Preparation,mechanical and thermal properties of Si3N4 ceramics by gelcasting using low–toxic DMAA gelling system and gas pressure sintering

In this work, Si₃N₄ ceramics were fabricated through an aqueous gelcasting method using a low–toxic monomer called N, N–dimethylacrylamide (DMAA) followed by gas pressure sintering at 1850 °C for 2 h under 6 MPa N₂ atmosphere. The effect of solid loading on performance of slurries, green and sintered bodies was investigated systematically. The results show that the slurries with a solid loading as high as 50 vol% (viscosity 0.17 Pa.s at 100 s^–1) were achieved. With the increase of solid loading (30–50 vol%), the green bodies exhibited a monotonically decreased, however high enough in general, flexural strength of 16.50–11.52 MPa, which was comparable to that of widely–used neurovirulent acrylamide (AM) gelling system. In regard to the sintered bodies, increasing solid loading significantly promoted sintering and improved mechanical properties and thermal conductivity as a result of the increased density, bimodal distribution structure, as well as suitable interfacial bonding strength. The best performance parameters of Si₃N₄ ceramics, bulk density of 3.25 g/cm³, apparent porosity of 0.67%, flexural strength of 898.92 MPa, fracture toughness of 6.42 MPa m^1/2, Vickers hardness of 2.81 GPa, and thermal conductivity of 34.69 W m^–1 K^–1, were obtained at 50 vol% solid loading. This work renders low–toxic DMAA gelling system promising prospect in preparation of high–performance Si₃N₄ ceramics by gelcasting.     

C/C composite surface modified by electrophoretic depositing SiC nanowires and its brazing to Nb

A novel surface treatment method by electrophoretic depositing SiC nanowires on the C/C composite was introduced to reinforce the C/C–Nb brazed joints. Results showed that the electrophoretic deposition (EPD) process of SiC nanowires could improve the wettability of the liquid AgCuTi alloy on the C/C substrate because of the reaction between SiC nanowires and active element Ti in the AgCuTi alloy. With the introduction of SiC nanowires, the formation of continuous brittle Ti₃Cu₄ layer was inhibited and the Ti₃Cu₄ changed into lumps. The thickness of the TiC reaction layer was 500 nm when the EPD time was 5s which was larger than that of the original brazed joint. As the EPD time continued to increase, the thickness of the TiC reaction layer decreased gradually and the size of brittle Ti₃Cu₄ phase in the joint became smaller and smaller. With the combined effects of the change in the Ti₃Cu₄ morphology and the TiC reaction layer thickness, the average shear strength of joints achieved a peak of 48 MPa when the EPD time was 30s, which was 60% higher than that of the original brazed joints.     

Ultra-high-temperature ablation behavior of SiC–ZrC–TiC modified carbon/carbon composites fabricated via reactive melt infiltration

To improve the ablation resistance under the ultra-high temperature, the matrix of the carbon/carbon (C/C) composite was modified with a ternary ceramic of SiC–ZrC–TiC via reactive melt infiltration. The obtained ceramic matrix was composed of Zr-rich and Ti-rich solid solution phases of Zr_1−xTi_xC and SiC. This composite exhibited an excellent ablation property at 2500 °C with low mass and linear ablation rates of 0.008 mg s⁻¹ cm⁻² and 0.000 μm s⁻¹, respectively. The ablation mechanism was revealed with various microstructure characterizations and compared with those of C/C–SiC and C/C–TiC composites. Results showed that the degradations of these composites were primarily caused by the loss of the protective oxide scale via volatilization under the ultra-high temperature and flushing by high-speed airflow. The high ablation resistance of the C/C–SiC–ZrC–TiC composite was attributed to the protection of a multiphase oxide scale with high viscosity and low volatility.     

Revealing the strengthening mechanism in Si3N4 ceramic joint by atomic force microscopy coupled with nanoindentation techniques

The composite filler has been widely introduced for joining ceramic. However, the underlying formation and strengthening mechanisms in the joint remain uncertain. In this study, a commercial Ag–Cu–Ti brazing alloy with Mo particles reinforcement has been introduced for joining Si₃N₄ ceramic and the effect of Mo particles on the microstructure and flexural strength of the joint was investigated. Nanoindentation was employed to characterize the mechanical properties for reaction phases in the joints. The modulus and hardness values for Cu–Ti intermetallics and brazing alloy in the joint were first reported, providing a strong evidence to elucidate the strengthening mechanism. In addition, the strength was increased from 200 MPa, with Ag–Cu–Ti alone, to a maximum of 429 MPa while using Ag–Cu–Ti + 5 vol.% Mo composite filler. We are convinced that, for a well-bonded joint, the thermal expansion mismatch between the joined materials and the plastic deformation in the brazing alloy determined the joint strength.     

Grain growth stagnation in the dense nanocrystalline yttria prepared by combustion reaction and quick pressing with an ultra-high heating rate

Combustion reaction plus quick pressing was a developing technique that used the Joule heating effect of combustion reaction to sinter ceramics, and allows very high heating rate, short soaking duration and high pressure for densification of ceramics. By taking advantages of the particular conditions of this method, pure yttria ceramics with a relative density of 98.5% and an average grain size of 50 nm were obtained at 1620 K and 170 MPa. Moreover, the investigation on the grain growth of sintered yttria was carried out by analyzing the microstructure evolutions and responsible mechanisms. The combined effect of the ultra-high heating rate and the high pressure applied on compact at the peak temperature was effective in suppressing particle coarsening and enhancing densification. Besides, under the decreased sintering temperature and soaking duration, the retained nanostructure assisted to inhibit final-stage grain growth while without impeding the further densification of nanocrystalline ceramics.     

碳纤维在高温下的结构、性能演变研究

针对碳纤维在碳／碳烧蚀防热复合材料中应用的基础问题,论述了不同碳纤维结构、成分、表面特征,及其力学性能和热物理性能的高温演变规律,揭示了碳纤维灰分含量对碳纤维力学性能和热氧化性能的影响。确定了在碳／碳复合材料复合成型过程中,碳纤维结构受基体碳影响的变化规律和碳纤维表面特征对碳／碳材料宏观力学性能的影响。阐明了碳／碳复合材料中碳纤维的力学性能对纤维发生折断烧蚀的阻碍作用和通过控制碳／碳成型最高温度实现提高性能的途径。     

C/C复合材料的SiC/Si-B4C涂层在500~1 500℃的抗氧化机制

为提高C/C复合材料的宽温域抗氧化性能,开发了一种新型SiC/Si-B₄C复合涂层,利用热重法对C/C复合材料的SiC/Si-B₄C复合涂层进行氧化试验,研究了试样从室温到1 500℃的氧化行为,在1 500℃保温2 h后,试样增重仅为2.21%。分别对SiC、Si和B₄C三种粉体进行了不同温度（500~1 500℃）的氧化试验,分析了涂层各组分的高温氧化行为,阐明了SiC、Si和B₄C的有效抗氧化温域,通过氧化动力学计算得到SiC和Si的氧化活化能分别为196.7 kJ/mol和167.3 kJ/mol。结果表明,SiC/Si-B₄C涂层中各组分的抗氧化性能形成了良好的协同作用,复合涂层具有良好的宽温域自愈合能力,在600~1 500℃范围内表现出良好的抗氧化性能。     

A semi-empirical power-law model for the dip-coating of a substrate into a particle-containing,non-Newtonian,complex fluid system

The apparent viscosity of a particle suspension of ZrSi₂ particles, polyhydromethylsiloxane (PHMS) preceramic polymer and n-Octane solvent, used to process polymer-derived ceramic composite coatings, is shown by viscometric experiments to be shear-thinning. The suspension is dip-coated onto substrates and the measured entrained coating thickness, h_0, is observed to be a power-law function of U, the substrate extraction speed, as h₀ = 0.5051U^0.5. The experimentally observed semi-empirical model is directly compared to the results of a variety of theoretically derived Landau-Levich scaling laws and other models that have similar liquids and that include other effects. None of these cases predicts the scaling observed in these experiments. A correction factor is introduced to quantify the difference between the semi-empirical model with existing theoretical models. Possible explanations for the observed scaling behavior are presented.     

Enthalpy driving force and chemical bond weakening: The solid-solution formation mechanism and densification behavior of high-entropy diborides (Hf1−x/4Zr1−x/4Nb1−x/4Ta1−x/4Scx)B2

(Hf_0.2Zr_0.2Nb_0.2Ta_0.2Sc_0.2)B₂ was designed to improve the densification and solid-solution formation of high-entropy transition metal diborides, and its phase stability was predicted using the energy distribution of the local mixing enthalpy of all possible configurations. It was found that (Hf_0.2Zr_0.2Nb_0.2Ta_0.2Sc_0.2)B₂ are enthalpy-stabilized materials. The two-component metal diborides formed by transition metal diborides (HfB₂, ZrB₂, TaB₂ and NbB₂) with ScB₂ are thermodynamically favorable, based on the mixing enthalpy. Therefore, the introduction of ScB₂ in high-entropy metal diborides is beneficial to reduce the mixing Gibbs free energy during the boro/carbothermal reduction process, which enables the formation of single-phase solid solution at low temperatures. Even high-entropy metal diboride powders with large particle sizes, 25–57 µm, can achieve sintered density up to ~97% due to the introduction of ScB₂ in high-entropy metal diborides, owing to its weakening action on the TM d - B p and the TM dd bonding.     

Effect of oxidation on the bending fatigue behavior of an advanced SiC/SiC CMC component at 1000 °C in air

The present study elucidates the effect of oxidation during static and fatigue loading in SiC/SiC CMC structured component, which shows damage in the stress-concentrated region. It is made of Tyranno SA3 fiber, BN (Boron nitride) interphase, and CVI (chemical vapor infiltration) + PIP (polymer impregnation and pyrolysis) hybrid matrix. The comparison based on strength and fracture morphology was made. After annealing, the as-received sample showed minute oxidation and slightly enhanced strength. The fatigued sample without annealing under low stress showed higher retained strength than the as-received sample due to smooth debonding. The fatigued sample with annealing under high stress showed a loss in strength than the as-received sample owing to the formation of a significant amount of borosilicates glasses, which further promoted SiO₂ formation between fiber and matrix and caused the brittle failure. However, simultaneous filling borosilicate glasses into the pores oppositely aided in maintaining the retained strength.