Construction and Building Materials xxx (2014) xxxxxx

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Construction and Building Materials

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Characterization of sustainable bio-based mortar for concrete repair

M. Guadalupe Sierra-Beltran , H.M. Jonkers, E. Schlangen
Delft University of Technology, Faculty of Civil Engineering & Geosciences, Department of Materials & Environment, Stevinweg 1, 2628 CN Delft, The Netherlands

h i g h l i g h t s
 O2 consumption was used to characterized bacterial activity in bio-based mortar.
 Bio-based agents used in SHCC enhanced its self-healing capacity.
 Bio-based SHCC exhibits good mechanical and bonding behaviour as a repair material.

a r t i c l e

i n f o

Article history:
Available online xxxx
Keywords:
Concrete repair
Bio-based mortar
Bacteria
Crack healing
Bond stress
Restrained shrinkage

a b s t r a c t
The paper describes mechanical properties, self-healing capacity and bonding behaviour of a sustainable
bio-based mortar repair system for concrete. Two different mixes of strain-hardening cement-based composites (SHCC) have been used. The bio-based agent added to the SHCC consists of both bacteria and food
for the bacteria. The metabolic activity of bacteria was monitored by oxygen prole measurements,
which reveals O2 consumption by bacteria-based samples, but not by control samples. The mechanical
properties of the mortar (exural behaviour, compression strength and drying shrinkage) are evaluated.
The bonding behaviour with the concrete substrate is evaluated based on pullout tests and restrained
shrinkage.
2014 Elsevier Ltd. All rights reserved.

1. Introduction
Currently available concrete repair systems face durability-related problems that have a huge impact on national economies.
In the United States of America, for instance, the annual direct
costs for maintenance and repair of concrete highway bridges
due to corrosion of the reinforcement sum up to 4 billion dollars
[1]. Most of the durability-related problems of repair systems are
due to the lack of compatibility with the concrete substrate. A combination of physical, chemical and mechanical processes results in
the failure of concrete repair [2,3]. Restrained volume changes due
to drying shrinkage or differential thermal expansion induce surface cracking in the repair system and interface delamination between repair and concrete substrate. Additionally, currently
available repair systems are largely based on environmental unfriendly materials such as epoxy systems, acrylic resins or silicone-based polymers. This paper focus on the characterization of
a concrete compatible and sustainable bio-based repair system

Corresponding author. Address: Delft University of Technology, Stevinweg 1,

Room 6.19, 2628 CN Delft, The Netherlands. Tel.: +31 (0)152789405; fax: +31
(0)152786383.
E-mail
addresses:
m.g.sierrabeltran@tudelft.nl
(M.G.
Sierra-Beltran),
H.M.Jonkers@tudelft.nl (H.M. Jonkers), h.e.j.g.schlangen@tudelft.nl (E. Schlangen).

that features better bonding and improved durability and sustainability characteristics compared to existing repair systems.
The European Standards describe the principles and methods
for protection and repair of concrete structures [4]. The repair system studied in this paper was designed as a product for concrete
restoration by applying or spraying mortar (repair methods 3.1
and 3.3), structural strengthening by adding mortar (repair method
4.4) or replacing contaminated or carbonated concrete (repair
method 7.2) [4].
A special type of strain-hardening cement-based composite
(SHCC), called Engineered Cementitious Composite (ECC) has been
studied as repair material for concrete structures for overlay
applications and patch repair [57]. ECC was micro-mechanically
designed to have a large strain capacity with a low percentage of
randomly distributed polymer bres [8]. Because of the presence
of bres the material develops multiple micro-cracks prior to
failure. The crack width remains below 0.1 mm [9]. In concrete repair materials bres are also used to control drying shrinkage and
service load-related cracking [5]. Repair materials crack when
subjected to differential shrinkage: the early-age shrinkage
deformation of the new repair material is restrained by the old
concrete substrate that has already undergone shrinkage. Tensile
stress is developed in the repair layer and a combination of tensile
and shear stresses built up along the interface between the repair
layer and the concrete substrate [5]. When applied as a repair

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material, ECC is capable of carrying more tensile load and accommodate larger tensile strain than other repair systems [6]. Under
differential shrinkage ECC will suppress localized brittle fracture
in favour of distributed micro-crack damage [5,6].
Autogenous healing can be understood as a natural process of
lling and sealing cracks without any external operations and
works [11]. Li and Yang [10] investigated autogenous crack healing
in ECC. They reinforced ECC with only 0.5% per volume of PVA bres in order to achieve wide cracks. They reported that ECC with
a maximum crack width of 50 lm achieved full recovery of
mechanical and transport properties due to autogenous healing.
Between 50 and 150 lm, partial recovery could be attained. Autogenous healing behaviour in SHCC heavily depends on the availability of unhydrated cement and other supplementary cementitious
materials, such as blast furnace slag or y ash. Low water/binder
material ratio and high percentage of binder material and a control
small crack width appear to promote autogenous healing in ECC
[12,13].
Conventional ECC is designed without coarse aggregates and
with only a small amount of ne sand in order to control the fracture toughness of the matrix [8]. This characteristic leads to higher
water to cement/binder ratio and eventually to a high value of
shrinkage [14]. Li [5] and Yang et al. [15] reported drying shrinkage
strain values of 1200  106 to 1800  106 for conventional ECC,
and Zhou [6] reported a drying shrinkage strain value of
2900  106 for ECC designed using limestone powder instead of
sand as ller. In similar drying conditions of 20 C and 60% relative
humidity, normal concrete has a drying shrinkage strain of
400  106 to 600  106 [16]. Conventional ECC uses micro-silica
with maximum grain size of 200 lm [10,17]. In this way the bres
in ECC are only separated by ne aggregate particles which are allowed to move freely between the bres. Particles that are bigger
than the average distance between bres will cause the bres to
concentrate in balls and lead to an irregular distribution of the bres [18]. As mentioned above, the particle size is limited in ECC
in order to limit the fracture toughness to a level in which the crack
initiation could occur before the tensile load reaches the maximum
bre-bridging stress that will result in failure of the bre bridges
[17].
To improve the durability of the concrete repair system as
well as to improve the bonding with the concrete substrate this
paper proposes a bio-based agent to be included in the ECC mix.
The bio-based agent consists of alkali-resistant bacteria and a
food source for those bacteria. When applied in concrete, this
bio-based agent has the capacity to produce calcite-based minerals inside cracks thus reducing the permeability of the concrete
[19,20]. The precipitated minerals lead to the closure of cracks
with a maximum crack width of 460 lm [20]. In case of surface
cracking in the repair mortar due to restrained shrinkage or
other mechanical processes the bio-based agent is capable of
healing these cracks to ensure the durability of the repair
product.
Repair materials are frequently subject to limited evaluations
driven by manufacturers rather than by users [21]. This is due to
a lack of widely accepted testing methods. If only the isolated
properties of repair materials are studied the more important
properties of the composite system are neglected. In this research,
the performance of the composite repair system as well as the
interaction between the repair and concrete substrate have been
investigated. Restrained shrinkage tests have been conducted on
a simulated repair system, that contains one layer of old concrete
substrate and one layer of new repair material to simulate real repair conditions.
For this study, two ECC-type mortars with particles containing a
bacterial-based agent have been studied as a sustainable bio-based
repair system for concrete. The mechanical properties of the ECC

materials are evaluated by means of exural and compression tests

and free drying shrinkage measurements. The behaviour of the ECC
material as a repair mortar is evaluated by means of restrained
shrinkage measurements and the bonding behaviour with the concrete substrate is evaluated based on pullout.

2. Experimental investigation
2.1. Materials
Ordinary Portland cement CEM I 42.5N, y ash (FA), blast furnace slag (BFS),
limestone powder (LP), sand (S) have been used. The chemical composition of the
powder materials are given in Table 1 and the mix designs in Table 2. The sand
has an average and maximum grain size of 250 lm and 500 lm respectively. In
the mix design, BFS, FA and Portland cement are considered as binder materials,
and the limestone powder is considered as inert ller material. Polyvinyl alcohol
(PVA) bres with a length of 8 mm and diameter of 40 lm have been used in the
content at 2% by total volume. These PVA bres have a tensile strength of
1600 MPa. The surface of the bres is coated with 1.2% oil by weight to optimize
the bre-cement matrix bond [22].
The bio-based agent considered for this research is an alkaliphilic (alkali-resistant) spore-forming bacteria and calcium lactate as a nutrient source for the bacteria. Both the bacteria and the food source are embedded in lightweight aggregates.
Bacteria from genus Bacillus and more specically related to the species B. cohnii
[23], originally isolated from alkaline soil samples were chosen for this research
[24]. Previous studies show that these bacteria are capable of healing cracks by direct and indirect calcium carbonate (CaCO3) formation [19,20]. The direct CaCO3
precipitation is due to the bacterial metabolic conversion of calcium lactate according to the following reaction:

CaC6 H10 O6 6O2 ! CaCO3 5CO2 5H2 O

The indirect formation is due to reaction of metabolically produced CO2 molecules

with Ca(OH)2 minerals (portlandite) present in the concrete matrix, according to:

5CO2 5CaOH2 ! 5CaCO3 5H2 O

The latter reaction is homologous to carbonation, a slow process that naturally

occurs in concrete due to inward diffusion of atmospheric carbon dioxide, whose
rate is however substantially enhanced by the metabolic conversion of calcium lactate [24]. The production of in total six calcium carbonate equivalents is possible
due to the process of bacterial calcium carbonate conversion, which will result in
efcient crack sealing.
To prepare the bio-based agent, lightweight aggregates (LWA) were rst
impregnated with calcium lactate (150 g/L) and yeast extract (7.5 g/L) solution followed by a second impregnation with a bacterial spore solution. Between impregnations the LWA were dried in an oven at 37 C for 5 days. The obtained
impregnated LWA contains 15% (by weight) calcium lactate and 1.2  107 bacterial
spores per gram of particles. The LWA particles have sizes ranging between 0.25
and 2 mm.
Bacterial spores are known to be able to withstand high mechanical forces and
are characterized by a long-term viability of up to 200 years under dry conditions
[25]. When mixed directly into concrete the number of viable spore cells in concrete decrease in time [24]. Later studies by the same author established that bacteria immobilized in porous expanded clay particles prior to concrete mix addition
substantially increased bacterially-mediated self-healing in comparison to unprotected addition of bacteria [19,20]. Furthermore bacterial spore viability increased
to more than 6 months when added protected inside porous particles to a concrete mixture [19]. Oxygen consumption measurements provided evidence of bacterial activity in concrete specimens up to several months after concrete casting
[20].

Table 1
Chemical composition (weight%) of the powders materials.
Compound

CEM I 42.5

BFS

FA

LP

CaO
SiO2
Al2O3
Fe2O3
MgO
K2O
Na2O
SO3
CaCO3

63.3
19.5
5.6
2.3
1.1
0.9
0.3
2.7

40.8
35.4
13
0.5
8.0
0.5
0.2
0.1

7.1
48.4
31.4
4.4
1.4
1.6
0.7
1.2

0.3
0.1
0.1
0.2

98.8

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Table 2
Mix design of mortars by weight (in kg/m3).

Type

Mix 1 control

Mix 1B
Bio-based

Mix 2
control

Mix 2B
Bio-based

Cement
BFS
FA
LP
Sand
LWA
Water
SP
PVA
w/b*

493

592
394

414
7
26
0.38

461

553
267

101
385
16
26
0.38

440
131
558

440

379
7
26
0.34

405
121
516

308
97
364
16
26
0.35

Water-to-binder ratio.

Superplasticizer (SP), Cretoplast SL01 from CUGLA (Breda, The Netherlands),

was used to achieve a workable condition of the mixtures. The specimens were prepared in a Howard mixer following different mixing sequences for each mix. For
Mix 1 rst all the powders were pre-mixed for 1 min. Then the water and superplasticizers were added and mixed. Later the PVA bres were slowly added and
mixed. For Mix 1B the mixing continued by adding the particles impregnated
with the bio-based agent and mixing at low speed. Due to the presence of sand
in Mix 2 the mixing sequence was modied to assure the proper consistence of
the paste at the moment the bres were added. First, 90% of the powders and
75% of the sand were mixed for 1 min. Water and superplasticizers were then added
and mixed followed by the PVA bres. Then the remaining powders and sand were
added and mixed. The mixing sequence for Mix 2B continued with addition of the
particles with bio-based agent.
The fresh mixtures were cast into moulds with dimensions of
240 mm  60 mm  10 mm
for
exural
tests
and
dimensions
of
160 mm  40 mm  40 mm for compression tests and free drying shrinkage measurements. After 24 h the specimens for exural and compression tests were
demoulded and moist cured in plastic bags at 95% relative humidity (RH),
25 2 C for 7, 28 and 56 days. The specimens for free drying shrinkage were placed
in a climate controlled room under conditions of 50 2% RH and 20 2 C.
2.2. Testing methods
2.2.1. Compression test
The compressive strength of the mortars was determined by testing at least four
40 mm cubic specimens at different ages. The cubic specimens were cut out of
beams of 160 mm  40 mm  40 mm.
2.2.2. Flexural test
A four-point bending test was performed under displacement control at a loading rate of 0.01 mm/s. The samples for exural tests have dimension
120 mm  30 mm  10 mm. They were cut out of specimens casted with dimensions 240 mm  60 mm  10 mm. The support span of the exural loading was
110 mm and the loading span was 30 mm. During the exural tests load and
mid-span deection were recorded. To investigate the self-healing capacity seven
and 28 days old specimens were loaded to a mid-span-deection of 2.5 0.2 mm.
When this deection was reached the load was released, after which the specimens
were removed and cured in water until age 56 days. At this age the surface cracks
were observed by means of a stereomicroscope. Afterwards, the specimens were
tested to failure to evaluate the mechanical properties. Specimens with and without
bio-based agent were kept in separate water containers to avoid cross contamination. Reference specimens from each mixture were cured under the same conditions as the pre-loaded specimens and were tested at 56 days.
2.2.3. Oxygen consumption and optical observations
Oxygen is consumed by aerobic bacterial metabolic conversion of calcium lactate [20]. In this research optical oxygen microsensors (micro-optodes) have been
used for the quantication of oxygen consumption of samples containing the biobased agent and for control samples. 3-month old specimens that have been aircured were placed in water 48 h prior to testing and cut just before the test. The
measurements were performed on the fresh fracture surface of these samples in order to monitor the O2 consumption and there for the bacterial activity. The cut samples were submerged in a solution with pH 11. Oxygen microproles were
measured in vertical steps of 20 lm, from 2.5 mm above towards the surface of
the specimens in the pH 11-solution at room temperature.
Microanalysis and electron imaging was done with an Environmental Scanning
Electron Microscope (ESEM, Philips XL30 Series) equipped with an Energy Dispersive X-ray (EDAX) element analysing system under hi-vac condition. The integrity
of the samples was maintained by impregnation using a low viscosity epoxy under
vacuum.

2.2.4. Interface bonding test

The tensile bond strength between the bio-based mortars and a concrete substrate was determined according to EN 12636 [26]. The surface of a 28-day old concrete samples was rst sand-blasted and then a primer was applied (Hechtprimer
Cement from CUGLA). Immediately after, a 12 mm layer of Mix 1B was casted on
top. After 28 days curing a ring groove was drilled through the mortar layer and
about 12 mm into the concrete substrate. Cylindrical steel dollies were then glued
to the mortar. The bonding tests were performed at age 35 days.
2.2.5. Free drying shrinkage
Drying shrinkage measurements were performed for all mortars on three
40 mm  40 mm  160 mm specimens up to 120 days after an initial curing of
1 day in the mould. The drying shrinkage specimens were stored in a drying room
at 20 2 C and 50 2% RH.
2.2.6. Restrained shrinkage
The restrained shrinkage of the two repair materials were studied by means of a
layered system consisting of a concrete substrate and a repair mortar, as can be
seen in Fig. 1. The dimensions of the concrete substrates are 500  100  100 mm
and the thickness of the repair layer casted on-top is 12 mm. The mix designs for
all the materials are reported in Table 3. The concrete samples were demoulded
after 24 h and then sealed with plastic and aluminium foil. After 7 days the cover
was removed exposing the samples to RH 50 5% and 20 2 C. The samples were
then cured under these conditions for 2 years. During this curing time any potential
shrinkage in the substrates occurs. To prepare the concrete samples for the restrained shrinkage test one side of the samples was roughened with a chisel and
steel brush to remove slurry cement from the surface of coarse aggregates, and later
this surface was cleaned with high-pressure air. The concrete substrates were then
moist-cured for 3 days after which the roughened side was dried. After casting a
12 mm thick repair layer on top of this contact surface the whole samples were covered with plastic and cured for 24 h. After demoulding, the layered specimens were
placed in a room with ambient conditions RH 50 5% and 20 2 C. For each specimen two dial gauges were used to record the interface delamination in terms of
interface vertical separation distance at end locations of the specimens as a function
of drying time. For practical applications such as the one represented in this test,
the author found that 2% per volume of bres could be reduced to 1.7% with only
a minor reduction in the deection capacity. The lower amount of bres will improve the mixing and ensure a uniform distribution of the bres in the mortar when
being mix at a construction site.

3. Results and discussion

3.1. Compressive strength
The average compressive strength of the four mixes is shown
in Fig. 2. The compressive strength of Mixes 2 and 2B are higher
than the strength of Mixes 1 and 1B. This is due to: A lower
water-to-binder ratio, higher binder content and the presence of
blast furnace slag. Mixes 1 and 1B full the compressive strength
requirement for repair material of concrete structures Class R3
(P25 MPa) according to the standards NEN 1504-3 [27]. Mixes 2
and 2B have compressive strengths higher than 45 MPa, fullling
the requirement for Class R4 in the same standard. In spite of the
fact that the mixes with bio-based agents have a lower amount
of cement than the control mixes and that the LWA containing
the bio-based agent are much weaker than the other ller components the average compressive strength at 7, 28 and 56 days of the
mixes with bio-based agent is higher than the average compressive
strength of the control mixes. This may be an effect of the presence
of calcium lactate in the bio-based agent. Jonkers and colleagues
[24] reported the same effect. Mix 2B has a lower amount of biobased agent compared to Mix 1B, and the increase of compressive
strength is less noticeable for Mixes 2B compared to Mix 2, than for
Mix 1B compared to Mix 1. For Mixes 1 and 1B the water-to-binder
ratio is 0.38, while for Mix 2 it is 0.34 and for Mix 2B it is 0.35. An
increased water-to-binder ratio may have inuenced the average
compressive strength.
3.2. Flexural behaviour
The ductility and deformation capacity of ECC can be investigated either directly by a uni-axial tensile test or indirectly by a

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Fig. 1. Layered repair system setup under restrained shrinkage.

Table 3
Mix design for layered system by weight (in kg/m3).
Repair mortars

Concrete substrate

Type

Control

Bio-based

CemI 42.5N
FA
LP
LWA
Water
SP
PVA
w/b*

483
580
387

420
21
22
0.4

449
538
260
123
390
20
22
0.4

CemIII 42.5 LH HS
Sand
Gravel

340
836
1017

Water
SP

169
0.7

w/b*

0.5

Water-to-binder ratio.

Fig. 2. Average compressive strength.

exural test. Qian and Li [28] reported that the deection capacity
is linearly correlated with tensile strain capacity for truly strainhardening materials. Hence, the deection capacity can be used
for quality control of SHCC type material due to the simplicity of
four point bending test compared to uni-axial tensile test.
Therefore the deection capacity is of major concern for the ECC
mortar repair system since its structural application will require
high deformation and energy dissipation capacity. The deection
capacity herein is dened as the deection that corresponds to
the maximal exural stress, i.e. exural strength in exural
stressdeection curve (Fig. 3).
The exural behaviour of the mortars is illustrated in Fig. 3 and
summarized in Tables 4 and 5. All mixtures show high deection
capacity which is typical for SHCC. The addition of bio-based agent
results in a slight decrease of the average exural strength measured at 56 days (Table 4) from 11.6 MPa for Mix 1 to 11.1 MPa
for Mix 1B, and from 12.7 MPa for Mix 2 to 10.4 MPa for Mix 2B.
The deection capacity, on the other hand, increased due to the
presence of particles with bio-based agent (Table 5).
Fig. 3 shows the representative exural stressdeection curve
of the reloading tests, along with a preloading test curve and a reference test to failure at 56 days for Mix 1B. Note that in this paper
for the reloading curve the permanent residual deection left from

the preloading stage is taken into account. Reloaded specimens for

both Mix 1 and Mix 1B have a higher strength than the reference
specimens. Different results were obtained with the reloaded specimens of Mix 2 that had lower exural strength than the reference
samples. The results for Mix 2B reloaded specimens were about the
same as the reference samples. The results are slightly better for
mixes with bio-based agent, but in order to know if this is due to
the healing process it is necessary to study the crack healing by
means of microscopic observation and oxygen consumption measurements in order to understand the healing mechanisms with
and without the bio-based agents.
No signicant difference was observed regarding the exural
strength, deection capacity, number of cracks or decrease of stiffness for samples pre-loaded at an early age (7 days) compared to
samples pre-loaded at 28 days. Stiffness is dened as the secant
of the initial rising branch of the stressdeection curve. For the
data in this study the rst point was chosen at 1.5 MPa and the second point at 3.5 MPa. The decrease of stiffness during the reloading, to about half of the initial stiffness for all mixes and
preloading ages, show no inuence from the age or preloading.
Apparently if the cracking behaviour is important for the self-healing capacity of the material it is the cracking behaviour in the rst
seven days that makes the differences as the samples pre-loaded
after either 7 or 28 days do not show a signicant difference.
By pre-loading the samples of mixes 1 and 1B the deection
capacity decreases, as can be seen in Table 5. A special situation
arises with reference samples of Mix 2 tested at 56 days. The
deection capacity for all 4 samples tested was considerably lower
than the pre-loaded samples, and fewer cracks developed prior to
failure. This was not the expected behaviour for a SHCC material.
Since the four tested samples were initially 1 specimen, it is possible that for instance this single specimen was not casted properly.
A second sample was then cut and tested at age 90 days. These
specimens have a similar exural strength than the specimens
tested at 56 days, and a higher deection capacity along with a
higher number of cracks. The deection capacity of reloaded samples is then compared to the reference at 90 days in Table 5. The
reloaded specimens have a higher deection capacity. For mix 2B

Fig. 3. Typical exural stressdeection curves for M1B.

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Table 4
Average exural stress at pre-load level and exural strength after healing (standard deviations are indicated between brackets).
Pre-load level
7 days
Mix 1

Pre-loaded

After healing
28 days

9.11 [0.58]
10.6 [0.67]

Reference
Pre-loaded

Mix 1B

7.74 [0.21]
9.13 [0.60]

Reference
Pre-loaded

Mix 2

10.21 [0.40]
11.47 [0.42]

Reference
Reference 90d
Preloaded

Mix 2B

7.69 [0.52]
10.21 [0.64]

Reference

56 days

Heal/Ref.

11.63
11.68
11.59
11.85
11.28
11.12
11.73
11.12
12.74
12.61
10.44
10.19
10.39

1.00
1.01

[2.30]
[0.82]
[1.28]
[0.21]
[1.19]
[1.73]
[1.47]
[0.71]
[1.50]
[0.99]
[0.11]
[1.49]
[0.20]

1.07
1.01
0.92
0.87

1.01
0.98

Table 5
Mid-span deection at pre-load level and after healing (standard deviations are
indicated between brackets).

Mix 1

Pre-loaded

Pre-load level

After healing

7 days

56 days

Heal/Ref.

4.66
5.69
7.30
6.61
5.42
7.66
4.81
4.87
2.73
3.71
5.64
7.28
5.67

0.64
0.78

28 days

2.41 [0.07]
2.61 [0.14]

Mix 1B

Reference
Pre-loaded

2.35 [0.02]
2.69 [0.09]

Mix 2

Reference
Pre-loaded

2.43 [0.07]
2.44 [0.05]

Mix 2B

Reference
Reference 90d
Preloaded

2.28 [0.11]
2.35 [0.16]

Reference

[1.28]
[1.03]
[1.58]
[0.81]
[0.70]
[1.88]
[1.46]
[1.25]
[0.15]
[1.01]
[0.21]
[1.07]
[0.45]

0.86
0.71
1.30
1.31

0.99
1.28

Fig. 4. Healed specimen after reloading.

the deection capacity is fully recovered by the reloaded

specimens.

3.3. Oxygen consumption and optical observations

Due to the exural testing method multiple cracks with different widths were generated. To investigate the surface crack closure
the surface cracks were evaluated with a stereomicroscope. Fig. 4
shows typical cracking pattern in a sample of Mix 1B subjected
to 2.5 mm deection, healing and reloading. The appearance of
crack closing would be mostly due to the precipitation of calcium
carbonate on the surface of the specimens. Whereas in control
specimens most of the cracks under reloading pass through the
pre-existing cracks, in specimens with bio-based agent some
cracks deviate from the healed pre-existing crack and form new
cracks. This shows the potential of the bio-based agent to improve
the mechanical properties of healed specimens. To conrm this potential oxygen concentration prole measurements were done towards the surface of submerged Mix 1 and Mix 1B samples.
Fig. 5 shows the prole measurement for a control Mix 1 and a
Mix 1B sample after 18 h submerged in solution with pH 11. The O2
proles of control samples show an almost homogeneous and constant O2 concentration in the 2.5-mm water column above the
sample surface. In contrast, the O2 concentration of the bio-based
sample progressively decreases in the diffuse boundary layer
(0.6-mm water layer overlaying the sample surface). This oxygen
consumption measured above the bio-based agent is due to bacterial metabolic activity. This means that 3 months after casting bacteria impregnated in LWA are viable and can, in the presence of

water, metabolize the organic food source and consume oxygen.

Similar behaviour was observed with bacteria immobilized in expanded clays [20].
More detailed information of the crack healing can be obtained
by observing preloaded specimens in the Environmental Scanning
Electron Microscope (ESEM). The selected samples were not reloaded. As can be seen in Fig. 6 the LWA particles have a very sound
bonding with the cement matrix. The crack breaks the particle and
this will expose the bacteria impregnated in the LWA aggregate to
the water present in the crack in the same way as the sample used

Fig. 5. Measured oxygen concentration microproles towards surfaces of submerged control and bio-based samples.

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for oxygen proles measurements. Therefore oxygen consumption

and precipitation of minerals is expected in the cracks in specimens with bio-based agents.
Figs. 7 and 8 show the microstructure and the chemical composition of healing products found in different cracks in M1B samples.
Surface crack sealing took place in some cracks (Fig. 7). It is clear
from the chemical composition that this healing product formed
in the crack mouth is based on calcium but is not only composed
of calcium carbonate (CaCO3). Small silica and alumina concentrations are present too. Other cracks that were only partially sealed
or whose mouths remained opened showed healing products with
different morphology inside the internal crack (Fig. 8). Loose forms
of healing products (Fig. 8a and b) could be seen in cracks with
crack width about 30 lm, and EDS results revealed a high concentration of calcium, silica and alumina. Other cracks were partially
lled with needle-like healing product (Fig. 8c) formed with high
concentrations of sulphur, silica and alumina (crack width
35 lm). Deeper into the crack, where the crack widths are 20 lm
or less, a dense healing product is found (Fig. 8d) with similar composition to the loose particles seen in Fig. 8a and b. To investigate
the variability of the healing minerals the concentrations were
determined at different randomly selected spots of multiple specimens for which the semi-quantitative results are demonstrated in
Figs. 9 and 10. Based on the Si, Ca and S content the healing products inside the cracks (similar to those shown in Fig. 8a, b and d)
can be considered a mixture between CH (calcium hydroxide)
and CSH (calcium silicate hydrate) (Fig. 9). But the high alumina
content of these products reveals a combination of AFt and Afm
phases with a sulphur deciency (Fig. 10). AFm phases are typied
by monosulfate [(Ca2Al(OH)6)2SO4 6H2O] and AFt phases by ettingrite [(Ca3Al(OH)6)2(SO4)3 26H2O] [29]. The S deciency of the AFm
phases

can be explained if the sulphate was replaced by carbonate
or hydroxide (OH) [29]. On the other hand, the needleCO2
3
like minerals seen in Fig. 8c shows strong characteristics of AFt
phases and ettingrite combined with CSH (Figs. 9 and 10). The results also reveal that the healing minerals in the mouth of the
cracks are a mixture of CaCO3 and CH (Figs. 9 and 10).
In M1 control samples only cracks with a crack width below
20 lm exhibited crack healing (Fig. 11). The chemical composition
of healing products inside these cracks is similar to the chemical
composition of healing products in samples with bio-based healing
agent as can be seen in Figs. 9 and 10.
3.4. Interface bonding strength
The pullout tests were carried out on ve samples of Mix 1B
casted on top of a concrete substrate. The average bonding strength

Fig. 6. LWA inside mortar samples M1B.

Fig. 7. Photomicrograph and EDS analysis of supercial healing product (crack

mouth) in M1B sample.

at 35 days is 2.89 N/mm2. The failure occurred in all cases in the

mortar. This bonding strength fullled the bonding requirement
for repair material of concrete structures Class R3 (P1.5 MPa)
according to the standards NEN 1504-3 [27]. These tests were done
according to EN 12636 [26]. The samples were cured under water
prior to testing.
3.5. Free drying shrinkage
The free drying shrinkage measurements for all mortars up to
120 days are shown in Fig. 12. Each value in this gure represents
the average of three specimens. The shrinkage strain for Mix 2 is
lower than for Mix 1. This is due to the higher cement content
(Table 2) as cement paste is the source of shrinkage [30]. Fine
aggregates like sand and ller materials like limestone powder
are inert and therefore help to control the deformations due to
shrinkage depending on their particle sizes. Mix 2 has sand as ller,
which has a larger particle size than the limestone powder in
Mix 1.
The mixes with LWA with bio-based agent have a higher drying
shrinkage. It is possible that in Mixes 1 and 2 the absence of LWA
lead to the densication of the cement matrix, which prevents
internal moisture evaporation [31]. Nonetheless, Fig. 12 shows that
the shrinkage strain of mixes Mix 1 and Mix 2 is less than 0.25%
after 120 days and below 0.35% for Mix 1B and Mix 2B. This is
one order of magnitude lower than its tensile strain capacity
(36.5%) estimated for these ECC materials based on its mid-span
deection capacity [28,32]. This implies that any potential
restrained shrinkage will lead to a strain-hardening stage of the
ECC material. During this stage because of the materials ductility,
stress caused by shrinkage deformation will form multiple
micro-cracks that do not progressively increase but maintain a

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Fig. 8. Photomicrographs and EDS analyses of internal healing products in M1B sample. (a) Crack 2 internal. (b) Crack 3 internal. (c) Crack 4 internal. (d) Crack 5 internal.

certain maximum crack width. There will be no localized fracture

failure. Once micro-cracked, the effective modulus of the ECC
repair materials will be substantially reduced, as seen in the reduced slope of the bending stressdeection curve in the deection-hardening stage (Fig. 3), thus further suppressing tensile
stress build-up in the repair material due to continued restrained
shrinkage [5].

3.6. Restrained shrinkage

The average values of interfacial delamination height at both
ends as a function of time are shown in Fig. 13. The control repair
mortar completed most of its interface delamination at early ages
within 14 days it reached 90% of the delamination registered at
200 days. The bio-based repair mortar continues to delaminate

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Fig. 9. Chemical analysis of healing products by EDS. Atomic ratio plot of S/Ca vs Si/
Ca. ETT = ettingrite.

Fig. 10. Atomic ratio plot of healing products; the limits of composition used to
characterized the phases are shown.

Fig. 13. Specimen-end delamination heights at different ages.

up to 60 days. At 28 days the repair registered 90% of the total

delamination and at 60 days 97%. As can be seen, the control mortar repair exhibited interface delamination height 4.5 times higher
than the bio-based mortar. The bio-based mortar has a signicantly greater resistance to delamination due to shrinkage than
the control mortar, despite its higher free drying shrinkage values.
It is possible that the bio-based mortar has a higher creep/stress
relaxation, therefore drying shrinkage does not result in stress
and thus not in delamination. Mortar M1B, with a slightly higher
bending capacity than control mortar M1 (Table 5), is able to release tensile and shear stresses in the interface so that delamination is lower. This higher capacity may be due to a change in the
brematrix interface and a possible coating effect of inert particles, LWA, on the bre surface. The LWA with the bio-based agent
may be introducing initial aws that assist in triggering multiple
micro-cracks during tensioning of the composites [33].

4. Conclusions

Fig. 11. Photomicrograph of internal healing products in M1 sample.

The main objective of this study was to clarify whether biobased self-healing via bacteria-mediated calcium carbonate production will result in improved mechanical properties and bonding
strength of a concrete-compatible bre-reinforced repair system.
Results show that a SHCC type material with bio-based agent full
the requirements for a structural repair material in terms of compressive and bonding strength. When applied as a repair material
the mortar with bio-based agent shows reduced delamination from
the concrete substrate compared to mortar without the bio-based
agent. Furthermore, after cracking and healing the mixtures with
bio-based healing agent show a slightly better recovery of both
exural strength and deection capacity from control mixtures
without bio-based healing agent. Although oxygen measurements
indicate that bacteria were metabolically active in the bio-based
specimens, observed amounts of calcium carbonate precipitate
did not appear to substantially differ from control specimens.
The reason for the apparent uncoupling between metabolic activity
and lack of enhanced calcium carbonate precipitation can possibly
be attributed to limited amounts of feed applied and this remains
to be claried in pending studies.

Acknowledgements

Fig. 12. Free shrinkage strain of repair mortars at different ages.

Arjan Thijssen and Ger Nagtegaal are acknowledged for help

with ESEM analysis and laboratory support, Virginie Wiktor and
Jure Zlopasa for valuable discussion on the subject. The authors
would like to acknowledge the nancial support from STW, Project
11342 Bio-based repair and performance improvements of aged
concrete structures, Bio-Retrot. The authors would like to

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M.G. Sierra-Beltran et al. / Construction and Building Materials xxx (2014) xxxxxx

express appreciation for materials supplied and laboratory tests

done by Cugla B.V. and BAS Research & Technology.

References
[1] FHWA-RD-01-156. Corrosion cost and preventive strategies in the United
States. Report by CC Technologies Laboratories, Inc. to Federal Highway
Administration (FHWA), Ofce of Infrastructure Research and Development.
2001.
[2] Emberson NK, Mays GC. Signicance of property, mismatch in the patch repair
of structural concrete, Part 1: properties of repair systems. Mag Concr Res
1990;42(152):14760.
[3] Emmons PH. Concrete repair and maintenance illustrated. West
Conshohocken, PA: ASTM International; 1994. pp. 155164.
[4] NEN-EN 1504-9. Products and systems for the protection and repair of
concrete structures Part 9. 2008.
[5] Li M. Multi-scale design for durable repair of concrete structures. PhD thesis.
USA: University of Michigan at Ann Arbor; 2009.
[6] Zhou J. Performance of engineered cementitious composites for concrete
repairs. PhD thesis. Netherlands: Delft University of Technology; 2011.
[7] Sierra-Beltran MG, Jonkers HM. Bio-based mortar for concrete repair. In: Forde
MC, editors. Proceedings of 14th int. conf. structural faults and repair, 2012.
[8] Li VC. From micromechanics to structural engineering the design of
cementitious composites for civil engineering applications. J Struct Mech
Earthquake Eng 1993;10(2):3748.
[9] Li VC. Advances in ECC research. ACI Special publication on concrete: Material
Science to Applications. SP206-23; 2002. p. 373400.
[10] Li VC, Yang EH. Self healing in concrete materials. In: Self healing materials: an
alternative approach to 20 centuries of materials sciences; 2007. p. 16193.
[11] de Rooij M, Van Tittelboom K, De Belie N, Schlangen E, editors. Self-healing
phenomena in cement-based materials. Springer; 2013. p. 117.
[12] Qian S, Zhou J, de Rooij MR, Schlangen E, Ye G, van Breugel K. Self-healing
behavior of strain hardening cementitious composites incorporating local
waste materials. Cem Concr Compos 2009;31(9):61321.
[13] Yang Y, Yang EH, Li VC. Autogenous healing of engineered cementitious
composites at early age. Cem Concr Res 2011;41(2):17683.
[14] Buffenbarger J, Hondo F, Nmai C, Tomita R. Shrinkage-reducing admixtures for
concrete. ACI Concr Int 1998;20(4):317.
[15] Yang EH, Yang Y, Li VC. Use of high volumes of y ash to improve ECC
mechanical
properties
and
material
greenness.
ACI
Mater
J
2007;104(6):30311.
[16] Neville AM. Properties of concrete. 4th ed. Harlow: Longman; 1995.

[17] Sahmaran M, Lachemi M, Hossain KMA, Ranade R, Li VC. Inuence of aggregate

type and size on ductility and mechanical properties of engineered
cementitious composites. ACI Mater J 2009;106(3):30816.
[18] de Koker D, van Zijl GPAG. Extrusion of engineered cement-based composite
material. In: Proceedings of 6th Rilem Symposium on Fiber-Reinforced
Concretes (FRC)-BEFIB; 2004.
[19] Jonkers HM. Bacteria-based self-healing concrete. Heron Self-healing Mater
2011;56(1/2):112.
[20] Wiktor V, Jonkers HM. Quantication of crack-healing in novel bacteria-based
self-healing concrete. Cem Concr Compos 2011;33:76370.
[21] Vaysburd AM, Brown CD, Bissonnette B, Emmons PH. Realcrete versus
Labcrete searching for tests that give reliable results. Concr Int
2004;26(2):904.
[22] Li VC, Wu C, Wang S, Ogawa A, Saito T. Interface tailoring for strain-hardening
polyvinyl alcohol-engineered cementitious composite (PVA-ECC). ACI Mater J
2002;99(5):46372.
[23] Spanka R, Fritze D. Bacillus cohnii sp. nov., a new, obligately alkaliphilic, ovalspore-forming bacillus species with ornithine and aspartic acid instead of
diaminopimelic acid in the cell wall. Int J Syst Bacteriol 1993;43(1):1506.
[24] Jonkers HM, Thijssen A, Muyzer G, Copuroglu O, Schlangen E. Application of
bacteria as self-healing agent for the development of sustainable concrete.
Ecol Eng 2010;36:2305.
[25] Schlegel HG. General Microbiology. 7th ed. Cambridge: University Press; 1993.
[26] NEN-EN 12636. Products and systems for the protection and repair of concrete
structures test methods determination of the adhesion concrete to
concrete; 1999.
[27] NEN-EN 1504-3. Products and systems for the protection and repair of
concrete structures Part 3; 2005.
[28] Qian S, Li VC. Simplied inverse method for determining the tensile strain
capacity of strain hardening cementitious composites. J Adv Concr Technol
2007;5(2):23546.
[29] Lachowski EE, Mohan K, Taylor HFW, Moore AE. Analytical electron
microscopy of cement pastes: II, pastes of portland cements and clinkers. J
Am Ceram Soc 1980;63(7,8):44752.
[30] Brandt AM. Cement-based composites. Routledge Taylor and Francis Group;
2009.
[31] Ozbay E, Karahan O, Lachemi M, Hossain KMA, Duran Atis C. Investigation of
properties of engineered cementitious composites incorporating high volumes
of y ash and metakaolin. ACI Mater J 2012;109(5):56571.
[32] Zhou J, Qian S, Sierra Beltran MGM, Ye G, van Breugel K, Li VC. Development of
engineered cementitious composites with limestone powder and blast furnace
slag. Mater Struct 2010;43(6):80314.
[33] Lawler JS, Zampini D, Shah SP. Permeability of cracked hybrid ber-reinforced
mortar under load. ACI Mater J 2002;99(4):37985.

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