Creep and Stress Rupture Behavior of an Advanced Silicon Nitride: Part II, Creep Rate Behavior

In Part I of this paper, experimental observations on creep testing of 74 tensile specimens of an advanced silicon nitride were presented. In this part, equations are developed for predicting creep rates in the primary and secondary regimes in the temperature range 1477–1673 K. The resulting model predicts creep strain rates to within a factor of two. The underlying phenomenological basis, which employs an activation energy approach, is discussed. The mechanisms that are likely to be responsible for the transiency of the primary creep regime and for the unique stress and temperature dependencies of the creep rates are explored.     

Kinetics and Mechanisms of High-Temperature Creep in Silicon Carbide: II, Chemically Vapor Deposited

Chemically vapor deposited (CVD) silicon carbide was subjected to constant compressive stresses (110 to 220 MN/m²) at high temperatures (1848 to 2023 K) in order to determine the controlling steady-state creep mechanisms under these conditions. An extensive TEM study was also conducted to facilitate this determination. The strong preferred crystallographic orientation of this material causes the creep rate to be very dependent on specimen orientation. The stress exponent, n , in the equation εασⁿ was calculated to be 2.3 below 1923 K and 3.7 at 1923 K. The activation energy for steady-state creep was determined to be 175 ± 5 kJ/mol throughout the temperature range employed. At temperatures between 1673 and 1873 K, the controlling creep mechanism for CVD Sic is dislocation glide, which is believed to be controlled by the Peierls stress. Although the activation energy does not change, the increase in the stress exponent for samples deformed at 1923 K suggests that the controlling creep mechanism becomes dislocation glide/climb controlled by climb.     

Creep and Stress–Strain Behavior after Creep for SiC Fiber Reinforced, Melt-Infiltrated SiC Matrix Composites

Silicon carbide fiber (Hi-Nicalon Type S, Nippon Carbon) reinforced silicon carbide matrix composites containing melt-infiltrated silicon were subjected to creep at 1315°C at three different stress conditions. For the specimens that did not rupture after 100 h of tensile creep, fast-fracture experiments were performed immediately following the creep test at the creep temperature (1315°C) or after cooling to room temperature. All specimens demonstrated excellent creep resistance and compared well to the creep behavior published in the literature on similar composite systems. Tensile results on the after-creep specimens showed that the matrix cracking stress actually increased, which is attributed to stress redistribution between composite constituents during tensile creep.     

Dynamic fatigue behavior of lithium hydride at elevated temperatures

The fatigue properties of lithium hydride (LiH) are crucial to its application as neutron shielding and moderating at elevated temperatures. The dynamic fatigue tests of LiH were investigated with the notched 3-point bend (3 PB) specimens over ranges of loading rates at RT up to 400 °C. At RT, the results showed that slow crack growth (SCG) occurred prior to failure as the minor deviation from linearity to nonlinearity in the load-deflection curves. In addition, the fracture strength of LiH decreased with decreasing stress rate and the SCG zone gradually became smaller with higher stress rates, indicating evident dynamic fatigue phenomenon. However, the trends were quite different at 200, 300 and 400 °C due to accumulative creep damage for low stress rates at elevated temperatures. With increasing temperature and decreasing stress rate, there existed a transition of the dominated failure mechanism, from SCG to creep rupture. Evidence of very small SCG zone could also be detected at the notch for the failure dominated by creep rupture.     

Creep rupture of a linear polyethylene: 1. Rupture and pre-rupture phenomena

The creep rupture behaviour of a high-density polyethylene was studied for material prepared at two different cooling rates. The rupture phenomena were dependent upon the morphology. The slow-cooled specimens had a degenerated spherulitic structure and all underwent brittle rupture. The fast-cooled specimens had a banded spherulitic structure and exhibited either ductile or brittle rupture depending upon the applied stress. Ductile creep rupture was associated with a large tertiary creep strain, with macro-necking and a stress whitening which corresponded to an increase in volumetric strain. Brittle creep rupture was associated with an absence of macro-necking, and either an absence or a small amount of tertiary creep. Stress whitening corresponding to a decrease in volumetric strain was a feature of both forms of failure above a threshold value of stress.     

Creep properties of melt infiltrated SiC/SiC composites with Sylramic™-iBN and Hi-Nicalon™-S fibers

Isothermal tensile creep tests were conducted on 2D woven and laminated, 0/90 balanced melt infiltration (MI) SiC/SiC composites at stress levels from 48 to 138 MPa and temperatures to 1400°C in air. Effects of fiber architecture and fiber types on creep properties, influence of accumulated creep strain on in-plane tensile properties, and the dominant constituent controlling the creep behavior and creep rupture properties of these composites were investigated. In addition, the creep parameters of both composites were determined. Results indicate that in 2D woven MI SiC/SiC composites with Sylramic™-iBN or Hi-Nicalon™-S fibers, creep is controlled by chemical vapor infiltration (CVI) SiC matrix, whereas in 2D laminated MI SiC/SiC composites with Hi-Nicalon™-S fibers, creep is controlled by the fiber. Both types of composites exhibit significant variation in creep behavior and rupture life at a constant temperature and stress, predominantly due to local variation in microstructural inhomogeneity and stress raisers. In both types of composites at temperatures >1350°C, residual silicon present in SiC matrix to reacts with SiC fibers and fiber coating causing premature creep rupture. Using the creep parameters generated, the creep behaviors of the composites have been modeled and factors influencing creep durability are discussed.     

Compression Creep Characteristics of 8-mol%-Yttria-Stabilized Cubic-Zirconia

Constant stress compression creep tests were conducted on 8-mol%-yttria-stabilized cubic-zirconia (8YCZ) over stress (ς), temperature, and grain-size ranges from ∼20 to 300 MPa, 1673 to 1773 K, and 4 to 8 μm, respectively. Creep data were analyzed in terms of the relationship [epsivdot] ∝ς ⁿ , where [epsivdot] is the strain rate and n the stress exponent. Although the experimental data yielded a stress exponent of n & 2, analysis of the results with compensation of significant concurrent grain growth revealed that the true stress exponent was n ∼ 1. The results were consistent with deformation by the Coble creep mechanism. Experiments at stresses greater than ∼100 MPa revealed a transition from grain-size-dependent Coble diffusion creep to grain-size-independent intragranular dislocation creep.     

Comparison of the Creep and Creep Rupture Performance of Two HIPed Silicon Nitride Ceramics

Measurements of the tensile creep and creep rupture behavior were used to evaluate the long-term mechanical reliability of a commercially available and a developmental hot isostatically pressed (HIPed) silicon nitride. Measurements were conducted at 1260° and 1370°C utilizing button–head tensile specimens. The stress and temperature sensitivities of the secondary creep rates were used to estimate the stress exponent and activation energy associated with the dominant creep mechanism. The stress and temperature dependencies of creep rupture life were determined by continuing individual creep tests to specimen failure. Creep deformation in both materials was associated with cavitation at multigrain junctions. Two-grain cavitation was also observed in the commercial material. Failure in both materials resulted from the evolution of an extensive damage zone. The failure times were uniquely related to the creep rates, suggesting that the zone growth was constrained by the bulk creep response. The fact that the creep and creep rupture behaviors of the developmental silicon nitride were significantly improved compared to those of the commercial material was attributed to the absence of cavitation along two-grain junctions in the developmental material.     

Behaviour of concrete under thermal steady state and non-steady state conditions

Stress–strain behaviour of concrete at elevated temperatures is extremely complex and is not completely understood up to now. The creep properties of concrete at temperatures up to 300°C thus need to be determined, as well as the thermal stability of concrete during repeated cycles of heating and cooling. In this report the results of recent high temperature experiments with normal concrete specimens are presented. The main objectives of the tests were to investigate the dependence of strength and elasticity on temperature and to study the creep and deformation characteristics of concrete at temperatures up to 450°C. Transient creep data, i.e. data derived under transient temperature conditions, are compared with creep data which were measured at constant elevanted temperatures. The results suggest that transient creep values and steady state creep values in some cases may be of the same magnitude. The creep measurements appear to be in good agreement with data presented by other workers. However, the scatter in all data increases significantly with increasing temperature and differences of more than 100% can be observed. When loaded concrete specimens were cooled down to ambient temperature exptraordinarily large compressive strains can be observed. The experiments indicate clearly the considerable strain capacity of normal structural concrete can be used at temperatures higher than 100°C. In areas of high stress concentrations a tures. On the other hand, with respect to the whole structure it is necessary to limit the deformations. For a constant maximum temperature this can only be done by limiting the admissible stresses. The test results permit an initial estimation of maximum permissible stress and temperature values.     

Accelerated characterization of a chopped fiber composite using a strain energy failure criterion

The creep and creep rupture response of a chopped fiber composite material (SMC-R50) were investigated experimentally and analytically. The goal of this research was to use the short time laboratory data to predict long time creep and creep rupture behavior. The creep response data up to 200 min duration were obtained at various constant temperature and stress levels. The short time creep data were then modeled using a modified power law equation. The modified power law equation contains the parameters of the so-called accelerated characterization procedure. Using this power law equation, the short time creep response at the elevated temperatures were able to successfully predict the long time creep response at a lower temperature and stress level. To predict the creep rupture behavior, the modified power law equation was then coupled with a strain energy based failure criterion. It was found that the same parameters that were used in the prediction of the long-time creep response can also be used to predict the creep rupture. At a given temperature level, the strain energy density related to creep rupture was found to be a constant. Furthermore, this strain energy density was found to increase with an increase in temperature. With a limited amount of data, it was found that the strain energy based failure criterion coupled with the modified power law equation can be used to predict long time creep rupture behavior.     

The creep mechanism of ceramic matrix composites at low temperature and stress,by a material science approach

This paper deals with the creep mechanism for ceramic matrix composites reinforced by long ceramic fibers in a ceramic or glass-ceramic matrix, tested at low stresses (<400 MPa) and low temperatures, respectively <1673 K for the former and <1373 K for the latter. The macroscopic results give few ideas on the mechanism, but observations at different scales until high resolution evidence brittle damages which lead the authors to use the damage mechanics approach and to demonstrate that a damage creep mechanism is operating for these CMCs in two steps: (1) matrix microcrack development until its saturation, (2) followed by the opening of some of these microcracks enabling under certain conditions creep of the SiC fibers which bridge the microcracks. This was enlightened by precise damage observations on stepping creep tests and by their quantification with automatic image analysis.     

Application of the SIMS Method in Studies of Cr Segregation in Cr-Doped CoO: II, Depth Profiles

Surface segregation-induced depth profiles of Cr were determined for Cr-doped CoO single crystals equilibrated at different temperatures (1373–1673 K) and oxygen partial pressures (10²–10⁵ Pa). It was shown that the shape of the depth profiles depends on both conditions of annealing and subsequent cooling procedure. It has been observed that during slow cooling of specimens from the condition of segregation equilibrium at elevated temperatures to the temperature of the experiment (room temperature), there is substantial change of the concentration profile involving desegregation of Cr (Cr diffusion from the surface to the bulk) resulting in its depletion. It has also been shown that the rate of the desegregation process (the process which results in a decrease of surface concentration) is slower than the lattice transport kinetics of Cr in CoO. It is concluded that the desegregation is rate-controlled by the decomposition of a spinel-type bidimensional surface structure which is formed at elevated temperatures as a result of Cr segregation.     

High-Temperature Tensile Behavior of a Boron Nitride-Coated Silicon Carbide-Fiber Glass-Ceramic Composite

Tensile properties of a cross-ply glass-ceramic composite were investigated by conducting fracture, creep, and fatigue experiments at both room temperature and high temperatures in air. The composite consisted of a barium magnesium aluminosilicate (BMAS) glass-ceramic matrix reinforced with SiC fibers with a SiC/BN coating. The material exhibited retention of most tensile properties up to 1200°C. Monotonic tensile fracture tests produced ultimate strengths of 230–300 MPa with failure strains of ∼1%, and no degradation in ultimate strength was observed at 1100° and 1200°C. In creep experiments at 1100°C, nominal steady-state creep rates in the 10⁻⁹ s⁻¹ range were established after a period of transient creep. Tensile stress rupture experiments at 1100° and 1200°C lasted longer than one year at stress levels above the corresponding proportional limit stresses for those temperatures. Tensile fatigue experiments were conducted in which the maximum applied stress was slightly greater than the proportional limit stress of the matrix, and, in these experiments, the composite survived 10⁵ cycles without fracture at temperatures up to 1200°C. Microscopic damage mechanisms were investigated by TEM, and microstructural observations of tested samples were correlated with the mechanical response. The SiC/ BN fiber coatings effectively inhibited diffusion and reaction at the interface during high-temperature testing. The BN layer also provided a weak interfacial bond that resulted in damage-tolerant fracture behavior. However, oxidation of near-surface SiC fibers occurred during prolonged exposure at high temperatures, and limited oxidation at fiber interfaces was observed when samples were dynamically loaded above the proportional limit stress, creating micro-cracks along which oxygen could diffuse into the interior of the composite.     

Effect of the Matrix and Matrix Bonding on the Creep Behavior of a Unidirectional Carbon–Carbon Composite

Creep tests were performed on single-bundle carbon–carbon specimens at high temperatures (>2310°C) and at high stress levels (>770 MPa). It was found that the creep was very strongly dependent on the filament–matrix interfacial bond. When the bond was good, the typical creep was 3.6% after 5.9 h with the primary creep a high percentage of the total deformation. When the bond was absent (dry bundle), rupture with strain was approximately 140%, and it occurred after only 0.39 h. The marked improvement in creep resistance is attributed to the ability of the matrix to distribute loads evenly and to produce a plastic flow inhibiting triaxial stress state among the filaments.     

Flexural Creep Deformation of ZrB2/SiC Ceramics in Oxidizing Atmosphere

Flexural creep of ZrB₂/0–50 vol% SiC ceramics was characterized in oxidizing atmosphere as a function of temperature (1200°–1500°C), stress (30–180 MPa), and SiC particle size (2 and 10 μm). Creep behavior showed strong dependence on SiC content and particle size, temperature and stress. The rate of creep increased with increasing SiC content, temperature, and stress and with decreasing SiC particle size, especially, at temperatures above 1300°C. The activation energy of creep showed linear dependence on the SiC content increasing from about 130 to 511 kJ/mol for ceramics containing 0 and 50 vol% 2-μm SiC, respectively. The stress exponent was about 2 for ZrB₂ containing 50 vol% SiC regardless of SiC particle size, which is an indication that the leading mechanism of creep for this composition is sliding of grain boundaries. Compared with that, the stress exponent is about 1 for ZrB₂ containing 0–25vol% SiC, which is an indication that diffusional creep has a significant contribution to the mechanism of creep for these compositions. Cracking and grain shifting were observed on the tensile side of the samples containing 25 and 50 vol% SiC. Cracks propagate through the SiC phase confirming the assumption that grain-boundary sliding of the SiC grains is the controlling creep mechanism in the ceramics containing 50 vol% SiC. The presence of stress, both compressive and tensile, in the samples enhanced oxidation.     

Experience with a full notch creep test in determining the stress crack performance of polyethylenes

A laboratory method to measure the stress crack resistance of polyethylenes was developed and has since been applied in our laboratory for more than twelve years. The experience gathered since our first paper is herewith reported. The creep rupture test of circumferentially notched specimens cut from plaques or pipes has proven to be a rapid and reliable method to evaluate the stress crack performance. Surfactant-assisted stress cracking was employed to accelerate testing. The stress crack resistance of several polyethylene samples was studied with respect to its dependence on stress, temperature, and environment. The creep rupture behavior at different temperatures could be superposed by horizontal shifting when the stresses were normalized in proportion to the respective bulk yield stresses. The notch tip radius turned out not to be very crucial, and variation of the nominal concentration of the surfactants, nonylphenolpolyglycolethers, scarcely affected slow crack growth. Acceleration of testing by surfactants equalized property differences to a noticeable extent but did not influence the ranking of the materials. The activation energy of crack growth was in the expected range. Defects introduced into the line by butt joint welding were precisely modeled by the full notch creep test.     

Cavity Development During Creep Deformation in Alumina with a Bimodal Grain Size Distribution

An alumina sample, codoped with equimolar proportions of magnesia and zirconia, exhibited a bimodal grain size distribution after hot-pressing. Flexural creep experiments were performed on this material at temperatures of 1673 and 1773 K in air. Inspection of the deformed specimens revealed extensive creep cavitation, with cavities developing preferentially in the coarse-grained regions. The nucleation, growth, and interlinkage of the cavities led to the formation of cracks. Crack growth occurred in the coarse-grained regions by the linkage of cavities with the crack tip. However, several cracks were observed to terminate after extending up to a fine-grained region of a specimen. A model has been developed to rationalize the observation that preferential cavitation occurs in the coarse-grained regions of a specimen undergoing creep deformation.     

Dense Amorphous Zirconia–Alumina by Low-Temperature Consolidation of Spray-Pyrolyzed Powders

Metastable amorphous ZrO₂-Al₂O₃ powders were hot-pressed at low temperatures (873 and 923 K), under moderately high pressures (500 and 750 MPa), and amorphous pellets with 1%-8% porosity were obtained. Crystallization of the amorphous pieces in the temperature range of 1173–1673 K produced a range of ultrafine microstructures, the finest of which had grains of tetragonal (ZrO₂-40-mol%-Al₂O₃) solid solution 6–8 nm in size that formed at 1173 K. Submicrometer grain sizes of the equilibrium monoclinic ZrO₂ and alpha-Al₂O₃ were stable against coarsening at 1673 K. The new technique was applied to produce a SiC-reinforced composite with an amorphous ZrO₂-80-mol%-Al₂O₃ matrix; the high matrix sinterability overcame the reinforcement constraint. The results suggest a possible solution to the difficulties in the bulk processing of amorphous, nanocrystalline, and other novel ceramics.     

Predicting the creep rupture life of polyethylene pipe

A number of techniques have been developed in the past for the prediction of the dependence of the creep rupture life of polyethylene pipe on applied stress and temperature. It is now proposed that, using a modified form of the activated rate procss equation in which the activation volume varies predictably with temperature, a generalized equation may be derived which describes the “brittle” creep rupture curve over a range of temperatures, and also allows the use of a Larson-Miller type equation. Since the known “ductile” creep rupture curve at 20°C can be extrapolated from measurements carried out over a short period at room temperature in the laboratory, the intersection point between the extrapolated “ductile” curve and the calculated “brittle” curve can easily be calculated. If the proposed method is applied to creep rupture data obtained from Hoechst AG (GM5010, HDPE pipe) as an example, a transition at about 11 years is predicted.     

Tensile Creep and Creep Rupture Behavior of Monolithic and SiC-Whisker-Reinforced Silicon Nitride Ceramics

The tensile creep and creep rupture behavior of silicon nitride was investigated at 1200° to 1350°C using hotpressed materials with and without SiC whiskers. Stable steady-state creep was observed under low applied stresses at 1200°C. Accelerated creep regimes, which were absent below 1300°C, were identified above that temperature. The appearance of accelerated creep at the higher temperatures is attributable to formation of microcracks throughout a specimen. The whisker-reinforced material exhibited better creep resistance than the monolith at 1200°C; however, the superiority disappeared above 1300°C. Considerably high values, 3 to 5, were obtained for the creep exponent in the overall temperature range. The exponent tended to decrease with decreasing applied stress at 1200°C. The primary creep mechanism was considered cavitationenhanced creep. Specimen lifetimes followed the Monkman–Grant relationship except for fractures with large accelerated creep regimes. The creep rupture behavior is discussed in association with cavity formation and crack coalescence.