Acoustic emission monitoring of slow strain rate tensile tests of 304L stainless steel in supercritical water environment

An experimental set-up has been developed to perform slow strain rate tensile (SSRT) tests on tubular 304L stainless steel (SS) specimens in supercritical water (SCW) environment (550 °C, 250 bar). The supercritical water is circulated inside an internally pressurized tubular specimen mounted into a universal mechanical test rig and heated by a single loop resistance heating furnace. The set-up enables in situ monitoring of acoustic emission and electrochemical potential during the SSRT test. The SCW environment is found to significantly influence the mechanical performance of the material as a result of corrosion processes. A correlation between acoustic emission response and change of electrochemical potential is revealed. The findings are compared with preliminary results of tests performed on bulk SS specimens under the same condition in a commercial autoclave. The advantages and potentialities of both set-ups are discussed.     

Detection and characterization of stress-corrosion cracking on 304 stainless steel by electrochemical noise and acoustic emission techniques

This paper focuses on the corrosion process of 304 stainless steel in acidic NaCl solution during slow strain rate testing experiment by using electrochemical noise (EN) and acoustic emission (AE) techniques. Meanwhile, the EN and AE characteristics of corrosion process were studied. The results show that stress corrosion occurs easily in the experimental system, and corrosion forms develops gradually from localized corrosion including stress corrosion and pitting corrosion to general corrosion. The AE signal characteristics of pitting corrosion, crack and bubble break-up are significantly different during the corrosion process.     

Notched tensile tests of cold-rolled 304L stainless steel in 40 wt.% 80 °C MgCl2 solution

The effects of cold-rolling (20% thickness reduction) and sensitization treatment (600 °C/10 h) on the microstructure, tensile properties and susceptibility to stress corrosion cracking of 304 stainless steel in 80 °C MgCl₂ (40 wt.%) solution were investigated. The increase in hydrogen traps, which retarded hydrogen diffusion to the strained region, accounted for the low loss in notched tensile strength (NTS) of such a cold-rolled specimen, as compared to the solution-treated specimen in the corrosive environment. By contrast, the high NTS loss of sensitized specimens in MgCl₂ solution was attributed mainly to the formation of stress-induced martensite near grain boundary regions.     

Microstructural characteristics of the oxide scale formed on 304 stainless steel in oxygenated high temperature water

The microstructural characteristics of oxide scale formed on type 304 stainless steel in oxygenated high temperature water have been investigated. From outer to inner layer, the oxide scale consists of faceted spinel particles, irregularly shaped hematite particles and a compact layer of nano-sized spinels. Some outmost spinels formed on top of other particles are depleted in Cr, while the hematite particles tightly embedded into the inner layer contain more Cr in the inner than in the outer part. The inner nano-sized oxide grow inwards directly from the bottom of outer particles. The related oxidation mechanism is discussed.     

Electrochemical polishing as a 316L stainless steel surface treatment method: Towards the improvement of biocompatibility

A 316L stainless steel (316L-SS) surface was electrochemically polished (EP) in an electrolyte of a new chemical composition at different cell voltages, with the aim of improving its corrosion resistance and biocompatibility. X-ray photoelectron spectroscopy results revealed that the EP-formed oxide films were characterized by a significantly higher atomic Cr/Fe ratio and film thickness, in comparison to the naturally-grown passive oxide film formed on the untreated (control) 316L-SS surface. As a result of the increase in the oxide film thickness and relative Cr enrichment, the EP-treated 316L-SS surfaces offered a notable improvement in general corrosion resistance and pitting potential. In addition, the attachment of endothelial cells (ECs) and smooth muscle cells (SMCs) to the 316L-SS surfaces revealed a positive effect of electropolishing on the preferential attachment of ECs, thus indicating that the EP surfaces could be endothelialized faster than the control (unmodified) 316L-SS surface. Furthermore, the EP surfaces showed a much lower degree of thrombogenicity in experiments with the platelet-rich plasma. Therefore, the use of the electrochemical polishing technique in treating a 316L-SS surface, under the conditions presented in this paper, indicates a significant improvement in the surface’s performance as an implant material.     

A comparative H2S corrosion study of 304L and 316L stainless steels in acidic media

H₂S corrosion of 304L and 316L in oxygen-free Na₂SO₄ + Na₂S solution at pH 3 and temperature of 60 °C were investigated by EIS, potentiodynamic polarisation, multi-component Pourbaix diagrams and microstructure characterization. At similar conditions, lower corrosion rate was observed on 316L, attributed to its denser (1.5 times) and smoother (6%) surface layer and confirmed by SEM micrograph. During polarisation, H₂S increases significantly the critical current density on 304L and passivation current density, i_p, on 316L. Higher i_p on 316L was associated to simultaneous FeS₂–MoS₂ preservation, confirmed by XRD examination. H₂S could have an inhibiting effect on 304L in passivity region.     

Study of localized corrosion of 304 stainless steel under chloride solution droplets using the wire beam electrode

Localized corrosion of 304 stainless steel under droplets of 1 M sodium chloride solution was investigated by the wire beam electrode (WBE) method. It was found that the current distributions were heterogeneous with isolated anodic current peaks mostly located near the edge of the droplet. During the corrosion process, the stainless steel WBE exhibited the stochastic characteristics with the disappearance of some anodic sites. In addition, stainless steel suffered more serious localized corrosion with the increase of the droplet size. The increase of the cathodic area and the three-phase boundary (TPB) length was believed to be the reason.     

Soft X-ray absorption spectroscopy study of the effects of Si, Ce, and Mo ion implantation on the passive layer of AISI 304 stainless steel

The chemical modifications introduced in the passive layer of AISI 304 stainless steel after Si, Ce, and Mo ion implantation were investigated and compared with non-implanted steel by soft X-ray absorption spectroscopy. The influence of ion implantation on the passive properties was evaluated by measuring soft X-ray absorption spectra at the Cr, Fe, Ni, Mn and Si 2p in addition to oxygen 1s thresholds. All ion implanted samples show a relative Cr-enrichment at the surface as compared with non-implanted samples. Fe 2p as well as O 1s spectral changes reveal chemical differences in the passive layer as a function of the element ion-implanted.     

Investigation of intergranular corrosion of 316L stainless steel diffusion bonded joint by electrochemical potentiokinetic reactivation

Electrochemical potentiokinetic reactivation technique (EPR) was employed to assess degree of sensitization in 316L stainless steel diffusion bonded joint (DBJ). The result showed the degree of sensitization of DBJ was much smaller than that of base material (BM). No chromium carbides precipitated at grain boundaries in DBJ after 100 h treatment at 650 °C, while chromium carbides could be seen clearly in the BM after 8 h treatment, indicating that DBJ has better intergranular corrosion resistance than BM. Diffusion bonding technique will not increase intergranular corrosion susceptibility of 316L DBJ. Reactivation potential has the biggest effect on sensitization.     

Stress corrosion cracking detection using non-contact ultrasonic techniques

In this work a method is presented for detecting and locating stress corrosion cracking (SCC) in stainless steel pipe samples. The method combines laser generation and either laser or electromagnetic acoustic transducer (EMAT) detection, scanning the generation point across the sample surface. Using laser-generated ultrasonic waves that interact with the cracks, and performing time–frequency analysis techniques to examine changes in the generated wavemodes, surface plots that clearly resolve the spatial extent and geometric alignment of the cracks are created and presented here. The method is demonstrated using components removed from service after exhibiting SCC.     

Monte Carlo simulation of stress corrosion cracking on a smooth surface of sensitized stainless steel type 304

Stress corrosion cracking (SCC) on a smooth surface of structural metal materials occurs by initiation and coalescence of micro cracks, subcritical crack propagation and multiple large crack formation or final failure under combination of material, stress and corrosive environment. In this paper, a Monte Carlo simulation of the SCC process is proposed based on stochastic properties for micro crack initiation and concepts in fracture mechanics for crack coalescence and propagation. The procedure is as follows: The possible number of grain-sized micro cracks which can be initiated is set for a given space and initiation times for all cracks are assigned by random numbers based on exponential distribution. Sites and sizes of cracks are assigned by uniform random numbers and normal random numbers, respectively. Coalescence and propagation of cracks are determined based on fracture mechanics. The emphasis in the model is put on the influence of semi-elliptical surface cracks. Numerical simulations are carried out based on the results of creviced-bent-beam tests for sensitized stainless steel type 304 under high-temperature and high-purity water containing dissolved oxygen and the influence of micro crack initiation rate and coalescence condition on the simulation results is discussed.     

Surface chemistry and corrosion behaviour of 304 stainless steel in simulated seawater containing inorganic sulphide and sulphate-reducing bacteria

Although many studies have been carried out regarding the role of sulphide anions in promoting microbial corrosion of various metal substrates, very little is known about the differences between inorganic sulphide and biogenically-derived sulphide by sulphate-reducing bacteria (SRB) and what the reasons for differing corrosion behaviour between the two types of sulphide may be towards common metals. In this study, various electrochemical and surface analytical techniques were employed to study the effect of the inorganic and biogenic sulphide (active SRB present) on the surface chemistry and corrosion behaviour of 304 stainless steels in a simulated seawater-based modified Baar’s (SSMB) medium. Clear differences in the surface chemistry of the sulphurised passive film by inorganic and biogenic sulphide (active SRB present) were quantified by X-ray photoelectron spectroscopy (XPS). The transformation of metal sulphides in abiotic and biotic sulphide solutions with the exposure time was correlated with different corrosion behaviour of 304 stainless steels.     

Determination of the sensitized zone extension in welded AISI 304 stainless steel using non-destructive electrochemical techniques

Extension of sensitized zone (SZ) in welded AISI 304 stainless steel was determined by two non-destructive electrochemical tests: double loop electrochemical potentiokinetic reactivation technique (DLEPR) and local electrochemical impedance spectroscopy (LEIS). Welding was carried out using the shielded metal arc with two selected welding energies: the first one (0.7 kJ mm⁻¹) does not promote the sensitization of the 304 steel and it constitutes the reference sample and the second one (2.2 kJ mm⁻¹) which leads to the precipitation of chromium carbides in the grain boundaries after the welding process. The non-destructive DLEPR and LEIS tests allowed the length of the SZ to be determined and a good agreement between the two techniques and the microstructure of the two welded samples was shown. The presence of an inductive loop on the local impedance diagrams seems to reflect a galvanic coupling between the weld string (anode) and the welded stainless steel plates (cathode) which will be very prejudicial to a good corrosion resistance of the welded system. The results showed that the two electrochemical tests could be applied in practical cases in industrial field.     

Electrochemical characteristics of zirconium oxide treated Type 304 stainless steels of different surface oxide structures in high temperature water

Electrochemical polarization analyses were conducted to investigate the impact of different oxide structures on corrosion resistance of ZrO₂-treated Type 304 stainless steel specimens in high temperature water. All specimens were pre-oxidized in high temperature water containing either 300 ppb dissolved oxygen or 50 ppb dissolved hydrogen, followed by a hydrothermal deposition treatment with ZrO₂ nanoparticles. Experimental results revealed that the corrosion potentials and corrosion current densities on the ZrO₂-treated specimens were lower than those on the untreated ones, and the decreases in these parameters were more distinct on the ZrO₂-treated specimens with oxides developed under dissolved oxygen condition.     

Sensitivity of stress corrosion cracking of stainless steel to surface machining and grinding procedure

An investigation has been undertaken to establish the effect of surface preparation method on the susceptibility of a 304 stainless steel to stress corrosion cracking under simulated atmospheric corrosion conditions. MgCl₂ was deposited onto four-point bend specimens, which were then placed in a chamber with a relative humidity of 45% and temperature of 60 °C. These test conditions were designed to reflect external exposure of stainless steel components in industrial plant, including nuclear reactor components, situated in a coastal region, but with the severity of the exposure conditions enhanced to allow discrimination of the effect of surface preparation in a short timescale (up to 1500 h). Four surface preparation methods were evaluated: transverse grinding, longitudinal grinding, transverse dressing using an abrasive flap wheel, and transverse milling. For each case, surface topography, surface defect mapping, near-surface microhardness mapping, residual stress and electron back-scattered diffraction measurements were undertaken. Stress corrosion cracks were observed for the ground and milled specimens but not for the dressed specimens, with cracks apparently originating at corrosion pits. The density of cracks increased in the order: transverse ground, milled and longitudinal ground, with the cracks notably much smaller in length for the transverse ground condition. The propensity for cracking could be linked to the high residual stress and apparent nanocrystalline microstructure at the surface. There was a greater propensity for pitting to initiate at local defect sites on the surface (laps, deeper grooves). However, the tendency was not overwhelming, suggesting that other factors such as more general roughness or the distribution of MnS inclusions had an influence, perhaps reflecting the severity of the environment.     

AE response of type 304 stainless steel during stress corrosion crack propagation

Acoustic emission (AE) signals generated by transgranular stress corrosion cracking (TGSCC) and intergranular stress corrosion cracking (IGSCC) have been compared by means of slow strain rate tensile tests (SSRT) performed using both solubilised and sensitised type AISI 304 stainless steel in a 1 M NaCl + 1 M HCl solution. Results show that the AE activity during the propagation of TGSCC is much higher than the AE activity during the IGSCC propagation. However, no significant difference was found between the mean amplitude and rise-time of the AE signals registered during the propagation of TGSCC and those measured for IGSCC propagation.     

Corrosion resistance of welds in type 304L stainless steel made with a nickel-copper-ruthenium welding consumable

Ni-Cu-Pd welding consumables have been recently developed for 300-series austenitic stainless steels such as Type 304L (SS304L) to reduce the amount of Cr(VI) in the welding fumes. In this study, a modified filler metal that replaces Pd with Ru was evaluated. Initial tests conducted on button-melted samples and bead-on-plate welds indicated that Ni-Cu-Ru exhibited good corrosion properties. Actual Ni-Cu-Ru arc welds made on SS304L were successfully produced and the corrosion performance was comparable to or better than that of Ni-Cu-Pd welds. These welds are a suitable replacement for welds made with standard 300-series welding consumables, such as SS308L.     

Simulation analysis of electrochemical nature of real passive films with artificial passivation films

Simulation experiments using oxide thin films with analogues composition and thickness of passive films on Fe-Cr alloys have been performed to reveal the function of alloying elements in passive films. The objective of the present paper is to review recent results of the simulation experiments using Fe₂O₃-Cr₂O₃ films. The thinning rate of the films was measured as a function of potential in 1 M HCl by in-situ ellipsometry. The potential-dependent change of the rate well simulated the potential-dependent dissolution behavior of Fe-Cr alloys. The composition of the films having resistance against given environment was obtained by the simulation experiments.     

The semiconducting properties of passive films formed on AISI 316 L and AISI 321 stainless steels: A test of the point defect model (PDM)

The semiconductor properties of passive films formed on AISI 316L in 1 M H₂SO₄ in three temperatures and AISI 321 in 0.5 M H₂SO₄ were studied by employing Mott–Schottky analysis in conjunction with the point defect model (PDM). Based on the Mott–Schottky analysis in conjunction with PDM, it was shown that the calculated donor density decreases exponentially with increasing passive film formation potential. Also, the results indicated that donor densities increased with temperature. By assuming that the donors are oxygen ion vacancies and/or cation interstitials, the diffusion coefficients of the donors for two stainless steels are calculated.