Synergistic Effects of Frequency and Temperature on Damage Evolution and Life Prediction of Cross-Ply Ceramic Matrix Composites under Tension-Tension Fatigue Loading

In this paper, the synergistic effects of loading frequency and testing temperature on the fatigue damage evolution and life prediction of cross-ply SiC/MAS ceramic-matrix composite have been investigated. The damage parameters of the fatigue hysteresis modulus, fatigue hysteresis dissipated energy and the interface shear stress were used to monitor the damage evolution inside of SiC/MAS composite. The evolution of fatigue hysteresis dissipated energy, the interface shear stress and broken fibers fraction versus cycle number, and the fatigue life S–N curves of SiC/MAS composite under the loading frequency of 1 and 10 Hz at 566 °C and 1093 °C in air condition have been predicted. The synergistic effects of the loading frequency and testing temperature on the degradation rate of fatigue hysteresis dissipated energy and the interface shear stress have been analyzed.     

Synergistic Effects of Temperature,Oxidation and Multicracking Modes on Damage Evolution and Life Prediction of 2D Woven Ceramic-Matrix Composites under Tension-Tension Fatigue Loading

In this paper, the synergistic effects of temperature, oxidation and multicracking modes on damage evolution and life prediction in 2D woven ceramic-matrix composites (CMCs) have been investigated. The damage parameter of fatigue hysteresis dissipated energy and the interface shear stress were used to monitor the damage evolution inside of CMCs. Under cyclic fatigue loading, the fibers broken fraction was determined by combining the interface/fiber oxidation model, interface wear model and fibers statistical failure model at elevated temperature, based on the assumption that the fiber strength is subjected to two-parameter Weibull distribution and the load carried by broken and intact fibers satisfy the Global Load Sharing (GLS) criterion. When the broken fibers fraction approaches to the critical value, the composite fatigue fractures. The evolution of fatigue hysteresis dissipated energy, the interface shear stress and broken fibers fraction versus cycle number, and the fatigue life S–N curves of SiC/SiC at 1000, 1200 and 1300 °C in air and steam condition have been predicted. The synergistic effects of temperature, oxidation, fatigue peak stress, and multicracking modes on the evolution of interface shear stress and fatigue hysteresis dissipated energy versus cycle numbers curves have been analyzed.     

Damage Monitoring of Unidirectional C/SiC Ceramic-Matrix Composite under Cyclic Fatigue Loading using A Hysteresis Loss Energy-Based Damage Parameter at Room and Elevated Temperatures

The damage evolution of unidirectional C/SiC ceramic-matrix composite (CMC) under cyclic fatigue loading has been investigated using a hysteresis loss energy-based damage parameter at room and elevated temperatures. The experimental fatigue hysteresis modulus and fatigue hysteresis loss energy versus cycle number have been analyzed. By comparing the experimental fatigue hysteresis loss energy with theoretical computational values, the interface shear stress corresponding to different cycle number and peak stress has been estimated. The experimental evolution of fatigue hysteresis loss energy and fatigue hysteresis loss energy-based damage parameter versus cycle number has been predicted for unidirectional C/SiC composite at room and elevated temperatures. The predicted results of interface shear stress degradation, stress–strain hysteresis loops corresponding to different number of applied cycles, fatigue hysteresis loss energy and fatigue hysteresis loss energy-based damage parameter as a functions of cycle number agreed with experimental data. It was found that the fatigue hysteresis energy-based parameter can be used to monitor the fatigue damage evolution and predict the fatigue life of fiber-reinforced CMCs.     

Relationship Between Hysteresis Dissipated Energy and Temperature Rising in Fiber-Reinforced Ceramic-Matrix Composites Under Cyclic Loading

In this paper, the relationship between hysteresis dissipated energy and temperature rising of the external surface in fiber-reinforced ceramic-matrix composites (CMCs) during the application of cyclic loading has been analyzed. The temperature rise, which is caused by frictional slip of fibers within the composite, is related to the hysteresis dissipated energy. Based on the fatigue hysteresis theories considering fibers failure, the hysteresis dissipated energy and a hysteresis dissipated energy-based damage parameter changing with the increase of cycle number have been investigated. The relationship between the hysteresis dissipated energy, a hysteresis dissipated energy-based damage parameter and a temperature rise-based damage parameter have been established. The experimental temperature rise-based damage parameter of unidirectional, cross-ply and 2D woven CMCs corresponding to different fatigue peak stresses and cycle numbers have been predicted. It was found that the temperature rise-based parameter can be used to monitor the fatigue damage evolution and predict the fatigue life of fiber-reinforced CMCs.     

基于迟滞耗散能的纤维增强陶瓷基复合材料疲劳寿命预测方法

纤维增强陶瓷基复合材料(CMCs)在疲劳载荷作用下,纤维相对基体在界面脱粘区往复滑移导致其出现疲劳迟滞现象,迟滞回线包围的面积,即迟滞耗散能,可用于监测纤维增强CMCs疲劳损伤演化过程。提出了一种基于迟滞耗散能的纤维增强CMCs疲劳寿命预测方法及考虑纤维失效的迟滞回线模型,建立了迟滞耗散能、基于迟滞耗散能的损伤参数、应力-应变迟滞回线与疲劳损伤机制(多基体开裂、纤维/基体界面脱粘、界面磨损与纤维失效)之间的关系。分析了疲劳峰值应力、疲劳应力比与纤维体积分数对纤维增强CMCs疲劳寿命S-N曲线、迟滞耗散能和基于迟滞耗散能的损伤参数随循环次数变化的影响。疲劳寿命随疲劳峰值应力增加而减小,随纤维体积含量增加而增加;迟滞耗散能随疲劳峰值应力增加而增加,随应力比和纤维体积分数增加而减小;基于迟滞耗散能的损伤参数随纤维体积分数增加而减小。      

Fatigue Hysteresis of Carbon Fiber-Reinforced Ceramic-Matrix Composites at Room and Elevated Temperatures

When the fiber-reinforced ceramic-matrix composites (CMCs) are first loading to fatigue peak stress, matrix multicracking and fiber/matrix interface debonding occur. Under fatigue loading, the stress–strain hysteresis loops appear as fiber slipping relative to matrix in the interface debonded region upon unloading/reloading. Due to interface wear at room temperature or interface oxidation at elevated temperature, the interface shear stress degredes with increase of the number of applied cycles, leading to the evolution of the shape, location and area of stress–strain hysteresis loops. The evolution characteristics of fatigue hysteresis loss energy in different types of fiber-reinforced CMCs, i.e., unidirectional, cross-ply, 2D and 2.5D woven, have been investigated. The relationships between the fatigue hysteresis loss energy, stress–strain hysteresis loops, interface frictional slip, interface shear stress and interface radial thermal residual stress, matrix stochastic cracking and fatigue peak stress of fiber-reinforced CMCs have been established.     

Microstructure of brazed joints between mechanically metallized Si<Subscript>3</Subscript>N<Subscript>4</Subscript> and stainless steel

Brazing has been increasingly used to join metals to advanced ceramics. Brazing covalent materials requires either the use of active filler alloys or the previous metallization of the surface. To that end, a new and simple mechanical technique has been applied to metallize advanced ceramics, thus avoiding the use of costly Ti-based active filler alloys. The mechanical metallization of Si₃N₄ with Ti was employed as an alternative route to deposit active metallic films prior to brazing with stainless steel using 72% Ag--28% Cu or 82% Au—18% Ni eutectic alloys. The brazing temperatures were set to 40°C or 75°C above the eutectic temperature of each filler alloy. Ti-films of average thickness 4 μm produced adequate spreading of both filler alloys onto Si₃N₄ substrates, which were subsequently brazed to stainless steel. The interface of Si₃N₄/310 stainless steel basically consisted of a reaction layer, a precipitation zone and an eutectic microconstituent. Mechanically sound and vacuum-tight joints were obtained, especially upon brazing at relatively lower temperatures. Increasing the brazing temperature resulted in thermal cracking of the Si₃N₄, possibly due to increased thermal stress.     

Si<Subscript>3</Subscript>N<Subscript>4</Subscript>/TiN composites produced from TiO<Subscript>2</Subscript>-Modified Si<Subscript>3</Subscript>N<Subscript>4</Subscript> powders

Si₃N₄/TiN composites have been produced by hot pressing at temperatures from 1600 to 1800°C in a nitrogen atmosphere, using silicon nitride powders prepared by self-propagating high-temperature synthesis and surface-modified with titanium dioxide nanoparticles. We examined the effect of TiO₂ content on the microstructure, phase composition, and mechanical strength of the ceramics. It is shown that titanium nitride can be formed by the reaction Si₃N₄ + TiO₂ → TiN + NO + N₂O + 3Si. The Si₃N₄/TiN composites containing 5–20% TiN have a low density, high porosity, and a bending strength of 60 MPa or lower. In Si₃N₄/TiN ceramics produced using calcium aluminates as sintering aids, the silicon nitride grains are densely packed, which ensures an increase in strength to 650 MPa.     

Design of Si<Subscript>3</Subscript>N<Subscript>4</Subscript>-based ceramic laminates by the residual stresses

Ceramic laminates with strong interfaces between layers are considered a very promising material for different engineering applications because of the potential for increasing fracture toughness by designing high residual compressive and low residual tensile stresses in separate layers. In this work, Si₃N₄/Si₃N₄-TiN ceramic laminates with strong interfaces were manufactured by rolling and hot pressing techniques. The investigation of their mechanical properties has shown that the increase in apparent fracture toughness can be achieved for the Si₃N₄/Si₃N₄-20 wt.%TiN composite, while further increase of TiN content in the layers with residual tensile stresses lead to a formation of multiple cracks, and as a result, a significant decrease in the mechanical performance of the composites. Micro-Raman spectroscopy was used to measure the frequency shift across the Si₃N₄/Si₃N₄-20 wt.%TiN laminate. These preliminary Raman results can be useful for further analysis of residual stress distribution in the laminate.     

Strain-induced artificial multiferroicity in Pb(Zr<Subscript>0.53</Subscript>Ti<Subscript>0.47</Subscript>)O<Subscript>3</Subscript>/Pb(Fe<Subscript>0.66</Subscript>W<Subscript>0.33</Subscript>)O<Subscript>3</Subscript> layered nanostructure at ambient temperature

Layered nanostructures (LNs) of the commercial ferroelectric Pb(Zr_0.53Ti_0.47)O₃ (PZT) and the natural ferroic relaxor Pb(Fe_0.66W_0.33)O₃ (PFW) were fabricated with a periodicity of PZT/PFW/PZT (~5/1/5 nm, thickness ~250 nm) on MgO substrates by pulsed laser deposition. The dielectric behavior of these LNs were investigated over a wide range of temperatures and frequencies, observing Debye-type relaxation with marked deviation at elevated temperatures (>400 K). High dielectric constant and very low dielectric loss were observed below 100 kHz and 400 K, whereas the dielectric constant decreases and loss increases with increase in frequency, similar to relaxor ferroelectrics. Asymmetric ferroelectric hysteresis loops across UP and DOWN electric field were observed with high remanent polarization (P_r) of about 33 μC/cm². High imprint (~5–7 V across 250 nm thin films) were seen in ferroelectric hysteresis that may be due to charge accumulation at the interface of layers or significant amount of strain (~3.21) across the layers. Room temperature ferromagnetic hysteresis was observed with remanent magnetization 5.32 emu/cc and a coercive field of ~550 Oe. Temperature and field dependent leakage current densities showed very low leakage ~10⁻⁷–10⁻⁵ A/cm² over 500 kV/cm. We observed imprint in hysteresis that may be due to charge accumulation at the interface of layers or active role of polar nano regions (PNRs) situated in the PFW regions.     

Fabrication,dielectric and ferroelectric properties of Ba<Subscript>0.6</Subscript>Sr<Subscript>0.4</Subscript>TiO<Subscript>3</Subscript> film with preferred orientation

Ba_0.6Sr_0.4TiO₃ films were fabricated by RF magnetron sputtering method. The X-ray diffraction (XRD) showed that the preferred orientation of films growing on platinum Si substrates can be tailored by sputtering pressure. The processing parameters such as sputtering pressure and substrate temperature were optimized to obtain a developed perovskite film with (110) preferred orientation. The polarization hysteresis loops and permittivity–voltage curves of the (110)-oriented film have been investigated,which demonstrated that the film is in ferroelectric phase at room temperature. Besides, it had excellent fatigue properties without polarization reduction after about 10¹⁰ switch cycles, and showed low leakage current (10⁻⁹–10⁻⁷ A/cm²) within an applied voltage of 5 V. Finally, the leakage current mechanism was studied.     

Microstructure characterization of in situ synthesized porous Si<Subscript>3</Subscript>N<Subscript>4</Subscript>–Si<Subscript>2</Subscript>N<Subscript>2</Subscript>O composites using feldspar additive

Porous Si₃N₄–Si₂N₂O bodies fabricated by multi-pass extrusion process were investigated depending on the feldspar addition content (4–8 wt% Si) in the raw silicon powder. The diameter of the continuous pores was about 250 μm. The polycrystalline Si₂N₂O fibers observed in the continuous pores as well as in the matrix regions of the nitrided bodies can increase the filtration efficiency. In the 4 wt% feldspar addition, the diameter of the Si₂N₂O fibers in the continuous pores of the nitrided bodies was about 90–150 nm. A few number of rope typed Si₂N₂O fibers (∼4 μm) was found in the case of 8 wt% feldspar addition. However, in the 8 wt% feldspar addition, the matrix showed highly porous structure composed of large number of the Si₂N₂O fibers (∼60 nm). The relative densities of the Si₃N₄–Si₂N₂O bodies with 4 wt% and 8 wt% feldspar additions were about 65% and 61%, respectively.     

Interface roughness influence on exchange bias effect in La<Subscript>2/3</Subscript>Ca<Subscript>1/3</Subscript>MnO<Subscript>3</Subscript>/La<Subscript>1/3</Subscript>Ca<Subscript>2/3</Subscript>MnO<Subscript>3</Subscript> bilayers

A Monte Carlo simulation study of La_2/3Ca_1/3MnO₃/La_1/3Ca_2/3MnO₃ bilayers exchange bias (EB) properties by using a classical Heisenberg model and Monte Carlo method with Metropolis algorithm is addressed. Samples were built atom-by-atom in order to resemble the real roughness. In this model, several contributions included nearest neighbors exchange interactions; two different interface couplings, magnetocrystalline anisotropy and Zeeman term, were considered. Here, an influence of the relaxation steps on the interface roughness is present. Our study focuses on the influence of interface roughness on hysteresis loops, particularly EB field (H _ex) and coercive force (H _c). Results reveal that H _ex and H _c decrease as the interface roughness increases.     

The Multiferroic Properties of (Bi<Subscript>0.9</Subscript>Ba<Subscript>0.1</Subscript>)(Fe<Subscript>0.95</Subscript>Mn<Subscript>0.05</Subscript>)O<Subscript>3</Subscript> Films

(Bi_0.9Ba_0.1)(Fe_0.95Mn_0.05)O₃ films were prepared on LaNiO₃-coated surface oxidized Si substrates. XRD and Raman measurements confirm that the (Bi_0.9Ba_0.1)(Fe_0.95Mn_0.05)O₃ film has pure R3c structure. Clear ferromagnetism with saturated magnetization of about 25 emu/cm³ has been observed at room temperature. The ferroelectric properties of the (Bi_0.9Ba_0.1)(Fe_0.95Mn_0.05)O₃ film was confirmed by the observation of the ferroelectric domains and the converse piezoelectric coefficient d ₃₃ versus applied voltage hysteresis loops by piezoelectric force microscopy (PFM). The observation of ferromagnetism and ferroelectricity in (Bi_0.9Ba_0.1)(Fe_0.95Mn_0.05)O₃ films indicates the potential multiferroic applications.     

Microstructure and properties of SiC-whisker-reinforced Si<Subscript>3</Subscript>N<Subscript>4</Subscript> ceramics with calcium aluminate additions

Silicon-nitride-based ceramics containing Al₂O₃-CaO sintering aids and reinforced with silicon carbide whiskers have been prepared by hot pressing at 1650°C in a nitrogen atmosphere, and their microstructure, phase composition, and mechanical properties have been studied. The results indicate that the Si₃N₄ ceramic containing 15 wt % calcium aluminate additions and 10 wt % SiC fibers has a dense microstructure with a uniform distribution of skeletal and dendritic silicon carbide crystals. The observed variations in the morphology of the crystals are tentatively attributed to the secondary crystallization of silicon carbide from the eutectic calcium aluminate melt during cooling.     

Two-Band Calculations on the Upper Critical Field of Sc<Subscript>2</Subscript>Fe<Subscript>3</Subscript>Si<Subscript>5</Subscript>

The ternary compound Sc₂Fe₃Si₅ has attracted much attention because of the various anomalous physical properties. The specific heat experiment and energy band structure calculation suggest that Sc₂Fe₃Si₅ is a two-gap superconductor. Based on this, we analyze the upper critical field for superconducting Sc₂Fe₃Si₅ crystals using the two-band Ginzburg-Landau theory. A two-parameter variational approach is adopted to obtain the upper critical field in arbitrary direction. The temperature and angular dependences of the upper critical field are plotted. The results reproduce the experimental data in a very broad temperature range and strongly support previous specific heat data and theoretical calculation, pointing to the existence of two energy gaps in Sc₂Fe₃Si₅. The anisotropy of the upper critical field is also studied and is about 2, in accordance with the experimental result. Moreover our calculations indicate that Sc₂Fe₃Si₅ has rather a three-dimension character, in agreement with the energy band calculation.     

M<Subscript>23</Subscript>C<Subscript>6</Subscript> precipitation behavior in a Ni-base superalloy M963

The M₂₃C₆ precipitation behavior in a cast Ni-base superalloy M963 was investigated after tensile creep testing at 800°C and strain-controlled low cycle fatigue testing at 700–950°C. During high temperature creep and low cycle fatigue, the primary MC decomposed into M₆C continuously, and a great amount of secondary carbide, chromium-rich M₂₃C₆, precipitated preferentially in the periphery of MC and γ +γ′ eutectic at grain boundaries. M₂₃C₆ was rarely present in grain interior, indicating that grain boundary promoted M₂₃C₆ carbide precipitation. The M₂₃C₆ precipitation was closely dependent on the stress state and testing temperature, seemed to be independent of the total strain amplitude. M₂₃C₆ is unstable during low cycle fatigue testing. The occurrence of M₂₃C₆ precipitation was sharply reduced during low cycle fatigue testing at 950°C. Crack was easily initiated at interface between MC and matrix, while fine M₂₃C₆ was effective to prevent grain boundary migration.     

Mechanical properties and microstructure of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/mullite composite

An Al₂O₃/5 vol.% mullite composite was synthesized by using reaction sintering of Al₂O₃/0.78 wt.% SiC at 1,600 °C for 2 h in air. The phase analysis of the Al₂O₃/mullite composite was carried out using X-ray diffraction (XRD). There were two kinds of mullite in alumina/mullite composite, namely, 3Al₂O₃·2SiO₂ and Al_5.65Si_0.35O_9.175. The microstructure of the Al₂O₃/mullite composite was investigated using scanning electron microscope (SEM) and transmission electron microscope (TEM). The mechanical properties such as Young’s modulus, Poisson’s ratio, hardness, toughness and strength of the Al₂O₃/mullite composite were investigated. The influence of mullite on the composite is discussed.     

Effect of Tb substitution on the magnetic properties of exchange-biased Nd<Subscript>2</Subscript>Fe<Subscript>14</Subscript>B/Fe<Subscript>3</Subscript>B

Tb-substituted (Nd,Tb)₂Fe₁₄B/Fe₃B nanocomposite ribbons have been synthesized by melt spinning of Nd₃Tb₁Fe₇₆Cu_0.5Nb₁B_18.5 alloys. Tb substitution has significantly enhanced the value of coercivity and Curie temperature. Highest value of coercivity has been obtained as 4.76 kOe for the sample annealed at 953 K for 10 min. Curie temperature of Tb substituted sample, Nd₃Tb₁Fe₇₆Cu_0.5Nb₁B_18.5 is 549 K while Curie temperature of the sample without Tb, Nd₄Fe₇₆Cu_0.5Nb₁B_18.5 is 535 K. Recoil hysteresis loops measured along the major demagnetization curve are steep having small recoil loop area. Temperature dependence of coercivity, remanent ratio and maximum energy product have been measured for the sample annealed at 893 K and 923 K for 10 min. At 5 K, coercivity and maximum energy product of the sample annealed at 893 K for 10 min are 5.2 kOe and 11.5 MGOe respectively and the sample annealed at 923 K for 10 min are 6 kOe and 13.1 MGOe respectively.     

Catalytic effect of Ti<Subscript>5</Subscript>Si<Subscript>3</Subscript> on thermal decomposition of Li<Subscript>3</Subscript>AlH<Subscript>6</Subscript>

Fine Ti₅Si₃ powder has been mechanochemically synthesized from a mixture of elemental Ti and Si powders. When Ti₅Si₃ is added as a catalyst into Li₃AlH₆, it shows a good catalytic ability by reducing the decomposition temperature and improving the decomposition kinetics as well. Although its catalytic effect is not as good as well-known TiCl₃, the use of Ti₅Si₃ has a benefit of releasing more hydrogen than TiCl₃ during dehydrogenation. This can be explained by that Ti₅Si₃, unlike TiCl₃, does not incur any chemical reactions with Li₃AlH₆ and thus remains inert during milling for dispersion.