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.     

Characteristics of hydrogen-assisted intergranular fatigue crack growth in interstitial-free steel: role of plastic strain localization

The behavior of intergranular fatigue crack growth in an interstitial-free (IF) steel in a hydrogen environment was investigated at different frequencies. Focusing on the plastic strain localization, we observed details of the striation-like feature on the intergranular fracture surface, slip behavior around microvoids, and crystallographic orientation gradient underneath the fracture surface. It was determined that the intergranular fatigue crack growth mechanism in the IF steel is microvoid formation at the crack tip and subsequent coalescence with the crack. Moreover, it was found that the grain boundaries, acting as propagation paths, suffer from pre-damage arising from plastic strain localization near the grain boundaries even before the main crack propagates to a certain location. Therefore, fatigue cracks in a hydrogen environment easily propagate to the grain boundaries. The frequency dependence of fatigue crack growth in the hydrogen environment is significantly smaller than that in a low carbon steel, probably because of the frequency dependence of the pre-damage evolution behavior.     

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.     

Improvement of fatigue-crack growth resistance by grain-boundary reaction precipitates at high temperature

Effects of grain-boundary reaction precipitates on fatigue-crack growth rate were investigated using austenitic 21 wt% Cr-4 wt% Ni-9wt% Mn heat-resisting steel at 973 K in air. Grain boundaries were serrated by-the grain-boundary reaction precipitates. The crack growth rate was considerably decreased by these precipitates, especially at low crack growth rates. Fatigue cracks extended to the serrated grain boundaries or to the interface between the grain-boundary reaction nodule and the grain. Therefore, the cracks grew along zigzag paths, and brittle intergranular fracture was inhibited. The decrease in the fatigue-crack growth rate was explained by these changes in fracture mode.     

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.     

Improvement of Intergranular Stress Corrosion Crack Susceptibility of Austenite Stainless Steel through Grain Boundary Engineering

Intergranular stress corrosion crack susceptibility of austenite stainless steel was evaluated through threepoint bending test conducted in high temperature water. The experimental results showed that the frequent and efficient introduction of low energy coincidence site lattice boundaries through grain boundary engineering resulted in an apparent improvement of the intergranular stress corrosion crack resistance of austenite stainless steel.     

S32750双相不锈钢相界与晶界特征对其力学性能和耐蚀性能的影响EI北大核心CSCD

通过固溶处理获得不同初始组织状态的S32750双相不锈钢样品,然后进行厚度压下量80%的冷轧变形和1050℃的退火处理,采用SEM-EBSD和XRD技术研究合金相界与晶界特征以及相组成分布情况,并利用拉伸实验、纳米压痕和双环电化学动电位再活化法(DL-EPR)分析不同初始状态样品的组织对力学性能与耐晶间腐蚀性能的影响规律。结果表明:高温固溶处理的合金样品经冷轧退火后晶粒细小均匀,两相分布接近1∶1,且相界占内界面(晶界+相界)比例较高,同相晶粒团簇程度最低,表现出优异的综合力学性能。合金样品经敏化处理后,σ相易沿α相晶界析出,高温固溶并经轧制退火后的样品中,由于α晶界比例较少且满足K-S取向关系的相界比例较高则又表现出良好的晶间腐蚀抗力。因此,通过适当的工艺来调控合金的相界与晶界分布可以实现材料强度和晶间腐蚀抗力的同步改善。     

Grain boundary character distribution and its effect on corrosion of Ni–23Cr–16Mo superalloy

Grain boundary character distribution (GBCD) of the Hastelloy C2000 alloy (Ni–23Cr–16Mo) and the effect of coincidence site lattice (CSL) grain boundaries on corrosion resistance were examined by electron backscattered diffraction and electrochemical experiments. Various deformation followed by annealing was applied to optimise the GBCD of the alloy. After grain boundary engineering (GBE) treatment, the proportion of CSL boundaries increased from 37.7% to 62.4% and the corrosion current density of the specimens decreased in NaCl solution. The results indicated that GBE treatment is responsible for preferable corrosion resistance due to the increase of the fraction of special low energy grain boundaries with perfect grain boundary atom arrangement after thermomechanical process.     

Grain boundary engineering and the role of the interfacial plane

Abstract

Grain boundary engineering (GBE) involves the use of microstructural design to improve bulk material properties and enhance resistance to intergranular degradation. More specifically, the patented GBE procedure involves the design and control of fcc metallic microstructures using thermomechanical treatments and grain boundary characterisation based on the coincidence site lattice model. The phenomenon of multiple twinning is used to create a ‘twin limited’ microstructure, i.e. a microstructure composed entirely of special grain boundaries and triple junctions that is highly resistant to intergranular degradation. However, the theory behind GBE is not fully developed and therefore further study of the interfacial geometry, including the grain boundary plane and its role in GBE, is required to improve understanding of multiple twinning with the ultimate aim of improving the bulk and intergranular properties of metallic materials. An introduction to GBE is presented, including a number of cases where grain boundary design has improved the properties of fcc alloys for industrial applications. The theoretical characterisation of grain boundaries, including interfacial structure and geometry, is reviewed, highlighting the problems associated with microstructural characterisation based on limited knowledge of the grain boundary geometry. The importance of the grain boundary network is discussed: the grain boundary and triple junction character distributions are known to have a significant influence on bulk properties. Finally, the role of the interfacial plane is considered. It is concluded that although GBE has produced significant results, its theoretical basis and the ultimate creation of twin limited microstructures require further development.     

Correlation between the intergranular brittleness and precipitation reactions during isothermal aging of an Fe–Ni–Mn maraging steel

Evolution of the intergranular brittleness of an Fe–10Ni–7Mn (weight pct) maraging steel was correlated with precipitation reactions during isothermal aging at 753 K. Intergranular brittleness of the Fe–Ni–Mn steel raises after aging treatment which occurs catastrophically at zero tensile elongation in the underaged and peakaged steels. The intergranular failure is attributed to grain boundary weakening due to the formation of coarse grain boundary precipitates associated with solute-depleted precipitate-free zones during isothermal aging. Further, evidences of planar slip bands were found within the grains of a peakaged specimen loaded by tensile deformation. Those inhomogeneously deformed bands were identified to apply large strain localization in the soft precipitate-free zones at grain boundaries which is assumed to fascinate microcracks initiation at negligible macroscopic strains in the underaged and peakaged steels. During further aging, concurrent reactions including (i) overaging of matrix precipitates, (ii) spheroidization of grain boundary precipitates, (iii) growth of precipitate-free zone in width and (iv) diffusional transformation to austenite take place which increase tensile ductility after prolonged aging.     

Production of very fine grained AISI 304 steel with high special grain boundary density by grain boundary engineering

Abstract

AISI 304 stainless steel was subjected to grain boundary engineering by applying cycles of calibre rolling and subsequent heat treatment. After three cycles the grain size started to decrease, and after the fourth cycle a very fine grained material having high fraction of special grain boundaries was produced. Due to the short heat treatment at 850°C, only partial recrystallization occurred after the first three cycles, which was proven by the large amount of low angle boundaries. The stored elastic strain energy helped the grain boundary movement and the formation of annealing twins in the fourth cycle, which caused the formation of very fine grained structure with a large amount of special grain boundaries.     

Warm multiaxial forging of AISI 1016 steel

In this work, the microstructural evolution in AISI 1016 steel processed by using warm multiaxial forging technique is studied. With increase in multiaxial forging strain, a finer substructure evolved. Structural evolution in pearlite phase is addressed in detail considering the strain paths and strain rate. Pearlitic cementite fragmented into ultrafine particles of about 100–300 nm size. Warm multiaxial forging process also dispersed the ultrafine cementite particles into the ferrite matrix. Based on the grain boundary characterization and textural evolution, mechanism of ferrite grain refinement is explained. Up to six strain steps, crystallographic slip is the dominant mode of deformation and grain subdivision and recovery is the mechanism for ferrite grain refinement. At nine strain steps, dominant deformation mechanism appears to be grain boundary sliding and random grain rotation. After nine strain steps, initial grains of average 17 μm size reduced to submicron sized grains with the fraction of high angle grain boundaries exceeding 0.7. Double-n behavior is observed during tensile testing of some multiaxially forged steels. Tensile strength and hardness values of multiaxially forged steel increased by more than 100% after eighteen warm multiaxial forging strain steps, whereas ductility reduced by only about 30%.     

Improving resistance to dynamic embrittlement and intergranular oxidation of nickel based superalloys by grain boundary engineering type processing

Abstract

Polycrystalline nickel based superalloys are prone to grain boundary attack by atmospheric oxygen either in the form of time dependent intergranular cracking during dwell time within a low cycle fatigue loading spectrum, known as hold time cracking, or in the form of intercrystalline oxidation at higher temperatures. In the case of hold time cracking of IN718 it has been shown that the crack propagation velocity is determined by local microstructure and environmental conditions, reaching values up to 10 μm s^?1 under four-point bending conditions at 650°C in air. The governing mechanism for this kind of time dependent quasi-brittle intergranular failure has been recognised to be 'dynamic embrittlement', i.e. diffusion of the embrittling element into the elastic stress field ahead of the crack tip, followed by stepwise decohesion. In a very similar way to intercrystalline oxidation, this damage mechanism seems to depend on the local microstructure. Assuming that oxygen grain boundary diffusivity is particularly slow for special coincident site lattice (CSL) grain boundaries, bending and oxidation experiments were carried out using specimens that underwent successive steps of deformation and annealling, i.e. grain boundary engineering. It has been shown that an increase in the fraction of special CSL grain boundaries yields a higher resistance to both intercrystalline oxidation and hold time cracking by dynamic embrittlement.     

Influence of deformation induced ferrite,grain boundary sliding,and dynamic recrystallisation on hot ductility of 0·1–0·75%C steels

Abstract

The influence of C on hot ductility in the temperature range 600–1000°C has been examined for three C contents (0·1, 0·4, and 0·75 wt-%). Using a strain rate of 3 × 10^?3 s^?1, tensile specimens were heated to 1330°C before cooling to the test temperature. For the 0·4%C steel, two further strain rates of 3 × 10^?2 and 3 × 10^?4 s^?1 were examined. At the strain rate of 3 × 10^?3 s^?1, increasing the C content shifted the low ductility trough to lower temperatures in accordance with the trough being controlled by the γ–α transformation. Thin films of the softer deformation induced ferrite formed around the γ grain boundaries and allowed strain concentration to occur. Recovery to higher ductility at high temperatures occurred when these films could no longer form (i.e. above Ae₃) and dynamic recrystallisation was possible. The thin films of deformation induced ferrite suppressed dynamic recrystallisation in these coarse grained steels when tested at low strain rates. Recovery of ductility at the low temperature side of the trough in the 0·1%C steel corresponded to the presence of a large volume fraction of ferrite, this being the more ductile phase. For the 0·4%C steel decreasing the strain rate to 3 × 10^?4 s^?1 resulted in a very wide trough – extended to both higher and lower temperatures compared with the other strain rates. The high temperature extension was due to grain boundary sliding in the γ. Recovery of the ductility only occurred when dynamic recrystallisation was possible and this occurred at high temperatures. At the low temperature end, thin films of deformation induced ferrite were present and recovery did not occur until the temperature was sufficiently low to prevent strain concentration from occurring at the boundaries. Of the two intergranular modes of failure grain boundary sliding produced superior ductility. At the higher strain rates there was less grain boundary sliding, which led to a lower temperature for dynamic recrystallisation. Higher strain rates also increased the rate of work hardening of deformation induced ferrite, reducing the strain concentration at the boundaries. Ductility started to recover immediately below Ae₃, resulting in very narrow troughs. Finally, it was shown that the 2% strain that occurs during the straightening operation in continuous casting is sufficient to form deformation induced ferrite in steel containing 0·1%C.

MST/1809     

Microstructural evolution and mechanical behavior of warm multi-axially forged HSLA steel

Detailed studies are conducted on the microstructural evolution and mechanical behavior of a high strength low alloy (HSLA) steel processed by warm multi-axial forging (MAF). After nine MAF strain steps, the initial ferrite grains of average 13-μm size reduced to submicron-sized grains with over 0.7 fraction of high angle grain boundaries. Pearlitic cementite is fragmented and refined to about 50–100 nm size particles. The microstructure evolution with respect to fraction of HAGB with increase in number of strain steps is more sluggish in HSLA steel as compared to plain carbon steel of comparable carbon content. This is ascribed to the Zener pinning effect of (Ti, Nb) carbide particles. Tensile strength and hardness values of MAFed steel increased by more than 45 and 58 %, respectively, after nine warm MAF strain steps, whereas the fracture strain was reduced from 21 to 12 %.     

ESEM observations of SCC initiation for 4340 high strength steel in distilled water

The stress corrosion cracking (SCC) initiation process for 4340 high strength steel in distilled water at room temperature was studied using a new kind of instrument: an environmental scanning electron microscope (ESEM). It was found that the applied stress accelerated oxide film formation which has an important influence on the subsequent SCC initiation. SCC was observed to initiate in the following circumstances: (1) cracking of a thick oxide film leading to SCC initiation along metal grain boundaries, (2) the initiation of pits initiating SCC in the metal and (3) SCC initiating from the edge of the specimen.All these three SCC initiation circumstances are consistent with the following model which couples SCC initiation with cracking of a surface protective oxide. There is a dynamic interaction between oxide formation, the applied stress, oxide cracking, pitting and the initiation of SCC. An aspect of the dynamic interaction is cracks forming in a protective surface oxide because of the applied stress, exposing to the water bare metal at the oxide crack tip, and oxidation of the bare metal causing crack healing. Oxide crack healing would be competing with the initiation of intergranular SCC if an oxide crack meets the metal surface at a grain boundary. If the intergranular SCC penetration is sufficiently fast along the metal grain boundary, then the crack yaws open preventing healing of the oxide crack. If intergranular SCC penetration is not sufficiently fast, then the oxidation process could produce sufficient oxide to fill both the stress corrosion crack and the oxide crack; in this case there would be initiation of SCC but only limited propagation of SCC. Stress-induced cracks in very thin oxide can induce pits which initiate SCC, and under some conditions such stress induced cracks in a thin oxide can directly initiate SCC.     

Grain boundary engineering: an overview after 25 years

Abstract

In 1984, 'grain boundary design', later known as 'grain boundary engineering (GBE)', was proposed. The central premise of GBE is that specific thermomechanical treatments, mainly on face centred cubic materials which readily form annealing twins, can be used to improve resistance to various forms of intergranular degradation such as corrosion, cracking or embrittlement. Engagement with the concept has accelerated in recent years. This overview charts the progress of GBE from its inception 25 years ago to the present day, including suggestions of key topics for ongoing or future research. These topics comprise confirmation of which boundaries are 'special' in terms of crystallography and properties, optimisation of processing regimes, new approaches to GBE in systems without annealing twinning and incorporation of connectivity metrics, especially in three dimensions.     

X80管线钢焊接接头微观断裂行为的TEM原位观察

为了从微纳米尺度研究管线钢的断裂方式,通过透射电镜原位拉伸方法,从焊缝区和热影响区直接取样,直观测试了X80管线钢在晶粒尺度范围的裂纹生长、扩展等断裂过程和机理.研究表明:在原位拉伸过程中,晶内发射的螺型位错与刃型位错速率之比约为4∶1;晶界裂纹为不连续扩展,而裂纹在晶内沿其DFZ的方向萌生扩展,其扩展是连续的.在加载过程中,裂纹会越过晶界扩展,当裂纹越过大角度晶界时,裂纹扩展方向改变约为30°,扩展方式也会有所变化;当裂纹越过小角度晶界时,裂纹扩展方向不变,扩展方式也不变.     

Effects of grain boundary- and triple junction-character on intergranular fatigue crack nucleation in polycrystalline aluminum

The effects of grain boundary- and triple junction-character on intergranular fatigue crack nucleation were studied in coarse-grained polycrystalline aluminum specimens whose grain boundary microstructures were analyzed by SEM-EBSD/OIM technique. Fatigue crack nucleation occurred mainly along grain boundaries and depended strongly on both the grain boundary character and grain boundary configuration with respect to the persistent slip bands. However, it was little dependent on the geometrical arrangements between the grain boundary plane and the stress axis. Particularly, random boundaries become preferential sites for fatigue crack nucleation. The fatigue cracks were also observed at CSL boundaries when the grain-boundary trace on the specimen surface was parallel to persistent slip bands. On the other hand, no intergranular fatigue cracks were observed at low-angle boundaries. The fatigue cracks were observed at triple junctions as well as grain boundaries. Their nucleation considerably occurred at triple junctions where random boundaries were interconnected. The grain boundary engineering for improvement in fatigue property was discussed on the basis of the results of the structure-dependent intergranular and triple junction fatigue crack nucleation.     

Mechanical fatigue of Sn-rich Pb-free solder alloys

Recent fatigue studies of Sn-rich Pb-free solder alloys are reviewed to provide an overview of the current understanding of cyclic deformation, cyclic softening, fatigue crack initiation, fatigue crack growth, and fatigue life behavior in these alloys. Because of their low melting temperatures, these alloys demonstrated extensive cyclic creep deformation at room temperature. Limited amount of data have shown that the cyclic creep rate is strongly dependent on stress amplitude, peak stress, stress ratio and cyclic frequency. At constant cyclic strain amplitudes, most Sn-rich alloys exhibit cycle-dependent and cyclic softening. The softening is more pronounced at larger strain amplitudes and higher temperatures, and in fine grain structures. Characteristic of these alloys, fatigue cracks tend to initiate at grain and phase boundaries very early in the fatigue life, involving considerable amount of grain boundary cavitation and sliding. The growth of fatigue cracks in these alloys may follow both transgranular and intergranular paths, depending on the stress ratio and frequency of the cyclic loading. At low stress ratios and high frequencies, fatigue crack growth rate correlates well with the range of stress intensities or J-integrals but the time-dependent C* integral provides a better correlation with the crack velocity at high stress ratios and low frequencies. The fatigue life of the alloys is a strong function of the strain amplitude, cyclic frequency, temperature, and microstructure. While a few sets of fatigue life data are available, these data, when analyzed in terms of the Coffin–Mason equation, showed large variations, with the fatigue ductility exponent ranging from −0.43 to −1.14 and the fatigue ductility from 0.04 to 20.9. Several approaches have been suggested to explain the differences in the fatigue life behavior, including revision of the Coffin–Mason analysis and use of alternative fatigue life models.