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highlights
● The moisture exchange has significant influence on the cement hydration and microstructure of interfaces in concrete repairs.
● The interface is of higher porosity than the repair material.
● The microstructure has a significant influence on the bond strength of the interfaces.
articleinfo Resumen
Article history: Uno de los parámetros clave para la realización de reparaciones de hormigón es la calidad de la interfaz entre
Received 28 August 2014 el material de reparación y el sustrato de hormigón. Para comprender las propiedades de la interfaz en
Received in revised form 15 February 2016 reparaciones de concreto con materiales de reparación cementosos, la hidratación del cemento y la
Accepted 25 February 2016 microestructura se estudiaron experimentalmente mediante prueba de agua no evaporable, porosimetría de
intrusión de mercurio y técnicas de microscopía electrónica de barrido. Los resultados experimentales revelan
que el intercambio de humedad entre el material de reparación y el sustrato de concreto da como resultado un
Keywords: cambio del contenido de humedad en el material de reparación y, por lo tanto, afecta el proceso de hidratac ión
Concrete repairs del cemento y el desarrollo de la estructura de poro. Las imágenes de electrones retrodispersados demuestran
Interface la existencia de una zona de transición interfacial de alta porosidad, ya que las partículas de cemento del
Cement hydration material de reparación tienen un empaque pobre en la superficie del sustrato de concreto.© 2016 Elsevier Ltd.
Microstructure All rights reserved.
http://dx.doi.org/10.1016/j.conbuildmat.2016.02.203
0950-0618/© 2016 Elsevier Ltd. All rights reserved.
766 J. Zhou et al. / Construction and Building Materials 112 (2016) 765–772
Tape
Substrate
(a) (b)
PVC
(c) (d)
Fig. 1. Preparation of the concrete substrate for casting the repair material.
25 25
55 Concrete
substrate
2.1. Non-evaporable water test value of 200 MPa. The mercury intrusion volume at every pressure step was
recorded. The measurement was carried out with 125 pressure steps ranging from
Powers and Brownyard [22] suggested that the degree of hydration of cement 0.004 MPa to 200 MPa in logarithmic distribution. The equilibrating time for every
paste is proportional to the non-evaporable water content. Consequently, the step was 30 s.
degree of hydration was often studied by measuring the non-evaporable water con- Assuming that all pores in samples can be filled by mercury at the maximum
tent [23,24]. In this study, this method was used to investigate the cement hydra- pressure, the pore volume Vpore is equal to the total mercury intrusion volume
tion of the repair material. Vintrusion. The porosity / can be calculated by dividing the total mercury intrusion
The powder sample was further dried at a temperature of 105 °C for 24 h to volume by the bulk volume of the sample Vsample:
remove the evaporable water. Simultaneously, the crucibles were dried in a furnace Vintrusion
at a temperature of 1000 °C for 2 h, and the weight of the crucibles W1 was mea- /¼ ð5Þ
V sample
sured. Around 1.1 g powder (W2 ) was added into the crucibles. The crucibles were
then placed in a furnace at a temperature of 1000 °C for 3 h to remove the non- The bulk volume of the sample can be calculated:
evaporable water. The weight of the crucibles with the sample was measured and
recorded as W3. Three parallel measurements were done. The non-evaporable water Wmercury
Vsample ¼ Vpen — ð6Þ
content wn per gram of the cement can be calculated as: qmercury
W1 þ W2 — W3 ð2Þ where Vpen is the volume of penetrometer and qmercury is the density of mercury.
wn¼
W 3 — W1
2.7. SEM and BSE image analysis
The degree of hydration a can be calculated by dividing the measured non-
evaporable water content by the maximum non-evaporable water content at com-
BSE mode was selected for SEM study, since it allows to quantitatively deter-
plete hydration wn,max:
mine by image analysis the major phases in hardened Portland cement paste,
wn i.e. pore, hydration products and unhydrated cement. The BSE image acquisition
a¼ ð3Þ
was conducted using an environmental-SEM. The acceleration voltage of 20 kV
wn;max
was used. The spot size was 4.0 nm and the magnification was 500×. The working
The maximum non-evaporable water content at complete hydration is a cement distance was 10 mm. The pressure inside the chamber was set at 0.5 Torr.
composition dependent parameter. According to Copeland et al. [25], this value can A typical BSE image of hardened Portland cement paste is given in Fig. 3(a).
be calculated as follows: Pores, hydration products and unhydrated cement can be distinguished by their
wn;max ¼ wC 3 S × ðC 3 SÞ þ wC 2 S × ðC 2 SÞ þ wC 3 A × ðC 3 AÞ þ wC 4 AF × ðC 4 AFÞ ð4Þ gray levels as shown in Fig. 3(b). The hydration products appear gray, and the unhy-
drated cement particles appear light gray. Since the pores are filled with epoxy,
where wC3S, wC2S, wC3A and wC4AF are the non-evaporable water contents of the four which has a low backscattering contrast, porosity appears black. Air voids, which
major mineral phases of Portland cement given in Table 3. (C3 S) (C2S) (C3 A) and appear large black dots, were present in very few images, and they were eliminated
(C4 AF) are the contents of the four major mineral phases in Portland cement CEM I in image analysis. Area fraction of each phase can be determined by counting the
42.5N, which is given in Table 3. The calculated non-evaporable water content of number of the pixels of the corresponding area. According to the stereology theory
the Portland cement CEM I 42.5 at complete hydration is 0.225 g/g. [26,27], the three-dimensional information of microstructure can be derived from
BSE images, by assuming that the volume fraction of each phase is equal to their
area fraction in the BSE images. Consequently, porosity and degree of hydration
2.6. MIP
can be calculated, which is described in details in the following paragraphs. In order
to ensure 95% accuracy, more than 12 images taken in each specimen were used in
MIP is one of the most popular methods used to investigate the pore structure
the BSE image analysis [28].
of cementitious materials, which can provide a valid measurement of total porosity.
Since pores and unhydrated cement can easily be distinguished from the other
The test procedure is described as follows. The weight of the freeze-dried samples
phases, their pixels were first counted. The number of the pixels of hydration
was measured and recorded as Wsample . The freeze-dried samples were put into a
products nhp [–] was calculated by subtracting the number of the pixels of porosity
penetrometer closed with a steel cap. After the weight of the penetrometer with
npore [–] and unhydrated cement nuc [–] from the total number of the pixels of the
the samples Wsample + Wpen was measured, it was placed in the low-pressure cham-
BSE image ntotal [–].
ber. The chamber was evacuated to a pressure of 50 lmHg, and mercury filled the
penetrometer. Pressure was gradually increased from 0.004 MPa to 0.15 MPa. The nhp ¼ ntotal — npore — nuc ð7Þ
penetrometer was removed from the low-pressure chamber, and its weight
Wsample + Wpen + Wmercury was measured. The penetrometer was then placed in the The porosity / can be calculated by dividing the pixels of the pores by the total
high-pressure chamber, and pressure was gradually increased to the maximum pixels:
npore
/¼ ð8Þ
Table 3 ntotal
Non-evaporable water contents of the four major mineral phases of Portland cement
According to Powers’ model [22], the hydration products have a volume
[8] and the contents of the four major mineral phases in the Portland cement CEM I
2.1 times larger than that of the hydrated cement particles. Therefore, the equiva-
42.5N.
lent pixels of the hydrated cement nhc [–] holds:
Mineral phase Non-evaporable water content [g/g] Weight [%] nhp
nhc ¼ ð9Þ
C3S 0.187 65.8 2:1
C2S 0.158 14.8 The degree of hydration a can be calculated by dividing the pixel of the
C3A 0.665 8.3 hydrated cement particles by the total pixels of the cement particles before
C4AF 0.213 11.1 hydration:
Pore HP UC
Pore
HP
UC
where qw is the density of water (1 g/cm3) and qce is the density of Portland cement
(3.15 g/cm3). 3.3. Microstructure of the interface
25 25
20 20
Unsaturated Saturated
60 concrete concrete
substrate substrate
Fig. 5. Degree of hydration of the reference and the repair material at the age of 28 days obtained from non -evaporable water test (dimension in mm).
770 J. Zhou et al. / Construction and Building Materials 112 (2016) 765–772
25 25
20 20
Unsaturated Saturated
60 concrete concrete
substrate substrate
R S R S
Fig. 7. BSE images of the interface between the repair material (R) and the concrete substrate (S) at the age of 28 days.
Table 4
Degree of hydration a, porosity / and w/c ratio x in the interfacial transition zone and in the middle layer of the repair material at 28 days obtained from the BSE image analysis.
interfacial transition zone is 46%–53% higher than that in the repair porosities obtained from accounting the pixels in Eqs. (7)–(11),
material. The porosity in the interfacial transition zone is 81% to correct the estimation of the w/c ratio in BSE image analysis.
higher than that in the repair material. The experimental results The w/c ratio of the repair material on the saturated concrete sub-
also revealed that the high moisture content in the concrete sub- strate becomes 0.398, which agrees the expected value of 0.4. The
strates results in higher porosity, higher degree of hydration and w/c ratio of the repair material on the unsaturated substrate
higher w/c ratio in both the repair material and the interfacial tran- becomes 0.359. This reveals that the water absorption of the unsat-
sition zone. This is in a good agreement with the experimental urated substrate causes a 10% reduction of the w/c ratio of the
results of non-evaporable water test and MIP. repair material in this study.
Since the saturated substrate does not absorb water from the
repair material, the w/c ratio of the repair material should be about 3.5. Bond strength
0.4, and the BSE image analysis, however, gives a value of 0.36. This
reveals that the BSE image analysis underestimates the w/c ratio of Table 5 gives the results of the bond strength between repair
the repair material. This is because the resolution of the BSE material and concrete substrate. The unsaturated concrete sub-
images was 0.25 lm and the pores with a size smaller than this strate results in a higher bond strength than the saturated concrete
value were not detectable. As a result, the number of the pixels substrate. Under uniaxial tensile load, the specimens with the flat
of porosity was underestimated, and the porosity was, therefore, substrates all failed in the interface. It implies that the interface is
underestimated. Since the number of pixels of the hydration prod- the weakest plane in the specimens with the flat concrete
ucts was calculated by subtracting the numbers of pixels of the substrate.
pores and the unhydrated cement particles from the number of
total pixels, the underestimation of the porosity causes an overes-
Table 5
timation of the hydration products. According to Eq. (11), the over- Bond strength between repair material and concrete substrate.
estimation of the hydration products results in an underestimation
Concrete substrate Bond strength [MPa]
of w/c ratio.
Since MIP can provide a valid measurement on total porosity, Unsaturated 1.13 ± 0.27
Saturated 0.92 ± 0.23
the porosities obtained from MIP were used, by replacing the
J. Zhou et al. / Construction and Building Materials 112 (2016) 765–772 771
[14]