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Lime Mortars Containing Ceramic Material as Pozzolan
Written By
Leane Priscilla Bonfim Sales, Aline Figueiredo da Nóbrega, Iranilza Costa da Silva, Ana Cecília Vieira da Nóbrega, Arnaldo Manoel Pereira Carneiro, Fabiola Luana Maia Rocha and Diego de Paiva Bezerra
Submitted: 28 June 2023Reviewed: 28 June 2023Published: 29 November 2023
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Lime mortars have been indicated for restoration and conservation interventions in historic buildings, however, the slow hardening of these mortars does not favor their use and dissemination in construction areas. The inclusion of pozzolans improves these properties, and although the results achieved are not close to those found in conventional cementitious mortars, they are seen as compatible materials for restoration services, since they present moderate mechanical responses and chemical compatibility. This chapter aims to show the impact of different pozzolans on fresh and hardened lime mortar’s properties, including mechanical, rheological, and microstructural properties. In addition, an overview of historical mortars is presented.
Federal University of Paraíba, João Pessoa, Brazil
Aline Figueiredo da Nóbrega*
Federal University of Paraíba, João Pessoa, Brazil
Iranilza Costa da Silva
Federal University of Pernambuco, Recife, Brazil
Ana Cecília Vieira da Nóbrega
Federal University of Rio Grande do Norte, Natal, Brazil
Arnaldo Manoel Pereira Carneiro
Federal University of Pernambuco, Recife, Brazil
Fabiola Luana Maia Rocha
Federal University of Paraíba, João Pessoa, Brazil
Diego de Paiva Bezerra
Federal University of Paraíba, João Pessoa, Brazil
*Address all correspondence to: alinefnobrega@hotmail.com
1. Introduction
Among materials found in secular constructions, lime mortars stand out and were used until at least the beginning of twentieth century [1]. Studies that analyze the coatings of old buildings show that not only aerial lime was found, but also natural hydraulic lime and lime with the addition of pozzolans [2, 3, 4].
The use of lime in mortars has been rescued and is indicated in restoration interventions in historical buildings to ensure physical and chemical compatibility of new mortars, with respect to old ones [5, 6]. This is because using Portland cement in restoration and conservation works presents incompatibilities, in view of its different characteristics in relation to original mortar, such as high rigidity, low porosity and presence of alkaline hydroxides that can react forming soluble salts [7]. Such characteristics lead to pathologies such as fissures and efflorescence.
Lime mortars have some disadvantages compared to those produced with Portland cement, such as lower mechanical strength and very long hardening time [8]. Studies show that lime and pozzolan mixture implies changes in setting and hardening mechanism and in rheological responses, as well as in improvement in performance regarding water permeability, durability and mechanical resistance [6, 9, 10, 11].
There is evidence of use of volcanic ash and ground ceramic fragments as natural pozzolans throughout history and it was associated with obtaining resistant and durable mortars [12], but in recent works, metakaolin is among the most used pozzolans in lime-based mixtures, justified according to authors by its high pozzolanic activity [5, 6, 8, 9, 10, 13, 14, 15, 16] and Veiga et al. [17] reinforces that lime mortars added with pozzolans in general are chemically and physically compatible with old mortars, having a similar composition and ability to accommodate the movement of masonry structures.
Throughout the useful life of a structure, there is inevitably a need for conservation and restoration, in view of its exposure to environmental weather and wear due to human use.
Various types of binders were used in the past, some like clays and bitumen were ready to use, and others required heating and mixing with water before application [18]. Also according to the authors, aerial binders such as gypsum and lime were initially used. Then hydraulic binders came up, resulting from the calcination of impure lime or from the calcination of pure lime with materials with silica and alumina.
Thus, until mid-nineteenth century, lime was the main binder for laying and coating mortars and its use was frequent in ancient historical civilizations [19]. Veiga [20] mentions that aerial lime mortars are part of almost all old buildings and performed structural functions, when used in masonry blocks, to protective, adhesion and decorative functions, when used in plasters, laying mortars and paintings, respectively.
Currently, studies have been developed to know its properties from a technical point of view, recover lost technology and define application, mixing and maintenance techniques [19].
The application of mixtures based on currently conventional binder, Portland cement, presents, in conservation and restoration services in historical buildings, physical and chemical incompatibilities with original materials of structure [5], since it is associated with high mechanical resistance, high modulus of elasticity, low permeability to water vapor and the presence of alkaline hydroxides that can react forming soluble salts [7].
As for the use of cement in repairs to old buildings, Veiga [21] also points out other common drawbacks, such as the difference in surface texture and the way it reflects light, the presence of soluble salts that can be transported to interior of walls and crystallize, leading to element degradation as well as excessive stiffness and limited ability to allow wall to dry. Magalhães [22] presents old wall pathologies associating them with their possible causes.
Despite current imposition of productivity, reduction of costs and deadlines and absorption of non-specialized labor in the field of civil construction, conservation and restoration services demand care to avoid future pathologies. Compatibility between masonry materials and laying and coating mortars contribute to proper functioning of wall and increase its durability. In the past, the mix of materials for this purpose was based on local availability [23].
Therefore, in most severe cases of old coatings degradation, it is necessary to replace all original material with material that is close to previous one and that is durable [17], where the original material is usually lime-based mortars [5, 6].
Grilo et al. [15] point out that some properties are specific to lime-based materials, such as moderate mechanical properties, good performance in water vapor transmission and durability.
Veiga [21] compares performance of current and old external coatings mortars in terms of permeability. While currently, the focus is on ensuring walls watertightness, either by cutting capillarity in foundations, waterproofing and watertight window frames, the ancient walls were thick and porous and admitted water entry, but also allowed expulsion of water to be easy and fast.
Many times, the lack of knowledge about old mortars constitution and techniques applied for adequate restoration interventions lead those responsible for such services to adopt replacement of entire coating, which deprives building of its character and is a solution that presents a performance and durability inferior to that of pre-existing, as reported by Ref. [21].
This concept, in addition to being related to the conservation of history, is also linked to sustainability concept, since an inadequate solution can accelerate degradation process. The author emphasizes that it is necessary to understand degradation degree and know materials that makeup coating and their properties.
Given the current context, Sec [23] points out that it is important to encourage application of mortars compatible with existing walls, using products available on market and suitable for current situation.
Although in Europe, studies involving lime or lime and pozzolan mortars are vast [5, 6, 7, 8, 14, 16, 24, 25, 26], Veiga [20] states that lime-based mortars use is still rare in rehabilitation works and conservation of old buildings.
Veiga [20] attributes this to the need for scientific knowledge regarding local conditions and raw materials nature, lack of training on part of professionals to perform service, and difficulty of controlling planning in view of time required for application and drying of multilayers and waiting for favorable temperature conditions.
Lime can be aerial or hydraulic depending on the chemical composition of its raw material, limestone. Aerial lime, like any aerial binder, hardens by chemical reaction with carbon dioxide (CO2), and limestone to be burned at a maximum of 900°C must fundamentally consist of CaCO3 or CaMg(CO3)2 [23, 27]. Hydraulic lime, on the other hand, hardens in contact with water and is obtained through burning at about 1200°C of marly limestones that have up to 20% clay, and thus contain clayey compounds such as SiO2, Al2O3 and Fe2O3 [23].
Still from a raw material perspective, aerial lime can be calcitic when its main constituent is calcite (CaCO3); or dolomite when there is a high magnesium content in limestone and its main constituent is dolomite CaMg(CO3)2. Vinagre [27] mentions that European standard EN 459-11 (2011) determines that calcitic lime has at least 70% (by mass) of calcium oxide and magnesium oxide sum, with a maximum of 5% of magnesium oxide, and at least 55% of available lime, while dolomite must present 80% as a minimum value of these oxides sum, of which more than 5% correspond to magnesium oxide.
When limestone is subjected to burning/calcining, CO2 is released and the limestone becomes quicklime CaO (calcitic lime) or CaO + MgO (dolomitic lime). Lime can be marketed as such or hydrated, and depending on the slaking process, in powder or paste form [12, 27].
Hydraulic lime can be natural, when its raw material already has the aforementioned clayey compounds, or artificial, in a pre-defined mixture of calcium hydroxide, calcium silicates and calcium aluminates [23]. Thus, the mixture of lime and pozzolana can be seen as an artificial hydraulic lime.
The Portuguese standard [28] presents types and requirements of limes aimed at applications in civil construction field. This group includes aerial and hydraulic limes. Air lime hardens in carbon dioxide presence and hydraulic lime hardens in carbon dioxide and water presence, that is, there is carbonation and hydration reaction.
Lime with hydraulic properties is subdivided into three groups: natural hydraulic lime, formulated lime, and hydraulic lime [28]. The first is a consequence of burning more or less clayey or siliceous limestones, reduced to powder by slaking with or without grinding, but it should be noted that grinding is limited to 0.1%. Formulated lime is the result of mixing aerial lime or hydraulic lime with hydraulic or pozzolanic material and, hydraulic lime, is the product of mixing lime with other materials such as cement, slag, fly ash, limestone filler and others. All hydraulic limes are further classified according to their 28 days compression resistance.
Hydrated lime has the advantages of low drying shrinkage and good vapor permeability, but it also has disadvantages such as low initial strength, slow hardening (24–48 h), low water resistance and easy dissociation in humid environments, on the other hand, hydraulic lime has moderate strength, faster hardening speed (4–12 h), good water resistance and salt erosion resistance [29].
The state of the art is vast within limes field, in view of various types presented above and possibilities found throughout analysis of old constructions. Among studies found, there are works that evaluate historic buildings and identify materials present [30], while others are focused on the characterization of mixtures based on different types of lime in the fresh and hardened state; in this context, curing conditions, types of addition, proportion of materials, types of aggregates, use of additives, rheology, among others, are included as study variables.
Veiga [20] reviews aspects related to aerial lime mortars in an attempt to understand limitations of their use in restoration interventions. The author associates the mortar performance with lime type, carbonation degree, porosity, nature and size of aggregates present, among others. A survey of compressive strengths was carried out and shows that values vary between 0.3 and 1.6 MPa, depending on mortar composition, calcination level and slaking methods. Aspects regarding its application are also presented. Some of the limitations raised involve understanding short-term degradation factors, influence of local factors and management of lime time, either regarding appropriate environmental conditions for application or regarding the waiting time between layers application.
The binder: aggregate ratio in lime mortars ranges from 1:1 to 1:2.5, with 1:3 and 1:4 also being found, as stated by Veiga [20]. Still according to the author, the proportion of 1:3 in volume has been adopted as a reference. In fact, in [6, 9, 14], among the different proportions studied is 1:3. Nogueira et al. [31] also bring considerations about aggregates packaging and paste volume, differentiating thick and thin mortars, and point to proportions of 1:2.7 and 1:1.8, respectively.
About the mixing water, Seabra et al. [7] report that aerial lime paste demands a high water content, as it consists of small particles and therefore a high specific surface area. Bakolas et al. [32] and Azeredo [33] used a water/binder factor in pure lime and lime and metakaolin paste equal to 1.0.
Therefore, lime mortars have some drawbacks such as slow hardening, high shrinkage and low strength [8]. Such limitations are alleviated with the inclusion of pozzolans in their composition, providing lime mortars with improved performance in terms of water permeability, durability and mechanical resistance [9, 10].
The improved properties observed in lime and pozzolana pastes are associated with hardening reactions of these pastes that differ from lime pastes. While the former hardens by the simultaneous occurrence of carbonation and pozzolanic reaction, lime pastes react exclusively by carbonation. In the following topic, the conditions and mechanisms for the occurrence of reactions are presented, as well as the main compounds formed in these pastes.
The hardening mechanisms of these materials are different: while aerial lime pastes and mortars harden with air through carbonation, those using natural hydraulic lime or lime with pozzolana harden in contact with air and water, occurring simultaneously carbonation and hydration or pozzolanic reaction [34].
Lime pastes and mortars harden due to the reaction of calcium or magnesium hydroxide with carbon dioxide in the air, this reaction is called carbonation. The product formed from this reaction is calcium or magnesium carbonate, depending on the reagent. When pozzolan is added to aerial lime pastes and mortars, hardening is achieved through the pozzolanic reaction and carbonation, and the preponderance between the processes will depend on the curing conditions of the environment and lime composition.
Carbonation is controlled by carbon dioxide diffusion at the reaction site and the main factors involved in reaction are CO2 concentration, moisture content and permeability [27, 35]. The mechanism of the carbonation reaction is also presented by the authors in Figure 1. The carbonation reaction is very slow, it occurs from outside to inside of mass and takes about 6 months to 1 year, or depending on weather conditions, even longer [27].
Figure 1.
Mechanism of the carbonation reaction, according to Ref. [35].
The pozzolanic reaction is defined by calcium hydroxide with siliceous or silico-aluminous materials reaction in water presence and is controlled by siliceous phase dissolution that occurs in an alkaline medium [36].
Shi and Day [37] present the pozzolanic reaction mechanism in lime and pozzolan pastes which can be seen in Figure 2. Although mortars do not have significant resistance up to 3 days at 23°C, micrographs of this age shown by authors indicate that all pozzolan particles are covered by a layer of CSH gel.
Figure 2.
Mechanism of the pozzolanic reaction in lime and pozzolana pastes, according to Ref. [37].
Although Shi and Day [37] only mention C-S-H and hydrated tetracalcium aluminate (C4AH13) formation, the main compounds formed in mortars and lime and pozzolan pastes resulting from the pozzolanic reaction with calcium hydroxide are hydrated calcium aluminates and silicoaluminates such as stratlingite (C2ASH8), hydrogarnet (C3AH6), monocarboaluminate (C4ACH11), as well as C-S-H and C4AH13, [5, 6, 10, 14, 16], especially when pozzolan is metakaolin.
One of the most influential aspects in these compounds’ formation, in hardening process, and in mortars characteristics is their curing condition, as presented by Azeredo et al. [10]. In this work, the authors evaluated pastes lime and metakaolin behavior resulting from the calcination of kaolin residue cured at different relative humidities: 65% and 100%. The results showed that wet curing favored the pozzolanic reaction to the detriment of carbonation, and was the only one that formed stratlingite. Moist curing mortars reached higher strengths.
On the other hand, as a result of substitution proportions of lime by pozzolan, the produced mortar acquires less or more hydraulic properties and influences the speed of consumption of calcium hydroxide. Gameiro et al. [5] present the replacement of 50% lime with metakaolin as the best result regarding the extension of the pozzolanic reaction up to 180 days.
The inclusion of pozzolan and the consequent setting and hardening associated with the pozzolanic reaction produces compounds with better properties, such as resistance and hardening time [6, 38]. However, it is important to emphasize that this time is still slow in relation to Portland cement-based materials [39].
According to Ref. [23], in the past, pozzolans were classified as sand and, when they were mixed in lime mortars, gave them property of hardening under water. In the absence of natural pozzolans, from volcanic origin, Sec [23] mentions that sieved ceramic residues and “baked” clays were often used, and only in twentieth century, the use of fly ash and silica fume began.
As shown, pozzolans’ inclusion in lime mortars leads to simultaneous hardening by carbonation and pozzolanic reaction in moisture presence and improves properties such as durability and setting time.
Among pozzolans, it is observed that metakaolin is pozzolanic material commonly studied in lime and pozzolan mortars and pastes. It stands out for its pozzolanic activity and consequent significant improvement in properties of these mortars [5, 6, 8, 9, 10, 13, 14, 15, 16]. This pozzolan is derived from the calcination of kaolinite clay, between 600°C and 850°C [23].
However, there are studies that analyze mortars with lime and other ceramic materials as pozzolans, such as brick residue [40], expanded clay, rice husk ash, red brick dust and tile dust and yellow brick [41]. Besides, other materials are seen as blast furnace slag, fly ash [41] and nanosilica [26, 42].
5.1 Influence of pozzolans on lime mortars
5.1.1 Microstructural aspects
As seen, carbonation is responsible for calcium carbonate formation in lime mortars, however when there is a pozzolanic reaction, other compounds arise, resulting from this reaction and may vary according to mortar composition and curing conditions.
Azerêdo et al. [10] studied microstructural characteristics of hydrated lime pastes and calcined kaolin residue varying curing conditions and the lime: metakaolin ratio. The main phase formed in wet curing was stratlingite and in dry curing monocarboaluminate, in addition, wet curing and the highest content of metakaolin favored calcium hydroxide consumption. Wet curing also improved compressive strength of mortars [33]. Aspects related to setting and hardening mechanism of lime pastes and mortars were reviewed by Alvarezet al. [34].
The main compounds formed in lime and metakaolin mortars and pastes resulting from pozzolanic reaction with calcium hydroxide are hydrated calcium aluminates and silicoaluminates such as stratlingite (C2ASH8), hydrated tetracalcium aluminate (C4AH13), hydrogarnet (C3AH6), monocarboaluminate (C4ACH11), as well as hydrated calcium silicate (CSH) [5, 6, 10, 14, 16].
Moropoulou et al. [43] compared microstructural evolution of hydrated calcium silicate phase (C-S-H) in pozzolanic pastes. Powdered calcium hydroxide Ca(OH)2 was used as a reagent and, as a silicon source, silica fume or tetraethyl orthosilicate solution. The authors conclude that limiting factor in pozzolanic reaction rate is siliceous phase dissolution since CSH phase in pastes with silica fume was identified in less than 1 hour, but in pastes with tetraethyl orthosilicate in just 10 minutes.
5.1.2 Mechanical behavior
Velosa et al. [39] evaluated mortars with aerial lime, with aerial lime and three types of metakaolin and with cement. The results showed that there was an improvement in compressive and tensile strength and in modulus of elasticity in lime and metakaolin mixtures compared to pure aerial lime, but responses were still lower than cementitious mortar results. The authors also observed that, when comparing the three metakaolins used, the higher alumina content and the lower the alkali content, there were better mechanical results. The percentage of Al2O3 in metakaolins analyzed by authors ranged from 28 to 32%.
Veiga et al. [26] studied the application and performance of coating mortars with aerial lime and different materials, namely: hydraulic lime, white cement, natural pozzolan from Cabo Verde, metakaolin and silica fume, applied in recovery of old fortresses near the coast of Lisbon exposed to saline atmosphere, erosion by wave action, temperature variation and wind. From a mechanical point of view, in long term, in situ lime mortar panels with Cabo Verde pozzolan and metakaolin showed a behavior similar to that of lime and white cement mortar. Other characteristics such as resistance to water penetration and adhesion to substrate were satisfactory for mortars with metakaolin and Cabo Verde pozzolan, even though they were more permeable than those containing Portland cement. The silica fume, however, did not show enough mechanical resistance after 3 months and the authors report the lowest proportion used since they considered the highest reactivity. Thus, they suggest future studies with similar proportions for comparison.
In addition to metakaolin and Microsilica et al. [41] tested six other types of pozzolans: blast furnace slag, fly ash, expanded clay, rice husk ash, red brick dust, and tile and yellow brick dust. Among objectives of this work, in addition to comparing pozzolans performance in lime-pozzolana mortars, it sought to understand pozzolans properties and their effects on reactivity. Thus, it was observed that amorphicity is a preponderant factor for reactivity and improvement of mortar resistance, even more than silica content of the pozzolan. Of analyzed materials, metakaolin and blast furnace slag showed highest resistances, within same proportion of lime-pozzolana-sand (1:1:3 ratio). It should also be noted that metakaolin was included in pozzolans group with highest water demand, with a water/binder ratio (w/agg.) equal to 1.5, while slag was among those that required the lowest water content. (a/agl. = 0.5), and even so, metakaolin showed greater resistance.
Matias et al. [40] studied mortars with ceramic residues in different granulometries for replacement as a fine material and as an aggregate. The residues showed different pozzolanicity and consequently resulted in mechanical responses consistent with them, so the greater pozzolanic activity, the better mechanical resistance. Among the main conclusions, authors pointed out that even replacement of particulate matter such as sand proved to be a promising solution.
Table 1 presents mechanical behavior results of lime and lime and pozzolan mortars with regard to compressive and flexural strength and elastic modulus. It is emphasized that other data, with different composition ratios and test ages, can be found in respective works.
Mechanical behavior of lime and lime and pozzolan mortars.
It can be seen in Table 1, the difference in mortar resistance when volume or mass ratio was used, so that resistances were significantly increased in mass ratio, but regardless of this, insertion of pozzolans in mortar composition was generally accompanied by improvement in mechanical resistance.
5.1.3 Rheological behavior
With regard to the rheological characterization of lime and lime and pozzolana pastes, there are few studies. Fourmentin et al. [44] analyzed lime slurries and observed a better fit to the Herschel-Bulkley model, where fluid needs a flow stress to initiate flow and apparent viscosity decreases with increasing shear rate. Although in paper by Betioli et al. [45], cementitious pastes have better adjusted to model in question, they are usually characterized as Bingham fluids [46, 47, 48].
Sales et al. [11] observed that both lime and lime metakaolin pastes followed the same behavior. Additionally, the authors observed that presence of metakaolin reduced paste initial yield stress from 2 to 1 Pa and viscosity. In case of cementitious pastes that include pozzolanic additions, the behavior that best fits is also that of Herschel-Bulkley [45, 46, 47, 49, 50, 51, 52, 53, 54, 55, 56, 57].
Zhang et al. [58] studied aerial lime and metakaolin pastes for initial fluidity, macroscopic rheological properties, viscoelasticity and initial dissolution hydration. The authors varied water/binder ratio, the superplasticizer and metakaolin content. The superplasticizer increased fluidity. The pastes fitted Bingham and Herschel-Bulkley model. Also according to authors, variation in viscoelastic characteristics had more influence on water and superplasticizer content than on metakaolin content, so dispersion is more prominent than formation of the network structure of the lime-metakaolin pastes.
5.1.4 Influence of existing commercial additives
Arizzi and Cultrone [14] analyzed eight lime and metakaolin mortars with varying metakaolin content, proportion of binder: aggregate and different types of additives. The additives did not produce morphological and mineralogical changes in mortars, but they reduced necessary water content and, consequently, reduced porosity and increased resistance. Even so, an increase in metakaolin content stands out among variables analyzed and results in changes in the most significant properties.
A more recent study also shows lime mortars behavior with metakaolin and with nanosilica, another pozzolan with potential use in lime mortars [42]. The authors also incorporated three additives: an adhesion improver, waterproofing agent and viscosity modifier. The objective was to evaluate the influence of combination on several properties, such as fluidity, hardening time, adhesion, cracking, porous structure, resistance to freezing and durability. The general conclusion regarding additives was that nanosilica increased strength and durability while metakaolin improved adhesion and cracking.
Historical buildings require conservation and restoration services with compatible mortars, that is, similar to original materials. Prior to the emergence of Portland cement, the widespread binder was lime. In addition to lime, historical records also point to the use of pozzolans in old buildings, which justifies their use nowadays, along with the improvement in properties, such as hardening time and durability. Pozzolans also influence the setting and hardening mechanisms, the resulting chemical compounds and rheological aspects.
However, for its current use, studies have been carried out, since much knowledge of practice and construction techniques was lost with the advent of Portland cement and the absence of old records. In addition, the inclusion of pozzolans in lime mortars implies particularities in setting and hardening process, being influenced by the type of pozzolan used and its pozzolanic activity, replacement content in mortar, environmental conditions of application and curing, among others.
Therefore, this chapter highlighted the factors that influence lime mortars and how they respond to inclusion of pozzolans in terms of setting and hardening mechanisms, mechanical performance, formed hydration products and rheological aspects.
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Written By
Leane Priscilla Bonfim Sales, Aline Figueiredo da Nóbrega, Iranilza Costa da Silva, Ana Cecília Vieira da Nóbrega, Arnaldo Manoel Pereira Carneiro, Fabiola Luana Maia Rocha and Diego de Paiva Bezerra
Submitted: 28 June 2023Reviewed: 28 June 2023Published: 29 November 2023
Open access peer-reviewed chapter
