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Abstract
In order to investigate the self-healing capability of fibre reinforced cementitious composites (FRCC), mechanical
properties and surface morphology of crack in FRCC were studied. Three types of FRCC specimens containing (1)
polyethylene (PE) fibre, (2) steel cord (SC) fibre, and (3) hybrid fibres composite (both of PE and SC) were prepared.
These specimens, in which cracks were introduced by tension test, were retained in water for 28 days. The self-healing
capability of the specimens was investigated by means of microscope observation, water permeability test, tension test
and backscattered electron image analysis. It was found that many very fine fibres of PE were bridging over the crack and
crystallization products became easy to be attached to a large number of PE fibres. As a result, water permeability coef-
ficient decreased and tensile strength was improved significantly. Therefore amount of the PE fibre per volume was
indicated to have a great influence on self-healing. Furthermore, by means of backscattered electron image analysis, it
was also shown that the difference of hydration degree in each FRCC has only little influence on the self-healing capa-
bility in case of the employed test series.
that the growth rate of calcium carbonate within the Table 1 Employed materials in this study.
crack was dependent on crack width and water pressure, High-early-strength
but that it was independent of concrete composition Cement ρ = 3.14 g/cc
Portland cement
(type of cement and aggregate) and type of water (i.e. ρ = 2.61 g/cc
hardness of water). On the other hand, Granger et al. Aggregate Silica sand (no.7)
Diameter: 180μm
(2007) carried out an experimental program of me- Mixing ρ = 2.2 g/cc
chanical test on ultra high performance concrete and Silica fume
Materials Diameter: 0.15μm
concluded that the self-healing of the pre-existing crack Viscous Water-soluble
was mainly due to hydration of anhydrous clinker on the ρ = 1.1 g/cc
Agent cellulose
crack surface and that the stiffness of newly formed Polyethylene (PE) Mentioned below
crystals is close to that of primary C-S-H. While there Fiber
Steel cord (SC) Mentioned below
are many studies of self-healing of concrete, there are Nominal diameter:
quite few of such studies on FRCC. Li et al. (1998) car- Screw Bar Steel screw bar
6mm (M6)
ried out experimental studies on self-healing capability
of SHCC and concluded that self-healing of the induced
micro cracks was observed not only by formation of a
distinct deposit inside the cracks but also by almost
complete recovery of the pre-cracking stiffness. Homma
et al. (2008a, 2008b) reported the summary of a series
of experimental study on the self-healing capability of
FRCC.
In this paper, the experimental study of the FRCC’s
self-healing capability is reported. The capability is PE fiber (length=6mm) SC fiber (length=32mm)
evaluated by water permeability test, microscope meas-
urement, tension test and backscattered electron image. Tensile
Types of Length Diameter Modulus Density
strength
Fiber (mm) (mm) (GPa) (g/cc)
(MPa)
2. Self-healing
PE fiber 6 0.012 73 2580 0.97
Self-healing is the natural process of crack repair that can SC fiber 32 0.4 200 2850 7.84
occur in concrete in the presence of moisture. The depo-
sition of calcium carbonate is said to be generated ac-
cording to the following reactions (Edvardsen 1999). Table 2 Mix proportion of FRCC specimens investigated
+
H2O + CO2 ⇔ H2CO3 ⇔ H + HCO3 ⇔ 2H + CO 3 (1)
- + 2- in this paper.
Silica fiber
Types of Water/ Sand/ SP/ PE fiber SC fiber
fume/ content
Ca 2+ + CO 3 2- ⇔ CaCO 3 (pHwater>8) (2)
Mix Binder Binder
Binder
Binder (Vol. %) (Vol. %)
(piece/m3)
FRCC(SC) - - 0.75 187×104
Ca 2+ + HCO3 - ⇔ CaCO3 + H + (7.5 < pHwater < 8) (3) FRCC(PE) 0.45 0.45 0.15 1.5 - 221×108
0.09
HFRCC 0.75 0.75 111×108
The carbon dioxide CO2 in the air is dissolved in water Note: Binder = Cement + Silica fume; SP = Superplasticizer (Polycarboxylate)
and the calcium ion Ca2+ is derived from concrete.
These CO2 and Ca2+ are combined with each other to Types of Mix
Table flow
(cm×cm)
Air content (%)
produce calcium carbonate crystals. Then the calcium
FRCC(SC) 16.3×16.0 0.90
carbonate crystallization made in this way is attached to
FRCC(PE) 13.6 ×13.8 5.13
crack surface and fibers. As a result, crack width is re-
HFRCC 14.7×14.7 3.36
duced and after a certain time the crack is repaired.
3. Experimental procedure
composite: HFRCC).
In this study, the self-healing capability is evaluated by In all series, four specimens of 25×75×75[mm] were
the microscope observation, water permeability test, prepared. After standard curing for one week, cracks
tension test and backscattered electron image analysis. were introduced in each specimen by means of a
Table 1 shows the employed materials and Table 2 uni-axial tension test. Figure 1 shows the outline of the
shows the mix proportions together with the fresh prop- tension test. During this test, each specimen was
erty. In this study three types of FRCC were studied: (1) stretched to different strain levels in order to have dif-
containing micro polyethylene fibre (φ=12µm, ferent maximum crack width. In Fig. 2, the relations
length=6mm) (FRCC(PE)), (2) containing steel cord between elongation and stress under uni-axial tension are
fibre (φ=0.4mm, length=32mm) (FRCC(SC)), and (3) shown. The nonlinearity is corresponding to the accu-
containing both of PE and SC fibres (i.e. hybrid fibre mulation of multiple cracking. After the tension test, the
D. Homma, H. Mihashi and T. Nishiwaki / Journal of Advanced Concrete Technology Vol. 7, No. 2, 217-228, 2009 219
3.5 MORTAR1
Screw bar (M6)
MORTAR2
3
2.5
Stress [MPa]
Fixing nut
2
1.5
0.5
0
0 0.5 1 1.5 2 2.5 3
Elongation[mm]
MORTAR
4
3.5 FRCC(SC)1
Fig. 1 Test set-up of uni-axial tension test. FRCC(SC)2
3
FRCC(SC)3
2.5 FRCC(SC)4
Stress [MPa]
2
Pipette
1.5
Distilled Water 1
0.5
0
Plexiglas 0 0.5 1 1.5 2 2.5 3
Elongation[mm]
Plate specimen
FRCC(SC)
4
3.5 FRCC(PE)1
Rubber tube FRCC(PE)2
3
FRCC(PE)3
2.5 FRCC(PE)4
Stress [MPa]
2
Screw bar
1.5
1
Fig. 3 Schematic description of water permeability test. 0.5
0
0 0.5 1 1.5 2 2.5 3
Table 3 Maximum crack width evaluated by means of Elongation[mm]
0.5
crack surface was observed by means of a digital mi- 0
croscope and the crack width was measured as shown in 0 0.5 1 1.5 2 2.5 3
Table 3. These values were obtained on the inlet side of Elongation [mm]
(Nishiwaki and Mihashi 2003) is shown in Fig. 3. The deposition of crystallization products was not seen. Even
water permeability coefficient was evaluated by the wa- if there were fibres bridging the crack, in the case when
ter flow speed through the plate specimen. After the crack width was too wide and PE fibres were dropped out,
water permeability test, all specimens were kept for 28 little attachments of the crystallization products could be
days in water tank of 20ºC which is usually used for confirmed. After 3 days, in FRCC(PE) and HFRCC, the
standard curing. In order to investigate the effect of the thickness of crystallization products attached to the crack
self-healing of crack, water permeability tests and mi- surface and PE fibres increased as the time advanced.
croscopic measurement were conducted again at 3, 14 However, in FRCC(SC), the crack surface remained to be
and 28 days. After 28 days, the uni-axial tension test was clear. Therefore it can be concluded that amount of the
performed again, too. PE fibres per volume has a great influence on the
self-healing.
4. Experimental Results and Discussion After 3 days, it was also observed that steel cords on
the crack surface in FRCC(SC) and HFRCC corroded
4.1 Microscopic observation and the volume expanded.
The formation of crystallization products (Fig. 4) that Figure 5 shows the time dependence of mean thick-
might be the source of self-healing was monitored just ness of the crystallization products attached to the crack
after the tension test and at the end of 3, 14, and 28 days surface (summation of products thickness on both sides
after water permeability test. Additionally the thickness of the crack surface). The increasing rate of the mean
of the crystallization products on the crack surface was thickness during the first 3 days is higher than that after 3
also measured by means of a digital microscope. Table 4 days. This could be because Ca2+ diffusion speed from
shows the typical crack surface photographs in FRCC the inside of FRCC was reduced as the time advanced
(PE), FRCC (SC), and HFRCC at the elapsed time of 0 since the formation of the crystallization product layer
day (immediately after tension test and before immersion may prevent the diffusion (Edvardsen 1999). Order of the
in water), at 3 days, 14 days and 28 days. amount of the attached products in each FRCC material
The reason why some values of the maximum crack was FRCC(SC) < HFRCC < FRCC (PE). This order is
width are different from ones shown in Table 3 is that not corresponding to that of the piece number of mixed fibres
only the inlet side for water permeability test but both per unit volume shown in Table 2 (i.e. FRCC(SC) <
sides of each specimen were observed by the digital HFRCC < FRCC (PE)). Therefore it can be concluded
microscope for measuring the crack width and the thick- that the piece number of mixed fibre per unit volume has
ness of crystallization products. It can be clearly seen in the dominant influence on the thickness of the crystalli-
Table 4 that the crack surface of all specimens immedi- zation products attached to the crack surface.
ately after tension test is clear and there are no chemical Figure 6 shows the relationship between the maxi-
products on the surface. At 3 days, however, in the crack mum crack width and the mean attachment thickness at
surfaces of FRCC(PE) and HFRCC, many crystallization 28 days. In each type of mix, totally 8 data of the maxi-
products were confirmed to be attached and this attach- mum crack width measured from both sides of each
ment is done not only to crack surface but also to many specimen are plotted. In this figure, when the slope of
PE fibres. Furthermore in FRCC(PE), even though crack regression line equals to 1, the attachment thickness is
width reached 100μm, crack was confirmed to be re- thought to reach the crack width and it can be said that
paired by the crystallization products attached to many the crack was repaired. According to the results shown in
fibres bridging the crack. However in the place of little this figure, when crack width is less than 100μm, the
fibre bridging, especially in almost all FRCC(SC), the
120
Mean thickness of cristallization
FRCC(SC)
100 FRCC(PE)
HFRCC
80
products[μm]
60
40
20
0
0 5 10 15 20 25 30
Time [days]
300 600
(a)
Attachment thickness [μm]
y=x (b)
250 FRCC(SC) 500
FRCC(PE) FRCC(PE)
200 400 y = 0.3673x
HFRCC
50 100 FRCC(SC)
y = 0.0287x
0 0
0 200 400 600 800 0 1000 2000 3000 4000
Crack width [μm] Crack width [μm]
(a) (b)
Fig. 6 Relationship between the maximum crack width and the mean thickness of crystallization products observed on
each specimens surface .
slope was close to 1 and crack was repaired easily in each applied. Darcy’s law states:
series. However, when crack width is wider than 100μm,
the slopes of the regression lines are much lower than 1. h (1)
Q = kA
Among these three regression lines shown in Fig. 6(b), l
the slope of FRCC(PE) is highest. It confirms that where Q = the flow rate through the specimen (dV/dt); V
FRCC(PE) is repaired most easily.
= the total volume of water that travels through the
sample; k = the water permeability coefficient and the
4.2 Water permeability test
parameter under this study, l = the thickness of the
The water permeability coefficient was calculated as
specimen, and A = the surface area of the plate specimen.
follows. Since the water flow in this study is assumed to
Then, because the flow is continuous, the amount of
be continuous through the laminar, Darcy’s law can be
222 D. Homma, H. Mihashi and T. Nishiwaki / Journal of Advanced Concrete Technology Vol. 7, No. 2, 217-228, 2009
Water permeability
Permeability
dV ⎛ dh ⎞ 1.E-05
= − A' ⎜ ⎟
dt ⎝ dt ⎠ (2)
1.E-06
1.E-07
of water
[m/s]
where dh/dt= the differential of pressure between the 1.E-08
initial pressure head h0 and the remaining pressure head FRCC(SC)
Coef ficient of
1.E-09
h1 at the measured time t; A’ = the cross-sectional area of
Coefficient
FRCC(PE)
the pipe. 1.E-10
HFRCC
By combining Equations (1) and (2), Equation (3) is 1.E-11
obtained. 1.E-12
0 0.5 1 1.5 2
h A' dh
k A=− Residual elongation [mm]
l dt (3)
Fig. 7 Relationship between the coefficient of water
By integrating Equation (3), Equation (4) is obtained. permeability and residual elongation.
t h
A' 1 dh
k ∫ dt = −l
A h∫0 h
FRCC(SC) HFRCC FRCC(PE)
0
(4) 1.E-04
Waterpermeability
Permeability 1.E-05
The water permeability coefficient is finally given by
Equation (5). 1.E-06
1.E-07
A' h0
k =l ln
[m/s]
Coef ficientofofwater
1.E-08
At h1 (5) 1.E-09
FRCC(SC)
By the use of this coefficient of water permeability, the
Coefficient
1.E-10 FRCC(PE)
self-healing capability of each FRCC was evaluated. 1.E-11 HFRCC
Figure 7 shows the relationship between the coeffi-
1.E-12
cient of water permeability and residual elongation just
0 0.2 0.4 0.6 0.8
after the tension test. The coefficient of water perme-
The maximum crack width [mm]
ability tends to increase as residual elongation increases,
but this tendency is quite variable and dependent on the Fig. 8 Relationship between the coefficient of water
type of fibre. This could be because the residual elonga- permeability and the maximum crack width.
tion doesn’t indicate the maximum crack width but re-
flects the summation of crack widths and fibre reinforced
cementitious composites make multiple cracking gener- 125
ated. FRCC(SC)
Mean attachment width [μm]
coefficient of smoothness a
aIAg 3
k= w
12v (6) Fig. 9 Relationship between the coefficient of smooth-
ness and mean attachment thickness.
where w:crack width [mm]; a:flow rate coefficient
indicating smoothness of crack surface ( 0 < a ≤ 1 ) to
estimate the influence of the crack geometry ; I : pressure From Equation (6), the coefficient of water perme-
gradient (h/d) ; h : height of fluid column on the inlet ability is proportional to cube of crack width: w and the
side ; d : length of crack in flow direction ; v : kinematic coefficient a. The result of Fig. 8 is corresponding to this
viscosity [m2/s]; g : gravity acceleration. l : length of theory basically. This tendency, however, also has vari-
crack at a right angle to the flow direction [m]. ability in the small range of the maximum crack width
D. Homma, H. Mihashi and T. Nishiwaki / Journal of Advanced Concrete Technology Vol. 7, No. 2, 217-228, 2009 223
Water permeability
permeability
Permeability
Water permeability
Water Permeability
Permeability
Uncracked Uncracked Uncracked
1.E-05 1.E-05 1.E-05
No.1 0.035mm No.1 0.019mm No.1 0.017mm
1.E-06 No.2 0.076mm 1.E-06 No.2 0.038mm 1.E-06 No.2 0.081mm
No.3 0.088mm No.3 0.119mm No.3 0.407mm
1.E-07 No.4 0.757mm 1.E-07 No.4 0.368mm 1.E-07 No.4 0.710mm
[m/s]
Coefficientofofwater
of water
[m/s]
Coefficientofofwater
[m/s]
1.E-08 1.E-08 1.E-08
Coefficientof
Coefficient
Coefficient
Coefficient
1.E-10 1.E-10 1.E-10
Permeability
the range where elongation is small. This is because fibre FRCC(SC)3 w=0.088
Waterpermeability
1.E-05
reinforced cementitious composites generically make 1.E-06 FRCC(PE)3 w=0.119
multiple crack in the range of small elongation. HFRCC2 w=0.081
Figure 9 shows the relationship between the coeffi- 1.E-07
[m/s]
cient indicating the smoothness of crack surface and
ofwater
1.E-08
attachment thickness at 28 days. From this figure, it was
1.E-09
Coefficientof
50000
[Counts]
50000
CaCO3 CaCO3
30000
30000
C ou n ts
10000
10000
Pure Calcium
CaCO3 Carbonate sample
CaCO3
00 CaCO3 CaCO3
4 4 4
3.5 3.5 3.5
Before Self-healing Before Self-healing Before Self-healing
Tensile stress [MPa]
After Self-healing
Tensile stress [MPa]
3 3 After Self-healing 3 After Self-healing
2.5 2.5 2.5
2 2 2
1.5 1.5 1.5
1 1 1
0.5 0.5 0.5
0 0 0
0 1 2 3 4 5 6 0 1 2 3 4 5 6 0 1 2 3 4 5 6
Elongation [mm] Elongation [mm] Elongation [mm]
Fig. 13 Comparison of tensile property of specimens before and after 28 days of self-healing.
response of FRCC. In case of FRCC(PE), specimens This is because FRCC (SC) didn’t contain any polyeth-
showed a tendency of quasi-brittle fracture because ylene fibres. In case of FRCC (SC), some specimens
the length of the used polyethylene fibres was short. showed multiple cracking in a small strain range but the
After the first crack occurred, tensile stress soon de- others didn’t. While there was a scatter in the cracking
creased accompanying the strain softening behaviour. behaviour in the small strain range, a dominant crack was
Multiple cracking was observed in the range of small easily localized in any cases.
strain, though a dominant crack was localized as the In order to compare the strength recovery due to the
strain increased. In case of HFRCC, the length of steel self-healing of each FRCC specimen, the strength re-
cord had the concavity and convexity to create the high covery rate (c) was defined as follows:
bond strength while the short polyethylene fibres made
the matrix tough enough to prevent the spalling of matrix σ 2 −σ 0
c= ×100
when the steel cord was pulled out from the crack surface σ 1 −σ 0 (6)
(Mihashi and Kohno 2007). As a result, HFRCC showed
a very ductile stress versus elongation relation. Multiple where σ0 = the stress at the unloading in the first tension
cracking was observed but finally a dominant crack was test, σ1 = the tensile strength in the first tension test, and
localized as observed in FRCC (PE). FRCC (SC) σ2 = the tensile strength after the self-healing.
specimens which contained only steel cord showed lower By use of this c, it can be possible to judge the recov-
strength and a little less ductility than those of HFRCC. ering capability of the strength in each FRCC as follows.
D. Homma, H. Mihashi and T. Nishiwaki / Journal of Advanced Concrete Technology Vol. 7, No. 2, 217-228, 2009 225
[MPa]
350
Stress[MPa]
σ1
σ2 HFRCC Perfect
σ0 After self-healing 200 recovery
Tensile
150
100
50 recovery
0
Residual 0 0.5 1 1.5 2 2.5 Deterioration
Elongation [mm] -50
Elongation
First tension test (FRCC) Residual elongation [mm]
Second tension test (self-healing FRCC)
Fig. 15 Relationship between recovery rate and residual
Fig. 14 Schematic of the relationship between tensile elongation.
stress and tensile elongation of FRCC.
Corrosion Corrosion
If c is over 100, this specimen can be considered to be Figure 16 shows a comparison of crack surfaces after
recovered perfectly. If c is over 0 and under 100, this one the second tension test. By observing the crack surface, it
was recovered a little. If c is equal to 0, this one was not was confirmed that corrosion of steel cord was observed
recovered. If c is under 0, this one was deteriorated. not only on the surface of specimens with crack but also
Figure 15 shows the relationship between the strength on the surface of inside of the crack in case of FRCC
recovery rate c and residual elongation in each FRCC (SC). In case of HFRCC, however, the corroded steel
material. It can be seen in Fig. 15 that after 28 days the fibre was observed only on the surface of the specimen
recovery rate of the FRCC (SC) was almost zero or even (i.e. the external surface of the crack) but it was not ob-
minus. This could be because the self-healing products served on the internal surface of the crack. This could be
were not attached to the crack surface and steel cords because in HFRCC a lot of calcium carbonate crystals
were corroded during 28 days. not only covered the surface of the crack but also at-
In the case of FRCC (PE), the recovery rate c is plotted tached to the matrix around steel cord fibres. It corre-
over 0 and under 100. The tensile strength after sponds to the increase of tensile strength of HFRCC after
self-healing didn’t reach the first tensile strength, but the self-healing.
could reach the first unloading stress. This could be be-
cause a lot of calcium carbonate crystals attached to 4.5 The measurement of hydration degree
many fibres. This indicated that, if the calcium carbonate In order to make sure whether this difference of tensile
crystals attach to the crack surface, the tensile strength strength healing is due only to the crystallization of
after self-healing can be recoverable. Moreover it can calcium carbonate or the difference of the hydration
also be seen in Fig. 15 that the strength recovery rate degree of each FRCC has any effects on the difference of
becomes higher as residual elongation is smaller. tensile strength healing, the hydration degree of each
In the case of HFRCC, the recovery rate was higher FRCC was measured. The measurement of hydration
than 100 when the residual elongation was less than even degree was done by mean of the backscattered electron
2mm. It means that the tensile strength after self-healing image (Igarashi et al. 2004) as shown in Fig. 17. The
could reach not only the first unloading stress, but also backscattered electron image was converted to a binary
the first tensile strength. This could be because, as well as image on each divided constituent phase and the volume
FRCC (PE), a lot of calcium carbonate crystals attached fraction of the constituent phase was measured. By use of
to crack surface with very fine fibres. Moreover the bond this volume fraction, the hydration degree of FRCC was
property of the steel cord damaged by pull out stress calculated as follows.
might be recovered by the self-healing products.
226 D. Homma, H. Mihashi and T. Nishiwaki / Journal of Advanced Concrete Technology Vol. 7, No. 2, 217-228, 2009
Sand Pores
Unhydrated
+
cement
Others
Pores, Sand
+
Others
Duotone
Others
Pore
+
Unhydreted
Backscattered Electron Image cement
Binarized Image
Fig. 17 Backscattered electron image of FRCC(PE).
Volume f ractions of constituent phases
5. Conclusions
UH i
α =1− (7)
UH 0 This paper presented some results of an experimental
study on the self-healing capability of the fibre rein-
where UHi is area fraction of unhydrated cement particle forced cementitious composites. Based on the experi-
at the age of ti; UH0 is the initial area fraction of unhy- mental study, the following conclusions were obtained:
drated cement particles. 1) Self-healing of cracks in FRCC materials was con-
In Fig. 18, volume fractions of constituent phases and firmed.
the hydration degrees in each FRCC specimen are shown. 2) In the case of FRCC containing a lot of very fine
The hydration degree of each FRCC shows about 65% fibres such as polyethylene, the formation of
and there was no change in the hydration degree of each self-healing products becomes easy to be attached
FRCC. Therefore it could be shown that the influence of to the crack surface due to the tight space between
the hydration degree difference of each FRCC on the fibres.
tensile strength healing was little. It means that the 3) The self-healing products were confirmed to be
dominant source of the self-healing is the crystallization calcium carbonate crystals by means of raman
of calcium carbonate. spectroscopy analysis.
D. Homma, H. Mihashi and T. Nishiwaki / Journal of Advanced Concrete Technology Vol. 7, No. 2, 217-228, 2009 227
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Yang, Y.-Z., Lepech, M. D. and Li, V. C. (2005). China, F. H. Wittmann et al. (eds.) 231-241.
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