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To cite this article: Jean-Didier Mertz , Mikaël Guiavarc’h & Paolo Pagnin (2012): Dilation
behaviour of lime mortars for restoration work: application to the compatibility of cracked stone
reassembling, European Journal of Environmental and Civil Engineering, 16:5, 527-542
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European Journal of Environmental and Civil Engineering
Vol. 16, No. 5, May 2012, 527–542
1. Introduction
Building stones and repair mortars are continuously submitted to environmental
conditions which determine the weathering and damage degree of the materials
3. Materials
3.1. Limestones
The two studied rocks are extreme types: a hard grey limestone (in DJ) and a soft clay-
rich limestone (in V) both affected by severe cracks from different origins.
The main building stone in DJ is a very compact and hard limestone from the
Upper Senonian formation (Dessandier, Antonelli, Hamiane et al., 2008), mainly formed
by micritic calcite and non-clay minerals. Several generations of tectonic fractures affect
this rock, mainly clogged by iron oxide/hydroxide and calcite veins. Moreover, vein fill-
ing suggests syntaxial growth from the edges of the crack. Cracks in the field blocks,
that may or may not result from freeze–thaw stress, grow in two directions: (i) along or
at the interface between the filling material and the rock matrix showing a structural
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weakness plane (Figure 1); and (ii) in a vertical direction resulting from a compressive
or bending stress. Other situations show an anthropogenic origin of the cracks due to
the partial reconstruction of the site. These vertical cracks are developed in a parallel or
perpendicular direction to the bedding.
According to the rock type, this stone has a low porosity between 0.5 and 3%
(EN1936), a specific surface area of 0.9–1.8 m2 g–1, a water saturation coefficient (Hir-
schwald, 1912) about 0.52–0.79 and a high compressive strength between 50 and 216
MPa (EN1926).
The tested limestone from the Volubilis site (V) is a building material used com-
monly for houses. Alteration is developed in various directions from the bedding planes
with concentric desquamated cups or plates contributing to the block destruction (Fig-
ure 2). Such peeling evolution underlines the competition in crack development
between external factors and the natural stone heterogeneity.
This local and soft molassic calcarenite is a rich terrigeneous rock from the Miocene
formation (Dessandier, Antonelli, Bouzidi et al., 2008). Formed by many clasts and
shell fragments, the stone is composed of micritic calcite (70–80%), dolomite, quartz
grains, apatite, iron oxide/hydroxide and clay minerals. XRD analysis (< 2 μm) shows
that the clay complex is composed of 12% kaolinite, illite and smectite. Swelling prop-
erties of smectites justify the high surface specific area of the stone (3.6 m2 g–1). This
Figure 1. Djemila site, wall of the Septimien temple. Location of cracks in the calcitic veins.
530 J.-D. Mertz et al.
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Figure 2. Volubilis site, baths of Gallienus. Alteration ‘in ball’ and peeling of the molassic
limestone.
porous material (36%) improves high water transfer properties, such as high water satu-
ration coefficient (0.98) and mechanical properties about 12 MPa in compressive
strength.
The selected mortars correspond, on one hand, to the need for testing local and
home-made products, and on the other hand, to assessing ready-to-use formulations
which present well known injectability and mechanical properties adapted to the treat-
ment of fine and hair cracks (Kalagri, Miltiadou-Fezans, & Vintzileou, 2010). The
tested mortars are traditional hydrated lime products and pre-proportioned products,
optimised for restoration work in Europe (Table 1).
4. Origin of dilation
Porous materials exposed to air moisture variations can change in volume. For free salt
conditions, the modification in volume is characterised by an expansion during the
increasing water saturation phase and by a contraction within the desaturation phase
(Delgado-Rodriguez, 2001; Jimenez-Gonzalez & Scherer, 2006). Soluble salts can dis-
turb this evolution and underline the major influence of crystal growth on the effects of
water sorption (Lubelli, van Hees, Huinink, & Groot, 2006; Ruedrich, Kirchner, Seidel,
& Siegesmund, 2005; Ruedrich et al., 2007).
European Journal of Environmental and Civil Engineering 531
strength
(MPa)
Adherence < 0.05 < 0.08 nm 1.4⁄⁄⁄
(MPa)
D (kg 1570 1590 1780 1510
m3)⁄⁄⁄⁄
Hg (%) 36.3 34.9 22.5 34.9
<r> (μm) 0.28 0.42 0.11 0.22
SSA (m² g–1) 8.8 5.5 10.1 8.0
Use Filling mortar Filling mortar Ready-to-use Ready-to-use injection
injection grout
grout
—: not measured.⁄mass proportion of the mortar components: lime/pouzzolana/stone dust = 71/199/112 g
mixed with 0.5 ml Glenium 51 additive (BASF company).
⁄⁄
after Rousset B. (2004), report EC/BR/0460, EC-Lausanne, 9p, unpublished.
⁄⁄⁄
according to data sheets (3w.kremer-pigmente.com).
⁄⁄⁄⁄
D, apparent bulk density.ΦHg, porosity open to mercury.
<r> and SSA, average pore radius and surface specific area, calculated by mercury injection porosimetry (MIP
Micromeritics Autopore V).
When exposed to an RH change, the total dilation behaviour results from the
microstructural properties of the porous media, pore size distribution and connectivity.
In addition, presence of clay minerals has a major influence on the importance of dila-
tion (Franzini, Leoni, Lezzerini, & Cardelli, 2007; Jimenez-Gonzales, Rodriguez-Nav-
arro, & Scherer, 2008; Mertz, 2007; Sébastian et al., 2007). Thus, stone deformation
is more sensitive to the disjoining pressure in clays minerals to a change of RH than
to their crystallographic properties, which are not directly involved in the expansion–
contraction mechanism.
Several damages have been also reported involving the effect of temperature
(Ondrasina, Kirchner, & Siegesmund, 2002; Weiss et al., 2004). For example, marbles
often present high dilation values due to the tensorial properties of calcite (Figure 3).
According to the statistical orientation of the crystallographic c-axis in the stone (Gas-
con & Balbas, 1986; Kleber, 1959; Rosenholtz & Smith, 1949), large thermal anisot-
ropy could induce significant deformation of limestones and especially ornamental
marbles (Figure 4).
These variations enable different volume dilations according to the size, fitting and
the proportion of the minerals species. Studies performed on cement pastes (Meyers,
1950; Zoldners, 1972) have shown that the thermal dilation coefficient is a nonlinear
function of the internal moisture state in a porous network. This relation (Grasley &
Lange, 2007) indicates that hygric and thermal requirements should be considered
532 J.-D. Mertz et al.
30
25 calcite
coefficient (10-6.K-1)
15
10
0
0 10 20 30 40 50 60 70 80 90
-5
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Figure 3. Change of thermal dilation coefficient of calcite and quartz at 20°C as a function of c-
axis position.
Figure 4. Deformation and fracturation of a funerary marble plate due to thermal variations.
Jewish Cemetery (Sélestat, F-67).
5. Method
5.1. Dilation measurement
Global volumic dilation is of particular interest because it concerns all the phenomena
for which the direction of measurements is essential. Nevertheless, it is more suitable to
European Journal of Environmental and Civil Engineering 533
For constant humidity conditions, the linear thermal dilation coefficient , is:
a ¼ DL=ðLDTÞ; ð2Þ
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with L, the initial length of the sample; ΔL, length variation; and ΔT, temperature gradi-
ent.
0.8
0.4
Time (h)
Stability (µm)
0.0
0 50 100 150 200 250 300
-0.4
-0.8
-1.2
-1.6
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-2.0
Figure 6. Monitoring of the stability of the eight sensors versus time for isothermal conditions
(T = 21 ± 0.1°C).
solution (K2SO4) inducing a theoretical air moisture of 97% RH at 20°C (Figure 7).
This humidity variation does not introduce any significant modification of the delivered
signal of the sensors during preliminar calibration. Thus when the system is in charge,
the sensor response is only the result of hygric deformation of the specimen without
any correction. Previous tests for time calibration were performed because RH steady
state is a function of the sample volume, pore structure and hygroscopicity. The results
showed that moisture equilibrium between the air atmosphere and the porous material
has a duration of around 4–6 days.
Thermal dilation measurements were carried out for a variation in temperature ΔT =
40 ± 1°C. The time taken to reach temperature stability between the two stages (5 to
45°C) is around 12 hours. The RH inside the chamber during the cycle shows a small
decrease of humidity which does not exceed 2–4% RH (Figure 8).
The total dilation of the steel frame-holder induces an important error due to its
own dilation. During the experiments a continuous correction (blank) is introduced by
100 24
80
Relative humidity (%)
Temperature (°C)
23
60
22
0 2 4 6 8 10
40
21
20
0 Time (days) 20
Figure 7. T/RH conditions performed during hygric dilation tests (black triangles: humidity;
grey curve: temperature).
European Journal of Environmental and Civil Engineering 535
50
14
10 40
Temperature (°C)
6
30
2
-2 0 2 4 6 8 10 20
-6
10
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-10
Figure 8. T/RH conditions performed during thermal dilation tests (black triangles: temperature;
grey curve: relative humidity).
using an Invar® bar (nickel steel alloy FeNi36), which has the same length as the sam-
ples, to determinate the true dilation of the whole steel frame-holder. Within the tests,
the samples and the Invar bar were submitted to the same variation in temperature.
Because the theoretical value α of Invar is well known, ΔLinvar is deduced for the
applied temperature conditions.
This correction allows calculation of the thermal expansion ΔLsample of the samples
submitted to the change of temperature ΔT:
where ΔLsample measured is the measured expansion of the sample, and Δxinvar measured is
the measured expansion of the Invar bar αinvar = 1.5 × 10–6 K–1.
Samples are parallelepiped or cylindrical test-tubes of 60 mm height. Four speci-
mens of each material were tested for reproducibility validation.
0.9 100
0.8
Vv
0.7 80
Vh
Hygric dilation (10-3 )
0.6
T(°C) - RH(%)
0.5 60
0.4
0.3 40
0.2
0.1 Dj6 20
0 Dj5
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-0.1 0
0 20 40 60 80 100
Time (h)
Figure 9. Hygric monitoring of hard (DJ5, DJ6) and clay-rich (V) limestone types (Vv and Vh:
respectively perpendicular and parallel to the bedding; open circles: relative humidity; T = 21.3 ±
0.1°C).
35 50
30
40
Thermal expansion (µm)
25
20 Dj5
30 Temperature (°C)
15
Dj6
10 20
Vv
5
Vh 10
0
-5 0
0 50 100 150 200 250
Time (h)
Figure 10. Comparative thermal dilations of hard (DJ5, DJ6) and clay-rich (Vv and Vh)
limestone types (open circles: temperature; 2 < RH < 4%).
pendicular direction than for the stratigraphic plans (Figure 9). Such differentiation is
attributed to the distribution of smectitic swelling minerals with respect to the bedding.
The opposite behaviour in dilation processes of the two limestones highlights the dual-
ity between pore structure and mineralogy.
To investigate the compatibility between the materials, the same experiments were
carried out on the mortars. Hygric dilations of home-made mortars (0.8 to 1.1 × 10–3)
present similar expansions (Figure 11).
But expansion properties of mortars and grouts (Figures 11 and 12) show different
kinetics according to their microstructural characteristics. The home-made mortar binder
European Journal of Environmental and Civil Engineering 537
2 100
T(°C) - RH(%)
1 60
0.5 40
0 20
NHL
CL
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-0.5 0
0 100 200 300 400
Time (h)
Figure 11. Hygric dilation of lime mortars CL (black curves) and NHL (grey curves) (open
circles: humidity; T = 21.3 ± 0.1°C).
2 100
Hygric dilation (10 -3)
1.5 PLM 80
T(°C) - RH(%)
1 LEDAN 60
0.5 40
0 20
-0.5 0
0 100 200 300 400
Time (h)
Figure 12. Hygric dilation of grouts PLM (grey curves) and LEDAN (black curves) (open
circles: humidity; T = 21.3 ± 0.1°C).
(calcitic lime [CL], natural hydraulic lime [NHL]) presents a high surface specific area
(SSA: 5–9 m² g–1) due to the very fine lime and pouzzolana addition. Nevertheless,
SSA of ready-to-use grouts and especially the PLM product is still higher because the
use of fine micronized silica (>100 m² g–1) still increases external surfaces and the glo-
bal SSA of this grout (10.1 m² g–1). These additives fill the intergranular pore spaces
that significantly reduce the average pore radius <r> of the materials (Table 1). Accord-
ing to the Kelvin law, the pore size <r> in which condensation can occur is proportional
to 1/RH. Exposed to high relative humidity of up to 95% RH, vapour adsorption capac-
ity of the injection grouts increases as the pore network structure is more microporous.
Structural properties and composition could explain the large hygric dilation of the
PLM product which differs from the LEDAN product by (i) the rate of water vapour
538 J.-D. Mertz et al.
adsorption and (ii) the final dilation coefficient value (Figure 12). The inverse correla-
tion between specific surface area and average pore size justifies the different hygric
swelling kinetic of these products.
Thermal behaviours show large differences between home-made mortars and grouts.
The ready-to-use products present a higher mechanical strength and develop a moderate
final dilation (5 to 10 × 10–6 °K–1) close to the stones (Figures 12 and 14). In contrast,
home-made mortars (Figure 13) are characterised by a high dilation value (αth= 10 to
15 × 10–6 °K–1) but a slow dilation kinetic. The gradual expansion could be the result
of both the porosity and the weak cohesion of the mortars, reducing heat conductivity
at grain boundaries due to the dilation contrast between the trapped air (36 to 37 × 10–6
°K–1) into the pore and the minerals.
Direct analysis of the plotted dilation data based on the αth and ɛhyg calculated coef-
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60
CL
NHL 40
50
Thermal expansion (µm)
40
Temperature (°C)
30
30
20 20
10
10
0
-10 0
0 50 100 150 200 250
Time (h)
Figure 13. Comparative thermal dilation of the mortars CL (black curves) and NHL (grey
curves) (open circles: temperature; 2 < RH < 4%).
European Journal of Environmental and Civil Engineering 539
60
PLM 40
50
LEDAN
Temperature (°C)
30
30
20 20
10
10
0
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-10 0
0 50 100 150 200 250
Time (h)
Figure 14. Thermal dilation of the injection grouts PLM-M (grey curves) and LEDAN (black
curves). (open circles: temperature; 2 < RH < 4%).
18
16
Thermal dilation coefficient
14
12
α th (10 /°K)
10
-6
8
DJ
6 LEDAN
PLM
4 NHL
2 CL
V
0
0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6 1.8 2
-3
Hygric dilation ε hyg (10 )
Figure 15. Dilation coefficient values of the materials (ɛhyg calculated for ΔRH = 85%).
when the adherence of the mortars is low (< 0.08 MPa). Conversely, the tested injection
grouts and the calcarenite (V) are not really affected by temperature because their T-val-
ues are not realistic in natural environments. They are mainly reactive to air moisture
despite the arid climatic conditions in the Djemila and Volubilis sites. This static analy-
sis underlines the importance of dilation parameters which are generally missed in the
data sheet of the products.
7. Conclusion
Expansion of stones and mortars likely to be used for the treatment of cracked rocks
was carried out during controlled temperature and humidity changes. Unidirectional
540 J.-D. Mertz et al.
180
Thermo-
160
hygric
140 threshold
120 (°C)
100
80
60
40
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20
0
Dj CL NHL LEDAN PLM V
Acknowledgement
The research was supported by the UE project MEDISTONE n°015245 FP6-INCO-MPC2.
References
Al-Saad, Z., & Abdel-Halim, M.A.H. (2001). Laboratory evaluation of various types of mortars
for the conservation of Qsar al-Bint monument, Petra-Jordan. Engineering Structures, 23,
926–933.
Baudran, A. (1969). Conception et réalisation d’un dilatomètre absolu enregistreur pouvant foncti-
onner à haute température en atmosphère contrôlée. Utilisation pour l’étude du comportement
de minéraux argileux. Bulletin de la Societe Francaise de Ceramique, 82, 3–48.
Benavente, D., Cultrone, G., & Gomez-Heras, M. (2008). The combined influence of mineralogi-
cal, hygric and thermal properties on the durability of porous building stones. European Jour-
nal of Mineralogy, 20, 673–685.
Binda, L., Baronio, G., Marrochino, E., & Vaccaro, C. (2004). Chemical and mineralogical char-
acterization of historic mortars in Ferrara (northeast Italy). Cement and Concrete Research,
34, 1471–1475.
European Journal of Environmental and Civil Engineering 541
Brimblecombe, P., & Camuffo, D. (2003). Long term damage to the built environment. In P.
Brimblecombe (Ed.), The effect of air pollution on the built environment. Air pollution
reviews (pp. 1–30). London: Imperial College Press.
Bromblet, P. (2000). Evaluation of the durability and compatibility of traditional repair lime-based
mortars on three limestones. International Journal for Restoration of Buildings and Monu-
ments, 6, 513–528.
Cooper, H.W., & Simmons, G. (1977). The effect of cracks on the thermal expansion of rocks.
Earth and Planetary Science Letters, 36, 404–412.
Delgado-Rodriguez, J. (2001). Swelling behaviour of stones and its interest in conservation. Mate-
riales de Construccion, 51(263–264), 183–195.
Dessandier, D., Antonelli, F., Bouzidi, R., El Rhoddani, M., Kamel, S., Lazzarini, L., Leroux, L.,
& Varti-Matarangas, M. (2008). Atlas of the ornamental and building stones of Volubilis
ancient site (Morocco). BRGM (Ed.), final report RP-55539-FR, 170p.
Dessandier, D., Antonelli, F., Hamiane, M., Khalfallah, C., Lazzarini, L., Leroux, L., Riache, C.,
Downloaded by [University of Prince Edward Island] at 09:26 15 April 2013
Taoutaou, H., & Varti-Matarangas, M. (2008). Atlas of the ornamental and building stones of
Djemila ancient site (Algeria). BRGM (Ed.), final report RP-56277-FR, 171p.
Dessandier, D., Bromblet, P., & Mertz, J.-D. (2000). Durability of tuffeau stone in buildings:
influence of mineralogical composition and microstructural properties. In V. Fassina (Ed.), 9th
International Congress on Deterioration and Conservation of Stone (vol. 1, pp. 69–78). Ven-
ice: Elsevier.
Franzini, M., Leoni, L., Lezzerini, M., & Cardelli, R. (2007). Relationship between mineralogical
composition, water absorption and hygric dilatation in the Macigno sandstones from Lunigi-
ana (Massa, Tuscany). European Journal of Mineralogy, 19, 113–123.
Gascon, F., & Balbas, M. (1986). Modelo tensorial en la dilatacion lineal termica anisotropa de
marmoles. Boletin Geoologico y Minero de España, 97, 793–802.
Grasley, Z.C., & Lange, D.A. (2007). Thermal dilation and internal relative humidity of hardened
cement paste. Materials and Structures, 40, 311–317.
Henriques, F.M.A. (2004). Replacement mortars in conservation: an overview. In D. Kwiatkowski
& R. Löfvendahl (Eds.) Proceedings of the 10th International Congress on Deterioration and
Conservation of Stone, vol. II (pp. 973–983). Stockholm, 27 June–2 July 2004.
Hirschwald, J. (1912). Handbuch der bautechnischen Gesteinsprüfung. Berlin: Borntraeger.
Jimenez-Gonzalez, I., Rodriguez-Navarro, C., & Scherer, G.W. (2008). Role of clay minerals in
the physicomechanical deterioration of sandstone. Journal of Geophysical Research, 113,
F02021. doi: 10.1029/2007/JF000845.
Jimenez-Gonzalez, I., & Scherer, G.W. (2006). Evaluating the potential damage to stones from
wetting and drying cycles. In M.S. Konsta-Gdoutos (Ed.), Measuring, Monitoring and Model-
ing Concrete Properties (pp. 685–693). The Netherlands: Springer.
Kalagri, A., Miltiadou-Fezans, A., & Vintzileou, E. (2010). Design and evaluation of hydraulic
lime grouts for the strengthening of stone masonry historic structures. Materials and Struc-
tures, 43, 1135–1146.
Kleber, W. (1959). Einführung in die Kistallographie. Berlin: VEB Verlag Technik.
Knöfel, D., & Schubert, P. (1993). Mörtel und Steinergänzungsstoffe in der Denkmalpflege. Ber-
lin.
Lubelli, B., van Hees, R.P.J., Huinink, H.P., & Groot, C.J.W.P. (2006). Irreversible dilation of
NaCl contamined lime-cement mortar due to crystallization cycles. Cement and Concrete
Research, 36, 678–684.
Maurenbrecher, A.H.P., Trischuk, K., Rousseau, M.Z., & Subercasseaux, M.I. (2007). Les mor-
tiers de rejointoiement pour la conservation des maçonneries anciennes (Rapport de recher-
che 225), March 2007. Ottawa, Canada, KIA OR: Institut de recherche en construction et
CNRC.
Mertz, J.-D. (2007). Salt damage, dilation and actual practices in sandstone conservation. In
Dombaumeistertagung in Strassburg : Tagungsdokumentation, Strasbourg, october 10–14,
2006. Fondation de l’Oeuvre Notre-Dame, 2007, 153–156.
Meyers, S.L. (1950). Thermal expansion characteristics of hardened cement paste and of concrete.
Proceedings of the Highway Research Board, 30, 193.
Ondrasina, J., Kirchner, D., & Siegesmund, S. (2002). Freeze-thaw cycles and their influence on
marble deterioration: a long-term experiment. Geological Society of London, Special Publica-
tions, 205, 9–18.
542 J.-D. Mertz et al.
Rozenholtz, J.L., & Smith, D.Z. (1949). Linear thermal expansion of calcite, var. Iceland spar and
Yule marble. American Mineralogist, 34, 846–854.
Ruedrich, J., Kirchner, D., Seidel, M., & Siegesmund, S. (2005). Deterioration of natural building
stones induced by salt and ice crystallisation in the pore space as well as hygric expansion
Processes. In Siegesmund, S., Auras, M., Ruedrich, J., & Snethlage, R., (Eds.) Geowissens-
chaften und Denkmalpflege. Zeitschrift deutsche Geologische, 156(1), 59–73.
Ruedrich, J., Seidel, M., Rothert, E., & Siegesmund, S. (2007). Length changes of sandstones
caused by salt crystallisation. In R. Prikryl & B.J. Smith (Eds.), Building Stone Decay: From
Diagnosis to Conservation. Geological Society, London, Special Publications, 271, 199–209.
Sasse, H.R., & Snethlage, R. (1996). Methods for evaluation of stone conservation treatments, In
N.S. Baer & R. Snethlage (Eds.) Saving our architectural heritage: The conservation of his-
toric stone structures (pp. 223–243). (Report of the Dahlem Workshop), Berlin, 3–8 March
1996.
Sebastian, E., Cultrone, G., Benavente, D., Rodriguez-Navarro, C., & Linares, L. (2008). Swelling
Downloaded by [University of Prince Edward Island] at 09:26 15 April 2013