UKIERI __________________________________________________________________________________________ Concrete Congress - Innovations in Concrete Construction

REINFORCED CONCRETE CORROSION CONTROL WITH THE USAGE OF NANO-COATINGS: COMPARISON WITH TRADITIONAL AND HIGH PERFORMANCE APPLICATION SYSTEMS
Th Zafeiropoulou, E Rakanta, G Batis National Technical University of Athens, Greece

ABSTRACT. This paper studies the effectiveness of various categories of organic coatings when applied on concrete surface, regarding reinforcement corrosion. Three major categories of organic coatings were examined, including a high performance epoxy coating, a chlorinated rubber coating and two acrylic dispersions, one of which is based on the dispersion of nanoparticles and consists of a nanotechnology paint system. An appropriate series of tests was contacted in order to examine and verify the coatings protection capabilities against corrosion. The implemented evaluation methods included electrochemical measurements, such as half-cell potential, linear polarization technique and impedance spectroscopy in order to calculate crucial electrochemical parameters. Physicochemical and mechanical properties were also assigned aiming to evaluate the effectiveness of each coating system. From the results so far, it is observed that acrylic dispersion nano-coatings are able to compete high performance application paints regarding the protection they offer against reinforcement corrosion. Keywords: Corrosion, Acrylic Dispersion, Electrochemical Measurements, Nano-Coatings Mrs Th Zafeiropoulou is a Material Scientist, having received her degree from University of Patras. Since 2008 she is a member of the Materials Science and Engineering Laboratory in the framework of PhD studies. Her dissertation deals with the protection of steel rebars by corrosion with the usage of organic coatings. Dr Eleni Rakanta is a Chemical Engineer from NTUA. She has over 10 years of experience and her research area is in the field of anticorrosion methods, protection of reinforced concrete structures and chemical admixtures. She has participated in a number of industrial and research projects on Section of Material Science and Engineering of NTUA. Professor G Batis received his Diploma and PhD in Chemical Engineering from NTUA. From 2003 he is Professor of Material Science and Engineering Section in NTUA. His research interests are in the field of anticorrosion methods, cathodic prevention, protection of reinforced concrete and other metal constructions, protection of ancient monuments, development of new anticorrosive paints, performance evaluation of novel materials, etc.
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INTRODUCTION
Reinforced concrete structures have the potential to be very durable and capable of withstanding a variety of adverse environmental conditions. However, reinforcement corrosion has been established as the predominant factor causing widespread premature deterioration of concrete construction worldwide, especially of the structures located in the coastal marine environment [1]. In most cases, the deterioration of reinforced concrete structures can be ascribed to chloride induced corrosion caused by high concentrations of chloride ions penetration into concrete [2]. Protection of reinforcement is normally achieved using a variety of methods such as corrosion inhibitors or cathodic protection, however, surface treatment with organic coatings is widely adopted for various reasons. It consists of a cost effective protection method, which offers a satisfying protection level and decorative purposes are served as well, either for new constructions or for rehabilitation of deteriorated concrete structures [3]. A number of tests have been established in order to survey the effectiveness of the applied coatings [4]. Chlorinated rubber coatings are widely used for corrosion protection of surfaces. The material has excellent chemical and water resistance [5]. The coatings have, for a long time, been applied to steel, concrete and other building surfaces which are regularly exposed to water or chemicals as in swimming pools, road markings, marine building and bridge construction etc. A large number of pigments can be used in this type of paint, similar to most other oleo-resin type paints. Among these are titanium dioxide, mica form iron oxide, zinc powder, red lead and metallic lead [6].

Both chlorinated rubber and epoxy coatings have been applied on the footings and piers, to avoid concrete deterioration due to sulfate attack. However, concrete coatings of several generic types are now marketed for protecting concrete at both above and below ground levels. Studies [7,8] have shown encouraging results on the performance of vapor barriers, vapor permeable coatings, surface penetrating sealers and protective coatings. Silane / siloxane sealants with a topcoat and an acrylic coating were the most effective in reducing reinforcement corrosion, because they delay the time-to-initiation of reinforcement corrosion [9]. The performance of concrete slabs coated with acrylic-based coating against chloride and atmospheric carbon dioxide attacks have also been examined. The slabs were exposed to repeated cyclic wetting by sodium chloride solution followed by drying. After longterm exposure the results showed no chloride penetration into the concrete beneath the coating [10]. Nanotechnology based organic coatings have recently been introduced and are already in wide use due to their significant properties which involve ultra-thin application, easy clean, antimicrobial properties and UV protection. In the present study four types of organic coatings were evaluated electrochemically and physicochemically, regarding the protection they offer to embedded steel rebar when cement mortar specimens are exposed to highly corrosive environments under the presence of chloride ions. The electrochemical techniques include Linear Polarization Technique and Half-cell Potential measurements which are usually used for corrosion monitoring in coated specimens and also Electrochemical Impedance Spectroscopy which is an often used method when rebars are coated but is not widely adopted for coated cement mortar specimens.
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EXPERIMENTAL PROCEDURE
The experimental procedure included the construction of reinforced and plain cylinder cement mortar specimens. After the application of the organic coatings the specimens were partially immersed in 3.5 wt% NaCl solution for a period of one year. Electrochemical measurements were conducted to six specimens for each coating in order to evaluate corrosion due to chloride ingress. Physicochemical and mechanical properties were also determined.

Specimens Cement II 32.5N, Greek quarry sand of 250 m - 4 mm maximum grain dimension and drinkable water from NTUA water supply network, appropriate for preparing specimens according to ELOT 452 [11] were used for the construction of the specimens. Steel rebars type B500C (ELOT 1421-3 [12]) were used, having 12 mm nominal diameter and 100 mm length. The w/c ratio was 0.55. The specimens were cylindrical formed in 40 mm 100 mm and steel rebars were axially embedded in each one, located as shown in Figure 1. Prior their installation into the mortars, steel rebars were cleaned according to ISO/DIS 8407.3 [13] and weighted to a 0.1 mg accuracy.

Figure 1 Dimension of cement mortar specimens The rebars were embedded 80 mm deep into the mortar and consequently 20 mm exerted. Both ends of the rebar were sealed with a mixture of two different epoxy resins. Only the middle section (7 cm) of the bar was left, exposed to the concrete. The specimens remained molded for 24 h at ambient conditions (25C and 50% RH) in the laboratory. After removing the cast they were stored in the curing room (20 C, 99% RH) for 24 h and thereafter were left to dry for 8 days under laboratory conditions (25C and 50% RH). In order to receive electrochemical measurements, a copper wire was enwrapped to each steel rebar.

Organic Coatings Four different types of organic coatings were used, including an acrylic dispersion, an acrylic nanotechnology based coating, an epoxy coating for high application uses and a chlorinated
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rubber sealant and their composition is given in Table 1. The coatings were applied by brush on the surface of the specimens at two layers, the second layer 24h after the first one. Dry film thickness of all coatings was measured using ultrasonic thickness gauge meter according to ASTM D 6132-08 Standard Test Method [14]. Table 1 Chemical composition of the applied coatings NOMECLATURE Ref Acr DESCRIPTION Specimens without coating application Primer with siloxanes in organic solvent. Water soluble 100% pure acrylic coating, solids b.v.: 39 3%. No dilution. Viscosity: 100 5 KU, spreading rate:1012 m /l Nanotechnology paint system, 100% acrylic resin, solids b.v.: 64%. Diluted 5% v/v with water. Spreading rate: 6-9m2/l. Two-component, anticorrosive epoxy primer (solids 58%). Two component pure epoxy paint, hardened with amine. Solids b.w.: 95%. Spreading rate: 6m2/kg. Primer with special resins. HS paint, Liquid rubber acrylic based sealant. Density: 1.370.5 g/cm3. THICKNESS (m) 250

Acr_nano Epox

250 300

CR

250

EVALUATION METHODS
The anticorrosive behavior of four organic coating systems was under investigation in the present study. Traditional, high performance and new technology coatings were compared regarding the protection they offer under a highly corrosive environment. All specimens were partially immersed in 3.5 wt% NaCl solution for a period of one year and during this period electrochemical measurements were conducted including half-cell potential, linear polarization technique and electrochemical impedance spectroscopy. Physicochemical parameters such as water vapor, liquid water transmission rate and chloride penetration were evaluated for each system. Adhesion resistance was also determined.

Half-cell Potential Measurements For a period of one yeear steels half-cell potential was periodically measured versus a SCE, according to ASTM C876-879 [15].

Linear Polarization Technique (LPR) Tests were conducted using a Potentiostat / Galvanostat Model 263A from EG&G Princeton Applied Research and an associated software package to analyze the obtained data. The
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electrochemical parameter of polarization resistance (Rp), was defined, as described in ASTM G59-97(2009) [16]. The experimental set up was consisted of three electrodes where steel rebars represented the working electrode, saturated calomel electrode (SCE) the reference electrode and a carbon bar served as the counter electrode. The potential scan range was10mV from Open Circuit Potential (OCP) and the scan rate was 0.166 mV/s.

Electrochemical Impedance Spectroscopy (EIS) In the present study the impedance was measured using a Solarton SI 1260, Impedance/Gainphase analyzer. The measurements were performed at room temperature ( 25C, 50% RH) using a three-electrode electrochemical cell, consisting of the working electrode, saturated calomel electrode (SCE) as reference and carbon bar as counter electrode. The measuring frequency ranged from 105 Hz down to 10-2 Hz. Spectra were treated using the Software Zplot / Z-view (Scribner Assoc. Inc.).

Transmission Rates / Mechanical Properties Water vapour transmission rate (WVTR) and liquid water transmission rate (wt) were determined according to DIN EN 7783-181 2:1999 [17] and DIN EN 1062-3 [18] respectively. For the evaluation of chloride ions penetration the experimental set up consisted of two permeation cells, each of 500 ml volume, in which the tested sample acted as a membrane between two solutions. As a substrate for coating systems was used a high water permeability film with 5cm diameter and 3mm thickness. The total dry thickness of each coating system was equal to 300 10m and was applied by film applicator. The first cell was filled with sodium chloride solution (2.0% w/v NaCl), whereas distilled water was used in the second cell. The painted side of the membrane was facing the salt solution. Chlorides will traverse the membrane from the concentrated solution to the diluted one under natural diffusion driving force. For the determination of the total amount of chlorides passed through the coated membrane, conductivity measurements were periodically performed with a Sension7 conductivity meter by Hach, which were afterwards converted into concentration values. Figure 2 represents the experimental set up that was used in this study. Adhesion resistance tests were conducted in proportion to ADTM D4541 [19] and three tests were performed for each determination.

Figure 2 (a) Experimental set up for the evaluation of Cl- penetration

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Figure 2 (b) Permeation cell

EXPERIMENTAL RESULTS AND DISCUSSION

Half-cell Potential Measurements Half cell potential measurements of steel rebars is the most typical procedure to the routine inspection of reinforced concrete structures regarding the corrosion trend of the samples. They are simple, inexpensive and virtually non-destructive techniques to assess the corrosion risk of steels in concrete and they can be used to estimate the corrosion risk even if there are no signs of corrosion on the concrete surface, which is a significant advantage for inspecting existing concrete structures. However, different organizations have different recommendations on half-cell potential measurements and in the present study ASTM C 876 879 [15] suggestions are adopted for the interpretation of the results. In Figure 3 are presented the corrosion potentials as a function of exposure period for cement mortars specimens covered with organic coatings and immersed in 3.5 wt.% NaCl solution. Potential readings are highly influenced by the surface treatment of the specimens which causes changes in their resistivity, as long as the constituents of the cement mortars remain the same.

Figure 3 Average half-cell potential values for six specimens as a function of exposure time for reinforced cement mortars partially immersed in 3.5 wt.% NaCl solution. According to Table 2 [20] at the end of the exposure period Acr coating presented potential values that are indicative of severe corrosion, Epoxy coating as well as Acr_nano coating attained values that revealed high risk of corrosion and only Chlorinated rubber coating
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demonstrated intermediate corrosion values. For all specimens Ecorr reduction to such electronegative values versus time is due to chloride induced corrosion and indicates that all steel rebars are in an active corrosion state, regardless the applied coating on cement mortars surface. Such electronegative values are not surprising because they are in agreement with what reported by other authors [21-23]. However, corrosion potential measurements can be misleading because they measure the corrosion condition and not the corrosion rate and consequently they do not provide information regarding the thermodynamics of the corrosion. Table 2 Corrosion potential and corrosion condition. [20] CORROSION POTENTIAL OF STEEL REBARS > -126 -126 to -276 < -276 < -426 CORROSION CONDITION Low (10% risk of corrosion) Intermediate corrosion risk High (90% risk of corrosion) Severe corrosion

Linear Polarization Technique The most popular of the electrochemical techniques is the Linear Polarisation Resistance (LPR) method. LPR technique consists of a non-intrusive method that can be used relatively rapidly and portable instrumentation has been developed [24] suitable for use in the field test. The principal of LPR is based upon disturbing the corrosion equilibrium on the surface of steel reinforcing bars by the introduction of a small perturbative DC electrical signal using a surface counter electrode. The response of the equilibrium to this perturbation is measured with respect to a reference half-cell on the surface of the concrete. In the article a small current step I may be used as the perturbative signal and the resulting potential is E measured and the polarisation resistance Rp is given by:
Rp =

(1)

From which the corrosion rate, Icorr, can then be calculated corr =

c 1 B = 2.303 ( + c ) R p R p

(2)

Where , c are the anodic and cathodic Tafel slopes respectively and Rp is the polarization resistance (Ohm). For SternGeary constant B a value of 26mV has been adopted for active corroding steel bars and 52mV for passive conditions. In order to determine the corrosion current density, icorr, the surface area, A, of steel that has been polarized needs to be accurately known: I icorr = corr A (3)
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Obtained Rp values are highly correlated with a number of factors, including surface treatment, corrosive environment and the materials that were used for the construction of the specimens. In the present study the corrosive environment as well as the materials of the specimens remained stable and consequently all changes to Rp values are due to differences in the surfaces treatment. Linear polarization measurements were periodically performed to six specimens for each coating and polarization resistance (Rp) values are presented in Figure 4.
POLARIZATION RESISTANCE (-cm2)

TIME (DAYS)

Figure 4 Polarization Resistance after one year of exposure to 3.5 wt.% NaCl solution. Average values of six reinforced cement mortar specimens for each coating system According to Table 3 [20], at the end of the exposure period all specimens exhibited low to moderate corrosion rate, except specimens covered with the acrylic dispersion which demonstrated high corrosion rate. Table 3 Polarization resistance values and corresponding corrosion rate [20] Rp (k.cm2) >260 52-260 26-52 <26 CORROSION RATE Passive condition Low to moderate corrosion Moderate to high corrosion High corrosion rate

Electrochemical Impedance Spectroscopy EIS technique was chosen based on the fact that it provides information on the electrodes process that occurs on the steel mortars interface, in addition to the kinetics of the reaction. In general, impedance consists of complex resistance when current flows through a circuit made
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of capacitors, resistors, or insulators, or any combination of these [25] and is commonly depicted as a complex function, having both real and imaginary components. It is usually plotted in Nyquist diagram, as imaginary part vs. real part, proving a convenient method for the determination of important electrical parameters. In the present study a typical plot for all measurements conducted is given in Figure 5.

IMAGINARY PART ()

REAL PART ()

Figure 5 Typical Nyquist diagram The salient features of the spectrum are labelled as follows: 1) the cement mortar resistance (Rc) which is highly related to the microstructure and pores of the cement based material and is given by the high frequency limit of the diagram, 2) the steel-cement mortar interface film resistance (Ri) which is given by the diameter of the high frequency loop. The interfacial film actually represents the layer formed on the steel surface and its impedance properties are affected by cement hydration products deposited in the layer and/or corrosion products of steel diffused into the layer18, 3) the polarization resistance (Rct) which is given by the low frequency limit and varies according to the electrochemical state of the reinforcing steel surface. In the present study Rc values were determined for all coatings because the variations of the high frequency loop are due to the used surface treatment. The results of EIS measurements are depicted in Figure 6, where is shown a comparative Nyquist plot for all coating systems.

IMAGINARY PART ()

REAL Z ()

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Figure 6 Nyquist plot after 40 days of immersion

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In Table 4 are presented the crucial values from EIS technique for all coated specimens. Table 4 Average Rc values for all coatings COATING Ref Acr Acr_nano Epox Cr Rc () 39.117 143.56 166.24 353.42 286.19

From the results it can be observed that Chlorinated rubber and Epoxy coatings are presenting the higher Rc values and thus higher porosity coverage is accomplished. The Nano-coating system exhibited higher electrochemical values compared to the traditional coating system.

Water Vapour and Liquid Water Transmission Rate The results for water vapour (WVTR) and liquid water transmission rate (wt) of all types of coating systems are presented in Figure 7 and Figure 8 respectively. The best combination for an effective coating is to exhibit high WVTR and low wt values.

Figure 7 Average water vapour transmission rate for six specimens for each coating According to ASTM standards [17] all coatings can be classified to Category II (medium water vapour permeability) and only Acr_nano coating is subsumed to Category I (high water vapour permeability). Regarding water permeability, all coatings can be considered as waterrepellent coatings, because they present very low liquid water permeability. According to ASTM standards [18] they can be subsumed to Category III (low liquid water permeability). In contrast, the traditional coating can be assigned to Category II (medium liquid water permeability). Consequently Acr_nano coating exhibits the best balance regarding the
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WATER VAPOUR TRANSITION RATE WVTR (g/m2d)

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aforementioned physicochemical properties because it demonstrates low water uptake values and additionally consists of a high breathable coating.

Figure 8 Average liquid water transmission rate of six specimens for every coating

Chloride Permeability Chloride permeability results are presented in Figure 9. It can be observed that chlorinated rubber coating exhibits the best behavior towards chlorides permeability, because demonstrates the lowest concentration of NaCl through time.

WATER TRANSITION RATE wt (Kg/m2h 1/2)

TIME (DAYS)

Figure 9 Average % w/v NaCl consentration versus time

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Epox and Acr_nano coatings also exhibit low transmission rates compared to traditional systems. The results from chloride permeability are in agreement with liquid water transmission rates for all the coatings.

Adhesion Resistance Adhesion resistance test was performed according to the related standard method and results are presented in Table 5. For every measurement, six specimens were used. Table 5 Adhesion resistance for the used coatings COATING Acr Acr_nano Epox Cr ADHESION RESISTANCE (MPa) 0.4 0.6 3 1.5

As it shown, Epox coating attained the greatest adhesion resistance among the other coatings. A slight difference is noticed among the nanotechnology and the traditional coatings, whereas the adhesion resistance of the chlorinated rubber coating was found to be higher than both aforementioned coatings.

CONCLUDING REMARKS
In the present study four organic coatings were compared regarding their physicochemical and mechanical properties, as well as, their protection level against induced chloride corrosion.From the electrochemical measurements for corrosion evaluation, it can be drown: The chlorinated rubber coating demonstrated the highest Rp and Ecorr values which are indicative of the high resistance against corrosion. This can be observed from all electrochemical measurements. Physic chemically, the aforementioned coating can be considered as water repellent and not permeable to chloride ions. Epoxy coating achieved a satisfying protection level and appears to be the most durable coating, mechanically, but its low permeability values are constraining its uses. Moreover, the nanotechnology coating exhibited the best transmission rates among all the coatings and its protection against corrosion appears to be rather satisfying. It should finally be noted that nanotechnology coatings are designed for conventional purposes but are competing high performance application systems, such as Cr coatings.

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REFERENCES
1. RAUPACH M. AND SCHIEBI, Macrocell sensor systems for monitoring of the corrosion risk of the reinforcement in concrete structures, NDT&E International, 2001, No. 34, Vol. 34, pp 435-442. LIU Y AND SHI X., Corrosion Reviews, 2009, Vol. 53, pp 27. THOMAS N., The barrier properties of paint coatings, Progress in Organic Coatings, 1991, Vol. 19, No. 2101121. BASHEER P., BASHEER A.M., CLELAND D. J. AND LONG A. E., Surface treatments for concrete: assessment methods and reported performance, Construction and Building Materials, 1997, .Vol. 7-8, pp 413-429 LAMBOURNE R., Paint and surface coatings: theory and practice, London: Ellis Horwood, 1987 CHANDLER K.A. AND BAYLISS, D.A., Corrosion protection of steel structures, Elsevier Applied Sciences, 1985 SWAMY, R.N., SURYAVANSHI A.K. AND TANIKAWA, S. Protective ability of an acrylic based surface coating system against chloride and carbonation penetration into concrete ACI Materials Journal 1998, Vol. 95, No. 12, pp 101112. KAMAL M.M. AND SALAMA A.E., Protection of reinforced concrete elements against corrosion by polymer coatings In: Dhir RK, Green JW, editors, Proceedings of International Conference on Protection of Concrete, London: E & FN Spon; 1991, pp 281291 IBRAHIM, M., AL-GAHTANI A.S. AND MASLEHUDDIN. M. Use of surface treatment materials to improve concrete durability, ACI Materials Journal, 1999, pp 36 40. SWAMY R.N., SURYAVANSHI AK AND TANIKAWA S., Protective ability of an acrylic based surface coating system against chloride and carbonation penetration into concrete, ACI Materials Journal, 1998, Vol.95, No.2, pp 10112. HELLENIC ORGANIZATION FOR STANDARDIZATION ELOT 452, Determination of total Hg content to water with Atomic Absorption Spectroscopy, Athens, 1983 HELLENIC ORGANIZATION FOR STANDARDIZATION ELOT 1421-3, Steel for the reinforcement of concrete Weldable reinforcing steel Part 3: Technical class B500C, Athens, 2005 ISO/DIS 8407.3, Procedures for removal of corrosion products from corrosion test specimen. ASTM D 6132-08 Standard Test Method for Nondestructive Measurement of Dry Film Thickness of Applied Organic Coatings Using an Ultrasonic Gage, Vol.06.01, 2008 ASTMC876-87, Standard test method for half-cell potentials of reinforcing steel in concrete, Vo. 03.02, 1987 ASTM G59-97(2009), Standard test method for conducting potentiodynamic polarization resistance measurements, Vol. 03.02, 2009

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17. 18. 19. 20. 21.

DIN EN 7783-2:1999, Determination and classification of water-vapour transmission rate (permeability), Vol. 09.99, 1999. DIN EN 1062-3, Determination and classification of liquid-water transmission rate (permeability), 2008. ASTM D4541 - 09e1, Standard Test Method for Pull-Off Strength of Coatings Using Portable Adhesion Testers, Vol. 06.02, 2009. BROOMFIELD J., Corrosion of steel in concrete understanding, investigation and repair, 1st Edition, E & FN SPOK, UK, 1997, Vol. 5, pp 16-21. BATIS G., PANTAZOPOULOU P., AND ROUTOULAS A., Corrosion protection investigation of reinforcement by inorganic coating in the presence of alkanolaminebased inhibitor, Cement and Concrete Composites, 2003, Vol. 25, No. 3, pp 371377. KOULOUMBI N. AND BATIS G., The anticorrosive effect of fly ash, slag and a Greek pozzolan in reinforced concrete, Cement and Concrete Composites, 1994, Vol. 16, No. 4, pp 253260. ZAFEIROPOULOU, TH., RAKANTA, E., AND BATIS, G., Performance evaluation of organic coatings against corrosion in reinforced cement mortars, Progress in Organic Coatings, 2011, Vol 72, pp 175-180. LAW D., MILLARD S. AND BUNGEY J., Linear polarisation resistance measurements using a potentiostaticallycontrolled guard ring, NDT&E International, 2000, Vol. 1, pp. 1521. PARK S. M. AND YOO J.S., Electrochemical impedance spectroscopy for better electrochemical measurements, Analytical Chemistry, 2003, Vol. 75, No. 21, pp 455461.

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