Yunan Prawoto, K. Ibrahim, and W.B.

Wan Nik

EFFECT OF pH AND CHLORIDE CONCENTRATION ON THE CORROSION OF DUPLEX STAINLESS STEEL

*Yunan Prawoto
Faculty of Mechanical Engineering Universiti Teknologi Malaysia, 81310 UTM, Skudai, Johor, Malaysia

K. Ibrahim
.ExxonMobil Exploration and Production Malaysia Inc 15:041E, Menara ExxonMobil, Kuala Lumpur City Centre 50088 Kuala Lumpur, Malaysia

and W. B. Wan Nik

Faculty of Maritime Studies and Marine Science University Malaysia Terengganu, 21030 Kuala Terengganu, Malaysia

:
) (austeniticferritic . , . , . . 50223 . UNS S . 84 , ASTM G . PREN

:Corresponding Author E-mail: yunan.prawoto@gmail.com 9002 Paper Received 17 September 2009; Paper Revised 18 October 2009; Paper Accepted 16 December

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ABSTRACT Stainless steels are widely used as structural materials even in aggressive environments due to their good mechanical and corrosion properties. In particular, duplex (austeniticferritic) stainless steels are becoming common materials for oil and gas applications, specifically facilities that were built after the 1970s. This expansion in the utilization of such materials can be attributed to their excellent combination of properties, such as higher strength, good resistance to stress corrosion cracking, and comparable cost to conventional austenitic stainless steels. This research is mainly concerned about the corrosion performance of a duplex stainless steel alloy under several conditions using various pH and chloride concentrations at different temperatures. Corrosion rates and pitting morphology of the selected duplex stainless steel were systematically evaluated during this study. The effects of pH and chloride concentrations on the corrosion behavior of duplex stainless steel were carried out in accordance with UNS S32205. The effect of pH was has been determined by using different test solutions at different test temperatures. The duration of immersion tests were set in accordance to the ASTM G48 standard. However, the effect of chloride concentrations on the corrosion of the selected alloy is determined by pitting corrosion measurements using simple metallography and software analysis as well as PREN (Pitting Resistance Equivalent Number). Key words: duplex stainless steel, pH, chloride concentration, corrosion

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EFFECT OF pH AND CHLORIDE CONCENTRATION ON THE CORROSION OF DUPLEX STAINLESS STEEL

1. INTRODUCTION Stainless steel is one of the most important materials in the engineering world. The materials wide applications in chemical, petrochemical, off-shore, and power generation plants prove that it is one of the most reliable materials. In particular, duplex (austeniticferritic) stainless steels are very popular in the oil and gas industries built after the 1970s. This expansion is associated with their excellent combination of properties, such as higher strength than austenitic stainless steel, better stress corrosion resistance, and similar price to conventional stainless steels [1]. With the aging of those structures, quantification of all factors that can contribute to the failure became more important. Two of those factors are the chloride effect and the effect of pH. These two factors are essential components of a failure analysis tool since a lot of the failures related to environments are linked to corrosion. Understanding the effect of the pH and the chloride concentration is a key factor in life assessment as well as in the failure analysis of structures utilizing duplex stainless steel. As in other metals, corrosion in duplex stainless steel breaks down essential properties due to chemical reactions with its surroundings. Certain environments offer opportunities for these metals to combine chemically with elements to form compounds and return to their lower energy levels. Ultimately, it corrodes on contact with water (and moisture in the air), acids, bases, salts, oils, aggressive metal polishes, and other solid and liquid chemicals. It can also corrode when exposed to gaseous materials like acid vapors, formaldehyde gas, ammonia gas, and sulfur containing gases.

Duplex stainless steel Traditionally, the word duplex stainless steel refers to a mixture of body-centered cubic (BCC) ferrite and facecentered cubic (FCC) austenite crystal structures. Most duplex stainless steels are intended to contain similar amounts of ferrite and austenite phases in the annealed condition. Duplex stainless steels generally have similar corrosion resistance to austenitic alloys and they typically have better stress corrosion cracking resistance than austenitic stainless steel. They have existed for more than 60 years. The early grades were simple alloys of chromium, nickel, and molybdenum. The first wrought duplex stainless steels were produced in Sweden in 1930 and were used in the sulfite paper industry. These grades were developed to reduce the intergranular corrosion problems in the early, high-carbon austenitic stainless steels. One of the first duplex grades developed specifically for improved resistance to chloride stress corrosion cracking (SCC) was 3RE60. AISI type 329 became well-established after World War II and was used extensively for heat exchanger tubing for nitric acid service. In subsequent years, both wrought and cast duplex grades have been used for a variety of process industry applications, including vessels, heat exchangers, and pumps. Duplex stainless steels also generally have greater tensile and yield strengths, but poorer toughness than austenitic stainless steels. Nowadays, type 2205 is the most widely used duplex stainless steel grade. It finds applications due to both excellent corrosion resistance and high strength [2]. 2. METALLURGICAL PROPERTIES AND MAIN ALLOYING ELEMENTS IN DUPLEX STAINLESS STEELS Compared to conventional austenitic stainless steels, duplex stainless steels are stronger and more resistant to localized corrosion, particularly pitting, crevice corrosion, and stress corrosion cracking. They are characterized by high chromium (1928%), molybdenum (up to 5%), and lower nickel content than austenitic stainless steels. They can be divided into four groups. The first group is Lean Duplex, such as 2304, which contains no deliberate molybdenum addition. The second group is 2205, the work-horse grade accounting for more than 80% of duplex usage. The third group is 25% chromium duplex, such as Alloy 255 and DP-3. The fourth group is Super Duplex, with 2526% chromium and increased molybdenum and nickel compared with 25% chromium grades, including grades such as 2507, Zeron 100, UR 52N+, and DP-3W [3]. Compared to austenitic stainless steels, duplex stainless steels differ mainly in their chromium, nickel, and molybdenum contents. Chromium is a ferrite former. At higher chromium content, more nickel is necessary to form an austenitic or duplex structure. Higher chromium also promotes the formation of intermetallic phases. There are usually at least 18% Cr in austenitic stainless steels and at least 22% in second-generation duplex stainless steels. Chromium also increases the oxidation resistance at elevated temperatures. This chromium effect is important

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because of its influence on the formation and removal of oxide scale or heat tint resulting from heat treatment or welding. On the other hand, nickel is an austenite stabilizer. That means that the addition of nickel to iron-based alloys promotes a change of the crystal structure of stainless steel from body-centered cubic (ferritic) to face-centered cubic (austenitic). Ferritic stainless steels contain little or no nickel, duplex stainless steels contain an intermediate amount of nickel, such as 4 to 7%, and the 300-series austenitic stainless steels contain at least 8% nickel (see Figure 1). The addition of nickel delays the formation of detrimental intermetallic phases in austenitic stainless steels but is far less effective than nitrogen in delaying their formation in duplex stainless steels. The face-centered cubic structure is responsible for the excellent toughness of the austenitic stainless steels. Its presence in about half of the microstructure of duplex grades greatly increases their toughness relative to ferritic stainless steels [4].

Figure 1. Schematic of the microstructural change due to nickel increment. Increasing the nickel content changes the microstructure of a stainless steel from ferritic to duplex to austenitic

The addition of nitrogen promotes structural hardening by the interstitial solid solution mechanism, which raises the yield strength and ultimate strength values without impairing toughness. Moreover, the two-phase microstructure guarantees higher resistance to pitting and stress corrosion cracking in comparison with conventional stainless steels [5]. 3. PROPERTIES AND CHARACTERISTICS Coinciding with the 1970s development of offshore gas and oilfields in the North Sea, a second-generation duplex was introduced and quickly became the duplex steel of choice. With the deliberate addition of nitrogen as an alloying agent, both improved toughness in the heat-affected zones of welds and excellent chloride corrosion resistance was achieved, thus, quickly becoming the workhorse of stainless steels, accounting for more than 80% of duplex use. Its popularity is also cost-based with the replacement of the nickel content with the less-expensive addition of nitrogen [5]. Duplex alloys are essentially a compromise possessing some of the ferritic stress corrosion

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cracking resistance and much of the superior formability of the common austenitic stainless alloys, at a cost saving over the high nickel alloys. Duplex stainless steels generally have similar corrosion resistance to austenitic alloys except they typically have better stress corrosion cracking resistance. Duplex stainless steels also generally have greater tensile and yield strengths, but poorer toughness than austenitic stainless steels. A significant feature of duplex stainless steel is that its pitting and crevice corrosion resistance is greatly superior to that of standard austenitic alloys. Pitting resistance equivalent numbers (PREN), a standard industry measure, are often in the high 30s, while the latest duplex alloys have a PREN in excess of 40. This is an increasingly common specification for certain offshore duties. However, PREN numbers only provide an approximate grading of alloys and do not account for the microstructure of the material. An acceptance corrosion test on material in the supply condition is so much more meaningful [6]. Duplex stainless steels have exceptional mechanical properties. Their room temperature yield strength in the solution-annealed condition is more than double that of standard austenitic stainless steels not alloyed with nitrogen. This may allow the design engineer to decrease the wall thickness in some applications. The typical yield strengths of several duplex stainless steels are compared with that of 316L austenitic stainless steel between room temperature and 300C (570F). Because of the danger of 475C (885F) temper-embrittlement of the ferritic phase, duplex stainless steels should not be used at temperatures above those allowed by the applicable pressure vessel design code for prolonged periods of time. The mechanical properties of wrought duplex stainless steels are highly anisotropic. This is mainly the result of the elongated grains and the crystallographic texture that results from hot or cold rolling. While the solidification structure of duplex stainless steel is typically isotropic, it is rolled or forged and subsequently annealed with both phases present. The appearance of the two phases in the final product reveals the directionality of the processing. The strength is higher perpendicular to the rolling direction than in the rolling direction. The impact toughness is higher when the crack propagates perpendicularly to the rolling direction than in the rolling direction. The measured toughness will be higher for a longitudinal (L-T) Charpy test specimen than for other test directions. The impact energy of a transverse specimen from a duplex stainless steel plate will typically be 1/2 to 2/3 that of a longitudinal specimen. Despite the high strength of duplex stainless steels, they exhibit good ductility and toughness. Compared with carbon steel or ferritic stainless steels, the ductile-to-brittle transition is more gradual. Duplex stainless steels retain good toughness even to low ambient temperatures, for example, -40C/F; however, ductility and toughness of duplex stainless steels are lower than those of austenitic stainless steels. Austenitic stainless steels typically do not show a ductile-to-brittle transition and maintain excellent toughness down to cryogenic temperatures. 3.1. Usage in Corrosive Environment Following the rule of material selections, attention at every stage of the design, construction, and operation must be given for any application. For duplex stainless steels, mostly their usage is for offshore oil and gas application. Thus, the specification and use of materials which combine corrosion resistance with high mechanical strength is a fundamental requirement [7]. Metals manufacturers have spent much time and effort in developing alloys specifically to meet offshore needs. The alloys developed have had to be suitable for shafts and bolting, as well as many other applications. These have included sea water and process pipework, water injection and booster pumps, line shaft pumps, emergency shutdown valves, anchorages and tensioners for riser protection systems, multiphase pumps, and remotely operated vehicle components. The most significant contribution to the fight against corrosion offshore has been made by duplex stainless steels. These have often been adopted on offshore structures in preference to carbon steel or other stainless steels. The value of the duplex stainless steel is that it combines the basic toughness of the more common austenitic stainless steels with the higher strength and improved corrosion resistance of ferritic steels. The optimum chemical composition of these steels provides a high level of corrosion resistance in chloride media together with high mechanical strength and ductility. Other benefits include the ability of some duplex stainless steels to be used at quite low sub-zero temperatures and to resist stress corrosion cracking [8]. Offshore structures themselves present different requirements of materials depending upon whether their application is topside, splash zone, or subsea. Topside, duplex materials are suitable for a wide range of bolting applications, and materials such as Ferralium alloy 255 provide up to B7 steel strength, excellent corrosion resistance, and a service life equal to the life of the system, thereby contributing to reduced maintenance costs. In the splash zone, the alloy has already demonstrated its suitability for sea water resistance with over 15 years service on North Sea installations, and has been widely employed for riser bolting and components on riser protection systems [9].

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Other applications which can benefit from the use of these high alloy super duplex steels involve piping systems, pumps (where the good erosion and abrasion resistance is employed), valves, heat exchangers, and other equipment. There are many other applications for duplex stainless steel, such as heat exchangers, tubes and pipes for the production and handling of gas and oil, and desalination plants. Also, this stainless steel is applied to pressure vessels, pipes, tanks, and heat exchangers for the processing and transport of various chemicals, or in process industries handling solutions containing chlorides. In addition, duplex stainless steel is applied in rotors, fans, shafts, and press rolls where the high corrosion fatigue strength can be utilized. It also applied to cargo tanks, piping, and welding consumables for chemical tankers. Table 1 summarizes the performance of the duplex stainless steels in various environments [10,11]. Table 1. Performance of Different Alloys in Different Environment Environment Chlorides Chlorides/Halides Hydrochloric Acid Hydrofluoric Acid Sulfuric Acid General Acidic Attack Problem Pitting, crevice corrosion Stress corrosion cracking Pitting, crevice corrosion Pitting, crevice corrosion Pitting, crevice corrosion Critical Pitting Poor 300 Series SS 300 Series SS Titanium, Duplex, 20 Cb-3 Duplex Alloys Copper-Nickel (Alloy 601) 300 Series SS Good Duplex alloys 317L Duplex alloys Alloy 22, 276 Silver, Gold 20 Cb-3 317L Duplex Alloys Best Alloy 276 Alloy 600/625 Zirconium, Tantalum Copper, Alloy 400 Alloy 622 Alloy 25-6 Mo Alloy 625

4. EXPERIMENTAL METHOD The tests samples were prepared from a pipe that was then split and flattened into plates by using Computer Numerical Control Wire Electrical Discharge Machining (CNC WEDM). A GDS 500A Glow Discharge Spectrometer was employed to determine the chemical composition. The results of the chemical composition and the mechanical properties are shown in Table 2 and Table 3, respectively.

Table 2. Result of GDS and Standard Composition of UNS S32205 Element Fe C Cr Ni Mo N Mn Si Result of GDS (wt. %) 66.0 0.0136 22.2 6.27 3.07 0.0892 1.12 0.637 Table 3. Result of Tensile Test Properties Tensile stress (MPa) Modulus of elasticity (GPA) As received sample 489.66 220.63 Standard UNS S32205 620 200 UNS S32205 (wt. %) Balance 0.020 22.1 5.6 3.1 0.18 2.0 1.0

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A longitudinal section of the specimen was cut and mounted into a standard cylindrical mould by using Automatic Hydraulic Mounting Machine in order to carry out the grinding and polishing process. The sample was then ground to 4000 grit, and polished in accordance to the standard procedures. The polished samples were etched using Kallings No. 2 (5g copper chloride, 100ml hydrochloric acid, and 100ml ethanol) to reveal the microstructure of the duplex stainless steel for examination by optical microscopy. Immersion test A total immersion test was carried out to measure the corrosion performance of the specimens. All specimens were pre-stressed to the standard values and according to the test conditions. The microstructures of the stressed region of the specimens were analyzed by using an image analyzer. Any possible cracking that formed during the corrosion test was identified. Eighteen specimens were prepared according to ASTM G48 [13]: Standard Test Methods for Pitting and Crevice Corrosion Resistance of Stainless Steels and Related Alloys by use of ferric chloride and sodium chloride solutions. The immersion test was done under two different temperatures, 25oC and 50C for 72 and 144 hours. These temperatures were selected due to their common applications with duplex steels. Solutions with different percentages varying the chloride concentration and acidity (pH) of the solution were used. Table 4 shows the immersion test conditions, including test temperatures, the types of solutions, immersion durations, pH, and chloride concentrations of the solution. Table 4. Immersion Condition of Specimens Specimen T(C) Solution Period (Days) 6 6 6 6 6 6 3 3 3 3 3 3 6 6 6 6 6 6 Chloride concentratio n 1% 5% 10% 1% 5% 10% 1% 5% 10% 1% 5% 10% 1% 5% 10% 1% 5% 10% 5.95 5.13 5.07 3.43 3.29 3.15 5.95 5.13 5.07 3.43 3.29 3.15 5.95 5.13 5.07 3.43 3.29 3.15 pH Corrosion rate (mm/y) 0.3461 1.1458 1.3389 2.3848 3.5686 6.7230 0.2273 0.9402 1.1922 2.3371 3.4530 6.3182 0.0868 0.2181 0.3419 1.2552 1.6199 2.8866

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18

50 50 50 50 50 50 50 50 50 50 50 50 25 25 25 25 25 25

FeCl3 1% FeCl3 5% FeCl3 10% NaCl 1% + HCl 5% NaCl 5% + HCl 5% NaCl 10% + HCl 5% FeCl3 1% FeCl3 5% FeCl3 10% NaCl 1% + HCl 5% NaCl 5% + HCl 5% NaCl 10% + HCl 5% FeCl3 1% FeCl3 5% FeCl3 10% NaCl 1% + HCl 5% NaCl 5% + HCl 5% NaCl 10% + HCl 5%

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Metallographic examinations were used to confirm the presence of corrosion, and it is imperative to note that this usually occurs with no significant loss in mass of the test specimens, inasmuch as the duplex stainless steel has high resistance to general corrosion. Furthermore, quantitative pitting analysis was also performed using simple software. 5. RESULTS AND DISCUSSIONS Visual inspection and the corrosion rate Figure 2 shows the representative of the visual inspection. In general, ferrichloride produces general thinning and pitting while the combination of the sodium chloride and hydrochloride produces a fibrous-like, feathery appearance corrosion attack.

Figure 2. Appearance of representative samples after immersion

Graphical representation of the effect of the pH is shown in Figure 3. As the pH is decreasing (acidity increase), the corrosion rate is increasing. This is because low pH solutions accelerate corrosion by providing hydrogen ions. Hydrogen attacks and damages the surface of steel and increases the weight loss. The temperature plays an important role in accelerating the corrosion rate of metals. The higher the temperature is, the higher the corrosion rate is. The chloride concentration also increases the corrosion rate (Figure 4). The addition of chloride ions has a noticeable effect on the corrosion behavior of stainless steel in acidic solutions, since in the presence of this ion, a passivity breakdown process takes place above a certain potential that decreases with the chloride concentration. Chloride ions slowly penetrate into the surface, at which the protective film is destroyed and the steel begins to corrode. Chloride corrosion tends to evenly pit the entire surface area of the specimens with shallow, flat-bottomed, irregular shaped pits. Chloride penetration in metal is due to the presence of different mechanisms, mainly diffusion and capillary absorption. Temperature also influences the corrosion rate, as shown in Figure 5. This is due to temperature dependant on the chemical reactivity.

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Figure 3. Effect of the pH on the corrosion rate

Figure 4. Effect of the chloride concentration on the corrosion rate

Figure 5. Effect of the temperature on the corrosion rate

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Microstructure and pitting morphology Many pittings are visible using the naked eye (as indicated by the arrows in Figure 6), but using cross section and optical micrograph, the diameter and depth of the pits can be determined accurately. An example is shown in Figure 7, which shows the photomicrograph of a typical pitting on one of the specimens. Table 5 shows the average of the pitting depth. Clearly the effect of the pH and the chloride concentration is strong. The pitting density was also evaluated. To do so, a random (2 x 2) cm2 area was selected on each specimen, and the amounts of small, medium, and large pits in the area were counted. Table 6 shows the pitting density for representative specimens.

Figure 6. Surface appearance showing the pitting existence

Figure 7. Typical morphology of the pits

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Table 5. Pitting Depth Acidity pH 5.13 83.53 m Depth of pitting 94.51 m 98.17 m 15.64 m Average 72.96 m pH 5.07 238.8 m 221.2 m 148.2 m 136.5 m 186.18 m

Table 6. Pitting Density Average Per 4 cm2 Area Size of pitting Small Medium Large Total pH 5.13 19 9 1 29 pH 5.07 9 11 7 27

A specimen immersed in a solution with higher pH (low acidity) has more pits but shallower pitting. A specimen immersed in a solution with lower pH (high acidity) has fewer pits but with a greater depth. Although there are more pits on specimens with a higher pH, the greater depth of narrower pits makes it lose less weight than specimens exposed in lower pH. This explains why the corrosion rate of the specimen immersed in solution with lower pH is higher than the specimen immersed in solution with higher pH.

Area fraction analysis To determine which phase is mostly attacked by the pitting corrosion, the area fraction method is used. This method was applied to the photomicrograph of the specimens using Omninet . Figure 8 shows the photomicrograph of specimen 2 before and after using the software. The area fraction for austenite phase fell from 50.9% to 23.4%. This proves that the mixture of sodium chloride and hydrochloric acid creates a pitting corrosion attack mostly on the austenite phase. Similar area fraction reductions were also witnessed on samples tested with other solutions. The site of preferential pitting nucleation is confirmed by using this method. This can be explained by the fact that austenite with a crystal structure of face-centered cubic (FCC) has a solid solubility of carbon, while ferrite with a crystal structure of body-centered cubic (BCC) has much less solid solubility of carbon. Carbon is a weak element with very low corrosion resistance. The galvanic effect created by two cells of austenite and ferrite also synergizes phase dependency of the corrosion pitting nucleation.

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Figure 8. Area fraction analysis

Table 7. PREN for Each Phase Phase Austenite Ferrite % Cr 20.86 23.86 % Mo 2.43 3.51 %N 0.38 0.05 PREN 34.96 36.24

6. CONCLUSIONS The effect of pH and chloride concentration on corrosion behavior of duplex stainless steel, represented by UNS S32205, has been determined. Decreasing pH increases the corrosion rate. Similarly, increasing temperature increases corrosion rate. This can be achieved well using different solutions with different temperatures and periods of immersion, according to the ASTM G48 standard. Similarly, increasing chloride concentration increases corrosion rate. Pitting corrosion preferentially attacks the austenite phase. This can be quantified easily using simple metallography and software analysis, as well as PREN (Pitting Resistance Equivalent Number). The effect of pH and chloride concentration on the corrosion behavior of duplex stainless steel, represented by UNS S32205, has been determined. Decreasing pH (increasing acidity) increases the corrosion rate. This can be achieved well using different solutions with different temperatures and periods of immersion, according to the ASTM G48 standard. Similarly, increasing chloride concentration increases corrosion rate. Pitting corrosion preferentially attacks the austenite phase. This can be quantified easily using simple metallography and software analysis, as well as PREN (Pitting Resistance Equivalent Number). REFERENCES
[1] [2] J. Charles, Super Duplex Stainless Steels: Structure and Properties, Proceedings of the Conference of Duplex Stainless Steels 91. Les Editions de Physique, 1991, pp. 151168. C. M. Schillmoller, Practical Guidelines for the Fabrication of Duplex Stainless Steels. London: International Molybdenum Association, 2001.

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[3] [4] [5] [6] [7] [8] [9] Iris Alvarez-Armas, Duplex Stainless Steels: Brief History and Some Recent Alloys, Recent Patents on Mechanical Engineering, 1(2008), pp. 5157. R. N. Gunn, Duplex Stainless Steels: Microstructure, Properties and Applications. Cambridge, England:Abington Publishing, 1997. D. S. Bergstrom, J. J. Dunn, J. F. Grubb, and W. A. Pratt, US20036551420B1 (2003). Marcelo Martinsa and Luiz Carlos Casteletti, Microstructural Characteristics and Corrosion Behavior of a Super Duplex Stainless Steel Casting, Materials Characterization, 60(2009), pp. 150155. A. D. Mercer, Corrosion in Seawater Systems. New York: Ellis Horwood Publishing, 11990. J. Nowacki and A. Lukojc, Microstructural Transformations of Heat Affected Zones in Duplex Steel Welded Joints, Mater Charac, 56(45)( 2006), pp. 436441. A. Miyasaka, K. Denpo, and H. Ogawa, Prediction of Application Limits of Stainless Steels in Oilfield Equipment, Proceedings of Stainless Steels 91, The Iron and Steel Institute of Japan, Tokyo, Japan, 1(1991), p. 241. M. B. Rockel, Duplex Stainless Steels for the Chemical Petroleum and Process Industry. Texas: VDM Technologies Corporation, Texas, 1983. E. N. Simons and E. Gregory, Stainless and Heat-Resisting Steel. New York: Pergamon Press, `1986. ASTM Standard: G48 07, Standard Test Methods for Pitting and Crevice Corrosion Resistance of Stainless Steels and Related Alloys by Use of Ferric Chloride Solution, ASTM Annual Book of Standards, 0102(2007).

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