Construction and Building Materials 231 (2020) 117142

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Construction and Building Materials

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

Effects of superabsorbent polymer on interfacial transition zone and

mechanical properties of ultra-high performance concrete
Jianhui Liu a, Nima Farzadnia b,⇑, Caijun Shi a,*
a
Key Laboratory for Green & Advanced Civil Engineering Materials and Application Technology of Hunan Province, College of Civil Engineering, Hunan University, Changsha
410082, China
b
Center for Infrastructure Engineering Studies, Department of Civil, Architectural and Environmental Engineering, Missouri University of Science and Technology, Rolla, MO, USA

h i g h l i g h t s

SAP can densify the interfacial transition zone.

SAP can reduce micro-cracks around the fibers.

Steam curing can partly compensate the bond strength loss of fibers caused by the SAP.

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

Article history: In this study, two particle sizes of superabsorbent polymer (SAP) with different contents (0–0.6%) were
Received 1 August 2019 incorporated in the UHPC samples cured under two regimes: water and steam curing. The interfacial
Received in revised form 16 September transition zone (ITZ) associated properties, namely compressive strength, flexural strength, and pullout
2019
behavior of steel fiber were evaluated. Micro-hardness method and backscattered electron (BSE) imaging
Accepted 2 October 2019
Available online 10 October 2019
examinations were also applied to investigate the underlying mechanisms of SAP performance in UHPC.
The results show that the use of SAP densified the ITZ and reduced micro-cracks around the fibers.
However, the pores left from SAP impaired the bonding strength and ITZ of UHPC, when high contents
Keywords:
Bonding strength
and large size of SAP particles were incorporated. Steam curing, though, partly compensated the bond
Interfacial transition zone strength loss of fibers caused by the SAP.
Super-absorbent polymer Ó 2019 Elsevier Ltd. All rights reserved.
Steel fiber
Ultra-high performance concrete

1. Introduction of internal curing agents, such as lightweight aggregates (LWA)

Ultra-high performance concrete (UHPC) is an advanced
cement-based composite with superior mechanical performance,
high toughness, and excellent durability [1,2]. The flexural proper-
ties of UHPC are significantly improved owing to the addition of
fibers (e.g., steel and synthetic fibers). The dense interfacial transi-
tion zone (ITZ) between fibers and the matrix further enhances the
bond strength between them, which can provide strain-hardening
behavior in tension, and transform the brittle rupture to a ductile
failure [3]. However, one of the major problems with UHPC is its
high early autogenous shrinkage as a result of its ultra-low
water-to-binder ratio (w/b) and high binder content [4,5]. Internal
curing is one of the common methods to reduce autogenous
shrinkage by gradually providing extra water for the hydration. It
involves the absorption of the curing water within the structure
⇑ Corresponding authors.
E-mail addresses: farzadnian@mst.edu (N. Farzadnia), cshi@hnu.edu.cn (C. Shi).
[6] and superabsorbent polymer (SAP) [7], and water release over-
time upon drop of the internal relative humidity (IRH) of the
matrix. SAP is available in various sizes and types [4] and has
recently attracted more attention than LWA as it does not require
pretreatment. However, release of water from SAP leave pores at
later ages that may impair the mechanical properties [7]. This
effect can be further accentuated in fiber-reinforced UHPC as it
hypothetically reduces the bond strength at ITZ of fibers and
matrix.
The toughness and strain-hardening behavior of UHPC mainly
correspond to the bond strength between the fiber and matrix,
which is significantly related to the properties of the interface of
fiber and the matrix. Lyubimove et al. [8] first conducted an in-
depth study on the interface area of aggregate in the conventional
concrete at the mesoscale and proposed the concept of the ‘‘inter-
facial transition zone.” Later, a large number of scholars used mod-
ern testing techniques to study the nature of ITZ and its effect on
mechanical properties and durability of cement-based materials.

https://doi.org/10.1016/j.conbuildmat.2019.117142
0950-0618/Ó 2019 Elsevier Ltd. All rights reserved.
2 J. Liu et al. / Construction and Building Materials 231 (2020) 117142
It was found that thickness of the interfacial layer of fiber and
aggregate is generally 50–100 lm in conventional concrete, and
its hardness mainly varies with the characteristics of the matrix
[9–11]. In the ITZ, a weak area was detected (also known as the
weak valley) in which initial cracks propagate upon exertion of
external loads. The weak zone can be formed due to the higher
porosity of the ITZ as well as concentration of calcium hydroxide
(CH) crystals that are aligned in the ITZ with a high orientation
index and a broad orientation range [12]. The fiber interface area
in conventional fiber reinforced concrete is discussed in [13]. For
UHPC, the porosity is very low, which limits the growth of CH crys-
tal inside the voids [2]. The CH content in conventional concrete is
reported to be 20–40% higher than the UHPC [12].
Furthermore, the ill-formed CH crystals will be susceptible to
higher rate of consumption with the presence of supplementary
cementitious materials (SCMs) in UHPC to form a C-S-H gel. It
can be further accentuated when UHPC is cured at elevated tem-
peratures (steam curing). It is reported that the addition of 20%
fly ash enhanced the ITZ of normal concrete [14] and fracture
toughness [15,16], and 15–25% silica fume was the optimal content
to further densify the ITZ of steel fiber the UHPC matrix [17]. Com-
pared to conventional concrete, there are almost no large-sized CH
crystals inside the UHPC [2]. Therefore, the ITZ structure of UHPC is
much improved, and the C-S-H in UHPC is mainly high-density C-
S-H with high rigidity and hardness [18].
However, the incorporation of ultra-low w/b and high content
of SCMs can lead to rapidly induced self-desiccation and crack
formation at early ages [19]. Autogenous shrinkage is one of the
most critical issues to be addressed in UHPC, which causes con-
siderable cracking potential at early age. A shrinkage peak of 64
millionths/hour and total shrinkage of 400 millionths were mea-
sured in the first 24 h in UHPC [20]. The use of SAP is an effective
way to reduce the autogenous shrinkage because it can restrain
the instant drop of IRH and control the self-desiccation, as the
critical drive of autogenous shrinkage [4,7,21]. The addition of
SAP could also improve the hydration degree and densify the
matrix around the SAP [22,23]. However, the desorption of water
from SAP can leave pores [24,25] and impair the properties of the
matrix [26]. In UHPC that fiber has a significant influence on the
flexural enhancement, the formation of such pores can weaken
the ITZ and bond strength of fibers and reduce the effectiveness
of fibers in flexural strength.
The overarching purpose of this study is to investigate the effect
of the size and content of SAP on mechanical properties of rein-
forced UHPC. The tensile ductility and toughness of UHPC are
mainly related to the bond strength of the interfacial zone between
fibers and UHPC matrix, which makes it have potential applications
in long-span bridges and industrial structure members. Therefore,
understanding the effect of SAP on microstructure, especially at the
interface of steel fibers, is crucial. Besides, steam curing a
Table 1
Chemical composition of cement, silica fume and fly ash.
SiO2 Al2O3 Fe2O3 CaO MgO SO3 Na2Oeq
Cement 20.76 4.58 3.27 62.13 3.13 2.80 0.57
Silica fume 93.90 – 0.59 1.85 0.27 – –
Fly ash 54.29 32.55 5.53 1.34 2.56 – –
Table 2
Physical properties of Portland cement.
Density (kg/cm3) Specific Surface Area (m2/kg) Setting Time/Min
Initial
3.15 348 152
commonly used curing method for UHPC [27], was applied and
the effect of elevated temperature on the bond strength of the
interfacial zone between fibers and UHPC matrix was compared
with water cured. The steam curing enhances the mechanical
properties and durability due to accelerating effect of temperature
on the hydration of clinker, pozzolanic reaction of silica fume and
the reaction of quartz powders, which further increases the
amount of C-S-H phases. However, there is no relevant research
on the combination SAP with steam curing. In this paper, SAP par-
ticles with two size ranges and two contents were incorporated in
the UHPC samples cured under two regimes: water and steam cur-
ing. Accordingly, the ITZ associated properties, namely compres-
sive strength, flexural strength, and pullout behavior were
evaluated. Micro-hardness method and BSE image were also
applied to investigate the underlying mechanisms of SAP perfor-
mance in the fiber-reinforced UHPC.
2. Experiment
2.1. Raw materials and mix proportion
The cementitious materials used in this work comprised P.I.
42.5 Portland cement (according to Chinese standard of GB
175-2007), silica fume, and fly ash. The physical properties and
chemical compositions are shown in Tables 1 and 2. Fine aggregate
(natural sand) with a maximum particle size of 2.36 mm was used.
Its fineness modulus and apparent densities were 2.7 and
2610 kg/m3, respectively. SAP was an angular covalently cross-
linked acrylamide/acrylic sodium copolymer with two different
sizes. Its particle size is shown in Fig. 1, measured by laser particle
size analyzer. The water absorption of SAP was 210 g/g in tap
water, which was measured by the tea bag method [28]. Straight
brass-coated steel fibers measuring 0.2 mm in diameter and
13 mm in length with a tensile strength of 2000 MPa were used.
Polycarboxylate-based superplasticizer (SP) with a water reduction
capacity of 25% was used. The mixture proportions of UHSC are
shown in Table 3. R0.18 and R0.22 were cast as control groups with
w/b of 0.18 and 0.22, respectively. Two size ranges of SAP (denoted
as small (SS) and large (SL) at contents of 0.3% and 0.6% were used.
The additional water content was adjusted according to the
absorption capacity of SAP [5].
2.2. Casting and curing
All mixtures were prepared and tested at room temperature
(20 ± 2 ). Initially, all dry materials were mixed at 60 rpm for
2 min in order to improve the dispersibility of silica fume particles;
then, 90% of water and SP mixture was added and mixed for 2 min
at 120 rpm; and finally, the remaining water and SP were added
R2O C3S C2S C3A C4AF Loss on Ignition
– 56.53 21.94 6.44 10.40 1.86
1.03 – – – – 0.3
0.19 – – – – 3.19
Flexural Strength Compressive Strength
(MPa) (MPa)
Final 3d 28 d 3d 28 d
212 5.6 8.6 28.6 51.2
 J. Liu et al. / Construction and Building Materials 231 (2020) 117142 3

25 react with CH, the compressive and flexural strength tests were
conducted up to 56 days.
SL
2.3.2. Pullout strength
Parricle size distribution(%)

20
15
10
5 vertical holes at a depth of 5 mm each to ensure adequate embed-
0
10
Fig. 1. Particle size distributions of SL and SS.
and mixed for 2 min before casting. After casting, the samples were
placed into the standard curing room (RH > 95%, 20 ± 2 °C) for 24 h
and then demolded. The demolded samples were cured under two
regimes; (i) two-day (2-d) water curing and (ii) two-day (2-d)
steam curing before exposure to drying condition. The drying
condition represents humidity and temperature of 50% ± 4 and
20 ± 2 °C, respectively that continued to the time of testing.
The corresponding samples under steam curing were marked with
‘-S’ (e.g., R0.18-S). In this study, the terms water curing and steam
curing are used throughout the manuscript that refer to a duration
of 2 d.
SS
The pullout behavior and bond strength of fibers were evalu-
ated using dog-bone shape samples according to [17,29]. The mold
size and shape are shown in Fig. 2. The preparation of molds was as
follows: (i) the molds were divided into two halves by a plastic clip
with four fibers perpendicularly positioned form the center. The
plastic clip had four holes with an evenly distributed space of
15 mm, as shown in Fig. 2; (ii) four fibers were passed through
the holes using a self-made bamboo substrate designed with four
ded fibers length (5 mm in the pullout half) and orientation of
fibers (iii); the fibers were fixed in the plastic clips using super
glue; and (iv) the plastic clips were first put into two parallel slots
100 1000 located at the center of steel molds. A plastic film was used to cover
the whole casting zone in the mold crossing the plastic clip to pre-
Size (μm) vent the adhesion of the two halves to the matrix entirely. The
UHPC was then cast into the molds. The samples were demolded
24 h after casting and cured according to Section 2.2.1.
An MTS testing machine with a 20 kN load cell was used to
carry out the pullout testing, according to CECS13-2009 [30] at a
loading rate of 0.5 mm/min. For each matrix, five samples were
tested. The bond strength was calculated as follows [17]:
Pmax
smax ¼ ð1Þ
npdl
where smax (MPa) is the bond strength of the embedded fiber based
on the maximum pullout load; Pmax (N) is the maximum pullout
load; d (mm) is the diameter of a single fiber;l (mm) is the embed-
ment length of the fiber in pullout half (5 mm); n (4) is the number
of fibers embedded in a dog-bone sample.

2.3. Experimental methods 2.3.3. Backscattered electron (BSE) imaging

For the BSE observation, small specimens from freshly broken
2.3.1. Compressive and flexural strength samples were soaked in ethyl alcohol to stop further hydration
The compressive and flexural strength tests were conducted in for 48 h and then dried at 60 in a vacuum oven for 48 h before
compliance with GB/T 17671-1999. The flexural strength of UHPC testing until a constant mass was reached. They were ground to
was obtained using prism samples measuring obtain a relatively smooth surface, then mounted in epoxy resin
40 mm  40 mm  160 mm, and an average of three tested sam- and subjected to further grinding and polishing to ensure high
ples was reported. The test adopted an MTS microcomputer- smooth surface quality [31,32]. The polished specimens were then
controlled Electromechanical Universal Test Systems using a sputtered with gold and examined using a QUANTA 450 with the
three-point loading method with a testing span of 100 mm. Dis- back-scattered detector in the high vacuum mode. At last, the
placement control method was adopted during loading, and the BSEM images were processed by Image-J software to obtain the
control speed was 1 mm/min. A force of 500 N was preloaded to histogram of the grey level to calculate the porosity of the UHPC
fix samples before the test. Six samples were used to measure matrix around steel fiber [33].
the compressive strength after the flexural strength. The loading
speed was set at 2.4 kN/s. The strength value of the sample at fail- 2.3.4. Micro-indentation
ure was recorded, and the average value of six samples was Micro-indentation test was applied to measure microhardness
reported. In this paper, we used fly ash to partially replace Portland of ITZ. The indentations were tested using an Hvs-1000 Vickers
cement. As fly ash has low reactivity and needs a longer time to hardness tester with a square-based pyramid indenter, as shown

Table 3
Mixture proportions of UHPC matrix.

No. Binder (%) s/b Total w/b Effective w/b SAP (%) Steel fiber (%) Superplasticizer (%)
cement fly ash silica fume
R0.18 55 20 25 1.1 0.18 0.18 0 2 3
R0.22 55 20 25 1.1 0.22 0.22 0 2 3
SS0.3 55 20 25 1.1 0.20 0.18 0.3 (SS) 2 3
SS0.6 55 20 25 1.1 0.22 0.18 0.6 (SS) 2 3
SL0.3 55 20 25 1.1 0.20 0.18 0.3 (SL) 2 3
SL0.6 55 20 25 1.1 0.22 0.18 0.6 (SL) 2 3

Note: s/b and w/b refer to sand to binder ratio, and water to binder ratio, respectively; Total w/b is calculated as the ratio of total water content, including the water absorbed
by the SAP, to binder, while the water absorbed by SAP was excluded for effective w/b.
4 J. Liu et al. / Construction and Building Materials 231 (2020) 117142

Fig. 2. Illustration of dog-bone shape mold (mm).

in Fig. 3. Micro-indentation is based on applying a static load for a 3. Results

known period and measuring the response in terms of the size of
the indentation. In this study, a 498 mN load was applied for
10 s on specimens identical to those used for the BSE test, and
the micro-hardness or Vickers hardness (HV) was calculated
according Eq. (2). Ten points within the area of 50 mm from the
fiber edge were indented. During the indentation process, areas
with sand/SAP were avoided. The micro-hardness was captured
during the measurement, and the average values of 10 indenta-
tions were reported.
2Psinða=2Þ
Hv ¼
S R0.18 (w/b of 0.18), respectively. As the age prolonged to 28 d,
where Hv is micro-hardness or Vickers hardness (MPa); P is load
force (N); a is the angle between the opposite faces of the indenter
(136°); S Indentation area (mm2).
3.1. Compressive strength
Fig. 4 shows the compressive strength development of UHPC up
to 56 d under two curing regimes. Fig. 4a shows the strength devel-
opment of samples under the water curing regime. As shown, the
incorporation of SAP in UHPC decreased the compressive strength
of samples at an early age comparing to the control samples with
w/b of 0.18. However, UHPC mixtures with 0.3% SAP (SS0.3 and
SL0.3) obtained relatively higher compressive strength at 3 d than
ð2Þ that of samples with w/b of 0.22, but 18.6% and 32.0% lower than
the same trend was observed; however, the compressive strength
development of SS0.3 was more rapid than the counterpart sam-
ples. It shows that the extra water added by internal curing was

(a) Vickers hardness tester (b) Schematic diagram of indentation

Fig. 3. Micro-indentation test.

200
R0.18
Compressive strength (Mpa)
175 SS-0.3
SL-0.3
150
125
100
75
50
0 10 20
Time (d)
(a) Water cured UHPC
more active on the strength development of UHPC when lower
contents of the SAP with small particles were applied. The incorpo-
ration of 0.3% of SAP with large particles (SL0.3) also led to com-
pressive strength comparable to control samples with w/b of
0.22. In the previous study [7], the incorporation of 0.6% SAP
obtained a higher compressive strength than control samples
(the same total w/b) in non-reinforced UHPC, which can indicate
that the hybrid use of SAP and fiber can change the optimum con-
tent of SAP. In this study, the addition of 0.6% SAP had an adverse
effect on the fiber-reinforced UHPC. The compressive strength of
SS0.6 and SL0.6 at 56 d were 9.6% and 15.4% lower than R0.22,
respectively. The minimum strength was recorded for samples
when higher contents of SAP with large particles were
incorporated.
Fig. 4b shows the compressive strength development of steam
cured UHPC samples within the first 56 d. The samples were under
2-d steam curing before exposure to the drying condition. As can
be seen, the compressive strengths of all groups were higher than
the water curing samples at all ages. However, results showed that
the compressive strength had only a slight increase with prolonga-
tion of the hydration age after steam curing. Results are indicative
that the steam curing compensated the negative effect of SAP on
the compressive strength of UHPC. There was an insignificant dif-
ference between the R0.22 and samples with the SAP after steam
curing. Similar to the water cured samples, the R0.18 had the high-
est compressive strength at 3 d. As the drying duration prolonged,
the compressive strength of samples with 0.3% SAP (SS0.3 and
SL0.3) increased slightly at a level higher than the R0.22. Unlike
water cured samples, the samples with large SAP obtained similar
strength to that of R0.22 at all ages.
3.2. Flexural strength
Fig. 5 shows the flexural strength development of UHPC up to
56 d under two curing regimes. As shown in Fig. 5a, at 3 d, the sam-
ples with 0.3% SAP had similar flexural strength with the R0.18,
though, incorporation of higher contents of SAP with larger parti-
cles reduced the flexural strength. With the increase of age, the
flexural strength of UHPC with small SAP particles increased signif-
icantly, while the adverse effects of SAP with large particles were
maximum when 0.6% SAP was applied (SL0.6). The results show
that the flexural strength of SS0.3 gained higher strength than
R0.18 as age prolonged to 56 d, while the SS0.6 obtained similar
flexural strength. On the other hand, the flexural strength of UHPC
with large SAP particles increased at the same rate as the R0.22. At
J. Liu et al. / Construction and Building Materials 231 (2020) 117142 5
200
R0.22
Compressive strength (Mpa)
SS-0.6 175
SL-0.6
150
125
100
R0.18-S R0.22-S
75 SS0.3-S SS0.6-S
SL0.3-S SL0.6-S
50
30 40 50 60 0 10 20 30 40 50 60
Time (d)
(b) Steam cured UHPC
Fig. 4. Compressive strength of UHPC at different ages.
56 d, the SL0.3 had the same flexural strength as R0.18. However,
the flexural strength of SL0.6 dropped even lower the R0.22. Incor-
poration of SAP with large particles at 0.6% decreased the flexural
strength by 12.6%, 4.1%, and 6.3% at 3, 28, and 56 d compared to
R0.22. A comparison with the results from compressive strength
shows that the SAP, in general, was more active on flexural
strength independent of size as it maintained the flexural strength
higher than the R0.22 or for some mixtures higher than R0.18.
Fig. 5b shows the development of the flexural strength of the
UHPC sample under 2-d steam curing. As can be seen from the fig-
ure, the flexural strength of UHPC at 3 d developed up to more than
90% of the strength at 56 d, when samples were under steam cur-
ing. The R0.18 obtained the highest strength, followed by samples
with SAP with small particles. However, the content was an essen-
tial factor as the flexural strength of SS0.3 and SL0.3 were higher
than SS0.6 and SL0.6 at all ages, respectively. All UHPC samples
with SAP, except for SL0.6, were between the reference group of
R0.18 and R0.22. The results are conclusive that steam curing
increased the flexural strength of UHPC samples, especially at early
age compared to that of samples cured in water. Unlike in com-
pression, the combined use of SAP with large particles and steam
curing was not as effective on flexural strength as compared with
water cured samples.
3.3. Pullout strength
Fig. 6 shows the pullout load-slip curves of UHPC samples at
28 d. Generally, pullout behavior can be divided into four distinct
regions, as shown in Fig. 6a, including well-bonded region (Region
I: OA), partially debonded region (Region Ⅱ: AB), fully debonded
region (Region III: BC), and removal of fiber (Region Ⅳ: CD)
[34,35]. Fig. 6b and c show that within a pullout slip of about
0.5 mm, at the well-bonded region (Region I), the pullout load-
slip behavior was observed to have linear-elastic properties. All
curves showed an increased pullout load with the increase of slip
until reaching the fully deboned region (Region III). When the peak
load was achieved, it remained almost stable, although the pullout
slip increased. The results suggest that UHPC samples showed slip-
hardening behavior owing to the high matrix packing density
around the fiber, causing a high frictional coefficient and fiber sur-
face pressure [36]. In this range, the load-slip curve did not show
obvious descending load, but a part of the fiber had already
debonded from the UHPC matrix. With continued loading, the fiber
was gradually pulled out from the matrix (Region Ⅳ). Once the
fiber is fully debonded from the matrix, the pullout behavior is
6 J. Liu et al. / Construction and Building Materials 231 (2020) 117142

30 30
Flexural strength (Mpa)

Flexural strength (Mpa)

25 25

20 20

15 R0.18 R0.22 15 R0.18-S R0.22-S

SS-0.3 SS-0.6 SS0.3-S SS0.6-S
SL-0.3 SL-0.6 SL0.3-S SL0.6-S
10 10
0 20 40 60 0 10 20 30 40 50 60
Time (d) Time (d)
(a) Water cured UHPC (b) Steam cured UHPC
Fig. 5. Flexural strength of UHPC at different ages.

(a) Typical pullout load-slip curves of steel fiber, derived from [37].

120 120
R0.18-S
100 SS0.3 100

R0.18 SS0.3-S
80
Pullout load (N)

80
Pullout load (N)

R0.22-S
SS0.6
60 60 SS0.6-S
R0.22

40 40
SL0.3-S
20 SL0.6 SL0.3 20
SL0.6-S

0 0
0 1 2 3 4 5 6 0 1 2 3 4 5 6
Pullout slip (mm) Pullout slip (mm)

(b) Water cured UHPC (c) Steam cured UHPC

Fig. 6. Fiber pullout load-slip curves of UHPC matrix with or without SAP at 28 d. (See above-mentioned references for further information.)
 J. Liu et al. / Construction and Building Materials 231 (2020) 117142 7

governed by frictional bond shear stress with the interface, and
fiber is gradually pulled out from the matrix.
As can be seen from Fig. 6, the embedded fibers in the UHPC
matrix with SAP experienced debonding at a different pullout load
capacity compared to the reference mixtures without SAP, which
was dependent on the size and content of SAP. For water cured
samples (Fig. 6.b), the SAP with small particles (SS0.3) increased
the pullout load capacity, higher content (SS0.6) caused a slight
decrease compared to R0.18. SAP with large particles led to a sig-
nificant reduction in the pullout load capacity at 28 d. Also, a
slip-hardening behavior and a slow descending branch were
observed when the small SAP was used. However, the slip-
hardening behavior was not evident for the UHPC samples when
SAP with large particles was incorporated. Similar behavior was
also shown in the steam cured samples (Fig. 6.c). However, the
control group of R0.18 had the largest peak value of pullout load
and an apparent softening pullout behavior.
To further characterize the effect of curing and hybrid use of
SAP and fibers on pullout behavior, the bond strength of each sam-
ple was calculated according to equation (1) (Fig. 7a). The results
were conclusive that the bond strength of steam cured UHPC sam-
ples was larger than samples cured in water. However, a different
behavior regarding the effect of SAP content and size was observed.
For the water cured samples, the SAP with small particles at lower
content (SS0.3) had a beneficial effect on the bond strength
between steel fiber and UHPC matrix, and the highest bond
strength was recorded. On the other hand, this beneficial effect
was lower with an increase in SAP content. On the contrary, the
incorporation of 0.3% and 0.6% SAP with large particles decreased
the bond strength by 29.8% and 25.9% compared to SS0.3 and
SS0.6, respectively.
For the steam cured samples, the bond strength was higher than
those cured in water. However, the steam curing regime was more
effective on the reference mixture of w/b 0.18. A decrease of 15.3%,
27.3%, 34.8%, and 36.4% was observed for the SS0.3, SS0.6, SL0.3,
and SL0.6, respectively, as compared to R0.18. Like water cured
samples, the steam cured UHPC samples with small SAP particles
had higher bond strengths than R0.22. In general, the incorporation
of SAP with large particles, independent of the content and curing
regime, had a negative impact on the bond strength.
Fig. 7b shows the effects of SAP particle size and content on
pullout energy of UHPC 28 d under two curing regimes. Pullout
energy is the mechanical energy consumed during fiber pullout
testing, which can be obtained by integrating the area under
pullout load-slip curves. For the water cured samples, the SAP with
small particles had a beneficial effect on the pullout energy
between steel fiber and UHPC matrix in samples with lower con-
tent of SAP(SS0.3), and the highest pullout energy was recorded.
However, the increase in SAP particle size significantly reduced
the pullout energy. For the steam cured samples, the pullout
energy was higher than those cured in water except for SS0.3
and SS0.6. The results show that the use of small SAP is more ben-
eficial for bond properties of steel fiber in UHPC water curing is
applied.
3.4. Microhardness of the interfacial transition zone (ITZ)
To investigate the effect of the size and content of SAP on the
interface of steel fibers and the matrix, the micro-hardness of ITZ
was obtained. The microhardness results are used to represent
the density of ITZ and explain the performance of fibers in flexural
strength, and pullout strength. Fig. 8 shows the hardness of the
area within 50 mm from fibers for R0.18, R0.22, SS0.6, and SL0.6
at 3 and 28 d. The hardness of ITZ with 0.6% SAP was less than that
of R0.18 at all investigated ages. Also, the results showed that SAP
with small particles led to higher ITZ hardness than that of SAP
with large particles. On the other hand, the results of SS0.6 and
SL0.6 have a great standard deviation, which may be caused by
the left pores from SAP around steel fibers. However, the results
show that the hardness of ITZ with small particle SAP (SS0.6)
was larger than R0.22 by 5.3% at 28 d for water cured samples. It
means that the internal curing of SAP increased the density of
ITZ to a level higher than R0.22 due to enhanced hydration degree
[22], which contributed to an increase in the bond strength of
fibers. However, the larger pores left after desorption of water from
large SAP particles that can aggravate to weaken the ITZ and loosen
the interface adhesion between fibers and the matrix. The results
are in good agreement with the negative effect of large SAP on flex-
ural strength and pullout performance of UHPC.
The curing regime also had a distinctive influence on the micro-
hardness. The results show that the steam curing increased the
hardness of SS0.6 and SL0.6 compared to water cured samples.
The hardness of ITZ of SS0.6 improved by 6.9% compared to
R0.22, and it was almost similar to that of R.18. On the other hand,
an analogy of results from 3 d to 28 d shows that exposure of steam
cured samples to the drying condition had no significant effect on
the hardness of samples, which is in a good agreement with the
results from mechanical properties (Figs. 4 and 5).

12 450
Water cured UHPC Water cured UHPC
Steam cured UHPC Steam cured UHPC
Pullout energy (N-mm)

10
Bond strength (MPa)

360

8 270

6 180

4 90

R0.18 R0.22 SS-0.3 SS-0.6 SL-0.3 SL-0.6 R0.18 R0.22 SS-0.3 SS-0.6 SL-0.3 SL-0.6
(a) Bond strength (b) Pullout energy
Fig. 7. Bond strength and pullout energy of UHPC with or without SAP at 28 d.
8 J. Liu et al. / Construction and Building Materials 231 (2020) 117142
240
3d 28d 3d-S 28d-S
200
Hardness (Mpa)
160
120
80
40
0 the porosity of ITZ (regions 1 and 2) for samples without SAP
R0.18 R0.22 SS0.6 SL0.6
Fig. 8. Micro-hardness of UHPC matrix around steel fibers at 3 d and 28 d.
3.5. BSE examinations
BSE technique was also used to explain the effect of SAP on
fiber-reinforced UHPC properties (Figs. 9 and 10). Fig. 9 shows
the microstructure of the UHPC matrix without SAP (R0.18) under
the investigated curing regimes at 3 and 28 d. Since the steel fiber
is distributed randomly in the matrix, and the displayed surface is
elliptical in the case where the cutting surface was not perpendic-
ular to the fiber. At 3 d, there was an apparent gap between the
UHPC matrix and the steel fiber in water cured samples (Fig. 9a).
However, the ITZ of steel fiber in steam cured samples was denser,
and less porosity was observed (Fig. 9b). The denser microstructure
of the ITZ of steam cured samples improved the bond between the
steel fiber and matrix and increased the bond strength (pullout
strength) and flexural strength. Micro-cracks were observed
around the steel fiber in water cured UHPC samples as the drying
aged increased to 28 d (Fig. 9c), showing a more significant influ-
ence of drying than steam cured samples. On the contrary, there
was almost no cracking around the steel fiber in the tested speci-
mens associated with steam cured samples. The microcrack can
reduce the hardness of the ITZ as shown in Fig. 8 and consequently
reduce the flexural strength and bond strength (Figs. 5 and 7).
Fig. 10 shows the effects of SAP on the microstructure of the
UHPC matrix around steel fiber at 28 d. The images show that
the interface of fibers and the matrix are dense when SAP was
incorporated in the UHPC samples, independent of the curing
regime. With an analogy of the Figs. 9 and 10, it can be stated that
the micro-cracks were reduced in samples with SAP showing their
effectiveness in internal curing. The BSE results can explain the
working mechanism of SAP as well as its beneficial effects on the
ITZ of steel fiber on the mechanical properties and the restraining
effects on the shrinkage. By comparing Fig. 10a and Fig. 10c, it is
apparent that the small particles of SAP were more effective than
larger ones restraining the propagation of the microcracks in the
regions associated with the ITZ. As shown in Fig. 10b, there are
fewer micro-cracks in the interface of fibers, and the matrix when
the SAP was incorporated in the steam cured UHPC. However, SAP
may be particularly close to or even attach to the steel fiber (as
shown in Fig. 10d), which can impair the bond strength. The large
standard deviation recorded for SS0.6 and SL0.6 in Fig. 8 can
explain the aggravated negative impact of pores on the hardness
and bond strength. If the SAP is not attached to the fiber, the addi-
tion of internal curing water would improve the hydration degree
and be beneficial to the bond strength. However, upon attachment
of SAP to steel fiber, the left SAP pores would reduce the contact
area between the steel fiber and matrix and reduce the bond
strength (SL0.6).
To study the effect of size and content of SAP on the porosity of
ITZ, BSE pictures were analyzed using the Image J analysis tech-
nique, and the porosity of ITZ was captured and calculated in per-
centage. The area around steel fiber was divided into two regions,
annotated as region 1 (0–50 lm) referring to the ITZ of UHPC [38]
and region 2 (50–100 lm) as shown in Fig. 11a. Then, the BSE
images were processed by Image-J software to obtain the his-
togram of grey level [33], as shown in Fig. 11b. From this picture,
the threshold value of pores was estimated. Also, the porosity
was calculated by pores area divided by the total area, as shown
in Fig. 11c.
Fig. 12 shows the calculated porosity of regions 1 and 2 for
UHPC samples with or without SAP at 3 and 28 d. Fig. 12a shows
(R0.18) at 3 and 28 d. At 3 d, the highest porosity of ITZ was
observed in the water cured R0.18.
Besides, a significant difference in porosity between regions 1
and 2 was detected indicating a border in region between the ITZ
and the matrix of about 50 mm, which is consistent with the ITZ
thickness in UHPC [17] and ordinary mortar [39]. This region can
be as high as 100 mm in normal concrete. However, the steam cur-
ing reduced the porosity of regions 1 and 2 by 48.6% and 31.9% at
28 d, respectively, comparing to those cured in water. It shows that
the steam curing significantly reduced the porosity around the
steel fiber, which is consistent with the results of microhardness.
At 28 d, the progressive hydration decreased the porosity of
R0.18. Albeit, the reduction was more significant in the water
cured samples as the great proportion of hydration occurred of
steam-cured samples within the early ages [27]. The results of
compressive strength and flexural strength (Figs. 4 and 5) also
showed that the early-age properties of steam cured UHPC
improved, indicating the occurrence of accelerated hydration. Fur-
thermore, regions 1 and 2 of the water cured UHPC had a distinct
difference in porosity. However, under the steam curing regime,
the difference between regions 1 and 2 was minimal, which means
that the density of the ITZ was more similar to that of bulk paste
and the ITZ of steam cured UHPC is less than 50 lm.
Fig. 12b shows the porosity of ITZ (regions 1 and 2) for samples
with SAP (SS0.6 and SL0.6) at 3 and 28 d. The results show that the
addition of SAP reduced the porosity around steel fibers, especially
for the SS0.6. A reduction of 35.5.% and 27.6% was observed for
regions 1 and 2 at 28 d, respectively, comparing to that of R0.18.
Two mechanisms can be used to explain the densification of ITZ:
the first one is that the addition of SAP increased the hydration
degree of matrix and densified the microstructure; on the other
hand, the addition of SAP reduced shrinkage cracks and increased
the density. Also, the difference between regions 1 and 2 was
insignificant at 28 d. The porosity of ITZ was reduced as the density
of the ITZ was more similar to that of bulk paste. The steam cured
SS0.6 showed the minimum porosity in both regions. Furthermore,
steam curing was effective on samples with large SAP particles
(SL0.6) as its porosity reached the same level to that of SS0.6-S
and R0.18-S at 28 d. It may result from the reduced effect of drying
on the UHPC samples and refrained formation of cracks at the ITZ
of fiber (Fig. 10d). However, the adverse effect of left pores from
SAP can dominate in most cases.
4. Discussion
4.1. Effects of SAP size and content on ITZ
For the performance of SAP in internal curing, the dominant fac-
tor is the dispersion distance of SAP that depends on the content
 J. Liu et al. / Construction and Building Materials 231 (2020) 117142 9

(a) Water cured UHPC at 3 d

(b) Steam cured UHPC at 3 d

Steel
fiber Steel
fiber

(c) Water cured UHPC 28 d (d) Steam cured UHPC at 28 d

Fig. 9. Microstructure of UHPC matrix (R0.18) without SAP at 3 and 28 d.

and particle size of SAP [25]. For UHPC, the water migration dis- which the SAP dispersion may affect the ITZ of fibers and the
tance is considerably less than other conventional concretes due matrix and the associated properties.
to its denser microstructure, which requires SAP to have a shorter Having assumed that all the fibers are identical and homoge-
dispersion distance. On the other hand, despite the beneficial neously distributed, and the fiber diameter and length are df and
restraining effect of SAP on shrinkage [4], the results of this study lf , respectively, for the fiber content b, the fiber spacing Sf is calcu-
showed that incorporation of SAP, especially with large particles, lated by Eq. (2) [40], as follows:
impaired the mechanical properties of UHPC, which is attributed
sffiffiffiffiffiffiffiffiffiffiffiffiffi
to the pores left after the desorption of water from SAP. Dispersion
3 pdf lf
2
of SAP and thereby the left pores can also govern the performance Sf ¼ ð2Þ
of UHPC. Therefore, it is essential to address the mechanism by 4b
10 J. Liu et al. / Construction and Building Materials 231 (2020) 117142

Steel
Steel
fiber
fiber

Steel
fiber

(a) Water cured UHPC (SS0.6) (b) Steam cured UHPC (SS0.6)

Steel
fiber
Steel
fiber

(c) Water cured (SL0.6) (d) Steam cured (SL0.6)

Fig. 10. The microstructure of the UHPC matrix with SAP at 28 d.

with the same assumption for SAP, And considering the average
particle diameter to be ds (measured by laser particle size analyzer),
and the density of UHPC and SAP are qc and qs , when the volume is
Vc , and the SAP content isa(account for binder materials), the distri-
bution spacing of SAP particle could be calculated by Eq. (3).
vffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
p ffiffiffiffiffi u
u Vc  qc  c  a ds
Ss ¼ Vc =t
3 3
¼ qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
qs  6 pd3s 3 6
p  a  c  qqc
s
where c is the percentage of binder materials in UHSC, 47.6%.
In this study, the density of UHPC is 2433 kg/m3, and the den-
sity of SAP is 1310 kg/m3. Therefore, Eq. (3) could be changed into
Eq. (4).
ds
Ss ¼ 0:84 p ffiffiffi
3
a microstructure would lower the compressive strength. What is
Fig. 13 shows that the spacing decreased with the increase of
SAP content. Also, the spacing of SAP distribution is in direct pro-
portion to the diameter of the SAP particle. According to Eq. (2),
the average spacing of steel fiber is 2.73 mm. From the average
data, the spacing of large SAP particles is closer to that of steel
fiber, and the spacing factor of SAP with smaller particles is much
lower than that of steel fiber. From this data, it can be concluded
that at a given content, particles of smaller size are more widely
distributed in the matrix. Fig. 14 shows the schematic distribution
of SAP with two sizes. The small spacing between SAP particle is
beneficial for internal curing as the migration of internal curing
water to the nearest un-hydrated binder particles is facilitated,
especially for UHPC that has a dense microstructure. Also, the area
of possible contact with the steel fiber will be reduced, which is
beneficial for the bonding properties of steel fiber. It explains the
considerable advantage of small particles of SAP on bond strength
and flexural strength over the impaired properties reported for the
samples with large SAP.
ð3Þ
4.2. Effects of size and content of SAP on properties of fiber-reinforced
UHPC
4.2.1. Compressive strength
The compressive strength of UHPC mainly depends on its total
porosity. The addition of SAP increases the hydration degree and
reduces the capillary pores of the UHPC matrix [5,22,41]. However,
the left pores after the desorption of water from the SAP
ð4Þ
more, the incorporation of SAP with large particles can aggravate
this behavior, as shown in Fig. 4. That is to say, the prediction of
the combined effect of SAP on the compressive strength of fiber-
reinforced UHPC is difficult. On the other hand, it should be stated
that the steam curing regime reduced the effects of SAP particle
size on compressive strength of UHPC comparing to those cured
in water with the same duration of curing.
4.2.2. Flexural strength
The flexural strength of UHPC mainly depends on the density of
the ITZ and the bond between the matrix and steel fibers. As shown
in Fig. 15, there is a linear relationship between the flexural
 J. Liu et al. / Construction and Building Materials 231 (2020) 117142 11

Fig. 11. Image analysis process of BSEM picture.

25% 25%
R0.18 at 3d Region 1 Region 1
Region 2 Region 2
20% 20% SL0.6
SS0.6 at 3d
at 3d
15% 15%
Porosity
Porosity

R0.18
at 28d

R0.18-S SS0.6 SL0.6

10% 10% at 28d
at 3d R0.18-S at 28d SL0.6-S
SS0.6-S
at 28d at 28d at 28d

5% 5%

0% 0%
(a) without SAP (b) with SAP
Fig. 12. Porosity of ITZ of fibers in UHPC.

strength and bond strength for samples with and without SAP. It
means that bond strength is a decisive factor of the flexural
strength. SAP acted as internal curing material, reduced the shrink-
age [5,41], and lowered the occurrence of associated micro-
cracking of UHPC. The addition of SAP also improved the hydration
degree, evident from the result of microhardness and porosity
around the steel fibers. The reduced micro-cracking and improved
hydration degree densified the ITZ and enhanced the bond strength
and flexural strength of UHPC. This behavior was reflected in the
higher flexural strength of SS0.3 at 28 d. However, the left pore
can compromise the beneficial effect of SAP and weaken the ITZ.
This effect increased with the increase of SAP content and SAP par-
ticle size, which was reflected from the lowest strength obtained
by SL0.6. Another mechanism other than the pores after desorption
of water that can weaken the ITZ is the probability of attachment of
some SAP to steel fibers. The attached SAP can significantly reduce
the contact area between steel fiber and matrix and reduce bond
strength and flexural strength.
It should be mentioned that the addition of SAP increased flex-
ural to compressive strength ratio compared with Reference UHPC,
as shown in Table 4, especially for water cured UHPC sample. It
means that the internal curing of SAP is more beneficial for the
development of flexural strength than compressive strength. This
is consistent with the relationship between flexural strength and
bond strength of steel fiber. Generally, when micro-cracks propa-
gate through paste due to load, steel fibers can bridge the micro-
cracks. The addition of small SAP could reduce micro-cracks under
drying conditions and increase interfcial bonding strength of steel
12 J. Liu et al. / Construction and Building Materials 231 (2020) 117142

2500 compressive strength to a level higher than that of the reference

d
S = 0.84 3 mixtures with w/b of 0.22, indicating the beneficial effect of
Spacing of SAP, ds (μm)

2000 internal curing on strength development of UHPC. In general,

SL-0.3,
1613.3μm
a higher content or a larger particle size SAP aggravated the
SL-0.6, SL adverse effects of SAP that can be related to the left pores from
1500 1280.5μm Particle size of
277.2 μm desorption of water from SAP. On the other hand, the calcula-
tion of distribution spacing of SAP particles showed that the
1000
large SAP had a higher disperse distance, which was not benefi-
cial for UHPC.
SS-0.3, SS-0.6,
500 SS
For steam cured UHPC, results showed that a short-term steam
288.6μm 229.1μm Partice size of 49.6μm
curing regime increased the compressive and flexural strength.
0 Besides, the steam curing partly compensated the effect of size
0.1 0.3 0.5 0.7 0.9 and content of SAP on mechanical properties. The SAP-
Content of SAP, α (%) containing UHPC samples had a compressive and flexural
strength between R0.18 and R0.22, except for those that incor-
Fig. 13. Calculated spacing of SAP in UHPC.
porated high content of large SAP (SL0.6). The combination of
steam curing and internal curing by small SAP led to fewer
fibers. This is one of critical factors contributing to increasing flex- micro-cracks of fiber-reinforced UHPC.
ural to compressive ratio.

5. Conclusion
30
Based on the above experimental results and discussion, the fol-
lowing concluding remarks can be withdrawn: Flexural strength (MPa) 28

The addition of SAP to UHPC affected the ITZ of steel fiber in two
fashions: (i) The internal curing of SAP densified the ITZ of steel 26
fiber (increased micro-hardness and reduced porosity), and
reduced the micro-cracking of the UHPC matrix upon drying:
(ii), the left pores from SAP led to some adverse effects on ITZ 24
properties. These two effects were governed by the particle size
and content of SAP, and curing regime of UHPC, which resulted
in variations in the properties UHPC, namely, compressive 22 y=18.95+1.09*x, r2=0.90
strength and flexural strength.

For water cured UHPC, the incorporation of low content of SAP
with small particles (0.3%) increased the flexural strength of 20
UHPC because of the internal curing provided by SAP. The addi- 4 5 6 7 8 9 10
tion of SAP, though, reduced the compressive strength of UHPC Bond strength (MPa)
at all ages when compared to the reference mixtures with w/b
of 0.18. However, SAP with small particles improved the Fig. 15. Relationship between flexural strength and bond strength.

Fig. 14. Distribution of small and large SAP under some content in the UHPC matrix.
 J. Liu et al. / Construction and Building Materials 231 (2020) 117142 13

Table 4
Effect of SAP on the flexural to compressive strength ratio of UHPC.

R0.18 R0.22 SS0.3 SS0.6 SL0.3 SL0.6 R0.18-S R.22-S SS0.3-S SS0.6-S SL0.3-S SL0.6-S
3d 0.199 0.244 0.243 0.258 0.256 0.247 0.163 0.162 0.171 0.170 0.166 0.159
28 d 0.163 0.178 0.176 0.199 0.181 0.203 0.162 0.166 0.166 0.168 0.162 0.164
56 d 0.168 0.164 0.188 0.192 0.181 0.184 0.164 0.167 0.171 0.174 0.167 0.166

[16] G.L. Golewski, Determination of fracture toughness in concretes containing

Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
Acknowledgment
The authors gratefully acknowledge the financial support from
the Ministry of Science and Technology under Project No.
2018YFC0705400 and the National Science Foundation of China
under Project Nos. U1305243 and 51378196. The first author also
gratefully acknowledges the financial support from the program
of China Scholarships Council (No. 201806130109).
Appendix A. Supplementary data
Supplementary data to this article can be found online at
https://doi.org/10.1016/j.conbuildmat.2019.117142.
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