structural spalling [1,2]. Zhu et al. studied fire resistance performance of
cementitious composites containing recycled glass cullets (RGCs). RGCs below 0.6 mm can
apparently prevent spalling/cracks under high temperature [6]. Ultra -fine recycled glass
cullet (size < 0.6 mm) shows best thermal insulation property in cementitious composites.
Ali et al. [7] reported that integrating the glass powder into concrete could improve its
residual strength after high temperature heating. Selim et al. [8] investigated effect of
elevated temperature and cooling regimes on the compressive strength, microstructure and
radiation attenuation of fly ash–cement composites modified with miscellaneous
nanoparticles. Compressive strength values for all composites were enhanced by heating up
to 250 degree C whereas, they were suppressed after firing 750 degree C. Akbar et al. [15]
investigated the effects of elevated temperatures (up to 900 degree C) on the reinforcement
mechanism of recycled carbon fiber (rCF) based cement composites. The reinforcing effect
of recycled carbon fiber (rCF) was promising up to 600 degree C due to the release of high-
pressure steam through channels on the surface of recycled carbon fiber (rCFs). At 900
degree C, recycled carbon fiber (rCFs) were fully decomposed and resulted in empty tunnels
which subsequently effected the performance of cement composites. A sharp decrease in
the compressive and splitting tensile strength was observed at 800 degree C while the
flexural strength was significantly reduced at 600 degree C. Karimi et al. [16] used bacteria
for healing of crack (bacillus subtilis) and does water permeability test result (depth of water
penetration). A maximum reduction of 50% was achieved in water penetration depth as a
result of the presence of bacteria in the concrete mixture. Zhang et al. [17] studied effects of
carrier on the performance of bacteria-based self-healing concrete. It was observed that the
batch prepared carrier has good quality stability, can achieve secondary strength growth,
has low porosity and small pore size, and can greatly extend the survival time of
microorganisms. The reaction involved in the self-healing of concrete can be expressed
through straightforward equilibrium suggested by (Jonkers et al. 2010) [18]. The bacteria
metabolically convert 1 mol of calcium lactate, Ca (C 3H5O3)2 into 1 mol of calcium carbonate
equation (1) [19-20].
Ca (C3H5O3)2 + 6O2 + (alkaliphilic Bacillus) = CaCO3 + 5CO2 + 5H2O……………. (1)
In addition Pattharaphon et al. [25] quoted in his paper about the mechanism of
carbonation at high temperature. The amount of portlandite (Ca(OH) 2) was determined by
the mass change at approximately 450–550 degree C, as portlandite transforms into CaO
and H2O [26,27], while the amount of calcium carbonate or calcite (CaCO 3) was obtained
through mass change during decarbonation that occurs around 650–900 degree C [27,28].
Usman et al investigated that the severity and duration of fire significantly affect the
strength and stiffness of concrete structure [11]. Generally, concrete exhibits better fire
resistance than steel. It is very rare for the concrete structure to entirely collapse even after
the severe fire [12-13]. This is mainly due to low thermal conductivity of concrete that
maintains relatively low temperature within the concrete core during the fire. The durability
of concrete is threatened by various processes of physical, chemical, mechanical, and
biological nature. The degradation of concrete is particularly affected by the opening and
propagation of cracks [31]. By adding various healing agents or components in the
conventional concrete, the cracks can be repaired without human intervention
[32].Durability of concrete can be improved by using bacteria (bacillus subtilis) as an agent
which heals the crack or opening in the concrete. It includes a phenomenon called bio-
calcification as a part of metabolic activity of bacteria. It is the technique via which the
micro-organism externally secretes calcium precipitate, in which the occurrence of a
carbonate ion forms CaCo3 which fills up the voids within the concrete texture hence making
it greater compact [33]. However, tremendous fire disasters can seriously degrade the
mechanical properties of concrete because of high temperatures (up to 1200 degree C in
tunnels) [3–5]. In this paper Vedratnam et al. investigated post fire self-healing of two types
of cement based composites. Vedratnam et al. performed fire testing, compressive strength
testing and morphological technique (SEM) on these two types of cement based
composites. One cement based composite having bacteria and calcium lactate inside the
carbon fiber balls. The other one is bacteria and calcium lactate in encapsulated form. It is
observed that cracks are healed because weight of encapsulated bacteria based
cementitious composites is increased by 170 grams after 28 days of curing. Whereas weight
of carbon fiber balls based cementitious composite is increased by 10 grams.

2. Materials and methods

2.1 Material

The concrete consisted of ordinary Portland cement (OPC), sand, coarse aggregate, and
replacement of 8% of sand and 10% of coarse aggregate with carbon fiber ball. Calculation of
compressive strength and self- healing of post fire concrete containing carbon fiber ball is one
target of this study. Bacteria is filled inside the carbon fiber ball and it is glued with epoxy
over the whole surrounding of the ball. Carbon fiber ball with epoxy is selected because it
provides initial swelling effect of carbon fiber during fire. Bacteria come out from the carbon
fiber ball. Water to cement ratio is been kept between 0.5.The other target of this study is to
calculate compressive strength and self-healing of post fire concrete containg bacteria and
calcium lactate encapsulated in gelatine capsule.

2.2 Mixing and Specimen preparation

2.2.1 Preparation of carbon based concrete
Bacteria (bacillus subtilis) with calcium lactate in powder form is mixed and filled in carbon
fiber balls. These balls are glued with epoxy. Cement, fine and coarse aggregate are premixed
for 1 min, then the carbon fiber balls are gradually added and mixing continued for 2 more
minutes to obtain an almost uniform distribution of materials. Mould has been taken 125 cm 3
by volume. Dry mixing was necessary to avoid adhesion and workability reduction of carbon
fiber ball after its exposure to water. Once the solid particles were well-mixed, water was
added, and mixing was continued for 3 more minutes. Five series of concrete are cast in
cubical molds to produce specimens with a side of 50 mm. After demolding, the specimens
were cured in tap water for 28 days. The specimens were divided into two sets: The first set
was subjected to the compressive strength test and self-healing behavior without the effect of
fire, and the second set was used to study the effect of fire on compressive strength and self-
healing behavior. In the second set, each specimen (side 50 mm) is kept on heater one by one
with the support of material having high melting point to know the effect of fire. The bottom
is supported by metal rod having high melting point.
2.2.2 Preparation of bacterial concrete with mixing of calcium lactate in
encapsulated forms
Compared to normal concrete, bacterial concrete possesses higher durability and engineering
concrete properties. The production of calcium carbonate in bacterial concrete is limited to
the calcium content in cement. Hence calcium lactate is externally added to be an additional
source of calcium in the concrete. The influence of this addition on compressive strength and
self-healing capability of cracks with the effect of fire is highlighted in this study. The
bacterium used in the study is bacillus subtilis and was added encapsulated form to the
concrete. Bacillus Subtilis is a self-healing agent in the concrete. Based on many types of
research, bacteria are encapsulated using different materials and chemical compounds.
Encapsulation is done to protect the bacterial spore [20]. Bacillus subtilis spore powder with
10% replacement of coarse aggregate and 8 % replacement of sand. Cement was mixed to
concrete. Calcium lactates is added to the concrete mixes to test the effect on properties of
concrete. Actually, the specimens were divided into two sets: The first set was subjected to
the compressive strength test and self-healing behavior without the effect of fire, and the
second set was used to study the effect of fire on compressive strength and self-healing
behavior.
Mix design of CBC (carbon based concrete) (Kg/m3):

Mix description
Cement Coarse aggregate Fine Water
aggregate
Plain concrete as
control
443.5 Kg 1273 Kg 594.5 Kg 221.75 Kg

Figure –1
Calcium Lactate, Bacillus Subtilis (Bacteria) and Gelatin capsules

Figure – 2
Bacillus Subtilis and Calcium Lactate filled Gelatine Capsules
 Figure – 3
Cement coated Gelatine Capsules Filled with Bacillus Subtilis and Calcium
Lactate
2.3 Experimental Programme

A total 6 samples of carbon fiber balls based concrete are prepared and three of them
undergoes fire testing. The procedure of fire testing is as follow- Connecter is connected to
computer through data cable. Two thermo couples are connected to two faces of each sample.
The other end of thermo couple is connected to data analoger through wire. A total 6
encapsulated bacteria based cementitious composite sample size of 100 mm have prepared
and weighted first and it is observed that weight of each sample is 2 kg then 3 samples out of
6 undergoes fire testing applying same procedure as performed in fire testing of carbon fiber
balls based cementitious composites. Algaifi et al. [22] quoted Jonkers, Thijssen, Tziviloglou,
Wiktor about the effect of curing conditions (i.e., wet-dry and water immersion cycle) on the
productivity of CaCO3 for bio-mortar crack. The results demonstrated that water immersion
condition performed better than wet-dry cycle, in which crack widths of up to 0.36 mm was
fully closed in the immersion water condition, while no precipitation was observed in the
wet-dry cycle. So fire tested 6 samples are left in water for curing for 28 days.

3. Result and Discussion-

 Fire Testing Photographs

Figure -4 Figure -5 Figure – 6

Fire testing photographs reveals region of maximum temperature as indicated by a
small point. Theses photographs also signifies various temperature regions by
different colors.

3.1 Scanning Electron Microscopy Results-

SEM used to investigate the role of microbiologically induced mineral precipitation in

healing associated with micro crack closure, enhancing the durability and strength aspects of
concrete. It can be seen by Rauf et al. [29] that calcite crystals of size 50 micro meter existed
in deformed lamellar form. Cubic sample of 50 mm side and 10 cm side were water cured for
28 days after fire testing. It is found that the weight is increased by 20 grams in carbon fiber-
bacteria based cementitious composite and 170 grams in encapsulated bacteria based
cementitious composite respectively. Then their SEM testing is conducted in pantnagar SEM
laboratory and resulting photographs are shown below.

Figure 7 Figure 8

Figure 7 shows the result of SEM testing of concrete having bacteria and calcium lactate
inside carbon fiber ball and figure 8 shows bacteria and calcium lactate inside gelatine
capsule respectively. Both are treated with fire. Both are water cured for 28 days before fire
testing.

Figure 9

Figure 9 shows the characterization of concrete having bacteria (bacillus subtilis) and calcium
lactate inside carbon fiber ball and bacteria. Bacterial precipitation may be achieved through
conversion of calcium compound such as Calcium lactate. Crack openings let oxygen
penetrate inside concrete and bacteria along cracked surfaces convert calcium lactate into
calcium carbonate and carbon dioxide. If there are portlandite particles in the vicinity reaction
with produced carbon dioxide would yield more calcium carbonate which may as well be
used for healing. Therefore, it may be understood that this mechanism would be more
efficient in case of fresh concrete when there are still unhydrated calcium hydroxide particles.

Figure 10 Figure 11
 Figure 12 Figure 13

3.2 Mechanical Testing:

Figure (a) Figure (b)

50

)
℃
perature ris
e( 40

30
Power-based self-healing concrete
atic tem
Capsule-based self-healing concrete
Normal concrete
20
Adiab

10

0
0 2 4 6 8 10
 c. Adiabatic temperature rises
Comparison of the compressive behavior.

Figure 17

a. Evolution of compressive strength over time b. The stress-strain relationship [17]

Compressive strength test is the most important of many tests applied to the concrete,
which gives an idea of all the characteristics of concrete. One judges by this single test
whether or not Concreting has been done properly. One determines by this single test
whether or not Concreting has been done properly. Concrete compressive strength depends
on many factors such as water cement ratio, cement density, concrete content performance
and quality control during concrete production, etc [33]. The addition of bacteria to the
control specimen enhances the compressive strength about 3.9% at 28 days [21].In this paper
Vedratnam et al. performed compressive strength testing on 50 mm side cubic shaped carbon
fiber and bacteria based composite and it was found that post fire compressive strength of
carbon fiber based cement composites is 4.8 MPa and deformation is 37 mm. Post fire
compressive strength of encapsulated bacteria based composite decreases and it is 1.2 MPa
which is quiet lower than the compressive strength of concrete without the effect of fire.
Deformation is 28 mm in post fire encapsulated bacteria based composite. Result shows that
compressive strength reduction is less in carbon fiber based composite.

4. Conclusion

 Weight of bacteria and calcium lactate filled gelatin capsules mixed concrete has
increased up to 170 gram after recurring of 28 days which shows the sign of self-
healing.
 Weight of bacteria and calcium lactate filled carbon fiber balls has increased up to 20
gram after recurring of 28 days which is the sign of self-healing in sample.
 Samples are more porous which are under fire exposure. It is cleared from SEM
images.
  Cracks are filled up to an extent because of self-healing. It is shown in the
photographs.
 Temperature rises slowly when sample is exposed in low flame and reaches to its
peak value taking more time.
 Crack appears after 50 minutes duration in fire exposure. Samples without fire testing
are less porous.
 In samples of bacteria and calcium lactate filled carbon fiber balls , carbon fiber balls
are bursted in the exposure of fire at a particular temperature and bacteria with
calcium lactate comes out from carbon fiber balls. Chemical reaction takes place and
precipitation of calcium carbonate occurs in the damage region. Thus the self-healing
takes place.
 In samples of bacteria and calcium lactate filled gelatin capsules, gelatin capsules are
broken and precipitation of calcium carbonate takes place due to chemical reaction in
crack region.
 Compressive strength reduction is less in carbon fiber based composite.

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