304奥氏体不锈钢离子辐照后再活化性能测试和表面形貌观察

对核电用奥氏体不锈钢进行固溶和敏化处理,对部分固溶试样进行Fe 和He 辐照,随后测量了4种处理状态试样的再活化率(EPR),并观察表面形貌.结果表明:经He 辐照试样出现了2.88%的再活化率,敏化试样的再活化率是19.5%,固溶试样和经Fe 辐照试样的再活化率为0.离子辐照试样的表面形貌与固溶或敏化试样完全不同.     

Electrochemical Evaluation of Radiation-Induced Segregation in Austenitic Stainless Steels with Oversize Solute Addition

Effect of different levels of oversize element, cerium, on radiation-induced segregation (RIS) in type 316 stainless steel was investigated. The effect of prior cold-work on RIS was also investigated. Samples with 0.00, 0.01, and 0.04 wt.% cerium were irradiated to 0.70 dpa using 4.8 MeV protons at 300 °C. Characterization of proton-irradiated specimens was carried out using electrochemical potentiokinetic reactivation (EPR) test followed by atomic force microscopic examination. The specimen with prior cold-work (without cerium addition) showed the lowest EPR values indicating the lowest chromium depletion in this material. The specimen with 0.04 wt.% cerium showed the lower EPR value as compared to the specimen with 0.01 wt.% Ce. The irradiated specimen with prior cold-work showed linear features after the EPR tests and such features were attributed to decoration of dislocations, generated due to prior cold-work, by point defects produced during irradiation. The resistance to RIS offered by cold-work (linear features) has been more effective as compared to that by the addition of oversize solute addition.     

Field studies of corrosion behaviour of copper alloys in natural seawater

Eight copper alloys were tested in a one-year field deployment in the North Atlantic Ocean. The corrosion behaviour was characterized by weight loss, optical and electronic microscopy analyses. The biofouling performance was quantified in terms of the biomass accumulation. The testing program included specimens in tensioned and untensioned configurations, as well as a set for seasonal deployments. The seasonal corrosion rates were 140% higher, and the rates of tensioned specimens were 39% higher than those of the untensioned specimens after 12 months of deployment. Good biofouling resistance was observed for all but one alloy, which exhibited heavy fouling by barnacles.     

Characterisation by X-ray absorption near-edge spectroscopy of KMnO4-based no-rinse conversion coatings on Al and Al alloys

No-rinse conversion coatings based on KMnO₄, were applied to aluminium alloys and pure aluminium, and examined with X-ray absorption near edge spectroscopy (XANES). Some specimens were prepared beforehand and other specimens were freshly prepared immediately before testing, so that early changes in the coatings could be studied. A significant difference in composition was found between the one-week old specimens and the fresh. The old specimens consisted predominantly of Mn oxides, while the fresh specimens contained a substantial proportion of KMnO₄. When fresh specimens were rinsed with de-ionised water, soluble KMnO₄ was removed and the spectrum now showed evidence for mixed oxides, but no KMnO₄, like the older specimens. Monitoring of specimens after exposure to 0.5% NaCl solution showed little further change in the film.     

Evaluation of delayed fracture property of outdoor-exposed high strength AISI 4135 steels

Delayed fracture properties of AISI 4135 high strength steels with 1490 and 1310 MPa of tensile strength, represented as B15 and B13, respectively, have been studied by means of slow strain rate test (SSRT) of notched bar specimens after outdoor exposure at rural and coastal areas. The exposed specimens were kept at humid medium before SSRT to reproduce active hydrogen entry influenced by the rust layer and to homogenize hydrogen distribution. The influences of exposure site and exposure time on fracture stress have been investigated. The susceptibility of B15 to delayed fracture was obviously higher than that of B13.     

Influence of molybdate species on the tartaric acid/sulphuric acid anodic films grown on AA2024 T3 aerospace alloy

AA2024 T3 alloy specimens have been anodised in tartaric acid/sulphuric media and tartaric acid/sulphuric media containing sodium molybdate; molybdate species were added to the anodising bath to enhance further the protection provided by the porous anodic film developed over the macroscopic alloy surface. Morphological characterisation of the anodic films formed in both electrolytes was undertaken using scanning electron and transmission electron microscopies; the chemical compositions of the films were determined by Rutherford backscattering spectroscopy that was complemented by elemental depth profiling using rf-glow discharge optical emission spectrometry. The electrochemical behaviour was evaluated using potentiodynamic polarisations and electrochemical impedance spectroscopy; the corrosion performance was examined after salt spray testing. The porous anodic film morphology was little influenced by the addition of molybdate salt, although thinner films were generated in its presence. Chemical composition of the anodic film was roughly similar; however, addition of sodium molybdate in the anodizing bath resulted in residues of molybdate species in the porous skeleton and improved corrosion resistance measured by electrochemical techniques that was confirmed by salt spray testing.     

Microstructure and intergranular corrosion resistance of UNS S17400 (17-4PH) stainless steel

UNS S17400 or 17-4PH is a precipitation hardening martensitic stainless steel with many industrial applications. Quite different mechanical properties can be produced in this material by varying the aging temperature. In this work, the influence of aging temperature on the intergranular corrosion susceptibility was evaluated by electrochemical and metallographic tests. The microstructural features were investigated by X-ray diffraction, optical and scanning electron microscopy. Intergranular chromium carbide precipitation occurs in specimens aged at high temperatures, although NbC carbides were also observed. The results obtained by double loop electrochemical potentiodynamic reactivation tests (DL-EPR) show that the susceptibility to intergranular corrosion resistance increases with the increase of aging temperature. Healing due to Cr diffusion in the 600-650 °C range was not observed by DL-EPR tests.     

Effect of hydrogen on the fracture behavior of high strength steel during slow strain rate test

The effect of hydrogen on the fracture behavior of the quenched and tempered AISI 4135 steel at 1450 MPa has been investigated by means of slow strain rate tests on smooth and circumferentially-notched round-bar specimens. Hydrogen was introduced into specimens by electrochemical charging and its content was measured by thermal desorption spectrometry (TDS) analysis. Results showed that the steel had high hydrogen embrittlement susceptibility. For both smooth and notched specimens, the fracture mode was changed from microvoid coalescence (MVC) to brittle intergranular (IG) fracture after the introduction of a small amount of diffusible hydrogen. Fracture initiated in the vicinity of the notch root for notched specimens, while it started from around the center in smooth specimens. The fracture stress decreased with increasing diffusible hydrogen content, and the decreasing trend was more prominent for specimens with a higher stress concentration factor. Taking into account the stress-driven hydrogen diffusion and accumulation in the vicinity of the notch root, the local diffusible hydrogen concentration and local fracture stress in notched specimens have been calculated. According to numerical results, the relationship between the local fracture stress and local diffusible hydrogen concentration was independent of stress concentration factor, which could account for the effect of hydrogen on the fracture stress of the steel.     

Mechanical behaviour of SSRT specimens optimized for IGSCC concerns

Simulating testing conditions leading to evaluate the intergranular stress corrosion cracking sensitivity of structural alloys is crucial to estimate the lifetime of in-service components. Former studies have pointed out that a simple modification of the design of slow strain rate tensile specimens was particularly convenient for evaluating the susceptibility to intergranular stress corrosion cracking of nickel-base alloys. The aim of the present work is to characterize and model the mechanical behaviour of such specimens. Validation of proposed modelling relies mainly on tensile tests carried on specimens equipped with strain gages. One of the striking results is that, for a given displacement rate of the heads of the specimen, a much slower strain rate can be obtained locally in comparison with the strain rate of an equivalent smooth specimen.     

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.     

Electrochemical reactivation methods applied to PM austenitic stainless steels sintered in nitrogen-hydrogen atmosphere

Exposure methods (ASTM A262 Practice A and Modified Strauss Test) and electrochemical reactivation methods such as EPR and EPRDL was applied to PM 304L and PM 316L stainless and comparisons with wrought stainless steels were made. Sintering in vacuum and nitrogen-hydrogen atmosphere was chosen. The latter was the focus of the work and the former was used on comparative basis. It was seen how nitrogen in PM stainless steels plays a relevant role both when is dissolved and when is in intermetallic precipitates. A set of heat treatments were applied: annealing and sensitizing at 375, 675 and 875 °C. The results indicate that the electrochemical reactivation methods are suitable to evaluate the degree of sensitization of PM austenitic stainless steels.     

Use of EPR test to study the degree of sensitization in resistance spot welding joints of AISI 304 austenitic stainless steel

The degree of sensitization (DOS) in resistance spot welding (RSW) joints is considered as the combined effect of intergranular corrosion (IGC) and transgranular corrosion (TGC) in the heat affected zone (HAZ) and of interdendritic corrosion (IDC) in the weld nugget (WN). The DOS is evaluated from electrochemical potentiokinetic reactivation (EPR) tests. The application of EPR test to RSW joints is optimized and an electrochemical minicell is used to study the effect of heat input on IDC in the WN.     

Thermal and mechanical stabilities of Hi-Nicalon SiC fiber under annealing and creep in various oxygen partial pressures

Thermal and mechanical stabilities were investigated on Hi-Nicalon SiC fibers under annealing and creep in various oxygen partial pressures by mass change, mechanical properties as well as microstructural features. In the case of mechanical stability, the tensile strength of fiber is strongly dependent on the oxygen partial pressure of testing environment, but a weak dependence of BSR creep resistance on oxygen partial pressure is appeared. The analyses of surface morphology and mass change indicated the thermal stability of fiber under annealing in different environments was different. At different exposure temperatures and oxygen partial pressure levels, the different oxidation regimes are responsible for the strength degradation and microstructure change of fibers. Furthermore, the microstructure change is also affected by the stress applied through BSR test. This means the thermal stability of fibers is related to not only the exposed environments, but also the mechanical state of fibers.     

Improving the corrosion behaviour of powder metallurgical 316L alloy by prepassivation in 20% nitric acid

The electrochemical improvement of PM 316L stainless steels by pre-alloyed powder prepassivation in 20% nitric acid in comparison with as-received specimens has been studied in this work. For comparison purposes a simultaneous study was carried out on similar composition wrought AISI 316L steels. Corrosion resistance was studied using evolution of the corrosion potential vs. time, anodic polarisations curves and Zero Resistance Ammeter technique. Reductions of the corrosion rate (i_corr) were observed in prepassivated specimens in neutral chloride media. Crevice resistance was higher for prepassivated specimens and for higher densities and annealing as post-heat treatments.     

Exfoliation corrosion of extruded 2024-T4 in the coastal environments in China

Exfoliation behavior of extruded 2024-T4 in four coastal environments was investigated by the field testing and laboratory-accelerated test. At the Wanning, Qionghai and Qingdao test sites, exfoliation appeared on 2024-T4 after 6, 10 and 20 years exposure, respectively. At the Guangzhou test site, 2024-T4 did not suffer exfoliation after 20 years exposure. In the laboratory-accelerated test, the effects of relative humidity, temperature and Cl⁻ amount on exfoliation were studied. Exfoliation could not occur on extruded 2024-T4 when RH was below 75%. Above this RH, the higher the temperature or the Cl⁻ amount was, the more serious exfoliation the specimen suffered.     

Effects of tungsten on the hydrogen embrittlement behaviour of microalloyed steels

The effects of tungsten (W) additions (0, 0.1, 0.5 and 1 wt.%) on the hydrogen embrittlement behaviour of microalloyed steels were systematically investigated by means of slow strain rate tests on circumferentially notched cylindrical specimens, and the mechanism of hydrogen-induced embrittlement was discussed. W addition is found to increase the activation energy of hydrogen desorption. Microstructural features affect the hydrogen embrittlement behaviour and fracture modes of microalloyed steels. It is suggested that the hydrogen-induced embrittlement in the studied microalloyed steels with different W additions is caused by the combined effects of decohesion and internal pressure in the presence of hydrogen.     

Effect of biofilm on ennoblement and localized corrosion of stainless steel in fresh dam-water

AISI 304 stainless steel specimens were exposed in-situ to fresh dam-water for nearly 2 years. Open circuit potential (OCP) of the specimens becomes remarkably ennobled after exposure for about 40 days. The ennobled OCP of coupons is greatly affected by both immersion depth and sunlight. It is found that ammonium, nitrate, nitrite and chloride ions are enriched in the biofilm. It is suggested that the reduction of nitrate may be partly responsible for the OCP ennoblement. Localized corrosions at welds and crevices of specimens are attributed to both the OCP ennoblement of specimens and the chloride ion enrichment in the biofilm.     

Self-healing polymer coatings with cellulose nanofibers served as pathways for the release of a corrosion inhibitor

Polymer coatings containing cellulose nanofibers were applied to carbon steel for corrosion inhibition. The specimens were scratched with a knife-edge, and then polarization resistance was monitored in a sodium chloride solution. The polarization resistance of the scratched specimen containing nanofibers and corrosion inhibitor was higher than that of a polymer coating that contained only a corrosion inhibitor. The optimal mixing ratio of corrosion inhibitor for cellulose nanofibers was 4. Empty holes were confirmed on a cross-section of the polymer coating after the corrosion test, which showed that the nanofibers served as pathways for the release of the corrosion inhibitor.     

Determination of the critical hydrogen concentration for delayed fracture of high strength steel by constant load test and numerical calculation

The critical hydrogen concentration for hydrogen induced delayed fracture of the AISI 4135 steel at 1320 and 1450 MPa has been determined by constant load tests in combination with numerical calculations, and thus the concept of a critical hydrogen concentration has been verified. The time to fracture was obtained for circumferentially notched round bar specimens under a constant load after electrochemically pre-charged with various hydrogen contents. A numerical model was then developed for calculating the accumulated hydrogen concentration in the vicinity of the notch root, taking into account the driving effect of the hydrostatic stress on hydrogen transport. The results showed that the delayed fracture of the steel occurred when a critical hydrogen concentration at the location of the stress peak was reached by accumulation, and that the time to fracture was related to the stress-driven hydrogen accumulation process. The critical hydrogen concentration was dependent not only on the strength level, but also on the stress concentration factor of the specimens.     

The initial stage of pitting corrosion on coated steels investigated by photon rupture in chloride containing solutions

A photon rupture method, film removal by a focused pulse of pulsed Nd-YAG laser beam irradiation, has been developed to enable oxide film stripping at extremely high rates without contamination from the film removal tools. In the present study, Zn-55mass%Al alloy and Al-9mass%Si alloy-coated steel specimens covered with protective nitrocellulose film were irradiated with a focused pulse of a pulsed Nd-YAG laser beam at a constant potential in 0.5 kmol m⁻³ H₃BO₃-0.05 kmol m⁻³ Na₂B₄O₇ (pH = 7.4) with 0.01 kmol m⁻³ of chloride ions to investigate the initial stage of localized corrosion. At low potentials, oxide films on both coated alloys were reformed after the nitrocellulose films were removed by this method. The oxide film formation kinetics follows an inverse logarithmic law, in agreement with Cabrera-Mott theory. However, at high potentials, localized corrosion producing corrosion products occurs at the area where nitrocellulose film was removed. Nevertheless, when the applied potential is less noble, the dissolution current of the Zn-55mass%Al-coated steel samples is higher than that of Al-9mass%Si-coated samples.