Effects of Temperature and Pressure on Stress Corrosion

CHINESE JOURNAL OF MECHANICAL ENGINEERING Vol. 30,aNo. 1,a2017

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DOI: 10.3901/CJME.2016.0420.056, available online at www.springerlink.com; www.cjmenet.com

Effects of Temperature and Pressure on Stress Corrosion Cracking Behavior of 310S Stainless Steel in Chloride Solution

ZHONG Yunpan1, ZHOU Cheng2, CHEN Songying1, *, and WANG Ruiyan1

1 Key Laboratory of High-efficiency and Clean Mechanical Manufacture, Shandong University, Jinan 250061, China 2 Qingdao Boiler and Pressure Vessel Supervisory Institute, Qingdao 266071, China

Received October 21, 2015; revised March 11, 2016; accepted April 20, 2016

Abstract: 310S is an austenitic stainless steel for high temperature applications, having strong resistance of oxidation, hydrogen

embrittlement and corrosion. Stress corrosion cracking(SCC) is the main corrosion failure mode for 310S stainless steel. Past researched

about SCC of 310S primarily focus on the corrosion mechanism and influence of temperature and corrosive media, but few studies

concern the combined influence of temperature, pressure and chloride. For a better understanding of temperature and pressure’s effects

on SCC of 310S stainless steel, prepared samples are investigated via slow strain rate tensile test(SSRT) in different temperature and

pressure in NACE A solution. The result shows that the SCC sensibility indexes of 310S stainless steel increase with the rise of

temperature and reach maximum at 10MPa and 160℃, increasing by 22.3% compared with that at 10 MPa and 80 ℃. Instead, the

sensibility decreases with the pressure up. Besides, the fractures begin to transform from the ductile fracture to the brittle fracture with

the increase of temperature. 310S stainless steel has an obvious tendency of stress corrosion at 10MPa and 160℃ and the fracture

surface exists cleavage steps, river patterns and some local secondary cracks, having obvious brittle fracture characteristics. The SCC

cracks initiate from inclusions and tiny pits in the matrix and propagate into the matrix along the cross section gradually until rupture. In

particular, the oxygen and chloride play an important role on the SCC of 310S stainless steel in NACE A solution. The chloride damages

passivating film, causing pitting corrosion, concentrating in the cracks and accelerated SSC ultimately. The research reveals the

combined influence of temperature, pressure and chloride on the SCC of 310S, which can be a guide to the application of 310S stainless

steel in super-heater tube.

Keywords: 310S stainless steel, SSRT, stress corrosion, chloride, temperature

1 Introduction

Austenitic stainless steels, which possess high corrosion resistance and good mechanical properties, are widely used in piping systems in the petrochemical industry and nuclear power plants[1]. 310S is an austenitic stainless steel for high temperature applications(about 800℃), especially in oil, gas and petrochemical industries containing hot concentrated acids. Due to the high levels of nickel and chromium in the chemical compositions, 310S is extremely resistant to oxidation, hydrogen embrittlement(HE) and corrosion[2–4]. SCC is a common corrosion mechanism for austenitic stainless steel, which also is the main corrosion failure mode for 310S stainless steel. Even if damage of SCC has been observed over more than a century, SCC mechanisms are still under debate. The two most classical categories of mechanisms are anodic dissolution and

* Corresponding author. E-mail: [email protected] Supported by National Basic Research Program of China(973 Program,

Grant No. 2011CB013401), and General Administration of Quality Supervision, Inspection and Quarantine of China(Grant No.2011QK235)

© Chinese Mechanical Engineering Society and Springer-Verlag Berlin Heidelberg 2017

hydrogen induced cracking[5]. Due to the deficiencies and limitations of above mechanisms, several new mechanisms have been proposed during the past few decades, such as slip dissolution model, tunnel corrosion model and hydrogen induced plasticity theory[6–7].

Many researches on the corrosion of 310S stainless steel have been done so far. BEHNAMIAN, et al, researched the stress corrosion cracking behavior of austenitic alloys in pure supercritical water. The result showed that crack initiations were readily observed in all samples, signifying susceptibility to stress corrosion cracking. The microcracks in 316L stainless steel and Inconel 625 were almost intergranular, whereas transgranular microcrack initiation was observed in 310S stainless steel[8]. The transgranular cracking mode was also found in all sensitized type 310 specimens in boiling saturated magnesium chloride(MgCl2) in ALYOUSIF and NISHIMURA’s research[9]. WANG Wenwen’s works shows the crack initiates in the corrosion product film(CPF) of 310S specimen and the existence of the CPF-induced stress yields first the specimen and facilitates SCC[10]. UCHIDA, et al, found the susceptibility to SCC of 310S stainless steel under constant load conditions increased in the order of [111], [101] and [001]

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tensile axis and the normal stress to the [100] crack plane strongly controlled the SCC growth[11].

Some research shows hydrogen and temperature are the important influential factors for SCC of 310S stainless steel. LU, et al, found that hydrogen dissolved into austenitic stainless steels promotes the initiation and propagation of stress corrosion cracking in 42% MgCl2 boiling solution. The hydrogen-promoted SCC was likely to be a result of the degradation of passive film induced by hydrogen[12]. And WANG, et al, compared the plasticity loss induced by hydrogen entering into the samples with that induced by the anodic dissolution process, finding hydrogen played a negligible role in SCC of 310S stainless steel in a boiling MgCl2 solution[13]. LIM, et al, showed that temperature and pressure had profound effect on the corrosion behavior of 310S stainless steels in a Li/Na carbonate melt in a cathode gas atmosphere[14]. Similarly, FRANGINI, et al, also reported temperature significantly affected the corrosion behavior of type 310S stainless steel in the eutectic Li + K carbonate melt[15].

Chloride irons are the most common agent for stress corrosion cracking of austenitic stainless steels. Numerous studies have shown that austenitic stainless steel in Cl- solution are more susceptible to SCC. For instance, PARDAL, et al, found the high Cl- in seawater leading the stress corrosion of the inert gas generator mirror plate made of AISI 310S stainless steel by the failure analysis[16]. And LU Guocheng, et al, reported that the extremely low chloride concentration also could induce SCC for Type 304

austenitic stainless steel because of the chloride anion enrichment in the occluded cell[17].

The 310S stainless steel is widely used for super-heater tube in utility boiler due to its good heat resistance and corrosion resistance. Up to now, the pressure of the utility boiler has reached the high pressure (9.8MPa), ultrahigh pressure(13.7MPa) and even subcritical pressure (16.2 MPa). In this article, the 310S stainless steel specimen would be analyzed with SSRT under the simulated operating condition of super-heater in utility boiler, aiming to know the effect of temperature, pressure and chloride irons on the SCC for 310S stainless steel.

2 Experimental Test

2.1 Material and Test Specimen Material used in this experiment is Type 310S stainless

steel whose chemical composition is listed in Table 1. The specimens were processed into tensile rod samples in round sharp. Design of the rod samples fulfils the requirements described in ASTM E8, and the physical dimensions of these samples are shown in Fig. 1. The gage length of each sample was machined down to 25 mm in length and approximately 5mm in diameter. Before the test, the surfaces of the specimen were subsequently abraded with silicon carbide(SiC) papers of 400, 800 and 1200 grit, cleaned in an ultrasonic bath with acetone for 2-4 min, rinsed in ethanol and dried with an electric drier[18].

Table 1. Chemical composition of Type 310S stainless steel in mass fraction

C Mn Si P S Cr Ni N V Fe

0.054 1.766 0.605 0.016 0.001 5 24.65 19.41 0.002 8 0.181 Bal.

Fig. 1. Dimensions of the rod sample used in SSRT

2.2 Test Environment and Apparatus

The test solution is solution A of NACE standard TM-0177, containing 0.5% NaCl and 0.05% CH3COOH, prepared by using deionized water. To know the effects of temperature and pressure on SCC of 310S austenitic stainless steel, specimens are put into the same solution at different temperature and pressure. The different test environments are detailed in Table 2. The test apparatus is slow strain rate test system(SERT-5000- D9H, Toshin Co. Ltd.), consisting of a draw mechanism, a corrosion cell, a computer-control system and a gas compressor.

2.3 Test Procedure

Before the tensile specimens were placed into the cell, enough test solution was poured into the cell so that the test section of specimens could be immersed by the solution. The specimen was pre-drawn two or three time firstly, and then pulled at a constant extension rate of 2×10–6 m/s until the sample was ruptured. After the test, the fracture was cleaned with ultrasonic, and the fracture morphologies were observed using a scanning electron microscope (SEM), and the chemical compositions of the fracture were analyzed by an energy disperse spectroscopy (EDS).

3 Results and Discussion

3.1 Evaluation methods of stress corrosion sensitivity The stress corrosion sensitivity was measured by the

stress corrosion sensibility index which was obtained through the comparison of characteristic parameters in inert medium and corrosive medium. The formula is shown as follows:

ZHONG Yunpan, et al: Effects of Temperature and Pressure on Stress Corrosion Cracking Behavior of 310S Stainless Steel in Chloride Solution

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NTP corSCC

NTP

100%.I I

II

-= ´ (1)

Where INTP is the test parameters in the N2(such as tensile strength Rm, elongation rate φ, inner product power P). Icor is the test parameters in corrosive medium.

Generally, when ISCC < 25%, it shows that the samples have no obvious stress corrosion. When 25% ≤ ISCC ≤ 35%, it shows the samples have a tendency of stress corrosion. When ISCC > 35%, it shows the samples have no obvious stress corrosion[19].

3.2 SSRT results

The stress/strain curves obtained from slow strain rate tests performed for samples in different environments are shown in Fig. 2. SSRT test results of these samples are summarized in Table 2. As it is shown in Fig. 2, all the tensile curves show the trend of dynamic strain aging(DSG) and get more notable with temperature up. Theories of KATAD[20] and ASKINSON[21], et al, suggested that DSG will promote environmentally assisted cracking(EAC), which causes the markedly reduced of metal material. The tensile strength of samples decrease with the increase of temperature and decrease more at 10 MPa than that at 16 MPa. When the test temperature is 160℃ and the pressure is 10MPa, tensile strength of samples is smallest which decrease by 10.21%. Similarly, the elongation rate and inner product power also decrease more at 10 MPa than that at 16 MPa, showing 310S stainless steel is more likely to have stress corrosion at 10 MPa. Especially when the test temperature is 160℃ and the pressure is 10 MPa, the sensibility indexes of tensile strength, elongation and inner product power exhibit the biggest values. As it shown in Table 2, the sensibility index of the inner product power is ISCC=27.4% > 25% at 10MPa and 160℃, which shows that 310S stainless steel has an obvious tendency of SCC in this environment.

Curves in Fig. 3 show that tensile strength decreases and the SCC sensitivity increases with temperature up. High temperature enhances convection and the diffusibility of caustic ion in the solution and also enhances the propagation rate of the crack. The result in Table 2 shows that the SCC susceptibility is higher in 10 MPa than in 16 MPa in the same temperature.

Fig. 2. Curves of slow strain test for 310S stainless steel.

Fig. 3. Influence of temperature on the stress

corrosion sensitivity

Table 2. Sensitivity indexes of 310S stainless steel obtained from slow strain rate test

Type Environment Tensile strength

Rm/MPa Elongation rate

φ/% Inner product

power P

Sensitivity index ISCC /%

Rm φ P

310S NTP(N2) 625.13 55.46 30 149.2 — — —

310S 10 MPa 80 ℃ 572.69 47.44 23 393.6 8.39 14.46 22.40

310S 10 MPa 120 ℃ 562.47 50.71 23 703.4 10.02 8.56 21.38

310S 10 MPa 160 ℃ 561.30 47.14 21 887.7 10.21 15.00 27.40

310S 16 MPa 80 ℃ 584.21 51.62 25 904.7 6.55 6.92 14.08

310S 16 MPa 120 ℃ 579.42 51.99 25 516.5 7.31 6.27 15.37

310S 16 MPa 160 ℃ 570.91 50.25 23 764.4 8.67 9.39 21.18


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3.3 Fracture surface appearance

The sample fracture positions of 310S stainless steel is located about in the middle of the samples. The overall fracture surfaces are analyzed by SEM, shown in Fig. 4. The fracture surface shows a very obvious necking phenomena at low temperature and it has no obvious change with the pressure increasing. When the temperature rises to 160℃, the fracture surface has no obvious necking phenomena. The fracture is typical ductile fracture at NTP and 80℃ and all the shear lip region, shear fracture region and ductile fracture region could be seen obviously. The samples show mixed mode with a few brittle features in edge region and ductile features in the center at 120℃, and the region of brittle features increase when the temperature rises to 160℃. Generally, the deeper and bigger the dimple is, the better the ductility is and the longer the duration is[22]. As seen from the Fig. 5, the dimples get much shallower and smaller with increasing temperature at 10 MPa, indicating that 310S stainless steel begins to transform from the ductile fracture to the brittle fracture.

Fig. 4. Overall fracture surfaces of 310S stainless steel samples

in different environment.

Fig. 6 shows the profile surface of samples in different environment. It can be seen that there are many cracks and tiny pits on the profile surface. Tiny cracks initiate from the bottom of pitting holes and grow into big transverse cracks under the tensile stresses. The scanning electron micrographs for the fracture surface appearance of 310S stainless steels tested in NACE A solutions are investigated,

as shown in Fig. 7. It shows that the fracture surface of samples in high temperature environment is relatively smooth and flat. There are some small cleavage planes near the shallow dimple region on the fracture surface and the intersection of these cleavage planes forms cleavage steps and river patterns, as show in Fig.7(a). In addition, some local secondary cracks are found running across the fracture surface showed in Fig.7(b), which indicates that 310 S strain steel has a strong tendency of SCC at 160℃. Fig.7(c) shows that the SCC cracks initiate from inclusions and tiny pits in the matrix and propagate into the matrix along the cross section gradually until rupture. The mismatches exist between the inclusions and matrix which provide favorable conditions for the initiation of pits. The big pits would be formed after the separation of inclusions and matrix under the continue effect of tensile stress. Stress concentration will be easily formed at the edge of pits that causes the initiation of cracks finally[23].

Fig. 5. Dimples on the fracture surfaces in different temperature at 10 MPa

Fig. 6. Magnification images for profile surface of samples.

3.4 Major chemical composition analysis

As shown in Fig. 8, energy spectrum analysis of fractures is done in edge region, in the center and in the crack respectively. No enrichment phenomenon is observed about Mn, Si, Fe and Ni. But the distributions of Cl- and oxygen are strongly heterogeneous. The content of Cl- in edge region is 5.49%, three times more than that in the center of fracture surface, as seen from in Table 3. This result


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indicates that Cl- penetrates into stainless steel from the profile surface at the beginning. Chloride ions attach to the passivation film, squeezing out oxygen atoms, combining with metal cation into soluble chloride, as a result, cause the appearance of pitting holes. In addition, Chloride ions go into the deeper with the propagation of cracks. The content of Cl- in the crack is 21.79%, far greater than that in

other position, showing there is an enrichment phenomenon of Cl- in the crack. High content chloride ions in the crack combine into metal chloride which cause hydrolysis making the local solution acidulated and accelerated stress corrosion cracking finally. Consequently, chloride ions have a big impact on stress corrosion, or it is to blame for the stress corrosion of 310S stainless steel in NACE A solution.

Fig. 7. Magnification images for fracture surface of samples in high temperature environment. The oxygen content is diverse in different region on the

fracture. The oxygen content in the brittle fracture zone is 14.3%, which is three times than that in dimples region in the center of fracture surface, as shown in Fig. 8 and Table 3. Fig. 8(c) shows many small cubical and spherical oxide particles distribute in the dimples region at the size of 400-900nm. A thick metal oxide film is attached to the fracture surface of samples after the tensile test in the oxygen and chloride media. The crystal structure of metal oxides in the oxide film is different from austenite stainless steel substrate which is face-centered cubic and an interface existed between the oxide film and substrate[24]. The out-migration metal cation leaves lots of vacancies on the surface of alloy substrate during the growth of oxide film and makes the substrate tend to shrink. An additive stress is induced between the oxide film and the substrate when the

oxide film hinders its shrinkage[25]. The oxygen and chloride change the structure of oxide film, enhancing the thickness of oxide film and also increase the additive stress. The additive stress would always exist and keep high value in the whole process of tensile stress corrosion. The total stress reaches the critical value with the superposition of external stress force and additives stress and causes the movement and multiplication of dislocations[26]. When the local plastic deformation promoted by corrosion reaches the critical condition, local stress concentration would break the atomic bond and causes nucleation of stress corrosion cracks. The media prevents the cracks to interfere with passivation to blunt into a void and makes the substrate appear cleavage fracture. In this process, the theory of positive dissolving can be a reasonable explanation for stress corrosion crack of 310S stainless steel[27].

Fig. 8. Energy spectrum analysis of fractures in different position

Table 3. Content of atoms of corrosion product in different position in mass fraction

Position C O Na Si Cl Cr Mn Fe Ni

a 3.86 14.30 8.69 0.84 12.86 16.57 0.51 32.67 9.67 b 4.23 6.67 6.65 1.06 5.03 21.94 1.27 42.63 10.45 c 4.59 4.25 3.22 0.63 3.59 23.08 1.37 41.42 17.78 d 4.18 2.36 33.7 — 25.69 11.56 0.23 15.74 6.48

3.5 Discussion

The previous analysis shows that the failure mode of samples is predominantly brittle fracture with a little ductile feature in some region. The brittle fracture region increases


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and cleavage planes appear on the fracture surface with temperature up. When temperature goes up, the ion product of water increases and high temperature also increases the activity of Cl- and H+ in solution, which make Cl- easier to penetrate the passivation membrane and accelerates the diffusion rate of H+ into metal[28]. The higher temperature widens the susceptibility zone to SCC and causes the susceptibility zone shift negatively, which makes it more susceptible to SCC[29]. The passivation potential of SCC decreases with the temperature up and makes it difficult for the repassivation of samples that has already been pitted by stress corrosion cracking[30]. Besides, in high temperature environment the passivation membrane in metal surface becomes thicker but worse protection than in room temperature. The passivation membrane is more vulnerable to rupture under the action of tensile stress and causes the appearance of pits[31].

Stress corrosion cracking is a complex process and tensile stress and corrosion medium are two requirements. In the corrosive environment, Cl- destroys the passive film on the surface of simples constantly and makes the metal surface contact with solution. The reaction in the weakly acidic NACE solution is showed as follows:

22Fe O 2FeO+ , (2)

22FeO 2H Fe H O+ ++ + . (3)

When the metal on the surface dissolves, the metal

surface forms corrosion pitting and the crack tips appear with the action of stress concentration around the pits. The following equation is the reaction of Fe2+ in the crack tips:

22 2Fe 2H O Fe(OH 2H .+ ++ +） (4)

The regional pH in the crack tips decreases as the

reaction progress. Following reaction occurs when the concentration of H+ increases to some extent:

2H 2e 2H+ + , (5)

2H H H+ . (6) Fe(OH)2 will make a further reaction with O2 in the

oxygenated NACE solution as follows:

2 2 2 34Fe(OH) O 2H O 4Fe(OH+ + ） , (7)

3 2 3 22Fe(OH) Fe O • 3H O . (8) The Fe2O3·3H2O embeds in the cracks and generates

lateral tensile stress as the volume of Fe2O3·3H2O is greater than the dissolved Fe. The tensile stress results in the propagation of crack and the stress corrosion extent promotes furthermore. The above chemical reactions are slow in room temperature and therefore samples have no obvious tendency of SCC. When the temperature increases,

the destruction of passive film is promoted and the chemical reactions are more severe, resulting in an obvious phenomenon of SCC[32].

The dissolved oxygen concentration is proportional to the oxygen gas partial pressure. In normal temperature and pressure, the dissolved oxygen concentration in distilled water is 9.17 mg/L. To expel air in the corrosion cell, the nitrogen is forced into the cell before the test and the test pressure is also controlled by passing over the nitrogen gas with compressor. Eq. (2) shows that when the oxygen pressure is greater than the decomposition pressure of FeO, the Fe will be oxidized, otherwise, the FeO decomposes. So when the test pressure increases, the oxygen gas partial pressure remains constant, but the dissolved oxygen pressure increases, which accelerates the oxidation of Fe and the formation of oxide films[33]. The rapid formation of oxide films inhibits the corrosion of matrix, which explains why the SCC susceptibility is higher in 10MPa than in 16MPa in the same temperature.

4 Conclusions

(1) With the rise of temperature, the sensibility index of tensile strength, elongation and inner product power increases and reaches the biggest values at 10 MPa and 160℃, increasing by 22.3% compared with that at 10MPa and 80℃. Conversely, the SCC susceptibility of samples is higher in 10MPa than in 16 MPa.

(2) The fracture is ductile fracture at NTP and 80℃ and shows mixed mode with a few brittle features in edge region and ductile features at 120℃ and 160℃. 310S stainless steel begins to transform from the ductile fracture to the brittle fracture with the increase of temperature.

(3) 310S stainless steel has an obvious tendency of stress corrosion at 10 MPa and 160℃and the fracture surface exists cleavage steps, river patterns and some local secondary cracks, having obvious brittle fracture characteristics. The SCC cracks initiate from inclusions and tiny pits in the matrix and propagate into the matrix along the cross section gradually until rupture.

(4) The oxygen and chloride play an important role on the SCC of 310S stainless steel in NACE solution. There is an enrichment phenomenon of Cl- in the cracks. Cl- penetrates into stainless steel through the pitting holes on the profile surface at the beginning and goes into deeper with the propagation of cracks. References

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Biographical notes ZHONG Yunpan, born in 1991, is currently a master candidate at School of Mechanical Engineering, Shandong University, China. He received his bachelor degree from Shandong University, China, in 2013. His main research interests include stress corrosion of austenitic stainless steel and martensitic stainless steel. Tel: +86-15665737556; E-mail: [email protected] ZHOU Cheng, born in 1972, is the director of Qingdao Boiler and Pressure Vessel Supervisory Institute, a part-time graduate tutor of Shandong University, China, he dedicates in metal corrosion and pressure vessel safety research. Email: [email protected] CHEN Songying, born in 1966, is currently a professor and a PhD candidate supervisor at School of Mechanical Engineering, Shandong University, China. His main research interests include stress corrosion of strainless steel, fluid machinery and fluid mechanics. Tel: +86-13906416257; E-mail: [email protected] WANG Ruiyan, born in 1990, is currently a master candidate at School of Mechanical Engineering, Shandong University, China. E-mail: [email protected]

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Effects of Temperature and Pressure on Stress Corrosion