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 Smart Materials and Structures

Smart Mater. Struct. 29 (2020) 105035 (8pp) https://doi.org/10.1088/1361-665X/aba53b

A new type capsule-based healing agent

for concrete and its protective function
of spores
Xuan Zhang1,2,3 and Chunxiang Qian1,2,3
1
School of Materials Science and Engineering, Southeast University, Nanjing 211189, People’s Republic
of China;
2
Research Center of Green Building & Construction Materials, Southeast University, Nanjing 211189,
People’s Republic of China
3
Jiangsu Key Laboratory for Construction Materials, Southeast University, Nanjing 211189, People’s
Republic of China

E-mail: [email protected] and [email protected]

Received 28 April 2020, revised 8 June 2020

Accepted for publication 13 July 2020
Published 17 September 2020

Abstract
To prolong the survival time of bacteria in the concrete and improve the self-healing ability of
the late-age cracks, a new type of core–shell structure capsule-based healing agents were
prepared for loading spores. The performance and protective ability of the capsules were tested.
The self-healing concrete was prepared by mixing the substitution of fine aggregates with an
equal amount of capsule-based healing agents. And the slump, compressive strength and
repair-ability of concrete were carried out. The results showed that the capsule could provide
long-term protection for loaded spores under the erosion of simulated pore solution of concrete
for at least 203 d. Furthermore, the concentration and the cumulative amount of calcium ions of
the crack zone solution were significantly increased. The slump and compressive strength of
concrete do not change significantly with a low dose of capsule-based healing agents. However,
the fluidity of fresh concrete will be greatly improved with the increase of dosage. Compared
with adding spore powder directly, the self-healing ability of late-age crack (the repair-ability to
crack area and the water impermeability of crack) will be improved obviously by adding
capsules. Therefore, using capsule loading to protect spores is a potential solution for the
long-term maintenance of the self-healing ability of concrete.
Keywords: capsule-based healing agent, self-healing concrete, bacteria, spores, protection

(Some figures may appear in colour only in the online journal)

1. Introduction [6], and microbial self-healing [7]. Among them, bacteria-

based healing has shown promising results towards full-scale
Cracks in concrete are one of the key factors that determine the application and commercialization phase of self-healing con-
strength and durability of concrete-built structures [1]. How- crete [8]. However, the bacteria-based self-healing technology
ever, the occurrence of cracks in concrete is inevitable [2]. still grapples with many challenges, the biggest one of which
A potential solution to this crucial problem is the application is how to ensure the long-term survival of bacteria in concrete
of self-healing technology [3]. Self-healing concrete has the [9]. Therefore, researchers screened the bacteria that were res-
ability to repair its small cracks autonomously [4] and has istant to alkaline surroundings and converted the obtained bac-
recently attracted interest in civil engineering [1]. To achieve teria into spores [10], further increasing their tolerance to harsh
this goal, various self-healing methods have been developed environments. Even so, 99.8% of spores lose viability on the
such as shape memory alloys [5], electrochemical deposition 22nd day [11]. The high alkalinity and narrow living space

1361-665X/20/105035+8$33.00 1 © 2020 IOP Publishing Ltd Printed in the UK

Smart Mater. Struct. 29 (2020) 105035 X Zhang and C Qian

inside the concrete make it difficult for the spores to keep alive Table 1. The chemical composition of sulfur-aluminate cement (%).
for a long time [12]. Therefore, the direct addition of spores to MgO Al2 O3 SiO2 SO3 Cl- K2 O CaO Fe2 O3
concrete is often used to repair the early-age cracks. To pro-
long the survival time of spores, many kinds of carriers that 1.71 33.38 8.18 7.90 0.11 0.22 43.10 1.96
can protect spores have been developed, such as light-weight
aggregate [13], microcapsule [14], and compressed powder
[8]. Lightweight aggregate-based bacteria concrete has yiel-
ded to improve crack sealing efficiency, but the decrease in
compressive strength might limit its application [8]. Microcap-
sules are generally prepared by organic substances. However,
the compatibility with the concrete matrix and the increase
of long-term shrinkage is not conducive to its promotion in
practical projects [15]. The concrete mixed with the powder-
based healing agent may result in a significant reduction of
its flexural strength and compressive strength [10]. It can
be seen that selecting a reasonable carrier is necessary and Figure 1. Capsule-based healing agents.
important for self-healing concrete [16]. Encapsulation-based
self-healing technology is an effective method for healing
the crack-deteriorated cementitious materials [17]. There are
many challenges for this technology. For capsule materials,
it should have suitable viscosity, fitted elastic modules, strain
capacity, and bonding strength [18]. In addition to the capsule
materials and healing agents, the crack propagation behavior
of encapsulation-based self-healing concrete, kinetics of heal-
ing agent in discrete crack surfaces, and other comprehensive
factors are also worth studying [19]. Among these issues, the
most important one is that the selected carrier will not have a
negative impact on the performances of concrete [12], and it
also has a good protective function of loaded spores.
Figure 2. Structure of the capsule-based healing agent.
The purpose of this study was to prepare a new kind of spore
carrier to prolong the survival time of spores to ensure its self-
healing ability of later-age crack. Thus, a novel kind of heal- is approximately 3–4 mm in diameter, the diameter of the inner
ing agent with a core–shell structure was prepared. The single- layer is approximately 2 mm, and the thickness of the outer
particle strength, crushing value and protection ability of the layer is about 1 mm.
capsule-based healing agent were tested. Also, the ability to
change the calcium ion condition of the solution in the crack
zone was determined. The self-healing concrete was prepared 2.2. Other materials
by replacing some fine aggregate with capsule-based healing
agents, the properties of fresh concrete, harden concrete and Ordinary Portland cement with a strength grade of P·II42.5
crack self-healing ability was tested. Capsule-based healing was used. The fine aggregate used was river sand with a fine-
agents are promising to be used for practical engineering. ness modulus of 2.6. The coarse aggregate used was granite
gravel with a maximum particle size of 25 mm. The mixing
water and the curing water used in the test are tap water. The
2. Materials superplasticizer was a polycarboxylic acid high-performance
water-reducer agent, and the maximum rate of water reduction
2.1. Microbial healing agent was in the range of 30%–35%.
The capsule-based healing agents were bulk prepared as
shown in figure 1. The core–shell structure of the healing agent
2.3. Preparation for microbial self-healing concrete
is shown in figure 2. To avoid the influence of nutrients and
spores powder on the properties of concrete, healing agent was Four groups of self-healing concrete mixed with different
loaded in the inner layer of the capsule. The healing compon- capsule-based healing agent dosages were prepared for the
ents in the inner of section of the capsules was mainly com- slump of fresh concrete testing. For group CH5, CH10 and
posed of spore powder and calcium nitrate. The outer layer of CH15, capsule-based healing agents replace 5%, 10% and
the capsule is a kind of low alkalinity cementitious material, 15% ratio of fine aggregates, respectively. Reference concrete
which can provide a suitable physical and chemical environ- added with 0% healing agents. The mix proportions of con-
ment for the loaded spores. The low basic cementitious mater- crete are shown in table 2.
ial used in this paper is sulfur-aluminate cement. Its chemical CH representing capsules. The number behind the letter
composition and proportion are shown in table 1. The capsule represents the addition percentage of capsules.

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Smart Mater. Struct. 29 (2020) 105035 X Zhang and C Qian

Table 2. Mix proportion of concrete mixed with capsule-based healing agents.

No. Cement (kg/m3 ) Water (kg/m3 ) Sand (kg/m3 ) Stone (kg/m3 ) Water reducer (kg/m3 ) Dosage of capsules (kg/m3 )

CH0 412 165 590 1254 2.06 0

CH5 412 165 560.5 1254 2.06 29.5
CH10 412 165 531 1254 2.06 59
CH15 412 165 501.5 1254 2.06 88.5

Three contrast tests were designed to compare the self- 3.2. Methods for the properties of concrete
healing ability of concrete mixed with different types of heal-
3.2.1. General properties of concrete. The slump of the
ing agents. For the reference concrete group CH0, no healing
fresh concrete was tested following China Standard GB50080-
agents were added. Capsule-based healing agents were added
2016 ‘Standard for test method of performance on ordinary
to group CH5. For group S, the powder healing agents without
fresh concrete’. The experiments of compressive strength were
capsule were added. The number of added spores must keep
performed with a 10 cm × 10 cm × 10 cm sample. Then
consistent in CH5 and S to ensure that the samples were com-
the specimens were cured for 28 d in the standard conditions
parable. The mix proportions of self-healing concrete mixed
where the temperature was 20 ± 2 ◦ C and the relative humidity
with different types of healing agents are shown in table 3.
was not less than 95%. The compressive strength of hardened
concrete was tested following China Standard GB/T 50 081–
3. Methods 2019 ‘Standard for the test methods of concrete physical and
mechanical properties’.
3.1. Test methods for the properties of capsule-based
healing agents 3.2.2. Methods for the cracking area repair rate. Exper-
3.1.1. Strength properties of capsule-based healing agent. iments were conducted with φ10 cm × 10 cm cylindrical
The instrument used to measure the particle strength of capsule sample. The curing environments were: the temperature
is intelligent particle strength tester (KY-20, Jiangsu Keyuan 20 ± 2 ◦ C, RH ≥ 95%. After curing for 28 d, the specimens
Electronic Instrument Co. Ltd.). The range of it is 0–200 N, were cracked. Then the cracked specimens were immersed in
and the instrument sensitivity is 0.1 N. The crushing value of water for 28 d at a curing temperature of 20 ± 2 ◦ C.
capsules was tested according to China Standard JGJ52-2006 The images of the cracks before and after repair were col-
‘Standard for technical requirements and test method of sand lected with a high-definition camera. The collected images
and crushed stone (or gravel) for ordinary concrete’. were imported into the Image J software for binary image pro-
cessing, and then the number of pixels occupied by the crack
area before and after the repair was read. The ratio of the num-
3.1.2. Protective function of capsule. To investigate the ber of pixels reduced by the repair to the total number of pixels
protection function of the capsule on bacteria, the healing of the pre-repair crack area is considered as the area repair rate
agents were soaked in the simulated pore solution of con- (R). The larger the R is, the better the self-healing performance
crete. OD600 refers to the absorption of the bacterial solution at is. The calculation formula of cracking area repair ratio R is
the wavelength of 600 nm. The absorption value was propor- as follows [20]:
tional to the number of bacteria in the solution. The growth of
A0 − A1
bacteria was commonly monitored by OD600 .The maximum R= × 100% (1)
OD600 value within 36 h was used as the index to measure A0
the ability of spore recovery, and the growth curve of spores
loaded by the healing agent was measured every 7 d. A0 representing the number of pixels occupied by the pre-
repair crack area, A1 representing the number of pixels occu-
pied by the post-repair crack area.
3.1.3. Concentration of Ca2+ in the solution in crack zone.
To measure the change capacity of the capsule-based healing 3.2.3. Methods for the properties of water impermeability.
agent for the ion condition of the crack zone solution, the con- The specimens prepared methods are the same as the crack-
crete sample was prepared added with capsules loading cal- ing area repair ratio test. Based on the amount of seepage in a
cium source. After the sample hardens, a crack with a width of given time, the seepage coefficient (K) is calculated according
about 0.5 mm is prepared along the Middle Line of the sample. to Duthie’s law.
Next, the water was injected into the crack zone. At every 24 h
intervals, the solution of the crack zone was extracted for the Q×L
K= (2)
measurement of calcium ion concentration. After extraction, A × ∆h
the water was injected into the crack zone immediately for
the next time measurement. The concentration of calcium ions K is the water permeability coefficient with unit m/s. Q is
was quantified with Calcium ion meter (MP523-03). water flow with unit m3 /s. L is the length of the specimen with

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Smart Mater. Struct. 29 (2020) 105035 X Zhang and C Qian

Table 3. Mix proportion of concrete mixed with two kinds of healing agents.

No. Cement (kg/m3 ) Water (kg/m3 ) Sand (kg/m3 ) Stone (kg/m3 ) Water reducer (kg/m3 ) Dosage of healing agents (kg/m3 )

H0 412 165 590 1254 2.06 0

CH5 412 165 560.5 1254 2.06 29.5
S 412 165 580.17 1254 2.06 9.83
H representing healing agent. CH representing capsule-based healing agent. S representing spore powder healing agent. The number behind the letter
represents the addition percentage of healing agent.

unit m. A is the permeability area of the specimen with units 135

m2 . ∆h is the head difference with unit m. 120
The complexity of the problem is due to the difficulty of
105

Particle strengthen/N
ensuring the width of the crack consistency of samples, and
the relatively large difference between the measured water per- 90
meability is induced. Therefore, the water permeability coef- 75
ficient of the crack is transformed into a relative permeabil-
60
ity coefficient (k) to enable effective comparison between dif-
ferent samples. The permeability coefficient of the pre-repair 45
and post-repair crack is marked as K0 and K1, respectively. 30
The relative permeability coefficient k is the ratio of K1 to K0.
The smaller the k is, the better the self-healing ability of crack 0 10 20 30 40 50 60 70 80 90 100
is. The calculation formula of relative permeability coefficient Particle number
was as follows (3):
Figure 3. Single-particle crush strength distribution plots.

K1
k= (3) 4.2. The protective function of capsule for spore
K0
The capsule should provide a suitable chemical space to avoid
the effects of high alkaline cement hydration products besides
k is the relative permeability coefficient. K 1 is the permeabil- the physical protective ability [21]. The resurrection ability of
ity coefficient of pre-repair crack with unit m/s. K 0 is the per- encapsulated and non-encapsulated spore changes as a func-
meability coefficient of post-repair crack with unit m/s. tion of time is shown in figure 4. The maximum OD600 of
spores that can be reached within 36 h was 1.82 before soaked
in simulation solution. For unprotected spores, the resurrection
3.3. Identification of the crack repair products ability largely disappeared after soaked in the simulation solu-
The repair products in crack zone were tested using XRD tech- tion for 28 d. For the spores under the protection of the capsule,
niques. the resurrection ability is still at a good level after soaked in
the simulation solution for 203d. The maximum OD600 value
within 36 h was still about 1.8, and there was no significant
4. Results and discussion decrease compared with the untreated spores. The outer layer
materials offer adequate protection for loaded spores against
4.1. Strength of the capsule-based healing agent the high alkaline damage of the simulation solution.

The capsule-based healing agent should have certain phys-

4.3. The ability to change the conditions of the crack zone
ical strength: prevent the extrusion and shearing function on
solution
the particles during the mixing process [12] on one side and
provide a certain physical space for spores against the extrac- Some calcium resource was also added in the preparation pro-
tion function of cement hydrate on the other side [21]. For cess of healing agents. Therefore, the calcium resource release
accurate single pellet crush strength, 100 particles were selec- together with spores when concrete cracking. The calcium
ted randomly and the results were shown in figure 3. The crush resource dissolves and changes the ion conditions of the solu-
strengths of the single-particle are shown between 60 N and tion during the germination period of spores. The concentra-
85 N and the average strength is 76 N. The lower and the higher tion of calcium ions has an important effect on the mineraliz-
strength is most likely due to the uneven wall thickness of ation rate. As can be seen from the data in figure 5, the max-
the single-particle during the preparation process. The crush- imum concentration of calcium ions increased to 7000 mg l−1
ing value of capsule-based healing agents is 18%. Accord- due to the added calcium resources. The concentration of cal-
ing to the Chinese National Standard ‘Sand for construction’ cium ions is only 821 mg l−1 in the crack zone solution of the
(GB/T14684), the particles can be used for the preparation of specimen without healing agents. The total mass of calcium
C60 concrete. carbonate that can be mineralized in the crack zone depends on

4
Smart Mater. Struct. 29 (2020) 105035 X Zhang and C Qian

2.0
1.8
1.6
1.4
1.2
OD600

1.0
0.8
0.6
0.4 Non-encapsulated spores
Encapsulated spores
0.2
0 21 42 63 84 105 126 147 168 189 210
Time (d)

Figure 4. Comparison of the resurrection ability of encapsulated

Figure 7. Slump of concrete mixture mixed with capsule-based
and non-encapsulated spores.
healing agent.

Figure 5. Ca2+ concentration of crack zone solution.

Figure 8. Compressive strengthen of concrete mixed with
capsule-based healing agent.

solution in the crack zone is 3.098 mmol on day 5. However,

the accumulative amount of calcium ions dissolution was only
0.481 mmol in the control group. Thus, calcium sources con-
tinue to dissolve, providing a large number of available cal-
cium ions for microbial mineralization. It can be concluded
that it is necessary to encapsulate some calcium sources in cap-
sules.

4.4. Influence of the capsule-based healing agent on

concrete mixture slump

For the capsule-based healing agent (figure 7), the slump of

concrete mixed with a low mixture ratio (5%) of capsules has
not been significantly changed. While the dosage of capsules
Figure 6. Accumulative amount of Ca2+ dissolution. was increased to 10% and 15%, the slump of the concrete mix-
ture increased by 43% and 81% respectively. This is because
the capsule is spherical and has a smooth appearance, it needs
the accumulated soluble calcium ions, which directly affected less slurry to be wrapped than complex-shaped aggregate, and
the extent of the crack that can be repaired. As shown in fig- has low flow friction resistance, which greatly improves the
ure 6, the cumulative amount of calcium ions dissolves in the fluidity of the mixture. On the other hand, the diameters of

5
Smart Mater. Struct. 29 (2020) 105035 X Zhang and C Qian

Figure 9. Comparison of three kind concrete repair effect.

Therefore, less cement paste is used to wrap the surface of fine

aggregate, more cement paste is available to lubricate aggreg-
ate, and finally, the fluidity of concrete is increased [22].

4.5. Influence of the capsule-based healing agent on

concrete compressive strengthen

It can be seen from figure 8 that the early and late compressive
strength of the concrete specimen has no significant changes
under the condition of low dosage (5%). However, the early
compressive strength of concrete is negatively affected when
the content of capsules increases, but the late strength is still
similar to the comparison group. Therefore, the compressive
strength development course of concrete may be changed with
a large amount of capsule-based healing agent addition.
Figure 10. Comparison of the relative permeability coefficient
between three kinds concrete. 4.6. Cracking area repair rate of concrete

The repair results for samples of three kinds of concrete are

shown in figure 9. Though there was no healing agent mixed
into ordinary concrete, it still shows some repair effect, and the
cracking area repair rate is 19% after 28 d. When mixing with
spore powder, the cracking area repair rate rose to 51% at 28 d.
The addition of a capsule-based healing agent led to the crack-
ing area repair rate continued to increase up to 95% at 28 d.
The repair effect significantly improved after adding a heal-
ing agent. For the cracks with 28 d cracking ages, the cracking
area repair rate adding with the capsule-based healing agent
is 44% higher than the one with spore powder. The reason
was apparent from the data in figure 4, it is difficult to main-
tain long-term activity for spores with the alkaline damage of
concrete simulated solution. The spores rapidly undergo apop-
tosis, which causes a drastic decrease of resurrected microor-
Figure 11. XRD spectrum of mineralization products obtained in ganisms. Finally, the repair efficacy gradually deterioration as
crack mouth. the cracking date was delayed. To ensure a good level of the
repair effect, it is necessary to take some measures to protect
the spores. It should be explained that although the spore can-
capsule-based healing agents are 3–4 mm. The addition of cap- not survive for more than 28 d in an alkaline solution, the crack
sules causes the increase of fineness modulus, which will lead still shows some repair effect with 28 d cracking ages. The
to a decrease of the specific surface area of fine aggregate. reason is that the condition of the simulated pore solution may

6
Smart Mater. Struct. 29 (2020) 105035 X Zhang and C Qian

be harsher than the actual inter conditions of concrete, it can 203 d under the erosion of the concrete pore simulated solu-
be considered as an accelerated erosion test, and the concrete tion. Moreover, the concentration and cumulative amount
has some self-repairing ability. of calcium ions of the solution in the crack zone were sig-
nificantly improved by the capsule-based healing agent.
• The slump of fresh concrete will not change mixed with a
4.7. The relative permeability coefficient of concrete small amount of capsule-based healing agent. The fluidity
As can be seen from figure 10, for the weak self-healing of fresh concrete will increase greatly over the increase of
effect of the cement-based material, the relative permeability the addition amount of spherical capsules. No obvious neg-
coefficient of the concrete specimen without healing agents ative effect on the compressive strength was observed when
decreases gradually with the increase of curing age, but the the dosage of capsules below 15%.
decreasing extent is small (25%). For the concrete mixed with • Compared with the concrete mixed with spore powder,
spore powder, the self-healing ability of crack was improved the repair effect of the crack of the concrete mixed with
compared with the ordinary concrete and the relative per- capsule-based healing is better. The protection of capsule
meability coefficient was decreased by 56%. This was due to for spores makes it show an advantage in repairing the late
the unsatisfactory crack repair effect caused by spores apop- cracking age crack of concrete.
tosis. For the concrete adding with the capsule-based healing • The main mineral induced by microorganisms is calcite
agent, the relative permeability coefficient of the crack is fur- type calcium carbonate, which is also the main repair
ther reduced up to 82%. This was consistent with the observa- products of crack.
tion shown in figure 9. The cracks of concrete mixed with the
capsule-based healing agents were blocked by more mineral- Acknowledge
ized products resulting in a significant reduction of its water
permeability. Once again, the protective effect of the capsule This work was financially supported by the National Natural
on spores was further verified. Science Foundation of China (51 738 003).

4.8. Identification of the repair products in crack zone ORCID iD

As indicated before, the crack of concrete mixed with the Xuan Zhang  https://orcid.org/0000-0002-3313-9514
healing agent will be repaired by mineralized products, which
increases cracking area repair rate and decreases the relative
permeability coefficient. To specify the role of the healing References
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