2. Experimental. 1. Introduction
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1 Electrical conductivity and corrosion protection properties of conductive paint coatings School of Materials and Mineral Resources Engineering, Universiti Sains Malaysia, Penang, Malaysia Abstract Purpose The purpose of this paper is to investigate the electrical conductivity and corrosion protection properties of a conductive coating composed of epoxy resin and carbon black in a sodium chloride (NaCl) solution Design/methodology/approach The conductive coating was prepared by combining epoxy resin, hardener, and carbon black The electrical conductivity of the paint was studied with a DC current-voltage meter and field emission scanning electron microscopy The corrosion protection properties of the paint were characterized by open circuit potential measurements and electrochemical impedance spectroscopy Findings The highest conductivity observed was Scm 2 1 for the coating containing 20 wt% carbon black The coating protected mild steel in a 30 percent NaCl solution for up to five days Originality/value The results shown in this paper provide an insight into conductive paint and corrosion protection for future industrial applications and development Keywords Coatings, Electrical conductivity, Paints, Epoxy resins, Corrosion resistance, Shearing Paper type Research paper 1 Introduction In general, a paint coating can be defined as any liquid, liquefiable or mastic composition that is converted to a solid film after application of a thin layer to a substrate The paint coating protects metallic surfaces by acting as a barrier between the metal and the environment Primarily, a paint coating consists of pigments and a binder, such as epoxy resin Epoxy resin is the binder of choice due to its low cost and good physical properties Paint coatings are typically non-conductive; however, in certain cases, a low cost thin conductive film (coating) with good electrical and physical properties is required, especially for the development of transportation and electronic technologies (Azim et al, 2006; Leong and Chung, 2006) In recent years, there have been extensive studies on resinbased conductive coatings The most common conductive fillers are graphite (Azim et al, 2006; Zheng and Wong, 2003), carbon black-silver (Leong and Chung, 2006), silica (Zhang et al, 2007), short carbon fibers (Tsotra and Friedrich, 2004), carbon nanofibers (Johnson et al, 2003), and silver-coated carbon nanotubes (Wu et al, 2007) The work described in this paper is focused on the electrical conductivity and corrosion resistance of a conductive coating composed of epoxy resin and carbon black Thus, the objective of the work was to study the conductivity and morphology of the coating in order to develop a structure-activity relationship, and to test the conductive epoxy resin carbon black material when applied to a mild steel system in a corrosive environment The current issue and full text archive of this journal is available at wwwemeraldinsightcom/ htm 57/4 (2010) q Emerald Group Publishing Limited [ISSN ] [DOI / ] 2 Experimental 21 Coating preparation The conductive coating was prepared by mixing epoxy resin (ER, DER113, Dow Chemical Co) with polyamide (A062, Eastech) The ratio of epoxy resin to polyamide was 1:1, and xylene used as a solvent Table I shows the materials used in the preparation of the conductive coating Carbon black, with a particle size of 426 mm, was used as the conductor The concentration of carbon black required in the conductive coating (CB, N220 Cabot Corporation) was calculated using the following formula: CB% ¼ weight of CB weight of CB þ weight of ER and polyamide : 22 Coating characterization Electrical conductivity tests were conducted on an advance test machine (Japan) The conductivity was determined using the equation J ¼ se, where J is the current density and E is the intensity of electrical strength The conductivity (s) was calculated from the slope of a plot of J versus E Each sample was tested at least three times under the experimental conditions The morphology of the samples was characterized with an optical microscope (Olympus, BX51M) and a field emission scanning electron microscope (FESEM) (FESEM, Zeiss Suprae, 35VP) 23 Corrosion characterization A conductive coating was spread onto a mild steel panel with dimensions of 20 5 cm, and the sample was dried at room temperature After the coating had fully cured and the thickness The authors would like to thank ExxonMobil Exploration & Production (M) Inc ( /E113) for financial support 204
2 was maintained at approximately 50 mm, a tube 70 cm long with a diameter of 18 cm was fixed onto the coating and filled with 30 wt% sodium chloride (NaCl) The coating area exposed to the electrolyte solution was 3142 cm 2, which is larger than the area proposed by ASTM G5, as the tube had to be wide enough to accommodate the reference (12 mm) and counter (2 mm) electrodes The open circuit potential (OCP) was measured over time using a saturated calomel electrode as the reference electrode and a multimeter for data collection A salt bridge was used to connect the 30 wt% NaCl and saturated potassium chloride electrolytes A frequency response analyzer (Autolab PGSTAT 30 instrument, Eco Chemie BV) was used to study the coating resistance (R c ) A platinum electrode was used as the counter electrode in the measurement of R c 3 Results 31 Analysis of electrical conductivity Figure 1 shows the electrical conductivity of different concentrations of carbon black in an epoxy resin The variation in electrical conductivity can be separated into two types: Type I For Type I samples, a small increase in conductivity was observed from CB0 to CB10 The maximum conductivity was approximately Scm 21 and was observed with a carbon black concentration of 10 wt% (sample CB10) Type II For Type II samples, a sharp increase in conductivity was observed from CB10 to CB20 The conductivity increased sharply to Scm 2 1 following the addition of 15 wt% carbon black to the epoxy resin, and Figure 1 Conductivity with varying amounts of carbon black in an epoxy resin Conductivity, σ (S cm 1 ) Electrical conductivity and corrosion protection properties Table I Composition of the conductive coating Sample name Epoxy resin (g) Polyamide (g) Carbon black (g) CB CB CB CB CB E E E E E E+00 Region I Region II Carbon black (wt%) reached a maximum of Scm 21 with a carbon black concentration of 20 wt% (sample CB20) To study the distribution of carbon black in an epoxy resin, an FESEM was used Figure 2 shows the FESEM micrographs of resins containing various concentrations of carbon black Pure epoxy resin showed an almost homogenous morphology (Figure 2(a)) Figure 2(b) shows a coating containing 5 wt% carbon black; however, the amount of carbon black in the resin was so low that it could not be detected As shown in Figure 2(c), carbon black regions were formed when the concentration of carbon black was increased In sample CB10, it was evident that a carbon black network had begun to form in the epoxy resin matrix Figure 2(d) shows that the carbon black regions in CB15 were closer to each other compared to CB10 In CB20 (Figure 2(e)), carbon black covers almost all of the epoxy resin 32 Analysis of corrosion activities Based on the electrical conductivity results, 20 wt% carbon black (CB20) was selected as the optimal concentration for corrosion studies An OCP measurement was conducted using a mild steel panel coated with CB20 and exposed to a solution of 30 wt% NaCl Figure 3 shows the OCP of a CB20 coated mild steel system versus exposure time The initial potential was 2018 V, which slowly decreased until the third day On the fourth day, the potential decreased sharply to 2047 V and then continued to gradually decrease until the tenth day to 2052 V As shown in Figure 4, the initial R c of the CB20 mild steel system was V The resistance increased from initial exposure to V on the third day After the third day, the resistance decreased sharply until the 12th day, when it reached a value of V After the 12th day, the resistance gradually declined until the end of the exposure The color of the coating turned from black to a mixture of black and brown after two weeks of exposure Figure 5 shows CB20 samples before and after the surface was exposed to 30 wt% NaCl The sample was examined to observe changes in color after exposure to a corrosive environment Optical microscope observations revealed that a portion of the CB20 surfaces turned from black to a mixture of black and brown (Figure 5(a) and (b)) To observe this area in greater detail, FESEM morphology analysis was performed The results were compared to the original sample (Figure 5(c)) and to the sample after it had been exposed to an electrolyte (Figure 5(d)) The brown area shown in the figure has corroded and the black area is the original conductive coating 4 Discussion The electrical conductivity of Type I conductive paint coatings was low and was attributed to the resin behaving as an insulator In Type II samples, a sharp increase known as the percolation threshold emerged when the filler content reached a critical amount The addition of 15 wt% carbon black transformed the epoxy resin insulator into a semiconductor The conductivity results from this work were quite consistent with those reported by others, which were on the order of Scm 2 1 (Tsotra and Friedrich, 2004; Zheng and Wong, 2003) In general, electrons move freely between carbon black particles through direct contact and by jumping from one particle to another (tunneling effect) when particle-to-particle separations are on the order of several nanometers 205
3 Figure 2 FESEM micrographs of the conductive coating CB0 CB5 (a) (b) CB10 CB15 Epoxy resin (c) (d) Carbon black CB20 (e) 10 µm Figure 3 OCP of CB20 coated mild steel in 30 wt% NaCl solution Potential (vs SCE) Exposure time (hours) Figure 4 Coating resistance of CB20 coated mild steel in 30 wt% NaCl solution R c (Ω) 20E+05 16E+05 12E+05 80E+04 40E+04 00E Exposure time (days) 206
4 Figure 5 Optical and FESEM micrographs of CB20 coated mild steel before (a and c) and after (b and d) contact with a 30 wt% NaCl solution Optic-before Optic-after (a) 008 mm (b) 008 mm FESEM-before FESEM-after (c) 10 µm Corroded area (Brownish) (d) Intact area (Black) 10 µm (Zhang et al, 2007) Based on conductivity measurements, a small amount of carbon black (eg in CB5 and CB10 samples) does not increase the conductivity of the coating The movement of electrons is impossible in these coatings because particles are too far apart and the epoxy resin acts as an insulator These results are verified by FESEM micrographs, as shown in Figure 2(b) and (c) However, in the CB15 sample, particles were closer to one another than in CB10 (Figure 2(d)) and electrons could move by direct particle contact or tunneling When carbon black particles are in direct contact (Figure 2(c)), the flow of electrons is easier and conductivity is at a maximum The corrosion protection of the sample with the highest conductivity, namely, CB20, was evaluated by OCP and electrochemical impedance spectroscopy Based on the plot of potential vs ph, the CB20 coated mild steel system, which has a potential of 2060 V and a ph of 70, lies at the intersection of the Fe 2þ /FeOH þ interface (Pourbaix, 1974) This result indicated that mild steel was corroded and the oxidized product likely precipitated at a neutral ph and formed a layered Fe 2 O 3 /Fe 3 O 4 structure (Fahlman et al, 1997) The CB20 coating was able to protect mild steel for approximately five days after which the potential declined to about V At this stage, the CB20 coated mild steel system was considered a failure The unstable and rapid changing R c was attributed to the sample adsorbing and transporting salt water to the mild steel surface 5 Conclusions The following conclusions can be made from the study: An increase in CB content from 10 to 20 wt% progressively increased the conductivity of the coating The sample with 20 wt% CB showed the highest conductivity Morphology studies suggested that the conductivity depended on the distribution of carbon black throughout the coating The carbon black in epoxy resin needed to be 20 wt% in order to improve electrical conductivity The coating protection of the sample lasted approximately five days After five days, corrosion was observed References Azim, SS, Satheesh, A, Ramu, KK, Ramu, S and Venkatachari, G (2006), Studies on graphite based conductive paint coatings, ProgOrgCoat,Vol55,pp1-4 Fahlman, M, Jasty, S and Epstein, AJ (1997), Corrosion protection of iron/steel by emeraldine base polyaniline: an X-ray photoelectron spectroscopy study, Synth Met, Vol 85, pp Johnson, JA, Barbato, MJ, Hopkins, SR and O Malley, MJ (2003), Dispersion and film properties of carbon nanofiber pigmented conductive coatings, Prog Org Coat, Vol 47, pp Leong, CK and Chung, DDL (2006), Improving the electrical and mechanical behavior of electrically conductive 207
5 paint by partial replacement of silver by carbon black, J Electron Mater, Vol 35, pp Pourbaix, M (1974), Atlas of Electrochemical Equilibria in Aqueous Solutions, National Association of Corrosion Engineers, Houston, TX Tsotra, P and Friedrich, K (2004), Short carbon fiber reinforced epoxy resin/polyaniline blends: their electrical and mechanical properties, Compos Sci Technol, Vol 64, pp Wu, HP, Wu, XJ, Ge, MY, Zhang, GQ, Wang, YW and Jiang, J (2007), Properties investigation on isotropical conductive adhesives filled with silver coated carbon nanotubes, Compos Sci Technol, Vol 67, pp Zhang, W, Blackburn, RS and Dehghani-Sanij, AA (2007), Effect of silica concentration on electrical conductivity of epoxy resin-carbon black-silica nanocomposites, Scripta Materialia, Vol 56, pp Zheng, W and Wong, S-C (2003), Electrical conductivity and dielectric properties of PMMA/expanded graphite composites, Compos Sci Technol, Vol 63, pp Corresponding author AA Mohamad can be contacted at: azmin@engusmmy To purchase reprints of this article please reprints@emeraldinsightcom Or visit our web site for further details: wwwemeraldinsightcom/reprints 208
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