Creep-rupture properties and grain-boundary sliding in wrought cobalt-base HS-21 alloys at high temperatures

The effects of serrated grain boundaries on the creep-rupture properties of wrought cobaltbase HS-21 alloys were investigated at 1311 and 1422 K. The amount of grain-boundary sliding and the initiation and growth of grain-boundary cracks were also examined during creep at 1311 K. Specimens with serrated grain boundaries exhibited longer rupture life and larger rupture ductility than those with straight grain boundaries, but these specimens had almost the same rupture life and rupture ductility under lower stresses at 1422 K, because serrated grain boundaries were also formed in specimens with originally straight grain boundaries. The average amount of grain-boundary sliding during creep at 1311 K increased with time (or with creep strain), but was almost the same in both specimens with serrated grain boundaries and those with straight grain boundaries at the same creep strain. Grain-boundary cracks or voids initiated in the early stage of creep in those specimens at 1311 K. Therefore, the strengthening by serrated grain boundaries at high temperatures above about 1311 K was attributed to the retardation of growth and linkage of grain-boundary cracks and voids.     

Effects of high-temperature ageing on the creep-rupture properties of cobalt-base L-605 alloys

Effects of high-temperature ageing on the creep-rupture properties of cobalt-base L-605 alloys were investigated at 1089 and 1311 K in air. The specimens with serrated grain boundaries and those with normal straight grain boundaries were aged for 1080ksec at 1273 or 1323 K to cause the matrix precipitates of tungsten-rich b c c phase and M₆C carbide. The creep-rupture strength of both specimens were improved by the high-temperature ageing. The rupture strength at 1311 K was the highest in the specimens with serrated grain boundaries aged at 1273 K, while the specimens with straight grain boundaries aged at 1273 K of the highest matrix hardness had the highest rupture strength at 1089 K. The high-temperature ageing did not decrease the rupture ductility of specimens. The ruptured specimens with serrated grain boundaries exhibited a ductile grain-boundary fracture surface which consisted of dimple patterns and steps, regardless of whether high-temperature ageing was carried out. The fracture mode of the specimens with straight grain boundaries was changed from the brittle grainboundary fracture to the ductile one similar to that of the specimens with serrated grain boundaries by high-temperature ageing, since large grain-boundary precipitates which gave nucleation sites of dimples were formed during the ageing. The grain-boundary cracks initiated in the early stage of creep (transient creep regime) in both non-aged and aged specimens of L-605 alloys in creep at 1089 and 1311 K, although the time to crack initiation is shorter in the specimens with straight grain boundaries than in those with serrated grain boundaries. Thus, the period of crack growth and linkage occupied most of the rupture life. The strengthening mechanisms of the aged specimens were also discussed.     

Creep rupture strength and grain-boundary sliding in austenitic 21 Cr-4Ni-9Mn steels with serrated grain boundaries

The effect of grain-boundary strengthening on the creep-rupture strength by modification of the grain-boundary configuration is studied using austenitic 21 Cr-4Ni-9Mn steel in the temperature range from 600 to 1000° C in air. Grain-boundary sliding is also examined on a steel with serrated grain boundaries during creep at 700° C. The improvement of creep-rupture strength by the strengthening of grain boundaries is observed at high temperatures above 600° C. The 1000 h rupture strength of steels with serrated grain boundaries is considerably higher than that of steels with straight grain boundaries, especially at 700 and 800° C. The strengthening by serrated grain boundaries is effective in retarding both the crack initiation and the crack propagation at 700° C, while it does not improve the life to crack initiation at 900° C. Grain-boundary sliding is considerably inhibited by the strengthening of grain boundaries at 700° C. The amount of it in steels with serrated grain boundaries is less than about one-third of that of steels with straight grain boundaries at the same creep strain. The stress dependence of grain-boundary sliding rate in the steady-state regime is also examined from the steels with these two types of grain-boundary configuration.     

Effects of high-temperature ageing on the creep-rupture properties of high-tungsten cobalt-base superalloys

The effects of high-temperature ageing on creep-rupture properties were studied using cobalt-base superalloys containing about 14–20 wt% tungsten (W) at 1089 K (816 °C) and 1 311 K (1038 °C) in air. A high-temperature ageing for 1080 ks at 1273 K after solution treatment caused grain-boundary and matrix precipitates of W solid solution and carbide phases in these alloys, and grain boundaries were serrated especially in the alloys with higher W content. The high-temperature ageing largely improved the rupture life in the alloys with higher W content, particularly under lower stresses at 1089 K, whereas it caused the creep ductility to decrease a little in the alloy containing 20% W. The high-temperature ageing also improved the rupture life without decreasing creep ductility in these alloys under higher stresses at 1311 K. Under the same ageing conditions of 1080 ks at 1273 K, the initiation of grain-boundary cracks was retarded in the solution-treated and aged specimens, as well as in the aged specimens with serrated grain boundaries, for the alloys with higher W content at both 1089 and 1311 K. A large amount of grain-boundary serration also occurred in the non-aged specimens of the alloys with higher W content during creep at 1311 K, and contributed to the strengthening of the alloys. The solution-treated and aged specimen had almost the same rupture strength as the aged specimens with serrated grain boundaries in these cobalt-base alloys. The rupture strength of the solution-treated and aged specimens largely increased with increasing W content under the lower stresses at 1089 K and under the higher stresses at 1311 K. A ductile grain-boundary fracture surface, which was composed of dimples and grain-boundary ledges associated with grain-boundary precipitates, was observed in the solution-treated and aged specimens, as well as in the aged specimens with serrated grain boundaries at both 1089 and 1311 K. The fracture surface of the non-aged specimens was a brittle grain-boundary facet at 1089 K, but it became a ductile grain-boundary fracture surface, as serrated grain boundaries were formed owing to grain-boundary precipitates occurring during creep at 1311 K.     

Effects of serrated grain boundaries on the crack growth in austenitic heat-resisting steels during high-temperature creep

The effect of serrated grain boundaries on creep crack growth is investigated using an austenitic 21Cr-4Ni-9Mn steel principally at 700° C. The relationship between the microstructure of specimens and the crack growth behaviour is discussed. The creep crack growth rate in the specimens with a surface notch is relatively reduced by serrated grain boundaries especially in the early stage of crack growth. The life of crack propagation in the specimens with serrated grain boundaries is longer compared with that of the specimens with straight grain boundaries. It is confirmed in the surface crack growth of smooth round bar specimens crept at 700° C that serrated grain boundaries are effective in retarding the growth of a grain-boundary crack less than about 4×10^–4 m long, and that this effect decreases with increasing crack length. It is suggested that crack deflection due to serrated grain boundaries caused a decrease in the stress intensity factor of the grain-boundary crack and resulted in a decrease of the crack growth rate in the steel. The crack arrest at the deflection points and the circumvention of crack path on the serrated grain-boundaries may also contribute to the retardation of the grain-boundary crack growth during creep. Further, it is deduced from the experimental results on the notched specimens that the creep fracture is caused by the linkage of the main crack to many microcracks and voids on the grain-boundary at 900°C.     

Characterization of grain-boundary configuration and fracture surface roughness by fractal geometry and creep-rupture properties of metallic materials

Grain-boundary configuration in heat-treated specimens and fracture surface roughness in creep-ruptured specimens of several kinds of metallic material were quantitatively evaluated on the basis of fractal geometry. Correlations between the fractal dimension of grain boundary, that of fracture surface profile, the creep-rupture properties and the fracture mechanisms of the alloys are discussed. In heat-resistant alloys, the fractal dimension of a nominally serrated grain boundary was always larger than that of a straight grain boundary in the same alloy. The relative importance of the ruggedness of grain boundaries was estimated by the fractal dimension difference between these two grain boundaries. There was a quantitative relationship between the increase of the fractal dimension of the grain boundary and the improvement of rupture ductility and rupture strength owing to grain-boundary serration in the alloy. A similar correlation was also found between the increase in the fractal dimension of the fracture surface profile and the improvement of the creep-rupture properties, since in some cases the fractal dimension of the fracture surface profile was correlated with that of the grain boundary. Both grain boundary and fracture surface profile were assumed to exhibit a fractal nature between one grain boundary length (upper bound) and an interatomic spacing (lower bound). In carbon steels with ferrite-pearlite structure, according to the increase in pearlite volume fraction, the rupture ductility decreased and the fracture mechanism changed from transgranular fracture in pure iron and low-carbon steels to intergranular fracture at ferrite-pearlite grain boundaries in medium-carbon steels, and further to intergranular fracture at pearlite grain boundaries in high-carbon steels. The correspondence between the fractal dimension of the grain boundary and that of the fracture surface was confirmed in ruptured specimens of ferrite-pearlite steels when the grain boundary was the fracture path.     

Effects of grain-boundary configuration on the high-temperature creep strength of cobalt-base L-605 alloys

The effects of grain-boundary configuration on the high-temperature creep strength are investigated using commercial cobalt-base L-605 alloys with low carbon content in the temperature range 816 to 1038° C (1500 to 1900° F). Serrated grain boundaries are formed principally by the precipitation of tungsten-rich b c c phase (the same as ₂ phase found in Ni-20Cr-20W alloys) on grain boundaries by a relatively simple heat treatment in these alloys. The creep rupture properties are improved by strengthening of grain boundaries by the precipitation of tungsten-rich bcc (₂) phase. The specimens with serrated grain boundaries have longer rupture lives and higher ductility than those with normal straight grain boundaries under low stress and high-temperature creep conditions, while the rupture lives and the creep ductility of both specimens are almost the same under high stresses below 927° C. The matrix of the alloys is strengthened by the precipitation of carbides at temperatures below 927° C and by the precipitation of tungsten-rich ₂ phase at 1038° C during creep. It is found that there is an orientation relationship between tungsten-rich a2 phase particles and-Co matrix, such that (0 1 1)₂ ¶ (1 1 1) _-Co and [1 1]₂ ¶ [1 0] _-Co. The fracture surface of specimens with serrated grain boundaries is a ductile grain-boundary fracture surface, while typical grain-boundary facets prevailed in specimens with straight grain boundaries.     

Effects of the creep deformation on the fractal dimension of the grain boundaries in an austenite steel

The change in the fractal dimension of the grain boundaries during creep was investigated using an austenitic SUS304 steel at 973 K. The fractal dimension of the grain-boundary surface profile (the fractal dimension of the grain boundaries, D, 1 < D < 2) in the plane parallel to the tensile direction (in the parallel direction) and in the transverse direction, was examined on specimens deformed up to rupture (about 0.30 creep strain). Grain boundaries became serrated and the fractal dimension of the grain boundaries increased with increasing creep strain, because the density of slip lines which formed ledges and steps on grain boundaries increased as the creep strain increased. The increase in the fractal dimension due to creep deformation was slightly larger under the higher stress (118 MPa) than under the lower stress (98 MPa), while the increase of the fractal dimension with strain was a little larger in the specimens tensile-strained at room temperature (293 K) than in the crept specimens. These results were explained by the grain-boundary sliding and the diffusional recovery near grain boundaries, which lowered the increase of the fractal dimension with the creep strain. The fractal dimension of the grain boundaries in the parallel direction was slightly larger than that in the transverse direction in both creep at 973 K and tensile deformation at room temperature, especially at the large strains. This could be correlated with the shape change of the grains by creep or plastic deformation. Grain-boundary cracks were principally initiated at grain-boundary triple junctions in creep, but ledges, steps and carbide precipitates on serrated grain boundaries were not preferential nucleation sites for the cracks.     

The creep-rupture properties and the initiation and growth of the grain-boundary cracks in the cobalt-base HS-21 alloy

The effect of the grain-boundary microstructures on the creep-rupture properties and the initiation and growth of the grain-boundary cracks was investigated using four kinds of specimen of various grain-boundary microstructures in the cobalt-base HS-21 alloy at 1089 K in air. Both the rupture strength and the creep ductility increased with increasing mean value of the fractal dimension of the grain boundaries, Dgb. The strain to crack initiation was largest in the specimen of the highest value (1.241), while the strain was much the same in the specimens of the Dgb value less than 1.162. This was explained by the local variation in the grain-boundary microstructures in these specimens. The mean value of the fractal dimension of the grain-boundary fracture, Df, was close to the value of Dgb, although the value of Df was a little higher than that of Dgb in the specimens of the lower Dgb values. The fracture appearance changed from a brittle grain-boundary fracture to a ductile one with increasing values of Dgb and Df. The crack-growth rate is the surface-notched specimens decreased with increasing value of Dgb. The threshold stress intensity factor for crack growth was higher in the specimens with the higher Dgb values. This revised version was published online in November 2006 with corrections to the Cover Date.     

The fractal dimension of grain-boundary fracture in high-temperature creep of heat-resistant alloys

The fractal dimension of the grain-boundary fracture in high-temperature creep was estimated by the vertical section method on several creep-ruptured specimens of the cobalt-nickel- and iron-based heat-resistant alloys. Grain-boundary microcracks linked to the fracture surface were also taken into account in the present analysis by the box-counting method. In the specimens containing many grain-boundary microcracks linked to the fracture surface, the fractal dimension of the grain-boundary fracture was larger in the scale range of more than about one grain-boundary length than in the scale range less than this length. Thus, there was a cross-over in the fractal dimension of the grain-boundary fracture at about one grain-boundary length in these specimens. In the specimens containing much fewer microcracks, there was no clear cross-over in the fractal dimension of the grain-boundary fracture with regard to the scale of the analysis, irrespective of creep-ductility and grain-boundary configuration of the specimens. The fractal dimension of the grain-boundary fracture was generally larger in specimens with serrated grain boundaries than in specimens with straight grain boundaries in these heat-resistant alloys, because the fractal dimension of the grain boundary and the number of the grain-boundary microcracks were larger in the former specimen. The fractal dimension of the grain-boundary fracture did not tend to converge to unity when the scale of the analysis approached the specimen size. The inclusion of near-specimen size data with regard to the scale of the analysis did not affect the fractal dimension of the grain-boundary fracture in these alloys. Thus, the grain-boundary fracture in the creep-ruptured specimens exhibited a fractal nature, at least in the scale range below specimen size, although there was a cross-over in the fractal dimension of the grain-boundary fracture in specimens containing a large number of grain-boundary microcracks.     

Fractal dimension of the grain boundary fracture in creep-fracture of cobalt-based heat resistant alloys

The effects of grain boundary configuration and creep conditions on the fractal dimension of the grain boundary fracture (D _f) were investigated using commercial cobalt-based heat resistant alloys, namely, HS-21 and L-605 alloys. Creep-rupture experiments were carried out under the initial creep stresses of 19.6–176 MPa in the temperature range from 1089–1422 K in air. The value of D _f was larger in specimens with serrated grain boundaries than in those with straight grain boundaries in the HS-21 alloy under the same creep condition, and the difference in the value of D _f between these specimens was large in the scale range of the analysis which was less than about one grain boundary length. However, there was almost no difference in the value of D _f between the specimens with serrated grain boundaries and those with straight grain boundaries in the L-605 alloy, because there was no obvious difference in the microstructure between these specimens. The value of D _f increased with decreasing creep stress in the scale range of the fractal analysis larger than about one grain boundary length in both HS-21 and L-605 alloys, while the stress dependence of D _f was larger in the HS-21 alloy. The stress dependence of D _f was explained by the stress dependence on the number of grain boundary microcracks linked to the fracture surface. The value of D _f estimated in the scale range smaller than about one grain boundary length showed essentially no stress dependence in both L-605 and HS-21 alloys.     

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.     

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.     

Effect of vanadic corrosion on creep-rupture properties of Superni-600 at 650–750°C

The effect of vanadic corrosion on creep-rupture properties of a nickel base superalloy Superni-600, at 650–750°C, has been investigated. Sodium metavanadate and sodium metavanadate plus 15 wt% sodium sulphate were used as the corrodent salts. Weight change studies have also been made to understand the mechanism of corrosion. Both sodium metavanadate and the sodium metavanadate/sodium sulphate mixture are found to be aggressive and to reduce the creep-rupture life. The degradation of creep-rupture properties and possible hot corrosion reactions are discussed. Cracking and fluxing of the protective scales, together with easier crack nucleation and growth at grain boundaries in the presence of a liquid deposit accounts for the enhanced creep rates and reduced rupture lives.     

An evaluation of the grain-boundary sliding contribution to creep deformation in polycrystalline alumina

The occurrence of grain-boundary sliding during creep in fine grained alumina was examined by inscribing marker lines on the tensile surfaces of specimens, prior to testing in four-point bending mode. There was considerable microstructural evidence for the occurrence of grainboundary sliding and grain rotation during creep deformation. Experimental measurements of the offsets in the marker lines at grain boundaries reveal that the grain-boundary sliding contribution to the total strain during creep deformation is 70 ± 6.2%. The extensive grain boundary sliding observed, together with the other mechanical properties, suggests that polycrystalline alumina exhibits superplastic characteristics. Several possible rate controlling mechanisms are examined critically in light of the present results and it is concluded that creep occurs either by an independent grain-boundary sliding mechanism or by an interface controlled diffusion mechanism.     

The relationship between intergranular cavitation and superplastic flow in an industrial copper base alloy

Intergranular cavitation has been observed during the superplastic deformation of a fine grain sized (1 m) Cu-2.8% Al-1.8% Si-0.4% Co alloy when tested at temperatures 500° C. High voltage electron microscopy revealed that the cavities could be nucleated at twin boundary/grain boundary intersections. The maximum elongation occurs at a higher temperature than that of the maximum strain-rate sensitivity and this is explained in terms of grain-boundary migration, at the higher temperature, which restricts the cavitation process. This explanation was put forward on the basis of texture analysis which was used to study the deformation characteristics at the temperatures of maximum elongation and strain-rate sensitivity. The final fracture mode is shown to change with test temperature: (i) at 400° C no cavitation occurs and fracture is by ductile rupture, (ii) at 500 to 550° C cavitation occurs and fracture is by the interlinkage of voids by an intergranular void sheet (IVS) mechanism and (iii) at 800° C grain growth occurs and fracture occurs by the propagation and interlinkage of grain-boundary cracks along the grain boundaries.     

Mechanisms of interdiffusion in Pd-Cu thin film diffusion couples

Interdiffusion in sputter-deposited polycrystalline Pd-Cu bilayers (thickness of each sublayer: 50 nm) was studied in the temperature range 175 °C-250 °C by sputter-depth profiling in combination with Auger electron spectroscopy. X-ray diffraction and transmission electron microscopy investigations revealed that the layers are polycrystalline, consisting of columnar grains separated by grain boundaries oriented more or less perpendicularly to the film surface. Considerable diffusional intermixing occurred in the studied temperature range, which was accompanied by the sequential formation of (ordered) phases Cu₃Pd and CuPd. Volume interdiffusion coefficients were determined using the so-called ‘centre-gradient’ and ‘plateau-rise’ methods. Grain-boundary diffusion coefficients of Pd through Cu grain boundaries were determined by the Whipple-Le Claire method and grain-boundary diffusion coefficients of Cu through Pd grain boundaries were determined by the Hwang-Balluffi method. It was found that both volume and grain-boundary diffusion coefficients decreased roughly exponentially with annealing time. Activation energies were determined which pertain to the same (defect) microstructure at each temperature. The differences with literature results for macroscopic diffusion couples were discussed.     

A study on the mechanism of serrated grain boundary formation in an austenitic stainless steel

Measurement of the activation energy for the formation of serrated grain boundaries (GB) has been carried out to understand its underlying formation mechanism in an AISI 316 stainless steel. The apparent incubation time necessary to initiate grain boundary serration was obtained at different aging temperatures, and the apparent activation energy for serration was carefully calculated from the Arrhenius relationship between incubation time and aging temperature. The activation energy for GB serrations in this alloy was measured to be approximately 148 ± 20 kJ mole⁻¹, which is consistent with the activation energy for lattice diffusion of carbon in γ-iron (142 kJ mole⁻¹). This result indicates that GB serration could be controlled essentially by the lattice diffusion of carbon to grain boundaries. Based on the through-thickness observation of serrated GBs, a straight boundary began to serrate from the surface at an early stage of the aging treatment, and then the serrated parts propagated throughout the entire grain boundary.     

Some elevated temperature mechanical properties of Magnox AL80

The influence of grain-boundary hydride (MgH₂) precipitation on the mechanical properties of Magnox AL80 has been investigated by carrying out slow tensile and fatigue tests. The presence of hydride precipitates at some grain boundaries was found to have a detrimental effect on the slow tensile ductilities at the lower end (20 to 40% h^–1) of the range of strain rates used (20 to 2000% h^–1) at 250° C and at 20% h–1 at 300° C. Grain-boundary cavities caused by the dissociation of the hydride precipitates were introduced either byin situ thermal treatment prior to testing at 250° C or by testing at higher temperatures and also resulted in lower tensile ductilities at slow strain rates. The fatigue lives of Magnox AL80 were not significantly influenced by the presence of grain-boundary hydride precipitates or cavities due to the dissociation of the precipitates. This is due to the majority of the boundaries being unsuitably oriented to experience high shear stresses. Long-term ageing at 450° C was found to reduce the subsequent fatigue strength at that temperature and this effect is associated with the boundaries becoming more prone to migration during fatigue cycling.     

Effect of dynamic strain ageing on the tensile properties of a modified 9Cr–1Mo steel

Tensile testing of a modified 9Cr–1Mo steel in two microstructural conditions (710T– normalized at 1100°C, tempered at 710°C, and 550T – normalized at 1100°C tempered at 550°C) in the temperature range 25–450°C, under strain rates of 2.3×10-5–2.3×10-3s-1, exhibited serrated flow curves, with serrations appearing almost at the onset of deformation and disappearing before ultimate strengths were attained. The serrated flow curves (characteristics of dynamic strain ageing) were accompanied by increased ultimate strengths, loss of ductility and negative strain-rate sensitivity, relative to the ambient temperature properties. However, the increase in ultimate strength and the reduction in ductility were much larger for 710T specimens, as compared to 550T ones. In the dynamic strain ageing regime, the work-hardenability of 710T specimens increased rapidly while that of 550T specimens remained practically unaffected. Based on the microstructural consideration and the observed activation energy of 45 kJ mol-1, it is proposed that serrations are initiated by a nitrogen atmosphere formation on the waiting dislocations by a pipe diffusion mechanism, and they disappear by diffusion to the precipitate sinks during deformation. Because the fine alloy carbide precipitates in 550T specimens are more effective sinks than those of 710T ones, they can cause much faster depletion of the atmosphere, resulting in a much smaller effect of dynamic strain ageing on the tensile properties of 550T specimens.