Chapter 2

Background

2.1 Motivation

Cement composite should be understood as a material made up of a minimum of

two components: a cement matrix and aggregate, in such a way that it should have
properties superior to the components considered separately. The layered systems
made of cement composites and that are used in construction typically consist of an
overlay with a constant or variable thickness, usually made of cement mortar and a
substrate, for which mainly concrete is used for their construction (Fig. 2.1).

Fig. 2.1 Explanation of the basic concepts contained in the title of the book

© Springer Nature Switzerland AG 2019 3

Ł. Sadowski, Adhesion in Layered Cement Composites,
Advanced Structured Materials 101, https://doi.org/10.1007/978-3-030-03783-3_2
4 2 Background

Fig. 2.2 Examples of layered systems made of cement composites: a newly built concrete screeds
in utility buildings, b newly built industrial concrete floors, c existing screeds

Layered systems made of cement composites can be newly built (e.g. floors) or
existing ones (Fig. 2.2). The layered systems made of cement composites are mainly
appropriate for concrete structures, roads and pavements. They can also form repaired
concrete elements, which after surface repair, involving the casting a repair overlay,
become a layered system. The correct exploitation and durability of layered systems
made of cement composites depends on the proper level of their adhesion [1].
Considering the above, in this monograph the level of adhesion should be under-
stood as the value of the pull-off adhesion f b (in MPa). It is assessed in practice using
the pull-off method and compared with the minimum value defined in the standard
or by the designer. The multi-scale approach should be understood as research on
the level of adhesion in scales from macro to nano.
A big disadvantage of the pull-off method is that damage that requires repair
is created at each measurement point at the end of the examination. In addition, it
is required that one control measurement falls on a surface of approximately 3 m2 .
Figure 2.3a shows a view of a sample distribution of testing areas located on a section
of a large-floor surface car park according to EN 12504-3 [2]. In practice, these
shortcomings have an impact on limiting the number of necessary measurements.
It is therefore reasonable to evaluate the level of adhesion using non-destructive
methods.
The higher the pull-off adhesion f b value, the better the bond is considered to
be. Based on these measurements, the “adhesion map” of the assessed surface of a
layered system can be obtained, which can then be used e.g. for the rough location of
defective regions (Fig. 2.3b). According to Adams and Drinkwater [3], on the basis of
this kind of macroscopic examinations it is also possible to assess whether the failure
occurred at the contact between the layers (adhesive damage), or in the material of
the overlay or substrate (cohesive damage). However, this kind of evaluation does
not allow the question as to why this happened to be.
Bearing in mind the correct operation and durability of layered systems made of
cement composites, more recently actions have been taken to increase the pull-off
adhesion f b over the required minimum value. According to Sadowski [4], these
actions may include the following:
2.1 Motivation 5

Fig. 2.3 A sample large-surface floor subjected to measurements using the pull-off method: a the
distribution of testing areas in accordance with the requirements included in EN 12504-3, b view
of the overlay damage in the evaluated area, c view of the repaired damage, d exemplary adhesion
map

• appropriate treatment of the surface of the concrete substrate, resulting in an

increase in the effective relative surface area, orientation of the surface texture,
removal of the cement laitance, surface exposure of the aggregate, etc.,
• increasing the maximum aggregate grain size in the concrete substrate,
• the application of different bonding agents,
• strengthening of the concrete substrate using impregnating agents,
• modification of the composition of the material, especially the overlay, with addi-
tives and nano-additives that “seal” its structure,
• modification of the composition of the material, especially the overlay, with admix-
tures that affect the viscosity of the concrete mix.
The effect of a given action on the level of adhesion assessed using the pull-off
method at macro scale does not allow for a deeper analysis of the results.
In the assessment of the effect of these activities on the level of adhesion, research
in a multi-scale approach may be very helpful. This would require the use of modern
testing methods other than the pull-off method. The results of this research can
significantly support decision-making in the matter of the sensible choice of a specific
surface treatment or bonding agent that significantly improves adhesion, as well as
the selection of a given type of additive or admixture that positively interferes with the
structure of a cementitious composite. By knowing the distribution and structure of
the air pores in the concrete in the interphase zone, it is possible to deliberately select
an additive that will reduce porosity. In turn, knowledge of the chemical composition
of the concrete in the interphase zone can help in the selection of a suitable adhesive
substance that is appropriate for increasing the adhesion in this zone. The search
for relations between the properties of cement composites in the interphase zone
determined on the macro scale, and also the properties defined in the meso, micro and
nano scales, seems to be not only interesting, but above all justifiable in this situation.
6 2 Background

These relationships can be of great importance in practice, because they can allow
the anticipated macroscopic properties to be obtained using appropriate structure
modeling. Researchers and engineers may be especially interested in improving the
durability of layered systems made of cement composites.
The analysis of the mechanisms of the adhesion between overlay made of cement
mortar and concrete substrate is a very comprehensive engineering task. It has been
investigated for decades. For example, in 1956 Felt [5] stated that “it became apparent
that factors influencing the bond of new and old concrete have been not easily isolated
and controlled. The most important factor has been the condition of the old surface-
its cleanness, roughness and strength or soundness. If the surface has been clean,
slightly rough and free of weak outer skin, a good bond has been generally obtained,
otherwise a relatively poor bond has been obtained”. Even though now the theoretical
knowledge is relatively large, the practical issues related to the evaluation of layered
systems made of cement composites to achieve a high quality of adhesion are still
ineffectively addressed. This may be due to the fact that the knowledge on the methods
and scales to ensure the obtaining of a satisfactory long-term adhesion is limited. It
should be noted that even though a lot of progress has been made, the improvement
of the adhesion is still usually performed empirically in the macro scale, i.e. many
samples with different microstructures are manufactured and evaluated until the
desired features are obtained.
Bearing this in mind, the aim of this work is to indicate the possibility of using
available modern research methods and descriptors for the identification of the level
of adhesion in layered systems made of cement composites in a multi-scale approach,
and also the indication of the extensive literature, which includes, among others,
examples of the author’s own research.

2.2 Semantic and Etymological Context

Figure 2.4 shows the semantic context of the identification of the adhesion level in
layered systems made of cement composites (based on [6]). Therefore, this exam-
ination should be understood as an assessment of the phenomenon of the adhesion
between overlay and substrate of a certain thickness made of a composite material
that is composed of both aggregate and a liquid cement matrix that is maturing over
time. Between the two materials, a thin layer or border in the form of an “interface”
is created. However, according to [7], unlike the “interface” that is created after the
casting the overlay made of cement mortar onto a concrete substrate, it should be
referred to as an “interphase” due to the maturing of the material of the overlay. Usu-
ally, the interphase zone is a layer of weakness. However, in some cases this zone
may be a layer of strength rather than weakness (e.g. after proper surface treatment
or application of a bonding agent). Some researchers call this zone the interface zone
or overlay transition zone.
2.3 Mechanism of Adhesion 7

Fig. 2.4 The semantic context of the identification of the adhesion level in layered systems made
of cement composites

2.3 Mechanism of Adhesion

As pointed out by Kinloch [8], “on one hand, adhesion is understood as a process
through which two bodies are brought together and attached—bonded—to each
other, in such a way that external force or thermal motion is required to break the
bond. On the other hand, we can examine the process of breaking a bond between
bodies that are already in contact. In this case, as a quantitative measure of the
intensity of adhesion, we can take the force or the energy necessary to separate the
two bodies”. This sentence explains the duality of the term of adhesion, as can be
perceived from the following two different angles:
• the conditions and kinetics of the process of joining of two materials,
• the quantitative measure of the separation process of the two materials.
Good adhesion is a key factor to obtain a monolithic layered system made of
cement composites. In its functional state, as a result of loading and service con-
ditions, the stresses act within the interphase between the overlay made of cement
mortar and the concrete substrate. The level of adhesion within this interphase must
bear these stresses. This is not easy considering the variability of the involved mate-
8 2 Background

Fig. 2.5 Principal mechanisms of the adhesion

rials. It is therefore not surprising that the main cause of failure of layered systems
made of cement composites is the failure of adhesion.
The mechanism of the adhesion of layered systems made of cement composites
may be divided into three main groups: mechanical interlocking, physical bonding
and chemical bonding (Fig. 2.5).
The proposed principal mechanisms can be subdivided further. According to
Weiss [9], overlays are designed to withstand very specific and often extreme loading
conditions or to fulfil very particular well defined functions.
The mechanism of the mechanical interlocking is mainly related to locking by
friction and locking by dovetailing. In this mechanism the morphology of the locking
materials affects the forces within the interphase.
The mechanism of physical bonding is mainly related to Van der Waals and
hydrogen bonds. Usually, the physical bonding is very weak. According to Weiss
[9], the interaction energies are less than 50 kJ·mol−1 . They are also present at a
distance of 0.3–0.5 nm.
The mechanism of chemical bonding is mainly related to ionic and atomic
bonding.

2.4 Functional State of Adhesion

Similarly to Mathia and Louis [10], it may also be stated that the functional state of the
adhesion changes with time (Fig. 2.6). Three fundamental states can be distinguished:
• an initial state. This state happens at the moment of contact between the liquid
material of the overlay and the hardened concrete substrate. After this state the
creation of the interphase occurs during the maturing of the cementinous material
of the overlay,
2.4 Functional State of Adhesion 9

Fig. 2.6 Three fundamental states of the mechanisms of the adhesion in layered systems made of
cement composites

• a functional state. This state happens when the interface is created and the layered
system made of cement composites is ready to perform its specific function during
its service-life,
• the final state. This state happens at the end of the service-life of a layered system
made of cement composites.
In most layered systems made of cement composites, the mechanisms presented in
Fig. 2.6 are interacting together and are responsible for adhesion. Very often, one of
the mechanisms plays a dominant role. According to Pertie [11] and Czarnecki [12],
the adhesion mechanism has a multi-scale character. Thus, the level of adhesion of
layered systems made of cement composites should be evaluated in different scales
of observation. Kinloch [13] pointed out that the science of adhesion is a truly multi-
disciplined subject. Thus, all aspects of surface chemistry, physics, rheology, polymer
chemistry, stress analysis, polymer physics, and fracture phenomena should be taken
into account to fully interpret the functional state of the level of the adhesion in
layered systems made of cement composites.
10 2 Background

2.5 Principal Scales of Observation

Based on the author’s own experience, performed research and according to Sadowski
[4], the investigations (observations) of the level of adhesion of layered systems made
of cement composites have been proposed to be performed in principal four scales
of observation:
• I scale (macro): observation over 1 m,
• II scale (meso): observation from 1 to 10−3 m,
• III scale (micro): observation from 10−3 to 10−9 m,
• IV scale (nano): observation below 10−9 m.
In this concept the value of the information relating to the properties of the inter-
phase zone depends not only on the scale of the observation. It also depends on the
magnification and resolution of the measurements. According to Cardon and Hiel
[14], it may be defined as the sum of the lengths of any nature.
This proposal should not be considered as the final guide to the scales of the
observation of the level of adhesion of layered systems made of cement composites.
Further studies are needed. It is expected, that this proposal will be updated based on
the developments and research in this field. It is advisable for configurations of other
materials to distinguish other scales. This may be for example the submicrometric
scale divided between the micro scale and nano scale. Also nothing stands in the way
to divide for example the picometric scale in order to observe lower scale phenomena
than in the nano scale.

2.5.1 Macro scale

At the first scale (I—macro) the level of adhesion is evaluated primarily on the basis
of pull-off measurements. Interlayer pull-off adhesion f b , which is useful, e.g. to
create the so-called “adhesion maps”, is then evaluated. In this scale the interphase
may be distinguished as the idealized homogenous model of a layered system made
of cement composites. The macroscopic mechanism of the creation of the adhesion
may be observed in two phases. The first phase occurs between the fresh and liquid
cementitious material of the overlay and the hardened concrete at the time of laying
the overlay (Fig. 2.7a). The “interface” is created at this stage. However, after the
casting an overlay made of cement mortar onto a concrete substrate, the “interphase”
is formed due to the maturing of the cementitious material of the overlay (Fig. 2.7b).
Similarly to Emmons and Vaysburd [15], this form a three-phasic model. This model
contains an overlay made of cement mortar, a concrete substrate, as well as an
interphase between them (Fig. 2.7).
In this scale the macroscopic properties of the interphase are the complex func-
tion of the concrete substrate morphology, the properties of the overlay made of
cement mortar and the environmental factors (e.g. temperature and moisture). They
2.5 Principal Scales of Observation 11

Fig. 2.7 Idealized

macroscopic model of the
observation of the level of
adhesion of layered systems
made of cement composites:
a at the time of laying the
fresh and liquid cementitious
material of the overlay, b at
the time when the interphase
is formed

are obtained by the visual inspection and analysis of the interphase along the geo-
metrical effective surface areas between the concrete substrate and overlay made of
cement mortar. According to Bissonnette et al. [7], the geometrical effective surface
area in the macro-scale is usually distinguished as a straight line between the overlay
and the substrate.

2.5.2 Meso scale

At the second scale (II—meso) the selected physical and mechanical parameters
are helpful. In particular, the parameters describing the surface morphology of the
concrete substrate are evaluated together with the distribution of the air voids along
the thickness of the interphase (Fig. 2.8). At this level the cement composite is
composed of three phases: the aggregates, the air voids and the cement matrix.
At the meso-scale, according to Pigeon and Saucier [16], the segregation of the
aggregate close to the concrete substrate can be responsible for the creation of an
interphase zone. As opposed to the geometric surface area at this scale and lower
scales, most of the adhesion mechanisms act on the effective surface area. It is proper
to note, that at the macro-scale the effective surface area is closer to the true surface
than the geometric surface.
12 2 Background

Fig. 2.8 Idealized model of the meso scale observation of the level of adhesion of layered systems
made of cement composites

2.5.3 Micro scale

At the third scale (III—micro), the structure of the smaller the air pores (mainly
micropores) of the cementitious composite in the interphase zone may be assessed
together with its changes over time. According to Pigeon and Saucier [16], at the
micro scale the interphase between the overlay made of cement mortar and concrete
substrate in a layered system made of cement composites may be similar to the
interfacial transition zone (ITZ) between the cement matrix and aggregates. In this
scale the “wall effect” exists within the interphase between the overlay made of
cement mortar and concrete substrate. As a result of it, the interphase may contain
smaller particles, have a lower mechanical strength and a higher porosity than the
bulk cementitious material of the overlay. For example, Zhou et al. [17] found that
for an analyzed layered system made of cement composites, the porosity in the
interphase has been 81% higher than that in the bulk cementitious material of the
overlay. This may occur at a distance from about 20 µm (as noted by Zhou et al.
[17]) to about 100 µm (as noted by Beushausen et al. [18]) from the surface of the
concrete substrate. As pointed out by Espeche and Leon [19], the mechanism of the
creation of pores in the micro scale should also be related to the chemical bonding
during the embedding activity between the reactive, fresh and liquid cementitious
material of the overlay and the hardened, old and dry concrete substrate (Fig. 2.9).
At this scale, He et al. [20] proposed dividing two zones within the interphase:
the reaction layer and the permeable layer. In this mechanism the effective surface
(microscopic morphology) improves the bonding within the permeable layer. On
the other side the bonding agents improve the bond within the reaction layer. Due
to the presence of these two processes, the interphase may be properly improved.
The cementitious material of the overlay (mainly fresh and liquid cement paste)
penetrates into the permeable layer. After that it reacts with the hardened concrete
substrate in the reaction layer. This process is progressing until the cementitious
2.5 Principal Scales of Observation 13

Fig. 2.9 Idealized model of the micro scale observation of the level of adhesion of layered systems
made of cement composites

material of the overlay is hardened. According to this model, the role of the bonding
agent can follow the sequence below:
• firstly, due to the demulsification, the bonding agent adsorb sand and cement
particles on the surface of the concrete substrate,
• the bonding agent infiltrates into cracks and holes on the surface of the concrete
substrate,
• with the drainage of water by the bonding agent, the films are being formed on the
surface of the concrete substrate,
• then during the cement hydration process, the chemical reactions happen between
bonding agent and cement hydrates.
In the model proposed by He et al. [20] it is visible that in the case of the application
of bonding agents the reaction layer will be denser and less porous due to formed
films. It will prevent the cracks from expanding and intensifying the amount of
hydration products. Consequently, it is visible that more cementitious material of the
overlay can permeate into the cracks and holes on the hardened concrete surface if
the effective surface (microscopic morphology) of the concrete substrate is large.

2.5.4 Nano scale

At the fourth scale (IV—nano) it is possible to observe the mechanism of phenomena

at the molecular level. It may include, for example, the assessment of the chemical
composition of the cement composite in the interphase zone. Especially the migra-
tion of elemental atoms from layer to layer may be interesting. The hypothetical
mechanism of the creation of the interphase at the nano-scale level is presented in
Fig. 2.10.
In the first stage of the mathematical model proposed by Xie and Xiong [21]
presented in Fig. 2.10a, the active ions Na+ , K+ , S04− , AI+ , Ca2+ and Si4+ will
permeate through the water film created at the interface from the fresh and liquid
14 2 Background

Fig. 2.10 Idealized model of the hypothetical mechanism of the creation of the interphase at the
nano-scale level: a permeation of active ions into the pores and the air voids of the hardened
concrete substrate through a water film, b hydration of the fresh and liquid cementitious material
of the overlay, c final hydrated state
2.5 Principal Scales of Observation 15

cementitious material of the overlay into the air voids and pores of the hardened
concrete substrate.
In the second stage (Fig. 2.10b), active ions will react with the hydrated cement that
is present in the bulk material of the concrete substrate. Then, the reaction products
will fill up the air pores of the bulk material of the hardened concrete substrate.
These products will finally form the penetrating layer. In this stage, the ettringite
(AFt) crystals that are porous and abundant in Ca(OH)2 , as well as other chemical
products form the strongly-affected layer.
In the last stage (Fig. 2.10c), the fresh and liquid cementitious material of the
overlay produces a flow of water into the bulk material of the hardened concrete sub-
strate. A consequence of this flow is the local increase of the water-cement ratio. This
leads to an increase in the size and amount of AFt and Ca(OH)2 orientational crys-
tals, They make the strongly-affected layer more porous than the bulk cementitious
material of the overlay.
Based on the mathematical model presented by Xie and Xiong [21], three layers
can be distinguished within the interphase between the overlay made of cement
mortar and the concrete substrate:
• the penetrating layer—it mainly contains prickly calcium silicate hydrates
(C–S–H) and small amounts of AFt or Ca(OH)2 . It is formed in the near sur-
face zone of the concrete substrate. It contains early constituents that react with
active chemical components in the cementitious material of the concrete substrate.
Its structure may be tighter than the bulk cementitious material of the concrete sub-
strate. The thickness of this layer is adversely proportional to the porosity of the
hardened concrete substrate, as well as to the ions activity and the water-cement
ratio in the overlay made of cement mortar,
• the strongly-affected layer—it mainly contains the predominant product phases
in the form of Ca(OH)2 and needle-shaped AFt crystals. These crystals grow
with a certain orientation perpendicular to the surface of the concrete substrate.
Due to the perpendicular orientation of the crystals, this layer is usually thick
and it is characterized by higher porosity. This layer is typically characterized
with other chemical products, cracks and water. It is normally the weakest part of
the interphase, strongly determining the performance of layered systems made of
cement composites. The thickness of the strongly-affected layer is influenced by
the age and the porosity of the hardened concrete substrate, and also the water-
cement ratio of the cementinous material used to make the overlay and substrate,
• the weakly-affected layer—it is located in the overlay made of cement mortar
and has almost the same micro-structure as the bulk cementitious material of the
overlay. The quantity and shape of crystals in this layer are similar to those in the
overlay made of cement mortar. The thickness of this layer depends on the nature
of the fresh material of the overlay and the bonding agent applied on the surface
of the concrete substrate.
It should be highlighted that the thickness and structure of the strongly-affected
layer should have the most significant influence on the level of adhesion of layered
systems made of cement composites. The level of adhesion depends also on the
16 2 Background

number of tiny crystals within the interphase. As noted by Xie and Xiong [21],
thanks to the huge specific surface area of tiny crystals, a larger interfacial area
between the fresh and liquid cementitious material of the overlay and the hardened
concrete substrate will be created. It will result in higher Van der Waal’s forces at
the nanoscopic interface morphology. They are mainly generated by the interactions
between crystals, as well as between crystals and aggregates.

2.6 Bibliographic Analysis

It is worth starting with the fact that the interest in the problem of adhesion in science
is noticeable in a number of publications (Fig. 2.11). The bibliographical analysis
presented in Fig. 2.11a shows that the number of publications regarding this problem
is growing steadily. There is a noticeable increase in this number in such fields as
“Materials Science”, “Engineering” and “Chemistry”. In turn, Fig. 2.11b shows that
by 2015, most studies about adhesion have been published in the United States and
China.
In turn, Fig. 2.12a shows that the number of publications that contain the words
“adhesion” and “concrete” in the “abstract, title or keywords” increased several
times in 2016 compared to 2004. There are a relatively small number of publications
regarding the adhesion between concrete layers. However, even here the growth is
also noticeable. From the analysis included in Fig. 2.12b, it can be concluded that
the number of publications containing the words “adhesion” in the “abstract, title or
keywords”, with regards to a different level of observation, has increased by about
270% (micro-scale) and 420% (nano-scale).
In recent years, the study of the level of adhesion mainly consisted of macro scale
evaluation using “adhesion maps” made using the pull-off method [22]. Also bending
[23, 24], shear [25, 26] and flexural strength [27–30] measurements are very popular.
These measurements are mostly performed on a large-scale layered systems made
of cement composites. For example, Sadowski and Hoła [31–33] showed that it is
possible to predict the value of the pull-off adhesion f b between the overlay made of
cement mortar and concrete substrate based on non-destructive testing methods and
artificial neural networks.
Research at lower scales of observation has consisted primarily of the observation
of places and the method of destruction of the interface formed after pull-off mea-
surements. Nowadays, the sand patch test and profilometric methods are still popular
for the assessment of concrete surface morphology [34]. However, for example Tayeh
et al. [35] or Siewczyńska [36] used more advanced three-dimensional methods to
evaluate the level of adhesion in layered systems made of cement composites. At
the meso scale, evaluation has been also made by impact-echo and ultrasonic echo
methods [37, 38], the ultrasonic method [39], the acoustic emission method [40] and
the infrared thermography method [41].
2.6 Bibliographic Analysis 17

Fig. 2.11 Analysis of the number of publications regarding adhesion and divided into: a individual
scientific disciplines, b country of publication (results for “adhesion” in the “abstract, title or
keyword” in the Scopus database—state for 23.12.2017)

In turn, evaluation on the micro scale has been mainly performed by scanning
electron microscopy [42–46] and porosimetry [17]). However, in recent years it has
been observed that the X-ray micro-computed tomography and nanoindentation has
18 2 Background

Fig. 2.12 Analysis of the number of publications regarding adhesion and divided into: a keywords,
b different levels of observation (results for “adhesion” in the “abstract, title or keywords” in the
Scopus database—state for 23.12.2017)
2.6 Bibliographic Analysis 19

been more frequently used for this purpose [47, 48]. Czarnecki and Garbacz [49],
and also Pietrie [11] pointed out that the adhesion in layered systems made of cement
composites, as a multi-scale problem, should be investigated at different levels of
observation.

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