Composites: Part B 41 (2010) 663–672

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Composites: Part B

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Polymeric and cementitious mortars for the reconstruction of natural stonestructures exposed to marine environments

C. Thomas a,⇑, I. Lombillo b,1, J.A. Polanco a, L. Villegas b, J. Setién a, M.V. Biezma a

a Dept. of Science and Engineering of Materials, University of Cantabria, School of Civil Engineering of Santander, Avda. Los Castros s/n, Santander 39005, Spainb Dept. of Structural and Mechanics Engineering, University of Cantabria, School of Civil Engineering of Santander, Avda. Los Castros s/n, Santander 39005, Spain

a r t i c l e i n f o

Article history:Received 19 February 2010Received in revised form 30 June 2010Accepted 7 August 2010Available online 21 August 2010

Keywords:A. Polymer–matrix compositesCement–matrix compositesB. CorrosionB. Mechanical properties

1359-8368/$ - see front matter � 2010 Elsevier Ltd. Adoi:10.1016/j.compositesb.2010.08.007

⇑ Corresponding author. Tel.: +34 942201827.E-mail addresses: carlos.thomas@unican.es (C.

unican.es (I. Lombillo).1 Tel.: +34 942201743.

a b s t r a c t

This study outlines the advantages and disadvantages of the use of composites in reconstruction activi-ties. The aim of the study is the reconstruction of a natural rocky arc exposed to a marine environment.Anchoring reinforcements of two types of stainless steel were analyzed. Also epoxy resins, polymeric,cement based mortars and cement based concrete, separately and in combination, have been studied.Durability, mechanical behaviour, protective effect of mortars and thermal compatibility were studied.The overall conclusion of the research is that polymeric mortars are the most appropriate for the recon-struction and/or rehabilitation of stone structures exposed to highly corrosive environments.

� 2010 Elsevier Ltd. All rights reserved.

1. Introduction

This work is part of the series of actions carried out in the pro-ject of reconstruction of the Horadada Island in the Bay of Santan-der (in the north of Spain), ranked as one of the 10 most beautifulbays in the world [1]. Horadada Island is a rocky natural arc, of70 m2, in the middle of the bay of Santander and therefore exposedto the sea and marine dynamics. The structure of the rock was acurious natural arc until 2005, when, after a winter storm, thetop of the structure, shaded in Fig. 1, collapsed and fell to the sea-floor. The structure was closely linked to the city of Santander and,for that reason, a series of actions was promoted with a view tostudying the technical feasibility of the reconstruction of the islandarc [2], using the most suitable technologies and materials.

As a result of the visual inspection of the recovered stone frag-ments from the seabed, a single type of strongly deteriorated lime-stone showing a large amount of porosity in the surface with adepth varying from a few millimetres to 2 cm was identified. Thedepth of degradation of the natural rock is shown in detail inFig. 2, in a sample coated with cementitious mortar prepared forcompatibility analysis.

The proposed reconstruction action is based on the relocation ofthe recovered remains by joining them to the rock abutments cur-rently existing [3,4].

ll rights reserved.

Thomas), ignacio.lombillo@

2. Materials

Once the marine environment in which the action is situatedwas assessed, two types of stainless steel were analyzed as mate-rials for the anchoring reinforcement, one supplied as a bar-shapedsmooth (AL) of 20 mm diameter and the other as a bar-shapedribbed (AC) of 16 mm diameter with improved adherent features.The chemical compositions of the two steels are shown in Table 1.To attach the reinforcements to the rock, the use of different adhe-sive materials has been considered: epoxy resins (AP), polymericmortars (APT), cement based mortars (K50) and cement concretes(K150).

Regarding the nature, manufacturing methods, physical andchemical properties of polymeric materials, most relevant proper-ties are reflected in the data sheet of each of the commercial prod-ucts used. AP is the commercial product BASF APOGEL SCBCONCRESIVE� 1360 [5], a two component ultra low-viscosity li-quid epoxy adhesive, and the APT is the BASF APOTEN MASTER-FLOW� MP [6], a three-component epoxy grout. In both cases, APand APT, mixtures of the resin with hardener were performedaccording to the specifications of the fabricant. In the case ofcementitious materials, K50 corresponds to the commercialcementitious mortar BASF MASTERFLOW 952 (Bettogrout 50) [7],and K150 the cementitious concrete BASF MASTERFLOW 952 PLUS(Bettogrout 150) [7]. The mixtures with water, of the hydraulicmaterials, were performed according to the specifications of thefabricant. The composites were analyzed at the age of 28 days:the polymeric materials were cured under laboratory conditions(19 ± 2 �C and 54 ± 3% humidity) and the cementitious matrix

Fig. 1. Horadada Island of Santander after collapse, and, with a shaded overlay, the pre-failure structural geometry.

Fig. 2. Detail of a rock cut coated with cementitious mortar.

Table 2Polymeric and cementitious adhesive materials analyzed.

Code Binder Aggregatetype

Aggregate max.size (mm)

Binder/aggregaterelationship (in weight)

AP Epoxy – – –K50 Cement Quartz 2 0.5APT Epoxy Quartz 2 0.5K150 Cement Quartz 12 0.5

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materials under 21 ± 1 �C and 98 ± 1% humidity. The characteristicsof the prepared materials are presented in Table 2.

Also, combinations of the two types of steels (AC and AL) withthe epoxy resin (AP), the two types of mortars (K50 and APT) andthe concrete have been analyzed. The decision to analyze thebehaviour of these materials in combination with steel reinforce-ments is based on the apparent excellent chemical resistance ofthe polymeric materials, in comparison with cementitious com-posites, under corrosive environments [8–12].

Furthermore, the compatibility between the composites and therock was studied. To do this, samples of bedrock impregnated inthe surface with epoxy resins (AP), polymeric mortars (APT), ce-ment based mortars (K50) and concrete (K150) were prepared.

3. Experimental analysis

The test program presented here is aimed at analyzing the suit-ability and compatibility of the different selected materials in mar-ine environmental conditions. For this purpose, experiments havebeen conducted on abrasion and erosion in adhesive materials;also the mechanical behaviour and the thermal deformationalcompatibility under heating gradients and the degradation by wet-ting–drying cycles have been determined. As regards compatibil-

Table 1Quantitative chemical analysis by optical emission spectroscopy. Task FeCrNi for stainless

Steel C Si Mn P S

AL 0.028 0.27 0.77 0.027 0.01AC 0.038 0.35 1.77 0.033 0.02

ity, the protective effect of the resin, mortars and concrete in thecorrosion of steel has also been studied.

3.1. Abrasion tests

This action is designed to obtain a comparative analysis of theabrasion behaviour of the selected materials. The test was carriedout based on criteria stipulated in the standard [13] in order toestablish a comparison between the behaviour of the reconstruc-tion materials and the original rock to replace in some elements.Abrasive corundum with a grain size of F80 has been used. Threeprismatic specimens with dimensions 40 � 40 � 160 mm, for eachof the materials, have been tested.

3.2. Erosion tests

The erosion tests were performed to assess the performance ofrepair materials when they are subjected to the action of hydrody-namic erosion of a moderate water pressure jet including solid par-ticles [2]. This situation reflects the actual conditions acting on thestructure. For the definition of the test, water pumping equipmentwas used working at a pressure of 5 bars, with addition of silicasand that made it possible to attack the surface of the sample withthe stem opening at a distance of 30 cm during a time of 60 s. Inorder to assess the effect exerted by the water flow, the volumeof eroded material was analyzed and a microstructural observationof the affected surface was performed. Have been tested three pris-matic specimens with dimensions 40 � 40 � 160 mm, for each ofthe materials.

steels.

Ni Cr Mo Cu Al

7 6.8 24.8 3.87 0.11 0.032 4.5 22.5 3.37 <0.10 <0.01

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3.3. Flexural, compressive and tensile strength and Young’s modulus

Tests for determining the flexural strengths [14] were carriedout on three prismatic standard samples, 40 � 40 � 160 mm ofeach of the materials under study. Also, have been manufactured,on one hand, three cylindrical standard samples of150 � 300 mm for the cementitious mortar and concrete [15]and, on the other hand, three cylindrical samples of 50 � 100 mmfor the epoxy resin and polymeric mortar for the determinationof the compression strength [16–18]. Tests for determining thetensile strength, Brazilian method [19], were carried out on threecylindrical samples of each material. As well, were prepared threeother samples instrumented with three strain gauges (120� sepa-rate) for the determination of the modulus of elasticity [20].

Table 3

3.4. Accelerated degradation in salt fog spray cabinet

This characterization was carried out by the exposure of differ-ent steel/composite combinations to a saline environment, follow-ing the guidelines of the standards [21,22]. To analyze thebehaviour shown by the materials – steel corrosion and protectivecapacity of the repair material – 16 types of samples were preparedby combining the epoxy, the polymeric mortar, cementitious mor-tar and the concrete with the two steels. In the first of the types,the steel was completely coated with composite and in the secondtype of samples, the steels were partially covered. The sampleswere subjected to a heavily corrosive atmosphere during 1000 h.The presence of chloride anions, on the passive layer of stainlesssteel, created a gradient of concentration that facilitated its diffu-sion, breaking the protective layer [23]. The pH was maintainedin the salt spray chamber simulating the seawater conditions [24].

Results of the wear traces of abrasion tests and eroded volume of erosion tests.

Material Abrasion traces average (mm) Eroded volume (cm3)

AP 13.85 0.28K50 16.70 2.85APT 15.40 0.48K150 20.35 3.21

3.5. Deformational compatibility under freeze–thawing and wetting–drying cycles

To evaluate the compatibility between, polymeric and cementi-tious materials with stones, the compatibility under freeze–thaw

Fig. 3. Partial results of abrasion test: (a) sample AP_6, (b) sam

conditions has been tested, with a program of 20 cycles, wherethe samples have been subjected to a thermal gradient programconsisting, first, in 12 h at temperature of �5 ± 1 �C in a freezerand, after this, another 12 h at 60 ± 1 �C in an oven.

To complete the characterization, a series of wetting–drying cy-cles was carried out, in which the samples were introduced into anoven at a temperature of 100 ± 5 �C for 16 h and then were sub-merged into water under laboratory conditions (19 ± 2 �C) for 8 h.This process was repeated 20 times, as in the case of deformationalcompatibility tests, to determine any differential behaviour be-tween the mortars with the rock on which they have been applied.

4. Results

4.1. Abrasion tests

According to the procedure established in the standard [13], inorder to measure the width of the abrasion traces between the lon-gitudinal outer limits of it, a line was drawn in the center of thetrace, perpendicular to its centerline and the distance was mea-sured, Fig. 3. Two abrasion traces have also been made on oppositesides, of three specimens of each sample, the representative mea-sure being the widest of them. These results are shown in Table 3.

4.2. Erosion tests

As for the erosion tests, in order to determine the resistance ofthe materials to this process, the eroded volume of the sample after

ple APT_15, (c) sample K50_7 y and (d) sample K150_6.

Fig. 4. Aspect of the sample after filling material.

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the application of the water jet with abrasive aggregate has beendetermined. The here proposed method is an economiser and fas-ter method compared to the determination of the mass loss meth-od that implies oven-drying before and after the test. In thisprocess, first, a non-stick plastic material was applied in the gapresulting from the erosive effect of the abrasive jet applied to thesurface of the specimen. After that, the filling material was spreadusing a spatula (Fig. 4). Then, using the same spatula, the excessmaterial was withdrawn so that its upper level was raised withthe surface of the specimen (Fig. 5). Fig. 6 shows some testedspecimens and the plastic volume rated, indicated above each

Fig. 5. Recovery process of filling material for further analysis.

Fig. 6. Volume plastic filler of the gap caused by erosion.

one. Finally, the filling plastic volume was measured by immersionin a distilled water container on a precision scale where the sub-merged weight provided directly the apparent volume [25]. The re-sults are shown in Table 3.

Regarding the microstructural analysis of the eroded surface, inthe case of the K50, microcrack shielding, crack-branching, aggre-gate spalling, crack-deflection, crack-blunting, crack-rim andcrack-bridging [26] are all observed. The Figs. 7 and 8 show withdifferent scales these effects of erosion. In the case of the APT,aggregate spalling and crack-blunting are observed (Figs. 9 and10) with different scales, but there are no microcracks in the ma-trix of the material, presenting a homogeneous surface and lessdeep erosion than in the case of K50 and K150.

4.3. Mechanical properties

Regarding the mechanical behaviour of adhesive materials, anhydraulic press with a load capacity of 1500 kN was used for thetests. It is based on the study of strengths of flexion and compres-sion with deformation registration. The results obtained in rela-tionship to the characterization of the resins, polymeric mortars,

Fig. 7. SEM-image cement mortar K50_8.

Fig. 8. SEM-image cement mortar K50_8.

Fig. 9. SEM-image polymer mortar APT_17.

Fig. 10. SEM-image polymer mortar APT_17.

Table 5Results of the inspection of the different combinations of steel with mortar.

Combination Coating Pittingcorrosion

Superficialcorrosion

Deepcorrosion

AC-AP Partial Yes Yes NoTotal No No No

AC-APT Partial Yes Yes NoTotal No No No

AC-K50 Partial Yes Yes NoTotal Yes Yes No

AC-K150 Partial Yes Yes NoTotal Yes Yes No

AL-AP Partial Yes No NoTotal No No No

AL-APT Partial Yes No NoTotal No No No

AL-K50 Partial Yes No NoTotal Yes No No

AL-K150 Partial Yes No NoTotal Yes No No

Fig. 11. AC-AP sample partially embedded.

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cementitious mortars and concretes here studied are presented inTable 4.

4.4. Accelerated corrosion of steels in salt spray chamber

After the 1000 h of exposure, the samples were extracted fromtheir partial or full covering. Then the surface appearance was ana-lyzed in order to detect the presence of corrosive processes insteels. These processes were classified, depending on their size,into pits, surface corrosion and deep corrosion. The results are pre-sented in Table 5.

A detailed analysis of the protective effect of polymeric andcementitious materials is presented here. Fig. 11 shows an AC

Table 4Results of flexural, compressive strength, modulus of elasticity and tensile strength.

Material rF (MPa) rc (MPa) E (MPa) rt (MPa)

AP 4.52 102.05 11,223 13.25K50 1.26 63.95 47, 485 5.32APT 3.84 136.95 17,571 16.61K150 1.04 69.41 37.479 8.15

specimen partially embedded in the resin AP, where it can be seenthat the corrosion is superficial and localized. The same resultswere observed in the sample AC specimen partially embedded inthe mortar APT, Fig. 12. The same effects are seen in the partiallyembedded AC-K50, Fig. 13, and in the partially embedded AC-K150, Fig. 14. The Fig. 15 shows the AC specimen fully embeddedin resin AP; in this case no corrosion of any kind has been detecteddue to the protective effect provided by the AP resin even when the

Fig. 12. AC-APT sample partially embedded.

Fig. 13. AC-K50 sample partially embedded.

Fig. 14. AC-K150 sample partially embedded.

Fig. 15. AC-AP sample totally embedded.

Fig. 16. AC-APT sample totally embedded.

Fig. 17. AC-K50 sample totally embedded.

Fig. 18. AC-K150 sample totally embedded.

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coating is a few millimeters thick. The same results were observedin the sample AC specimen fully embedded in the mortar APT,Fig. 16. In the case of the totally embedded AC-K50, Fig. 17, andAC-K150, Fig. 18 the protective effect against chloride is less, whichhas been highlighted by the detection of surface corrosion. In the

case of AL partially embedded in AP, as shown in Fig. 19, and inAPT, as shown in Fig. 20, the corrosion pitting was detected onlyin the uncoated surfaces of the sample. In the case of the AL-K50,pitting corrosion has been observed both in the directly exposedsurface and also in the coated surface, Fig. 21. The same effectsare seen in the partially embedded AL-K150, Fig. 22. In the case

Fig. 19. AL-AP sample partially embedded.

Fig. 20. AL-APT sample partially embedded.

Fig. 21. AL-K50 sample partially embedded.

Fig. 22. AL-K150 sample partially embedded.

Fig. 23. AL-AP sample totally embedded.

Fig. 24. AL-APT sample totally embedded.

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of AL fully embedded in AP and in APT, no corrosion was detectedof any kind, as shown in Figs. 23 and 24. Nevertheless, when the ALis fully embedded in the K50 cement mortar, Fig. 25, or in the K150concrete, Fig. 26, local and pitting corrosion have been found butnot superficial corrosion.

The results are justified because the passive layer of stainlesssteel under a polymer is thinner and less hydrated than that

Fig. 25. AL-K50 sample totally embedded.

Fig. 26. AL-K150 sample totally embedded.

Fig. 27. SEM-image of pitting corrosion on AL steel.

670 C. Thomas et al. / Composites: Part B 41 (2010) 663–672

formed on a stainless steel without any organic coating. However,the type of polymer influences the composition of the passivelayer, which is why using epoxy has resulted in some isolated pits[27,28]. In the case of the AL steel, the higher presence of Ni differ-entiates its excellent performance against AC steel to marine corro-sion, while improving its mechanical properties [29–32]. Animproved performance compared to the AC steel, as expected, is re-ported in the AL steel. The increase of Mo in steel improves the bar-rier effect of the passive film as a bilayer formed by oxides, anouter-rich Mo (VI) and an inner-rich Mo (IV). This layer acts as areal barrier to prevent chloride anions from penetrating the mate-rial. Thus, the outer layer, rich in Mo, is formed by oxides of Fe andCr as Cr(OH)3. There are no detected oxides of Ni dissolved in theelectrolyte or partially accumulated under the passive layer. TheAC steel has moderate surface corrosion especially in its most vul-nerable areas as a result of the cutting operations performed onthem. For the AL steel, some isolated corrosion pitting has been ob-served, only in a few samples; Fig. 27 shows a micrograph of a pit.

Fig. 28. R-AP_two sample impregnated with epoxy resin on the surface after thethermal gradient test.

4.5. Deformation compatibility

The polymeric materials show decolouration and softening dueto the effect of thermal gradients. This aging can lead to an associ-ated loss of properties, although there is no evidence of incompat-

ibility between polymeric materials and stone as there is noadhesion failure or disintegration detected in any of the cases.Figs. 28 and 29 show two specimens subjected to deformationalcompatibility by thermal gradients after the cycles: R-AP and R-APT combinations. In the case of cementitious mortar and concretehas been detected a small loss of mass of the adhesive material anddeformational no incompatibility. The Figs. 30 and 31 show theappearance of the cement mortar and concrete combined withthe natural stone after the test. The results are shown in Table 6.

Similarly to what happened with the thermal compatibilitytests, the results obtained in the case of the cycles of wetting–dry-ing do not show any appreciable incompatibility between poly-meric materials, AP and APT, and stone as there is no adhesionfailure or disintegration detected in any case. However, in this case,there is no evidence of degradation of the material. Figs. 32 and 33show some specimens of R-AP and R-APT subjected to deforma-tional compatibility by wet–dry gradients after the cycles. The ce-ment mortar and the concrete shows no signs of deterioration ordegradation and its compatibility with the rock on which it was ap-plied, after the cycles of temperature and wetting–drying, is simi-lar to that originally presented. The Figs. 34 and 35 show theappearance of the cement mortar and concrete combined withthe natural stone after the test. The results are shown in Table 6.

Fig. 29. R-APT_1 sample impregnated with polymer mortar on the surface after thethermal gradients test.

Fig. 30. R-K50_1 sample of stone impregnated on the surface with cement mortarafter the thermal gradients test.

Fig. 31. R-K150_2 sample of stone impregnated on the surface with concrete afterthe thermal gradients test.

Table 6Results of deformational compatibility under freeze–thawing and wetting–drying cycles.

Material Freeze–thaw cycles test Wetting–drying cycles test

Compatibility Mass loss (% in weight) Compatibility Mass loss (% in weight)

R-AP Excellent 0.05 Good 0.12R-K50 Good 1.74 Very good 0.37R-APT Very good 0.55 Good 0.56R-K150 Good 1.96 Very good 1.45

Fig. 32. R-AP_1 sample of stone impregnated on the surface with polymer resinafter the wetting–drying gradients test.

Fig. 33. R-APT_2 sample of stone impregnated on the surface with cement mortarafter the wetting–drying gradients test.

Fig. 34. R-K50_2 sample of stone impregnated on the surface with cement mortarafter the wetting–drying gradients test.

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Fig. 35. R-K150_1 sample of stone impregnated on the surface with concrete afterthe wetting–drying gradients test.

672 C. Thomas et al. / Composites: Part B 41 (2010) 663–672

5. Conclusions

The overall conclusion of the research is that polymeric mortarsare more appropriate for the reconstruction and/or rehabilitationof stone structures exposed to highly corrosive environments thanthe traditional hydraulic mortars because they offer better protec-tion against steel corrosion. Also have very good adhesive, mechan-ical and durability properties, which is proved when the maximumtemperatures do not exceed 100 �C. The following general conclu-sions can be drawn from this work:

There is a clear correlation in the results obtained for the abra-sion and erosion tests. However, the results are very similar in allcases. Under erosion tests, the best materials are the pure epoxyresin and the polymeric mortar, the cement base mortar showingthe worst behaviour. The resistance to abrasion and erosion ofthe tested materials can be ordered by the following criteria: RA-P > RAPT > RK50 > RK150. Furthermore, a fast and economicalmethod for evaluating this effect is proposed by measuring the vol-ume eroded.

Mechanical characterization tests again suggest that the poly-meric mortar is the most appropriate in all cases. It has good com-pression and excellent tensile strength. The addition of aggregateto the epoxy resin (polymeric mortar), and the addition of aggre-gate to the cementitious mortar (concrete) increases the resistance,although in polymeric materials this increase is not as significantas in cementitious.

By accelerated attack in a salt spray chamber, a cementitiousmortar allows the transport of corrosive agents because it hashigher permeability. This access is more aggressive in the AC steelsthan in AL steels. The AL steel has better resistant qualities to cor-rosion in marine environment through the increased presence ofMo. The Mo (VI) creates a protective layer on the surface of thesteel that protects against corrosion. In addition, the barrier effectdoes not depend on the type of coating analyzed.

Concerning the deformational compatibility tests against ther-mal gradients and cycles of wetting–drying, it seems that there isperfect compatibility of the polymeric mortar and cement mortarwith the natural rock. It is detected, in the case of the polymermortar, an appreciable decolouration associated to high tempera-tures (105� C) of exposure.

Acknowledgments

The authors of this paper wish to thank the Santander CityCouncil, Spain, for their confidence in the team who carried outthe studies on the technical feasibility for the reconstruction ofthe Horadada Island in the Santander bay.

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