The effect of test temperature on the intergranular cracking of Nb-A286 alloy in low cycle fatigue

The continuous low cycle fatigue behaviors of a Fe-base superalloy, Nb-modified A286 alloy, have been evaluated at the test temperatures of 650°C and 350°C under various total strain ranges. It was found that the change of the slope in the Coffin–Manson plot was closely related to the fatigue cracking with the test temperature. In the high temperature low cycle fatigue (HTLCF) of Nb-A286 alloy, the fatigue cracking exhibited the intergranular mode at 650°C and the transgranular mode at 350°C. The intergranular fatigue cracking at 650°C was due to the precipitation of the phase at the grain boundary assisted by the applied stress during low cycle fatigue. It is investigated whether the precipitate at the grain boundary provides the site for the grain boundary cavitation, which induces the intergranular cracking in low cycle fatigue. This is confirmed by the results of low cycle fatigue at 25°C after heat treatment which forms the phase at the grain boundary.     

Creep in pure and two phase nickel-doped alumina

Creep in pure and two phase nickel-doped alumina has been investigated in the stress range 0.70 to 4.57 kgf mm^–2 (1000 to 6500 psi), and temperature range 1450 to 1800° C, for grain sizes from 15 to 45 m (pure alumina) and 15 to 30 um, (nickel-doped alumina). The effect of stress, grain size and temperature on the creep rate suggests that diffusion controlled grain-boundary sliding is the predominant creep mechanism at low stresses and small grain sizes. However, the stress exponents show that some non-viscous boundary sliding occurs even at the lowest stresses investigated. This mechanism is confirmed by metallographic evidence, which shows considerable boundary corrugation in the deformed aluminas. At higher stresses and larger grain sizes the localized propagation of microcracks leads to high stress exponents in the creep rate equation. The nickel dopant, which introduces an evenly distributed spinel second phase into the alumina matrix, increases the creep rate and enhances boundary sliding and localized crack propagation. The weakening effect of the second phase increases with grain size, and tertiary creep occurs at strains of 0.5% and below in large grained material.     

Wedge crack nucleation in Type 316 stainless steel

Type 316 austenitic steel has been heat-treated to produce a range of grain sizes and then creep-tested at 625° C at various stresses so as to examine the nucleation and the factors which effect the nucleation of grain-boundary triple point or wedge cracks. An internal marker technique was used to evaluate the extent of the grain-boundary sliding in relation to the total creep strain. Triple point crack nucleation occurred over the entire range of grain sizes and stresses examined when the product of the stress and grain-boundary displacement reached a critical value; the effective surface energy for grain boundary fracture, estimated using an expression derived by Stroh, was in approximate agreement with the surface free energy value indicating that only limited relaxation occurred by plastic deformation. The first cracks were observed to form along grain boundary facets perpendicular to the applied stress direction and with the sliding grain boundaries at high angles (60 to 80°) to the crack growth direction. Subsequent cracking occurred under conditions which deviated slightly from this initial condition, and the increase in crack density with strain was expressed in terms of geometrical factors which take account of the orientation effects.     

Creep of chemically vapour deposited SiC fibres

The creep, thermal expansion, and elastic modulus properties for chemically vapour deposited SiC fibres were measured between 1000 and 1500°C. Creep strain was observed to increase logarithmically with time, monotonically with temperature, and linearly with tensile stress up to 800 MPa. The controlling activation energy was 480 ± 20 kJ mol^–1. Thermal pretreatments near 1200 and 145O° C were found to significantly reduce fibre creep. These results coupled with creep recovery observations indicate that below 1400°C fibre creep is anelastic with negligible plastic component. This allowed a simple predictive method to be developed for describing fibre total deformation as a function of time, temperature, and stress. Mechanistic analysis of the property data suggests that fibre creep is the result of -SiC grain boundary sliding, controlled by a small percentage of free silicon in the grain boundaries.     

The tensile and creep behavior of Mg–Zn Alloys with and without Y and Zr as ternary elements

Tensile–creep experiments were conducted in the temperature range 100–200 °C and stress range 20–83 MPa for a series of magnesium–zinc–yttrium (Mg-Zn-Y) and mangnesium-zinc–zirconium (Mg-Zn-Zr) alloys ranging from 0 to 5.4 wt% Zn, 0 to 3 wt% Y, and 0 to 0.6 wt.% Zr. The greatest tensile–creep resistance was exhibited by an Mg–4.1Zn–0.2Y alloy. The room-temperature yield strength increased with increasing Y content for Mg–1.6–2.0Zn alloys. The greatest tensile strength and elongation was exhibited by Mg–5.4Zn–0.6Zr. This alloy also exhibited the finest grain size and the poorest creep resistance. The measured creep exponents and activation energies suggested that the creep mechanisms were dependent on stress. For applied stresses greater than 40 MPa, the creep exponents were between 4 and 8. For applied stresses less than 40 MPa, the creep exponent was 2.2. The calculated activation energies (Qapp) were dependent on temperature where the Q _app values between 100 and 150 °C (65 kJ/mol) were half those between 150 and 200 °C for the same applied stress value (30 MPa). Deformation observations indicated that the grain boundaries were susceptible to cracking in both tension and tension-creep, where at low applied stresses grain boundary sliding was suggested where strain accommodation occurred through grain boundary cracking. Thus grain size and grain boundaries appeared to be important microstructural parameters affecting the mechanical behavior. Microstructural effects on the tensile properties and creep behavior are discussed in comparison to other Mg-based alloy systems.

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High temperature bending creep of a Sm-α-β Sialon composite

The four-point bending creep behavior of a Sm-- Sialon composite, in which Sm-melilite solid solution (denoted as M) was designed as intergranular phase, was investigated in the temperature range 1260–1350°C and stresses between 85 and 290 MPa. At temperatures less than 1300°C, the stress exponents were measured to be 1.2–1.5, and the creep activation energy was 708 kJ mol^–1, the dominant creep mechanism was identified as diffusion coupled with grain boundary sliding. At temperatures above 1300°C, the stress exponents were determined to be 2.3–2.4, and creep activation energy was 507 kJ mol ^–1, the dominant creep mechanism was suggested to be diffusion cavity growth at sliding grain boundaries. Creep test at 1350°C for pre-oxidation sample showed a pure diffusion mechanism, because of a stress exponent of 1. N^3– diffusing along grain boundaries was believed to be the rate controlling mechanism for diffusion creep. The oxidation and Sialon phase transformation were analyzed and their effect on creep was evaluated.     

Transient Creep Associated with Grain Boundary Sliding in Fine-Grained Single-Phase Al2O3

Transient creep data for high-purity polycrystalline alumina are examined at the testing temperature of 1150–1250 °C. The data are analysed in terms of the effect of stress and temperature on the extent of transient time and strain.In order to explain the observed transient creep, a time function of creep strain is proposed from a two-dimensional model based on grain boundary sliding. The grain boundary sliding is assumed to take place by the glide of grain boundary dislocations accommodated by dislocation climb in the neighboring grain boundaries. The time function for a creep strain obtained from the model is given in a form

Short-term flexural creep deformation in synroc-C

The flexural creep behaviour of synroc-C in an inert atmosphere was studied at temperatures of 860°C, 900°C and 940°C under constant-load conditions in four-point bending. Applied stresses ranged from 100 to 160 MPa. Individual creep curves show primary and secondary creep but little or no tertiary creep stage. The log of the creep rate was found to increase linearly with log of the applied stress at each temperature over the entire stress range. Analysis of the creep data using the Norton power-law function revealed that the stress exponent decreased from 3.3 ± 0.6 for the 860°C and 900°C data to 2.0 ± 0.2 for the 940°C data, and an activation energy of 440 ± 40 kJ/mol was obtained over the entire temperature and stress range. Comparative analysis with the theta-projection equation was found to adequately represent the data yielding an activation energy of 464 kJ/mol while also showing a trend for the stress exponent to decrease with increasing temperature. Microstructural examination revealed extensive cavitation on the tensile surface of the creep specimens subjected to higher stresses at 900°C and 940°C. Dynamic high temperature X-ray diffraction analysis indicated little change in the phase assemblage apart from a slight reduction in the amount of the hollandite phase at higher temperatures which was attributed to a minor amount of oxidation. The possible creep damage mechanism was explored with reference to creep test results and microstructural modifications and the implications of the observations are discussed.     

Influence of heat treatment on creep of a Mn–N stabilised austenitic stainless steel

Creep at 700 °C/196 MPa and 900 or 925 °C/27.4 MPa of 21Cr–4Ni–9Mn austenitic stainless steel is determined as a function of the heat treatment. The heat treatment variation involves altering the solution heat treatment cooling rate from water quenching to cooling at 6 or 4 °C/min causing: serrated grain boundaries versus planar grain boundaries, coarser intergranular carbides, and discontinuous precipitation of grain boundary reaction zones. Water quenching causes improved creep resistance. Creep fracture and cracking is intergranular. Coarse intergranular carbides and grain boundary reaction zones cause premature void formation and cracking, this damage leading to an accelerating creep rate and lowering creep resistance of the more slowly cooled conditions. During creep, grain boundary serrations, which may otherwise contribute to improved creep, are eliminated. Determining the individual influence of grain boundary serrations on creep requires a detailed investigation of various heat treatment parameters to prevent concurrent formation of grain boundary reaction zones and serrations.     

Effects of heat-treatment on the high-temperature ductility and fracture of 20 Cr/25 Ni/Nb stabilised austenitic steel

Stabilisation of 20 Cr/25 Ni steel by niobium not only increased the creep resistance but eliminated the tendency for cracking and thereby enhanced the ductility. No change in density was detected in fine-grained specimens solution-treated at 1000° C until well into tertiary creep, and elongations of 75 to 150% were obtained. After a solution-treatment at 1250° C the creep resistance was further increased and denuded zones were formed near grain boundaries. This caused the strain to be concentrated in grain boundary regions during creep, leading to the formation of both surface- and wedge-cracks at grain boundaries. However, in contrast to a niobium-free steel, these did not nucleate until the end of the secondary creep.     

Fatigue behaviour of sintered SiC; temperature dependence and effect of doping with aluminium

Cyclic and static fatigue behaviours were investigated using sintered -SiC materials with indentation-induced precracks, focusing especially on the temperature dependence and the effect of doping with aluminium. No effects of cyclic loading were observed in the crack growth of materials both with and without aluminium, tested for the whole temperature range of room temperature to 1500° C, suggesting that cyclic fatigue might be insignificant in SiC. However, there is static fatigue damage in the material, the causes of which seem to be different depending upon the temperature and the aluminium doping. The static fatigue observed at room temperature is environmentally assisted cracking, whereas the fatigue at high temperature (1500° C) seems to be controlled by the creep properties. In the high-temperature behaviour, doping SiC with aluminium makes its strength decrease for the case where the material is loaded to failure in a short time, but makes the resistance to cracking rather increase for the case where the sample is statically loaded at lower stresses for a relatively long time.     

Effect of impurities (graphite) on the high-temperature creep properties of NiAl

Previous high-temperature compression creep studies of NiAl have shown peculiar behaviour in the temperature range 700 to 900° C, which was perhaps due to precipitation of impurities in the matrix. To isolate the impurity effect, high-purity NiAl samples with 0.15 at% and 0.20 at% carbon (graphite) additions have been creep tested at four temperatures between 700 and 850° C. Addition of graphite has been shown to produce a significant reduction in the creep strength of the alloyS. However, alloys with higher graphite concentrations have shown better creep resistance than those with lower graphite concentrations. Transmission electron microscopy indicates the presence of competing softening and hardening mechanisms in the alloys. Softening is due to the graphite particles acting as a dislocation source. Hardening results from a grain-boundary hardening mechanism due to the graphite particles segregating at grain boundaries and a dislocation-impurity (fine graphite) interaction, developing a Cottrell-like atmosphere.     

Creep of CaO/SiO2-containing MgO refractories

Compressive creep of five commercially-available brands of CaO/SiO2-containing MgO refractories was measured over a temperature range of 1400-1550°C and compressive stresses of 0.10–0.30 MPa. All brands had a MgO content greater than 96 wt%, a CaO/SiO2 wt% ratio equal to or greater than 1.9, and a firing temperature greater than 1535°C. The more creep resistant brands were observed to have a combination of: (1) a larger average grain size and wider grain size distribution, (2) a low iron content, and (3) an absence of CaO-MgO-SiO2 compounds. Creep-stress exponents for three of the five brands indicated their creep was rate-controlled by diffusion, and their activation energy values indicated that creep was accommodated by grain boundary sliding through viscous flow of the calcium silicate grain-boundary phase. Two brands exhibited dramatic time-hardening behavior which resulted in their creep not being well-represented by the power-law creep formulation. The observed attributes among the brands were combined and a hypothetical CaO/SiO2-containing MgO refractory is proposed.     

Reverse cyclic fatigue of a hot isostatically pressed silicon nitride at 1370 °C

The uniaxial, reverse cyclic fatigue performance of a commercially available hot isostatically pressed silicon nitride was examined at 1370 °C in air and with a 1 Hz sinusoidal waveform using button-head tensile specimens. Specimens did not fail in less than 10⁶ cycles when the applied stress amplitude was less than 280 MPa. Slow crack growth occurred at stress amplitudes 280 MPa and failure always occurred during the tensile stroke of the waveform. Multi-grain junction cavities resulted (i.e., the accumulation of net tensile creep strain) as a consequence of the reverse cyclic loading even though the specimens endured half their life under tensile stresses and the other half under compressive stresses. The presence of multi-grain junction cavities was a consequence of the stress exponent of tensile creep strain being greater than the stress exponent of compressive creep strain. Lastly, it was observed that the static creep resistance of this material improved when it was first subjected to reverse cyclic loading at 1370°C for at least 10⁶ cycles at 1 Hz. Silicon nitride grain coarsening (which was a consequence of the completion of the to silicon nitride solution/reprecipitation process that occurred during the history of the reverse cyclic loading) lessened the capacity for grain boundary sliding resulting in an improved static creep resistance.     

Viscoplastic behavior of a FeCrAl alloy for high temperature steam electrolysis (HTSE) sealing applications between 700 °C and 900 °C

High temperature steam electrolysis (HTSE) is one of the most promising technologies for the industrial production of hydrogen. However one of the remaining problems lies in sealing at high temperature. The reference solution is based on glass seals which presents several drawbacks. That explains why metallic seals are under development. The expected seal will be submitted to creep under low stresses between 700 °C and 900 °C, possibly involving complex loading and thermal history. The candidate material investigated in this work is a FeCrAl (OC404, Sandvik) supplied as a 0.3 mm thick sheet. The ability of this material to develop a protective layer of alumina was studied first, as well as grain size growth during thermal ageing. Creep and tensile tests were performed between 700 °C and 900 °C to determine its mechanical properties. This database was used to propose and identify an elasto-viscoplastic behavior for the material. Creep was described by the Sellars-Tegart law. This law was then used to simulate and predict creep indentation tests performed in the same range of temperatures.     

Effect of Laves phase strengthening on the mechanical properties of high Cr ferritic steels for solid oxide fuel cell interconnect application

Two types of high chromium ferritic steels envisaged as construction materials for SOFC interconnects, were investigated in respect to microstructure and creep in the proposed application temperature range from 700 to 800 °C. The steel compositions mainly differed in the amounts of the Laves phase forming elements Nb, W and Si. The steel containing these alloying additions exhibited substantially higher creep resistance in the temperature range 700-800 °C than the high purity steel. The Laves phase formation occurred trans- as well as intragranular whereby the extent and size of grain boundary precipitates increased with increasing exposure time. Especially at 800 °C the precipitates inside the grains virtually completely vanished after longer exposure times and only intergranular precipitates remained. This change in precipitate morphology resulted especially at 800 °C in a decrease of creep resistance with increasing exposure time, although the Laves phase containing steel still exhibited higher creep strength than the high purity steel.     

The Measurement of Compressive Creep Deformation and Damage Mechanisms in a Single-Phase Alumina Part I Grain boundary sliding

Grain boundary sliding (GBS) has been hypothesized to act as the primary driving force for the nucleation and growth of grain boundary cavities in ceramics undergoing creep. In addition, GBS is often a major mode of deformation during high-temperature creep. This paper demonstrates the importance of GBS with mode II GBS measurements performed using a stereoimaging technique on a single-phase alumina tested under constant compressive stresses of 70 and 140 MPa at 1600 °C. Measurements were taken at constant time intervals during creep. The results support previous observations that GBS is stochastic and history independent. GBS displacements at given time intervals are shown to fit a Wiebull distribution. During steady-state creep, GBS displacements increased linearly with time at a constant sliding rate of 6.0 × 10–5 m s–1 at 70 MPa and 1.3 × 10–4 m s–1 at 140 MPa. Also, an average of 67% of the grain boundaries exhibited measurable sliding throughout the creep life of the 140 MPa test. Results of the GBS measurements are used to modify an existing creep model describing stochastic GBS. In part II of this paper [1], the GBS measurements reported are related to the associated creep cavitation measured in specimens tested under identical conditions.     

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.     

The effect of carbon containing atmosphere on the structure and mechanical properties of Fe-32Mn-9.4Al-1C-1.27Si alloy

The effect of a carbon containing atmosphere on the microstructure and mechanical properties of Fe-32Mn-9.4Al-1C-1.27Si alloy was investigated in this work. Surface oxide nodules and grain boundary oxides were found to form on this alloy when it was annealed in carbon-containing air at 1050 °C for 1 h. The oxidation reaction was thought to be the result of the green rot attack process. This alloy was embrittled severely by the carbon-containing air through the formation of surface oxide nodules and grain boundary oxide. The carbon-containing air enhanced the oxidation rate of this alloy at 1050 °C. The structure of the oxide nodules formed on this alloy in the carbon-containing air was similar to that observed on a FeMnAl alloy heated in 1000 °C air for 24 h.     

High creep exponents in a nearly-lamellar γ-based titanium aluminide intermetallic

Secondary creep data are reported for an extruded nearly-lamellar Ti-48Al-1.5Cr-alloy tested in a temperature range of 700 to 900°C. Within this temperature regime, this alloy exhibits a two-stage creep deformation behavior, with relatively high (approximately 8–12) creep exponents occurring in the high stress/high temperature regime. The high exponents in this regime are explained by dynamic recrystallization phenomena observed ₂ + in the nearly-lamellar microstructure.