António Santos Silva

Microstructural Characterization of Consolidant Products for Historical Renders: An Innovative Nanostructured Lime Dispersion and a More Traditional Ethyl Silicate Limewater Solution

The conservation and durability of historical renders must be carried out through compatible techniques and materials. An important operation is the restitution of historical renders cohesion, turned friable by the loss of binder, usually due to physical and/or chemical actions. Surface consolidation is based on the use of materials with aggregating properties. This operation is reached usually through the application of organic or mineral consolidants, but inorganic consolidants are becoming preferred due to better compatibility and durability. In this article two mineral compatible consolidation products were studied: a commercial suspension of calcium hydroxide nanoparticles in propanol and a limewater dispersion of ethyl silicate. Microscopy (optical and scanning electron microscopy) and X-ray microanalyses of the consolidation products and of the consolidated mortar specimens were carried out. To assess the mechanical properties and products efficacy, analyses of the compression, flexural strength, and superficial hardness were performed. Microscopy results show that limewater dispersion of ethyl silicate forms platelike silica gels, which can interfere in product penetration. Otherwise, nanolime particles permit homogeneous distribution and optimum penetration on the treated substrate, improving cementing action and the agglomeration process.

Fine sepiolite addition to air lime-metakaolin mortars

Abstract Lime-based mortars with admixtures of metakaolin (10,20 and 30 wt.%) and fine sepiolite (5 wt.%) were prepared with the aim of facilitating their use as repair mortars in lowhumidity conditions. The mechanical properties and the dynamic modulus of elasticity were studied after 28,90 and 180 days of curing. With an increasing amount of metakaolin in lime mortars, improved mechanical strength was observed mainly after 90 days. Addition of fine sepiolite, due to its adsorption properties for storing water for later supply to the mortar system and its microfibrous morphology,led to an improvement of compressive and flexural strength of blended air lime/air lime-metakaolin mortars, especially at later ages of curing. Incorporation of fine sepiolite into air lime-metakaolin mortars resulted in comprehensive densification of the core of the mortars. Air lime mortar containing 5 wt.% of fine sepiolite and 20 wt.% of metakaolin appears to be an optimal admixture.

Microstructural changes of lime putty during aging

AbstractThe microstructural development of lime putty is widely recognized and commonly associated with an increase in quality. Many heritage institutions encourage the systematic application of lime putties in conservation; however, all the issues associated with age are not fully understood. Changes occur during storage underwater, which traditionally took place in pits to prevent carbonation. The properties of mortars, plasters, and decorative finishes formed from lime putties are intimately linked to manufacturing parameters such as storage time. The hydration of calcium oxide was investigated using an environmental scanning electron microscope with particular attention to the nucleation of calcium hydroxide crystals on the surface of calcium oxide. Crystal modifications were monitored. The results obtained confirm and quantify the influence of slaking time in the microstructure of lime putties that is also reflected in the current referred special characteristics of the mortars produced with them, su...

Characterisation of Roman Mortars from the Archaeological Site of Tróia (Portugal)

Roman mortars from the industrial archaeological site of Tróia (Portugal) have been studied by means of chemical, mineralogical and microstructural analysis. The mortars are calcitic aerial lime mortars differing in the type and proportion of aggregates used, including crushed carbonaceous rocks (limestone and dolomite), siliceous sand and crushed ceramics. The results show that although these mortars have been subjected to a very aggressive environment they are still in a very good state of conservation.

Consolidation and chromatic reintegration of historical renders with lime-based pozzolanic products

Abstract Historical renders are exposed to several degradation processes that can lead to a wide range of anomalies, such as scaling, detachments, and pulverization. Among the common anomalies, the loss of cohesion and of adhesion are usually identified as the most difficult to repair; these anomalies still need to be deeply studied to design compatible, durable, and sustainable conservation treatments. The restitution of render cohesion can be achieved using consolidating products. Nevertheless, repair treatments could induce aesthetic alterations, and, therefore, are usually followed by chromatic reintegration. This work aims to study the effectiveness of mineral products as consolidants for lime-based mortars and simultaneously as chromatic treatments for pigmented renders. The studied consolidating products are prepared by mixing air lime, metakaolin, water, and mineral pigments. The idea of these consolidating and coloring products rises from a traditional lime-based technique, the limewash, widely diffused in southern Europe and in the Mediterranean area. Consolidating products were applied and tested on lime-based mortar specimens with a low binder–aggregate ratio and therefore with reduced cohesion. A physico-mechanical, microstructural, and mineralogical characterization was performed on untreated and treated specimens, in order to evaluate the efficacy and durability of the treatments. Accelerated aging tests were also performed to assess consolidant durability, when subjected to aggressive conditions. Results showed that the consolidants tested are compatible, effective, and possess good durability.

Characterization of Portuguese Historical Gypsum Mortars: A Comparison between Two Case Studies

The use of gypsum plaster for interior covering of walls and ceilings in the Portuguese architecture was particularly expressive in the period between the XVIII and the XX century. However, information about this important heritage is almost inexistent, which is leading to a fast loss of important patrimony. In this paper, the results of the characterization of gypsum plaster samples belonging to two buildings from the same historical period (end of the XIX century and beginning of the XX), situated in distant geographical regions of Portugal are presented and discussed. XRD, TGA-DTA, optical microscopy and SEM-EDS observations were used for the chemical and microstructural characterization. Some physical and mechanical properties, such as capillary absorption, dynamic elasticity modulus and compressive strength were also determined and a relationship between the characteristics observed in the samples and the technology associated to their use and application on site, as well as the possible existence of regional influences on all these aspects, are discussed.

Influence of Mineral Additions in the Inhibition of Delayed Ettringite Formation in Cement Based Materials – A Microstructural Characterization

The degradation of concrete structures caused by delayed ettringite formation (DEF) is a problem that affects many concrete structures worldwide [1]. This pathology is due to the formation of expansive ettringite inside the material and is very difficult to deal with, because presently there is no efficient method to repair concrete structures affected by DEF. Hence, there is an urgent need to find preventive methods that may enable the inhibition of DEF in new constructions. This paper presents the findings of a long-term study [2,3] on the expansion rate and microstructure of heat-cured concretes with different amounts of mineral additions, like fly ash, metakaolin, ground granulated blast-furnace slag, silica fume and limestone filler. For this purpose different concrete compositions were produced using the same binder, water/binder (w/b) ratios and aggregate type. The concretes were prepared and subjected to a heat-curing cycle and subsequently to two drying-humidification cycles. After these cycles the concrete specimens were immersed in water for long-term storage at 20 ± 2°C. Length changes of specimens were measured at regular intervals. The microstructures of old heat curing specimens were investigated by optical microscopy and SEM-EDS analysis. The results of the blended-concrete compositions were compared with control compositions, and the conclusions were extracted.

Earthen plasters based on illitic soils from Barrocal region of Algarve: contributions for building performance and sustainability

Clayish earth-based mortars can be considered eco-efficient products for indoor plastering since they can contribute to improve important aspects of building performance and sustainability. Apart from being products with low embodied energy when compared to other types of mortars used for interior plastering, mainly due to the use raw clay as natural binder, earth-based plasters may give a significant contribution for health and comfort of inhabitants. Due to high hygroscopicity of clay minerals, earth-based mortars present a high adsorption and desorption capacity, particularly when compared to other type of mortars for interior plastering. This capacity allows earth-based plasters to act as a moisture buffer, balancing the relative humidity of the indoor environment and, simultaneously, acting as a passive removal material, improving air quality. Therefore, earth-based plasters may also passively promote the energy efficiency of buildings, since they may contribute to decreasing the needs of mechanical ventilation and air conditioning. This study is part of an ongoing research regarding earth-based plasters and focuses on mortars specifically formulated with soils extracted from Portuguese ‘Barrocal’ region, in Algarve sedimentary basin. This region presents high potential for interior plastering due to regional geomorphology, that promote the occurrence of illitic soils characterized by a high adsorption capacity and low expansibility. More specifically, this study aims to assess how clayish earth and sand ratio of mortars formulation can influence the physical and mechanical properties of plasters. For this assessment four mortars were formulated with different volumetric proportions of clayish earth and siliceous sand. The results from the physical and mechanical characterization confirmed the significantly low linear shrinkage of all the four mortars, as well as their extraordinary adsorption-desorption capacity. These results presented a positive correlation with mortars ́ clayish earth content and are consistent with the mineralogical analysis, that confirmed illite as the prevalent clay mineral in the clayish earth used for this study. Regarding mechanical resistance, although the promising results of the adhesion test, the flexural and compressive strength results suggest that the mechanical resistance of these mortars should be slightly improved. Considering the present results the mortars mechanical resistance improvement may be achieved through the formulation of mortars with higher clayish earth content, or alternatively, through the addition of natural fibers to mortars formulation, very common in this type of mortars. Both those options will be investigated in future research.

27Al and 29Si NMR and XRD characterisation of clinkers: standard phases and new waste based formulations

Abstract 27Al and 29Si magic angle spinning (MAS) nuclear magnetic resonance (NMR) and powder X-ray diffraction (XRD) studies of Portland type cement clinkers are reported. Common phases in such cements (C2S, C3S, C3A and C4AF) were prepared with high purity grade chemical reagents to be used as reference, and characterised. Subsequently, clinkers with selected compositions were prepared by combining several industrial wastes and byproducts: Al rich anodising sludge, sludge from the filtration/clarification of potable water, sludge generated in marble sawing processes and foundry sand. The clinkers were found to contain the reference cementitious phases, the two characterisation techniques used (NMR and XRD) being complementary in the information provided. The general similarity of the major phases formed in waste based and reagent based formulations clearly demonstrates the potential of the use of wastes in cement formulations of industrial interest.

Characterisation of Decorative Portuguese Gypsum Plasters from the Nineteenth and Twentieth Centuries: The Case of the Bolsa Palace in Oporto

The use of gypsum plaster for the interior coating of walls and ceilings in the Portuguese architecture was particularly expressive in the period between the eighteenth and the twentieth century. However, information about this important heritage is almost nonexistent, which is leading to a rapid loss of important patrimony. In this paper the results of the characterisation of five gypsum plaster samples from the second half of the nineteenth century belonging to the Arabian Room of the Bolsa Palace, located in Oporto, North of Portugal, are presented and discussed. XRD and TGA-DTA techniques were used to establish the mineralogical composition, and the relative proportions of the binders. Optical microscopy and FESEM-EDS observations were performed both in fractured and polished surfaces in order to determine the stratigraphy and the composition of individual layers. The results of this characterisation work showed that the plasters used were mainly composed of gypsum and hydrated lime in different proportions – a feature that was correlated with the application techniques of the decorative elements analysed – and allowed the determining of the restoration interventions they had already been submitted to. Some physical properties like the dynamic modulus of elasticity and capillary absorption were also determined, and a correlation between the results obtained was established with previous studies performed by the authors.