Grain boundary engineering for improving stress corrosion cracking of 304 stainless steel

Grain boundary engineering (GBE) via low strain tension and annealing was used to enhance the resistance to stress corrosion cracking of a 304 stainless steel. Electron backscattered diffraction (EBSD) analysis exhibited that the GBE steel had a higher fraction of low-∑ coincidence site lattice (CSL) boundaries, larger grain-clusters, longer twin boundary chains, and fewer paths of connected non-twin boundaries with a more zigzag shape. Slow strain rate tests in high-temperature water showed that the GBE steel performed better plasticity, higher tensile strength, and similar yield strength compared to conventional steel. The low fraction of random boundaries in GBE steel resulted in a lower frequency of intergranular crack initiation, and the zigzag paths of non-twin boundaries made the intergranular crack propagation more difficult.     

Twins and twin-related domains in a grain boundary-engineered 304 stainless steel

ABSTRACT

The grain boundary (GB) network of a GB-engineered 304 stainless steel was investigated in three dimensions. The GB-engineered sample had a high proportion of twin-related boundaries (～70%). However, these boundaries were not distributed uniformly, but rather in large-sized twin-related domains (TRDs). All grains within a TRD can be connected by a tree-shaped twin-chain. Any two grains within a TRD have ∑3ⁿ-type misorientation, where the n-value could be determined according to the twin-chain. These results show that the formation of large-sized TRDs is correlated with extensively progressed multiple-twinning processes. A quadruple-junction has three twin-boundaries at most. Furthermore, all observed quadruple-junctions within TRDs have at least one twin-boundary. The common spatial morphologies of twin-boundaries are plane-shape, tunnel-shape and semi-closed tunnel-shape.

This paper is part of a thematic issue on Nuclear Materials.     

Production of nano/ultrafine grained AISI 201L stainless steel through advanced thermo-mechanical treatment

In recent years, great attention has been focused on the development of nanostructured stainless steels to improve their mechanical properties. This work reports the formation of nano/ultrafine grain structure in the AISI 201L stainless steel using advanced thermo-mechanical treatment. The cast specimens were first homogenized and then hot forged to provide a suitable microstructure prior to the treatment. Cold rolling was carried out with the reductions of 10-95% followed by annealing at temperature of 850 °C for 15-1800 s. X-ray diffraction, optical and scanning electron microscopy, and tensile and hardness tests were used to characterize the processed specimens. The results showed that the nanocrystalline austenitic structure with a grain size of about 65 nm was obtained by annealing at 850 °C for 30 s after the cold reduction of 95%. The yield strength, total elongation and hardness of this specimen were measured as 1485 MPa, 33% and 386 Vickers, respectively.     

冷变形对IF钢晶界特征分布及连通性的影响

为了研究冷轧工艺对IF钢显微组织的影响.本文借助电子背散射衍射技术,研究了20%到75%冷轧压下率的IF钢退火后的微观结构、晶界特征分布和晶界连通性.结果表明:随着冷轧压下率的增加,冷轧态晶粒逐渐由等轴状变为纤维状,退火态晶粒逐渐细化并变得均匀,小角晶界的出现频率呈下降趋势;随机晶界的出现频率呈明显上升趋势,且随机晶界占绝对优势;而CSL晶界在冷轧压下率40%以下时,变化较小,40%以上时,含量明显增加.大变形量轧制后的IF钢CSL晶界主要由Σ3晶界组成,而小变形量轧制后主要是Σ3和Σ13b晶界.对于75%压下率,还含有较多的Σ7,Σ9和Σ11等CSL晶界.通过增加冷轧压下率,0-CSL三叉晶界的含量减少,1-CSL三叉晶界的含量增加.因此,通过改变冷轧工艺,可以优化IF钢板的晶界特征分布及连通性.     

Control of precipitation behaviour of Hastelloy-X through grain boundary engineering

Grain boundary engineering (GBE) was employed to control the precipitation behaviour of Hastelloy-X alloy. The precipitate characteristics and thermal stability of grain boundary character distribution (GBCD) were investigated by aging at 850°C. M₆C carbides and µ phases were observed in the matrix and on grain boundaries, respectively. It revealed that the formation of µ phase was closely related to the grain boundary structure. GBCD effectively suppressed the nucleation and coarsening of µ phases on the grain boundaries. Owing to the Mo depletion in the vicinity of random grain boundary, the formation of the precipitates was inhibited on the adjacent grain boundaries. The thermal stability of the GBE-optimised microstructure was confirmed at 850°C for 720?h without significant microstructural degradation.     

Improvement of creep-fatigue life by the modification of carbide characteristics through grain boundary serration in an AISI 304 stainless steel

The modification of carbide characteristics through grain boundary serration and its subsequent effect on the creep-fatigue property at 873 K have been investigated, using an AISI 304 stainless steel. It was found that the grain boundaries are considerably serrated when a specimen is furnace-cooled. The grain boundary serration leads to a change in the carbide characteristics as well as grain boundary configuration, i.e., morphology of carbide from an acute triangular to a planar form and a lowered density. Additionally, an array of carbide particles is changed from a consistent to zigzag pattern, in terms of their preference to one grain to share the coherency. Planar carbides on serrated grain boundaries have a lower interfacial energy than that of triangular carbides on straight grain boundaries. It is suggested that the modification of carbide characteristics through the grain boundary serration has a remarkable influence on the improvement of creep-fatigue resistance.Department of Materials Science and Engineering, Korea Advanced Institute of Science and Technology, 373-1 Kusong-dong, Yusong-gu, Taejon 305-701, South Korea.     

Solving oxygen embrittlement of refractory high-entropy alloy via grain boundary engineering

Refractory high-entropy alloys (RHEAs), particularly NbMoTaW RHEAs, exhibit outstanding softening resistance and thermal stability at ultra-high temperatures, but suffer from room-temperature brittleness, which severely limits their processability and thus practical application. In this study, we successfully achieved large plasticity of >10%, along with high strength of >1750 MPa in the NbMoTaW RHEAs via grain boundary engineering with the addition of either metalloid B or C. It was revealed that the room-temperature brittleness of the as-cast NbMoTaW RHEA originates from the grain-boundary segregation of the oxygen contaminant which weakens grain-boundary cohesion. The doped small-sized metalloids preferentially replace oxygen at grain boundaries and promote stronger electronic interaction with the host metals, which effectively alleviates the grain boundary brittleness and changes the fracture morphology from intergranular fracture to transgranular fracture. Our findings not only shed light on the understanding of the embrittlement mechanism of RHEAs in general, but also offer a useful route for ductilization of brittle HEAs.     

Effect of martensite to austenite reversion on the formation of nano/submicron grained AISI 301 stainless steel

The martensite to austenite reversion behavior of 90% cold rolled AISI 301 stainless steel was investigated in order to refine the grain size. Cold rolled specimens were annealed at 600–900 °C, and subsequently characterized by scanning electron microscopy, X-ray diffraction, Feritscope, and hardness measurements. The effects of annealing parameters on the formation of fully-austenitic nano/submicron grained structure and the mechanisms involved were studied. It was found that annealing at 800 °C for 10 s exhibited the smallest average austenite grain size of 240 ± 60 nm with an almost fully-austenitic structure.     

Effects of aging temperature and grain size on the formation of serrated grain boundaries in an AISI 316 stainless steel

The effects of aging temperature and grain size on the formation of serrated grain boundaries have been investigated in an AISI 316 stainless steel. Grain size increased slightly over aging temperature ranges of 650–870 °C, resulting in predominantly serrated grain boundaries. However, when the temperature exceeded 880 °C, the grain size significantly increased, and grain boundary serration was not observed. The initial grain size also had an influence on the occurrence of grain boundary serration. For specimen having a large initial grain size of about 200 μm, no serrated grain boundary formed after aging treatment at 760 °C. Serrated grain boundaries were observed when “normal” initial grain sizes 55 μm were employed. It was found that the frequency of low angle boundaries markedly increased as the initial grain size increased from 55 to 200 μm. From the results obtained, it is possible to describe that the grain boundary serration could be considered as a spontaneous reaction that aims to reduce the total free energy of the system, and form a new interface of lower free energy. We proposed that the competition between grain growth and grain boundary serration during aging treatment reduces the total free energy of the alloy system: at temperatures exceeding 880 °C, the dominant process is the grain growth, while grain boundary serration predominates over the range of 650–870 °C.     

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。     

Effects of hot-carrier stress on high performance polycrystalline silicon thin film transistor with a single perpendicular grain boundary

This paper is a report on the effect of a single perpendicular grain boundary on the hot-carrier and high current stability in high performance polycrystalline silicon (poly-Si) thin film transistors (TFTs). Under a hot carrier stress condition (Vg = Vth + 1 V, Vd = 12 V), the poly-Si TFT with a single grain boundary is superior to the poly-Si without any grain boundary because of the smaller free carriers available for electric conduction. The shift of transconductance in poly-Si TFT with a single grain boundary is less than 5% after hot carrier stress during a period of 1000 s. The shift of transconductance is about 25% in the case of the poly-Si TFTs without a grain boundary in the channel. On high current stress, the poly-Si TFT without the grain boundary is less degraded than the poly-Si TFT with the grain boundary because the concentrated electric field near the drain junction is lower.     

微量Hf对大角度晶界含Re双晶合金高温持久性能的影响

采用籽晶法制备含有大角度晶界(约20°)的双晶试板,通过分析不同Hf含量(质量分数:0%,0.4%)的含Re合金晶界处析出相、γ/γ′组织、晶界成分及1100℃/100MPa横向持久性能,研究Hf对晶界组织及高温力学性能的影响。结果表明:Hf显著提高了铸态合金大角度晶界处共晶和碳化物体积分数;热处理后,Hf显著抑制了晶界胞状再结晶组织的形成,含Hf合金的1100℃/100MPa横向持久寿命均显著提高。晶界持久性能与晶界析出相种类、形貌、含量和成分密切相关,而Hf元素在晶界未发现显著的偏聚。本研究对先进镍基单晶合金中晶界缺陷的评价及Hf元素晶界强化作用机制的认识具有一定的指导意义。     

Amelioration of weld-crack resistance of the M951 superalloy by engineering grain boundaries

Fusion weld is a portable and economical joining and repairing method of metals.However,weld cracks often occur during the fusion weld of Ni-base superalloys,which hinder the applications of fusion weld on this kind of materials.In this work,the effects of microstructures of grain boundaries(GBs)of the prototype M951 superalloy on its weldability were investigated.The precipitated phases,the elemental segregations on GBs,and the morphologies of GBs can be largely altered by regulating the cooling rates of pre-weld heat treatments.With decreasing the cooling rate,chain-like M23X6 phase precipitates along the GBs,accompanying segregations of B,and GBs becomes more serrated in morphology.During fusion weld,the engineered GBs in the M951 superalloy with a low cooling rate favor the formation of the continuous liquid films on GBs,which together with the serrated GB morphology significantly prevents the formation of weld cracks.Our findings imply that the weld-crack resistance of the superalloys can be ameliorated by engineering GBs.     

Characteristics of the nitrided layer formed on AISI 304 austenitic stainless steel by high temperature nitriding assisted hollow cathode discharge

A series of experiments have been conducted on AISI 304 stainless steel using a hollow cathode discharge assisted plasma nitriding apparatus. Specimens were nitrided at high temperatures (520–560 °C) in order to produce nitrogen expanded austenite phase within a short time. The nitrided specimen was characterized by scanning electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, potentiodynamic polarization and microhardness tester. The corrosion properties of nitrided samples were evaluated using anodic polarization tests in 3.5% NaCl solution. The nitrided layer was shown to consist of nitrogen expanded austenite and possibly a small amount of CrN precipitates and iron nitrides. The results indicated that rapid nitriding assisted hollow cathode discharge not only increased the surface hardness but also improved the corrosion resistance of the untreated substrate.     

Potential energy of two structures of Σ = 110 1 1 tilt grain boundary in silicon and germanium with empirical potentials and tight-binding methods

Two atomic structures A and B of the Σ = 110 1 1 grain boundary were observed in silicon and germanium. We have performed a complete study of the stability of these two grain boundaries using some empirical potentials and also the semiempirical, tight-binding (TB) method. The TB method has confirmed the experimental observations at low temperatures. The A structure is more stable in silicon whereas for germanium the B structure is obtained. The empirical potentials, such as those of Keating (1966), Baraff et al. (1980) and of Stillinger and Weber (1985), give the A structure as the most stable for both germanium and silicon. The non-ability of these empirical potentials to make a difference between germanium and silicon and the advantage of TB method are discussed.     

掺杂(Fe、Nb)SrTiO3晶界组成的电子能量损失谱(EELS)分析

采用高空间分辨率扫描透射电镜（STEM）对掺杂（Fe^3 、Nb^5 ）SrTiO3晶界进行了观察，并利用采集的电子能量损失谱（EELS）对晶界组成进行了分析，结果表明，掺杂Fe的SrTiO3陶瓷晶界存在1nm左右的非晶膜，同晶体内部相比晶界缺Sr；三叉晶界为钛基玻璃相，Ti、O及Fe含量明显高于晶界，掺Nb的SrTiO3陶瓷晶界同晶粒相比同样缺Sr，三叉晶界主要以SiO2非晶相为主，Fe^3 、Nb^5 对Ti^4 的替位及在晶界的偏析引起SrTiO3晶格畸变是导致晶界组成变化的主要原因。     

Improvement of high temperature oxidation resistance of rare earth metal-added Fe–20%Cr–5%Al alloys by pre-annealing treatment

Abstract

Fe–20mass%Cr–5mass%Al alloy foils have recently been used as a catalytic converter substrate for automobiles because of their good oxidation resistance. In this study, the effect of pre-annealing on the oxidation behaviour of Fe–20mass%Cr–5mass%Al alloy foils containing a small amount of La–Zr and La–Hf was examined by a cyclic oxidation test at 1373K in air. The Al₂O₃ scale formed by oxidation was analyzed with a scanning electron microscope (SEM) and transmission electron microscope (TEM) equipped with an energy-dispersive X-ray spectrometer.

The oxidation rate of these alloys was reduced by pre-annealing in a reducing atmosphere. The Al₂O₃ scale which formed on the pre-annealing alloys was characterized by a thinner outer equiaxed grain layer and larger inner columnar grain size than the scale layer which formed on as-cold rolled alloys of the same material.

It is inferred that, with the pre-annealed alloys, the low-density of grain boundaries in the Al₂O₃ limited oxygen diffusion along the Al₂O₃ grain boundaries, resulting in a decreased growth rate of Al₂O₃ scale.