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Construction www.elsevier.com/locate/conbuildmat Construction and Building Materials 21 (2007) 1161–1169 and Building MATERIALS Atmospheric corrosion of steel reinforcing bars produced by various manufacturing processes E. Zitrou, J. Nikolaou, P.E. Tsakiridis *, G.D. Papadimitriou National Technical University of Athens, Department of Mining and Metallurgical Engineering, Laboratory of Physical Metallurgy, 9 Iroon Polytechniou Street, 157 80 Zografou, Athens, Greece Received 19 June 2006; received in revised form 26 June 2006; accepted 28 June 2006 Available online 17 August 2006 Abstract The aim of the present investigation is to evaluate the effect of manufacturing process upon the performance of reinforcing steel bars against atmospheric corrosion. Reinforcing steel bars produced by different manufacturing methods were exposed to the atmosphere in Athens for different periods of time. The progress of corrosion was evaluated by measuring the thickness of the corrosion layer formed on the surface of the bars. The morphology of the corroded layer was studied by optical and scanning electron microscopy (SEM), while X-ray diffraction analysis was used to identify the mineralogical composition of the corrosion products. Independently of the manufac- turing process used, the main corrosion product formed was lepidocrocite (c-FeOOH), followed closely by akaganeite (b-FeOOH) and goethite (a-FeOOH). Furthermore, it was found that the surface condition and the initial oxide layer on the steel bars, which is closely related to the manufacturing process, played a major role in the development of corrosion in atmosphere. Work-hardened reinforcing steel bars were found very sensitive to exhibition in the usual atmospheric conditions, followed by the Tempcore steel bars. The hot- rolled bars, either unalloyed or microalloyed with vanadium, presented the best corrosion behavior. � 2006 Elsevier Ltd. All rights reserved. Keywords: Reinforcing concrete bars; Atmospheric corrosion 1. Introduction The degradation of reinforcing steel due to corrosion is of great concern for the durability of concrete structures and implies serious economic losses [1]. Considerable research work has been carried out on measuring the amount of corrosion of reinforcing steel bars and evaluat- ing their corresponding bond strength with concrete [2–7]. The results indicate that the ultimate bond strength initially increases with increasing degree of corrosion, until it reaches a maximum value at about 4% weight gain, after which there is a sharp reduction in the ultimate bond strength up to 6% weight gain [2]. The change of bond strength is usually attributed to the increase of the surface roughness and to the volumetric expansion of the steel 0950-0618/$ - see front matter � 2006 Elsevier Ltd. All rights reserved. doi:10.1016/j.conbuildmat.2006.06.004 * Corresponding author. Tel.: +30 210 7722234; fax: +30 210 7722218. E-mail address: ptsakiri@central.ntua.gr (P.E. Tsakiridis). accompanying the development of the corrosion products [8]. Corrosion products on the surface of reinforcing steel bars generally exist before they are embedded in a concrete structure. This is because reinforcements are usually exposed to the atmosphere during transportation and stor- age in the building sites for a long period before installa- tion. Unfortunately, the progress and nature of corrosion products formed on the steel before embedment, has not received sufficient attention. The corrosion process in the atmosphere is affected by both steel chemistry and environ- mental conditions, namely duration of exposure, tempera- ture, and wet-dry cycles and the composition of the electrolyte that wets the metal surface [9,10]. In particular, steel bars can be contaminated by chloride ions from sea spray or windblown salt. The electrolyte is of crucial ther- modynamic and kinetic significance in the process. In fact, its presence triggers the typical electrochemical reactions mailto:ptsakiri@central.ntua.gr 1162 E. Zitrou et al. / Construction and Building Materials 21 (2007) 1161–1169 involved and its nature determines the extent of attack. In this respect, some of the hundreds of chemicals contained in the atmosphere can be incorporated into the electrolyte and play significant role in atmospheric corrosion of metals [9]. Exposed steel will be corroded in moist atmospheres due to differences in the electrical potential on the steel surface, forming anodic and cathodic sites. The metal oxidizes at the anode, where corrosion occurs according to: FeðmetalÞ ! Fe2þðaqÞ þ 2e� ð1Þ Simultaneously, reduction occurs at cathodic sites, typi- cal cathodic processes being: 1=2O2 þH2Oþ 2e� ! 2OH�ðaqÞ ð2Þ 2HþðaqÞ þ 2e� ! H2ðgasÞ ð3Þ The electrons produced during this process are con- ducted through the metal whilst the ions formed are trans- ported via pore water, which acts as the electrolyte. Electrolyte is formed due to the adsorption of moisture and condensation within the mineral deposits and oxida- tion products on the steel surface. From the above it is clear that the propensity of steel bars to atmospheric corro- sion is influenced by the nature of the mineral layer present on their surface. This layer begins to form as early as the manufacture of the bars and may facilitate or hinder corro- sion, serving either as a barrier or as a path for ion exchange with the atmosphere. Previous work has exam- ined the pitting corrosion of steel reinforcements and found that hot-rolled steels presented a slightly better pitting cor- rosion resistance than cold worked steels. This was attrib- uted to the compressive residual stresses on the surface of hot-rolled steel in contrast to the high tensile stresses devel- oped on cold worked steel [11]. The manufacture of reinforcing steel bars always involves, at some production stage, hot-rolling of billets, which is mostly performed in the austenitic condition of steel. During hot-rolling the steel surface is exposed to air and water, the latter being used for controlling the temper- ature of the rolls and/or the cooling rate of the steel. This leads to the formation of a particular oxide layer on the surface of the bars. Depending on the production method, the oxide surface film presents different composition, thick- ness and adherence to the metal substrate. In the case of thermomechanically strengthened steels (commonly known as Tempcore steels), drastic water cooling and the thermal cycle subsequent to self-tempering of the bar, contributes to the formation of a thin and well adherent protective layer on the surface, which is claimed to enhance the corro- sion resistance of steel bars [12]. The iron oxides act as a barrier, i.e., as a protective layer, slowing further corrosion processes down [13]. In the present investigation the effect of the steel manu- facturing method upon the performance of reinforcing con- crete bars against atmospheric corrosion is studied. Optical and scanning electron microscopy (SEM) was used to examine the corroded layer on the surface, while the pro- gress of atmospheric corrosion was evaluated by measuring the thickness of the corrosion layer. Furthermore XRD analyses were used in order to identify the mineralogical species present in the corrosion products. 2. Experimental Actual methods for the production of high-strength reinforcing steel bars may be classified into three distinct categories: (a) Hot-rolled steels: For these steels increasing the amount of alloying elements (mainly C and Mn) results in increased strength, but reduces their welda- bility. As an alternative issue, hot-rolled microalloyed steels are produced, in which small additions of strong carbide formers, such as Nb and/or V, enhance the strength mainly by grain refinement, without affecting their weldability. (b) Thermomechanically strengthened steels (Tempcore, Thermex, etc): The steel bars consist of a soft core of ferrite–pearlite microstructure and a hard and strong surface layer of bainite andtempered martens- ite. This particular microstructure is produced by drastic cooling of the surface of the bars through water spray after exiting the last rolling pass and while steel is in the austenitic condition. (c) Work-hardened steels: They are produced through twisting, drawing or cold rolling, of previously hot- rolled steel bars and present a slightly work-hardened microstructure, which provides the necessary strength. Four different sets of commercial reinforcing steel bars, namely: (a) hot-rolled, (b) hot-rolled microalloyed with vanadium, (c) Tempcore and (d) work-hardened were used. Chemical composition of the investigated reinforcing steels is shown in Table 1. Hot-rolled steel belongs to the class of 400 MPa yield strength and is not readily weldable, due to its high carbon content. All other steels, i.e., hot-rolled microalloyed with vanadium, Tempcore and work-hard- ened reinforcing steels are weldable and fall into the 500 MPa class of yield strength. The steel samples were cut 500 mm long and tagged to show the size and type of steel. Afterwards they were exposed in the atmosphere for periods of one, three, six and nine months, starting from September. The exposure took place on the roof of a two-floor building located 4 km north-east from the center of Athens and about 12 km from sea-shore, at the campus of National Technical University of Athens. It should be emphasized that the specimens were prepared immediately after their produc- tion in the steel plant and were exposed in the atmosphere in the as-received condition, i.e., without removing or cleaning the initial oxide layer from their surface. Table 2 summarizes the environmental conditions at the exposure site. The climatic conditions were obtained from Table 1 Chemical composition of reinforcement steel bars Type of steel rebars Chemical composition (%) C Si S P Mn Ni Cr Mo V Cu Sn Co Hot-rolled 0.375 0.287 0.029 0.022 1.304 0.064 0.085 0.009 0.003 0.197 0.016 0.000 Hot-rolled microalloyed with vanadium 0.246 0.154 0.043 0.014 1.029 0.143 0.127 0.023 0.050 0.502 0.020 0.011 Tempcore 0.219 0.193 0.047 0.015 0.870 0.106 0.082 0.014 0.001 0.261 0.016 0.010 Work-hardened 0.271 0.160 0.046 0.027 0.786 0.099 0.168 0.013 0.001 0.532 0.023 0.001 Table 2 Monthly average values of environmental conditions concerning the exposure periods Date Temperature (�C) Relative humidity (%) Rainfall (mm) Evaporation (mm) Wind speed (m/s) Sunlight duration (min) Solar irradiation (W/m2) Barometric pressure (hPa) 09/2002 22.20 73.68 34.00 118.80 2.34 4279.98 175.59 990.08 10/2002 17.42 73.67 36.60 161.20 2.09 14,308.47 152.47 994.44 11/2002 13.36 84.15 137.60 – 1.65 8986.84 95.53 994.97 12/2002 9.08 82.50 202.60 �9.20 2.88 4192.17 57.57 994.87 01/2003 10.32 77.85 97.40 �86.20 3.28 5641.82 71.40 991.71 02/2003 4.93 76.03 73.40 �53.40 3.42 5085.31 88.73 994.03 03/2003 8.42 68.36 29.20 105.40 3.22 10,420.70 150.66 994.89 04/2003 11.91 68.92 45.20 76.70 2.46 11,020.62 178.51 991.37 05/2003 21.37 55.74 18.20 100.40 2.28 19,537.62 253.03 991.41 06/2003 25.29 48.13 0.00 250.00 2.77 21,515.19 279.68 990.39 E. Zitrou et al. / Construction and Building Materials 21 (2007) 1161–1169 1163 the Meteorological Station at the National Technical Uni- versity Campus. In Athens environment, the major con- tributors to the atmospheric corrosion process are the SO2 and Cl � [14]. After the exposure period, optical and scanning electron microscopy (SEM) was used to investigate the corroded layer in polished sections. The preparation of polished sec- tions started by impregnating the selected sample with a low viscosity epoxy resin under vacuum. After cutting via micro-saw, the sample was grinded and polished down to 1 lm diamond paste on a lapping disk. The surface mor- phology was studied using a Jeol 6100 scanning electron microscope (SEM). Chemical composition of the rust on the surface of the specimens was carried out by a Noran TS 5500 electron dispersive spectrometer (EDS) connected to the SEM. The progress of atmospheric corrosion was evaluated by measuring the thickness of the external corro- sion layer. Eight measurements were performed for each sample and the average value and standard deviation was calculated. Furthermore XRD analyses were performed in order to identify the various corrosion products. The rust layer from the surface was carefully scraped from the metallic substrate using a razor blade and was ground in an agate mortar. XRD measurements were conducted with a Sie- mens D5000 diffractometer using nickel-filtered Cu Ka1 radiation (=1.5405 A), 40 kV voltage and 30 mA current. 3. Results and discussion 3.1. Macroscopic observation Exposure of the reinforcing steels to the atmosphere leads in general to the formation of corrosion products of variable composition and indefinite layering that exhibit cavities and cracks in various directions. The different col- ours observed in the metallographic microscope (orange, red, grey and brown) are ascribed to the presence of amor- phous and crystalline oxy-hydroxides, and the black zones to magnetite, as will be shown in next section. More specifically, hot-rolled steel and hot-rolled micro- alloyed with vanadium steel present a relatively uniform dark oxide layer at their initial state. Surface examination shows that atmospheric corrosion begins as a localized attack on the top of ribs. These points of maximum deformation are sites where the initial oxide layer is thin- ner. Upon extended exposure to the atmosphere, the attack becomes rather uniform, covering the entire surface. In the case of hot-rolled steel, the initial oxide layer remains nearly intact, even after three months of exposure to the environment, Fig. 1. Exposure for six months results in the formation of corrosion products on the metal sur- face, partial fragmentation and delamination, leaving areas of metal in direct contact with the corrosive environment. However, the remaining initial oxide layer is coherent to the metal substrate. Corrosion products on the surface of the hot-rolled microalloyed with vanadium steel are observed on the top of ribs as early as one month of atmospheric exposure, Fig. 2. Compared to the hot-rolled steel, the surface oxide layer is not fragmented, but consists of low adherence cor- rosion products. Atmospheric corrosion does not always form preferen- tially on the top of ribs. In the case of Tempcore steels, cor- rosion covers almost uniformly the surface of the bar and low adherence corrosion products are formed with time of exposure, Fig. 3. Fig. 2. Macroscopic aspect of hot-rolled vanadium microalloyed reinforcing steel (a) in the as-received state and after exposure to the atmosphere for a period of (b) 3 months, (c) 6 months and (d) 9 months. Fig. 3. Macroscopic aspect of Tempcore reinforcing steel (a) in the as received state and after exposure to the atmosphere for a period of (b) 3 months, (c) 6 months and (d) 9 months. Fig. 1. Macroscopic aspect of hot-rolled reinforcing steel (a) in the as-received condition and after exposure to the atmosphere for a period of (b) 3 months, (c) 6 months and (d) 9 months. 1164 E. Zitrou et al. / Construction and Building Materials 21 (2007) 1161–1169 The cold drawing employed for the production of work- hardened steel bars of this investigation, caused the frag- mentation of the initial oxide layer and resulted to a surface rather free of oxides, Fig. 4. As in the case of Tempcore steels, atmospheric corrosion seems to be uniform and is visible even as soon as after one month of exposure. 3.2. Scanning electron microscopy observations Figs. 5–8 show the width and morphology of the rust layers in cross sections perpendicular to the longitudinal Fig. 4. Macroscopic aspect of work-hardened reinforcing steel (a) in the as-r months, (c) 6 months and (d) 9 months. axis of the bars, as-received and after exposure to the atmo- sphere for three and six months. Reinforcing steels pro- duced by different processes show differencesnot only in the as-received state but also after atmospheric corrosion. Hot-rolled steel (Fig. 5) presents a relatively uniform oxide layer of about 10–15 lm in the initial state. It is clear that the thickness of the corrosion products is kept stable even after six months of exposure (Fig. 5c), protecting the substrate steel surface from further corrosion by block- ing air and humidity. The corrosion layer is crack free and coherent to the substrate metal surface. This is also visible eceived state and after exposure to the atmosphere for a period of (b) 3 Fig. 5. SEM micrographs of rust layers from hot-rolled reinforcing steel (a) in the as-received state and after exposure to the atmosphere for a period of (b) 3 months, and (c) 6 months and (d) surface morphology after 6 months. Fig. 6. SEM micrographs of rust layers from hot-rolled vanadium microalloyed reinforcing steel (a) in the as-received state and after exposure to the atmosphere for a period of (b) 3 months, and (c) 6 months and (d) surface morphology after 6 months. Fig. 7. SEM micrographs of rust layers from Tempcore reinforcing steel (a) in the as-received state and after exposure to the atmosphere for a period of (b) 3 months, and (c) 6 months and (d) surface morphology after 6 months. Fig. 8. SEM micrographs of rust layers from work-hardened reinforcing steel (a) in the as-received state and after exposure to the atmosphere for a period of (b) 3 months, and (c) 6 months and (d) surface morphology after 6 months. E. Zitrou et al. / Construction and Building Materials 21 (2007) 1161–1169 1165 by macroscopic observation as mentioned in previous section. The initial oxide thickness of hot-rolled vanadium microalloyed reinforcing steel is about 10–15 lm (Fig. 6a). As in the case of the hot-rolled steel, the increase of thickness of the corrosion products after six months (Fig. 6c) of exposure is small but the formation of cracks in the corrosion layer allows passage of water and air and results in delamination of the corrosion layer, leaving at some places the metal substrate in direct contact with the corrosive environment (Fig. 6d). Tempcore steel (Fig. 7) is characterized by a relatively thin (6 lm) initial oxide layer. Exposure to the atmosphere results in rapid formation of corrosion products, which is reflected by a significant increase of thickness of the rust layer (Fig. 7b,c). Work-hardened steels in the as-received state are practi- cally oxide free and the metal surface is in direct contact with the corrosive environment resulting in rapid forma- tion of rust (Fig. 8b–d). More detailed observation shows that in the case of the Tempcore and work-hardened reinforcing steels the corro- sion coating generally consists of two distinct layers, the inner one closer to the steel substrate and the outer one near to the external surface. The particle size of the inner corrosion products is smaller than that of the outer ones. 1166 E. Zitrou et al. / Construction and Building Materials 21 (2007) 1161–1169 The outer layer could be removed very easily from the sub- strate, while the inner one is more adherent. The layering observed for the Tempcore and work-hard- ened steels is not visible in the case of hot-rolled steels and vanadium microalloyed steels, since the corrosion layer remains during atmospheric corrosion remains basically the same formed during the production process. EDAX spot analyses revealed, independently of the steel type, the presence of sulfur and chloride in the corrosion products, which are probably in the form of iron sulfates and iron chlorides, respectively. Chloride and sulfate anions are able to pass through the initial layers of iron oxides and to initiate corrosion, resulting in rupture of the passive layer and causing localized attack. The forma- tion of sulfates takes place simultaneously with the genera- tion of iron chlorides. SO2 and O2 are initially absorbed on the surface and later on converted to sulfate ions with elec- trons provided by the dissolution of iron. The reaction of negatively charged sulfate ions with ferrous ions leads to the formation of ferrous sulfate (FeSO4) at anodic sites. Thereafter the ferrous sulfate oxidizes to ferric sulfate, which in turn hydrolyses to produce iron oxy-hydroxides, with generation of sulfuric acid [15]. The progress of atmospheric corrosion was evaluated quantitatively by measuring the thickness of the corrosion products, Fig. 9. Since carbon steels are not alloyed, it is not surprising that different types do not exhibit large dif- ferences in the atmospheric corrosion rate. Nevertheless, from the diagram of Fig. 9 it becomes clear that the type of steel exhibiting the lowest resistance to atmospheric corrosion is the work-hardened steel, fol- lowed closely by the Tempcore steel. Hot-rolled steels with or without vanadium microalloying may be considered as Fig. 9. Thickness of the externa the most satisfactory, presenting very similar behavior. As a matter of fact, the hot-rolling process leads to the cre- ation of a massive external iron oxides layer, which pre- vents the fast penetration of the corrosive anions of the atmosphere. On the other hand, the absence of the initial oxide layer in the case of the work-hardened steel, may be considered as partially responsible for its low corrosion resistance. The role of the residual stresses coming from the deformation process (twisting or stretching) should how- ever not be disregarded. In the case of the Tempcore steel the relatively low corrosion resistance may be attributed to both the low thickness of the initial oxide layer and to the heterogeneity of the microstructure, i.e. presence of tempered martensite, bainite and ferrite/pearlite in concen- tric layers. As in the case of the strain hardened steel, the role of the residual stresses coming from the quenching process should not be disregarded, although tempering may have weakened their effect. 3.3. Mineralogical analysis of the rust by X-ray diffraction The XRD diagrams (Figs. 10–13) show that the initial layer of the examined steels consists of hematite (Fe2O3), magnetite (Fe3O4) and wustite (FeO). The main corrosion product formed after exposure to the atmosphere is lepidocrocite (c-FeOOH), followed by akagaenite (b-FeOOH) and goethite (a-FeOOH), which are typical in the case of atmospheric corrosion of carbon steel, as it comes out from other studies [16,17]. The minerals, which are detected in the first months of exposure are mainly lepidocrocite and akaganeite. The absence or the low content of goethite in the rust layers is an indication of chloride ions present in the atmosphere. l corrosion products layers. 0 50 100 150 200 250 300 350 400 450 500 5 10 15 20 25 30 35 40 45 50 55 In te ns it y (c ps ) 6 Months 3 Months Initial 1. Magnetite - Fe3O4 2. Wustite - FeO 3. Hematite - Fe2O3 4. Lepidocrocite FeO(OH) 5. Akaganeite Fe(O,OH,Cl) 6. Goethite FeO(OH) 7. Iron - Fe 6 5 4,5 1 3 1 4 2 4 2 1 1 7 4 4 4 Fig. 10. X-ray diffraction of oxide layer and corrosion products of hot-rolled reinforcing steel in the initial state and after 3 and 6 months of exposure to the atmosphere. 0 100 200 300 400 500 600 5 10 15 20 25 30 35 40 45 50 55 In te ns it y (c ps ) Initial 3 Months 6 Months 1. Magnetite - Fe3O4 2. Wustite - FeO 3. Hematite - Fe2O3 4. Lepidocrocite FeO(OH) 5. Akaganeite Fe(O,OH,Cl) 6. Goethite FeO(OH) 7. Iron - Fe 6 4 4,5 1 3 1 4 2 1 7 7 4 4 5 3 2 Fig. 11. X-ray diffraction of oxide layer and corrosion products of hot-rolled microalloyed with vanadium reinforcing steel in the initial state and after 3 and 6 months of exposure to the atmosphere. E. Zitrou et al. / Construction and Building Materials 21 (2007) 1161–1169 1167 As a matter of fact, in environments with high levels of chlorides, akagaenite is formed instead of goethite [18,19]. It should be noticed that after six months of expo- sure at the open atmosphere wustite is converted to oxy- hydroxide,whereas the transformation of magnetite seems to be delayed, an indication that the external initial layer of the iron oxides acts as a barrier, a protective layer slowing further the corrosion processes down. 0 100 200 300 400 500 600 5 10 15 20 25 30 35 40 45 50 55 2θ In te ns it y (c ps ) 6 Months Initial 3 Months 1. Magnetite - Fe3O4 2. Wustite - FeO 3. Hematite - Fe2O3 4. Lepidocrocite FeO(OH) 5. Akaganeite Fe(O,OH,Cl) 6. Goethite FeO(OH) 7. Iron - Fe 6 5 4,5 1 3 1 2 4 2 1 1 7 4 4 4 1 Fig. 12. X-ray diffraction of initial oxide layer and corrosion products of temcore reinforcing steel in the initial state and after 3 and 6 months of exposure to the atmosphere. 0 50 100 150 200 250 300 350 400 450 500 5 10 15 20 25 30 35 40 45 50 55 2θ In te ns io n (c ps ) 1. Magnetite - Fe3O4 2. Wustite - FeO 3. Hematite - Fe2O3 4. Lepidocrocite FeO(OH) 5. Akaganeite Fe(O,OH,Cl) 6. Goethite FeO(OH) 7. Iron - Fe 6 Months 3 Months Initial 6 5 4,5 1 3 1 4 2 4 2 1 1 7 7 4 2 4 4 Fig. 13. X-ray diffraction of initial oxide layer and corrosion products of work-hardened reinforcing steel after 3 and 6 months of exposure to the atmosphere. 1168 E. Zitrou et al. / Construction and Building Materials 21 (2007) 1161–1169 E. Zitrou et al. / Construction and Building Materials 21 (2007) 1161–1169 1169 4. Conclusions The aim of the present research work is to evaluate the effect of reinforcing steel production method (hot-rolled, hot-rolled microalloyed with vanadium, Tempcore and work-hardened) upon their resistance to atmospheric corrosion. XRD analysis showed that the main corrosion product found was lepidocrocite (c-FeOOH), followed closely by akaganeite (b-FeOOH), which is typical of marine areas, and goethite (a-FeOOH). It is found that the stability of the initial oxide surface layer of the steel bar plays a critical role in further corrosion. 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Atmospheric corrosion of steel reinforcing bars produced by various manufacturing processes Introduction Experimental Results and discussion Macroscopic observation Scanning electron microscopy observations Mineralogical analysis of the rust by X-ray diffraction Conclusions References
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