Creep of Nextel™720/alumina–mullite ceramic composite at 1200 °C in air,argon, and steam

The tensile creep behavior of an oxide–oxide continuous fiber ceramic composite was investigated at 1200 °C in laboratory air, in steam and in argon. The composite consists of a porous alumina–mullite matrix reinforced with laminated, woven mullite/alumina (Nextel™720) fibers, has no interface between the fiber and matrix, and relies on the porous matrix for flaw tolerance. The tensile stress–strain behavior was investigated and the tensile properties measured at 1200 °C. The elastic modulus was 74.5 GPa and the ultimate tensile strength was 153 MPa. Tensile creep behavior was examined for creep stresses in the 70–140 MPa range. Primary and secondary creep regimes were observed in all tests. Creep run-out (set to 100 h) was achieved in laboratory air for creep stress levels ?91 MPa. The presence of either steam or argon accelerated creep rates and reduced creep lifetimes. Composite microstructure, as well as damage and failure mechanisms were investigated.     

Effect of frequency and environment on fatigue behavior of a CVI SiC/SiC ceramic matrix composite at 1200 °C

The fatigue behavior of a SiC/SiC CMC (ceramic matrix composite) was investigated at 1200 °C in laboratory air and in steam environment. The composite consists of a SiC matrix reinforced with laminated woven Hi-Nicalon™ fibers. Fiber preforms had boron nitride fiber coating applied and were then densified with CVI SiC. Tensile stress-strain behavior and tensile properties were evaluated at 1200 °C. Tension-tension fatigue tests were conducted at frequencies of 0.1, 1.0, and 10 Hz for fatigue stresses ranging from 80 to 120 MPa in air and from 60 to 110 MPa in steam. Fatigue run-out was defined as 10⁵ cycles at the frequency of 0.1 Hz and as 2 × 10⁵ cycles at the frequencies of 1.0 and 10 Hz. Presence of steam significantly degraded the fatigue performance. In both test environments the fatigue limit and fatigue lifetime decreased with increasing frequency. Specimens that achieved run-out were subjected to tensile tests to failure to characterize the retained tensile properties. The material retained 100% of its tensile strength, yet modulus loss up to 22% was observed. Composite microstructure, as well as damage and failure mechanisms were investigated.     

Correlation of elastic properties of melt infiltrated SiC/SiC composites to in situ properties of constituent phases

The ability to correlate the elastic properties of melt infiltrated SiC/SiC composites to properties of constituent phases using a hybrid Finite Element approach is examined and the influence of material internal features, such as the fabric architecture and intra-tow voids, on such correlation is elucidated. Tensile testing was carried out in air at room temperature and 1204 °C. Through-thickness compressive elastic modulus utilizing the stacked disk method was measured at room temperature. In situ moduli of constituent materials were experimentally evaluated using nano-indentation techniques at room temperature. A consistent relationship is observed between constituent properties and composite properties for in-plane normal and shear moduli and Poisson’s ratio at room temperature. However, experimental data for through-thickness compressive elastic modulus is lower than the calculated value. It is hypothesized that the existence of voids inside the fiber tows and their collapse under compressive loads is the cause of such discrepancy. Estimates for the change in elastic moduli of constituent phases with temperature were obtained from literature and used to calculate the elastic properties of the composites at 1204 °C. A reasonable correlation between the in-plane elastic moduli of the composite and the in situ elastic properties of constituent phases is observed.     

Impression creep behaviour of magnesium alloy-based hybrid composites in the transverse direction

The creep behaviour of a creep-resistant AE42 magnesium alloy reinforced with Saffil short fibres and SiC particulates in various combinations has been investigated in the transverse direction, i.e., the plane containing random fibre orientation was perpendicular to the loading direction, in the temperature range of 175–300 °C at the stress levels ranging from 60 to 140 MPa using impression creep test technique. Normal creep behaviour, i.e., strain rate decreasing with strain and then reaching a steady state, is observed at 175 °C at all the stresses employed, and up to 80 MPa stress at 240 °C. A reverse creep behaviour, i.e., strain rate increasing with strain, then reaching a steady state and then decreasing, is observed above 80 MPa stress at 240 °C and at all the stress levels at 300 °C. This pattern remains the same for all the composites employed. The reverse creep behaviour is found to be associated with fibre breakage. The apparent stress exponent is found to be very high for all the composites. However, after taking the threshold stress into account, the true stress exponent is found to range between 4 and 7, which suggests viscous glide and dislocation climb being the dominant creep mechanisms. The apparent activation energy Q_c was not calculated due to insufficient data at any stress level either for normal or reverse creep behaviour. The creep resistance of the hybrid composites is found to be comparable to that of the composite reinforced with 20% Saffil short fibres alone at all the temperatures and stress levels investigated. The creep rate of the composites in the transverse direction is found to be higher than the creep rate in the longitudinal direction reported in a previous paper.     

Microstructure effect on mechanical properties of in situ synthesized titanium matrix composites reinforced with TiB and La2O3

High temperature titanium matrix composites (TMCs) with different volume fraction of reinforcements were insitu synthesized by casting and hot forging. An effort was made to investigate the mechanical properties as a function of the microstructure of composites. Tensile tests were performed at room temperature, 600 °C, 650 °C and 700 °C respectively. Creep behavior at 650 °C was characterized in the stress range of 200-300 MPa. Results indicated that the composite with 2.11 vol.% reinforcements had the highest tensile strength and lowest steady state creep rate. Morphology of TiB whiskers was critical to mechanical properties of TMCs. TiB whiskers fracture and debonding acted as the dominant failure modes.     

Tensile properties and damage behaviors of Csf/Mg composite at elevated temperature and containing a small fraction of liquid

The mechanical properties of magnesium matrix composites reinforced by pyrolytic carbon coated short carbon fiber at temperatures close to and above the solidus temperature were investigated by tensile tests for the first time. Microstructural observations and fractographic analysis were carried out in order to reveal the damage mechanisms of the composites with different fraction of liquid. Tensile strength of the composites decreased monotonously with temperature, an exponential equation relating the tensile strength to temperature and liquid fraction was derived. The elongation increases monotonously with temperatures from 400 °C to 428 °C (solidus temperature), and then decreases gradually with increasing fraction of liquid except a trough at 432 °C. The composites almost have no ductility and cannot sustain tensile stress when the fraction of liquid reaches 8%. The amount and distribution of liquid phase in the composites directly determines their mechanical properties and damage behavior.     

Effect of oxidation on the creep behaviour of copper–chromium in situ composite

The creep deformation and fracture behaviours of a Cu–Cr in situ composite were investigated in air and in vacuum over a temperature range of 400–650 °C to study the effect of environment. The similarities of the activation energy and the stress exponent in air and in vacuum strongly suggest that the oxygen and/or the oxide have no direct effect on the deformation mechanism of Cu–Cr in situ composite. The higher creep rate of the composite in air than in vacuum is due to the gradual decrease of the cross-sectional area of the matrix due to increasing thickness of the oxide layer. The mechanism of damage was found to be similar for all the creep tests performed.     

Effect of β heat treatment temperature on microstructure and mechanical properties of in situ titanium matrix composites

TiB and La₂O₃ reinforced titanium matrix composites were in situ prepared by casting and hot working. An effort was made to investigate relationship between β heat treatment temperature, microstructure and mechanical properties. Tensile tests were performed at room temperature, 600, 650 and 700 °C, respectively. Results indicated that composites treated at 10 °C above β transus points obtained fine grain microstructures and superior mechanical properties. When composites were treated at 20 °C above β transus points, the larger α colonies sizes led extremely decreased strength and the effect of reinforcements’ volume fraction on matrix of composites was reduced; dominant failure modes at high temperatures also differed from the fine microstructure.     

Fatigue life evaluation for carbon/epoxy laminate composites under constant and variable block loading

This paper presents the results of current research on the fatigue life prediction of carbon/epoxy laminate composites involving twelve balanced woven bidirectional layers of carbon fibres and epoxy resin manufactured by a vacuum moulding method. The plates were produced with 3 mm thickness and 0.66 fibre weight fraction. The dog bone shape specimens were cut from these plates with the load line aligned with one of the fibre directions. The fatigue tests were performed using load control with a frequency of 10 Hz and at room temperature. The fatigue behaviour was studied for different stress ratios and for variable amplitude block loadings. The damage process was monitored in terms of the stiffness loss. The fatigue life of specimens submitted to block loading tests was modelled using Palmgren–Miner’s law and taking in to account the stress ratio effect. The estimated and experimental fatigue lives were compared and good agreement was observed.     

Dynamic compressive behavior of unidirectional IM7/5250-4 laminate after thermal oxidation

Fiber reinforced high temperature polymer matrix composites are currently gaining wide usage in aircraft structures, especially in airframe and engine inlet casing. The failure of composites in worst-case operational conditions mandates the extensive investigation of the mechanical behavior, and the durability in long-term performance and service life under thermal oxidation. In this work, unidirectional IM7 carbon fiber reinforced high-temperature BMI resin composite (IM7/5250-4) were isothermally aged in air for 2 months at 195 °C and 245 °C, respectively. The dynamic behavior of thermally aged composites was investigated on a split Hopkinson pressure bar (SHPB) in three principal directions. The results indicate that thermal oxidation leads to significant reduction in both stiffness and strength of the composites. Optical micrographs of fracture surface and failure pattern of composite after SHPB impact reveals oxidation induced debonding along the fiber–matrix interface due to oxygen diffusion under long-term exposure to elevated temperatures.     

High velocity impact on NCF reinforced composites

In the current paper, a series of high velocity impact tests using ?50 and ?25 mm ice spheres and 0.32 g granite stones on non-crimp fabric (NCF) composite plates are reported. The impact tests were performed using an air gun and velocities between 100 m/s and 199 m/s. The impact events were monitored using a high-speed camera, with a 20 million frames per second capacity, as well as by a displacement transducer for out-of-plane displacement measurements of the impacted plates. NCF composite plates of two different thicknesses were impacted. The composites were manufactured from carbon fibre and epoxy resin by vacuum infusion.     

Effect of NiCrAlY platelets inclusion on the mechanical and thermal shock properties of glass matrix composites

NiCrAlY platelets modified glass matrix composites were prepared. Their microstructures were characterized, their Young's modulus, fracture strength in bending, Vickers hardness, and indentation toughness were measured, and their thermal shock resistance was studied using quenching-strength and indentation-quench methods. With increasing NiCrAlY content, evident enhancements of the Young's modulus and indentation toughness were obtained. The NiCrAlY alloy inclusion could exert significant influences on the retained bending strength of the samples after quench tests, from 9.6 MPa for NiCrAlY-free glass to 32.0 MPa for 30 wt.% NiCrAlY-containing composites. The indentation-quench tests showed that NiCrAlY alloy inclusion elevated the critical quenching temperatures for propagation of pre-crack, from 150 °C for NiCrAlY-free glass to 225 °C for 30 wt.% NiCrAlY-containing composites. Inclusion debonding and intersection, crack deflection and bridging were observed, and are likely the micromechanisms accounted for the improvement of fracture resistance.     

Low-cycle fatigue behavior of AA2618-T61 forged disk

The cyclic stress–strain response and the low-cycle fatigue life behavior of an aluminum alloy AA2618-T61 forged disk were studied. Fully reversed strain-controlled tests were performed at 200 °C in air at a constant total strain rate and under the total strain ranges of 0.5–0.9%. Specimens cut from longitudinal direction of disk displayed cyclic hardening or softening which was dependent on the total strain range. The variation of low-cycle fatigue life with plastic strain amplitude followed a single-slope Coffin–Manson power-law relationship. Fracture of the samples was predominantly ductile fracture of high density microdimples.     

Allyloxy-modified starch with low degree of substitution for fiber reinforced thermoset starch composites

In the present work dough moulding compound premixes of allyl glycidyl ether modified (AGE)-potato starch, (DS) = 0.2, has been prepared and tested for its fiber reinforced composite properties. The AGE-starch was hydrolyzed with α-amylase under neutral condition for 6 h at 45 °C for improved process ability. The grafting and hydrolytic scission was confirmed by nuclear magnetic resonance (NMR) and size exclusion chromatography (SEC), respectively. Homogeneous composite premixes of AGE-starch, wood fibers, various amount of glycerol and ethylene glycol dimethacrylate were successfully mixed with a Brabender-kneader at 55 °C and cured by compression molding at 150 °C using 2 wt% of dibenzoyl peroxide. Adding 5 wt% of glycerol did not reduce the ultimate strength of the composites; 10% glycerol reduced the strength from 60 MPa to 40 MPa, and 16% glycerol to 14 MPa. The results with 5 wt% glycerol are comparable with earlier achieved results. The water absorption rate increased with increased glycerol content and the mechanical strength of the composites was lost completely when the moisture uptake reached 15 wt%.     

Thermo-viscoelastic responses of multilayered polymer composites: Experimental and numerical studies

This study presents experimental works and finite element (FE) analyses of nonlinear thermo-viscoelastic behaviors of multilayered (pultruded) composites under tension. Creep tests are conducted on E-glass/polyester composites having 0°, 45° and 90° off-axis fiber orientations at various temperatures and stresses. Isochronous creep curves show that the nonlinear stress–strain responses increase with time and temperature for composites tested at higher temperatures (75–125 °F) while there is no particular trend seen at lower temperatures (0–50 °F). A convolution integral model is used for the time–stress–temperature dependent responses. The nonlinear viscoelastic model is implemented in FE framework for analyzing responses of viscoelastic pultruded structures. Sensitivity analysis is conducted to examine error in measuring strains during experiments by simulating the creep tests using FE.     

Effect of thermal annealing treatment on structural, electrical and optical properties of transparent sol-gel ZnO thin films

Effect of thermal annealing in different ambients on the structural, electrical and optical properties of the sol-gel derived ZnO thin films are studied. XRD results show that the annealed ZnO films with wurtzite structure are randomly oriented. Crystallite size, carrier concentration, resistivity and mobility are found to be dependent on the annealing temperature. The change in carrier concentration is discussed with respect to the removal of adsorbed oxygen from the grain boundaries. The highest carrier concentration and lowest resistivity are 8 × 10¹⁸ cm⁻³ and 2.25 × 10⁻¹ Ω cm, respectively, for the film annealed at 500 °C in vacuum. The annealed films are highly transparent with average transmission exceeding 80% in the wavelength region of 400-800 nm. In all three ambients, the optical band gap value does not change much below 500 °C temperature while above this temperature band gap value decreases for nitrogen and air and increases for vacuum.     

The influence of subzero temperatures on fatigue behavior of composite sandwich structures

The fatigue lives and failure modes of foam core carbon/epoxy and glass/epoxy composite sandwich beams in 4-point bending were characterized from room temperature (22 °C) down to −60 °C. Similar previous investigations had focused on elevated temperatures only, but the low temperature fatigue behavior must be understood so that these materials may be evaluated for possible use in the hull structures of ships, which operate in cold regions. Core shear was found to be the dominant fatigue failure mode for the test specimens over the entire temperature range from 22 °C down to −60 °C. Significant increases in the useful fatigue life with brittle type core shear failure were observed at low temperatures by comparison with the corresponding room temperature behavior. Fatigue failure at the low temperatures was catastrophic and without any significant early warning, but the corresponding failures at room temperature were preceded by relatively slow but steadily increasing losses of stiffness. Two different approaches were used to investigate stiffness reductions during fatigue tests, and both approaches led to the same conclusions. Experimental observations regarding the location of fatigue crack initiation were confirmed by static finite element analyses for both materials.     

High temperature annealing of micrometric Zn2SiO4:Mn phosphor powders in fluidized bed

Micrometric Zn_1.8Mn_0.2SiO₄ phosphor powders prepared by spray pyrolysis have been annealed between 900 and 1200 °C under ambient air atmosphere to investigate their luminescence properties. Two original gas-solid fluidization processes have been tested in order to limit sintering phenomena, and the post-treated products have been compared with those annealed using a conventional process in crucible. The crystallinity, the size distribution, the outer morphology and the luminescence properties of powders before and after treatment have been analysed. Massive sintering phenomena occur in crucible from 1000 °C, whereas the original granulometry and spherical morphology are preserved till 1100 °C in fluidized bed. The luminescence efficiencies are comparable for the three processes and shown to be maximal after annealing at 1200 °C. It has been established that residual ZnO and manganese ions at oxidation state higher than 2+, still present after treatment at 1100 °C, are detrimental to good luminescence efficiency. Both disappear from samples post-treated at 1200 °C.     

Comparative study of resistivity characteristics between transparent conducting AZO and GZO thin films for use at high temperatures

This paper compares in detail the resistivity behavior of transparent conducting Al-doped and Ga-doped ZnO (AZO and GZO) thin films for use in an air environment at high temperatures. AZO and GZO thin films with thicknesses in the range from approximately 30 to 100 nm were prepared on glass substrates at a temperature of 200 °C by rf superimposed dc or conventional dc magnetron sputtering deposition, pulsed laser deposition or vacuum arc plasma evaporation techniques. In heat-resistance tests, the resistivity was measured both before and after heat tests for 30 min in air at a temperature up to 400 °C. The resistivity stability of AZO thin films was found to be always lower than that of GZO thin films prepared with the same thickness under the same deposition conditions, regardless of the deposition technique. However, the resistivity of all AZO and GZO thin films prepared with a thickness above approximately 100 nm was stable when heat tested at a temperature up to approximately 250 °C. It was found that the resistivity stability in both GZO and AZO thin films is dominated by different mechanisms determined by whether the thickness is below or above approximately 50 nm. With thicknesses above approximately 100 nm, the increase in resistivity found in GZO and AZO films after heat testing at a temperature up to 400 °C exhibited different characteristics that resulted from a variation in the behavior of Hall mobility.     

Effect of sintering temperature on magneto-transport properties of La0.67Ba0.33MnO3/Ba0.7Sr0.3TiO3 composites

La_0.67Ba_0.33MnO₃-20 wt.%-Ba_0.7Sr_0.3TiO₃ composites were sintered at different temperatures in order to explore the possibility of improving the magneto-transport properties of the composites. Detail studies on the magnetic and electrical transport properties for the sintered composite samples have been performed. Results show that the sintered composites have identical ferromagnetic to paramagnetic transition temperature and filamentary feature of metallic phase. When sintering temperature higher than 1300 °C, the composites show Efros-Shklovskii-like variable-range hopping in the temperature range lower than Curie temperature. For samples sintered lower than 1100 °C, a dome-like resistance peak appears at a temperature well below the Curie temperature. Magnetoresistance behavior indicates the existence of spin polarized tunneling in the low temperature range. Considering the contributions from Efros-Shklovskii-like variable-range hopping and spin polarized tunneling, the resistance peak can be well fitted.