Grain boundary engineering of titanium-stabilized 321 austenitic stainless steel

Grain boundary engineering (GBE) primarily aims to prevent the initiation and propagation of intergranular degradation along grain boundaries by frequent introduction of coincidence site lattice (CSL) boundaries into the grain boundary networks in materials. It has been reported that GBE is effective to prevent intergranular corrosion due to sensitization in unstabilized 304 and 316 austenitic stainless steels, but the effect of GBE on intergranular corrosion in stabilized austenitic stainless steels has not been clarified. In this study, a twin-induced GBE utilizing optimized thermomechanical processing with small pre-strain and subsequent annealing was applied to introduce very high frequencies of CSL boundaries into a titanium-stabilized 321 austenitic stainless steel. The resulting steel showed much higher resistance to intergranular corrosion after sensitization subsequent to carbon re-dissolution heat treatment during the ferric sulfate–sulfuric acid test than the as-received one. The high CSL frequency resulted in a very low percolation probability of random boundary networks in the over-threshold region and remarkable suppression of intergranular corrosion during GBE.     

Effect of grain boundary microstructure on fatigue crack propagation in austenitic stainless steel

The effect of grain boundary microstructure on fatigue crack propagation in austenitic stainless steel was investigated in order to control fatigue crack propagation. The fraction of low-Σ coincidence boundaries in specimens was controlled by thermomechanical processing. The specimen with the higher fraction of low-Σ boundaries (73%) showed the lower propagation rate of fatigue crack than the specimen with the lower fraction of low-Σ boundaries (53%). The ratio of intergranular fracture segments to the total crack length was lower for the specimen with the higher fraction of low-Σ boundaries. Moreover, the roles of grain boundaries in the fatigue crack propagation were investigated in connection with grain boundary microstructure, i.e., the character distribution and geometrical configuration of grain boundaries. It is evidenced that the approach to grain boundary engineering is applicable to controlling fatigue crack propagation in austenitic stainless steel.     

Weld decay-resistant austenitic stainless steel by grain boundary engineering

This paper presents an example of grain boundary engineering (GBE) for improving intergranular-corrosion and weld-decay resistance of austenitic stainless steel. Transmission and scanning electron microscope (TEM and SEM) observations demonstrated that coincidence site lattice (CSL) boundaries possess strong resistance to intergranular precipitation and corrosion in weld decay region of a type 304 austenitic stainless steel weldment. A thermomechanical treatment for GBE was tried for improvement of intergranular corrosion resistance of the 304 austenitic stainless steel. The grain boundary character distribution (GBCD) was examined by orientation imaging microscopy (OIM). The sensitivity to intergranular corrosion was reduced by the thermomechanical treatment and indicated a minimum at a small roll-reduction. The frequency of CSL boundaries indicated a maximum at the small roll-reduction. The corrosion rate was much smaller in the thermomechanical-treated specimen than in the base material for long time sensitization. The optimum thermomechanical treatment introduced a high frequency of CSL boundaries and the clear discontinuity of corrosive random boundary network in the material, and resulted in the high intergranular corrosion resistance arresting the propagation of intergranular corrosion from the surface. The optimized 304 stainless steel showed an excellent resistance to weld decay during arc welding.     

A new etching route for revealing the austenite grain boundaries in an 11.4% Cr precipitation hardening semi-austenitic stainless steel

A detailed metallographic characterization of a precipitation hardening semi-austenitic stainless steel is described. A new etching procedure based on the Lichtenegger and Blöch color etching solution, which is frequently used in duplex stainless steels to differentiate delta ferrite from austenite, has been used to differentiate martensite, austenite and the Chi-phase in this stainless steel. By changing the etching conditions, this etchant now reveals the austenite grain boundaries when the steel is in the austenitic state. Moreover, this solution is able to reveal also the prior austenite grain boundaries when the steel is in its martensitic state. This etching procedure represents a great advantage because it reveals, at the same time, different features of the microstructure.     

Improvement of Stress-rupture Life for Modified-HR6W Austenitic Stainless Steel

Stress-rupture life of HR6W austenitic stainless steel modified with B and Mg additions was measured, and the microstructures were analyzed by optical microscopy, X-ray diffraction, scanning electron microscopy and transmission electron microscopy equipped with energy dispersive spectroscopy. The results indicated that the enhancement of the stress-rupture life was mainly due to the precipitation with B in the elemental form at the grain boundaries, and the improvement of the form of carbides at grain boundaries and the removal of O and S elements by addition of Mg. The micro-alloying elements have a beneficial effect on stress-rupture life of the modified-HR6W austenitic stainless steel at high temperature.     

Microstructure and properties of austenitic stainless steel reinforced with in situ TiC particulate

Austenitic stainless steel reinforced with 5 vol.% TiC particulate was in situ synthesized by in situ reaction during melting process successfully and its microstructure, mechanical properties as well as oxidation behavior were investigated. Microstructure observations revealed that in situ TiC particulates with an average size of 2–10 μm distributed uniformly in the matrix and the interface boundaries between TiC particulates and austenite matrix were clean without any impurities and contaminations. Addition of TiC particulates refined the grain structure of austenitic matrix, but did not cause formation of any new phases in microstructure. Beneficial effects of TiC addition to austenitic stainless steel on both mechanical properties and oxidation resistance were found. Both at ambient and elevated temperature, tensile strengths of the steel with TiC addition were notably higher than those of its matrix alloy, however, a decrease in ductility also appeared, as exhibited by other particulate reinforced alloys. Besides tensile strengths, creep resistance of austenitic stainless steel was also significantly increased by TiC addition at elevated temperature of 923 K. Oxidation test at 1073 K revealed that TiC addition to austenitic stainless steel raised the oxidation resistance of the steel remarkably.     

Grain-size and heat-treatment effects in hydrogen-assisted cracking of austenitic stainless steels

Hydrogen embrittlement of 304L and 316L types austenitic stainless steels has been studied by charging thin tensile specimens with hydrogen through cathodic polarization. Throughout this study we have compared solution-annealed samples, having various prior austenite grain size, with samples given the additional sensitization treatment. The results of the tensile tests while undergoing cathodic charging show that the additional sensitization treatment and coarse-grained samples together, lower the mechanical properties in both 304L and 316L types, and the sensitized steel is more susceptible to hydrogen-assisted cracking. However, the room-temperature yield and ultimate strengths, and the elongation of type 316L, were much less affected depending on the heat treatment and prior austenitic grain size. The fracture surfaces of the specimens tested while cathodically charged show considerable differences between the annealed and the sensitized specimens. The sensitized coarse-grained specimens were predominantly intergranular in both 304L and 316L types, while the annealed 316L type specimens fracture shows massive regions of microvoid coalescence producing ductile rupture and the annealed 304L type specimens fracture were primarily transgranular and cleavage-like. Sensitization seems both to facilitate the penetration of hydrogen along the grain boundaries into the steel and to introduce susceptibility to fracture along grain boundaries while refined grain size improves resistance regardless of the failure mode.     

Failure of a Secondary Superheater Tube in a 140-MW Thermal Power Plant

This investigation was conducted to determine the cause of failure of a welded joint of a secondary superheater tube from a 140-MW thermal power plant. Chemical analyses along with detailed optical microscopic examination of a secondary superheater tube were carried out to predict the probable cause of failure. Microstructure of the secondary superheater tube welded between austenitic stainless steel to low alloy steel revealed presence of a thin layer of metal carbide along the weld interface which eventually led to intergranular cracking at austenite grain boundaries. It was concluded that the formation of brittle carbide layer was due to migration of carbon at elevated temperature led to failure of the tube.     

MECHANISMS AND FACTORS THAT INFLUENCE POSTWELD INTERGRANULAR UNDERCLAD CRACKING

Abstract— Forged components of ferritic steel can be protected by a welded austenitic stainless steel clad. Intergranular cracking can take place in the ferritic phase close to the ferritic austenitic interface. After developing a technique for fabrication of these cracks, the formation conditions are studied. Auger electron spectroscopy investigations of specimens containing a real crack opened inside the vacuum chamber are used for interpretation. Sulphur segregations embrittle the grain boundaries which are cracked by residual and thermal stresses during the postweld heat treatment.     

奥氏体不锈钢在石油精炼环境中应力腐蚀破裂

通过恒变形和恒载荷试验研究了敏化18—8型奥氏体不锈钢在连多硫酸介质中的应力腐蚀行为。研究表明,介质浓度在2.0～6.0％,PH 值在0.8～1.8范围是材料出现应力腐蚀破裂的敏感介质。断口分析表明,在该体系中破裂属晶间型。钢中晶界贫铬区的存在是产生晶间型应力腐蚀破裂的主要原因。     

Initiation of recrystallized grain structure under high-temperature low-cycle fatigue in 304 stainless steel

Initiation of recrystallized grains was observed under high-temperature low-cycle fatigue conditions in austenitic 18Cr-8Ni stainless steel. The fatigue tests were carried out using unbalanced fast-tension and slow-compression triangular strain wave-shape at 973 K in air. Recrystallized grains were initiated and grew along grain boundaries with the number of fatigue cycles. Accumulated grain-boundary sliding is considered to be the driving force for the recrystallization. Effects of the recrystallized grain structure on high-temperature fatigue failure were then examined under the conditions in which intergranular fatigue failure occurred. The recrystallized grain structure had no detrimental effects on the intergranular failure. The fatigue life was somewhat increased by the initiation of recrystallized grain structure.     

Effects of Deformation (Strain) and Heat Treatment on Grain Boundary Sensitization and Precipitation in Austenitic Stainless Steels

Sensitization, particularly the degree of sensitization (DOS) in type 316 stainless steel pipe is critically dependent upon the solution anneal of the mill-annealed or commercial material, and is particularly sensitive to low-temperature aging when the starting material is solution annealed between about 1,000°C and 1,100°C. It is observed that when the DOS is above about 10 C/cm² (quantitative electrochemical potentiokinetic reactivation units in Coulombs/cm²), noticeable carbide precipitation occurs in the grain boundaries and increases with increasing DOS. Transmission electron microscopy (TEM) examination of precipitation occurring in type 316 stainless steel pipe grain boundaries has shown them to exhibit many microstructural features that seem to be coincident with grain boundary microstructures, particularly ledges. Uniaxial, tensile strain prior to aging of solution annealed pipe was observed to have a dramatic effect on DOS of type 316 stainless steel pipe; DOS increases with increasing strain. This effect appears to be correlated with the propensity of dislocations to be generated near grain boundaries, and for grain boundary microstructural changes to be related with strain, as observed in type 304 stainless steel. The effects of strain on DOS, combined with instabilities connected with annealing of type 316 stainless steel, indicate that in the practical utilization of pipe, it is imperative to reduce deformation prior to service and during service applications, to avoid sensitization and, thus, minimize the probability of grain boundary cracking.     

200系列不锈钢钢丝失效分析

本文应用扫描电镜、能谱分析、电子显微镜等多种分析方法,对201及200Cu两种不锈钢钢丝的断裂原因进行了研究分析。结果表明,由于200系不锈钢的奥氏体稳定性较差,较易发生晶界腐蚀,在拉制过程中因所受应力不均匀,导致微裂纹产生,在随后的多次拉拔工艺中发生扩展开裂。     

Suppression of chromium depletion and sensitization in austenitic stainless steel by surface mechanical attrition treatment

The effects of surface nanocrystallization via surface mechanical attrition treatment (SMAT) on degree of sensitization (DOS) of an austenitic stainless steel were investigated by means of double loop electrochemical potentiokinetic reactivation (DLEPR) test. The treated sample with grain size about 10 nm showed very low degree of sensitization value which can be considered as the non-sensitized material. This is mainly due to the formation of twin boundaries in the microstructure of the SMATed sample which weren't susceptible to carbide precipitation because of their regular and coherent atomic structure and extreme low grain boundary energy as compared with those of other grain boundaries.     

Effect of extrinsic grain-boundary dislocations on M23C6 precipitate nucleation in an austenitic stainless steel

From a comparison of the isothermal precipitation curve for M₂₃C₆ grain-boundary precipitates in an austenitic stainless steel and of the spreading times of extrinsic grain-boundary dislocations (EGBDs), it has been shown that M₂₃C₆ precipitates cannot directly nucleate on EGBD lines lying on random high-angle grain boundaries. This process can occur only on coherent and incoherent twin and other special boundaries.     

Quantitative aspects of precipitation at grain boundaries in an austenitic stainless steel

This paper shows, in a quantitative manner, how the precipitation of niobium carbide in an austenitic stainless steel is affected by varying the amount of deformation prior to ageing. In particular, the extrinsic dislocation content of grain boundaries is shown to govern the overall size distribution of grain-boundary precipitates developed during ageing.     

Microstructural thermostability of high nitrogen austenitic stainless steel

A high nitrogen austenitic stainless steel, Fe–24Mn–18Cr–3Ni–0.62N, was isothermally annealed from 750 to 900 °C for different times to investigate the thermostability of its microstructures. Results show that the precipitates were Cr₂N and initially formed along the grain boundary. The time–temperature–precipitation diagram was established, according to which the critical cooling rate of this material with less than 0.1–0.5 vol.% of precipitated Cr₂N was specified as 30 °C/min. The microhardness of the matrix in samples annealed at different temperatures decreased with the diffusion of nitrogen from the matrix to grain boundaries.     

Effects of orientation,stress and exposure time on short intergranular stress corrosion crack behaviour in sensitised type 304 austenitic stainless steel

Intergranular stress corrosion cracking (IGSCC) in austenitic stainless steels occurs at susceptible grain boundaries after sensitisation. In this study, the effects of test duration, static stress (applied and residual) and microstructure orientation on the developed populations of short crack nuclei are reported for a sensitised type 304 austenitic stainless steel in an acidified potassium tetrathionate (K₂S₄O₆) solution. The crack populations were analysed using the Gumbel distribution method, showing an increase in the characteristic crack lengths with increasing time and grain size. There is a weak, but measurable effect of stress on crack length. Tensile stress increases crack growth and compressive residual stresses introduced by surface machining are shown to be beneficial. A significant dependence on sample orientation is observed and this cannot be explained in terms of the bulk microstructure properties or characteristics, which showed no significant variations.     

The precipitation of niobium carbide at grain boundaries in an austenitic stainless steel

Electron microscopy has been used to show that the precipitation of niobium carbide at the grain boundaries of an austenitic stainless steel can occur in a spatially non-random fashion. Preferential nucleation and growth of carbides occurs on grain-boundary defect structures. Where present, these defect structures include extrinsic grain-boundary dislocations and topographical discontinuities. An example of the precipitation of niobium carbide on an intrinsic dislocation array is also shown.     

Effect of grain boundary orientation on the sensitization of austenitic stainless steel

The effect of grain misorientation on the sensitization of grain boundaries in austenitic stainless steel was investigated by sensitizing samples consisting of a large number of 50–80 μm size grains that were sintered to flat, 10 mm2 single crystals. Seven different sensitization treatments were employed and samples were intergranulary corroded in the modified Strauss test. X-ray pole figures were obtained for each sample and were used to identify the grain misorientations that were resistant to sensitization. In general, macroscopic grain boundary geometry could not explain the sensitization behaviour of most grain boundaries. Nevertheless, the Σ = 9 boundary was found to be especially resistant to sensitization. Results suggest that grain misorientation primarily affects the growth of sensitization rather than its nucleation. Finally, the crystallographic plane of the grain boundary appears to have an effect on sensitization. This revised version was published online in November 2006 with corrections to the Cover Date.