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The Journal of Adhesion

ISSN: 0021-8464 (Print) 1545-5823 (Online) Journal homepage: https://www.tandfonline.com/loi/gadh20

The Adhesion Properties of Mortars in Relation


with Microstructure

S. Papaioannou, R. Argyropoulou, C. Tachos & N. Markantonis

To cite this article: S. Papaioannou, R. Argyropoulou, C. Tachos & N. Markantonis (2015) The
Adhesion Properties of Mortars in Relation with Microstructure, The Journal of Adhesion, 91:7,
505-517, DOI: 10.1080/00218464.2014.931228

To link to this article: https://doi.org/10.1080/00218464.2014.931228

Published online: 18 Nov 2014.

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The Journal of Adhesion, 91:505–517, 2015
Copyright # Taylor & Francis Group, LLC
ISSN: 0021-8464 print=1545-5823 online
DOI: 10.1080/00218464.2014.931228

The Adhesion Properties of Mortars in


Relation with Microstructure

S. PAPAIOANNOU1, R. ARGYROPOULOU1,2, C. TACHOS1, and


N. MARKANTONIS1
1
Civil Engineering Department, Technological Educational
Institute of Central Macedonia, Serres, Greece
2
Laboratory of Inorganic and Analytical Chemistry, Department of Chemical Engineering,
National Technical University of Athens, Athens, Greece

The interaction between masonry units and mortar is a crucial


factor for the quality of a wall. The most important factor is the
adhesion between bricks and mortar in order to construct a
masonry wall with adequate strength, good impermeability, and
durability. In this work mortars were produced with various
cement=lime=aggregates ratio. The adhesion properties of the mor-
tars with clay bricks were tested with a simplified tensile=tear testing
measurement. In order to investigate the adhesion properties in
relation with microstructure the mortars were characterized with
X-ray diffraction and were further investigated with scanning
electron microscopy and stereoscopy. It was found that adhesion
is favored by the formation of a Si–Al matrix with a low Ca content
in the brick=mortar interface and the formation of fine Ca–Al–Si
phases which can penetrate into the brick.

KEYWORDS Adhesion; Ceramics; Civil engineering; Destructive


testing; Microscopy; Mortars

1. INTRODUCTION

Masonry construction exists since ancient times and remains a large part of
the building stock in the world as it presents a number of advantages such

Received 29 March 2014; in final form 2 June 2014.


Address correspondence to R. Argyropoulou, Civil Engineering Department, Technological
Educational Institute of Central Macedonia, Terma Magnesias, Serres, Greece. E-mail: rachelargyr
opoulou@yahoo.gr
Color versions of one or more of the figures in the article can be found online at www.
tandfonline.com/gadh.

505
506 S. Papaioannou et al.

as durability, thermal and sound insulation, and great flexibility of plan form
[1]. Among the various parameters for the construction of a healthy masonry,
the interaction between masonry units and mortar is considered to be of
major importance. The most important factor is the adhesion between
masonry units and mortar, as poor adhesion leads to defective strength
and impermeability [2]. It has been reported that the initial shear strength
of the masonry depends on the mortar=unit adhesion [3] while the flexural
strength is directly related to bond strength [4]. Therefore, the understanding
of the interface behavior is crucial for design and assessment purposes [5].
The adhesion bond results from complex physicochemical processes during
the curing of the binding agent. Qualitatively, the adhesion is described by
the specific work per unit area needed to separate the joint elements [6].
There are a number of factors that influence the mortar=unit adhesion, i.e.,
the kind of units (surface characteristics, absorbency, etc.), the kind of mortar
(workability, water retentivity, etc.), and the application technique (filling of
joints, degree of pressure on units, etc.) [2,3]. With regard to mortars and
units, it is reported that their mineralogical composition and internal structure
affect the masonry joint strength. Thus, it is apparent that jointing materials
with different compositions and porous system will produce different physi-
cal–mechanical behavior [4]. Up to now, considerable work has been done
on the characterization of mortars from historic buildings [7,8] or for resto-
ration purposes [9], while the majority of research on the mechanical beha-
vior of modern masonry is mainly focused on the evaluation of shear and
flexural strength [3,4,6,10,11] with various mortars and units and on the mod-
eling of interface behavior and fracture mechanism [5,12–15], while limited
results concerning the microscopic level have been published [4].
In this work different cement–lime mortars were produced. The work-
ability of the fresh mortars and the compressive and flexural strength of the
hardened mortars were measured. The adhesion of these mortars to perfor-
ated clay bricks was qualitatively estimated with a simplified tensile=tear
testing measurement. The mortars were characterized by means of X-ray dif-
fraction (XRD) and scanning electron microscopy (SEM). The mortar=unit
interface was studied with stereoscopy. Finally, the results of the microstruc-
ture observations were associated with those from the adhesion test.

2. MATERIALS AND METHODS

2.1. Materials
For the preparation of mortars cement CEM IV=B (P-W) 32.5 R (Lafarge
Industry, Volos, Greece), lime putty and sand were mixed in different
ratios. Two types of aggregates were used: washed river sand from the area
(Serres, Macedonia, Greece) and crushed stone sand for mortars provided
from a quarry in the area. The choice not to use ready mixed mortars was
Adhesion Properties of Mortars and Microstructure 507

based on the fact that there are not such production units in many places in
Greece.
The moisture content was 2.8% for the river sand and 2.7% for the
crushed stone. The grading of the sand is presented in Table 1.

2.2. Mortars Material Testing


All materials except water were introduced in a mixing machine (CONTROLS
S.r.l., Milan, Italy) and were stirred for 5 min. The water was gradually added
with another 10 min of stirring. For all mortars the workability was measured
by flow table (CONTROLS S.r.l., Milan, Italy) according to EN 1015-3 [16]. The
initial and final setting time was measured by Vicat apparatus, (CONTROLS
S.r.l., Milan, Italy) according to EN 196-3 [17]. The mortars were then molded
in prismatic 40  40  160 mm metallic casts using a jolting table to compact
them and to remove any air bubbles and voids. Mortars remained in the mold
for 24 hr in relative humidity (RH) ¼ 90% and after this period they were
demolded and kept under room laboratory conditions (T ¼ 20 C, RH ¼ 60%)
for 28 days. After this period the mortars were tested in a three-point-bending
test according to EN 1015-11 [18] and in a compression test according to EN
1015-11 (INSTRON instruments, Massachusetts, USA). For the flexural test
three specimens of each mortar were measured after demolding. The two
halves of the prisms from the flexural test were subsequently submitted to
the compressive strength test, which means that six specimens of each mortar
were investigated in terms of compressive strength.

2.3. Adhesion Test


Specimens for the adhesion test were manufactured by assembling two
moistened horizontally perforated clay bricks with mortar. The thickness of
the mortar between the units was 5 mm. The adhesion between mortars
and masonry units was qualitatively tested with a tensile machine. According
to [6], the adhesion strength can be determined with a tear test in which
the mortar between the units experiences forces applied perpendicular to

TABLE 1 Grading of Sand

Percent finer than


Sieve
River sand Crushed stone sand

#4 100 100
#2 93 67.5
#1 71.6 39.4
# 0.25 3.7 17.9
63 mic 0.08 1
508 S. Papaioannou et al.

the mortar=unit interface. The ultimate strength is the maximum tensile force
required for the debonding per unit area of contact. This idea was followed
for the estimation of the adhesion. Metallic cylinders were inserted in the
holes of the bricks. The cylinders were then adapted to the grips of the testing
machine (INSTRON KN1200). Tensile forces were applied perpendicular to
the mortar=unit contact area. As samples were brittle, in order to obtain accu-
rate data, loading was kept slow by keeping the elongation rate constant at
1 mm=min. A photo of the test setup is presented in Fig. 1(a) and a simple
drawing of the test setup is depicted in Fig. 1(b). All measurements were
performed in a period of 32–35 days after the preparation of the mortars.
The qualitative characterization of adhesion test was as following:

. Poor–fair adhesion: rupture occurs along the brick=mortar interface with


no or little coverage of one brick surface with mortar.
. Good adhesion: rupture occurs in the mortar layer and bricks surfaces are
half-covered with mortar.
. Very good adhesion: rupture occurs in the mortar layer and both bricks
surfaces are totally covered with mortar.
. Excellent adhesion: no separation was observed, bricks break prior to any
rupture, which indicates that the adhesion and cohesion strength of the
mortar exceeded the strength of the masonry units.

In Fig. 2 the characterization of adhesion is presented. The adhesion


strength was calculated by dividing the rupture force to the mortar=unit
contact area.

FIGURE 1 (a) Photo of the adhesion test setup. (b) Simple scheme of the adhesion test setup.
Adhesion Properties of Mortars and Microstructure 509

FIGURE 2 Presentation of the qualitative characterization of adhesion test results.

2.4. Characterization of Mortars


The mineralogical study of the mortars was performed with XRD (Siemens
Diffractometer D5000, Munich, Germany), using CuKa1 radiation, graphite
monochromator, in a 2h range 5–60 , counting time 1.0 s. The power
conditions were 20 kV=30 mA. The patterns were evaluated by the DIFFRAC
AT Search program, provided by Siemens. The microstructure of the samples
was observed with SEM (Quanta 200, FEI Company, Hillsboro, Oregon, USA)
coupled with energy dispersive X-Ray spectroscopy (EDX) (Genesis 4000,
Mahwah, New Jersey, USA). The mortar=unit interface was observed
with stereoscopy (Leica 165 C equipped with Leica DFC 295 camera, Wetzlar,
Germany).

3. RESULTS AND DISCUSSION

In Table 2 the mixing ratios and the properties of mortars are presented. In the
table the standard deviation (s) for the flexural and compression test for each
mortar, is also depicted. The mixing ratio is in the form of the % weight
cement=lime=sand. Mortars 1–6 are made with river sand. Mortars 7–11 are
made with crushed stone sand. The water=cement (w=c) ratio was 0.7 for
the Mortars M1–M11. Preliminary tests with mortars, namely, Mortar A and
TABLE 2 Mixing Ratio and Properties of Mortars

Mixing Type of Flow Initial Final set Flexural Compressive Adhesion Adhesion
Mortar ratio aggregates (mm) set time (h) time (h) strength (MPa) strength (MPa) (qualitative data) strength (MPa)

Mortar A 1:1:6 River sand 100 2 24 2.5 s ¼ 0.22 12.5 s ¼ 0.83 Zero 0
Mortar B 1:1:6 River sand 117 1:45 24 2.3 s ¼ 0.14 8.1 s ¼ 0.40 Zero 0
Mortar 1 1:1:5 River sand 153 2:20 24 2.6 s ¼ 0.06 8.4 s ¼ 0.53 Excellent >0.15
Mortar 2 1:1:6 River sand 129 2 24 1.7 s ¼ 0.01 5.9 s ¼ 0.55 Good 0.09
Mortar 3 1:1:8 River sand 105 1:55 24 1.5 s ¼ 0.02 6.9 s ¼ 0.48 Poor 0.005

510
Mortar 4 1:2:6 River sand 155 3:25 24 1.0 s ¼ 0.08 3.1 s ¼ 0.37 Very good 0.092
Mortar 5 1:2:7 River sand 152 3:15 24 1.0 s ¼ 0.04 3.6 s ¼ 0.49 Good 0.061
Mortar 6 1:2:8 River sand 130 3:05 24 1.0 s ¼ 0.03 3.9 s ¼ 0.63 Good 0.061
Mortar 7 1:1:5 Crushed stone sand 169 2:20 24 2.0 s ¼ 0.02 9.4 s ¼ 0,72 Good 0.059
Mortar 8 1:1:6 Crushed stone sand 157 2:10 24 2.6 s ¼ 0.04 8.9 s ¼ 0.36 Good enough 0.052
Mortar 9 1:1:7 Crushed stone sand 150 1:45 24 1.5 s ¼ 0.05 6.1 s ¼ 0.45 Poor 0.028
Mortar 10 1:2:8 Crushed stone sand 155 2:30 24 2.7 s ¼ 0.01 12.0 s ¼ 0.63 Very good 0.108
Mortar 11 1:2:9 Crushed stone sand 148 2:45 24 2.9 s ¼ 0.06 13.4 s ¼ 0.70 Very good 0.123

s: Standard deviation.
Adhesion Properties of Mortars and Microstructure 511

Mortar B, showed that with ratios <0.7 the mortars had not adequate
workability resulting in zero adhesion with bricks. In particular, Mortar A
and Mortar B were prepared with a w=c ratio of 0.5 and 0.6, respectively.
From the results shown in Table 2, it can be said that in general for the
same type of sand and for the same cement=lime ratio an increase in the
aggregates content results in deterioration of workability, decrease of the
initial setting time, and deterioration of adhesion. With river sand and for
1:1 cement=lime ratio an increase of the sand content leads to a decrease
of flexural strength, but no evidence for compressive strength correlation is
found. More specifically, in comparison with Mortar 1, Mortar 2 presents a
35% decrease in flexural strength and a 30% decrease in compressive
strength. For Mortar 3 there is a 42% decrease in flexural strength and an
18% decrease in compressive strength, in comparison with Mortar 1. On
the contrary, with river sand and for the 1:2 cement=lime ratio an increase
of the sand content leads to an increase of the compressive strength (16%
for Mortar 5 and 26% for Mortar 6, in comparison with Mortar 4) while the
flexural strength remains constant. On the other hand, with crushed stone
sand and for 1:1 cement=lime ratio an increase of the sand content leads
to a decrease of compressive strength, while for the flexural strength such
relationship is not observed. More specifically, compared to Mortar 7, Mortars
8 and 9 showed a 5% and 35% decrease in compressive strength, respect-
ively. Concerning the flexural strength, Mortar 8 presented a 30% increase
in comparison with Mortar 7, while Mortar 9 showed a 25% decrease in com-
parison with Mortar 7. Therefore, it is evident that not only the mixing ratio of
raw materials, but also the microstructure of mortars, e.g., grain size, porosity,
and porous size, affect the mechanical behavior of mortars. For the same
cement=lime ratio use of crushed stone sand results generally in higher
values of strength than those obtained with river sand. For example, Mortar
8 presents 53% higher flexural strength and 51% higher compressive strength
than Mortar 2. The increase in strength can be attributed to the fact that the
crushed stone sand has grains with higher roughness than those of river sand
and it also presents a continuous grain-size distribution [2], while the river
sand has a large amount of material with grain size <1 mm and a small
amount of fine material (<0.25 mm) as depicted in Table 1. It has been
reported [3] that adhesion is highly affected by the workability of mortars
and the water absorbance of masonry units. This is evident for Mortars A
and B, taking into account that in this work moistened bricks of the same
quality were used. Moreover, by comparing workability and adhesion for
mortars made with the same raw materials and same cement=lime ratio,
e.g., Mortars 1–3, it is clear that a decrease in workability results in deterio-
ration of adhesion. On the other hand, mortars made with different raw
materials or mixing ratios as, for example, Mortars 1, 8, and 10 presented
similar values of workability but different adhesion. Therefore, the value of
workability alone is not an indicator for adhesion.
512 S. Papaioannou et al.

By the XRD measurements it was found that the river sand consists
mainly of quartz with the presence of albite in a small percentage, while
the crushed stone sand consists mainly of calcite with the presence of anker-
ite in a small percentage. In mortars made with river sand, quartz was the
main phase, followed by calcite, portlandite, C2S, and traces of other phases.
In mortars with crushed stone sand calcite was the main phase detected. In
Fig. 3 the XRD spectra of Mortar 9 is presented.
In Fig. 4(a)–(d) the SEM micrographs of Mortars 1, 2, 9, and 11 are
demonstrated. In these figures dark spots and bright spots are indicated with
white and black arrows, respectively. The EDX analysis of mortars is pre-
sented in Table 3 (data shown as wt%). Traces of Na, P, S, Cl, and Ti were also
detected in the samples. Mortar 1 (Fig. 4(a)) presents a large grain-size distri-
bution with grain size varying from 10 to 50 mm. Mortars 9 and 11 have more
dense and uniform grains with size 1–10 mm. In general, mortars made with
river sand have larger grain size than those with crushed stone sand and this
can explain why mortars with crushed stone sand presented higher values of
strength. The results are in agreement with findings from historic mortars,
where mortars with higher quartz content were more coarsely crystallized [7].
SEM observations of the brick=mortar interfaces are presented in
Fig. 5(a)–(d). In these figures the bright grains are indicated with black arrows
and the gray matrix is indicated with white arrows. As it can be observed, on
the surface of the bricks grains of the mortar have been embedded. This is evi-
dent for Mortar 1=brick and Mortar 11=brick interfaces (Fig. 5(a) and (d),
respectively), where many bright crystals can be observed on the brick

FIGURE 3 XRD spectrum of Mortar 9.


Adhesion Properties of Mortars and Microstructure 513

FIGURE 4 (a) SEM micrograph of Mortar 1. White arrow indicates a dark spot and black
arrow indicates a bright spot. (b) SEM micrograph of Mortar 2. White arrow indicates a dark
spot and black arrow indicates a bright spot. (c) SEM micrograph of Mortar 9. White arrow
indicates a dark spot and black arrow indicates a bright spot. (d) SEM micrograph of Mortar
11. White arrow indicates a dark spot and black arrow indicates a bright spot.

surface and these mortars presented the best adhesion. On the contrary, on
the Mortar 9=brick interface it can be seen that bright grains are sparsely
embedded on the brick surface. The EDX analysis (wt%) of the grains is
presented in Table 4.
In a study with concrete units [4] it was found that strong bond formations
are attributed to complex Ca–Al–Si phases within the block binder. Moreover,
in historic mortars the mechanical properties can be due to alkali–silicate reac-
tions at the brick fragment–lime interface [8]. On the other hand, in a study of
the adhesion of mortars made with cement, organic additives, and different
514 S. Papaioannou et al.

TABLE 3 EDX Analysis of Mortars

Mortar 1 Mortar 1 Mortar 2 Mortar 2 Mortar 9 Mortar 9 Mortar 11 Mortar 11


Dark Bright Dark Bright Dark Bright Dark Bright
spot spot spot spot spot spot spot Spot

C 5.48 6.40 7.24 8.23 6.32 13.62 13.16 14.58


O 42.34 45.72 35.83 38.80 54.05 39.87 49.73 45.50
Mg 1.27 3.26 0.16 1.70 1.49 1.09 1.20 1.36
Al 11.91 4.77 7.97 5.08 2.68 0.92 5.95 1.17
Si 20.61 11.47 29.64 11.32 9.02 2.59 10.83 3.34
K 7.64 2.17 13.57 1.25 0.36 0.51 1.21 0.60
Ca 6.15 19.82 4.84 27.06 17.95 38.23 14.50 29.42
Fe 3.52 4.12 0.24 3.50 1.41 0.57 2.26 0.78

kind of aggregates [19] it resulted that mortars with no CaO presented lower
strength. The above studies indicate that regardless of the type of masonry
unit and mortar used, adhesion is mainly attributed to Ca–Si complex reac-
tions. These results are in agreement with the results of the present study.
The bright crystals that seem to contribute to the adhesion consist mainly of
Ca–Si–Al, while adhesion improves by the number of these crystals. From
the results in Table 4 it results that the matrix on the brick=mortar interface
comprises Al–Si compositions with low Ca content and this is in agreement
with [4]. From the brick=Mortar 1 surface observations with stereoscopy it
was found that almost the whole surface of the brick is covered with mortar.
On the brick=Mortar 11 surface, it was observed that the mortar is spread to a
lesser extend on the brick surface. The same remarks hold for the
brick=Mortar 2 interface which presented less adhesion. For historic mortars
it is reported [7] that lime penetrates into the ceramic and causes reactions that
transform the microstructure of the ceramic imparting high strength. In [4] the
Ca–Al–Si phases were attributed to the use of fly ash in concrete blocks. From
the results of the present work, the adhesion seems to be highly affected by
the presence of Ca–Al–Si phases in the brick=mortar interface. These could
be formed from complex reactions among cement, lime, and aggregates or
could be partly attributed to fly ash in the pozzolanic cement used. By com-
paring the results shown in Table 3, it can be noticed that Mortars 9 and 11
are richer in Ca content than Mortars 1 and 2, but exhibit lower concentration
in Si and Al than Mortars 1 and 2 and this can be expected as Mortars 9 and 11
are made with crushed stone sand. On the other hand, in the brick=mortar
interface the grains of Mortars 9 and 11 have higher concentrations in Al
and Si, which can be attributed to the presence of the brick. Moreover, from
the results in Table 4, it is noticed that in bright grains of Mortars 1, 2, and 11
there is a similar Ca=Si=Al ratio. More specifically the Ca=Si=Al ratio in Mortars
1, 2, and 11 is 1=0.5=0.108, 1=0.49=0.09, and 1=0.45=0.14, respectively. In
Mortar 9 which presented a poor adhesion the bright grains on the interface
are deficient in Si and the Ca=Si=Al ratio is 1=0.3=0.16. Moreover, dark grains
in Mortars 1 and 11 present similar Si=Al=Ca ratio (1=0.49=0.14 and
Adhesion Properties of Mortars and Microstructure 515

FIGURE 5 (a) SEM micrograph of Mortar 1=brick interface. Black arrow indicates a bright
grain and white arrow indicates a dark grain. (b) SEM micrograph of Mortar 2=brick interface.
Black arrow indicates a bright grain and white arrow indicates a dark grain. (c) SEM micro-
graph of Mortar 9=brick interface. Black arrow indicates a bright grain and white arrow indi-
cates a dark grain. (d) SEM micrograph of Mortar 11=brick interface. Black arrow indicates a
bright grain and white arrow indicates a dark grain.

1=0.47=0.15, respectively), while those of Mortar 2 are richer in Al and Si but


poorer in Ca. Those of Mortar 9 have a completely different ratio. In fact, the
Si=Al=Ca for Mortar 2 is 1=0.11=0.04 and for Mortar 9 is 1=0.64=0.19.
As same mixing ratios lead to a different adhesion with the use of
different aggregates it can be concluded that in mortars the amounts of
raw materials should favor:

i. the formation of a Si–Al matrix with a low Ca content in the brick=mortar


interface and, at the same time,
516 S. Papaioannou et al.

TABLE 4 EDX Analysis of Grains on Brick=Mortar Interface

Mortar 1=brick Mortar 2=brick Mortar 9=brick Mortar 11=brick

Bright Dark Bright Dark Bright Dark Bright Dark


grain grain grain grain grain grain grain grain

C 7.81 3.93 11.67 4.92 15.14 9.81 9.32 6.74


O 48.32 49.04 46.63 43.51 47.76 47.84 47.14 48.01
Mg 1.40 4.64 1.21 1.03 1.59 0.98 1.27 2.40
Al 2.61 9.74 2.17 4.42 3.44 11.99 3.24 9.51
Si 11.94 20.08 11.27 40.54 6.85 18.76 10.52 20.04
K 0.56 2.85 1.04 1.03 0.66 2.95 1.02 2.10
Ca 24.01 2.88 22.92 1.78 21.08 3.70 23.42 3.07
Fe 1.78 5.43 1.10 0.31 1.33 1.41 1.33 7.18

ii. the formation of fine Ca–Al–Si phases which can penetrate in the brick
providing adhesion.

4. CONCLUSIONS

The adhesion bond of different mortars has been tested and it was associated
with their microstructure. The adhesion bond between mortar and masonry
units results from physicochemical processes taking place during the mortar
curing and the extend of these processes affect the extend of the bond. The
adhesion depends greatly on the formation of Ca–Al–Si phases in a Si–Al
matrix in the masonry unit=mortar interface. In the matrix, the Si=Al ratio that
favors adhesion is in the range 1=0.5, with a low Ca content (Si=Ca: in the
range 1=0.15). The fine Ca–Al–Si phases that penetrate into the brick should
have a Ca=Si=Al ratio in the range 1=0.45–0.5=0.09–0.15. The more fine
Ca–Al–Si phases are formed in a well-structured matrix the stronger adhesion
is achieved.

FUNDING

The authors would like to thank the Research Committee of the Technologi-
cal Educational Institute of Central Macedonia for the financial support under
the Grant SAT=CE=050613-104=01.

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