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Keywords: To address the issue of concrete structures being prone to crack failure, this study employs the response surface
Response surface methodology method (RSM) to evaluate the impact of adding zeolites and crystalline admixture (CA) on the self-healing
Self-healing concrete performance of mortar. Initially, zeolite amount, CA amount, and the water-to-binder ratio (W/B) are consid
Zeolites
ered as response factors, using ultrasonic pulse velocity (UPV), electrical resistivity, and the self-healing rate as
Crystalline admixtures
Water-to-binder ratio
the response target values. UPV and electrical resistivity are used to monitor self-healing process, while self-
healing rate quantifies healing of cracks. Subsequently, through designing experiments with RSM, a regression
model is established, achieving multi-objective optimization of the mortar self-healing rate, and experimental
validation is carried out for the optimized combinations. Finally, the mechanical properties of mortar specimens
are studied, and scanning electron microscopy (SEM) and X-ray diffraction (XRD) are used to analyze the
microstructure and crystal phase composition of the crack healing fillers. The quadratic polynomial model has a
high degree of fit, and the error between the measured and predicted values is less than 10%, indicating the
reliability of RSM in determining the optimal mix parameters for mortar self-healing. The SEM and XRD results
further confirm that the moisture released by zeolites promotes the activation reaction of CA, generating a larger
amount and more densely structured calcium silicate hydrate (C-S-H) gel. Moreover, the research results show
that although incorporation zeolites diminishes mortar specimens’ strength, incorporation zeolites promotes the
generation of C-S-H gel within the cracks, attributable to activation reaction of CA, ultimately promoting crack
healing and improving the strength of the mortar. Based on optimization analysis, the optimal amounts of ze
olites, CA, and W/B were determined to be 20%, 4%, and 0.45, respectively.
* Corresponding author.
E-mail address: zhangks@nefu.edu.cn (G.-Z. Zhang).
https://doi.org/10.1016/j.conbuildmat.2023.134015
Received 28 June 2023; Received in revised form 27 October 2023; Accepted 28 October 2023
Available online 3 November 2023
0950-0618/© 2023 Published by Elsevier Ltd.
H.-F. Li et al. Construction and Building Materials 409 (2023) 134015
practical feasibility of above healing methods, the broad adoption is the occurrence of autogenous shrinkage in concrete. For instance, the
currently restricted by high costs and intricate processing procedures. As study by Zhang et al. [25] shows that the internal curing property of
a result, the pursuit of cost-effective and user-friendly concrete crack zeolite contributes significantly to the reduction of the matrix’s autog
repair techniques remains a pressing need in contemporary research. enous shrinkage, thereby augmenting the material’s relative humidity.
Crystalline admixtures (CA), as a type of self-healing additive for Kazemian et al. [26] conducted an in-depth investigation on the role of
concrete cracks, have garnered substantial interest within the sphere of zeolite as an internal curing agent in enhancing the hydration process of
civil engineering [13]. The reactive chemicals present in CA undergo ultra-high performance concrete (UHPC). The heat generated during
reactions with hydration products of cement, forming microcrystals hydration was assessed by observing the temperature evolution of UHPC
such as ettringite and calcium silicate hydrate (C-S-H) gel. These mi over time. The results indicate that after 28 and 56 days of curing, in the
crocrystals possess the ability to infiltrate pores and crevices, thereby mixtures incorporated with zeolite, the hydration level demonstrated an
enhancing compactness and durability, and contributing to the extended elevation of 21 % to 26 %, respectively, than that in mixtures without
lifespan of concrete structures. In addition, research has found that CA is zeolite. This suggests that the zeolite’s internal curing mechanism can
a hydrophilic additive [14], which can perform its own activation re substantially augment the degree of hydration in cement particles.
action more effectively under the influence of water. Therefore, to Additionally, Zheng et al. [16] used zeolite as an internal curing agent in
augment the self-healing capacity and the mechanical properties of cementitious materials and assessed its impact on the internal curing
concrete integrated with CA, it is necessary to provide more moisture in performance of cementitious materials. Above study found that the in
the cement mortar matrix. This action is anticipated to stimulate the ternal curing effect manifested by zeolite effectively curtails the satu
activation reaction of CA. The internal curing technique seems to ach ration duration associated with the humidity of the cement paste, with
ieve the purpose of enhancing the self-healing ability of CA in the con the internal relative humidity increasing from 87.8 % to 92.0 % at 28
crete matrix. Internal curing technology is considered an effective days. The aforementioned studies suggest that the porous nature of
method for replenishing the internal moisture of the matrix [15], serving zeolite offers excellent internal curing effects, which seems to contribute
as a “reservoir” for storing moisture and timely providing ample mois significantly to the activation reaction of CA.
ture for the mortar matrix. This can be achieved by incorporating pre- In multi-factor research on concrete self-healing, determining the
soaked curing materials into the cement matrix, effectively addressing optimal content of each factor to obtain excellent self-healing perfor
the issue of insufficient moisture. In past studies, more researchers have mance is crucial. To achieve this goal, numerous scholars have under
been focusing on and conducting studies on the effects of various in taken in-depth investigations to determine the optimal mix ratio of
ternal curing materials on reduce for autogenous shrinkage in cement- different factors through experimental means. Techniques such as arti
based materials, including zeolites [16], porous ceramics [17], super ficial neural networks (ANN) [27], Genetic Algorithms [28], and
absorbent polymers (SAP) [18], and expanded perlite aggregates [19]. response surface methodology (RSM) [29] are used to determine the
Researchers have found that internal curing materials promote self- optimal mix ratio that can achieve the best healing capacity after being
healing effect of CA on mortar and simultaneously enhance self- affected by various factors. Among them, RSM, owing to its capacity to
healing performance of the mortar. For instance, Byoungsun et al. formulate precise mathematical models for the attainment of peak per
[20] investigated the interactions between CA and SAP as internal formance and the development of the most cost-effectively designed
curing materials and explored their synergistic effect on the self-healing mixtures in accordance with performance metrics, it has found extensive
performance of mortar cracks. Based on water flow tests and crack application in cement-based materials [13,30]. In addition, RSM can not
healing tests, it was found that the interaction between CA and SAP only reveal the significance of variables but also analyze the interactions
significantly improved self-healing capabilities. Upon reaching a crack between various factors. In recent years, this method has been widely
width of 0.256 mm, the water flow decreased by 100 %. However, the applied in concrete research, formulation of precise and suitable models
cracks in the control group specimens were still not fully healed after 56 for the design of mortar mix proportions. For example, Hou et al. [31]
days. Wang et al. [21] used porous ceramics as internal curing agents for used RSM to construct an optimization model, considering the rela
CA to carry out quantitative analyses on the width and area of cracks. tionship between variables (water-cement ratio, magnesium-
Observations post a 28-day period of aquatic immersion indicated that phosphorus ratio, and sand content) and responses (setting time and
pre-cracked specimens containing porous ceramics and CA demon compressive strength), thereby improving the performance of mortar in
strated better surface crack healing effects. Feng et al. [15] discussed the rapid repair applications. Li et al. [32] used RSM to examine how
impact of encapsulating CA in lightweight aggregate (LWA) on self- various constituents impact the rheological characteristics of self-
healing ability of concrete cracks. The experimental outcomes eluci compacting mortar, optimized the mortar mix ratio through regression
dated that encapsulating CA in lightweight aggregate can enhance the models, and achieved improvements in workability and compressive
repair efficiency of concrete cracks. Upon a curing duration of 7 days in a strength. He et al. [33] used RSM to analyze the effect of concrete micro-
water environment, the specimens with added CA showed a crack crack time and extent on mechanical properties and crack healing,
healing rate of 42.44 %. In contrast, the specimens without added CA providing a quantitative description of the changes during the healing
showed relatively poor healing effects, with a healing rate of 23.28 %. process and establishing a micro-crack extent control model.
Unfortunately, SAP as an internal curing agent can absorb hundreds of While existing studies have explored the impact of CA and zeolites on
times its own weight in water, the large pores formed by the release of the durability and crack healing performance of concrete, research on
water significantly reduce the strength of the material [22]. On the other the optimal dosages and healing mechanisms remains relatively limited.
hand, the complexity of the encapsulated lightweight aggregate pro Moreover, few studies have applied RSM to the process of self-healing
duction process poses a problem, porous ceramics and expanded perlite modification and optimization in mortar with internally mixed CA.
aggregate as internal curing materials have lower inherent strength, Therefore, to investigate the impact of zeolites, CA, and W/B on the self-
which leads to a reduction in mortar strength, decrease in mixing uni healing of mortar cracks. This study proposes using the RSM method,
formity, damage to durability, and a decrease in bonding strength, etc. adopting ultrasonic pulse velocity (UPV), electrical resistivity, and crack
[19,23]. Therefore, to fully exploit the advantages of internal curing microscopy observation as the three experimental means to discuss the
materials in enhancing self-healing performance of mortar cracks by CA, impact of zeolites, CA, and W/B on healing performance. By varying the
it is a need to further explore new internal curing materials to solve these dosages of zeolites, CA, and W/B, the study aims to optimize the self-
problems. healing effect of mortar cracks, thereby obtaining the optimal mixture
As a porous volcanic aluminosilicate mineral, zeolite exhibits design scheme. Based on RSM analysis, the innovative points of this
excellent internal curing properties, capable of absorbing 33 % of its study are as follows: Firstly, this study constructs a polynomial regres
own mass in water [24]. This feature is used by researchers to alleviate sion model through response surface optimization experiments, treating
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H.-F. Li et al. Construction and Building Materials 409 (2023) 134015
zeolites amount, CA amount, and W/B as independent variables, to trical resistivity, and self-healing rate as responses. Previous research
ascertain the impact of above variables on the self-healing performance. indicates that as zeolite is a porous material, addition of zeolite more
Secondly, RSM is applied to construct a precise prediction model, used than 20 % reduces the compressive strength of the specimens [37,38]. In
to determine the optimal combination of zeolites amount, CA amount, studies about CA as a self-healing agent being added to cement matrix, it
and W/B ratio, and experimental verification is conducted on the showed that the proportion of CA is controlled at 2–4 %, it not only
optimal combination determined by the RSM model to prove the accu improves the mechanical properties of the specimens but also enhances
racy and reliability of the model prediction. The optimization results can the healing effects of cracks [13]. The purpose of this study is to
provide more targeted optimization schemes for practical engineering investigate the impact of internal curing water released by zeolite on the
applications. Finally, through microscopic analysis by scanning electron healing effects of CA in the cement matrix. Numerous studies have
microscope (SEM) and X-ray diffraction (XRD), the mechanism of self- demonstrated that for ordinary concrete with a W/B ratio of above 0.4,
healing action of internally mixed CA mortar cracks by water pro CA can provide good healing capabilities in a cement matrix [39].
vided by zeolites as internal curing agents has been revealed. Therefore, in this study, in order to ensure that CA provides excellent
healing in the cement matrix consider using 0.4 and 0.5 as the target W/
2. Materials and methodology B ratio for this study. In summary, in the experimental process, zeolites
replaced 10 %, 15 %, and 20 % of the standard sand (by weight), CA
2.1. Materials replaced 2 %, 3 %, and 4 % of the cement (by weight), and the values of
W/B were 0.4, 0.45, and 0.5. The value of α was 1.682 to ensure the
The cement used in this study was ordinary Portland cement (OPC), accuracy of the model, and the values and coding levels of actual factors
purchased from Anhui Conch Cement Co., Ltd. Standard manufactured can be seen in Table 2. It included a total of 14 groups of factorial ex
sand was used. The sand used in this paper was manufactured according periments and 6 groups of central point tests to estimate the experi
to the ISO 679:2009 standard [34]. The density and water absorption of mental error.
the sand is 2580 kg/m3 and 0.57 %, respectively. The permeable crys
N = 2k + 2k + c (1)
talline admixtures (CA) were a gray powder, purchased from Zhong De
New Asia Building Materials Co., Ltd. Previous research findings indi Where k is the number of experimental factors, 2k is the factor point, 2k
cate that water absorption rate of natural zeolites was typically around is the axial point, and c is the number of experiments at the center point
26 % [35], which may limit the internal curing effect of zeolites. [40].
Therefore, to improve the pore structure of zeolites and thus enhance In the CCD, experimental variables include 8 factorial points, 6 axial
their internal curing effect, calcined zeolites are used as internal curing points, and 6 central points, as shown in Fig. 2. Correspondingly, a total
materials. Calcination is performed in a muffle furnace at 500 ℃ for 30 of 20 experiments (N) were conducted for three factors according to Eq.
min. The diameter of the zeolites ranges from 1 to 2 mm. The chemical (1). During the experiment, tests were conducted in alignment with the
compositions of Portland cement, zeolite, and CA are shown in Table 1. predetermined checkpoints in the experimental schema. Subsequently,
The polycarboxylate superplasticizer (SP) was added to make flow the data gathered from these test points were analyzed using response
ability of mortar between 200 and 220 mm. surface methodology. Response surface analysis primarily uses
nonlinear fitting methods to derive the optimum value through fitting
2.2. Application of response surface methodology (RSM) equations. For the relationship between interaction factors, a quadratic
polynomial can be used for fitting, as shown in Eq. (2). The fitting
2.2.1. Principle of RSM equation not only facilitates a more in-depth understanding of the
RSM is a predictive and evaluative tool based on mathematical experimental results but also contributes to the optimization of the
principles and statistical methods, used to analyze the interaction be experimental scheme. The experimental design of this study is shown in
tween factors and responses. By analyzing the experimental results, RSM Table 3.
establishes regression models using quantitative values, thereby ∑k ∑k ∑∑
analyzing, and optimizing factors affecting mortar performance [31,36]. y = β0 + β xi +
i=1 i
β x2 +
i=1 ii i
βij xi xj + ε (2)
This study uses the Central Composite Design (CCD) for experimental
i<j
design and uses Design Expert-13 software to establish the model, which where y represents predicted response value, xi represents the inde
includes 2k factorial points, 2k axial points, and c central points (k is the pendent values of each variable (i.e., CA, zeolites, and W/B), ε repre
number of factors, c is the number of central experiments) [32]. As sents the experimental error, β0 represents the value of the intercept, βi
shown in Fig. 1, the RSM analysis method usually includes three steps: 1) are the first-order (linear) model coefficients, βij represents the inter
Pose the problem, 2) Establish and fit the model, 3) Optimize and solve
action model coefficients, and βii represents the second-order
the model under constraints.
(quadratic) model coefficients [12].
Table 1
Chemical composition of the material. wt. (%).
Material Chemical composition (mass %)
CaO SiO2 Al2O3 Fe2O3 SO3 MgO Others Loss on ignition
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H.-F. Li et al. Construction and Building Materials 409 (2023) 134015
Fig. 1. Modeling process based on CCD. Notes: Ele. R represents electrical resistivity; CCD stands for Central Composite Design; ANOVA stands for Analysis
of Variance.
Fig. 2. Schematic of CCD. Notes: A represents the content of zeolites; B represents the content of CA; C represents W/B.
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H.-F. Li et al. Construction and Building Materials 409 (2023) 134015
Table 3 AASHTO T 358 and ASTM C597-22 [43] respectively. For each group of
Experimental Design. mixtures, three specimens are selected for analysis, with the ensuing
Test Specimen Zeolites (%) CA (%) W/B results being represented as the mean value.
A B C
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H.-F. Li et al. Construction and Building Materials 409 (2023) 134015
Table 4
Concrete mixture designs.
Mixture code Water (g) Cement Light aggregate
(g)
Sand Zeolites CA W/B Superplasticizer (g)
(g) (g) (g)
Fig. 4. Images of the introduced cracks: (a) experimental setup and (b) schematic diagram.
Fig. 5. Binarization result images: (a) The specimen pre-crack at 0 d, and (b) the specimen healed at 28 d.
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H.-F. Li et al. Construction and Building Materials 409 (2023) 134015
XRD tester (scanning angle: 10-70◦ , scanning speed: 6◦ /min). The self- factors are valid (F-value > 14), with a P-value < 0.0001, indicating that
healing filler was scraped out from the cracks with a scraper. The the models are extremely significant. The lack-of-fit data (P-value >
samples were soaked in anhydrous ethanol for 24 h to stop cement hy 0.05) indicate that the chosen model does not have a significant effect on
dration. Then samples have been dried in an oven at 40 ◦ C for 48 h. For the error. Referencing Table 6, it is clear that the three variables (zeolite
XRD tests, samples ground to 40–60 mesh with a sieve, and stored in a amount, CA amount and W/B ratio) significantly influence the UPV
sealed bag. value response, electrical resistivity, and self-healing rate. Moreover, the
interactions also have certain effects on the response results. The order
2.4.5. Scanning electron microscope of factors’ impact on 7 d and 28 d UPV value is respectively: A > C > A2
To observe the micro-morphology of the healed fillers at the crack > B > B2 > BC > AC > C2 > AB and B > B2 > A2 > A > C > AB > C2 > BC
site, SEM observation of the filler at the crack site of the specimen was > AC. The order of factors’ impact on 7 d and 28 d electrical resistivity is
conducted after 28 days of healing age. The self-healing filler was respectively: A > C > B2 > A2 > B > BC > C2 > AC > AB and B > A > C >
scraped out from the crack with a scraper. Then dried in an oven at 40 ◦ C C2 > B2 > AB > A2 > AC > BC. The order of factors’ impact on 7 d and 28
for 48 h. The SEM observation was carried out using TM250FEG d self-healing rate is respectively: A > B > AB > C > BC > B2 > A2 > AC
(Quanta, USA) and the results were collected under an accelerating > C2 and B > A > C > AB > B2 > A2 > AC > BC > C2. Among them, the
voltage of 10/20 kV. impact of CA on the UPV value, electrical resistivity, and self-healing
rate of the specimens is most significant. This is due to the addition of
3. Results and discussion CA, which reacts with the hydration products of cement to produce more
C-S-H gel, resulting in better healing effects for the mortar specimens.
3.1. Response surface methodology This ultimately increases the self-healing rate. Moreover, the study by
Oliveira et al. [13] also found that the activation reaction of CA makes
3.1.1. Results of the response surface model experiment the internal matrix of cement more compact, playing an excellent role in
The results of the RSM experiment are shown in Table 5. The pore filling. In summary, CA has the most significant impact on UPV
experimental data indicate that both of zeolites and CA amounts have value, electrical resistivity, and self-healing rate. In Table 6, there is no
significant impacts on the UPV value, electrical resistivity, and self- significant difference in P-value between zeolites (A) and CA (B). For
healing rate of mortar specimens. Otherwise, the W/B ratio also being mortars blended with zeolites, the addition of zeolites increases
a factor have been affected on above test results. It is worth noting that porosity, which leads to changes in porosity within the mortar matrix.
previous studies reported that low and high W/B ratios can adversely Consequently, there is a significant impact on the UPV value and elec
affect the self-healing effect of mortar specimens [45]. trical resistivity. Simultaneously, the addition of zeolite releases parts of
free water that reacts with unhydrated cement particles in the matrix,
3.1.2. Variance analysis resulting in ultimately having a significant effect on the healing rate. For
Analysis of Variance (ANOVA) is commonly used to test the signifi mortars mixed with CA, the addition of CA improves the compactness of
cance of the impact of different factors on experimental results, mainly the mortar matrix. Eventually, CA has a significant impact on UPV value
by examining the P-value to reflect whether the impact of each factor on and electrical resistivity. The activation reaction of CA within the
the response is significant. In order to determine the significant effects of cement matrix also enhances the crack healing effect. Ultimately, the
zeolite amount, CA amount, and W/B on the durability and crack experimental results confirmed that the P-values of zeolite (A) and CA
healing rate of mortar, the least squares method is used to fit the (B) on UPV value, electrical resistivity and self-healing rate were less
response surface model and perform variance analysis on the experi than 0.05, indicating no significant difference in P-value. For UPV value
mental results. The results of the variance analysis are shown in Table 6. and electrical resistivity, it should be highlighted that the W/B plays a
In variance analysis, the significance of factors is tested using the size pivotal role in modulating the hydration level within the matrix. The
of the P-value. When P < 0.05, it indicates that the factor is significant; if higher the W/B, the lower UPV value and electrical resistivity of the
P < 0.01, it indicates that the factor is extremely significant [46]. As specimen [47].
shown in Table 6, the models chosen for variance analysis of all three
3.1.3. Fitting accuracy analysis
This study examined the accuracy of the fitting model (as shown in
Table 5 Table 7) and found that the correlation coefficient (R2) of the quadratic
Experimental Results. model was close to 1, indicating a strong correlation between experi
Mixture code UPV value Electrical resistivity Self-healing rate mental values and predicted values, which confirms precision and
(m/s) (KΩ.cm) (%) dependability of the quadratic model [48]. In addition, the adjusted
7-day 28-day 7-day 28-day 7-day 28-day correlation coefficient (Adj-R2) is close to Pred-R2, with a value less than
ZC01 3810 4319 59.16 151.13 75.01 77.63 0.2. Additionally, each model manifests C.V. below 10 %, with the Adeq
ZC02 3669 4453 51.37 153.27 78.26 81.21 Precision exceeding 4, all of which indicate that the model has high
ZC03 3858 4487 60.87 154.46 82.59 85.25 fitting accuracy and reliability. Therefore, the constructed quadratic
ZC04 3723 4512 55.74 155.12 90.23 93.01
ZC05 3714 4236 55.79 149.19 78.73 80.11
regression model in the current investigation bears statistical signifi
ZC06 3601 4358 51.42 152.23 79.91 86.13 cance, demonstrating precise predictability and an exemplary level of
ZC07 3691 4387 56.94 152.89 81.38 87.87 fit, and can accurately predict the response values of UPV, electrical
ZC08 3621 4412 50.14 153.56 89.99 96.91 resistivity, and self-healing rate. Table 8 shows the coefficients of the
ZC09 3849 4269 62.34 150.58 81.43 82.13
fitted equation derived from the application of the least squares method,
ZC10 3663 4464 52.07 154.94 86.35 91.11
ZC11 3689 4231 56.93 150.46 74.21 80.21 and fitting equations for 7 d and 28 d UPV value, 7 d and 28 d electrical
ZC12 3746 4468 58.45 153.87 88.93 94.16 resistivity, as well as 7 d and 28 d crack self-healing rate were estab
ZC13 3779 4585 55.71 155.94 80.77 84.53 lished according to Eq. (2), as shown in Eq. (4) to (9).
ZC14 3630 4447 50.19 153.21 84.53 86.75
ZC15 3648 4531 52.68 152.84 82.18 86.21 7− dayUPVvalue=3670.93− 56.51A+14.27B− 50.05C+6.12AB+11.62AC
ZC16 3678 4587 52.12 152.48 81.56 84.99 − 13.13BC+26.38A2 +12.77B2 +8.18C2
ZC17 3670 4503 52.98 152.78 82.47 84.21
(4)
ZC18 3661 4499 53.23 152.99 83.25 85.64
ZC19 3674 4565 54.13 152.65 82.94 84.99
ZC20 3691 4573 53.89 153.97 81.45 85.60
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H.-F. Li et al. Construction and Building Materials 409 (2023) 134015
Table 6
ANOVA results.
Source UPV value (m/s) Electrical resistivity Self-healing rate (%)
(KΩ⋅cm)
7-day 28-day 7-day 28-day 7-day 28-day
F-Value P-Value F-Value P-Value F-Value P-Value F-Value P-Value F-Value P-Value F-Value P-Value
Model 38.43 <0.0001 26.94 <0.0001 26.80 <0.0001 17.43 <0.0001 33.11 <0.0001 49.45 <0.0001
A-Zeolites 158.43 <0.0001 30.99 0.0002 136.71 <0.0001 44.65 <0.0001 54.43 <0.0001 127.73 <0.0001
B-CA 10.10 0.0099 53.20 <0.0001 5.78 0.0370 59.24 <0.0001 211.21 <0.0001 279.77 <0.0001
C-W/B 124.28 <0.0001 28.70 0.0003 39.15 <0.0001 26.68 0.0004 6.81 0.0260 23.11 0.0007
AB 1.09 0.3210 5.59 0.0397 0.0072 0.9340 5.90 0.0356 15.49 0.0028 6.56 0.0283
AC 3.93 0.0757 0.0190 0.8932 0.4178 0.5326 0.3294 0.5787 0.1341 0.7218 1.75 0.2151
BC 5.01 0.0492 0.0637 0.8058 5.26 0.0447 0.0090 0.9265 5.16 0.0465 0.0980 0.7606
A2 36.43 0.0001 61.98 <0.0001 23.72 0.0007 1.21 0.2972 2.13 0.1750 1.91 0.1966
B2 8.54 0.0152 74.19 <0.0001 30.81 0.0002 6.37 0.0302 2.17 0.1717 4.61 0.0574
C2 3.50 0.0909 1.85 0.2032 1.20 0.2988 10.54 0.0088 0.0115 0.9166 0.0036 0.9534
Residual
Lack of fit 1.54 0.3244 0.3566 0.8589 2.25 0.1976 1.25 0.4048 3.30 0.1082 3.10 0.1201
Pure error
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H.-F. Li et al. Construction and Building Materials 409 (2023) 134015
curing age progresses, CA significantly increased UPV value of speci With the increase of CA, the self-healing rate gradually increases.
mens healed for 28 days, while the effect of changes in W/B on UPV
value decreased. Fig. 8 (c) and (d) represent the electrical resistivity
change trajectories for the specimens healed for 7 days and 28 days. In 3.2. Response surface curvature analysis
the specimens healed for 7 days, zeolites play a significant role, while
the electrical resistivity of the specimens healed for 28 days increases The response surface provides a vivid illustration of the interplay
sharply with the increase of CA content, making CA the most significant between two factors and its subsequent impact on the response value. An
factor in enhancing electrical resistivity among the three factors. Fig. 8 augmented curvature of the response surface typically denotes a sub
(e) and (f) illustrate the crack healing effect change trajectories for stantial influence resulting from the interaction of UPV value, electrical
specimens subjected to healing durations of 7 and 28 days respectively. resistivity, and self-healing rate. Conversely, a less pronounced curva
Despite exhibiting similar trajectories, but the self-healing rate at 28 ture indicates a less significant interaction effect [49]. The following are
days is superior to that at 7 days. Moreover, the incorporation of CA the response surface results of zeolites amount, CA amount, and W/B on
exerts a profound influence on self-healing rate, promoting it positively. UPV value, electrical resistivity, and self-healing rate.
Table 8
the coefficients of the factors in the fitted equation.
7-day UPV value 28-day UPV value 7-day Electrical resistivity 28-day Electrical resistivity 7-day Self-healing rate 28-day Self-healing rate
Fig. 6. Comparison of experimental and predicted: (a) the 7 d UPV value; (b) the 28 d UPV value;(c) the 7 d electrical resistivity; (d) the 28 d electrical resistivity; (e)
the 7 d self-healing rate; (f) the 28 d self-healing rate.
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H.-F. Li et al. Construction and Building Materials 409 (2023) 134015
Fig. 7. Comparison of predicted and actual values for (a) UPV value; (b) electrical resistivity; and (c) self-healing rate.
3.2.1. The influence of various factors on UPV value This phenomenon reflects the significance of various factors, which is
The UPV response surface of the mortar specimens designed by RSM consistent with the variance analysis results. This might be because,
after 7 d and 28 d of healing is shown in Fig. 9. Fig. 9 (a) and (d) show during the 7 d healing age, with the increase in W/B, the degree of
the effects of the interaction between zeolites and CA on the UPV value hydration reaction of the cement weakens, the generated hydration
of the specimens after 7 d and 28 d of healing age, respectively. With a products correspondingly decrease, thereby reducing the internal den
fixed CA content, the UPV value decreases with increase in zeolites sity of the mortar matrix. This change eventually leads to a decrease in
content after 7 d of healing age, and the minimum wave speed reduces to the UPV value. Observing Fig. 9 (e), it can be found that with a fixed W/
3601 m/s. Statistical variance analysis reveals a substantial impact of B, as the content of zeolites increases, the UPV value of the specimen
zeolites on UPV value. When zeolites content is fixed, the UPV value after 28 d of healing age first increases and then tends to stabilize, with
changes little with the increase in CA content, and the response surface the maximum wave speed reaching 4587 m/s. When the zeolites content
tends to be flat. This suggests that zeolites are the main factors affecting is fixed, the UPV value remains essentially unchanged with the increase
the UPV value after 7 d of healing age, possibly due to the incorporation in W/B. This might be because during the 28 d healing age, due to the
of zeolite sand introducing extra pores, increasing the number of pores occurrence of cement hydration, the change in W/B has no significant
in the mortar matrix. This leads to a reduction in the UPV value. With the effect on the UPV value. As the curing age increases, zeolites gradually
increase in both of zeolites and CA content, the UPV value of the spec release absorbed water, which promotes the hydration reaction of
imen significantly increases after 28 d of healing age. According to the cement. These hydration products can heal cracks and fill the internal
variance analysis in Table 6, the effects of zeolites and CA on the UPV pores of the mortar, ultimately leading to an increase in the UPV value.
value are extremely significant, and the interaction between the two is The study by Pandieswari et al. [50] also confirmed that the water
also significant. This may be due to the release of absorbed water from released by zeolites promotes the hydration reaction of cement, and
zeolites with age, which promotes the generation of C-S-H gel from the these hydration products can fill the internal pores of the mortar matrix.
CA activation reaction, thereby promoting crack healing and improving Fig. 9 (c) and (f) show the effects of the interaction between CA and W/B
the UPV value. This phenomenon was confirmed in the SEM analysis. on the UPV value of the specimens after 7 d and 28 d of healing age,
Fig. 9 (b) and (e) show the effects of the interaction between zeolites and respectively. With a fixed CA content, the UPV value of the specimen
W/B on the UPV value after 7 d and 28 d, respectively. With a fixed W/B, decreases with the increase in W/B after 7 d of healing age, when W/B is
the UPV value of the specimen decreases (negatively correlated) with fixed, the change in CA has a smaller impact on the UPV value. When W/
the increase in zeolites content after 7 d of healing, and the surface is B is 0.4 and the CA content is 4 %, the UPV value of the specimen is the
steeper. When the zeolites content is fixed, the UPV value also decreases highest, with a maximum value of 3768 m/s. Observing Fig. 9 (f), it can
with the increase in W/B, and the trend of surface changes is similar. be observed that as the specimen heals for 28 days, the UPV value
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H.-F. Li et al. Construction and Building Materials 409 (2023) 134015
Fig. 8. Impact trajectory diagrams of different factors on the response: (a) the impact on the 7 d UPV value; (b) the impact on the 28 d UPV value; (c) the impact on
the 7 d electrical resistivity; (d) the impact on the 28 d electrical resistivity; (e) the impact on the 7 d self-healing rate; (f) the impact on the 28 d self-healing rate. (A:
zeolites; B: CA; C: W/B).
gradually increases with the increase of CA, and the curve is more promoting the filling of internal pores and crack healing. By observing
jittery, finally tending to be flat, while the influence of W/B on UPV Fig. 10 (d), it can be seen that at 28 d of healing age, the electrical re
value is not significant, which is consistent with the variance analysis sistivity of the specimens gradually increases with the increase in the
results. This could be attributed to the fact that at the healing age of 7 amount of zeolites and CA added, increasing by 1.94 % and 2.14 %
days, when W/B is lower, the amount of free water inside the mortar respectively. The variance analysis results also confirmed the significant
matrix is relatively small, the degree of cement hydration reaction in impact of zeolites and CA on electrical resistivity. This may be due to the
creases, and the number of hydration products increases, making the fact that the free water released by zeolites promotes the positive
inside of the mortar matrix denser, leading to an increase in UPV value. contribution of the hydration reaction of cement and the activation re
Conversely, under high W/B conditions, the UPV value has been action of CA to crack healing. Fig. 10 (b) and (e) show the effects of the
decreased. Observing Fig. 9 (f), it can be observed that at the healing age interaction between zeolites and W/B on the electrical resistivity of the
of 28 days, the activation reaction of CA contributes greatly to the crack specimens after 7 d and 28 d of healing age, respectively. After 7 d of
healing, ultimately leading to an increase in UPV value. healing age, the electrical resistivity decreases with the increase in ze
olites content. When the W/B is 0.5 and zeolite amount is 20 %, the
3.2.2. The influence of various factors on electrical resistivity electrical resistivity of the specimen is the lowest, with the minimum
The electrical resistivity response surfaces of the mortar specimens value being 50.14 KΩ⋅cm. This is mainly because the addition of zeolites
designed by RSM at 7 d and 28 d healing are shown in Fig. 10. Fig. 10 (a) increases the internal pores of the matrix. The electrical resistivity in
and (d) show the effects of the interaction between zeolites and CA on creases with the decrease of W/B, while the zeolite content remains
the electrical resistivity of the specimens after 7 d and 28 d of healing unchanged. When the zeolite amount is 20 % and W/B is 0.4, the elec
age, respectively. After 7 d of healing age, the electrical resistivity de trical resistivity of the specimens reaches the highest, with a peak value
creases with the increase in zeolites content and increases with the in of 155.12 KΩ⋅cm. This is mainly due to the fact that as previously
crease in CA content, with zeolites having a greater impact and a steeper described, the decrease in W/B increases the degree of hydration reac
surface. Variance analysis results show that the effects of zeolites and CA tion of the cement inside the matrix, the number of hydration products
on electrical resistivity are significant, mainly due to the introduction of increases, making the interior of the mortar matrix denser, ultimately
additional pores by adding zeolites and the activation reaction of CA leading to an increase in electrical resistivity. Observing Fig. 10 (e), after
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H.-F. Li et al. Construction and Building Materials 409 (2023) 134015
Fig. 9. Three-dimensional response surface plots of UPV values: (a) the impact of zeolites and CA for 7 d; (b) the impact of zeolites and W/B for 7 d; (c) the impact of
CA and W/B for 7 d; (d) the impact of zeolites and CA for 28 d; (e) the impact of zeolites and W/B for 28 d; (f) the impact of CA and W/B for 28 d.
Fig. 10. Three-dimensional response surface plots of electrical resistivity: (a) the impact of zeolites and CA for 7 d; (b) the impact of zeolites and W/B for 7 d; (c) the
impact of CA and W/B for 7 d; (d) the impact of zeolites and CA for 28 d; (e) the impact of zeolites and W/B for 28 d; (f) the impact of CA and W/B for 28 d.
28 d of healing age, the electrical resistivity of the specimens increases resistivity of the specimens after 7 d and 28 d of healing age, respec
with the increase in zeolites content, and the surface is steep. Compared tively. After 7 d of healing age, when W/B remains constant, the elec
with zeolites, W/B contributes less to electrical resistivity. This is trical resistivity increases with the increase in CA content. When the CA
attributed to the fact that during the 28 d healing age, the internal curing content remains constant, the electrical resistivity slightly increases with
action of zeolites promoted the activation reaction of CA to produce C-S- the increase in W/B, thus the magnitude is small and the response sur
H gel, improving the effect of crack healing. Fig. 10 (c) and (f) show the face tends to be flat. This is mainly because the partial moisture inside
effects of the interaction between CA and W/B on the electrical the mortar matrix can promote the activation reaction of CA in the early
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H.-F. Li et al. Construction and Building Materials 409 (2023) 134015
Fig. 11. Three-dimensional response surface plots of self-healing rate of cracks: (a) the impact of zeolites and CA for 7 d; (b) the impact of zeolites and W/B for 7 d;
(c) the impact of CA and W/B for 7 d; (d) the impact of zeolites and CA for 28 d; (e) the impact of zeolites and W/B for 28 d; (f) the impact of CA and W/B for 28 d.
stage, causing the cracks to have a certain healing effect. However, the
Table 9
hydration reaction of cement is not sufficient for healing effect at an
Best solutions for different response values.
early age. This is because the degree of cement hydration is relatively
weak in the early stage [51,52]. After 28 d of healing age, the electrical Dependent variable Limit Optimum Solution
Lower Limit Upper Limit Goal
resistivity approximately increases linearly with the increase in CA
content, the curve surface is steeper, and the maximum resistivity in 7-day UPV value 3601 3858 Maximum
28-day UPV value 4231 4587 Maximum
creases to 154.94 KΩ⋅cm. At the same time, W/B also increases its
7-day Electrical resistivity 50.14 62.34 Maximum
change in electrical resistivity. This observation can be primarily 28-day Electrical resistivity 149.19 155.94 Maximum
ascribed to the extension of the healing age, the activation reaction of 7-day self-healing rate 74.21 90.23 Maximum
CA continues to produce more C-S-H, making the interior of mortar 28-day self-healing rate 77.63 96.91 Maximum
matrix denser. In addition, as the curing age increases, the hydration
reaction of cement continues.
water, thereby promoting the hydration reaction of cement, but the
contribution to healing effect of cracks is relatively limited. Fig. 11 (c)
3.2.3. The influence of various factors on healing effect
and (f) respectively represent the influence of the interaction between
The response surface of the healing rates of mortar specimens at 7
CA and W/B on the healing rates at 7 d and 28 d. At 7 d of healing age,
d and 28 d is shown in Fig. 11. Fig. 11 (a) and (d) respectively represent
when W/B is kept constant, the increase in the amount of CA causes the
the influence of the interaction between zeolites and CA on the healing
healing rate to increase, with a maximum increase of 11.5 %. However,
rates of the specimens at 7 d and 28 d. When the amount of zeolites is
when the amount of CA is kept constant, although the healing rate
kept constant, the healing rate of the mortar gradually increases at 7 d as
gradually increases with the increase of W/B, the increase is relatively
the amount of CA increases. This observation elucidates that the amount
small. In the 28 d healing age. CA also promotes the healing of cracks,
of CA exerts a substantial impact on healing at 7 d. When the amount of
with a maximum healing rate increase of 10.3 %. In contrast, the in
CA is kept constant, the healing rate also increases with the increase in
fluence of W/B on the healing rate is limited. This is mainly because the
the amount of zeolites, but the change is relatively small. Compared with
size of W/B mainly contributes to the hydration reaction of cement,
the specimens at 7 d, the specimens at 28 d of healing showed better
while the hydration products generated by the hydration of cement have
overall healing effects. CA plays a leading role in facilitating crack
a limited effect, and the activation reaction of CA has a certain healing
remediation, the increase zeolites content makes CA’s influence on crack
effect on cracks throughout the maintenance age.
healing more significant, variance analysis elucidates that interaction
In conclusion, from the F and P values obtained from the variance
between zeolites and CA exerts a substantial influence on crack healing.
This is attributed to the increase in zeolites content providing sufficient
moisture for the activation reaction of CA, promoting the activation Table 10
reaction of CA, generating more C-S-H to fill cracks, making healing rate RSM verification results under optimal conditions.
reach 96.91 % at 28 d, a 6.9 % increase from the healing at 7 d. Fig. 11 Response value Predictive value Actual value Relative error
(b) and (e) respectively represent the influence of the interaction be
7-day UPV value 3857.724 3880.642 0.59 %
tween zeolites and W/B on the healing rates at 7 d and 28 d. From the 28-day UPV value 4589.370 4620.449 0.67 %
results, the results suggest that combination of zeolites and W/B has a 7-day Electrical resistivity 61.792 63.541 2.75 %
limited improvement on the healing rate, although W/B has some 28-day Electrical resistivity 155.300 153.216 1.34 %
changes, but its contribution to the healing effect of the cracks is not 7-day self-healing rate 90.232 91.225 1.09 %
28-day self-healing rate 96.315 97.009 0.72 %
significant. On the other hand, zeolites can release the absorbed free
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H.-F. Li et al. Construction and Building Materials 409 (2023) 134015
analysis, it is indicated that the impact of CA on the crack healing rate is 5. Mechanical and microscopic analysis
extremely significant (large F value, P < 0.0001), the impact of zeolites
is significant (P = 0.0111 < 0.05), while the impact of W/B is not sig In this study, the optimal mixture ratios of zeolites amount, CA
nificant (P = 0.0947 > 0.05) [53]. This is attributed to the increase in CA amount, and W/B were determined to be 20 %, 4 %, and 0.45, respec
content leading to an increase in the amount of active substances in the tively. To analyze the mechanical and micro-properties of the mortar,
mixture. The active substances in CA chemically react with the cement the following four types of specimens were selected. The specimens
hydration products to form C-S-H gel to fill cracks, thereby improving without zeolites and CA, specimens with 20 % zeolites, specimens with
the crack healing effect. Therefore, the order of impact on the crack 4 % CA, and specimens with 20 % zeolites and 4 % CA were labeled as
healing effect is CA > zeolites > W/B. In addition, the interaction be Control, 20Z, 4CA, and 20Z4CA, respectively. In addition, the value of
tween CA and zeolites considerably influences the efficacy of crack W/B chosen for all specimens was 0.45.
healing (P < 0.05). However, both the interaction of CA with W/B and
that of zeolites with W/B do not exert significant influence upon the
healing rate (P > 0.05), thereby substantiating the credibility of the 5.1. Mechanical properties
constructed predictive model.
The compressive strengths of Control, 20Z, 4CA, and 20Z4CA spec
4. Optimization results imens at 7 d and 28 d of curing are shown in Fig. 12. Compared to the
control group, the compressive strength of the 20Z specimen decreased
To determine the optimal mixture ratio of each substance under the by approximately 22 % and 8.3 % at 7 and 28 days, respectively. The
best response, this study uses Design-Expert 13 software, based on RSM observed phenomenon can be ascribed to introduction of additional
to optimize the six response values. According to the data in Table 9, it is porosity in mortar matrix by the addition of zeolites, thereby reducing
found that the UPV value and electrical resistivity at 7 d and 28 d are the compressive strength. However, at curing age of 28 d, the hydration
positively correlated with the pore structure and crack healing inside the reactions happening within cement matrix and free water released by
mortar matrix, which means that when these values are larger, the in zeolites promoting these reactions led to a denser internal structure of
ternal structure of the matrix is denser, and the healing effect is better. the mortar matrix, thus somewhat compensating for the decrease in
When analyzing the self-healing effects at 7 d and 28 d, the closer the compressive strength at 28 d. Compared to the control group, the
healing rate is to 100 %, the better the healing effect. Therefore, in the compressive strength of the 4CA specimens increased by approximately
optimization process, the maximum self-healing rate is used as the 9.6 % and 19.4 % at 7 and 28 days, respectively. This can be attributed
optimization condition. Through this method, the optimal mixing ratio to the reactive substances in CA reacting with the hydration products of
of each substance was determined to achieve the best healing effect. cement, generating dense C-S-H gels that fill the pores, thereby further
Considering the six response values comprehensively, the optimal enhancing the compressive strength. For the 20Z4CA specimens,
conditions based on RSM were obtained: the ratios of zeolites amount, compared with the 4CA specimens, the compressive strength decreased
CA amount, and W/B are 20 %, 4 %, and 0.45, respectively. Table 10 by 8.8 % at 7 d of curing age, but increased by 3.6 % at 28 d. Although at
shows the predicted values of UPV, electrical resistivity, and healing 7 d of curing age, the pore-filling effect brought about by the activation
rate. In order to verify the accuracy of the RSM prediction, specimens reaction of CA was not sufficient to counteract the decrease in strength
were prepared with the optimal mixing ratio to test the actual values of due to the additional porosity introduced by zeolites [37], at 28 d the
each response. The experimental results showed that the measured free water released by zeolites further promoted the activation reaction
values of UPV, electrical resistivity, and healing rate have a high degree of CA, generating more C-S-H gel, which led to an increase in
of agreement with the predicted values, with a relative error of less than compressive strength at 28 d. Fig. 12 (b) shows the flexural strength
10 % (see Table 10). This result confirms the accuracy and reliability of results at 7 d and 28 d of curing age, with the influences of various
the established prediction model. factors on the flexural strength presenting similar trends to those of the
compressive strength. The mechanisms observed in the compressive
strength results also apply to the flexural strength results. Compared
with the control group, the specimens with zeolites added showed re
ductions in flexural strength at both 7 d and 28 d of curing age.
Fig. 12. Strength at 7 d and 28 d of curing age: (a) Compressive strength and (b) Flexural strength.
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H.-F. Li et al. Construction and Building Materials 409 (2023) 134015
Fig. 13. SEM images of fillers in cracks of specimens: (a) Control specimen; (b) 20Z specimen; (c) 4CA specimen; (d) 20Z4CA specimen.
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H.-F. Li et al. Construction and Building Materials 409 (2023) 134015
Fig. 15. Schematic diagram of self-healing mechanism of mortar cracks: (a) Control specimen; (b) 20Z specimen; (c) 4CA specimen; (d) 20Z4CA specimen.
16
H.-F. Li et al. Construction and Building Materials 409 (2023) 134015
Zeolites improve the self-healing effect but lead to a decrease in me Constr. Build. Mater. 267 (2021), 120963, https://doi.org/10.1016/j.
conbuildmat.2020.120963.
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Hong-Feng Li: . Xiang Ma: Methodology, Data curation, Writing – Preparation and application, Constr. Build. Mater. 301 (2021), 124119, https://
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review & editing. Guang-Zhu Zhang: Conceptualization, Supervision,
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Declaration of Competing Interest Building Materials. 267 (2021) 120992, doi: 10.1016/j.conbuildmat.2020.120992.
[18] R. Rohollah, K. Agnieszka J., F.C.R. Almeida, Effect of superabsorbent polymers on
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