Double Loop Electrochemical Potentiokinetic Reactivation Research Articles

Influence of ageing treatment time on microstructural evolution, sensitization and self-healing of Inconel 600

Samples of Inconel 600 were thermally aged at 739 °C from 1 up to 300 h followed by water quenching. The changes in microstructure were characterized and its effect on sensitization was evaluated by subjecting the heat-treated samples to double-loop electrochemical potentiokinetic reactivation (DL-EPR) tests. The evolution of the microstructure was analysed in terms of grain size, carbide formation and chromium diffusion by optical and scanning electron microscopy. The results showed that the formation of chromium carbides is rapid at this temperature, increasing the density of carbides at the grain boundaries in the early stages of the ageing treatment. The formation of Cr7C3 and Cr23C6 along the grain boundaries and within the austenitic matrix modified the corrosion behaviour as seen in the measurements of the degree of sensitization (DOS). A decrement in DOS was seen with ageing time up to 200 h, due to the redistribution of chromium, induced by the equilibrium between chromium at grain boundaries and within the matrix. Electron backscattering diffraction suggested that self-healing of the alloy may be due to the mechanism of near-boundary gradient zones, where the increased number of dislocations leads to precipitation of carbides by promoting diffusion and thereby decreasing the Cr-depleted zones.

Intergranular Corrosion Analysis of Austenitic Stainless Steels in Molten Nitrate Salt Using Electrochemical Characterization

This study investigates the influence of molten nitrate salt exposure on the intergranular corrosion (IGC) behavior of three grades of austenitic stainless steel (namely, AISI 304, AISI 304H, and AISI 321H). Two electrochemical techniques, double loop electrochemical potentiokinetic reactivation and potentiodynamic polarization methods, are applied after stainless steel is exposed to 600 °C molten nitrate salt, 60% NaNO3, and 40% KNO3 for varying immersion durations. Corrosion morphology is examined using optical microscopy and scanning electron microscopy images to assess susceptibility to IGC. IGC is prompted by the presence of chromium carbides at grain boundaries, which leads to chromium depletion around these carbides. The findings of the experiments reveal distinct IGC behavior among stainless steel grades. For AISI 304, the degree of sensitization (DOS) increases as exposure time progresses. However, AISI 304H and AISI 321H stainless steel exhibit diminishing DOS after 100 and 10 h of exposure, respectively. This trend is attributed to desensitization or the healing effect when stainless steel is exposed to molten salt for a prolonged time. The depletion and recovery of Cr near grain boundaries are confirmed by the inverse relationship to DOS of pitting potential.

Influence of precipitation on the intergranular corrosion sensitivity of aged Alloy 31 using a modified electrochemical potentiokinetic reactivation method

The influence of precipitation on the intergranular corrosion sensitivity of Alloy 31 aged at 950 ℃ for 0–96 h was investigated by microstructure analysis and the modified double loop electrochemical potentiokinetic reactivation method. The results reveal that the kinetics of the primary precipitated sigma phase agree with the Yamamoto equation. The degree of sensitization increases rapidly to 4 h, then decreases to 8 h with self-healing, but no further self-healing occurs after that. The degree of sensitisation depends on the Cr and Mo-depletion zone neighbouring the precipitated sigma phase.

Experimental investigation of microstructural, mechanical and corrosion properties of 316L and 202 austenitic stainless steel joints using cold metal transfer welding

The objective of the current experimental study is to investigate influence of dissimilar welding between 316 L Austenitic and 202 Austenitic Stainless Steel. This is achieved through the utilization of Cold Metal Transfer (CMT) Welding in conjunction with the GTAW mode. Various welding approaches are employed, including the use of ER316L and ER309L fillers, as well as a no-filler (autogenous) welding technique. Microstructural observation shows martensitic formation in the interface region. The tensile test was conducted by using Universal Testing Machine for the weldment and found that ER316L filler (721 MPa) has higher strength than ER309L (672 MPa) and autogenous weld (528 MPa). Charpy impact test was used to determine toughness of the weldment and found that ER309L Filler weld has toughness (87 J) which is higher than ER316L filler weld (5 4 J) and autogenous weld (23 J). Vicker's hardness test shows that autogenous weld hardness (avg. 193.34 HV) which is highest than ER309L filler (avg.188 HV) and ER316L filler weld (avg. 184.67 HV). The intergranular corrosion test by double loop electrochemical potentiokinetic reactivation (DLEPR) test shows sensitization at highest degree for autogenous weld (18.25 %) than ER316L filler weld (9.22 %) and ER309L filler weld (7.28 %).

Tensile Effect on Sensitization and Corrosion Resistance of Stainless Steels

The purpose of this research is to investigate cold work effect on corrosion behavior of stainless steels of type AISI 304, AISI 316L and AISI 2101. The specimen were processed through cold work simulated by the tensile test at various percentages elongation and then tempered at 600°C for different time intervals. Two electrochemical techniques and hardness test were utilized in this investigation. The first technique was the double loop electrochemical potentiokinetic reactivation (DL-EPR) that yields the values of degrees of sensitization (DOS). The second one was the cyclic potentiodynamic polarization (CPP) to study the ability of the metals to build or repair the damaged films under localized corrosion. The DOS values from the DL-EPR tests of the samples under the same heating conditions suggested that specimens drawn at higher percentage elongation tend to have more chromium depleted areas. Also, the test specimens with more exposure time to heat were more prone to chromium deficiencies. As for the ability of the metal to create or repair damaged film after corrosion has occurred, it was found that AISI 316L had hihger corrosion resistance than AISI 304. However, AISI 2101 stainless steel had highest corrosion resistance. In this study, it was also found that AISI 2101 did not exhibit pitting corrosion, but the crevice corrosion. This could be due the fact that AISI 2101 which is a duplex stainless steel has high corrosion resistance and could trigger the crevice corrosion take place before the pitting initiation.

An investigation of the effect of sensitization on the metallurgical characteristics of dissimilarly welded austenitic-ferritic stainless steel

Purpose The purpose of this study is to examine the effects of sensitization on the metallurgical characteristics of weld joints made up of austenitic stainless steel (AISI 316L) and ferritic stainless steel (AISI 430), using the gas tungsten arc welding (GTAW) process with ER316L filler wires. Design/methodology/approach A non-consumable tungsten electrode with a diameter of 1.6 mm was used during the GTAW procedure. The filler wire, ER316L, was selected based on the recommendation provided in literature. To explore the interconnections among the structure and properties of these weldments, the techniques including scanning electron microscopy and optical analysis have been used. In addition, the sensitization behaviour of the weldments was investigated using the double loop electrochemical potentio-kinetic reactivation (DLEPR) test. Findings Microstructural analyses revealed the occurrences of coarsened grains with equiaxed columnar grains and migrating grain boundaries in the weld zone. The results of the DLEPR test demonstrated that heat affected zone (HAZ) of AISI 430 was more susceptible to sensitization than HAZ of AISI 316L. Microstructure analysis also revealed the precipitation of large amounts of chromium carbide at the grain boundaries region of AISI 430 welded steel, causing more sensitization and, as a result, more failure or breaking at the side of AISI 430 weld in the dissimilar weldment of AISI 316L–AISI 430. Originality/value The present work has been carried out to determine the appropriate welding conditions for joining AISI 316L and AISI 430, as well as the metallurgical properties of the dissimilar weldment formed between AISI 316L and AISI 430. Owing to the difficulties in measuring the performance of these types of dissimilar joints given their unique mechanical and microstructural characteristics, research on the subject is limited.

The high temperature degradation of ferritic stainless steel in solid carbon atmospheres

Stainless steel is widely used for many components and parts in coal-fired thermal power plants. AISI 430 ferritic stainless steel (FSS) is one common grade to combat the degradation at high temperatures in coal combustion atmospheres containing flue gas, coal ash, and soot (impure solid carbon particles). However, the effect of the solid carbon particles on the degradation of FSS needs to be clarified. Graphite powder was used to simulate solid carbon atmospheres for investigating the degradation of AISI 430 at high temperatures of 1150℃ to 1350℃ in coal-fired boilers. After the carbothermic reduction, the mass gain of a pre-oxidized sample at 750℃ was approximately 0.0793 mg⸳cm-2 and increased when increasing the reduction temperature. The peak of Fe2O3 and Cr7C3 were detected by X˗ray diffraction (XRD) after the oxidation and reduction test, respectively. Besides, the degree of sensitivity (%DoS) of the samples was measured by double loop electrochemical potentiokinetic reactivation (DL-EPR) technique and increased around 30 times after heating the pre-oxidized sample to 1150℃.

On the Intergranular Corrosion Susceptibility of 304 Stainless Steel with Ultrafine Grains and Comparison with Micrometer Austenitic Grains Counterpart

The intergranular corrosion (IGC) susceptibility of ultrafine grains (∼430 nm) and micrometer grains (∼3.1 µm to 9.8 μm) 304 stainless steel obtained by cryogenic rolling and reversion annealing treatments were studied. Transmission electron microscopy results showed that after sensitized treatment at 650°C for 2 h, the micrometer grains were sensitized with many M23C6 precipitates at the grain boundaries, while no precipitates were in the ultrafine grains. The immersion corrosion tests in H2SO4-CuSO4 solution showed that ultrafine grains exhibited weaker IGC attacks than micrometer grains. The double-loop electrochemical potentiokinetic reactivation tests demonstrated the degree of sensitization decreased from 26.61% to 1.52% with the grain ultra-refinement from micrometer to ultrafine. Corrosion studies indicated that the ultrafine grains exhibited lower IGC susceptibility compared with micrometer grains. According to the findings, the large number of grain boundaries generated by grain ultra-refinement inhibited M23C6 precipitates at the grain boundaries during the sensitized process, thereby reducing the susceptibility of ultrafine grains to IGC.

Sensitization of 316L Stainless Steel made by Laser Powder Bed Fusion Additive Manufacturing

Additively manufactured (AM) 316L stainless steel (SS) manufactured by laser powder bed fusion (L-PBF) and wrought 316L SS were subjected to sensitization heat treatments at 700°C up to 100 h. Using two evaluation methods, double-loop electrochemical potentiokinetic reactivation (DL-EPR) and ditching tests, degree of sensitization (DOS) and intergranular corrosion (IGC) susceptibility was evaluated. It was found that the wrought samples showed slightly lower IGC susceptibility compared to their AM counterpart. DOS and IGC attacks increased with sensitization time for all samples. Dislocation cellular structures were found to have little to no impact on DOS and IGC for the AM samples. Sensitized at 100 h, the AM sample showed significant Cr depletion along high-angle grain boundaries (12.35 wt% on average) and exhibited Cr carbide precipitation. Mo-rich particles along grain boundaries were also observed. The DL-EPR test attacks the surface oxide film and grain boundaries while the ditching test attacks the melt pool boundaries and grain boundaries (IGC and pitting). Changes to the DL-EPR and ditching standards for AM application have been proposed in this work.

Microstructure and electrochemical evaluation of ER-308L weld overlays on AISI 321 stainless steel for repair applications

Weld overlaying is a promising and economical solution for repairing stainless steel structures. The present work deals with the deposition of ER-308L weld overlays on AISI 321 plate with Robotic gas metal arc welding setup. Microstructural examination depicts the presence of dendritic structures (equiaxed and columnar) and ferritic stringers. Energy-dispersive X-ray analysis confirmed the absence of precipitates and phases susceptible to corrosion in the as-deposited weld overlays. Specimens from ER-308L (weld overlay) and ER-308L&321-SS (interface) regions were subjected to electrochemical analysis using the Potentiodynamic polarization and double-loop electrochemical potentiokinetic reactivation measurements. Both overlay and interface sections exhibited comparable corrosion rate – 3.30 and 3.62 mils penetration per year, respectively with different passivation behaviour. The improved passivation behaviour of the ER-308L weld overlay authenticates the presence of δ-ferrite stringers. Double-loop electrochemical potentiokinetic reactivation tests highlighted the absence of sensitization on both weld overlay and interface specimens. This study presents the initial assessment results for repairing structural steel components subjected to corrosion damage.

High temperature degradation of AISI 304L stainless steel in atmospheres containing CO of biomass to liquid plants at 800 °C

Austenitic stainless steel (ASS) AISI 304L is required for the tube parts in biomass power plants due to high-temperature corrosion resistance properties. However, the high percentage of 35–40 % carbon monoxide and 25–35 % carbon dioxide in biomass atmospheres lead to deterioration in the ASS steels at high temperatures, resulting in chromium carbide formation and intergranular corrosion (IGC). This present work explored the degradation of the stainless steel AISI 304L in a simulated 15 %CO-N2 atmosphere at 800 °C at different testing times between 15 and 60 min. Besides, the ASS samples were pre-oxidized at 800 °C for six hours in air atmospheres before the test. Field emission scanning electron microscope (FE-SEM) and energy dispersive spectroscopy (EDS) were used for carbide characterization. The mass gain of samples was seemingly not changed after prolonging the reduction times. A double loop electrochemical potentiokinetic reactivation (dl-EPR) was used to observe the degree of sensitivity (%DOS) of AISI 304L samples. After the reduction test, the %DOS of samples exceeded the intergranular corrosion severity of 1 %, and the highest %DOS was 7.73 % after the reduction time of 45 min.

The Failure Mechanism of the 316 SS Heat Exchanger Tube in the Geothermal Water Environment.

In this work, the intrinsic reason for the premature failure of a 316 stainless steel heat exchanger tube in geothermal water environment is disclosed. The chemical composition of the tube was tested, and the microstructure was examined for material inspection. Fracture morphology and secondary cracks were analyzed, and electron backscattered diffraction was applied to explore the crack propagation mode. The corrosion morphology was observed. The electrochemical behavior was studied with cyclic polarization and double-loop electrochemical potentiokinetic reactivation. It is found that the main failure cause was stress corrosion cracking (SCC). Attacked by chloride ions, the tube is susceptible to SCC under the residual stress as a result of the substandard Mo and Ni content. The SCC mechanism is localized anodic dissolution, and the propagation mode is a mixture of transgranular SCC and intergranular SCC.

Corrosion behavior of wire arc additive manufactured and wrought 309 stainless steel in acidic solution

In this study, 309 stainless steel (309SS) was fabricated by wire arc additive manufacturing (WAAM) process and characterized using optical microscopy and X-ray diffractometry. Corrosion behavior of WAAM 309SS in 1 mol/L H2SO4 solution at room temperature was investigated in comparison to that of wrought 309SS using electrochemical impedance spectroscopy, pontentiodynamic polarization, and immersion test. Mott-Schottky analysis, double loop electrochemical potentiokinetic reactivation (DLEPR) test and galvanic corrosion test using zero resistance ammeter (ZRA) technique were also conducted. The results showed that WAAM 309SS exhibited lower corrosion resistance than AISI 309SS due to microstructural differences engendered by the additive manufacturing process. Galvanic corrosion test showed that galvanic effect between the two stainless steels was minimal despite the microstructural differences while DLEPR test revealed the absence of chromium-depleted zones in both WAAM 309SS and AISI 309SS.

DL-EPR vs. LSV-KOH: from simple detection of deleterious phases to analysis of morphology and high accuracy on determination of sigma phase in UNS S32750 stainless steel

ABSTRACT An optimised electrochemical technique, linear sweep voltammetry (LSV) in KOH solution (LSV-KOH) was confronted with the double loop electrochemical Potentiokinetic reactivation (DL-EPR) to verify which is the best technique to quantify deleterious phases (DP) in a UNS S32750 super duplex stainless steel. DL-EPR presented an error in determination of deleterious phases in the range of 6.9–100%. LSV-KOH show a better accuracy in quantification of deleterious phases volume fractions, the error range for LSV-KOH was 2.4–26.2%. When the morphology of sigma changes from lamellar to divorced, was observed modifications on LSV-KOH voltammograms. In specimens where lamellar morphology is present, the voltammograms show two peaks curve. Meanwhile, in specimens where occurred also divorced precipitation of sigma the voltammograms changes to a 3 peaks curve. This feature is due to the dissolution of sigma phase boundaries which has different compositions according to the form of sigma precipitation.

Ferritic-induced high-alloyed stainless steel produced by laser powder bed fusion (L-PBF) of 2205 duplex stainless steel: Role of microstructure, corrosion, and wear resistance

Stainless steels are dominant in application where combination of corrosion and mechanical resistances are requested. They have gained scientific attention in additive manufacturing (AM) field, and stainless steel products produced by AM find use in a wide array of applications. This study aims to evaluate the microstructure, the wear and corrosion resistances of a high-alloyed ferritic-induced stainless steel (FSS) obtained by laser powder bed fusion (L-PBF), from a duplex stainless steel (DSS) precursor, SAF 2205, used to produce gas-atomized powders. No heat treatment was applied to the ferritic-induced L-PBF stainless steel to restore the duplex structure. The L-PBF FSS was dense and high alloyed with Cr, Mo, and N (pitting resistance equivalent number, PREn, ~33), presenting a negligible corrosion current density in the order of 10−7 A.cm−2, with an enlarged passivation window ~ 1.2 V with respect to the corrosion potential, restraining the current density at the passivation plateau below 10−4 A.cm−2. Also, double-loop electrochemical potentiokinetic reactivation (DL-EPR) tests indicated unsensitized L-PBF FSS, with negligible degree of sensitization caused by the cyclic heat input during building up of the specimen. Besides be corrosion-resistant, the L-PBF FSS was hard (290 HV0.5) and wear-resistant against sliding wear, with a reduced specific wear rate of 5 × 10−4 mm3·N−1·m−1. The corrosion resistance of the L-PBF specimen (almost fully ferritic microstructure) was comparable to its hot-rolled precursor that displayed a duplex microstructure, albeit slight inferior. The L-PBF FSS was harder and more wear resistant than the DSS precursor. These results point out to the formation of a new high-alloyed ferritic-induced stainless steel, which are corrosion-resistant in chloride-rich medium and wear resistant in sliding conditions.

Effect of Some Environmental and Stainless Steel Metallurgical Variables on the Values of Degree of Sensitization Measured by the Double Loop-Electrochemical Potentiokinetic Reactivation Test

The double loop-electrochemical potentiokinetic reactivation (DL-EPR) method estimates the degree of sensitization in stainless steels with ir/ia, the ratio of peak current densities during reactivation (reverse) and activation (forward) scans. Beyond sensitization level, other metallurgical variables, like inclusion content and cold work, or testing environment variables, like solution deaeration and solution aging, could potentially affect ir/ia. Austenitic stainless steel Types AISI 304 (UNS S30400) and AISI 303 (UNS S30300) were tested to assess the effect of those secondary variables on ir/ia. AISI 303 stainless steel had similar chromium and nickel contents to AISI 304, but higher contents of sulfur, resulting in a higher volume fraction of inclusions. ir/ia increased with inclusion content and decreased with cold work in AISI 304 stainless steel. In all cases, the DL-EPR test could discriminate solubilized from thermally aged specimens because confidence intervals of respective samples never overlapped. The testing solution was 0.5 mol/L H2SO4 + 0.01 mol/L KSCN, (sulfuric acid and potassium thiocyanate solution) and a common practice is to freshly prepare it just before the test. Measurements are usually performed under deaerated conditions. However, deployment of the technique, especially in the field, could be facilitated if naturally aerated solutions prepared in advance in a laboratory can be used. The oxygen content in solution and solution aging did not have a statistically significant effect on ir/ia.

Hydrogen stress cracking of Alloy 716 under cathodic protection—root cause analysis, and an evaluation of quality control methods

A subsea fastener made of Alloy 716 (UNS N07716) experienced a brittle fracture in service. The investigations described herein suggested that the failure was caused by hydrogen stress cracking (HSC), thus, adding to the number of reported HSC incidents on precipitation hardened nickel-based alloys over the last two decades. Incremental step loading testing on notched tensile specimens showed a net section threshold stress of <44% of the fastener materials actual yield strength. X-ray diffraction revealed that the grain boundary (GB) precipitates were predominantly the σ–related precipitate F-phase, which were suggested to have a detrimental effect on HSC resistance—even in low amounts. The low amounts of GB precipitates were indicated by a low degree of sensitization in the double-loop electrochemical potentiokinetic reactivation test. Two additional heats from the same alloy were investigated to elucidate the effect of different GB precipitates on HSC resistance and to evaluate quality control methods that are discussed in the research community.

Study of strain induced martensite and its reversal on sensitization behaviour of metastable austenitic stainless steel

PurposeThe purpose of the present study is to investigate the effects of strain-induced martensite (SIM) and its reversal on metastable austenitic stainless steel (MASSs) through the analysis of metallurgical and sensitisation behaviour.Design/methodology/approachIn the present investigation, the samples of Cr-Mn ASS (also known as MASSs) including 15%, 30% and 50% cold worked, solution annealed samples with and without thermal ageing (at 700°C for 3 h) were analysed with the help of X-ray diffraction analysis, microstructure examination and electrochemical behaviour. The scanning electron microscope (SEMJOEL 6380 A) was used to examine the microstructure of the sample, and the double-loop electrochemical potentiokinetic reactivation test was used to determine the degree of sensitisation (DOS) in the samples. The cold worked solution annealed samples without thermal ageing are named as CR15, CR30 and CR50, respectively, and the samples with thermal ageing are named as CR15_TA, CR30_TA and CR50_TA, respectively.FindingsIn CR15, CR30 and CR50 samples, the DOS increased with increase in the extent of cold working, which was attributable to passivation deterioration. Because of the high degree of passivation at the grain boundaries, the DOS of CR15_TA and CR30_TA were practically identical. The DOS in the CR50_TA sample, on the other hand, was lowered due to SIM recovery in the austenite.Originality/valueThe present study sheds light on how to choose the right cold working percentage to avoid sensitisation in MASSs during the fabrication of metal forming components.

New Findings on Intergranular Corrosion Mechanism of 445J2 Ultra-Pure Ferritic Stainless Steel

A criterion for characterizing the intergranular corrosion sensitivity of 445J2 ultra-pure ferritic stainless steel was established using microstructure analysis and electrochemical impedance spectroscopy (EIS). The differences in the characterization results for the intergranular corrosion sensitivity of 445J2 stainless steel by EIS and the double loop-electrochemical potentiokinetic reactivation test were analyzed. The Mo-rich intermetallic compound did not cause depleted chromium zones in the sensitization temperature range of 500°C to 700°C but caused a surrounding elastic stress field. It was determined that the intergranular corrosion in 445J2 is due to the elastic stress field caused by the precipitated phase.

On-site weld quality assessment and qualification for stainless steels tanks

Stainless steel tanks are frequently degraded by localized corrosion in bioprocess industries. A case study of 2101 duplex stainless steel tank allowed to apply a portable electrochemical microcell system (PassivityScan) for on-site weld inspection and corrosion monitoring from the manufacturing until 12 months of operation. During the tank manufacturing, the double loop electrochemical potentiokinetic reactivation technique was applied to measure the sensitization degree on the welded regions. The manufactured tank was submitted to the passivation treatment to improve the passivation properties and corrosion resistance. On-site cyclic polarization tests were performed and confirmed the increase of passivation level of treated surface. The passivation level was measured again after 12�months of operation and detected a lower passivation level compared to the initial passivated surface, indicating that the passivation treatment lost its effect after that period. Therefore, an acceptance criterion to passivation level was empirically determined. PassivityScan is an advanced device to qualify the welds and the passivated surfaces, and useful for corrosion monitoring and the reliability maintenance.