Synthesis and characterization of 0.3 Vf TiC–Ti3SiC2 and 0.3 Vf SiC–Ti3SiC2 composites

In this work, two composite compositions—one with 30% (v/v) SiC, the other with 30% (v/v) TiC, balance Ti₃SiC₂—were synthesized and characterized. Fully dense samples were fabricated by hot isostatically pressing Ti, SiC and C powders for 8 h at 1500 or 1600 °C and a pressure of 200 MPa. Both TiC and SiC lower grain boundary mobility in Ti₃SiC₂. Coarsening of the SiC particles was also observed. At comparable grain sizes, all composites tested were weaker in flexure than the unreinforced Ti₃SiC₂ matrix, with the reduction in strength being the worst for the SiC composites. This reduction in strength is most probably due to thermal expansion mismatches between the matrix and reinforcement phases. The composite samples were exceptionally damage tolerant; in one case a 100 N Vickers indentation (in a 1.5-mm thick bar) did not reduce the flexural strength as compared to an unindented or as-fabricated samples. The same is true for thermal shock resistance; quenching samples from 1400 °C in room temperature water, resulted in strength reductions that were 12% at best and 50% at worst. In the 25–1000 °C temperature range, the thermal expansion coefficients of the two composites were indistinguishable at 8.2×10⁻⁶ K⁻¹. The Vickers hardness values depended on load; at 100 N, the hardnesses were ≈15 GPa; at 300 N, they asymptote to 7–8 GPa. For the most part, very few cracks emanate from the corners of the Vickers indents even at loads as high as 500 N. In the few cases where cracks did initiate, fracture toughness values were crudely estimated to lie in the 5–7.5 MPa √m range.     

Ultrafine hardmetals prepared by WC–10 wt.%Co composite powder

Ultrafine tungsten carbide–cobalt (WC–10 wt.%Co) composite powder was synthesized via spray-drying and direct reduction and carburization process in vacuum, which includes precursor preparation by spray-drying of a suspension of ammonium metatungstate (AMT) and cobalt carbonate (CoCO₃), calcination to evaporate volatile components, formation of tungsten–cobalt mixed oxide powder (CoWO₄/WO₃), ball-milling with carbon black, and subsequent direct reduction and carburization reaction in vacuum. The synthesis temperature of WC–10 wt.%Co composite powder without η or graphite phases is lower than 1000 °C. The calculated particle size by BET test is 0.29 μm. Coarse WC powder (FSSS: 0.9 μm) and Co powder (FSSS: 1.0 μm) (WC:Co = 9:1 in mass) were added into the obtained WC–10 wt.%Co composite powder with addition of 30 wt.%, 50 wt.% and 70 wt.%, respectively. Results show that the hardmetal fabricated from 70 wt.% (WC–10 wt.%Co composite powder) + 30 wt.% (90 wt.%WC + 10 wt.%Co coarse powder) mixed powders exhibits a fine microstructure as well as optimum mechanical properties.     

Elevated temperature compressive failure behavior of a 30 vol.%ZrCp/W composite

The elevated temperature deformation behavior of a 30 vol.%ZrC_p/W composite was tested on a Gleeble-1500D thermo-mechanical simulation device under a uniaxial compressive load. The micro-failure behavior of the composite is strongly affected by the adhesive strength of ZrC/W interface and the distribution of ZrC particles. The computational results by EET theory indicate that the adhesive strength of (Zr, W)C interface is higher than that of ZrC. The microcrack initiation and propagation mechanism varies with the deformation temperature. TEM results show that the initiation and propagation of the microcracks occur in three steps in 1300–1600 °C.     

PIP工艺制备2D C/SiC复合材料Z-向穿刺工艺

针对2D C/SiC复合材料存在碳布层间缺乏纤维增强,层间结合较差的问题,提出通过Z-向穿刺工艺提高碳布层间结合,克服材料使用时可靠性不高的问题,并比较了穿刺工艺对复合材料微观结构和力学性能的影响.结果表明,通过Z-向穿刺工艺制得试样2D C/SiC-Z_(pin)的弯曲强度、弯曲模量和剪切强度分别为247.8 MPa、37.8 GPa和32.1 MPa,而未穿刺试样2D C/SiC的弯曲强度、弯曲模量和剪切强度分别只有219.3 MPa、34.4 GPa和23.3 MPa,由此可见,采用Z-向穿刺工艺能明显提高复合材料的力学性能.微观结构分析认为,试样力学性能提高的根本原因在于采用Z-向穿刺纤维加强了碳布层间结合,使材料具有较好的整体性,克服了复合材料层间结合较弱对力学性能带来的不利影响.     

C/CF/Cu复合材料界面和抗拉强度研究

采用树脂碳化方法制备了碳/碳纤维(C/CF)先驱丝,用压力浸渗凝固成型方法制备了碳/碳纤维/铜(C/CF/Cu)复合材料,借助抗拉强度测试及扫描电镜下复合材料界面和相组成物分布观察,探讨了C、CF和Cu三组元复合界面特性以及碳纤维丝类型和C/CF先驱丝体积分数对C/CF/Cu复合材料抗拉强度的影响.结果表明,C/CF/Cu复合材料的微观界面是碳纤维单丝-树脂碳化碳-铜双复合界面,此界面属于无化学反应的弱复合界面,铜对C/CF先驱丝的机械锁紧力是提高界面强度和复合材料强度的关键因素.当凝固成型压力为28.5MPa时,1k碳纤维丝的C/CF先驱丝体积分数为25%和3k碳纤维丝的C/CF先驱丝体积分数为44.7%的复合材料的抗拉强度达到较高值,分别为595MPa和587MPa,均为纯铜抗拉强度的3倍以上.3k丝制成的一次C/CF先驱丝内碳纤维丝的数量较多,影响复合材料的界面强度,而选用1k碳纤维丝比较有利.     

La0.9Sr0.1Ga0.8Mg0.2O3−δ sintered by spark plasma sintering (SPS) for intermediate temperature SOFC electrolyte

The La_0.9Sr_0.1Ga_0.8Mg_0.2O_3−δ (LSGM) powders for intermediate temperature SOFC electrolyte have been synthesized by glycine-nitrate combustion process. The as-synthesized powders show almost pure perovskite phase. And then, the as-synthesized powders were sintered by SPS at 1300 °C to prepare electrolyte. The SEM, XRD and AC impedance were employed to characterize the microstructure, phase and electrical conductivities. Results show that the grain size is very fine, less than 1 μm, and the relative density of the pellet after sintering by SPS is about 94.7%. There is very little amount of secondary phases after SPS and the grain boundary and secondary phase resistance is very small. The electrolyte sintered by SPS shows higher conductivities than that sintered by conventional method at the same temperature. The activation energy at lower temperatures (400–700 °C) and higher temperatures (700–800 °C) is about 0.94 and 0.49 eV, respectively. Spark plasma sintering is a promising and effective method to sinter the LSGM electrolyte.     

Comparison of morphology and microstructure of ablation centre of C/SiC composites by oxy-acetylene torch at 2900 and 3550 °C

High-temperature application above 1600 °C of C/SiC composites requires evaluation of the ablation properties. The C/SiC composites were prepared by low pressure chemical vapor infiltration using CH₃SiCl₃ as precursor. As-prepared C/SiC composites were ablated by oxy-acetylene flame with the temperature of 2900 and 3550 °C. Above 3550 °C, subliming of carbon fiber and silicon carbide matrix was the main ablation behaviour. At 2900 °C, thermal decomposition and oxidation of SiC matrix were the main ablation behaviour. A carbon coating resulted from the pyrolysis of the acetylene prevented the C/SiC from oxidizing dramatically.     

Effect of C/SiC Volume Ratios on Mechanical and Oxidation Behaviors of Cf/C-SiC Composites Fabricated by Chemical Vapor Infiltration Technique

C/SiC volume ratios in carbon fiber-reinforced carbon-silicon carbide (C_f/C-SiC) composites may influence greatly mechanical and oxidation properties of the composites, but have not been well investigated yet. Herein, C_f/C-SiC composites with different C/SiC volume ratios were fabricated by chemical vapor infiltration (CVI) technique through alternating the thickness of a pyrocarbon (PyC) interlayer. The composites with C/SiC volume ratios of 0.37 and 0.84 exhibited the better comprehensive mechanical properties. The CS0.37 showed the highest flexural strength of 340.6 MPa, and CS0.84 had the maximum tensile strength of 139.1 MPa. The excellent mechanical properties were closely related to the relatively low C/SiC volume ratios and porosities, optimum interfacial bonding and reduced matrix micro-cracks. The composite with a low C/SiC volume ratio of 0.10 showed the best anti-oxidation performance due to its high SiC content. The oxidation mechanisms at 1100 °C and 1400 °C were discussed by considering the effect of the C/SiC volume ratios, pores and matrix micro-cracks, oxidation of carbon phase and SiC.     

Blast and tensile properties of tantalum/niobium lined SiC/SiC composite tubes for nuclear cladding

The mechanical performances such as tensile strength and blast property of metal lined SiC/SiC composite cladding tubes were investigated. Nb or Ta was selected as liner material, and the SiC/SiC composite layer was fabricated by winding and different precursor impregnation and pyrolysis (PIP) processes. The tensile strengths of different tube samples were measured at room temperature (RT) and 1200 °C, respectively. The blast property was investigated through the maximum water pressure of tubes. And the fracture microstructures were observed by SEM. The highest tensile strength at RT was 150.7 MPa. The blast strength was enhanced with the PIP process increasing from 1 to 4 cycles and the tube of 4 PIP cycles had the highest water pressure of 34.7 MPa. Compared with the metal tubes, the multi-layer structure improved tensile and blast properties significantly. The different processes such as PIP cycles and pyrolytic carbon (PyC) coating were important factors to enhance the mechanical performances of SiC/SiC-based tubes. However, the retention rate of tensile strength was only 18.5% at 1200 °C.     

表面硅化对C/C复合材料组织结构的影响

采用表面固相渗硅工艺在C/C复合材料表面制备SiC涂层 ,研究了制备工艺对涂层和C/C复合材料组织结构的影响。结果表明 :硅化反应时间对C/C复合材料的SiC涂层厚度影响不大 ;C/C复合材料组织中热解碳基体与碳纤维相比 ,更易与Si反应生成SiC ,说明碳纤维的稳定性高于热解碳 ,Si通过界面和材料缺陷扩散深入基体内部。     

Microstructure and mechanical properties of 3D fine-woven punctured C/C composites with PyC/SiC/TaC interphases

The 3D fine-woven punctured C/C-(P_yC/SiC/TaC) composites, composed of P_yC/SiC/TaC interphases and pyrocarbon (PyC) matrix, were synthesized by isothermal chemical vapor infiltration (ICVI) methods. The alternating layers and the structure of these composites were examined by polarized light microscopy (PLM), X-ray diffractometry (XRD) and scanning electron microscopy (SEM). It is found that the P_yC matrix has rough laminar (RL) structure, the TaC layer has NaCl-type cubic structure, and the SiC layer has few wurtzite type 10H-SiC besides β-SiC structure. The effects of fiber coating and the bulk density on the tensile and flexural properties of composites along X or Y and Z direction were investigated. It is shown that fiber coated 3D woven punctured C/C composites have good tensile and flexural strength, and the maximum of flexural strength is 375 MPa in X or Y direction at density of 1.89 g/cm³, which is about three times higher than that of samples without TaC/SiC fiber coating. The flexural strength and bending strength increase with increasing the density of the composites. The analysis of fracture surfaces reveals that fibers and fiber bundles are pulled out in composites, indicating that the composite exhibits a non-linear failure behavior through propagation and deflection of the cracks.     

Effect of annealing on the morphology evolution and densification of LiMn2O4 film from chitosan-containing solution

Dense LiMn₂O₄ films deposited on a Pt-coated silicon substrate were obtained by annealing the deposited Li–Mn–O-chitosan films under a two-stage heat-treatment procedure. It was demonstrated that the heat-treatment at 300 °C plays an important role in the subsequent densification of LiMn₂O₄ films. This is attributed to the formation and rearrangement of the nano-sized LiMn₂O₄ crystallites. The surface morphology of the calcined Li–Mn–O-chitosan films was highly related to the annealing temperature. Ridge-like bumps formed on the surface of the films after being heated at 200 °C for 1 h. With calcination at 400 °C or higher, the surface morphology turned into a wrinkle-like microstructure. This morphology transformation is ascribed to the flowing characteristics of the Li–Mn–O-chitosan films during heat-treatment and subsequent thermal decomposition of the precursor at higher temperatures. Moreover, the electrochemical tests showed that the 700 °C-annealed LiMn₂O₄ film possesses the highest discharge capacity of 56.3 μA h/(cm² μm) and best capacity retention of 90.7% after 50 charge/discharge cycles of all annealed films.     

In situ observation on fatigue crack growth in SCS-6/Ti-15-3 composite at elevated temperatures

Direct observation on fatigue crack growth behavior in SiC (SCS-6) fiber-reinforced Ti-15-3 alloy matrix composite subjected to a constant tension–tension loading mode was performed by scanning electron microscope using a single edge-notched specimen in vacuum at room temperature and 550 °C. The fatigue crack growth rate at 550 °C was lower than that at room temperature, and the difference between the fatigue crack growth rates at room temperature and 550 °C increased with increasing fatigue cycles. The crack opening displacement at 550 °C was smaller than that at room temperature when the crack length exceeded a definite value, though the interface friction stress between the fiber and matrix at elevated temperature was much smaller than that at room temperature. The above results were explained qualitatively by a residual stress mechanism at the crack front and the crack closure behavior at crack wake, which could be produced by matrix creep asymmetry in tension and compression at elevated temperature during each fatigue cycle.     

Comparison of thermal and ablation behaviors of C/SiC composites and C/ZrB2-SiC composites

A comparison was presented of the thermal and ablation behaviors of two carbon fiber reinforced ceramic-matrix composites (one with a SiC matrix and the other with a ZrB₂-SiC matrix). The C/SiC composite possessed a lower thermal conductivity (TC) and a higher emissivity in comparison to the C/ZrB₂-SiC composite. The two composites exhibited the good ablation-resistive properties with no obvious erosion rate after the arc-heated wind tunnel ablation tests. The surface of the C/SiC composite appeared to be coarse and had many rounded protrusions while a denser and more homogeneous glass oxide scale was formed for the C/ZrB₂-SiC composite. The maximum surface and back side temperatures of the C/ZrB₂-SiC composite were about 50 °C lower than those of the C/SiC composite, respectively, which was mainly attributed to the evaporation of the B₂O₃ as well as its higher TC.     

Continuous extrusion and tensile strength of self-reinforced HDPE/UHMWPE sheet

A specially designed fish-tail shaped extrusion die was used to continuously extrude self-reinforcing sheet of HDPE/UHMWPE. The result indicated that under conventional extrusion conditions, the tensile strength of extruded sheet was comparable to conventional molded HDPE samples and was almost the same in both MD (machine direction) and TD (transverse direction) directions. While at temperatures slightly above the melting point of HDPE, compared with conventionally extruded sheet, above 6-fold and 3-fold improvements were obtained in the MD and TD direction for HDPE/UHMWPE (I) system in the optimum extrusion windows of 15–30 MPa extrusion pressure, the die temperature ranging from 126 °C to 137 °C and a rotation speed of 15 rpm. For HDPE/UHMWPE (III) system, in the optimum processing windows, that is, 15–30 MPa extrusion pressure, 131–139 °C die temperature and 15 rpm extruder rotation speed, about 5-fold and 2–3-fold improvements were obtained in the MD and TD direction compared with conventionally extruded sheet, respectively.     

Grain growth and precipitation in an annealed cold-rolled Ni50.2Ti49.8 alloy

In this paper we present a transmission electron microscopic study on the effect of annealing on the microstructure of a cold-rolled Ni_50.2Ti_49.8 ribbon. Transmission electron microscopy of the as-received sample shows the presence of alternating amorphous and crystalline bands. The crystalline bands have widths of the order of a few microns and contain amorphous nanopockets and B2 nanograins, the latter at around 20 nm diameter and preferentially oriented with their normal along the 111 direction and perpendicular to the strip surface. As-received samples were annealed for 30 min at different temperatures up to 800 °C. Crystallization starts in the amorphous bands at around 350 °C and finally ends up with the coarsening of the grains in the entire sample. Annealing of the samples at 450 °C entirely transforms the amorphous bands into crystalline bands. At 800 °C the grain size increases to 30–50 μm with a formation of a tweed kind of morphology inside the grains when observed at room temperature. Diffraction patterns from such grains reveal the presence of diffuse intensity around 1/3110^* indicating the formation of the R-phase. NiTi₂ precipitates form at 450 °C while annealing at 600 °C and higher yields Ni₃Ti₂ precipitates. For samples annealed at 500 °C for a longer time, Ni₄Ti₃ precipitates have been observed along with the austenite to martensite transformation in the grains.     

Fracture and creep of an Al2O3-SiC (whisker)-TiC (particle) composite

High-temperature fracture strength and compressive creep of an electrodischarge-machinable composite, Al₂O₃-30.9 vol.% SiC whiskers-23 vol.% TiC particles have been studied to 1200 °C and 1450 °C, respectively, in inert atmosphere. Microstructures of fractured and deformed specimens were examined using scanning and transmission electron microscopy. Fast fracture occurred at T ≤ 1200 °C. Steady-state creep was achieved for T > 1350 °C at stresses < 80 MPa, with the rate-controlling mechanism being partially unaccommodated grain-boundary sliding, with a stress exponent of ≈ 1 and an activation energy of≈ 470 kJ/mol.     

Influence of deformation temperature on the ferrite grain refinement in a low carbon Nb–Ti microalloyed steel

Grain refinement is one of the effective methods to develop new generation low carbon microalloyed steels possessing excellent combination of mechanical properties. In the present work, the microstructural evolution and ferrite grain refinement at various deformation temperatures were investigated using single pass isothermal hot compression experiments for a low carbon Nb–Ti microalloyed steel. The physical processes that occurred during deformation were discussed by observing the optical microstructure and analyzing the stress–strain responses. The results show that there is a close relation between the microstructural evolution and true stress–true strain responses during the deformation. Microstructural observation indicates that very fine ferrite grains of about 1.8–3 μm are obtained by deformation at 830–845 °C, about Ar₃ ± 10 °C. The obtained stress–strain curves suggest the occurrence of strain-induced dynamic transformation (SIDT) of γ to at this deformation temperature range.     

C／C坯体对RMI C／C—SiC复合材料组织的影响

以PAN基炭纤维（Cf）针刺整体毡为预制体，用化学气相渗透（CVI）、浸渍炭化（IC）方法制备了不同炭纤维增强炭基体的多孔C／C坯体，采用反应熔渗（RMI）法制备C／C—SiC复合材料，研究了渗Si前后坯体的密度和组织结构。结果表明：不同C／C坯体反应溶渗硅后复合材料的物相组成为SiC相、C相及单质Si相；密度低的坯体熔融渗硅后密度增加较多；密度的增加与开口孔隙度并不是单调增加的关系，IC处理的坯体开口孔隙度低，但渗硅后复合材料的密度增加较多；IC坯体中分布分散的树脂C易与熔渗Si反应，CVI坯体中的热解C仅表层与熔渗Si反应，在Cf和SiC之间有热解C存在；坯体密度相同时，IC处理的坯体中SiC量较多，单质Si相含量少且分散较好，而CVI坯体中SiC量较少，单质Si相的量较多；制备方法相同时，高密度的C／C坯体，渗硅后C相较多。     

预制体对C／C复合材料热膨胀系数的影响

以天然气为前驱气体,整体碳毡和2D针刺碳毡为预制体,采用热悌度化学气相渗积技术制备了两种C／C复合材料,其表观密度均为1．74g／cm^3。借助光学显微镜和扫描电子显微镜观察了热解碳基体的生长特征和微观形貌,采用热膨胀仪测量了两种材料的热膨胀系数（CTE）,研究了由不同预制体增强C／C复合材料的CTE,解释了造成材料不同方向CTE差异的主要原因。结果表明,随着温度升高,材料A和B的CTE是逐渐升高的,且Z向CTE值均大于XY向。当两种材料在Z向的纤维体积分数接近时,随着XY方向纤维体积分数增大,材料在Z向的CTE增大,在XY向的CTE降低,两种材料存XY和Z向的CTE旱如下分布：αB—z〉dAz〉αA—xy〉αBxY-C／C复合材料的CTE主要取决于纤维体积分数和排市、碳基体及材料中的孔隙分布情况,前者起决定作用。