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.     

The influence of temperature cycling on the creep properties of Nickel 201 and Inconel 600 in combustion gas

The effect of temperature cycling on the creep behaviour of Nickel 201 and Inconel 600 in combustion gas has been studied. Specimens were tested both at constant temperature, 900° C, and at 900° C interrupted by temperarature drops down to 510° C. The creep straining has been analysed with respect to a weighted time parameter which includes the creep contribution during the lower temperatures of each cycle. With respect to this compensated time parameter, the temperature variations were generally observed to result in a strong acceleration in creep. The effect seemed to increase with increasing frequency of temperature drops, increasing grain size and decreasing stress. Thus, at low stress levels, large-grained specimens of both alloys experienced an acceleration even inabsolute creep rate upon cycling. The grain size dependency indicates that the destructive effect of the cycles is caused by crack formation. Surface cracking associated with grain boundary oxidation seemed to be the dominant cracking mode. It is suggested that, during creep in oxidizing environments, repeated periods of cooling might strongly accelerate the growth of surface creep cracks due to the difference in thermal expansion between metals and oxides. This difference causes high tensile stresses to arise in the metal in front of the grain boundary oxides, and the stresses are assumed to be high enough to nucleate microcracks along the boundary.     

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

Tensile creep behaviour of a silicon carbide-based fibre with a low oxygen content

The high-temperature mechanical behaviour and microstructural evolution of experimental SiC fibres (Hi-Nicalon) with a low oxygen content (<0.5 wt%) have been examined up to 1600 °C. Comparisons have been made with a commercial Si-C-O fibre (Nicalon Ceramic Grade). Their initial microstructure consists of -SiC crystallites averaging 5–10 nm in diameter, with important amounts of graphitic carbon into wrinkled sheet structures of very small sizes between the SiC grains. The fall in strength above 800 °C in air is related to fibre surface degradation involving free carbon. Crystallization of SiC and carbon further develops in both fibres subject to either creep or heat treatment at 1300 °C and above for long periods. The fibres are characterized by steady state creep and greater creep resistance (one order of magnitude) compared to the commercial Nicalon fibre. The experimental fibre has been found to creep above 1280 °C under low applied stresses (0.15 GPa) in air. Significant deformations (up to 14%) have been observed, both in air and argon above 1400 °C. The stress exponents and the apparent activation energies for creep have been found to fall in the range 2–3, both in air and argon, and in the range 200–300 kJ mol^–1 in argon and 340–420 kJ mol^–1 in air. The dewrinkling of carbon layer packets into a position more nearly aligned with the tensile axis, their sliding, and the collapse of pores have been proposed as the mechanisms which control the fibre creep behaviour.     

Silicon carbide fibre reinforced glass-ceramic matrix composites exhibiting high strength and toughness

Silicon carbide fibre reinforced glass-ceramic matrix composites have been investigated as a structural material for use in oxidizing environments to temperatures of 1000° C or greater. In particular, the composite system consisting of SiC yarn reinforced lithium aluminosilicate (LAS) glass-ceramic, containing ZrO₂ as the nucleation catalyst, has been found to be reproducibly fabricated into composites that exhibit exceptional mechanical and thermal properties to temperatures of approximately 1000° C. Bend strengths of over 700 MPa and fracture toughness values of greater than 17 MN m^–3/2 from room temperature to 1000° C have been achieved for unidirectionally reinforced composites of 50 vol% SiC fibre loading. High temperature creep rates of 10^–5 h^–1 at a temperature of 1000° C and stress of 350 MPa have been measured. The exceptional toughness of this ceramic composite material is evident in its impact strength, which, as measured by the notched Charpy method, has been found to be over 50 times greater than hot-pressed Si₃N₄.     

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.     

Estimation of remaining creep life of an aluminium alloy from creep crack density measurements

Long transverse test pieces of fully aged RR58 plate were stressed in tension at 278 and 308 MPa at 120° C for various fractions of their creep lives. The test pieces were subsequently sectioned, mechanically and electrolytically polished and the numbers of cracks per square millimetre were measured by optical microscopy. The crack density, n, increased linearly with creep strain at both stress levels. No accurate assessment of the variation of n with time was possible. Good agreement between the crack densities measured on duplicate microsections was achieved when the crack density was greater than 10 cracks mm^–2. The crack densities in the uniformly strained portions of 11 test pieces from the same plate, fractured at 150° C at stresses within the range 200 to 290 MPa were also measured. The crack density decreased from 45 cracks mm^–2 at 200 MPa to 4 cracks mm^–2 at 290 MPa. A regression equation n/ge=164 – 0.57 (where is the applied stress) was derived assuming linear n versus relationships at 150° C. The 90% confidence limits were derived for the determination of an unknown stress level from a single measurement of n/. Of the creep life prediction methods discussed, only the correlation of creep crack density and creep strain is of sufficient accuracy and this only when the creep stress and creep temperature are low, i.e. only for those conditions which would develop a high crack density at small fractions of the creep life.     

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.     

The creep behaviour of Synroc and alumina

The creep of Synroc C and alumina in four-point bending in argon was investigated in terms of the relaxed symmetric stress and the reference asymmetric stress; the alumina being used as a reference material. The creep tests were undertaken in the temperature range from 850°C to 1300°C. The rupture behaviour of Synroc at 950°C indicated a high stress exponent, and that the creep ductility was unusual in that the strain increased with increasing test time. A scanning electron miscroscopy examination of Synroc after creep revealed the development of defect-free oxidised surface layers. For Synroc, neither prior exposure to pre-heating in air, nor prior indentation affected the creep rate behaviour. This was attributed to the formation of the oxidised surface layers and the associated healing effects of the damage produced by the indentations.     

Tensile strength of silicon carbide fibre bundles at elevated temperatures

The mechanical properties of commercially available SiC-based ceramic fibres were measured in the temperature range from 400–1300°C. The measurements were performed in air and in inert gas atmospheres, respectively. The Nicalon and Tyranno fibres were tested as filament bundles and the decrease in strength occurring at temperatures above 600 °C was found in both atmospheres. To obtain a well-defined gauge length at the testing temperature, a furnace with very steep temperature gradients at both ends was built. To eliminate grip-induced damage in the heating zone the fibre bundles were fixed outside the furnace with cold grip units. These grips guaranteed the uniformity of load distribution imposed on to each of the individual filaments in the fibre bundle. A significant shrinkage of the fibres occurring during the creep test performed under low loads indicates a change in the microstructure of the fibres at high temperatures.     

Enhancement of the diffusional creep of polycrystalline Al2O3 by simultaneous doping with manganese and titanium

The effect of simultaneous doping with manganese and titanium on diffusional creep was studied in dense, polycrystalline alumina over a range of grain sizes (4–80m) and temperatures (1175–1250° C). At a total dopant concentration of 0.32–0.37 cation %, diffusional creep rates were enhanced considerably such that the temperature at which cation mass transport was significant was suppressed by at least 200° C compared to that observed in undoped material. The Mn-Ti (and Cu-Ti) dopant couple was far more effective in enhancing creep rates and suppressing sintering temperatures than the Fe-Ti couple. The enhanced mass transport kinetics are believed to be caused by significant increases in both aluminium lattice and grain-boundary diffusion. When aluminium grain-boundary diffusion is enhanced by increasing the concentration of divalent impurity (Mn²⁺, Fe²⁺) or by creep testing at low temperatures, creep deformation is Newtonian viscous.     

The creep of sapphire filament with orientations close to the c-axis

Sapphire filament oriented within 2 1/2° of the crystallographic c-axis underwent creep by a mechanism other than slip on the basal planes at temperatures above 1600° C. There was a stress below which creep could not be detected; this decreased from 180 MNm^–2 at 1600° C to 65 MNm^–2 at 1800° C. The total tensile strain obtained never exceeded 5%. Fracture occurred during a linear stage of creep in which the stress exponent of the strain-rate was approximately 6. The creep mechanism appeared to be slip on {20¯2¯1} 01 T2 (morphological unit cell). A filament in which the c-axis lay at 6° to the filament axis deformed by localized basal slip. The accompanying local latice rotations produced fracture at a small overall strain, usually less than 0.5%. The results demonstrate extreme anisotropy of creep in sapphire crystals.     

High-temperature creep response of a commercial grade siliconized silicon carbide

Creep studies conducted in four-point flexure of a commercial siliconized silicon carbide (Si-SiC, designated as Norton NT230) have been carried out at temperatures of 1300, 1370, and 1410°C in air under selected stress levels. The Si-SiC material investigated contained 90% -SiC, 8% discontinuous free Si, and 2% porosity. In general, the Si-SiC material exhibited very low creep rates (2 to 10×10^–10 s^–1) at temperatures 1370°C under applied stress levels of up to 300 MPa. At 1410°C, the melting point of Si, the Si-SiC material still showed relative low creep rates (0.8 to 3 × 10^–9 s^–1) at stresses below a threshold value of 190 MPa. At stresses >190 MPa the Si-SiC material exhibited high creep rates plus a high stress exponent (n=17) as a result of slow crack growth assisted process that initiated within Si-rich regions. The Si-SiC material, tested at temperature 1370°C and below the threshold of 190 MPa at 1410°C, exhibited a stress exponent of one, suggestive of diffusional creep processes. Scanning electron microscopy observations showed very limited creep cavitation at free Si pockets, suggesting the discontinuous Si phase played no or little role in controlling the creep response of the Si-SiC material when it was tested in the creep-controlled regime.     

Microstructure and mechanical characteristics of alpha-alumina-based fibres

The high-temperature mechanical behaviour of alumina-based ceramic fibres has been investigated by the comparison of a dense pure alumina fibre, a porous pure alumina fibre and a zirconia-reinforced dense fibre. Tensile and creep tests have been conducted up to 1300°C in air in parallel with microstructural investigations on the as-received and tested fibres. Room-temperature behaviour of the fibres is close to that of bulk materials having the same microstructure, but the fibre form allows higher failure stresses to be attained. High-temperature deformation of the three fibres is achieved by grain-boundary sliding ( ), and is accompanied by isotropic grain growth. The specific microstructures of each fibre induce differences in the creep threshold levels as a function of temperature and stress and also in creep rates and resistance to damage. Despite better resistance to creep and damage of the zirconia-reinforced fibre, alumina-based fibres are limited to applications below 1100°C. Grain boundaries are the principal cause of mechanical degradation at high temperature with these fibres.     

Creep rupture studies of two alumina-based ceramic fibres

Creep rupture tests were performed in air on two polycrystalline oxide fibres (Al₂O₃, Al₂O₃-ZrO₂) using both filament bundles and single filaments. Tests were performed at applied stresses ranging from 50–150 MPa over the temperature range 1150–1250 °C. Under these conditions, creep rates for the alumina-zirconia fibre ranged from 4.12 × 10^–8–7.70 × 10^–6s^–1. At a given applied stress, at 1200°C, creep rates for the alumina fibre were 2–10 times greater than those of the alumina-zirconia fibre. Stress exponents for both fibres ranged from 1.2–2.8, while the apparent activation energy for creep of bundles of the alumina-zirconia fibre was determined to be 648 ± 100kJmol^–1. For the alumina-zirconia fibre, the two test methods yielded similar steady-state creep rates, but the rupture times were generally found to be longer for bundles than for single filaments. The steady-state creep behaviour of these alumina-based fibres is consistent with an interface-reaction-controlled diffusion-controlling mechanism.     

Creep of reaction-bonded silicon nitride

The high temperature mechanical properties, mainly the creep behaviour of reaction-bonded silicon nitride (RBSN), a new engineering ceramic for the gas turbine, have been a point of considerable interest. During the recent development a remarkable increase of the creep resistance of RBSN has been reached and the latest data show creep rates of below 10^–6 h^–1 at 1300° C and 70 to 100 MM m^–2. Activation energies between 540 and 700 kJ mol^–1 and stress exponents of 1in vacuo. Methods to determine the amount of internal oxidation,namely X-ray diffraction analysis, electron microprobe analysis and Rutherford backscattering of -particles were used. The deleterious effects of the internal oxidation are explained in terms of the microstructure, mainly porosity and pore size distribution, and ways to avoid this effect are discussed.     

Effects of heat treatments on the creep properties of a hot pressed silicon nitride ceramic

Effects of heat treatment in an argon atmosphere at high temperatures for varying times on the creep properties of a Y₂O₃-Al₂O₃ (8-2 wt%) doped hot pressed silicon nitride (HPSN) ceramic were investigated. It was observed from the creep measurements that higher temperature, i.e. 1360C, and longer time, i.e. 8 h, heat treatment in an argon atmosphere improved the creep properties, (e.g. secondary creep rate) of this material. Heat treatment at a lower temperature of 1300C and for a shorter time of 4 h did not change the creep behaviour. Improvement of the creep properties was related to the crystallization of an amorphous grain boundary phase by heat treatment. Secondary creep rate parameters of the as-received material: stress exponent, n (2.95–3.08) and activation energy, Q (634–818 kJ mol^S–1), were in the range of values found by other investigators for various hot pressed silicon nitride ceramics.     

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.     

Steady-state creep of an alloy based on the intermetallic compound Ni3Al(γ′)

An investigation of the steady-state creep of a Ni₃Al.10 at% Fe alloy () has shown that two creep mechanisms were operative over the temperature range 530 to 930° C. The experimental data at low temperatures (below 680° C) were not consistent with any of the established creep theories. However, the experimental data were in good agreement with a proposed model for cross-slip from octahedral {111} planes on to cube {100} planes in Li₂ crystals. Above 680° C, the rate-controlling mechanism, which had an activation energy of 3.27eV atom^–1, is considered to be the removal/production of APBs during climb.     

The torsional creep of carbon fibre reinforced epoxide resins

The torsional creep of composite specimens containing 60% by volume of unidirectional HT-S carbon fibre, and of unreinforced epoxide resin has been studied. Measurements were made at temperatures of 25, 50, 75 and 90° C, in two environments — air and water. Torsional preloads of up to 40% of the ultimate torsional strength were applied. All the specimens showed primary and secondary creep behaviour during the 170 h test period, and a few resin ones tertiary creep. The effects, on the secondary creep rate, of varying the proportion of hardener in the matrix and the cure schedule were marked. The lowest creep rate for a given set of test conditions was obtained when the stoichiometric amount of hardener was used and the maximum cure given. Using specimens of this optimum type, more detailed studies of creep were performed. In all cases the activation energy for secondary creep lies between 5 and 6.3 kcal (g mol)^–1 indicating that the same basic mechanism occurs in each instance. The shear stress,, was found to be proportional to the logarithm of the secondary creep rate.