Grain boundary crystallography in two Fe-C-P alloys

Abstract

Misorientation, grain growth and brittle fracture were investigated in two iron - carbon alloys containing 0.06 wt-% phosphorus (0.06P) and 0.12 wt-% phosphorus (0.12P) after selected heat treatment schedules. A 'fracture surface serial sectioning' technique was devised and combined with misorientation measurements to reconstruct specimens after fracture. Anomalous grain growth occurred in the 0.06P specimen only, after 1000°C annealing. This was attributed to the inhomogeneous distribution of phosphorus at the interfaces. No evidence was found for the direct influence of misorientation angle distributions or coincidence site lattice distributions on anomalous grain growth. The proportion of Σ3s increased greatly after annealing at 1000°C, attributed to the twinning that developed in the austenite range. There was strong evidence that Σ3s were in general more resistant to brittle fracture than were random boundaries. It is suggested that alloys of this type could be 'grain boundary engineered' to improve fracture resistance.     

Segregation at the {013} symmetrical tilt grain boundary in dilute Fe-Si alloy bicrystals

The structure and segregation behaviour of the {013} symmetrical tilt grain boundary were studied in Fe-Si dilute alloy bicrystals. Structural features such as twins, cleavage tongues and steps at the grain boundary, revealed by brittle intercrystalline fracture, are described and the identity of the fracture surface with the grain boundary is discussed. The amounts of segregation of phosphorus and silicon obtained by Auger electron spectroscopy are correlated with the structure of the analysed regions. The scatter of measured values of concentration of phosphorus and silicon in different regions of the fracture surface is explained from a structural point of view. A repulsive interaction between phosphorus and silicon atoms was confirmed. Grain-boundary enrichment ratios for phosphorus of 185 and 278, and decreases of the silicon concentration to 63 and 60% of the bulk value, were found at the grain boundary in as-grown and annealed bicrystals, respectively.     

Influence of precipitation and segregation on hydrogen embrittlement in aged 9Cr–1Mo steel

Abstract

A study is reported of temper embrittlement and hydrogen embrittlement in a series of model 9Cr–1Mo steel alloys in which the levels of silicon and phosphorus have been varied to separate the formation of the brittle intermetallic (Laves) phase from the segregation of phosphorus during aging. Phosphorus segregation was mildly detrimental to ductility properties, Laves phase formation was more detrimental, and their effects combined produced the most severe loss in ductility. Hydrogen effects were additive to those of aging. In unaged material without silicon enrichment, only M₂₃C₆ precipitates were detected, with little phosphorus segregation. With silicon enrichment, phosphorus segregation to lath and grain boundaries was enhanced. This enhancement increased the susceptibility of the materials to hydrogen embrittlement, promoting transgranular cleavage and chisel fracture. In aged material, the high phosphorus alloys showed some grain boundary segregation, but only limited interaction with hydrogen. In the high silicon alloys, the formation of Laves phase was most evident. This enhanced hydrogen embrittlement resulted in extensive chisel, transgranular cleavage, and some intergranular fracture. In the high silicon high phosphorus alloy, both Laves phase formation and phosphorus segregation were evident. This resulted in enhanced susceptibility to hydrogen embrittlement, producing intergranular fracture. Thus, silicon controls the susceptibility to hydrogen embrittlement in unaged alloy by promoting phosphorus segregation and in aged alloy by promoting Laves phase formation. In the aged alloy, segregation of phosphorus can enhance the effect of silicon.

MST/1785     

The mechanism of elevated temperature intergranular cracking in heat-resistant alloys

Reheat or stress relief cracking phenomena have been reassessed in 2.25Cr1.5W heat-resistant alloys. During rupture test, time to intergranular failure increases with decreasing temperature and tensile stress and is shorter in the alloy containing a higher bulk content of phosphorus. Also the time to intergranular failure can be expressed by t = t₀·σ⁻ⁿ·exp(Q/RT) where t₀ is the proportional constant, n the stress exponent and Q the activation enthalpy. Matrix softening is accelerated under tensile stress and an active carbide growth occurs at grain boundaries oriented normal to the tensile stress direction. Because impurities segregate actively to dimples frequently observed at reheat intergranular fracture surfaces, the dimples are not micro-ductile fracture areas but the grain boundary carbide interfaces. The segregation concentration of the impurities is much higher at the grain boundary carbide interfaces than the carbide-free grain boundaries. The phosphorus segregation at the carbide interfaces of the alloy containing the higher bulk content of phosphorus is mainly replaced by the segregation of nitrogen, tin and tellurium in the alloy containing a lower bulk content of phosphorus. The elevated temperature intergranular cracking under tensile stress occurs finally due to the carbide-free grain boundary cracking following the decohesion of the grain boundary carbide interfaces.     

Influence of vanadium on grain boundary segregation of phosphorus in iron and iron-carbon alloys

The influence of vanadium on grain boundary segregation of phosphorus has been studied in iron and iron-carbon alloys by means of fracture experiments in a scanning Auger microprobe. The emphasis here is to study the effects of vanadium on the interaction processes operative under circumstances when structure in the interior of the grain (in the present case carbide formation) and grain boundary segregation form simultaneously. It is emphasized that to predict and analyse the behaviour of an alloy, it is important to consider atomic interactions both at the grain boundaries and in the grain interior and that between the constituents and the grain boundaries. The study suggests that the principal determining factor in the scavenging or retardation of migration of phosphorus to the grain boundaries is whether vanadium is present in the combined form (say, carbide) or is available in solid solution form. When vanadium is present in solid solution form, grain boundary segregation of phosphorus is low because of the chemical interaction of vanadium and phosphorus. However, as carbon is increasingly introduced in the alloy, vanadium now preferentially reacts with carbon in view of higher interaction for carbon as compared to phosphorus. A consequence of this is the increase in the grain boundary concentration of phosphorus. In such a situation the presence of excess carbon in addition to what is stoichiometrically required to precipitate the entire vanadium as vanadium carbides, serves as a palliative with regard to the reduction in the intergranular concentration of phosphorus. This palliative behaviour is explained in terms of the sitecompetition model. An effort is also made to examine the behaviour of segregating elements in terms of whole range of probable interactions (both at the grain boundaries and in the grain interior) and chemical interaction energies.     

Bruchgefüge des Stahles 100 Cr 6 in Abhängigkeit von der Austenitisierungsbehandlung im Durchstrahlungs- und Raster-Elektronenmikroskop untersucht

The appearance of fracture of steel 100 Cr 6 as a function of the austenitization treatment is examined by means of electron microscopes In a steel 100 Cr 6 was carried out the austenitization with temperatures between 860 °C and 1000 °C. The structure resulting from the heat treatment was examined in the light microscope, the area of fracture, in the electron microskope. The areas of fracture of several test pieces were etched for better visualization of the grain boundary. The area of fracture resulting from the grain size and the distribution of the separated particles is discussed. It is pointed out that the area of fracture is a function of the grain size as well as of the separated particles at the grain boundary.     

Effect of Grain Size on the Spall Fracture Behaviour of Pure Copper under Plate‐Impact Loading

The effects of grain size on the spall response were investigated for high purity copper materials by plate‐impact experiments including real‐time measurements of the free surface velocity profiles as well as post‐impact fractography studies on the soft‐recovered samples. High purity copper plates were cold rolled and heat treated to produce recrystallized samples with average grain sizes of 78, 273 and 400 μm, respectively. The spall strength estimated from the free surface velocity profile is nearly constant with no significant effect on the grain size. However, differences are observed in the acceleration rate of velocity rebound beyond the minima. This may be attributed to the effect of grain size on the growth rate of damage. Metallographic analyses of the fracture surface show that the characteristic feature of the fracture surface clearly depends on the grain size. In the 78‐ and 273‐μm samples, the fracture surfaces are decorated with large, high‐density ductile dimples suggesting that the preferential failure mode is ductile intergranular fracture. In the 400‐μm samples, the fracture surfaces have a rock candy appearance with small, high density brittle dimples as well as large ductile dimples suggesting that the fracture mode is a mix of both brittle intergranular fracture and ductile transgranular fracture.     

The effect of grain size and composition on the fracture toughness of Ti–Al–Nb alloys undergoing stress-induced martensitic transformation

The effect of grain size and composition on the fracture toughness of Ti–Al–Nb alloys in β solution-treated condition was investigated. The fracture toughness of the alloys was found to increase with an increase in grain size initially, reach a maximum and subsequently decrease with further increase in grain size. This trend was attributed primarily to the effect of grain size on the enhancement of fracture toughness due to stress-induced martensitic transformation (SIMT) at the crack tip, which in turn can be related to the effect of grain size on trigger stress for SIMT. Alloys containing higher Al and Nb showed a higher toughness for the same grain size, which was also explained in terms of effect of composition on the trigger stress.     

Influence of swaging on hydrogen charged tensile fracture of a 12 wt-%Cr steel

Abstract

The 12 wt-%Cr secondary hardening steel considered in this work is being evaluated for use in the first wall of fusion reactors. As the service temperature can approach 500°C, the microstructure of greatest interest has been a quenched and tempered structure obtained by tempering at 750°C after air cooling from the austenitizing temperature of 1050°C. This structure is susceptible to grain boundary failure whether internal hydrogen has been introduced by cathodic charging or not. In the uncharged condition failure is ductile, but follows prior austenite grain boundaries. Hydrogen charging results in a severe loss of ductility, and tensile fractures which are 30% brittle intergranular. This susceptibility to grain boundary fracture has been attributed both to phosphorus segregation to these grain boundaries and to a nearly continuous array of grain boundary carbides. This tendency for grain boundary fracture can be eliminated and the embrittlement associated with the introduction of internal hydrogen greatly reduced by swaging and subsequently retempering the quenched, and tempered microstructure. The improved properties of the swaged and retempered conditions are attributed to the effects of swaging on the prior austenite grain boundary structure and the orientation of the grain boundaries with respect to the tensile axis.

MST/376     

Non-equilibrium grain-boundary segregation of phosphorus in an Ni-Cr steel

In order to confirm the segregation characteristic of phosphorus in Ni-Cr steel at grain boundary, a grain boundary segregation kinetic curve of phosphorus is obtained using Auger electron spectroscopy. The results show that a peak concentration of phosphorus appears at about 60 min during isothermal ageing at 600 °C after quenching from 1000 °C. The boundary concentration of phosphorus decreases with decreasing (increasing) ageing time, when the ageing time is shorter (longer) than 60 min. These results are analyzed by the model of non-equilibrium grain boundary segregation, indicating that this peak is corresponding to the critical time for phosphorus non-equilibrium grain boundary segregation.     

Untersuchungen zur Festigkeit von Schrauben aus ultrafeinkörnigem und konventionellem Aluminiumwerkstoff EN AW‐7075

Investigation into strength of bolts made of ultra fine grain as well as coarse grain aluminium material AA7075 Results of investigation into strength and fracture behaviour with high level mean load of rolled 7075‐aluminiumbolts M6 are given. Bolts made of coarse grain as well as ultra fine grain structure produced by Equal Channel Angular Extrusion (ECAE) were tested. The ultimate tensile strength for both grain sizes was of a similar level. As a result of the first fatigue tests it seems that the fatigue strength of the ultra fine grain material is lower that the fatigue strength of the coarse grain material. An endurance limit of 23 MPa was found for the bolts made of coarse grain material using a modified staircase method. Furthermore, fracture behaviour of aluminium bolts is discussed.     

Temper embrittlement of hot work die steel

Abstract

The influence of the parameters of an additional tempering at 600°C on temper embrittlement in quenched and previously double tempered 5 wt-%Cr tool steel having a post-martensitic microstructure was investigated. A detailed examination of associated changes of fracture mechanism, microstructure, and precipitate was carried out. The dominant factor controlling the evolution of brittleness was the segregation of phosphorus to prior grain and lath boundaries as well as to martensite lath/carbide interfaces. The segregation effect of phosphorus at these interfaces was accompanied by cosegregation of sulphur and silicon together with simultaneous carbide precipitation.

MST/1132     

Einfluß der Korngröße auf Reibung und Gleitverschleiß von TZP?ZrO2-Keramik bei Festkörper- und Mischreibung

Effect of grain size on friction and wear of TZP? ZrO₂ ceramic in unlubricated and boundary lubricated sliding contact . Microstructures with systematically between 0.30 and 1.62 μm varying average grain sizes were produced by cold isostatically pressing and sintering of commercial 3 mol.% Y₂O₃ stabilized ZrO₂ powder. Hardness and fracture toughness of the different structures as well as the amount of tetragonal, cubic and monoclinic phases were measured. Wear tests were carried out on the different self-mated microstructures in unlubricated and oil or water lubricated unidirectional and unlubricated reciprocating sliding contact, respectively. Worn surfaces were systematically analysed using scanning electron microscopy. The experimental results showed a significant influence of the average grain size as well on mechanical properties such as hardness and fracture toughness as on tribological properties. Friction and wear are discussed in relation to grain size and phase stability of the microstructures and also as a function of the different tribosystems and lubricants used.     

800MPa级别钢熔敷金属热处理脆化机理研究

用于制造船体结构的10Ni5CrMoV钢,为了消除焊接残余应力,在焊后需对其焊接接头进行热处理。试验采用纯氩气体保护焊接10Ni5CrMoV钢,焊后热处理后发现其熔敷金属-50℃冲击韧性大幅下降。利用扫描电镜(SEM)、透射电镜(TEM)和俄歇电子能谱分析方法(AES)对熔敷金属热处理前后的组织和冲击断口进行分析,找出其冲击韧性下降的原因。试验结果表明:10Ni5CrMoV钢熔敷金属热处理后由于回复作用板条状组织变粗或消失,在晶界磷元素的偏聚和大量的碳化物在晶界析出导致其冲击韧性下降。     

Brittle fracture of polycrystalline tungsten

A comparative study of the brittle fracture of three varieties of polycrystalline tungsten has been carried out using mainly impact tests, scanning electron microscopy and Auger spectroscopy. It indicates the occurrence of two modes of brittle fracture, namely cleavage and intergranular fractures, whose proportions depend on temperature and on phosphorus segregation at the grain boundaries. Scanning Auger images indicate unambiguously that phosphorus is only located on the intergranular surfaces. No phosphorus is observed on cleavage planes. Fracture surfaces are the result of the propagation of a crack through the whole sample. As the propagation follows the path which requires the lowest expenditure of energy, it depends both on a geometrical factor and on the respective values of the cleavage (_cl) and intergranular (_l) works of fracture. Our results indicate an increase in _cl and _l with temperature (the effect being more marked in the case of _cl) and a large decrease in _l with phosphorus segregation at the grain boundaries. This impurity produces an intergranular embrittlement of the tungsten.     

Stress-induced non-equilibrium grain boundary segregation of phosphorus in a Cr–Mo low alloy steel

Grain boundary segregation of phosphorus under a 40 MPa tensile stress at 520 °C in a 0.025 wt.% P-doped 2.25Cr1Mo steel, which has already been thermally equilibrated, is examined using Auger electron spectroscopy. The segregation of phosphorus during stress-ageing has a non-equilibrium characteristic, i.e. it is non-equilibrium segregation. The segregation level first increases with increasing stress-ageing time until about 0.5 h and then diminishes with further increasing stress-ageing time, leading the boundary concentration of phosphorus to return to its thermal equilibrium value after ageing for about 15 h. Therefore, the critical time for this non-equilibrium grain boundary segregation of phosphorus is about 0.5 h at which the segregation is peaked. At this critical time, the boundary concentration of phosphorus is about 20.5 at.%, which is about 4.5 at.% higher than its thermal equilibrium level. Xu's kinetic model for stress-induced grain boundary segregation [T.D. Xu, Philos. Mag. 83 (2003) 889–899; T.D. Xu, B.-Y. Cheng, Prog. Mater. Sci. 49 (2) (2004) 109–208] is used to analyse the experimental results, demonstrating that the measured data may be well simulated by the model.     

Zur Zähigkeit von Vergütungsstählen

On Toughness of Quenched and Tempered Steels Toughness as consumed fracture energy is dependent on fracture mechanism. Grain size and loading conditions influence the transition from ductile dimple fracture to brittle cleavage fracture. In quenched and tempered steels packet size and particle distribution are of importance as well as brittle intergranular fracture modes by grain boundary segregation of impurities in ferrite (temper embrittlement) or precipitates in austenite. Anisotropy of toughness arises from banded structures.     

THE BRITTLE FRACTURE OF 475°C EMBRITTLED CAST DUPLEX STAINLESS STEEL

Abstract— The fracture behaviour of cast duplex stainless steels, heat treated to different ferrite contents and hardness was investigated using tensile and notched bend tests. The purpose was to identify the microstructural features which controlled the ductile-to-brittle fracture transition of 475°C embrittled duplex stainless steel. The results indicate that twin nucleated cleavage has a tensile stress fracture criteria and the brittle-to-ductile transition temperature depends on ferrite microhardness, ferrite grain size and constraint.     

THE EFFECT OF HYDROGEN ON FATIGUE AND DISLOCATION BEHAVIOR OF AN α/β TITANIUM ALLOY

Abstract— Fatigue thresholds and crack growth rates were studied in the experimental alloy, Ti—5Al—4Mo, as a function of temperature, grain size and hydrogen concentration. Deformation is confined to planar slip bands along which fracture occurred at low hydrogen concentrations. Hydrogen accelerated crack growth rates at various combinations of temperature, grain size and hydrogen with a corresponding change in fracture from "cleavage' to interface phase fracture. In addition, hydrogen was found to promote interface phase formation. It is proposed that stress-assisted hydrogen accumulation increases the interface phase hydrogen concentration which reduces the interface phase fracture stress. This process depends on the local stress and β -phase hydrogen concentrations, temperature and the time under load. At 340 K, hydrogen had a relatively small effect on crack growth due to a change in slip behavior with increased hydrogen concentration.     

Effect of beta flecks on mechanical properties of Ti–10V–2Fe–3Al alloy

The effects of beta flecks on tensile properties and low-cycle fatigue life were investigated at room temperature for Ti–10V–2Fe–3Al alloy. It was found that beta flecks had a significant influence on tensile ductility and low-cycle fatigue life. The greater the volume fraction of beta flecks (P_A) or maximum area of beta flecks (S_max), the lower the tensile ductility and low-cycle fatigue life. Extensive scanning electron microscopy (SEM) and light microscopy (LM) observation showed that under tensile load, cracks preferentially nucleated at β grain boundaries of beta flecks, then grew, connected and propagated along grain boundaries to form characteristics of intergranular fracture and quasi-cleavage fracture. While under an alternating load, beta flecks acted as sites for low-cycle fatigue crack nucleation due to inhomogeneous alternating strains between soft GB and aged beta matrix. The presence of beta flecks accelerates both the crack nucleation and early crack propagation.