Fatigue behaviour and residual strength evolution of 2D C/SiC Z-pinned joints prepared by chemical vapour infiltration

Z-pinned joints prepared by chemical vapour infiltration are widely used in ceramic matrix composite components. Excellent fatigue behaviour is important for structural safety. In this study, 2D C/SiC Z-pinned joints were loaded in axial direction of the pins under static and cyclic loading. Internal damage was monitored in situ by an acoustic emission system. The binding force between pin and hole is relatively strong. Meanwhile, the joints exhibite promising resistance to fatigue. The residual strength increased first with the fatigue cycles then decreased after 10⁵ cycles. Microstructural analysis indicated that full-developed cracks and local stress redistribution resultes in the increase in the strength of the joints. The acoustic emission analysis also provides a supplementary understanding of the damage mechanism. The results show that damage fully develops at the early stage of fatigue. When the specimen is reloaded, less AE events are collected before the fatigue maximum stress.     

Ring compression properties of SiCf/SiC composites prepared by chemical vapor infiltration

SiC fiber reinforced SiC matrix (SiC_f/SiC) composites prepared by chemical vapor infiltration are one of promising materials for nuclear fuel cladding tube due to pronounced low radioactivity and excellent corrosion resistance. As a structure component, mechanical properties of the composites tubes are extremely important. In this study, three kinds of SiC_f preform with 2D fiber wound structure, 2D plain weave structure and 2.5D shallow bend-joint structure were deposited with PyC interlayer of about 150–200?nm, and then densified with SiC matrix by chemical vapor infiltration at 1050?°C or 1100?°C. The influence of preform structure and deposition temperature of SiC matrix on microstructure and ring compression properties of SiC_f/SiC composites tubes were evaluated, and the results showed that these factors have a significant influence on ring compression strength. The compressive strength of SiC_f/SiC composites with 2D plain weave structure and 2.5D shallow bend-joint structure are 377.75?MPa and 482.96?MPa respectively, which are significantly higher than that of the composites with 2D fiber wound structure (92.84?MPa). SiC_f/SiC composites deposited at 1100?°C looks like a more porous structure with SiC whiskers appeared when compared with the composites deposited at 1050?°C. Correspondingly, the ring compression strength of the composites deposited at 1100?°C (566.44?MPa) is higher than that of the composites deposited at 1050?°C (482.96?MPa), with a better fracture behavior. Finally, the fracture mechanism of SiC_f/SiC composites with O-ring shape was discussed in detail.     

Oxidation behaviors and shear properties of z-pinned joint made of two-dimensional carbon fiber reinforced silicon carbide composite

Chemical vapor infiltration has been introduced for preparing z-pinned joint, which is made of two-dimensional carbon fiber reinforced silicon carbide composite. The effects of oxidation on the shear properties of the joint were investigated. The results showed that the joint strength increases with the increase of oxidation temperature, which is consistent with the oxidation consumption of the carbon phases. An exponential relationship is presented between the weight loss and the joint strength. In contrast, linear relationships are presented between the weight loss and the mechanical properties of the composite. The exponential relationship results from the coupled shear and bending stress states of the pin, according to the failure mechanisms of the joint. It is observed that in-plane and intra-layer cracks are formed under the shear stress. And these cracks are bridged by the fibers under the bending stress. Accordingly, the fiber bridging mechanism contributes to the joint strength before and after oxidation. For the conditions of this study, the joint strength can be roughly estimated as the plus of the in-plane shear strength and the tensile matrix cracking stress.     

Friction performance of C/C composites prepared using rapid directional diffused chemical vapor infiltration processes

A technology used to prepare C/C composites using a rapid directional diffused (RDD) chemical vapor infiltration process has been investigated. General RDD technologies were explored, and optimal parameters were determined. The friction and wear properties of this material were researched. The results showed that in the RDD process, propylene and nitrogen were rapidly and directionally diffused into the carbon preforms enabling carbon deposition to occur from the inside of the preform to the outside. This method prevents the formation of an outer crust on the surface of preforms and facilitates uniformity of densification. With the RDD process no surface machining was required between chemical vapor infiltration (CVI) cycles thereby enabling continuous densification and reducing the CVI cycle times. The optimum processing conditions for RDD CVI were as follows; furnace temperature 950 °C; and furnace pressure 6.7 kPa. The C/C composites produced using RDD CVI processing exhibited good friction performance. Their curves of the brake moment with the velocity are stable under dry conditions, and their wet brake moment is greatly reduced. The average thickness wear is decreased to 9.5×10⁻⁴ mm/surface/stop.     

Interlaminar shear behaviors of 2D needled C/SiC composites under compressive and tensile loading

The interlaminar shear strength of 2D needled C/SiC composites was measured using the double-notch shear test method. Interlaminar shear tests were performed under compressive and tensile loading. Shear stress–strain response and shear strain field evolution were studied using the digital image correlation (DIC) technique. The results show that the interlaminar shear strength of the specimen using the compressive loading method is 15% higher than that of the tensile loading method. Severe shear strain concentration was observed near the upper notch of the tensile loading specimen. Acoustic emission (AE) was utilized to monitor the damage during the tests. Typical damage mechanisms were categorized according to AE signal characteristics. The statistical results show that more matrix cracks were produced in the tensile loading specimen and no separate fiber/matrix debonding signal was detected in both specimens.     

Manufacturing 2D carbon-fiber-reinforced SiC matrix composites by slurry infiltration and PIP process

Sub-micrometer SiC particles were firstly added to the preceramic solution in the first infiltration step to enhance the mechanical properties of 2D C_f/SiC composites fabricated via polymer infiltration and pyrolysis (PIP) process. The effects of pyrolysis temperature and SiC-filler content on microstructures and properties of the composites were systematically studied. The results show that the failure stress and fracture toughness increased with the increase of pyrolysis temperature. SiC filler of sub-micron scale infiltrated into the composites increased the mechanical properties. As a result, for the finally fabricated composite infiltrated with a slurry containing 40 wt.% SiC filler, the failure stress was doubled compared to that without SiC filler addition, and the fracture toughness reached ≈10 MPa m^1/2.     

Ablation behavior of C/C-ZrC and C/SiC-ZrC composites fabricated by a joint process of slurry impregnation and chemical vapor infiltration

C/C-ZrC and C/SiC-ZrC composites were fabricated by a joint process of slurry impregnation and chemical vapor infiltration, in which ZrC matrix was obtained by slurry impregnation process, while C or SiC matrix was introduced by chemical vapor infiltration process. The as fabricated C/C-ZrC and C/SiC-ZrC composites have densities of 1.67 g cm^?3 and 1.91 g cm^?3 respectively. Tensile strength is 89.4±8.4 MPa and 182.2±14.0 MPa respectively for the as prepared C/C-ZrC and C/SiC-ZrC. Ablation behavior of the C/C-ZrC and C/SiC-ZrC composites under air plasma was studied and compared in detail. Due to different oxidation resistance and heat transfer capacity of the matrix, these two ZrC based composites showed various ablation behavior. The linear erosion rate is 48 µm s^?1 and 39 µm s^?1 respectively for C/C-ZrC and C/SiC-ZrC composites.     

A double layer nanostructure SiC coating for anti-oxidation protection of carbon/carbon composites prepared by chemical vapor reaction and chemical vapor deposition

A double layer nanostructure SiC coating was prepared by chemical vapor reaction and chemical vapor deposition to protect carbon/carbon composites from oxidation. The obtained dense coating reveals a typical crystalline structure and combines well with the substrate. The outer layer of the coating consists of SiC nanocrystals and nanowires, whereas the inner layer is mainly composed of SiC microcrystals, nanocrystals and nanowires. The oxidation and cyclic thermal shock test performed at 1400 °C in air demonstrates that the prepared dense nanostructure coating has excellent anti-oxidation behavior and thermal shock resistance at high temperature. After 400 h oxidation and 34 cycles of thermal shock from 1400 °C to room temperature, the weight loss of the coated sample is only 1.67%. In the oxidation process, the amorphous silica formed at the beginning of the oxidation crystallizes to cristobalite as oxidation time increased. The formation of cristobalite resulted in micro-cracks formed along grain boundaries in the cyclic thermal shock test. As only cracks are formed on the coating surface, it can be concluded that the formation of the penetration cracks may be the reason for the weight loss of the SiC coated composite.     

脉冲FCVI制备炭/炭复合材料的氧化行为

采用脉冲强制流动热梯度化学气相渗透工艺(IFCVI)制备了炭/炭复合材料(C/C复合材料),利用等温氧化实验对C/C复合材料在不同温度(673～1173 K)条件下的氧化行为进行了研究,并借助于扫描电子显微镜观察了C/C复合材料的氧化形貌.实验结果表明:C/C复合材料的基体在氧化反应中优先氧化,氧化反应速率随温度的升高而增大;在高于或低于临界温度973 K时,C/C复合材料的氧化反应分别受2种不同机制控制,其反应活化能分别为1.29×105 J/mol和2.94× 104 J/mol.     

Preparation of C/C composites by the chemical vapor infiltration (CVI) of propane pyrolysis

The preparation of C/C composites by the chemical vapor infiltration (CVI) of the pyrolysis carbon from propane was studied. Pyrolysis carbon was deposited at 30 torr and at temperatures between 1,173 and 1,233 K. The rate of carbon deposition increased slightly with time. The main gas products in the exit gas were methane, ethylene, and acetylene. The fraction of ethylene decreased and that of acetylene increased with the reaction temperature and the propane concentration. The produced propyl radicals reacted further at a high temperature and at a high propane concentration. These trends were similar to those of the reported data. Changes of the shapes of deposited carbon in the pores of preform were confirmed with SEM photos. The mathematical modeling of the system with the deposition rate constant from the reference estimated experimental data well.     

Joining of Ti-coated monolithic SiC using a SiCw/Ti3SiC2 filler by electric field-assisted sintering

Monolithic SiC, for the first time, was successfully joined using a SiC whisker-reinforced Ti₃SiC₂ composite (SiC_w/Ti₃SiC₂) filler via electric field-assisted sintering technique. A thin Ti coating layer was formed on the SiC surface to minimize the residual stress at the joint interface by transforming it into a TiC gradient layer. After optimizing process parameters, a joint strength higher than 250 MPa was obtained, which is higher than the other values reported in the literature. Failure occurred at the SiC base rather than the joining interface because of the improved joint strength by the incorporation of SiC_w. The addition up to 15 wt. % SiC_w in the filler layer improved the joint strength by various strengthening mechanisms. On the other hand, the joint strength was lower with 20 wt. % SiC_w addition, indicating the importance of thermal expansion mismatch between SiC_w and Ti₃SiC₂ to obtain a sound SiC joint.     

Strengthening/toughening of 2D C/SiC composites by coating

SiC and SiC_w/SiC coatings were prepared on two-dimensional carbon fiber reinforced silicon carbide ceramic matrix composites (2D C/SiC), and strengthening/toughening of the composite by the coatings was investigated. After coating, the density of the C/SiC composites was increased effectively and the mechanical properties were improved significantly. Compared with SiC coating, SiC_w/SiC coating showed the more significant effect on strength/toughness of the composites. Coatings had two effects: surface strengthening and matrix strengthening. The latter was the dominant effect. The surface strengthening can increase the crack initiation stress, while the matrix strengthening can enhance the crack propagation resistance. The former effect increased the strength and the latter effect increased the toughness.     

Ti3SiC2 friction material prepared by novel method of infiltration sintering

Titanium silicon carbide (Ti₃SiC₂) is a remarkable friction material for its combination of the best properties of metals and ceramics. The high purity Ti₃SiC₂ ceramic has been prepared by infiltration sintering (IS), and the effect of a small amount of Si on Ti₃SiC₂ ceramic formation was investigated. The results show that the purity of Ti₃SiC₂ ceramic could be increased significantly and the sintering time for Ti₃SiC₂ could be decreased remarkably when proper amount of Si was added in the starting mixture. The Ti₃SiC₂ sintered compact with a purity of 99.2?wt-% and a relative density of 97% was obtained by the IS from a starting mixture composed of n(Ti):n(Si):n(TiC)?=?1:0.3:2 at 1500°C with holding time of 2/3?h.     

Oxidation behavior of silicon carbide based biomorphic ceramics prepared by chemical vapor infiltration and reaction technique

The oxidation behavior of biomorphic SiC based ceramics with different microstructure and composition was studied at 1450 °C in airflow for 50 h by thermal gravimetric analysis (TGA). SiC with amorphous, coarse grain, crystalline and fine grain crystalline microstructures as well as SiC–Si₃N₄ composite ceramics were processed from paper preforms by chemical vapor infiltration and reaction technique. The ceramics were characterized by X-ray diffraction and scanning electron microscopy coupled with energy dispersive spectroscopy (SEM/EDX) before and after oxidation. The results show that the crystalline SiC with fine grain structure and SiC–Si₃N₄ composite ceramics show very good oxidation resistance at a temperature of 1450 °C.     

Microstructure and thermal stability of low-oxygen SiC fibers prepared by an economical chemical vapor curing method

Continuous SiC fibers (SiC-CVC fibers) with low oxygen content (~2 wt%) were prepared by pyrolysis of polycarbosilane (PCS) fibers cured with chemical vapor curing (CVC). PCS fibers were cured by cyclohexene vapor as curing agent. Their structure and properties were compared with those of SiC fibers obtained from electron beam irradiation curing (SiC-EB fibers). SiC-CVC fibers were similar to SiC-EB fibers, with distinctly better thermomechanical stability than that of fibers cured by thermal oxidation curing (commercial KD-I fibers). CVC is a more economical and practicable approach for preparing high-performance SiC fibers than other strategies.     

Failure analysis of C/SiC composites plate with a hole by the PFA and DIC method

The progressive failure analysis (PFA) and digital image correlation (DIC) method were used to study the strain distribution and failure evolution of C/SiC composites with a circular hole under tension. The nonlinear constitutive relation based continuous degradation strategy (NCRCDS) was combined with the PFA and compared with the sudden material property degradation strategy (SMPDS). The maximum strain criterion was adopted in the PFA to model local failure. The initiation and evolution of local failure around the hole were studied by PFA and DIC method. The results indicate that the local failure distribution simulated by PFA was close to that of the DIC measurement. The strain field was relevant to the surface topography and the microstructure of the material, and the strain distribution around the hole was affected by the arrangement and the damage of the fiber bundle. The simulated results of the strain distribution were in good agreement with the DIC measurements.     

Densification behavior and microstructure of carbon/carbon composites prepared by chemical vapor infiltration from xylene at temperatures between 900 and 1250 °C

Carbon/carbon composites were prepared by film boiling chemical vapor infiltration from xylene pyrolysis. Their densification behaviors such as the mass gain, the deposition rate and the density profile were investigated. The microstructure was studied by polarized light microscopy and characterized quantitatively with average extinction angle (Ae). Results showed that, under the particular experimental equipment and process, the initial deposition rate and the average Ae of pyrocarbon (PyC) increased with the increasing deposition temperature (T_d). The structural transition of PyC from rough laminar (RL) to smooth laminar along both the axial and radial directions of the composites was retarded as T_d increased from 900 to 1100 °C; PyC was deposited by the heterogeneous nucleation and growth. The homogeneous nucleation was generated producing isotropic PyC at the bottom of the composites for 1200–1250 °C deposition. The matrix produced at 1100–1250 °C was dominated by RL PyC, and the composites with high average density and uniform RL matrix were rapidly produced for T_d around 1100 °C.     

Degradation of boron nitride interfacial coatings fabricated by chemical vapor infiltration on SiC fibers under ambient air/room temperature conditions

Hexagonal boron nitride (h-BN) interfacial coatings were deposited on SiC fibers by chemical vapor infiltration (CVI) and their degradation behavior under ambient air/room temperature conditions was studied with time. Degradation of the interfacial coatings with time was investigated by characterizing the morphology and microstructure of these materials with scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and transmission electron microscopy (TEM). Thermogravimetry coupled with differential thermal analysis (TG-DTA) and X-ray photoelectron spectroscopy (XPS) was used to analyze the chemical reactions and phase transitions taking place in the BN coatings. The results showed that the as-deposited BN interfacial coatings fabricated by CVI were compact and well bonded to the SiC fibers. BN coatings remained relatively stable under ambient air/room temperature conditions for 50?h, while severe degradation was observed after 500?h of exposure. The degradation of BN interfacial coatings was mainly caused by two factors, namely, reaction with atmospheric air to produce boric oxide and amorphization of the hexagonal structure. The degradation observed under ambient air/room temperature might be due to incomplete crystallinity of BN interfacial coatings. Presence of water vapor may accelerate degradation of the coatings. The results of this degradation test can be used as a reference for the storage of BN coatings fabricated by CVI.