You are on page 1of 8

LIME-METAKAOLIN MORTARS APPLIED

ON THE SOLEDADE PALACE, RECIFE,


BRAZIL.
Bonilla, Tamara M. de A1 , Ferreira, Ana Florinda2, Nóbrega, Aline F3, Silva,
Elaine C. da R4, Souza, Marília L. de5 and Carneiro, Arnaldo M. P.6
1
Universidade Federal de Pernambuco, Brazil. tamara.bonilla@gmail.com
2
Universidade do Porto, Portugal. anaflorinda@hotmail.com
3,4,5,6
Universidade Federal de Pernambuco, Brazil. ampc@ufpe.br

Abstract
The purpose of this work was to evaluate lime mortars with pozzolanic addition of
metakaolin that were applied as plasters on original masonries of Soledade Palace,
architectural heritage of Recife, Brazil. The study involved the following
variables: 1. Application over internal/external substrates; 2. Substrates with/
without a lime-sand coat to increase brick-mortar bond; 3. Three proportions of
mortars; 4. Use of dry slaked lime or of matured lime putty. The mortars were
evaluated in function of its mechanical strengths and of brick-mortar bond. Results
indicated that these mortars are appropriate to be used in building restoration
works, since being prepared observing standards and good practices of execution
and applied in accordance with adequate techniques of restoration. Thus, these
mortars will be able to assure the integrity and durability of ancient masonries.

1 Introduction

This paper presents results of studies conducted by the Department of Civil


Engineering, Federal University of Pernambuco, with the Institute of National
Historical and Artistic Heritage, aiming to evaluate lime-metakaolin mortars for
restoration works. Studies included plasters applied based on the usual procedures
of the civil works on the secular brick masonry of Soledade Palace, Recife,
Pernambuco, Brazil. Built in the seventeenth century and modified over the
centuries, it was transferred to become IPHAN's regional headquarters and offered
by this Institution for study purposes during the restoration works and retrofitting.

2 Methodology

The performance evaluation of lime mortars involved the following steps:


 Planning - definition of traits and forms of application, calculation of the
amount of materials to be used;
 Production, implementation and evaluation - substrate preparation, preparation
of mortars, guidance applications, preparation of specimens and follow up for
90 days, age of the flexural bond strength test; implementation and evaluation
of mechanical strength tests and bond strength of the mortars.

2.1 Materials

The lime used here is classified as CH-I, and must have a maximum of 5% CO2
and 10% of unhydrated oxides [1], and minimum content of 88% of total oxides of
non-volatile basis (CaO + MgO) [6]. This is magnesian lime from dolomitic
limestone of the State of Paraiba.

Table 1. XRF of slaked lime.

Óxide MgO Al2O 3 SiO 2 P2 O5 SO 3 Cl K2 O CaO TiO 2


% 16,1 0,98 2,07 0,0534 0,0459 0,0362 0,17 79,7 0,105
Óxide MnO Fe2O 3 SrO ZrO 2 TOTAL
% 0,0314 0,667 0,0438 0,0168 100,0195
Source: NegLabise - DEGEO⁄UFPE.

The metakaolin utilized is extracted and processed in the State; its color is
white to favor the coloring of the plasters, which, after drying showed shades of
gray according to the proportion of lime used. Table 3 presents data obtained from
the manufacturer’s technical information on pink metakaolin.

Table 2. XRF of Metakaolin.

Óxide MgO Al2 O3 SiO2 P2 O5 SO3 Cl K 2O CaO TiO2


% 0,20 41,70 51,10 0,17 0,08 -- 1,54 0,13 0,61
Óxide MnO Fe2O 3 SrO ZrO 2 Rb2 O Y2 O3 Ga2O3 PbO TOTAL
% 0,04 4,28 0,03 0,04 0,02 0,03 0,02 0,03 100,02
Source: NegLabise - DEGEO⁄UFPE.

Table 3: Physicochemical properties of metakaolin


Property Values Property Values
Retention: ASTM# 200 sieve 1% Loss on ignition (L.O.I) < 2%
Blaine Fineness 1.500 m2/kg SiO 2+Al2O3 (average value) 91%
Specific Mass 2.560 Kg/m3 Fe2 O3+TiO2 (average value) 4.7%
Apparent Mass 480 Kg/m3 Pozzolanic Activity Index 900 mg
Color Pink (Modified Chapelle-IPT) Ca(OH) 2/g
Source: Manufacturer

The washed sand was the same as that used for the coatings of the works,
sieved in a 4.8 mm mesh. Quartz sand, maroon, with mica, without apparent
organic contamination, maximum diameter of 1.2 mm and 45% of particles
between 0.6 and 0.3 mm.
2.2 Substrates

The tested walls were those in the lower floor of the monument, which
underwent less interventions and different sunlight conditions, ventilation and
wetting: three walls of the main façade (SW) that were given six panels and six
different internal walls, sheltered from sunlight and ventilation.
The masonry has irregular surfaces and joints (consequent irregular thickness
of the plastering) with thickness ranging from 50 ± 5cm, and between 2 and ± 0.5
cm respectively, composition that uses irregular solid bricks: 20 ± 1 cm long, 10 ±
1 cm wide, and 5 ± 1 cm thick; colors vary from light yellow to dark red, spotted,
some have breakdowns, especially in damp walls resulting from infiltration.

2.4 Experimental Procedure

The research involved the following variables: 1. Mortars of three different mix
proportions, 2. Utilization of dry slaked lime or matured lime putty; 3. Application
of plasters on internal or external substrates, and 4. Application on clean substrate
or on substrate prepared with lime-sand roughcast. Three types of mix proportions
(in weight) were determined: type I–1:1:4, type II-1:1,04:11,07 and type III-
1:1,64:16,60 defined by previous Department experimental results. Water was
added by mason in the amount needed for the consistency of the plasters. The
hydrated lime was mixed with water to a pasty and smooth consistency, for a
seven-day maturation. For the application, 1m2 panels were placed on the walls
removing the non-original plasters, then washed for wetting and removal of
dustiness. Each panel received the three mix proportions of mortar in horizontal
stripes, in ascending order of the binder content. Mortar preparation followed the
following procedure: Weighing of materials: sand; metakaolin; matured or
unmatured hydrated lime; manual mixing of dry materials on an impervious
surface; gradual adding of water or previously weighed matured lime putty, and
manual homogenization until the point of consistency indicated by the mason. The
mortars were applied at the same thickness of the existing plasters (2 to 4.5 cm)
using the usual procedures for civil works, that is, in two layers by using the
masons trowel, capping with aluminum slats and finished with a wooden concrete
finishing trowel and a sponge. In the experiments, the local climate was tropical
summer: intense sunlight, warm, occasional and intense short-duration showers,
average temperature 30°C, and average relative air humidity of 70%. Mortars
were evaluated in three ways:
 At the monument, during application using qualitative observations:
homogenization, appropriate consistency for the application, instant adhesion
to substrates, ease of finishing, and initial shrinkage.
 At the DECIV/UFPE laboratory, using tests, to determine the mass loss rate
up to 90 days and mechanical strength at the age of 180 days.
 At the monument, after 90 days, using assays to test mortar binding with
analog equipment threaded to aluminum plates bonded with epoxy adhesive to
the surface of the coatings, which were previously cut with a diamond hole saw
coupled to an impact drill.

3 Outcome Analysis

 At the monument during the implementation


During mortar batching, the mixture of sand and metakaolin using dry slaked
lime was easier than the mix using matured lime, as it formed lumps of lime that
were hard to mix. Matured lime mortars presented more cohesion and plasticity
favorable to their application; however, mix proportions with higher binder
content of both types of lime adhered to the tools, hampering application and
finishing. The rapid loss of consistency due to metakaolin reactivity forced the
reduction of mortar setting times before their application and drying for leveling
purposes. The evaluation of the coating shrinkage was empirical; the cracking of
the coating was observed on the 90th day in terms of both number and opening of
the cracks. In the beginning, all panels apparently had an excellent interface with
the existing mortar, and no significant cracking on the coating edges was found.
However, all panels cracked at the interface of the different settings. Right after
the application, all coatings presented capillary cracking.
 At the DECIV/UFPE laboratory
The rate of mass loss indicates the water retention capacity of the mortars; the
graphs in Figures 1 and 2 relate the rate of mass loss (dm/dt) with time (days). The
rate of mass loss is achieved during a time t in days, using coefficient dm/dt = (m0
– md)/m0,where mo (initial mass on the day of the removal of the specimen from
the mold), md m (mass on any d day). In mortars produced with dry slaked lime,
the rate of mass loss in mortars I, II and III is similar at the first ages, and differs
from the 14th to the 28th day, where water retention is lower in mortar III, with
contains less binder; in mortars I and II, this rate is similar over this period,
showing the impact of lime in mortar water retention. From the 28th day, mortars I
and III present rates of mass loss similar to and higher than mortar II, which
indicates an optimal content of hydrated lime for the latter binder:aggregate ratio.
In mortars with matured hydrated lime, their behavior is similar to the previous
ones: up to the 14th day, the rate of mass loss is similar for all three proportions,
and from the 14th to the 28th day, the mortar I has a lower rate, but the rates of
mortars II and III are similar to and higher than those of the mortar I due to a
higher content of matured lime, which contributes to water retention. From the
28th day, the three mortars show no significant differences in the rate of mass loss,
which indicates that the maturation of lime contributes to water retention at older
ages, despite the difference in binder amount. Comparing the range of the rate of
mass loss between the matured and unmatured groups of lime, both are in the
range between 0.0 and 0.18. The mortars with greater water retention favor
hydraulic hardening reactions with metakaolin [8].
Fig. 1. Mass loss. Dry slaked lime mortars. Fig. 2. Mass loss. Matured lime putty.

Test results of flexural and compressive strengths are listed in Table 4, with the
following identification: application stage (1-first, 2-second), type of lime (nM-
dry slaked lime, M-matured lime putty) and mix proportion (I, II, III).

Table 4. Characteristics of Mortars and Mechanical Strength at 180 days.


Mortar Proportion w/d.m. w/b b/ag. fc (MPa) f t (MPa)
1nM III 1 : 1,64 : 16,6 0,21 1,60 0,15 0,82 0,13
1nM II 1 : 1,04 : 11,07 0,20 1,06 0,23 0,75 0,36
1nM I 1:1 : 4 0,25 0,66 0,60 6,42 2,49
2M III 1 : 1,64 : 16,6 0,21 1,55 0,17 0,39 0,16
2M II 1 : 1,04 : 11,07 0,21 1,10 0,25 1,82 0,53
2M I 1:1 : 4 0,31 0,92 0,53 4,75 0,75
2nM III 1 : 1,64 : 16,6 0,23 1,70 0,16 0,48 0,26
2nM II 1 : 1,04 : 11,07 0,21 1,08 0,24 1,71 0,78
2nM I 1:1 : 4 0,28 0,85 0,50 4,75 0,75

It was found that the lime maturation variable was not determinant of the
outcomes, though better results were expected for the mix proportions using
hydrated and matured lime, since magnesium limes may contain remaining
magnesium oxides, the hydration of which is more complex than calcium oxides
[6,8]. The variables that determined higher mechanical strengths were the higher
binder amount and the lower water amount, as demonstrated by water/dry
materials, water/binder and binder/aggregate ratios (Table 4); it is more
perceptible in type I mortars that presented significant outcome variability: mortar
1nM I presented higher mechanical strengths (lower w/d.m. and w/b ratios and
higher b/ag ratio). The values obtained for compressive and flexural strengths are
similar to the literature values for lime and metakaolin mortars with similar
proportions and w/b ratios [4].
 In the building after 90 days
Shrinkage. The internal coatings of types I and II presented a larger number
and a wider opening of the cracks, as compared to the external cracks. Generalized
cracking and mean openings of 6mm in the typical form of clay mineral shrinkage
(“alligator leather”). Coatings type III presented capillary cracking (<2mm) on the
external panels, and a smaller number, a smaller opening and a different format
(slanted) when compared to types I and II on the internal panels.
The flexural bond tests outcomes are listed in Table 5; the identification of
the panels refers to the stage of application (1-first, 2-second), the location of the
substrates (E-external, I-internal), lime ( nM-unmatured, M-matured); substrate
treatment (sC-no roughcast, C-roughcast) and mix proportion(I, II, III). The
indicated tension represents the mean fracture tension. Column Pts. indicates the
number of valid/lost points and column Break indicates where the flexural cut
occurred: A-plaster; S/A-substrate-plastering interface; S-substrate [2].

Table 5. Results of Flexural Bond Tests at 90 days.


Panel ft (MPa) Pts. Rupture Panel f t (MPa) Pts. Rupture
1E-nMsC I 0,6497 13 / 0 11-A/ 2-S/A 1I-nMsC I 0,1680 3/0 1-A/ 2-S/A
II 0,4419 9/0 6-A / 3-S/A II 0,1182 3/0 2-A/ 1-S/A
III 0,1850 8/1 7-A / 1-S/A III 0,0935 2/0 2-A
2E-MC I 0,3221 3/0 3-A 2I-MC I 0,2390 2/2 2-A/ 1-S/A
II 0,0935 1/0 1-S/A II 0,1668 2/1 1-A/ 1-S/A
III 0,0935 3/0 2-A / 1-S/A III 0,0935 3/1 3-A
2E-MsC I 0,5349 2/0 2-A 2I-MsC I 0,2567 3/0 3-A
II 0,1669 4/0 3-A / 1-S/A II 0,1400 1/2 1-A
III 0,1426 1/3 1-A III 0,0935 1/2 1-A
2E-nMC I 0,6186 3/0 2-A / 1-S/A 2I-nMC I 0,4369 1/2 1-A
II 0,3151 2/0 1-A / 1-S/A II 0,1584 3/0 1-A/ 2-S/A
III 0,2078 3/0 3-A III 0,0935 1/2 1-A

In these tests, mortars I and II (matured or unmatured) showed high surface


resistance, which caused difficulties to the tubular cutting, but lower strength and
internal cohesion; mortar III was the least resistant and friable both on the surface
and internally. In other words, in mortars I and II, the high binder amount and the
low incorporation of air in the manual mixing did not favor the carbonation of the
matrix. Being hardly porous, it did not allow an appropriate CO2 diffusion inside.
Surface resistance comes from the carbonation of the surface and from the binder
film. External plasters had higher bond strengths and this, along with lower
shrinkage, shows that the curing of the external panels was more efficient. As to
the types of ruptures, 60 of the 77 tested points underwent cohesive mortar
rupture, while the remaining points had adhesive rupture at the substrate/mortar
interface. As the outcomes of flexural bond strength tests show that the mortars
are cohesive, it can be said that the mortar break indicates that substrate/mortar
interface bond is higher than the mortar strength, which means that the adherence
of these mortars to the old masonry was efficient. However, it is not possible to
state that the roughcast variable had an impact on these results, as there was
cohesive rupture in most of the points of the roughcast panels. So, it is believed
that the location of the panels was a direct determinant of brick-mortar bond
regarding the roughcast variable.
4 Conclusions

From the outcome analysis of the three stages, it appears that:


As to the implementation, it is necessary to realize the peculiarities of lime-
metakaolin mortars and the difference between working with them and with
portland cement mortars, especially when conducting restoration works. The usual
procedures for civil works should be reviewed and adapted to features such as
lower plasticity [3], rapid hardening, different application and performance
requirements such as adherence, waterproofing without sealing, and durability.
These mortars require careful homogenization for the proper incorporation of air
that, in addition to improving the involvement of the aggregate grains by the
cement [3], will also provide plasticity at a lower w/b ratio. The control of the
materials (type and quality of lime, grain size and sand quality), as well as the
amount of water, are essential to promote the development of pozzolanic and
carbonation reactions to form a cohesive and wholesome cement matrix.
As to shrinkage, the maturation variable was not decisive for cracking,
presenting no significant differences as to the results. The panel location variable
was crucial, as the external panels presented less cracking and width than the
internal ones, that is, the setting of the latter was more efficient, and this can be
explained because, in general, the mortars were prepared based on a high m/w
ratio, and on the panels exposed to the afternoon sunlight there was evaporative
water loss, which did not occur inside the building. The binder content variable
was fundamental, as mortars types I and II cracked more frequently and presented
wider widths than type III. Other significant factors for the cracking of the panels
were the use of fine and misgraded sand, which neither promoted an efficient
internal carbonation, nor the expulsion of the water unnecessary for the hardening
reactions [7], and the width of the coating layers (~4.5cm) that should have been
applied in thin layers to allow the mismatching of the cracks [3]. The mass
variation results corroborate the comments on the empirical shrinkage, as the
mortar presenting the greatest mass variation also cracked more, in terms of
quantity and width (I-nM).
As to bonding, the numerical values of the proportion I bond strength were
compared with values reported in the literature, shown in the table below. The
results were compared to the results of mortars of the same proportion, dry slaked
lime, similar w/b ratios and different compositions: two mix proportions [3]
consisting of lime:natural pozzolan:sand and lime:kaolin at 800°C:sand; and a mix
proportion [5] consisting of lime:ground ceramic:sand. As benchmarks, we
considered the adherences obtained from the portland cement mortar used in the
plasters of the work (IPHAN); another portland cement mortar [9] and, finally, old
mortars [5], consisting of lime:natural clay:sand ("bastard" mortars) proportions of
1:0,3:0,1 to 1:3,4:1. The substrates were called 'M' (modern, ceramic bricks), and 'A'
(ancient, solid bricks, stone-filled joints in [5]). Portland cement mix proportions used
roughcast. Adherences of mortar I had results superior to the adherence values of
experimental mortars found in the literature [3,5] and above the values of
compared portland cement mortars [9], and this shows good adherence to the
substrate and shows the strength of the studied cement. Comparing to the
adherence data of the old mortars [5], the values are also superior to the values of
the latter, noting that the old mortars came from the ruins of façades [5].
Table 6. Comparison - Actual flexure bond versus the literature
Data Proportion Comp. w/b Substrata ft (MPa) Rupture Age (d)
Obt 1:1:4 sl:mk:s 0,66-0,92 A (E) 0,32 - 0,65 m – s/m 90
Obt 1:1:4 sl:mk:s 0,66-0,92 A (I) 0,17 - 0,44 m – s/m 90
[3] 1:1:4 sl:k:s -- M (I) 0,05 - 0,15 s 60
[3] 1:1:4 sl:np:s -- M (I) 0,06 - 0,13 s/m 60
[5] 1:1:4 sl:cc:s 1,32 A (E) 0,03 - 0,05 m 34
Obt 1:1:8 iphan pc:sl:s -- A (E/I) 0,19 - 0,39 s/m – s >28
[9] 1:6 pc:s 1,22 M (E) 0,23 - 0,56 m – s/m >28
[5] diversos lp:cl:s -- A (E) 0,03 - 0,31 m – s/m ∞

So, in order to be used in restoration works, it is necessary to examine the


original mortars and assess the use of mix proportion I for plastering, to avoid
problems of differential stiffness between the mortars and the old substrate.
Regarding mix proportions II and III, these had lower values than I, and higher
than the mix proportions in the literature [3,5] and than the old mortars [5],
approaching values of portland cement mortars, while mix proportion III proved
little cohesive. Therefore, mortar II suggests greater potential to be used in
restoration, as long as they are well prepared.

4 Acknowledgments
The authors would like to thank Unimin do Brasil for donating the metakaolin; to the staff of
Cifra Engenharia for the helpful contribution, and to Ayrton Farias for translating this paper.

5 References

1. ABNT (2003). NBR 7175:2003. Cal hidratada para argamassas. ABNT, Rio de Janeiro.
2. ABNT (2005) NBR 15258:2005. Argamassa para revestimento de paredes e tetos.
Determinação da resistência potencial de aderência à tração ABNT, Rio de Janeiro
3. Faria Rodrigues, MPSF (2004) Argamassas de revestimento para alvenarias antigas.
Contribuição para o estudo da influência dos ligantes. Universidade Nova de Lisboa.
http://hdl.handle.net/10362/1129. Accessed 07 june 2009.
4. Fortes-Revilla C, Martínez-Ramírez S, Blanco-Varela MT (2006) Modelling of slaked-lime
metakaolin mortar engineering characteristics in therms of process variables. Cement and
concrete composites 28:458-467. www.sciencedirect.com. Accessed 02 march 2009.
5. Góes ES (2006). Análise da resistência de aderência à tração para uso em edificações
históricas. UFBA, Salvador.
6. Guimarães JEP (2002). A Cal. Fundamentos e aplicações na Engenharia Civil. PINI, S. Paulo.
7. Margalha MG, Veiga MR, Brito J. Influência das areias na qualidade de argamassas de cal
aérea. http://conservacal.lnec.pt/pdfs/GORETI_Areia_APFAC.pdf Accessed 31 may 2009.
8. Rago F, Cincotto MA (1998). Influência do tipo de cal hidratada na reologia de pastas.
EPUSP, São Paulo.
9. Santos, HB (2008) Ensaio de aderência das argamassas de revestimento. UFMG, B.Horizonte.