Crystallographic features of intergranular crack initiation in fatigued copper polycrystals

In order to study the mechanism of grain boundary (GB) cracking in fatigued polycrystalline copper, specimens were fatigued in symmetrical push-pull at an intermediate constant plastic strain range at room temperature in dry air. The intergranular cracks were examined under the scanning electron microscope. Many GB cracks were found to have been formed by the impingement of persistent slip bands (PSBs) against the grain boundaries (PSB-GB cracks). The orientations of the grains adjacent to the cracks were determined by electron back-scattering patterns. The misorientations of the cracked boundaries were calculated and the boundary plane orientations were also determined. High-energy grain boundaries were found to be preferred sites for cracking. The activated slip systems in the component grains adjacent to the cracks were determined and analyzed. With these data, the cracking stresses due to the interaction between the PSBs and the boundaries were calculated for the observed PSB-GB cracks in a pile-up type dislocation model in a three-dimensional analysis. The results confirmed that, with reasonable assumptions, the estimated minimum theoretical shear stresses which are required to act in the PSBs for causing PSB-GB cracks were always smaller than the real shear stresses operating in the PSBs.     

电子束悬浮熔炼钼铼合金铸锭的热加工方法

电子束悬浮熔炼钼铼合金铸锭晶粒粗大,致使热加工性能变差,锻造过程出现开裂,文章分析了锻造过程材料的受力状态,认为是垂直晶界的拉应力导致沿晶开裂,据此提出了热轧开坯的工艺方法,且规定第1道次平行铸锭轴向喂料,轧制过程中材料产生剪切滑移变形,滑移面与晶界成一定夹角,不产生垂直晶界的拉应力,避免了拉应力作用下的沿晶开裂,获得优质热轧板。     

Role of Localized Deformation in Irradiation-Assisted Stress Corrosion Cracking Initiation

Intergranular cracking of irradiated austenitic alloys depended on localized grain boundary stress and deformation in both high-temperature aqueous and argon environments. Tensile specimens were irradiated with protons to doses of 1 to 7 dpa and then strained in high-temperature argon, simulated boiling water reactor normal water chemistry, and supercritical water environments. Quantitative measurements confirmed that the initiation of intergranular cracks was promoted by (1) the formation of coarse dislocation channels, (2) discontinuous slip across grain boundaries, (3) a high inclination of the grain boundary to the tensile axis, and (4) low-deformation propensity of grains as characterized by their Schmid and Taylor factors. The first two correlations, as well as the formation of intergranular cracks at the precise locations of dislocation channel–grain boundary intersections are evidence that localized deformation drives crack initiation. The latter two correlations are evidence that intergranular cracking is promoted at grain boundaries experiencing elevated levels of normal stress.     

The initiation of intergranular failure in inconel-600

The nature of slip interaction with the grain boundaries was examined on the polished surface of Inconel-600 pulled in tension at 370°C and at the initial strain rate of 1.65 × 10^?6 sec^?1. It was shown that the grain boundaries could not always accommodate slip taking place at the boundary regions. This led to the separation of grains at the boundary. Depending on the detailed morphology of the carbides, these intergranular cracks could form at axial strains as low as 10 pet. Since the cracking takes place in the inert atmosphere, it is concluded that the grain boundaries are inherently embrittled by the formation of carbides and/or by solute segregation. There was no evidence of grain boundary sliding, but when carbides were absent highly localized slip in the boundary region gave the appearance of grain boundary offsets. The implications of these observations to stress corrosion cracking are discussed.     

The fatigue of pseudoelastic polycrystalline β-cuznsn

The fatigue of polycrystalline pseudoelastic β-CuZnSn has been studied by cycling specimens to fixed stress. The fatigue life was found to decrease with increasing initial strain and decreasing specimen grain size. In both cases the results gave similar stress -vs - fatigue life curves, indicating that stress is the primary parameter controlling fatigue life. The results fitted a curve of the form △ε.N^B _f = constant, whereβ = 0.32 for the total initial strain, andβ = 0.29 for the initial elastic strain. The fatigue life appeared to be independent of strain rate. Fatigue cracks nucleated in the first cycle at three grain intersections and grew along grain boundaries until adjacent cracks linked up. In the later stages of crack growth, some intergranular cracking occurred when there were no suitably oriented grain boundaries. Both the intergranular and transgranular regions showed somewhat ill-defined fatigue striations.     

Surface deformation and crack initiation during fatigue of vacuum melted iron: Environmental effects

Samples of vacuum melted commercially pure iron were fatigued in the reverse bending mode in different environments including ultrahigh vacuum, oxygen, water vapor, and their combinations. Reverse bending alternating stress in ultrahigh vacuum produced a rumpled surface (without any prominent slip lines) with cracks initiated along grain boundaries. In the presence of oxygen, such fatigue generated well-developed slip lines. Fatigue cracks were observed more along slip lines than grain boundaries. When the same sample was fatigued in both ultrahigh vacuum and oxygen in succession, the resulting surface structure was dependent on the order in which two environments were employed. In water vapor, there was a reduction in surface deformation at low pressures (~ 1 x 10^-4 torr (1.33 x 10^-2 Pa)) and coarse, prominent slip lines at high pressures (0.17 to 0.7 torr (9.31 to 93.1 Pa)). It also caused grain sliding and void formation. In an environment of water vapor and oxygen, fatigue caused grain boundary cracking and reduced plastic deformation inside grains surrounded by those cracks. Possible reasons for these observations are discussed. Suggestions are also made for utilizing some of these findings to improve the fatigue performance of metals.     

Stress corrosion cracking of copper bicrystals with 〈110〉-Tilt ∑3, ∑9, and ∑11 coincident site lattice boundaries

The stress corrosion cracking (SCC) behavior of copper bicrystals with 〈HO〉-tilt ∑3(111), ∑9(221), and ∑11(311) coincident site lattice (CSL) boundaries was investigated. Stress corrosion cracking tests were carried out in 1 N NaNO₂ aqueous solution at 303 ±2 K using a slow strain rate technique (SSRT). Transgranular SCC occurred along the primary slip traces on the top surface of the bicrystal having a ∑3(111) coincidence boundary. No cracks initiated on the grain boundary except for very small and shallow corrosion pits. In contrast, for the bicrystals with ∑9(221) or ∑11(311) coincidence boundaries, corrosion pits and cracks initiated on the grain boundary and propagated into the crystal interior along {110} traces, which are almost perpendicular to the tensile axis. The SCC behavior is closely related to the activated slip systems and the degrees of crystal rotation owing to deformation. Susceptibility to intergranular SCC is affected by the angle between the Burgers vector of the primary slip system and the grain boundary plane. The susceptibility of the ∑23(111) boundary to SCC is remarkably low in comparison with the other two types of grain boundaries. Y. Nakazawa, formerly Graduate Student, Department of Mechanical Engineering, Doshisha University This paper is based on a presentation made in the symposium “Interface Science and Engineering” presented during the 1988 World Materials Congress and the TMS Fall Meeting, Chicago, IL, September 26–29, 1988, under the auspices of the ASM-MSD Surfaces and Interfaces Committee and the TMS Electronic Device Materials Committee.     

Plastic incompatibility and crack nucleation during deformation on four independent slip systems in tungsten carbide-cobalt

The problem of slip transfer across grain boundaries is considered for the case of a hexagonal material that is plastically inextensible along [0001]. The discontinuity in tensile strain that must necessarily exist across a grain boundary is a cause of intergranular and transgranular cracking on the basal plane. Intergranular cracking at many grain junctions and two-grain junctions is shown to arise out of in-plane and normal strain differences across grain boundaries, respectively. Experimental evidence from deformed WC-Co is adduced to support these predictions. Transgranular cracking on the basal plane is found to occur only in coarse grained material. Thin (− 500 Å) layers of cobalt between carbide grains do not appear to appreciably affect the onset of cracking if it is expected from an incompatibility standpoint. The implications of these results are discussed for the general case of deformation of brittle solids, both with and without a superimposed constraining pressure.     

Intergranular fracture in an Al-15 Wt Pct Zn alloy

Crack propagation rates for the intergranular fracture of an Al-15 wt pct Zn alloy tested in air, distilled H₂O, and 0.5M NaCl have been studied using a double cantilever beam specimen. This technique has been applied to two different types of specimens: polycrystals with large equiaxed grains and bicrystals. The susceptibility to intergranular fracture in air and 0.5M NaCl increases as the volume fraction of G.P. zones in the matrix increases. The microstructure which is most susceptible to fracture exhibits intense planar slip traces while the more resistant microstructures have a more diffuse surface slip pattern. The dependence of cracking rates on the microstructure is explained in terms of the blocking of inhomogeneous plastic flow in the matrix by grain boundaries, resulting in locally severe stress concentrations at the boundaries. Bicrystal tests substantiate these results and show that orientations favoring partial continuity of slip bands across grain boundaries are less susceptible to stress corrosion cracking than arbitrarily oriented boundaries with no slip continuity. WILLIAM J. KOVACS, formerly Graduate Student, Carnegie-Mellon University, Pittsburgh, Pa. This paper is based upon a thesis submitted by WILLIAM J. KOVACS in partial fulfillment of the requirements of the degree of Doctor of Philosophy in Metallurgy and Materials Science at Carnegie-Mellon University.     

Interface sliding,migration, and cracking during fatigue deformation of a superplastic aluminum-zinc eutectoid alloy

A superplastic aluminum-zinc eutectoid alloy was fatigue tested at 100 °C and 200 °C at different constant plastic strain amplitudes and strain rates. During fatigue deformation, the average peak stress increased with increasing strain rate and grain size and decreasing temperature. It was almost independent of the plastic strain amplitude. To detect interfacial sliding, interphase boundary migration, and intergranular cracking, selected areas on surfaces were examined before fatigue deformation and re-examined after fatigue deformation. Interface sliding, which was almost reversible, occurred on (Al)/(Al) and (Zn)/(Zn) grain boundaries and on (Al)/(Zn) interphase boundaries. Grains appeared to slide in groups. Cracks followed grain and interphase boundaries. Along an intergranular crack, most interfaces were (Zn)/(Zn) grain boundaries and (Al)/ (Zn) interphase boundaries. Grains deformed to accommodate interfacial sliding. The absence of slip lines suggested that diffusional creep made a significant contribution to deformation in grains of the zinc-rich phase. Deformation of the aluminum-rich phase involved the glide and climb of dislocations. J. W. BOWDEN, formerly Graduate Student, Department of Metallurgy and Materials Science, University of Toronto.     

Fatigue damage and crack nucleation mechanisms at intermediate strain amplitudes

Polycrystalline copper was fatigued in rotary bending at constant intermediate surface strain amplitudes at 26 Hz under ambient conditions. The specimens were interrupted at various life fractions, their surfaces prepared metallographically and scrutinised to ascertain the types of fatigue damages, namely, short cracks which are confined to individual grains or isolated grain boundary facets, and their role in fatal crack formation. The results show that, at intermediate strain amplitudes, slip band and twin boundary crack damages predominate during early stages of cycling, while grain boundary crack damages remain relatively insignificant even at the stage when fatal cracks have developed. However, depending on the strain amplitude level, the transgranular crack damages may or may not be instrumental in fatal crack formation. At the lower amplitude end of the transition region, fatal cracks are formed by interlinkage of slip band and twin boundary damages. At the higher amplitude end, even though grain boundary damages are negligible initially, they degenerate rapidly on further cycling and eventually evolve into fatal cracks. The present findings show that some 0.05% plastic strain amplitude is required to propagate intergranular cracks. Once the above condition is met, cracks would propagate rapidly along the interface and the crack nucleation mode would change from transgranular to intergranular.     

Fatigue Crack Initiation In WASPALOY at 20 °C

In two WASPALOY specimens, the orientations of grains that initiated fatigue cracks and adjacent ograins were measured using electron backscattered diffraction patterns (EBSP). Crystallographic relationships were found for crack initiating regions that resulted in slip transmission across areas larger than the initiating grain, and the initiating grain was usually larger than average. A similar evaluation of control areas on each specimen found that there was much less likelihood of slip transmission across grain boundaries. Schmid factors (SFs) were also evaluated. It is concluded that the reason that fatigue cracks formed at these locations was due to the lower stress required for slip initiation in these clusters of grains oriented for slip transmission across grain boundaries. Many of the cracks initiated within grain boundaries. A detailed crystallographic analysis of the adjacent grains suggests criteria for intergranular (IG) crack initiation. This article is based on a presentation given in the symposium entitled “Deformation and Fracture from Nano to Macro: A Symposium Honoring W.W. Gerberich’s 70th Birthday,” which occurred during the TMS Annual Meeting, March 12–16, 2006, in San Antonio, Texas, and was sponsored by the Mechanical Behavior of Materials and Nanomechanical Behavior Committees of TMS.     

Deformation structure and subsurface fatigue crack generation in austenitic steels at low temperature

In order to progress in the understanding of fatigue crack generation for high-strength alloys, the subsurface fatigue crack initiation sites were characterized and the deformation structure was investigated for the solution-treated 24Cr-15Ni-4Mn-0.3N and 32Mn-7Cr-0.1N austenitic steels. High-cycle fatigue tests of those steels were carried out at 4, 77, and 293 K. Subsurface crack initiation was detected in the lower-peak stress and/or in the longer-life range at the three temperatures. The subsurface crack initiation sites were intergranularly formed. The localized deformation and/or strain concentration by dislocation arrays of the (111)–〈110〉 system assisted intergranular cracking due to incompatibility at grain boundaries. Dislocation movements were restricted to their slip planes. Even at the lower stress level, dislocations had generated in more than one slip system and piled up to a grain boundary. The peak cyclic stress was lowered with the increasing size of the subsurface crack initiation site. The dependence of the subsurface crack size on the peak cyclic stress was discussed.     

The effects of hydrogen and segregation on fatigue crack nucleation at defined grain boundaries in nickel bicrystals

In order to explore the role of impurity segregation in intergranular fatigue crack initiation and propagation, tests have been made on nickel bicrystals, variously heat-treated to induce increasingly severe degrees of sulfur segregation, and using air, vacuum and hydrogen as the environment. The grains of the bicrystals were oriented to yield two types of boundaries: type I, with strong elastic-plastic incompatibility and type II, a compatible tilt boundary. If the boundaries were clean, persistent slip band cracking in the grains occurred in preference to intergranular cracking. Although equal degrees of sulfur segregation, as measured by Auger-spectroscopy, could be produced at the two types of boundaries by the heat treatments, the incompatible one was much more susceptible to intergranular cracking than the other, which could be made to crack intergranularly only by high partial pressures of hydrogen. The results show that high stresses associated with incompatibility coupled with a lowering of cohesive forces at the boundary produced by the segregant are the main factors controlling intergranular fracture.     

The Role of grain boundary misorientation in intergranular cracking of Ni-16Cr-9Fe in 360 °C argon and high-Purity water

The effect of grain boundary misorientation on the intergranular cracking behavior of pure Ni-16Cr-9Fe was assessed by determining if low-angle boundaries (LABs) or coincident site lattice boundaries (CSLBs) are more crack resistant than general high-angle boundaries (GHABs) in argon and high-purity water. Cracking susceptibility of boundary types was determined using constant extension rate tensile tests (CERTs) in 360 °C argon and in deaerated, high-purity water. Annealed samples contained 12 to 20 pct CSLBs, while CSLB-enhanced samples contained 27 to 44 pct CSLBs; GHAB proportions varied accordingly. Cracked boundary fractions for CSLB-enhanced samples tested in either environment ranged from 0.01 to 0.08, while those for annealed samples ranged from 0.07 to 0.10, indicating that samples with increased proportions of CSLBs are more crack resistant. No LABs cracked in either environment. In annealed samples, the proportion of CSLBs that cracked in water was 6.7 pct compared to 1.5 pct in argon; the proportion of GHABs that cracked in water was 9.3 pct compared to 6.6 pct for argon. Thus, CSLBs are more crack resistant than GHABs in either environment, and both are more crack resistant in argon than in water. The higher amounts of cracking and the higher CSLB cracking susceptibility in high-purity water indicate the presence of an environmental effect on cracking behavior. The beneficial effect of LABs and CSLBs is likely due to the ability of these boundaries to induce slip in neighboring grains by either transmitting or absorbing and re-emitting lattice dislocations, thereby reducing grain boundary stresses and the propensity for crack initiation. The results indicate that control of grain boundary proportions can improve the intergranular stress corrosion cracking susceptibility of pure Ni-16Cr-9Fe. Formerly Graduate Research Assistant, The University of Michigan.     

Grain boundary segregation in austenitic stainless steels and its effect on intergranular corrosion and stress corrosion cracking

This paper reports a study of grain boundary segregation, intergranular corrosion, and intergranular stress corrosion cracking in austenitic stainless steels. The results show that phosphorus, nitrogen, and sulfur all segregate to grain boundaries in these materials and that they can affect one another's segregation through site compctition. In particular, the results demonstrate that phosphorus segregation can be lowered by the presence of nitrogen and sulfur in the steel. Also, if manganese is present in the steel, sulfur segregation will be greatly decreased as a result of formation of manganese sulfides. Phosphorus, sulfur, and nitrogen will not initiate intergranular corrosion in the modified Strauss test, although if corrosion is initiated by chromium depletion, these elements might enhance the corrosion process. Phosphorus segregation does enhance corrosion in the Huey test, even in steels that have not undergone grain boundary chromium depletion, although there does not appear to be a precise correlation between the depth of corrosion penetration and phosphorus segregation. Intergranular stress corrosion cracking in 288 °C water at a pH of 2.5 and electrochemical potential of OV_SHE can occur in these steels even in the absence of chromium depletion if sulfur is present on the grain boundaries. Phosphorus segregation appears to have very little effect.     

The effect of microstructure on the mode of monotonie fracture,fatigue crack initiation,and stage i crack growth in an Fe-21 Pct Cr-11 Pct Ni heat resisting steel

This paper describes a study carried out at room temperature on an Fe-21 pct Cr-11 pct Ni heat resisting alloy under tensile and fatigue deformation. Specific microstructures were developed by heat treating the as-received alloy at different temperatures and times. The surface condition of all specimens displayed surface grain boundary oxidation to a maximum depth of 0.16 mm. In addition, the microstructure of specimens in one batch (B) contained intergranular chromium carbides. The major conclusions drawn from this study are that different microstructures respond differently to monotonie and cyclic modes of deformation. In particular, the embrittling effect of intergranular chromium carbides observed during the monotonie mode of deformation was different from that found when deformation was cyclic. During cyclic deformation these chromium carbides assisted in reducing the damaging effects of the surface grain boundary oxidation. Also during cyclic deformation, the overall fatigue life was found to depend on the mode of both fatigue crack initiation and Stage I crack growth. Fatigue life was reduced when crack initiation and Stage I crack growth were intergranular while it was enhanced when crack initiation occurred at slip bands and subsequent Stage I crack growth was transgranular. It was observed that surface grain boundary oxidation is a most deleterious micro-structural feature especially under fatigue loading but, if this feature is unavoidable then the presence of intergranular chromium carbides is considered to be highly beneficial in increasing the overall fatigue resistance of the material. Formerly a Postgraduate Student, School of Materials Science and Engineering, University of New South Wales, Kensington, New South Wales 2033.     

The Effect of Phosphorus Content on the Hydrogen Stress Cracking of High Strength 4130 Steel

A series of four 4130 base steels with various phosphorus concentrations was subjected to cathodic charging to determine the effect of P on hydrogen stress cracking resistance. Static fatigue curves for several different yield strengths were obtained for each alloy. At high yield strengths under applied loads of 60 to 80 pct of the yield, 50 ppm P (bulk concentration) was enough to provide sufficient grain boundary P for an impurity-hydrogen interaction which produced intergranular fracture along prior austenite grain boundaries. Decreasing yield strength and applied stress caused a transition in fracture mode to transgranular while the resistance to hydrogen stress cracking increased with decreasing P. Microhardness measurements of prior austenite grain boundaries were made to establish the role of P. The role of P is not apparently related to its capacity as a strengthening element but more probably as a hydrogen recombination poison. Grain boundary hardness measurements for low temperature tempers (200 °C) appear to be valid while those at 500 °C were not.     

Effects of partial recrystallization on high-cycle fatigue deformation and crack generation of a nitrogen-strengthened 32Mn-7Cr austenitic steel at liquid-nitrogen temperature

To achieve higher fatigue resistance against subsurface crack generation, both the refinement of grain structure and the introduction of mobile dislocations on various slip systems have been shown to be effective in the 32Mn-7Cr austenitic steel. A novel treatment which consisted of cold grooved rolling and partial recrystallization was introduced to modify the microstructure. High-cycle fatigue properties and fatigue-crack generation were investigated for both the solution-treated (ST) and the partially recrystallized (PR) materials at 77 K. The PR material displayed higher fatigue strength than the ST material, especially in the high-cycle regime. No subsurface crack generation was detected for the PR material; however, it appeared in the lower peak stress and/or in the longer-life range for the ST material. Intergranular facets formed a subsurface crack initiation site in the ST material. Since the dislocation structure that developed in the fatigued PR material assisted homogeneous and multidirectional plastic deformation, the localized deformation and/or the stress concentration at the grain boundaries by coplanar arrays were believed to be relieved. Therefore, intergranular cracking due to incompatibility at a grain boundary may disappear.     

The effects of environment on the elevated temperature fatigue behavior of nickel-base superalloy single crystals

The effects of air and vacuum on the fatigue behavior of a nickel-base superalloy, Mar-M200, in single crystal form were investigated. Between 800° and 1400°F fracture is entirely in the Stage I mode in air and vacuum, and fatigue life is unaffected by environment. At 1700° F in both environments, fracture is predominantly in the Stage II mode and fatigue life in air is greater than that in vacuum. At both temperatures, fatigue cracking in air is internally initiated, whereas in vacuum cracking is generally initiated at the specimen surface. Identical fatigue lives in air and in vacuum between 800° and 1400° F are attributed to the fact that internally initiated cracks in air are actually propagating in a high vacuum, surface cracking being inhibited by dynamic oxidation of emerging surface slip offsets. The subsurface portion of the Stage I fracture surface produced in air tests and all of the Stage I fracture produced in vacuum tests shows a dimpled structure, whereas the Stage I fracture surface produced while the crack propagation is in air shows a cleavage appearance. At 1700° F, bulk oxidation of surface initiated cracks interferes with the plastic blunting mechanism of Stage II crack growth normally observed at this temperature, internally initiated cracks causing ultimate failure. Shorter lives in vacuum are thought to result from enhanced Stage II surface crack propagation. Formerly with Materials Engineering and Research Laboratory, Pratt and Whitney Aircraft, Middletown, Conn.