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Hydration and moisture gradients of tile adhesives

Conference Paper · September 2009

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F. Winnefeld, J. Kaufmann, S. Harzer, M. Herwegh, A. Wetzel,
R. Zurbriggen

Hydration and moisture gradients of tile adhesives

Introduction
The trend to use fully vitrified, large-sized stoneware tiles has increased in the recent
years. Due to their low porosity and water absorption of less than 0.5 wt.-% they are
frost resistant and thus recommended for the application in the outside area. The large
formats are trendy for mainly aesthetic reasons.
However, technical problems appear which are related to higher shear forces upon de-
formations and poor adhesion of the cementitious adhesive mortar on the vitrified sur-
face of the tile.
These problems lead to increasing requirements concerning the properties of a tile adhe-
sive. The curing conditions increase the complexity of the system, because they are
varying from substrate to tile and from the rim to the centre of the tile. These conditions
cause moisture and hydration gradients parallel and across the mortar bed. Those gradi-
ents influence the shrinkage and expansion behaviour, initiating micro cracks preferen-
tially at the edges of the tiles /1/. The hydration and the water loss/adsorption of the tile
adhesive and their consequences, especially the film formation of the redispersible poly-
mer play a key role as shown in a previous study /2/.
The adhesion and failure mechanisms of polymer modified tile adhesives under these
conditions are currently investigated in a joint research project focussed on laboratory
and field studies /3-9/.
To investigate the influence of curing conditions on hydration and moisture gradients as
well as on the resulting properties (adhesion strength, shrinkage), the properties of two
tile adhesive mortars (wall application and floor application, respectively) in the system
tile – adhesive mortar - concrete slab are examined. Adhesive strength is measured at
different positions of the tile (30x30 cm) applying various curing regimes and curing
times. Length change measurements are performed on the tile and on upper and lower
side of the concrete slab. The gradient of cement hydration is studied by thermogravi-
metric analysis (TGA) and X-ray diffraction (XRD).

Experimental
The composition of the two tile adhesives (F1 for floor application and W2 for wall ap-
plication) is shown in table 1. The fully vitrified stoneware tiles used have dimensions
of 298 mm x 298 mm x 8 mm and belong to group BIa acc. to EN 14411:2003. They
exhibit water absorption levels less than 0.5 wt.-%. Their contact area to the mortar is
covered by an engobe based on MgO. Concrete slabs with dimensions of 400 mm x 400
mm x 38 mm acc. to EN 1323 are chosen as substrate. For the jointing of the mortar for
wall application a commercial product is applied.
 Material F1 W2
Table 1: CEM I 52.5 R 35.0 35.0
quartz sand 0.1-0.6 mm 15.0 15.0
Composition of the quartz sand 0.1-0.3 mm 31.6 31.6
tile adhesives dolomite filler (< 0.05 mm) 15.0 15.0
(in weight-%) unmodified cellulose ether 0.4 -
modified cellulose ether - 0.4
redispersible polymer powder 3.0 3.0
water 25.0 26.0

For mixing a spiral agitator (with a diameter of 80 mm and a speed of 750 rpm) was
used. The fresh mortar is mixed for 30 s, then moved with a spatula to control the wet-
ting and afterwards mixed again for 30 s. The trowel for the floor application has the
dimension of a=7/b=20/c=12 mm (M1) and the trowel for wall application a=8/b=8/c=8
mm (C4), respectively, as defined in /10/. The time between application and tile inlay-
ing was set to five minutes. After inlaying, the tile is loaded with 32.3 kg for 30 s. The
mortar for wall application was jointed one day after application.
The concrete slab – mortar – tile composite samples were stored as follows.
- dry: 28 days at 23°C and 50% relative humidity acc. to EN 12004
- wet: 7 days at 23°C/50% rel. humidity and 21 days storage in water acc. to EN 12004.
At the date of testing, the sample was cut for adhesive strength, TGA and XRD meas-
urements as shown in figure 1. Length change measurements were performed on a dif-
ferent set of samples. More experimental details are given in /4/.

Figure 1:

Scheme of locally resolved testing.

TGA and XRD of the mortar were
performed in the bulk mortar as
well as on the interface with the
tile.
Length change was measured using
separate specimens at several posi-
tions on the tile and on both sides
of the concrete slab.

Results and discussion

Adhesive strength
In general, mortar F1 for floor application (figure 2) yields higher adhesive strengths
compared to mortar W2 for wall application (figure 3). One important reason is the use
of different trowels. The trowel used for F1 creates a complete embedding of the tile
into the mortar and thus a better connection to the tile. In contrast, the trowel used for
W2 causes large cavities between the ripples, resulting in a poorer connection with the
tile. The engobe layer on the tile might also influence the adhesive strength, as it is not
uniformly distributed and more located at the rim of the tile.
The specimen with mortar F1 stored dry for 7 d shows highest adhesive strength at the
corners of the tile and lowest values at the centre. This can be explained by the fact, that
the mortar starts to dry out from the edges of the tile, and thus the film formation of the
polymer dispersion is more advanced /2/, providing an adhesion between mortar and
tile. However, the rapid drying of the mortar causes a poor hydration degree as deter-
mined by TGA and XRD measurements.
After 28 d of dry storage, the strength has decreased in the corners and the edges and in-
creased at the centre of the tile. This can be explained on one hand by the drying and
carbonation of the tile adhesive at the rim of the tile and by ongoing hydration and
polymer film formation at the centre of the specimen. On the other hand, the non-
uniform shrinkage of the tile adhesive (see figure 4 and text below) induces stresses es-
pecially at the interface between tile adhesive and tile, which decrease the adhesive
strength.
At an age of 56 d, adhesive strength at the rims of the tiles exhibits almost no change
compared to 28 d. However, the strength at the centre of the tile has decreased strongly
due to the continuing shrinkage processes.
In contrast to the dry storage, the curing under water leads to a much more uniform ad-
hesive strength distribution. When comparing the samples cured 7 d dry and 28 d wet,
the strength especially at the edges of the tile has decreased during the additional 21 d
storage under water. On one hand the wetting of the sample can influence the polymer
film formation or the polymer film itself, causing a reduction of adhesion. On the other
hand, the water storage causes an expansion of the concrete slab, which is partially re-
strained by the stiff tile. Thus, stresses are induced to the tile-mortar interface, which
cause this loss of adhesion.
After 56 days wet curing the adhesive strength has slightly and uniformly increased,
which is probably caused by the continuing hydration of the tile adhesive mortar due to
the ingress of water via the concrete slab. The increase in hydration degree could be
proven by TGA and XRD measurements.
After 7 d of dry storage the specimen with mortar W2 shows the lowest adhesive
strength at the rim and the highest adhesive strength in a zone between the rim and the
centre of the tile. Due to the - compared to F1 - less favourable structure of W2 with a
lot of cavities, which is induced by the trowel, the mortar W2 exhibits a faster drying.
This results in a poor hydration degree as obtained by TGA and XRD especially at the
rim of the tile. Thus, the poor adhesion can be explained. In the zone between rim and
core, where the highest strength can be found, film formation of the polymer occurs to-
gether with a reasonable hydration degree of the mortar. In the centre of the specimen
however, the film formation of the polymer is probably not yet completed, leading to a
lower adhesive strength of the mortar.
With increasing curing time at dry conditions (28 d and 56 d), the zone of highest
strength between rim and centre of the tile disappears. This can be interpreted by the
ongoing shrinkage processes, which cause stresses at the tile-mortar interface. These ef-
fects are stronger in the specimens tiled with W2 compared to those tiled with F1 (see
figure 4 and text below).
Wet curing again causes a uniform distribution of adhesive strength over the whole area
of the tile. The decrease in adhesive strength as well as the absolute strength values is
similar to the samples stored in dry conditions. A prolonged wet curing (56 d) does not
alter significantly the adhesive strength.

Shrinkage
The shrinkage of the specimen was measured on the tile as well as on the top and the
bottom side of the concrete slab (figure 4). Concerning the resulting stresses, the elastic
moduli of the materials are of great importance. By ultrasonic measurements (resonance
frequency method) it was found, that the dynamic elastic moduli of tile, adhesive mortar
and concrete slab are 63 GPa, 7 GPa and 33 GPa, respectively. Thus, it can be explained
that due to its high stiffness the deformations of the tile are generally low and only
slightly influenced by sample age and storage conditions. However, if shrinkage or ex-
pansion processes of the composite specimen (mortar and/or concrete slab) occur, this
stiffness can restrain the length changes of the sample and induce stresses especially at
the tile-mortar interface, as also shown by mechanical modelling /7/.
With mortar F1 and dry storage, the upper side of the concrete slab first exhibits an ex-
pansion due to its wetting by the application of the fresh mortar. Afterwards, both sides
of the concrete slab shrink. After 90 days of storage, the length difference between top
and bottom side of the slab sums up to about 0.25 mm/m. As the tile shows almost no
length change because of its very low water absorption and its high elastic modulus, a
stress is induced to the tile adhesive, leading to a decrease in adhesive strength over
time. In addition, the shrinkage of the specimen is not uniformly distributed, as the mor-
tar starts to dry out from the rim of the tile to the centre. This uneven distribution of free
water could be proved on fresh fractured specimens using infrared thermography.
The wet storage leads to an expansion of the concrete slab. The bottom side of the slabs
shows much more expansion than the top side, as its expansion is not hindered by the
stiff tile. Again, this non-uniform expansion of the concrete slab induces a stress con-
centration in the mortar. In contrary to the dry conditions, the expansion is probably
more uniformly distributed, as the ingress of water can occur from both sides of the
specimen. The length difference between top side and bottom side of the concrete slab
at 7 d (before immersion in water) is about 0.2 mm/m, whereas after 90 d storage under
water a length difference of about -0.1 mm/m is measured. From this observation it can
be concluded, that drying and wetting cycles cause a strong deformation of the speci-
men, which induces a stress especially to the boundary between tile and tile adhesive, as
the stiff tile exhibits only minor deformations
In principle, mortar W2 shows a similar behaviour. However, the absolute values of
length change exhibit some differences. The resulting length differences of the concrete
slab (top side – bottom side) are higher compared to F1 (0.25 mm/m after 7 d, 0.30
mm/m after 90 d dry storage as well as -0.25 mm/m after 90 d wet storage). The result-
ing higher stresses can explain, together with the use of a different trowel, the poorer
adhesion strength with mortar W2 compared to F1.
 [MPa]
1.75-2
1.5-1.75
1.25-1.5
1-1.25
0.75-1
0.5-0.75
0.25-0.5
0-0.25 7 d dry 28 d dry 56 d dry
_________________
30 cm
Figure 2:

Locally resolved adhesive strength of

the system concrete slab – adhesive
mortar F1 – tile
28 d wet 56 d wet
[MPa]
1.75-2
1.5-1.75
1.25-1.5
1-1.25
0.75-1
0.5-0.75
0.25-0.5
0-0.25 7 d dry 28 d dry 56 d dry
_________________
30 cm
Figure 3:

Locally resolved adhesive strength of

the system concrete slab – adhesive
mortar F1 – tile

28 d wet 56 d wet
0.5 tile 0.5 tile
concrete top dry concrete top dry
0.4 0.4
concrete below concrete below
length change / mm/m

length change / mm/m

0.3 tile 0.3 tile

concrete top wet concrete top wet
0.2 concrete below 0.2 concrete below
0.1 0.1
0.0 0.0
0.01 0.1 1 10 100 0.01 0.1 1 10 100
-0.1 -0.1
time / days time / days
-0.2 -0.2
-0.3 -0.3

Figure 4: Length change of tile and concrete in specimens tiled with F1 (left) and W2
(right). Samples stored in wet conditions were put under water after 7 days.
 Conclusion
The results reveal that the adhesion and the failure mechanisms of large-formatted tiles
are mainly controlled by (i) the hydration degree of the tile adhesive and its gradient, (ii)
moisture dependent film formation of the polymer and (iii) moisture gradients of the
system due to evaporation and water absorption. The different elastic moduli of the ma-
terials, especially the high stiffness of the tile, cause stress concentrations between the
different components, especially at the tile-mortar interface /8,9/. Besides the influence
of moisture, also thermal effects play a major role as observed on the building site /5,9/.
Financial support by Swiss Commission for Technology and Innovation is gratefully
acknowledged (CTI project No 8605.1 EPRP-IW). We would like to thank Hanspeter
Waser and Karsten Pass for their input in many technical and scientific discussions as
well as the laboratory team of Empa for their technical support.

References
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48-51.
/2/ Jenni, A. et al.: Influence of polymers on microstructure and adhesive strength of
cementitious tile adhesive mortars, Cem. Concr. Res. 35 (2005), 35-50.
/3/ Wetzel, A. et al.: Spatial and temporal evolution of physicochemical properties of
polymer-modified mortar at the interfaces of large-sized tiles, GDCh-Tagung
Bauchemie, Koblenz, 2008, Monographie Bd. 39, 237-245.
/4/ Wetzel, A. et al.: Setup for investigations of tile-mortar interface of large-sized
tiles, GDCh-Tagung Bauchemie, Koblenz, 2008, Monographie Bd. 39, 421-426.
/5/ Zurbriggen, R. et al: Failure mechanisms of outdoor applied large sized fully-
vitrified tiles, Technical Bulletin 03 MEDMA, Proceedings of the Middle East
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/6/ Wetzel, A. et al.: Wenn der Haftverbund versagt: Schadensmechanismen bei groß-
formatigen Feinsteinzeugfliesen, Farbe und Lack 115 (2009), Heft 3, 98-101.
/7/ Herwegh, M.: Critical stress concentrations in tile adhesive mortars: A numerical
modelling approach, 17. ibausil 2009, this volume.
/8/ Wetzel, A. et al.: Evolution of microstructures and critical adhesion patterns in
adhesives mortars applied under large-sized porcelain tiles, 17. ibausil 2009, this
volume
/9/ Greminger, A. et al.: Characteristic failure histories for tile damages in the exte-
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/10/ Kille, R.: Spachtelzahnungen für Bodenbelag-, Parkett- und Fliesenarbeiten,
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Authors
Dr. Frank Winnefeld
Dr. Josef Kaufmann
Sandy Harzer
Empa
Abt. Beton/Bauchemie
Überlandstrasse 129
CH-8600 Dübendorf
PD Dr. Marco Herwegh
Alexander Wetzel
Universität Bern
Institut für Geowissen-
schaften
Baltzerstrasse 1+3
CH-3012 Bern
Dr. Roger Zurbriggen
AkzoNobel Functional
Chemicals, Elotex AG
Industriestrasse 17a
CH-6203 Sempach Station

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