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Construction and Building Materials 201 (2019) 401–407

Contents lists available at ScienceDirect

Construction and Building Materials


journal homepage: www.elsevier.com/locate/conbuildmat

Effect of superabsorbent polymers on the drying and autogenous


shrinkage properties of self-leveling mortar
Jiayu Yang a, Laibao Liu a,⇑, Qilong Liao a, Jinming Wu b, Jianju Li c, Lihua Zhang a
a
State Key Laboratory of Environment-friendly Energy Materials, School of Material Science and Engineering, Southwest University of Science and Technology, Mianyang 621010,
PR China
b
Bejing BBMG Mortar Company Limited, Beijing, 102402, PR China
c
The Ninth Engineering General Troops of China Airfield Building, Chengdu 611430, PR China

h i g h l i g h t s

 Shrinkage characteristics of self-leveling have been proposed.


 Hydration heat and pore structure of self-leveling mortar were investigated.
 Drying and autogenous shrinkage are reduced by using superabsorbent polymer for internal curing.

a r t i c l e i n f o a b s t r a c t

Article history: This paper aims at putting forward the shrinkage control measures for evaluating the effect and mecha-
Received 25 August 2018 nism of shrinkage compensation of self-leveling mortar by analyzing the shrinkage characteristics of
Received in revised form 24 December 2018 cementitious self-leveling mortar (SLM). The drying shrinkage, autogenous shrinkage and mechanical
Accepted 28 December 2018
properties of the self-leveling mortar are analyzed by comparing it with the ordinary mortar. The differ-
Available online 3 January 2019
ence between the two kinds of matrix was explained by the result of hydration and pore structure. The
internal curing of self-leveling mortar was carried out by superabsorbent polymer. The variation of drying
Keywords:
shrinkage and autogenous shrinkage of self-leveling mortar were tested with the content at 0%wt, 0.2%
Shrinkage
Self-leveling mortar
wt, 0.4%wt and 0.6%wt. The pore structure and pore size distribution were also investigated. The
Internal curing experimental results show that the self-leveling mortar has larger the drying shrinkage and smaller
Superabsorbent polymers the autogenous shrinkage than those of ordinary mortar. The main reasons for this are the hydration
delay and the change of pore structure of self-leveling mortar caused by the addition of organic admix-
ture. The internal curing by using superabsorbent polymer has excellent effect on drying shrinkage and
autogenous shrinkage compensation which decrease by 10% and 10.2%, respectively, when the content is
0.4%wt.
Ó 2019 Elsevier Ltd. All rights reserved.

1. Introduction change) [3]. It is applicable to various fields, such as office build-


ings, schools, hospitals and so on. However, in order to obtain these
Cement-based self-leveling mortar (SLM) is made by mixing excellent performances, a large water-to-cement and cement-to-
cementitious materials, aggregates and mineral admixtures as well sand may be adopted in the design of material mix ratio, which
as chemical admixtures. It is a new kind of functional building also increases the risk of segregation, stratification and shrinkage
mortar [1]. SLM is widely used in China and world in the last dec- cracking of the mortar [4]. Meanwhile, the evaporation and fierce
ades owing to save of production cost and labor [2]. SLM becomes hydration reaction caused by large-scale construction of self-
popular due to its particular properties in fresh state (excellent flu- leveling mortar lead to significant drying shrinkage and chemical
idity, pumpability and homogeneousness) and hardened state shrinkage, respectively [5]. Drying shrinkage can be defined as
(rapid hardening, early strength, smooth surface and stable volume the volumetric change due to the drying of mortar [6]. The change
in volume of the mortar is related to the water loss of matrix. First,
the loss of free water during the drying process may lead to shrink-
⇑ Corresponding author at: School of Material Science and Engineering, age. As the drying process of mortar continues, the adsorbed water
Southwest University of Science and Technology, Mianyang 621010, PR China. maintained by hydrostatic tension in small capillaries is decreased
E-mail address: liulaibao@swust.edu.cn (L. Liu).

https://doi.org/10.1016/j.conbuildmat.2018.12.197
0950-0618/Ó 2019 Elsevier Ltd. All rights reserved.
402 J. Yang et al. / Construction and Building Materials 201 (2019) 401–407

significantly [7,8]. Then the loss of free water and adsorbed water hydration [26,27]. With the increase of curing age, the relative
produces tensile stresses, which compel mortar to shrink, thereby humidity of mortar decreases rapidly and the humidity gradient
causing cracks. Furthermore, in the drying condition, a high water- increases. At the same time, the free water in superabsorbent poly-
to-cement will increase drying shrinkage and deteriorate the per- mers is released continuously [28], which alleviates the rapid
formance of mortar [9,10]. As for autogenous shrinkage [11], at a decline of internal relative humidity. The free water released from
certain degree of hydration, when water and cement react in the superabsorbent polymers promotes the hydration of cement
hydration process, the water in the mixtures is gradually replaced [29]. A large number of hydration products will be filled in the
by the hydration products leading to a reduction in relative humid- pores left after the dissolution of the polymers and the pores left
ity in the microstructure. The decrease of relative humidity leads to after the evaporation of free water, and optimize the pore structure
an increase in the capillary pore pressure causing autogenous of the matrix [30–32]. The results show that the decrease of rela-
shrinkage deformations in the solid skeleton of the hydration tive humidity in cement-based materials will lead to a rapid
product. increase in the surface tension of water in the capillary, resulting
At present, established strategies for solving this contradiction in pressure stress on the capillary wall [33]. In fact, the deforma-
are as follows: first, using fast hard cementing systems, such as cal- tion of matrix occured when the relative humidity (35%) reduced,
cium aluminate cement (CAC) [1] and calcium sulfoaluminate and then gel water and interlayer water was lost, which is an
cement (CSC) [12], which not only reduce the risk of segregation important reason of cement stone shrinkage [34]. Although the
and stratification, also can high early mechanical properties be change of water content (relative humidity) is a key factor for
obtained and can construction efficiency be improved. In these shrinkage and cracking of cement-based materials, considering
cementitious systems, ettringite acts as the expansion source, the combined factors of material design, construction process
which compensate drying shrinkage and enhance the early and service environment, there are significant differences in form
strength of SLM [13]. In addition, organic admixtures such as cellu- of the shrinkage of Portland cement based self-leveling mortar.
lose ether, redispersible latex powder, water reducer and defoamer Therefore, the shrinkage characteristic of the self-leveling mortar
can be used to reduce the problems caused by plastic shrinkage is the key to study the shrinkage-cracking problem and put
[14–16]. The above methods have solved the most problems of forward appropriate solutions.
the self-leveling mortar in the construction stage and before hard- In spite of prior work related to the effect of SAP on the proper-
ening stage, but the long-term service performance of hardened ties of cementitious materials, the influence on SLM is unknown
mortar matrix (1d) has been seldom studied. Engineering prac- and has not been studied before. Since, this paper aims to clarity
tice shows that cracking, drying shrinkage and autogenous shrink- the shrinkage characteristic, mechanicals properties, hydration
age caused by rapid water loss and cement hydration are the main heat and pore structure characteristics of SLM by comparing with
forms of damage and failure of self-leveling mortar, which should ordinary mortar. In order to research the influence of the dosage
be studied and solved emphatically. of superabsorbent polymers on the drying shrinkage and autoge-
With the deepening of theoretical and applied basic research of nous shrinkage of the self-leveling mortar, the pore structure was
self-leveling mortar, more attention has been paid to the compre- measured after 28-days by the mercury intrusion method (MIP).
hensive application effect of hardened SLM by people, especially The mechanism of the action of superabsorbent polymers to the
the decline of service performance and service life caused by shrink- shrinkage compensation of the mortar is preliminarily analyzed.
age cracking [17]. The latest research shows that the drying shrink-
age of calcium aluminate cement based self-leveling mortar 2. Materials and methods
increases linearly with the prolongation of curing time. The drying
shrinkage value of sample with a-hemihydrate and anhydrite and 2.1. Materials
dihydrate gypsum is more than 0.1%. It indicates that adding gyp-
In the study, PO 42.5 Portland cement was obtained from market for all the
sum into calcium aluminate cement based self-leveling mortar has mortar mixes. The chemical composition of the cement was measured by X-ray flu-
little effect on the drying shrinkage compensation. The results of orescence (XRF) and illustrated in Table 1. The aggregates were composed of coarse
the same study by XU, linglin et al. [3] show that the drying shrink- quartz sand (40–70 mesh, Class A) and fine quartz sand (70–140 mesh, Class B). The
age of sulphoaluminate cement based self-leveling mortar is also mass ratio between the binder and sand was 1:1.5. Limestone powder (400 mesh)
was used as mineral filler. The limestone powder is 10% of sand by mass. The chem-
greater than 0.1%, and the trend is the same as that of calcium alu-
ical admixtures used in this research contained polycarboxylate-based superplasti-
minate cement. And there is no positive effect on drying shrinkage cizer (SP) dry power, a water retention admixture in powder, hydroxypropyl
by adding limestone powder and anhydrite. B. Yuan et al. discovered methyl-cellilose (HPMC), Redispersible latex powder. And anti-foam agent is also
that drying shrinkage is significantly increased with the increased of used.
limestone powder [18]. Moreover, using anhydrate in SLM cause
lower strength and higher drying shrinkage [13]. In a word, the 2.2. Mix proportion and sample preparation
above results indicate that the drying shrinkage of the fast hard
The mixture proportion of the specimens in the experiment is listed in Table 2.
cementing system will increase as the relative humidity continues
In addition, the dosage of superplasticizer, redispersible powder, HPMC, and anti-
decreasing after the paste hardening [19], and worse, the tendency form agent are 0.6%, 0.5%, 0.01% and 0.02% by mass of binder, respectively. The mix-
of continuous shrinkage of mortar volume is still not stable, which ture of ordinary mortar and self-leveling mortar were used for investigating the
will increase the risk of cracking and failure of mortar significantly. characteristic between ordinary mortar and self-leveling mortar. The dimension
Super absorbent polymers (SAP), act as the internal curing of the mold to measure fluidity was U 30 mm  50 mm.
The superabsorbent polymers (SAP 120–180 mesh) were incorporated at differ-
admixtures in high-performance concrete due to their ability to ent dosage of 0, 0.2, 0.4 and 0.6 percent (S-1–S-4) by weight of cement to investi-
absorb water quickly and release it slowly in the hydrate process, gate the internal curing effect and shrinkage reduction. The SAP were pre-wetted
cement-based matrix [20]. They were found to be especially (the water is 20 times by its own mass) in a beaker for 30 min.
efficient for internal curing to mitigate autogenous shrinkage in All the specimens were cured at 20 ± 2 °C, and the relative humidity was
50 ± 5%.
Portland cement-based materials [11,21–24]. The internal curing
of high strength concrete and ultra-high strength concrete with
super absorbent polymers reduce the value of autogenous shrink- 2.3. Test method

age by a large margin [25]. Compared with the reference sample, 2.3.1. Flexural strength and compressives strength
the method of internal curing can significantly improve the The strength testing was carried out according to GB/T 17671-1999 (refer to
chemical shrinkage and self-drying shrinkage caused by cement ISO:679) [35].
J. Yang et al. / Construction and Building Materials 201 (2019) 401–407 403

Table 1 age, the self-leveling mortar shows the same rule of volume change
Chemical composition of cement. as the ordinary mortar. In other word, the drying shrinkage and
Composition (%) autogenous shrinkage of both self-leveling mortar and ordinary
SiO2 Al2O3 Fe2O3 CaO MgO Na2O K2O SO3 TiO2 Loss mortar rise up dramatically, and reach the stable state on about
28th day. The difference is that the drying shrinkage of self-
19.57 4.95 3.05 63.86 0.41 0.44 0.36 4.59 0.42 2.35
leveling mortar is always greater than that of ordinary mortar.
Meanwhile, its autogenous shrinkage is smaller, which is 1.08
times and 93% of ordinary mortar, respectively. It can be concluded
Table 2
Mix proportion.
that organic admixtures, such as cellulose ether, redispersible latex
powder and the addition of water reducer and defoamer, may have
Sample Cement Sand Limestone powder Water Admixtures two effects on hardened self-leveling mortar: a) The drying shrink-
(g) (g) (g) (g) (g)
age of mortar is increased; b) The hydration process of cement is
M1 600 810 90 264 0 delayed.
M2 600 810 90 264 8.4
S-1 600 810 90 264 8.4
The experimental results of mechanical properties of self-
S-2 600 810 90 264 8.4 leveling mortar and ordinary mortar are listed in Fig. 2. The flexural
S-3 600 810 90 264 8.4 strength and compressive strength of self-leveling mortar are
S-4 600 810 90 284 8.4 respectively 2.1 MPa and 10.1 MPa at 1 day, which are 51.22%
and 43.72% of ordinary mortar, respectively, then the flexural
2.3.2. Shrinkage and compressive strength gradually catches up, and become
Shrinkage was carried out according to JC/T 603-2004 (refer to ASTM C596- greater than ordinary mortar with the increase of curing age. The
2001) [36]. The specification of sample was 25 mm  25 mm  280 mm. For the experimental results of mechanical properties of two kinds of mor-
drying shrinkage test, the reference length for each set was measured after 24 h tar show that organic admixtures can significantly reduce the early
of curing. For the autogenous shrinkage test, the samples were sealed with paraffin
mechanical properties of the mortar and have a significant effect
wax, after demolding. The sample can insert steel nail partially embedded at each
end. Then, the samples were measured daily until 28 days, and then recorded once on the hydration and structure formation process.
a week. The shrinkage ratio was calculated according to Eq. (1). The hydration heat release rate and hydration heat of the two
s ¼ ðln  l0 Þ=250  100% ð1Þ cement pastes are shown in Fig. 3. It can be seen that organic
admixtures can effectively delay the hydration process of cement,
where S is shrinkage ratio, %; l0 is its initial length measured after demolding, ln is the
the notable features of which include: 1. The second peak of hydra-
measured length of specimen cured for n day. 250 is the effective length of the
specimen.
tion heat release of the self-leveling mortar system was delayed
from 14 h to 33 h. 2. The heat of hydration decreased significantly,
2.3.3. Characterization and it was 40.1 J/g, 61.9 J/g and 302.8 J/g at 12 h, 24 h and 72 h,
The isothermal heat-conduction calorimeter (TA AIR, USA) was used to measure only 47.5%, 30.3% and 85.8% without doping, respectively. Cellulose
the heat evolution of samples after 72 h. The samples were prepared with a W/C of ether and redispersible latex powder are commonly organic poly-
0.5. Mercury intrusion porosimetry (MIP) analysis (Auto pore IV9500, USA) was
mer admixtures used for cement-based materials, which are bene-
conduct to determine the microstructural characteristics, such as total porosity
(%) and pore size distribution of specimen. Scanning Electron Microscopy (SEM, ficial to the working performance, mechanical properties, and
TM-4000, HITACHI) was used to characterize typical pores. The inner surfaces of microstructure of their. When being treated with water, the sur-
hydration mortar were sputtered with gold. face of cement particles begins to decompose rapidly, release a
large amount of Ca2+, Al3+ and SO24 , and form hydration products
3. Results and discussions such as CH, Aft and C-S-H gel. At the same time, organic polymers
also hydrolyze in large quantities. The hydration is delayed due to
3.1. Ordinary mortar (M1) and self-leveling mortar (M2) the adsorption on the surface of cement particles. With the
increasing of osmotic pressure, the film layer is destroyed, and
Fig. 1 shows the effect of curing age on dry shrinkage and auto- the reaction is accelerated again, which gradually catches up with
genous shrinkage of mortar. Clearly, with the extension of curing the hydration degree of the ordinary mortar in the later stage. The

Fig. 1. Shrinkage of M1 and M2. (a. drying shrinkage; b. autogenous shrinkage).


404 J. Yang et al. / Construction and Building Materials 201 (2019) 401–407

Fig. 2. Strength of M1 and M2. (a. flexural strength; b. compressive strength).

Fig. 3. Hydration heat evolution of M1 and M2 within 72 h: (a) heat evolution rate; (b) cumulative heat.

results of the hydration rate and heat discharge of the two kinds 3.2. Superabsorbent polymers (SAP)
of mortar demonstrate that the admixture has a great influence
on the hydration process of cement, which shows the difference The effect of superabsorbent polymers on drying shrinkage and
in the development process of mechanical properties autogenous shrinkage of self-leveling mortar is shown in Fig. 5. The
macroscopically. information clearly tells us that the inhibition effect of superab-
The pore structure characteristics of self-leveling mortar and sorbent polymers on drying shrinkage and autogenous shrinkage
ordinary mortar after 3 days and 28 days were measured by MIP. of self-leveling mortar is not obvious in the first 7 days. With the
The experimental results are shown in Fig. 4. It can be seen that extension of the age, the superabsorbent polymers began to play
the pore structure of the self-leveling mortar and the ordinary a contractile compensation effect, and when it developed at the
mortar are bimodal distribution after 3 days, the peak value 28 days, both the drying shrinkage and the autogenous shrinkage
appears at 32 nm and 39 nm, 350 nm and 590 nm, respectively, tended to be stable, but this effect was not positively related to
which indicates that the incorporation of the organic admixture the content of superabsorbent polymers. The shrinkage compensa-
significantly reduces the proportion of the coarse pores. The per- tion and inhibition effect are better in this research as the content
centage of capillary pores of 30 nm–40 nm is the highest when of superabsorbent polymers is 0.4%wt, and are reduced by 12.6%
samples are cured to 28 days. The pore becomes the main pore of and 15.5%, respectively. When the content of superabsorbent poly-
self-leveling mortar and ordinary mortar. The content of coarse mers is more than 0.6%, the drying shrinkage and autogenous
pore in self-leveling mortar is much lower than that in ordinary shrinkage have a tendency to increase again. With the increase of
mortar. The pore size optimization by adding cellulose ether and the content of superabsorbent polymers, the flexural strength
redispersible latex powder is one of the reasons why the mechan- and compressive strength of the mortar drop to 8.1 MPa and
ical properties of self-leveling mortar gradually catch up and 43 MPa, which decreased by 20.5% and 25.8% compare to the refer-
exceed those of ordinary mortar. The decease of coarse pores is ence, respectively (Fig. 6). After the decomposition of SAP, a large
very favorable for the strength of the hardened test block. And pore will be left, resulting in the decline of mechanical properties,
the result of this study is consistent with the existing literature consistent with the research results of the existing literature
and theory. [27,37,38].
J. Yang et al. / Construction and Building Materials 201 (2019) 401–407 405

Fig. 4. Pore size distribution curves of M1 and M2 (a. 3 days; b. 28 days).

Fig. 5. SLM with and without SAP (a. drying shrinkage; b. autogenous shrinkage).

Fig. 6. Effect of SAP on the flexural and compressive strength of SLM.

The effect of SAP on the pore structure of hardened specimens is statistics of different aperture ranges show that the addition of
shown in Fig. 7. The pore size distribution curve shows that SAP SAP has little effect on the coarse pores larger than 100 nm, and
makes the pore size distribution of the matrix more concentrated, the pores under 100 nm rise obviously. The pore content of the
and the capillary pore content larger than most probable pore 10–30 nm aperture range is increased by 37.5%, 41.6% and 34.3%,
(20–35 nm) decreases significantly, which is very beneficial to when the amount of SAP is 0.2%, 0.4% and 0.6%, respectively,
reduce the shrinkage caused by capillary pore force. The porosity corresponding to the decrease of the pore size at 30–100 nm of
406 J. Yang et al. / Construction and Building Materials 201 (2019) 401–407

Fig. 7. Effect of SAP on the pore size pore size distribution of SLM.

Fig. 8. SEM microstructure of SLM with SAP (b, c) and without SAP (a) at 28 days.

the reference sample. Pore composition and structural characteris- with the increase of curing age. The second peak of hydra-
tics of cement-based materials, including porosity, pore size distri- tion heat release of the self-leveling mortar system was
bution and the most available pore size, are important factors to delayed and the heat of hydration is smaller than ordinary
determine the mechanical properties, volume stability and dura- mortar. The situation is mainly due to a large number of
bility of cement-based materials. For shrinkage, the change of pore additives in self-leveling mortar.
size in the range of 10–100 nm is more closely related to the drying (2) SLM with SAP can significantly reduce drying and autoge-
shrinkage, which is consistent with the existing results [39–41]. nous shrinkage. The refinement of pore structure caused
Some SAP voids will be formed in the hardened self-leveling by SAP improved the properties of self-leveling mortar.
mortar after the desorption of SAP [38]. The mentioned results The formation of hydration diffusion layer reduces the size
indicate that the SAP voids almost have some negative impacts of voids. As a result, total porosity are reduced.
on the strength and pore structure [42]. Observation for the (3) SEM examination indicated the pores by desorption of SAP
microstructure around SAP voids, thus, is necessary. As seen in in the SLM. Expansion of the hardened bulk volume is
SEM micrographs (Fig. 8). There is a lot of C-S-H gel, Ca(OH)2 and mainly caused by Ca(OH)2 and Aft found in the pores.
Aft in the reference sample (Fig. 8a). However, macro pore can be
clearly found in SAP sample (Fig. 8b) [31]. Besides producing larger
pores, SAP can also has an influence on smaller pores in SLM [43]. Acknowledgements
This reduction can be attribute to the filling of pores with hydra-
tion products that were facilitated by SAP’s water supply (Fig. 8c) The authors gratefully acknowledge the analytical support of
[44,45]. As smaller pores are filled with later hydration products, SWUST Analysis and Test center, Mianyang, China. This work is
the products begin to exert pressure on the pore walls. There is a supported by Doctorate Foundation of Southwest University of
‘‘space competition” between hydration products and hardened Science and Technology (No. 17zx7132) and Postgraduate
microstructure. Consequently, this stress results in the ‘‘relative” Innovation Found Project by Southwest University of Science and
expansion of the hardened bulk volume at later stage [46]. Technology (No. 18ycx063).

Conflict of interest
4. Conclusions
None.
The aim of this paper is to study the shrinkage law and mecha-
nism of Portland cement based self-leveling mortar. Then, we put
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