Evolution of microstructure and texture during annealing of two high strength interstitial free steels containing Nb and or Ti

Abstract

Interstitial free steel containing Nb, recrystallised at a slower rate compared to Ti stabilised steel. The coincidence site lattice boundaries of the type Σ3, Σ13b and Σ39a appear to play a major role during the first stage of grain growth in both the Nb + Ti and Ti containing interstitial free steels. They do not seem to have any major role in the development of final texture in these materials. The distribution of grain boundary misorientation angles also changes with annealing time and show two maxima close to the misorientation angles 60° and 20–40°.     

Role of dislocation density and structure in grain boundary segregation of phosphorus and carbon in model Fe-P-C alloy

Abstract

The present study has investigated the effects of dislocation density, produced by tensile prestraining, on the grain boundary segregation of phosphorus and carbon in a Fe-0.06P-0.002C (wt-%) alloy during stress free isothermal annealing at 500°C for periods up to 1800 h. Changes in grain boundary segregation were followed using Auger spectroscopy, while changes in dislocation density and structure were observed using transmission electron microscopy techniques. The segregation of phosphorus (but not carbon) was enhanced, compared with unstrained specimens, during initial aging. Analysis of diffusion rates required to cause the observed increase in phosphorus segregation suggested that the kinetics of phosphorus segregation was enhanced by pipe diffusion. At intermediate aging times, desegregation of phosphorus was observed, an effect attributed to a reduction in intragranular solute levels resulting from phosphorus precipitation on dislocations. In the case of carbon this process continued to the longest aging times examined and, essentially, complete desegregation ensued. In contrast, at these long aging times, phosphorus segregation resumed, and this was associated with an increase in the binding energy of phosphorus to the carbon denuded grain boundary.     

Influence of phosphorus on the hot ductility of 2.25Cr1Mo steel

Abstract

The effect of phosphorus at two levels (0.01 and 0.06 wt-%) on the hot ductility of 2.25Cr1Mo steel has been investigated over the temperature range 700-1200 °C using a Gleeble machine. Auger electron spectroscopy indicated that phosphorus segregation to austenite grain boundaries had occurred in the higher phosphorus steel. A trough in the ductility - temperature curve was observed for both steels with the minimum ductility occurring at about 750 °C. The higher P containing steel gave the worst ductility throughout the temperature range examined. The ductility trough was caused by the formation of a thin pro-eutectoid ferrite layer along austenite grain boundaries, and this trough was accentuated by the presence of phosphorus at the austenite grain boundaries.     

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     

Effect of aging on high temperature brittle intergranular fracture in austenitic stainless steels

Abstract

The present paper describes the effect of aging on crack growth at 550–750°C in a series of 316 and 347 based stainless steels. Crack initiation parameters and crack growth rates have been measured, and detailed fractography and microstructural characterisation carried out. The study shows that the high temperature brittle intergranular fracture mechanism operates in these alloys, as expected from incidences of cracking in austenitic stainless steels used in power plant. High temperature brittle intergranular fracture leads to lower crack tip opening displacements at initiation, and slightly higher crack growth rates than ductile intergranular failure. Susceptibility to high temperature brittle intergranular fracture is enhanced by aging. This increased susceptibility is explained in terms of the increased hardness, the reduction in dissolved C, and grain boundary precipitation. The effects of temperature, composition, and loading mode on the behaviour of the aged alloys are determined.

MST/3100     

Modelling of continuous recrystallization in aluminium alloys

Microstructure and microtexture analyses have been made of three aluminium alloys after annealing alone and after concurrent straining and annealing, and simulative models of microstructure/microtexture evolution processes have been formulated. Both experimental and modelling results are presented as boundary misorientation distributions. For each alloy, the results show that annealing alone does not significantly alter the boundary misorientation distribution, while concurrent straining and annealing (up to a strain of 0.5) decreases the fraction of low-angle boundaries. To understand the mechanisms by which concurrent straining and annealing alter the boundary misorientation distribution, three simulative models of microstructure/microtexture evolution during concurrent straining and annealing have been formulated. Application of the models to experimentally determined initial microstructure/microtexture states shows that the boundary sliding (sub)grain rotation model decreases the fraction of low-angle boundaries, the dislocation glide (sub)grain rotation model increases the fraction of low-angle boundaries, and the (sub)grain neighbour switching model has a modest effect on the boundary misorientation distribution. A combination of the boundary sliding (sub)grain rotation model and the (sub)grain neighbour switching model most closely reproduces the boundary misorientation distributions found experimentally.     

Grain boundary and fracture surface analysis of Fe–C–P steel

Abstract

The present paper investigates the distribution of grain boundary types and fracture surface crystallography in an Fe–C–P alloy. It is shown that electron backscatter diffraction (EBSD) is an effective technique with which to conduct these investigations. The proportions of both Σ1 and particularly Σ3 (in coincidence site lattice notation)present after various heat treatments were higher than would have been expected for random generation. There was limited evidence that both higher annealing temperatures and longer annealing times promoted generation of Σ3 type boundaries. The standard EBSD technique was modified and extended to encompass both the novel ‘matched fracture’ specimen approach and direct mapping from fracture surfaces to provide crystallographic information. A correlation was noted between higher aging temperatures and proportions of cleavage fracture. Furthermore, there was a strong correlation between cleavage fracture surfaces exhibiting river markings and an {001} surface orientation.     

Isothermal embrittlement of Fe–8Mn alloys at 450°C

Abstract

Two Fe–8Mn alloys, one of which is alloy 193, stabilised with 0·17%Ti and 0·18%Al, were austenitised at 900°C, ice brine quenched and their DBTTs determined. In this condition, brittle fractures were predominantly cleavage, and thermodynamic calculations on alloy 193 showed that there were 0·0025 wt-%C and <0·03 ppm N in solid solution. Alloys were tempered for 6 min, 1 h and 10 h at 450°C and their DBTTs again determined; in this case, brittle fractures were mainly intergranular. In alloy 193, DBTT rose from 27 to 125°C in 6 min. Hardness values at 450°C were also monitored and the variation of hardness with time is discussed. It is thought that brittle fracture in alloy 193 is due to segregation of Mn per se to prior austenite grain boundaries, unlike an earlier investigation of a pure Fe–8Mn alloy (K1525), where embrittlement was due to a Mn–N and to a lesser extent a Mn–P interaction at prior austenite grain boundaries. The driving force for Mn segregation to prior austenite grain boundaries is thought to be the initial formation of reverted austenite at such sites.     

Stability of ZrO2–Y2O3 t′ phase formed during laser sealing

Abstract

Results are reported concerning the effect of thermal treatments in the temperature range 1050–1500°C for 1–1000 h on the stability of the t′ phase present in laser sealed layers of ZrO₂–8·5 wt-% Y₂O₃. Aging for up to 1000 h at 1050°C is not sufficient to cause significant transformation of the t′ phase. At temperatures >1300°C, the t′ phase is less stable and transforms to mixtures of the t and c phases in proportions which are a function of both the time and temperature of aging. An improvement in the fracture toughness of the sealed layer was found to occur when substantial proportions of t phase were produced by annealing.

MST/1529     

The role of active elements in Fe-Cr-Al alloys for heating element applications

The role of active elements (zirconium, cerium and yttrium) in grain growth and its subsequent effect on room-temperature tensile fracture behaviour of Fe-Cr-Al alloys has been investigated. The alloys containing active elements exhibited improved resistance to grain growth. Yttrium-containing alloy retained higher room-temperature tensile ductility even after heating at higher temperatures because of its superior resistance to grain coarsening. All the alloys, with and without active elements, exhibited a sudden drop in room-temperature tensile ductility, with concommitant change in fracture mode from dimple rupture to cleavage, in a narrow band of 39–44μm grain size. The ductile-brittle transition temperatures (DBTT) of these alloys were found to be 150°C and 215°C for grain sizes 25μm and 100μm respectively. The accelerated life test showed that the alloys containing active elements exhibited longer lives.     

Effect of annealing on tensile properties of electrodeposited nanocrystalline Ni with broad grain size distribution

Abstract

The microstructures and tensile properties of electrodeposited nanocrystalline Ni (nc-Ni) with a broad grain size distribution after annealing at 150, 200 and 300°C for 500 s were investigated. The as deposited broad grain size distribution nc-Ni sample exhibited a moderate strength σ_UTS of ～1107 MPa but a markedly enhanced ductility ?_TEF of ～10%, compared with electrodeposited nc-Ni with a narrow grain size distribution. Annealing below 200°C increased the strength but caused a considerably reduction in tensile elongation. This behaviour is attributed to the grain boundary relaxation and the increased order of grain boundaries after annealing, which can make the grain boundary activities, such as the grain boundary sliding and grain rotations, more difficult. Further annealing at 300°C decreased both the yield strength and tensile elongation significantly due to significant grain growth.     

Kinetics of grain growth in 0·1 at.-%B doped nickel aluminide containing 23·2 at.-%Al

Abstract

Nickel aluminide containing 23·2 at.-%Al and 0·1 at.-%B was cold rolled and fully recrystallised at 825, 850, 875, 900, 925, 975, and 1000°C. Increase in grain size as a function of isothermal annealing time at these temperatures was measured. All the data showed excellent fit with the developed equations. The value of m, the exponent of the grain growth equation (D^m - D^m₀ = Kt), was 2·5. The activation energy for grain growth was 263 kJ g-atom^-1. Small changes in the boron content had an appreciable effect on the kinetic parameters. This was attributed to the solute drag effect of boron.     

High speed rolling of Mg–3Al–1Zn alloy: texture and microstructure analysis

Abstract

High speed rolling (HSR) of 1000 m min^?1 was employed to successfully roll AZ31 alloy in one pass with 65% reduction in thickness at 300 and 450°C. The rollability, texture and microstructure after HSR, in comparison with low speed rolling (15 m min^?1), improved significantly. It is suggested that the double peak and weaker basal texture obtained after HSR are attributed to the activation of compression and double twins. After annealing, the double peak basal texture is replaced by a single peak one, which may be due to preferential grain growth of basal grains.     

Effects of Al content on the high-temperature mechanical properties of Al-TRIP steel

ABSTRACT

As-cast transformation-induced plasticity (TRIP) steels with two different aluminium contents (2.80 and 6.75?wt-%) were subjected to investigate the effect of aluminium content on the tensile strength and hot ductility. As the Al content increases from 2.80 to 6.75?wt-%, the third brittle zone of the steel is shifted from 950–750°C to 800–750°C. The 6.75?wt-% Al-TRIP steel is a typical δ-TRIP steel that contains 44.5 wt-% δ-ferrite compared with no δ-ferrite in the 2.80?wt-% Al-TRIP steel. The solidification behaviour of these two types of TRIP steel was compared by calculating equilibrium phase diagrams. The 6.75?wt-% Al-TRIP steel was found to have better ductility than the 2.80?wt-% Al-TRIP steel below 1100°C.     

Correlation between grain boundary misorientation and M23C6 precipitation behaviors in a wrought Ni-based superalloy

The correlation between the grain boundary misorientation and the precipitation behaviors of intergranular M₂₃C₆ carbides in a wrought Ni–Cr–W superalloy was investigated by using the electron backscattered diffraction (EBSD) technique. It was observed that the grain boundaries with a misorientation angle less than 20°, as well as all coincidence site lattice (CSL) boundaries, are immune to precipitation of the M₂₃C₆ carbides; in contrast, the random high-angle grain boundaries with a misorientation angle of 20°–40° provide preferential precipitation sites of the M₂₃C₆ carbides at the random high-angle grain boundaries with a higher misorientation angle of 55°–60°/[2 2 3] turn to retard precipitation of M₂₃C₆ carbides owing to their nature like the Σ3 grain boundaries and retard the precipitation of M₂₃C₆ carbides. The low-angle and certain random grain boundary segments induced by twins were found to interrupt the precipitation of the M₂₃C₆ carbides along the high-angle grain boundaries.     

Effect of phosphorus on stability of cold worked structure in 316Ti austenitic stainless steel

Abstract

The persistence of the effects of prior cold work through subsequent annealing treatment has been investigated by examining the changes in 0·2%yield strength and the microstructural evolution in phosphorus free and phosphorus containing type 316Ti stainless steels with various amounts of mechanical pretreatment. The results showed no specific influence of phosphorus on changes to a cold worked structure during short term treatment carried out in the range 800–1200°C where no second phase precipitation was observed. However, when second phase precipitation did occur the behaviour of the alloys examined was found to be slightly different. For long term annealing in the 600–800°C temperature range an abundant nucleation of fine carbides particles, particularly in the phosphorus containing steel, considerably improved the stability of the cold worked structure by decorating grain boundaries and by pinning the dislocations and, consequently, impeding their climb. This study has highlighted clearly the existence of an optimum annealing temperature for a given level of cold work and that there is an optimum amount of initial deformation for a given annealing temperature. The addition of phosphorus has been shown to result in an increase of strength in type 316Ti with perhaps an insignificant drop in ductility, although a full explanation of how the presence of phosphorus affects the recrystallisation process in a prestrained 316Ti type steel remains to be ascertained.     

Effects of phosphorus on creep behaviour of nickel and Ni–20Cr and on creep and strength of Nimonic 80A

Abstract

The influence of P on the creep behaviour of Ni, Ni–20Cr (wt-%), and Nimonic 80A was investigated by carrying out creep tests under various loads and at different temperatures. After creep fracture the samples were investigated using optical, scanning electron, and transmission electron microscopy. The grain boundary segregation was examined using Auger electron spectroscopy (AES). It was found that P segregates to the grain boundaries in all the materials investigated. The creep rate of Ni–20Cr and Nimonic 80A is decreased by the addition of P. Grain boundary segregation of P and its influence on strength was also investigated using AES for specimens aged between 600 and 700°C after fracture by a tensile test inside an ultrahigh vacuum chamber. Maxima of tensile strength are observed to be time dependent as a result of carbide precipitation, which is affected by the P segregation.

MST/1679     

Ductility and fracture of copper bicrystals with boundary SiO2 particles

Abstract

High temperature deformation andfracture ofCu-SiO₂ bicrystals with [001] twist boundaries of various misorientation angles were investigated under the condition of non-activation of grain boundary sliding. As the misorientation angle increases, the bicrystals became more susceptible to intergranular brittle fracture. Clear intermediate temperature embrittlement was observed in bicrystals with a random high angle boundary. The boundary segregation of O atoms was found to enhance intergranular fracture. Although the boundary SiO₂ particles provide stress concentration sites which cause early formation of boundary cavities, the boundary dependent deformation and fracture behaviour is essentially determined by inherent boundary strength, which is afunction of the misorientation angle.

MST/1969     

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     

Phase separation reactions in Ti–50V alloys

Abstract

Phase transformations in Ti–50V alloys containing oxygen in the range <0·095–0·36 wt-% have been studied at 750 and 400°C for times up to 1000 h. Results of electron microscopy, X-ray diffraction, and hardness testing indicate that oxygen widens the α+β phase field at 750°C and the metastable β phase miscibility gap at 400°C. The evidence is consistent with a phase diagram for high purity Ti–V alloys containing a stable α+β phase field with a β transus decreasing with increasing vanadium content. No evidence was obtained consistent with a β monotectoid form of diagram which has recently been proposed.

MST/1039