Tension-Compression Fatigue of a Nextel™720/alumina Composite at 1200 °C in Air and in Steam

Tension-compression fatigue behavior of an oxide-oxide ceramic-matrix composite was investigated at 1200 °C in air and in steam. The composite is comprised of an alumina matrix reinforced with Nextel?720 alumina-mullite fibers woven in an eight harness satin weave (8HSW). The composite has no interface between the fiber and matrix, and relies on the porous matrix for flaw tolerance. Tension-compression fatigue behavior was studied for cyclical stresses ranging from 60 to 120 MPa at a frequency of 1.0 Hz. The R ratio (minimum stress to maximum stress) was ?1.0. Fatigue run-out was defined as 10⁵ cycles and was achieved at 80 MPa in air and at 70 MPa in steam. Steam reduced cyclic lives by an order of magnitude. Specimens that achieved fatigue run-out were subjected to tensile tests to failure to characterize the retained tensile properties. Specimens subjected to prior cyclic loading in air retained 100 % of their tensile strength. The steam environment severely degraded tensile properties. Tension-compression cyclic loading was considerably more damaging than tension-tension cyclic loading. Composite microstructure, as well as damage and failure mechanisms were investigated.     

Stress-dependence and time-dependence of the post-fatigue tensile behavior of carbon fiber reinforced SiC matrix composites

The major objective of this paper is to phenomenally report the stress-dependence and time-dependence of fatigue damage to C/SiC composites, and to tentatively discuss the effects of the fatigue stress levels and the fatigue cycles on the post-fatigue tensile behavior. Results show that compared with the virgin strength of the as-received C/SiC specimens, the tensile strengths of the as-fatigued specimens after 86,400 cycles were increased by 8.47% at the stresses of 90 ± 30 MPa, 23.47% at 120 ± 40 MPa, and 9.8% at 160 ± 53 MPa. As cycles continued, however, the post-fatigue strength of the composites gradually decreased after the peak of 23.47%, at which the optimal strength enhancement was obtained because the mean fatigue stress of 120 MPa was the closest to thermal residual stress (TRS), and caused TRS relieve largely during the fatigue. Most interestingly, there was a general inflexion appeared on the post-fatigue tensile stress-strain curves, which was just equal to the historic maximum fatigue stress acted upon the as-fatigued specimens. Below this inflexion stress the tensile curves revealed the apparent linear behavior with little AE response, and above that nonlinearity with new damage immediately emitted highly increase rate of AE activities. This ‘stress memory’ characteristic was strongly relevant to damaged microstructures of the as-fatigued composites in the form of the coating/matrix cracks, interface debonding/wear, and fiber breaking, which resulted undoubtedly in reduction of modulus but in proper increase of strength via TRS relief.     

Effects of Steam Environment on Fatigue Behavior of Two SiC/[SiC+Si<Subscript>3</Subscript>N<Subscript>4</Subscript>] Ceramic Composites at 1300°C

The fatigue behaviors of two SiC/[SiC+Si₃N₄] ceramic matrix composites (CMC) were investigated at 1,300°C in laboratory air and in steam. Composites consisted of a crystalline [SiC+Si₃N₄] matrix reinforced with either Sylramic™ or Sylramic-iBN fibers (treated Sylramic™ fibers that possess an in situ BN coating) woven in a five-harness satin weave fabric and coated with a proprietary boron-containing dual-layer interphase. The tensile stress–strain behaviors were investigated and the tensile properties measured at 1,300°C. Tension–tension fatigue behaviors of both CMCs were studied for fatigue stresses ranging from 100 to 180 MPa. The fatigue limit (based on a run-out condition of 2 × 10⁵ cycles) in both air and steam was 100 MPa for the CMC containing Sylramic™ fibers and 140 MPa for the CMC reinforced with Sylramic-iBN fibers. At higher fatigue stresses, the presence of steam caused noticeable degradation in fatigue performance of both composites. The retained strength and modulus of all run-out specimens were characterized. The materials tested in air retained 100% of their tensile strength, while the materials tested in steam retained only about 90% of their tensile strength.     

Tension–compression fatigue of a SiC/SiC ceramic matrix composite at 1200 °C in air and in steam

Tension–compression fatigue behavior of a non-oxide ceramic composite with a multilayered matrix was investigated at 1200 °C in laboratory air and in steam. The composite was produced via chemical vapor infiltration (CVI). The composite had an oxidation inhibited matrix, which consisted of alternating layers of silicon carbide and boron carbide and was reinforced with laminated woven Hi-Nicalon™ fibers. Fiber preforms had pyrolytic carbon fiber coating with boron carbide overlay applied. Tension–compression fatigue behavior was studied for fatigue stresses ranging from 80 to 200 MPa at a frequency of 1.0 Hz. Presence of steam significantly degraded the fatigue performance. Specimens that achieved fatigue run-out were subjected to tensile tests to failure to characterize the retained tensile properties. The material retained 100% of its tensile strength. Composite microstructure, as well as damage and failure mechanisms were investigated.     

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.     

Enchanced high-temperature performances of SiC/SiC composites by high densification and crystalline structure

We report the enchanced in situ performances of tensile strength and thermal conductivity at elevated temperatures of the PCS-free SiC/SiC composite with a high fiber volume fraction above 50% fabricated by NITE process for nuclear applications. The composite was fabricated by the optimized combination of the fiber coating, the matrix slurry and the pressure-sintering conditions, based on our previous composites’ study history. The composite showed the excellent tensile strength up to 1500 °C, that it retained approximately 88% of the room-temperature strength. Also, the thermal conductivity of the composites represented over 20 W/m K up to 1500 °C, which was enough high to take the advantage of the assumed design value for nuclear applications. Microstructural observation indicated that the excellent high-temperature performances regarding tensile strength and thermal conductivity up to 1500 °C were the contribution to the high densification and crystalline structure in matrix.     

Notch Sensitivity of Fatigue Behavior of a Hi-Nicalon™/SiC-B4C Composite at 1,200 °C in Air and in Steam

The effect of holes on the fatigue life of a non-oxide ceramic composite processed via chemical vapor infiltration (CVI) was examined at 1,200 °C in laboratory air and in steam. The effect of holes on tensile strength at 1,200 °C was also evaluated. The composite comprised laminated woven Hi-Nicalon? fibers in an oxidation inhibited matrix, which consisted of alternating layers of silicon carbide and boron carbide. Fiber preforms had pyrolytic carbon fiber coating with boron carbon overlay applied. Unnotched specimens and specimens with a center hole having a radius to width ratio of 0.24 were tested in tension-tension fatigue at 0.1 Hz and at 1.0 Hz. The fatigue stresses ranged from 100 to 140 MPa in air and in steam. Fatigue run-out was defined as 10⁵ cycles at 0.1 Hz and as 2?×?10⁵ cycles at 1.0 Hz. The net-section strength was less than the unnotched ultimate tensile strength. Comparison of notched and unnotched data also revealed that the fatigue performance was notch insensitive in both air and steam environments. Composite microstructure, as well as damage and failure mechanisms were investigated.     

Effect of carbon nanofibers (CNFs) content on thermal and mechanical properties of CNFs/SiC nanocomposites

Carbon nanofibers dispersed β-SiC (CNFs/SiC) nanocomposites were prepared by hot-pressing via a transient eutectic phase route at 1900 °C for 1 h under 20 MPa in Ar. The effects of additional CNFs content between 1 and 10 wt.% were investigated, based on densification, microstructure, thermal and mechanical properties. The CNFs/SiC nanocomposites by the CNFs contents below 5 wt.% exhibited excellent relative densities over 98% with well dispersed CNFs. However, the CNFs/SiC nanocomposites containing the CNFs of 10 wt.% possessed a relative density of 92%, accompanying CNFs agglomerates and many pores located inside the agglomerates. The three point bending strength gradually decreased with the increase of CNFs content, but the indentation fracture toughness increased to 5.7 MPa m^1/2 by the CNFs content of 5 wt.%. The thermal conductivity was enchanced with the increase of CNFs content and represented a maximum value of 80 W/mK at the CNFs content of 5 wt.%.     

Effect of loading type on fatigue properties of high strength bearing steel in very high cycle regime

Very high cycle fatigue tests under axial loading at frequencies of 95 Hz and 20 kHz were performed to clarify the effect of loading type on fatigue properties of a high strength bearing steel in combination with experimental result of this steel under rotating bending. As a result, this steel represents the single P-S-N (probabilistic-stress-life) curve characteristics for surface-induced fracture and interior inclusion-induced fracture, just like that under rotating bending. However, fatigue strength is lower, where the run-out stress at 10⁹ cycles is evaluated to be 588 MPa, less than that under rotating bending with about 858 MPa. Occurrence probability of larger and deeper inclusion-induced fracture is much higher than that under rotating bending. Furthermore, the formation process of fine granular area (FGA) is independent of the type and frequency of loading, which is very slow and is explained as the crack nucleation process under the special dislocation mechanism. The stress intensity factor range at the front of FGA, ΔK_FGA, is approximately regarded as the threshold value controlling the stable propagation of interior crack. For the control volume of specimen under axial loading, the estimated value of fatigue limit by FGA is similar to experimental run-out stress value at 10⁹ cycles, but that by inclusion is larger. However, the corresponding estimated results under rotating bending are all conservative.     

Fabrication of SiCf/SiC composites by chemical vapor infiltration and vapor silicon infiltration

Three-dimensional (3D) silicon carbide fiber reinforced silicon carbide matrix (SiC_f/SiC) composites, employing KD-1 SiC fibers (from National University of Defense Technology, China) as reinforcements, were fabricated by a combining chemical vapor infiltration (CVI) and vapor silicon infiltration (VSI) process. The microstructure and properties of the as prepared SiC_f/SiC composites were studied. The results show that the density and open porosity of the as prepared SiC_f/SiC composites are 2.1 g/cm³ and 7.7%, respectively. The SiC fibers are not severely damaged during the VSI process. And the SiC fibers adhere to the matrix with a weak interface, therefore the SiC_f/SiC composites exhibit non-catastrophic failure behavior with the flexural strength of 270 MPa, fracture toughness of 11.4 MPa·m^1/2 and shear strength of 25.7 MPa at ambient conditions. Moreover, the flexural strength decreases sharply at the temperature higher than 1200 °C. In addition, the thermal conductivity is 10.6 W/mk at room temperature.     

High mechanical performance SiC/SiC composites by NITE process with tailoring of appropriate fabrication temperature to fiber volume fraction

Unidirectional SiC/SiC composites are prepared by nano-powder infiltration and transient eutectic-phase (NITE) process, using pyrolytic carbon (PyC)-coated Tyranno-SA SiC fibers as reinforcement and SiC nano-powder with sintering additives for matrix formation. The effects of two kinds of fiber volume fraction incorporating fabrication temperature were characterized on densification, microstructure and mechanical properties. Densification of the composites with low fiber volume fraction (appropriately 30 vol%) was developed even at lower fabrication temperature of 1800 °C, and then saturated at 3rd stage of matrix densification corresponding to classic liquid phase sintering. Hence, densification of the composites with high volume fraction (above 50 vol%) became restricted because the many fibers retarded the infiltration of SiC nano-powder at lower fabrication temperature of 1800 °C. When fabrication temperature increased by 1900 °C, densification of the composites was effectively enhanced in the intra-fiber-bundles and simultaneously the interaction between PyC interface and matrix was strengthened. SEM observation on the fracture surface revealed that fiber pull-out length was accordingly changed with fabrication temperature as well as fiber volume fraction, which dominated tensile fracture behaviors. Through NITE process, SiC/SiC composites with two fracture types were successfully developed by tailoring of appropriate fabrication temperature to fiber volume fraction as follows: (1) high ductility type and (2) high strength type.     

Fabrication and mechanical properties of monolithic MoSi2 by spark plasma sintering

Fine MoSi₂ powders containing a small amount of Mo₅Si₃ have been prepared by self-propagating high-temperature synthesis (SHS), followed by spark plasma sintering (SPS) for 10 min at 1200-1500°C and 30 MPa. Dense MoSi₂ materials, in which the grain size is ∼7.5 μm, have been fabricated at 1300°C. They exhibit excellent mechanical properties: Vicker’s hardness H_v (10.6 GPa), fracture toughness K_IC (4.5 MPa m^1/2), and bending strength σ_b (560 MPa). The strength of 325 MPa can be retained up to 1000°C.     

Cryogenic fatigue behavior of plain weave glass/epoxy composite laminates under tension-tension cycling

This paper focuses on understanding the tension-tension fatigue behavior of woven glass fiber reinforced polymer laminates at cryogenic temperatures. Tension-tension fatigue tests at frequencies of 4 and 10 Hz with a stress ratio of 0.1 were conducted at room temperature, 77 and 4 K. The fatigue stress versus cycles to failure (S-N) relationships and fatigue limits for 10⁶ cycles were obtained. Fractured specimens tested under fatigue tests were also examined with optical microscope.     

High temperature fatigue deformation behaviors of thermally sprayed steel measured with electronic speckle pattern interferometry method

High temperature fatigue (R=0) damage and deformation behaviors of SUS304 steel thermally sprayed with Al₂O₃/NiCr coating were investigated using an electronic speckle pattern interferometry (ESPI) method. Surface cracks and delamination occurred after 1×10⁵ cycles test when σ_max was 202 MPa at 873 K. The lengths and number of cracks and delamination largely decreased when σ_max or temperature decreased to 115 MPa or 573 K, respectively. Strain values along cracks measured with the ESPI method were much larger than other areas due to crack opening under the tensile load. The positions of strain concentration zones on strain distribution figures by ESPI method were well corresponded to those of cracks on sprayed coatings. Strain values decreased largely where local delamination occurred.     

Mechanical properties of 3D KD-I SiCf/SiC composites with engineered fibre-matrix interfaces

Three-dimensional (3D) silicon carbide (SiC) matrix composites reinforced with KD-I SiC fibres were fabricated by precursor impregnation and pyrolysis (PIP) process. The fibre-matrix interfaces were tailored by pre-coating the as-received KD-I SiC fibres with PyC layers of different thicknesses or a layer of SiC. Interfacial characteristics and their effects on the composite mechanical properties were evaluated. The results indicate that the composite reinforced with as-received fibre possessed an interfacial shear strength of 72.1 MPa while the composite reinforced with SiC layer coated fibres had a much higher interfacial shear strength of 135.2 MPa. However, both composites showed inferior flexural strength and fracture toughness. With optimised PyC coating thickness, the interface coating led to much improved mechanical properties, i.e. a flexural strength of 420.6 MPa was achieved when the interlayer thickness is 0.1 μm, and a fracture toughness of 23.1 MPa m^1/2 was obtained for the interlayer thickness of 0.53 μm. In addition, the composites prepared by the PIP process exhibited superior mechanical properties over the composites prepared by the chemical vapour infiltration and vapour silicon infiltration (CVI-VSI) process.     

Preparation and properties of negative thermal expansion Zr2WP2O12 ceramics

Using solid-state reaction method, Zr₂WP₂O₁₂ powder was synthesized for this study. The optimum heating condition was 1200 °C for 4 h. The obtained powder was compacted and sintered. The relative density of the Zr₂WP₂O₁₂ ceramics with no sintering additive was 60%. That of samples sintered with more than 0.5 mass% MgO was about 97%. The average grain size (D₅₀), as estimated from the polished surface of a sample sintered at 1200 °C for 4 h was about 1 μm. The obtained ceramics showed a negative thermal expansion coefficient of about −3.4 × 10⁻⁶ °C⁻¹. Young's modulus, Poisson's ratio, three-point bending strength, Vickers microhardness, and fracture toughness of the obtained ceramics were, respectively, 74 GPa, 0.25, 113 ± 13 MPa, 4.4 GPa and 2.3 MPa m^1/2.     

Effect of surface oxidation on thermal shock resistance of the ZrB2-SiC-ZrC ceramic

The isothermal oxidation of the ZrB₂-SiC-ZrC ceramic was carried out in static air at a constant temperature of 1000 ± 15 °C, 1200 ± 15 °C and 1400 ± 15 °C for 30 min, respectively. Compared with the original strength of 580 MPa, the strength for the specimen oxidized at 1000 °C, 1200 °C and 1400 °C for 30 min increased to 609 MPa, 656 MPa and 660 MPa, respectively, because the flaws in the surface of the specimen were sealed by the oxide layer. The thermal shock resistance of the specimens before and after the oxidation was measured by the water quenching. The measured ΔT_crit for the specimen oxidized at 1000 °C, 1200 °C and 1400 °C were 352 °C, 453 °C and 623 °C, respectively, which was obviously higher than 270 °C for the unoxidized specimen. The improvement in the thermal shock resistance was attributed to the formation the oxide layer on the surface of the specimen. The results here pointed to a promising method for improving strength and thermal shock resistance of ZrB₂-based ceramics.     

Interfacial control of uni-directional SiCf/SiC composites based on electrophoretic deposition and their mechanical properties

Interfacial control of uni-directional SiC_f/SiC composites were performed by EPD, and their mechanical properties at room temperature were evaluated. The effect of the thickness of carbon interphase on SiC fibers by EPD on mechanical properties of uni-directional SiC_f/SiC composites was also investigated. The average thickness of carbon coating on SiC fibers increased from 42 nm to 164 nm with an increase in the concentration of colloidal graphite suspension for EPD. Dense SiC_f/SiC composites were achieved and their fiber volume fraction was 47–51%. The SiC_f/SiC composites had a bending strength of 210–240 MPa. As the thickness of carbon coating was below 100 nm, the SiC_f/SiC composites (SC01 and SC02) fractured in almost brittle manner. In contrast, the SiC_f/SiC composites (SC03) showed a pseudo-ductile fracture behavior with a large number of fiber pullout as the thickness of carbon coating was above 100 nm. The fracture energy of SC03 was 3–4 times as high as those of SC01 and SC02 and the value was about 1.7 kJ/m². In consideration of the results of mechanical properties, the thickness of carbon coating on SiC fibers should be at least 100 nm to obtain high-performance SiC_f/SiC composites. The fabrication process based on EPD method is expected to be an effective way to control the interfaces of SiC_f/SiC composites and to obtain high-performance SiC_f/SiC composites.     

Relaxor ferroelectric like giant permittivity in PrCrO3 semiconductor ceramics

The electrical behavior of PrCrO₃ ceramics prepared by citric acid route and sintered at 1200 °C has been characterized by a combination of permittivity measurements, and impedance spectroscopy (IS). The effective permittivity obtained in frequency range 100 Hz to 1 MHz and temperature range 80–300 K, exhibits giant permittivity value of 3 × 10⁴ near room temperature. The response is similar to that observed for relaxor ferroelectrics. IS data analysis revealed the ceramics to be electrically heterogeneous semiconductor with room temperature resistivity <10² Ω m consisting of semiconducting grains with permittivity ?′ ∼ 100 and more resistive grain boundaries with effective permittivity ?′ ∼ 10⁴. We conclude, therefore that grain boundary effect is the primary source for the high effective permittivity in PrCrO₃ ceramics.     

Investigation of growth stresses in NiO scale formed on Ni at 1000 °C by a modified deflection method

The average growth stress of NiO scale formed on pure Ni at 1000 °C in air was investigated by a modified deflection technique. The growth stress in NiO scale was tensile with a magnitude of about 10 MPa during the 10-h oxidation period. The growth stress level decreased with increasing oxidation time or oxide thickness. It varied from 37 MPa for a scale thickness of 4.8 μm to 13 MPa for a thickness of 13.8 μm. At the later stage of oxidation, the growth stress did not change noticeably. The planar stress state in the substrate was both compressive and tensile during the first hour of the deflection test. After that, only compressive stress existed in the substrate alloy.