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Accepted Manuscript

Title: The effect of surface treatment on the microstructure of


the skin of concrete

Authors: Łukasz Sadowski, Damian Stefaniuk

PII: S0169-4332(17)32727-7
DOI: http://dx.doi.org/10.1016/j.apsusc.2017.09.078
Reference: APSUSC 37157

To appear in: APSUSC

Received date: 2-8-2017


Revised date: 2-9-2017
Accepted date: 11-9-2017

Please cite this article as: Łukasz Sadowski, Damian Stefaniuk, The effect of
surface treatment on the microstructure of the skin of concrete, Applied Surface
Sciencehttp://dx.doi.org/10.1016/j.apsusc.2017.09.078

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The effect of surface treatment on the microstructure of the skin of concrete

Łukasz SADOWSKI*, Damian STEFANIUK


Wroclaw University of Science and Technology, Faculty of Civil Engineering
Wybrzeże Wyspiańskiego 27, 50-370 Wroclaw, Poland
*Corresponding author: lukasz.sadowski@pwr.edu.pl, tel. +48 71 320 37 42

Graphical abstract

Highlights

 The effect of surface treatment on the microstructure of the skin of concrete was studied,

 The measurements were performed using X-ray micro computed tomography,

 The volume fraction of pores profiles obtained from the micro-CT images were used,

 The heterogeneity of the skin of concrete affects its overall microstructural properties,

 The thickness of the skin of concrete differ for various surface treatment methods.

Abstract: The aim of this study is to better understand the heterogeneity and microstructural properties of
the skin of concrete. The microstructural evaluation of the skin of concrete was performed using X-ray
micro computed tomography (micro-CT). The concrete surface was treated using four methods, due to
which different surfaces were obtained, i.e. a raw surface, a surface formed after contact with formwork, a
grinded surface and also a shotblasted surface. The results of the pore structure obtained from the micro-CT
images were used to assess the influence of selected surface treatment method on the nature of the skin of
concrete. It was shown that the thickness and unique nature of the skin of concrete differ for various surface
treatment methods.
Keywords: concrete; microstructure; substrate; surface treatment; structure of pores; X-ray micro computed
tomography

1. Introduction

The quality of concrete surface has recently become an important issue [1]. This is due to the desired
purpose of use of the skin of concrete [2]. As pointed out in [3], this can be the beginning of a functional
approach to concrete surface manufacturing. In this approach the functional performance concrete will play
a dominant role. Poor properties of the skin of concrete can lead to its deterioration [4, 5]. Furthermore, the
color, texture and other aesthetic properties of a concrete surface [6] are influenced by the properties of the
skin of concrete. This is mainly the effect of the chemical composition of cement, water and aggregates, the
curing and casting conditions, diffusion [7] as well as the microstructural properties of the skin of concrete.
The skin of concrete also plays an important role in chloride diffusion [9], sulphate attack [10], electrical [8]
and thermal [11] conductivities, friction [12], stiffness [13], adhesion [14], moisture transport [15], excess of
water [16], water absorption [17] or wetting [18]. The following fundamental questions arise: how to reduce
abrasive wear and friction? How to improve the adhesion of overlays, coatings or paints? How to improve
the adhesion between aggregate and the cement matrix? How to improve frost resistance? How to slow
down the diffusion process of chloride ions? How to reduce salt scaling? The answers can be obtained based
on the optimization of the skin of concrete. This can be achieved with appropriate dosing of ingredients and
also the proper selection of the surface treatment method. The optimization of the treatment of the skin of
concrete has recently allowed to obtain, e.g., hydrophobic [19], graffiti [20] or self-healing [21] protected
surfaces.
The skin of concrete is defined as the surface layer that has a thickness of up to half of the maximum
grain size of the aggregate in concrete [22-26]. It usually has a different composition than internal (bulk)
concrete. Thus, as indicated in [27], compressive strength can be a misleading parameter if it is used to
characterize the quality of concrete skin. It is due to the phenomena such as the wall effect [23], contact with
formworks [24] or segregation [25]. Internal concrete is more regular away from the skin. According to [26],
the skin of concrete can be divided into cement skin (about 0.1 mm thick), mortar skin (about 5 mm thick)
and concrete skin (about 30 mm thick). It is well known that these layers are mostly made of cement paste.
Their porosity is higher than in the internal regions of concrete [28]. The hardness of the concrete skin also
differs from bulk concrete and affects the frost resistance of the investigated concrete [29]. The
environmental exposure, mix design and oxygen permeability of the concrete affects the carbonation depths
of concrete skin [30]. During construction, maintenance or repair, the surface of concrete is usually left after
concreting (raw). In some cases it is left after contact with formwork [31]. However, in many cases the
concrete surface has to be treated using an appropriate technique [32, 33], and sometimes the concrete skin
has to be protected from salt scaling using even more advanced concrete surface treatments methods [34].
Nevertheless, there is a lack of knowledge of the microstructure of the skin of concrete. How is it
different in the skin of concrete and its internal structure? What is the thickness of the skin of concrete from
a microstructural point of view? How does it differ for the various applied surface treatment methods? The
answer to these questions can be obtained using, e.g. micro-computed tomography (micro-CT). Thanks to
this method it is possible to provide the quantitative information on the real sizes and spatial distribution of
pores in heterogeneous materials. Micro-CT has recently become a popular non-destructive tool for
investigating the internal microstructure of composites [36, 37]. It is also useful for evaluating the porosity
of concrete [38, 39]. Improvement of the microstructural properties of the skin of concrete is one of the main
challenges inspiring researchers and engineers [40-43].
Considering the above, the study focuses on the microstructural evaluation of the skin of concrete using
micro-CT. The principal aim of this study is to better understand the heterogeneity and microstructural
properties of the skin of concrete. The concrete surface was treated using four methods, due to which
different surfaces were obtained: a raw surface, a surface formed after contact with formwork, a grinded
surface and also a shotblasted surface. Special focus was placed on the results of the microstructural
properties within the skin of concrete using micro-CT. The most significant pore structure profiles as well as
the grayscale value profiles (directly correlated with the attenuation coefficient values) obtained from the
micro-CT images were used to assess the heterogeneous nature of the skin of concrete.

2. Experimental procedure

The concrete was made of coarse and fine aggregates. The coarse aggregate in the form of crushed
basalt gravel with a maximum grain size Dmax of 8 mm has been used. The fineness modulus of coarse
aggregate was equal to 4.51 together with a seed density of 2.62 Mg/m3 (mineral mine “Byczeń”, Kamieniec
Ząbkowicki, Poland). Aa a fine aggregate the river sand with a maximum grain size Dmax of 2 mm has been
selected. The fineness modulus of fine aggregate was equal to 1.53 together with a seed density of 2.60
Mg/m3 (mineral mine Temco Sp. z o.o., Paniowice, Poland).
The concrete was made using 352 kg/m3 of type II A-LL 42.5 R Portland cement, 165 l/m3 of water,
1086.6 kg/m3 of crushed basalt aggregates and 724.4 kg/m3 of fine aggregate. 40 kg/m3 of fly ash
(Kogeneracja S. A., Wroclaw, Poland) was used. Additionally, 2.0 l/m3 of plasticizer Visco Flow 6920,
based on polycarboxylates with a density of 1.07 g/cm3, was added to achieve a workable condition of the
mixture of the concrete. The mass water-cement ratio was equal to 0.47.
The existing substrates were stored in laboratory conditions. The air temperature and an air relative
humidity were equal to +20°C (±2°C) and 65% (±5%), respectively. The substrate used in the study was
concrete that was two years old. The surface of the substrate was treated with different methods in order to
diversify the surface morphology. Based on the performed literature survey, four most commonly used ways
of surface treatment were selected (Fig. 1).

The surface T1 was not specially treated. It was only path grabbed and left after concreting. This is
the most commonly used surface treatment method (probably due to economic reasons). The surface T2 was
also left after concreting, but it has been formed after contact with the steel formwork (as cast). The T3
surface was mechanically grinded. A hand-held angle grinder with an abrasive disc was used to obtain a
ground surface. The T4 surface was shotblasted. For this purpose, a lightweight buckshot with a diameter of
6 mm was used. In the case of T3 and T4 surfaces, dust was removed after finishing the treatment. Finally, a
dozen samples with a size of 20 x 20 x 20 mm were cut from the existing concrete substrates that were
treated differently (Fig. 1). One, the most representative (with no macro defects), sample for each surface
was selected, subjected to tests using micro-CT, analyzed and presented in the article. Note that, the samples
were made in laboratory conditions and therefore they were much more homogeneous than the samples that
would be made “in situ”. Taking into account the size of measured fraction of pores and the aggregates of
the studied materials, it can be considered that the size of the examined samples was representative.
X-ray micro-CT scanner presented, in Fig. 2, was used to obtain the 3D images of the samples'
microstructure. The X-ray source in this scanner, in order to produce radiation, is built of two electrodes, i.e.
an anode and a cathode. The X-ray beam is transmitted through the sample that is rotated on a stage with a
pre-set value of an angle unit step. The final intensity of the monochromatic beam (I) passing through the
homogeneous material at the detector can be expressed using Lambert-Beer’s law as:
I  x   I 0  e  x , (1)

where I0 is the initial energy (intensity) of the X-ray beam when it leaves the source, x is the thickness of the
material and µ is the linear attenuation coefficient. In general, the value of µ depends on the material
density, atomic number and X-ray energy. It varies with the selection of different materials [46].
The projection for each angle is recorded on a detector that is covered by a scintillator – the material that
transforms the ionizing radiation (absorbed energy) in the form of light. The scintillator is connected to a
charge coupled device (CCD) 11 Mp camera that changes the light into a digital signal.
To analyze the microstructure of the material within the skin of concrete, at first, the samples were
scanned using micro-CT scanner. After couple trial scans the optimal scanning parameters were found. The
exposure time was kept as 1600 ms. The energy of the X-ray beam was set to 80 kV/10 W. An angle
rotation of up to 360° at 0.15° steps and a resolution of 5.41 m/px was used. A 0.5 mm Al filter was
applied. Using the described setup, each scan took approximately four hours. As a result, a set of projections
(1200 for each tomographic scan) was acquired. Then, a reconstruction of the obtained projections was
made using NRecon software (Version 1.7.0.4; Bruker, Kontich, Belgium) based on the Feldkamp algorithm
[44]. In order to avoid the boundary effect, only a part of the 3D image of 12 x 12 [mm] and 5 mm deep was
reconstructed. It resulted in the width of the volume of interests (VOIs) equal to 2220 x 2220 pixels, while
the vertical extent was limited to 920 slices (voxel size = 5.41 μm). The reconstruction process results in a
3D stack of virtual 8-bit cross-section images with grayscale (GS) values from 0 to 255. After the
reconstruction, CT Analyser software (Version 1.16; Bruker, Kontich, Belgium) was used for image
processing, e.g., filtering, despeckling or segmentation. Filtering and despeckling was performed to reduce
the undesired noise in the obtained images. In turn, segmentation was made to properly assign pixels to solid
phase or pore space by converting grayscale images to binary images. For this purpose, a simple
thresholding was made using a constant value of GS for all samples. More sophisticated method for
segmentation was not needed because of a high contrast between an air and solid phase of concrete (for
more details see, e.g. [45]). In the next step, 2D images were set together to create a 3D models using CTVol
software (Version 3.2.0; Bruker, Kontich, Belgium). Finally, selected measures (described in details in the
next Section), i.e. the developed interfacial area ratio (Sdr), the GS values (the linear relationship of µ) and
volume fraction of closed pores (c), were evaluated and compared for all investigated samples. Considering
the scanning resolution and the size of VOI, small fractions of pores with diameters from 20 to 1000 μm,
which are associated with air voids, were observed. In details, the presented methodology applied for
acquiring the images of the microstructure of the skin of concrete using micro-CT, and the analysis of these
images after image processing, is presented in Fig. 3.

3. Test results, analysis and discussion


In the following point, the most significant concrete substrate surfaces were analyzed. Fig. 4 shows 3D
views of the morphology of the concrete surfaces of samples T1, T2, T3 and T4, which were obtained on the
basis of tests using the micro CT method. In turn, Fig. 5 shows reconstructions of the 3D microstructures. To
characterize the surfaces of the concrete treated using different methods, the interfacial area ratio Sdr was
calculated according to ISO 25178 [47]:

 2 
 z ( x, y )   z ( x, y ) 
2
1 
Sdr   1       1dxdy. (2)
A A   x    y 
 
As stated in ISO 25178 [47], Sdr is the ratio of the increment of the interfacial area within the definition area
(A). According to [47], a large value of the Sdr indicates the significance of the amplitude and spacing. In
relation to [48], the Sdr is the total area of all triangles formed over the texture. The values of Sdr for all the
investigated samples was evaluated using Wolfram Mathematica software [49]. Note that the value of Sdr
equal to 0% represents a perfectly flat surface. It should be noted, that a perfectly flat surface of concrete
substrate probably does not exist.

It is visible in Fig. 4 that the value of Sdr is strongly influenced by the surface treatment method of
the existing concrete substrate. The highest surface area of the surface of the existing concrete substrate is
observed for the shotblasted surface T4 (Sdr = 24.8%) and for the raw surface T1 (Sdr = 13.8%). In turn, the
ground surface T3 is characterized by the lowest surface area Sdr, amounting to 7.6%.

At first, qualitative visual assessment of Figs. 4 and 5 was made. It can be noticed that the
microstructure of the skin of concrete differs for the selected differently treated concrete samples.
Considering the above, the significant 2D microstructure views of all the considered samples are presented
in Fig. 6; the dark phase represents pores and the white phase stands for anhydrous cement. It can be seen in
Fig. 6 that within the skin of concrete in samples T1 and T2, a thin layer with higher greyscale (GS) values
(associated with higher attenuation coefficient µ values) occurs on the top of aggregates near the surface.
This zone, with a thickness of about 50-100 m, can be considered as a cement skin. The increased GS
values occurring in the aforementioned zone (cement skin) can be due to the higher density of the material, a
higher amount of unhydrated cement grains or decreased nanoporosity. However, such layer does not exist
in the T3 and T4 samples due to their mechanical treatment. Additionally, in the surface of T1 sample, some
horizontal gaps can be seen around 400-500 m from the surface. This can be the effect of patch grabbing,
which was only done in the case of the T1 surface treatment method.
Therefore, it is of interest of how and if the µ changes for different surface treatments of the existing
concrete substrate. The changes were distinguished within the material of the substrate to a depth of 800 m.
Based on this analysis, it seems useful to examine the GS values as a function along a sample's height,
which were obtained within the skin of concrete using the micro-CT method.
The microstructures of the skin of concrete for samples T1 and T2 are affected by an accumulation of
CaO within the cement skin [50]. It probably results from the absence of mechanical surface treatment on
the existing concrete substrate and consequently by leaving the laitance on this surface (samples T1 and T2).
Based on Fig. 7, the approximate thickness of the cement skin is around 100 m for sample T1 and 50 m
for sample T2. No cement skin has been observed for sample T3. In this case, the progress of GS values
along the samples' height is homogenous. As a result of the mechanical grinding process, the cement skin
was removed. Similar observations can be seen for sample T4. In this case, the cement skin was also
removed due to shotblasting. However, due to the exposure of the aggregate and absence of weak parts of
the cement matrix (result of shotblasting process), the GS values are noticeably higher near the surface.
However, the values of GS (the linear relationship of µ) presented in Fig. 7 can not only be accompanied
with material density. These analyzed values depend on many other material properties, such as the atomic
number of the matter and X-ray energy. Therefore the higher GS values can also indicate the change of
chemical composition in the cement paste, not only the change in the nanoporosity. Thus, in the further part
of the paper the volume fraction of pores near the surface of the concrete is analyzed. Considering the above,
Fig. 8 shows the 3D models of the structure of pores of samples T1-T4. Finally, Fig. 9 shows how the
volume fractions of pores  are formed as a function along the samples' height.
Based on the analysis of changes in the volume fraction of closed pores c along a sample's height, it
can be noticed that the mortar skin, as shown in Fig. 9, has a different thickness depending on the treatment
method used. The criterion used to define where the mortar skin begins and finishes was the stabilization of
the average values of the volume fraction of closed pores c. Considering the above, the thickness of the
mortar skin ranges from 30 m for the raw surface (sample T1) to about 60 m for the as cast surface
(sample T2). In these two cases (T1 and T2), the diagram of creaches its maximum in the mortar skin zone.
In Table 1, the average values of c within the mortar and concrete skin are presented. Due to the small
thickness of the cement skin and morphology of the surface of concrete substrate, it was not possible to
obtain the average values of the c in this zone. As presented in Table 1, the average value of c within the
mortar skin is twice as high as in the concrete skin (1.47 ± 0.54% and 1.12 ± 0.28% for samples T1 and T2,
respectively). The average values of c in the concrete skin reaches values from 0.48 ± 0.20% for sample T4
and 0.54 ± 0.27% for sample T3, to 0.62 ± 0.16% for sample T2 and 0.73 ± 0.24% for sample T1. Based on
Fig. 9, it can be seen that the mortar skins in samples T3 and T4 were also removed due to the applied
mechanical surface treatment method.

4. Conclusions
In the approach presented in the article, micro-CT tests were performed to study the microstructural
properties of the skin of concrete. The results presented in this work confirm the potential of micro-CT to
observe the microstructural properties of the heterogeneous material within the skin of concrete.
The concrete surface was treated using four methods. Due to this treatment, four different surfaces were
obtained. These surfaces were: raw one, formed after contact with formwork, grinded and shotblasted. The
volume fraction of pores profiles obtained from the micro-CT images were successfully used to assess the
nature of the skin of concrete. It was shown that the thickness of the skin of concrete differs for the various
surface treatment methods. However, the extreme heterogeneity of the material within the skin of concrete
remains the main problem that affects the overall microstructural properties of a concrete surface.
Based on the performed analysis, it can be noted that the mechanical treatment (grinding in the case of
sample T3 and shotblasting in the case of the T4 sample of the skin of concrete) results in the removal of the
cement and mortar skins. In general, this is the advantage of these treatment methods, as the mortar skin
exhibits a heightened porosity (see Table 1). However, grinding of the surface (sample T3) results in a
significant decrease (by about 50% compared to samples T1 or T2) in the value of the Sdr. This is not
beneficial for the application of the overlay due to the significant decrease of the contact area between two
layers [50]. For this particular example, the shotblasting surface (sample T4) seems to be the most desired
(an increase of Sdr by about 100% compared to samples T1 or T2 and by about 300% compared to sample
T3).
Despite the lack of cement and mortar skins, mechanical treatment methods need additional costs.
Therefore, the skin of the concrete is usually only path grabbed after concreting (sample T1) or formed after
contact with the formwork (sample T2). Based on the micro-CT results, the thickness of the mortar skin of
sample T1 is two times smaller than for sample T2. However, the volume fraction of closed pores within the
mortar skin of sample T1 is about 30% higher due to the horizontal gaps (see Fig. 6a). It was probably
caused by the patch grabbing. Thus, also bearing in mind the almost identical Sdr values for both samples,
the T1 and T2 samples seem to be comparable in the aspect of, i.e. laying the overlay on the existing
concrete substrate. The microstructural properties of the concrete skin will play a major role in the multi-
scale aspect of the creation of the interphase between existing concrete substrate and hardening overlay. As
pointed out in [51] it is probably one of the most challenging aspects at the moment and specific multi-scale
processing algorithms and numerical methods need to be developed for this purpose.

Funding sources
This work was supported by the National Centre of Science, Poland [grant no. 2014/15/D/ST8/00550
“Evaluation of the interlayer bond of variably thick concrete layers based on nondestructive tests using
artificial intelligence”].

Acknowledgements
The authors are very grateful to Dyckerhoff Poland for sharing the recipe for the existing concrete substrate.
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T1 T2 T3 T4
after concreting (raw) formed after contact with mechanically grinded shotblasted
the formwork (as cast) (ground)

T2 T3 T4
(raw) formed after contact with mechanically grinded shotblasted
the formwork (as cast) (ground)
T1 T2 A-A
400 mm

125 mm
T4 Existing substrate
T3
A
A 500 mm

500 mm - places from where the 20 x 20


x 20mm samples were cut
20 mm 20 mm 20 mm 20 mm

20 mm
20 mm

20 mm
20 mm

Fig. 1. View of the existing concrete substrate with differently treated surfaces and also samples
subjected to tests using micro-CT.

(a) Detector covered by a scintillator (b)


with 11 Mp CCD camera

0.05 mm Al filter
X-ray source
(I = 80 kV;
P < 10 W) Sample

Angle rotation
(up to 360° at
0.15° steps and
a resolution of X-ray micro-CT scanner
5.41 μm/px) Scyscan 1172

Fig. 2. Micro-CT test setup: a) scheme of the setup, b) view of the X-ray micro-CT scanner.
Fig. 3. Scheme of the procedure used for the evaluation of the microstructure of the skin of concrete
using micro-CT.
Fig. 4. 3D views of the morphology of the concrete surfaces, which were obtained on the basis of tests using
the micro-CT method for samples: a) T1, b) T2, c) T3 and d) T4.

Fig. 5. Reconstructions of the 3D microstructure of the skin of concrete, which were obtained on the basis of
tests using the micro-CT method for samples: a) T1, b) T2, c) T3 and d) T4.
Fig. 6. 2D reconstruction views of the microstructure of the skin of concrete, which were obtained on the
basis of tests using the micro-CT method for samples: a) T1, b) T2, c) T3 and d) T4.

Fig. 7. GS values as a function along a sample's height within the skin of concrete, obtained using the micro-
CT technique for samples: a) T1, b) T2, c) T3 and d) T4.
Fig. 8. 3D models of the pore structure obtained within the skin of concrete on the basis of tests using the
micro-CT method for samples: a) T1, b) T2, c) T3 and d) T4.

Fig. 9. Volume fraction of closed pores c as a function of a sample's height, obtained on the basis of tests
using the micro-CT method within the skin of concrete for samples: a) T1, b) T2, c) T3 and d) T4.
Table 1. Volume fraction of closed pores (c) and estimated values of the thickness of the mortar and
concrete skin for samples T1-T4.
Volume fraction of closed pores
Average thickness [mm]
Sample ϕc [%]
Mortar skin Concrete skin Cement skin Mortar skin
T1 1.47 ± 0.54 0.73 ± 0.24 0.10 0.30
T2 1.12 ± 0.28 0.62 ± 0.16 0.05 0.60
T3 - 0.54 ± 0.27 - -
T4 - 0.48 ± 0.20 - -

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