Facile synthesis of a carbon-rich SiAlCN precursor and investigation of its structural evolution during the polymer-ceramic conversion process

A liquid carbon-rich SiAlCN precursor is facilely synthetized by hydrosilylation between liquid polyaluminocarbosilane (LPACS) and 1,3,5,7-tetravinyl- 1,3,5,7-tetramethylcyclotetrasilazane {[CH₃(CH₂CH₂)SiNH]₄} (TeVSZ). The structural evolution during the polymer-ceramic conversion process is investigated by various methods. The results show that the main cured mechanism is β-addition on hydrosilylation, although α-addition on hydrosilylation, polymerization of vinyl groups and dehydrocoupling reaction between N–H bonds also occur during the cured process. During the pyrolysis process, dehydrogenation and dehydrocarbonation condensation reactions, transamination reactions occur, leading to formation of a three-dimensional network inorganic structure at 400–800 °C, where part of Al–O bonds convert to Al–N bonds. Then the network inorganic structure undergoes demixing and separation into amorphous SiAlCN(O) phase, where the amorphous turbostratic free carbon phase also form at 800–1200 °C. With demixing and decomposition of the amorphous carbon-rich SiAlCN(O) phase, the crystalline β-SiC and graphitic carbon start to form at about 1400 °C, the crystalline sizes of them both enlarge with increasing temperature. However, the crystal growth of β-SiC is distinctly inhibited due to existence of the rich carbon phase, tiny amounts of Al₂O₃ and AlN. In addition, a small amount of AlN can promote the formation of α-SiC at 1800 °C.     

单晶SiC的电助光催化抛光及去除机理

为满足电子半导体等领域对SiC超光滑、无损伤和材料高效去除的要求，提出了电助光催化抛光SiC的新方法。研究了光催化剂种类及其pH值对抛光液氧化性和抛光效果的影响，讨论了材料的去除机理。结果表明：以p25型TiO2为光催化剂配制抛光液所获得的最大氧化还原电位为633.11 mV，材料去除率为1.18 μm/h，表面粗糙度Ra=0.218 nm；抛光后SiC表面氧化产物中，Si-C-O、Si-O和Si4C4O4的含量明显增加，SiC表面被氧化并被机械去除是主要的材料去除方式。     

Highly efficient chemical mechanical polishing method for SiC substrates using enhanced slurry containing bubbles of ozone gas

In this study, a highly efficient method for chemical mechanical polishing (CMP) of silicon carbide (SiC) substrates using enhanced slurry was proposed and developed. The enhanced slurry contains bubbles of ozone gas generated by ozone gas generator in pure water mixed with a conventional commercially available slurry. Therefore, the enhanced slurry has an oxidizing effect on the Si-face of SiC substrates. To confirm the effectiveness of bubbles enclosing ozone gas, both nano-indentation test and X-ray photoelectron spectroscopy (XPS) analysis were conducted. As a result, the hardness decrease of the Si-face of the SiC substrate was confirmed through the nano-indentation test, and the generation of reaction products was confirmed on Si-face of SiC substrate in the XPS analysis. According to a series of experimental results of our proposed highly efficient CMP method for SiC substrates, the removal rate can be increased when the enhanced slurry was applied, comparing with that for the not only conventional commercially available slurry but also commercially available dedicated slurry.     

Fabrication and mechanical properties of large-scale SiC impeller via vacuum gelcasting and pressureless sintering

Impeller is the key part of centrifugal pump to convey liquid. And combined with the engineering practice, we fabricated two types of open and semi-open SiC ceramic impellers with diameter of 100 mm and 160 mm via gelcasting and pressureless sintering. B4C and C were used as the sintering additives and sprayed drying granulation method was adopted for the starting SiC powder processing. Given the size and shape complexity of impeller, the optimized pH value, dispersant content, and solid-loading content for the fabrication of the SiC impellers were determined to be 10-11, 0.8 wt%, and 40 vol%, respectively. For the open impeller, blade height, cover board thickness, drying shrinkage, and sintering shrinkage are 10.5 mm, 4 mm, 10.3%, and 21.3%, respectively. For the semi-open ones, the corresponding parameters are 41 mm, 10 mm, 10.3%, and 21.3%, respectively. The average density of the two types of impellers is 3.15 g/cm3, and the mechanical properties of both impellers, including average hardness, flexural strength, compressive strength, and fracture toughness are 2478 HV, 436 MPa, 2093 MPa, and 3.17 MPa·m1/2, respectively. All variation coefficient values are smaller than 5%, which indicates a good uniformity in densities and mechanical properties of both the impellers.     

In‐plane shear damage behaviours of 2D needled C/SiC composites

Understanding the in‐plane shear behaviour of composites is essential to establish the design basis for practical applications. This study aims to investigate the shear damage behaviours of 2D needled C/SiC composites by various characterization techniques. The effect of layer arrangement on shear modulus and strength was discussed via shear stress‐strain responses. The shear strain field evolution and uniformity variation were studied by digital image correlation. It shows that the uniformity of shear strain field changes with the shear load, and the shear strain field evolution consist of 5 stages. The electrical resistivity measurement results indicate that structural deformation and damage evolution caused the electrical resistivity change. Furthermore, the damage evolution has a double effect on the electrical resistivity variation. The acoustic emission monitoring shows that the shear damage evolution is a 3‐stage nonlinear process before failure. The shear damages were categorized via acoustic characteristics. Besides, the postfailure behaviours were also discussed in this study.     

Microwave synthesis of worm-like SiC nanowires for thin electromagnetic wave absorbing materials

Thin thickness is always the pursuit of excellent electromagnetic wave absorbing materials. Herein, SiC nanowires with worm-like morphology were synthesized by microwave heating the mixture of expanded graphite and silica. The worm-like SiC nanowires exhibit an excellent microwave absorption ability at a thin thickness. With the filling ratio of SiC nanowires increases in the matrix, the dielectric loss and microwave absorbing ability are significantly enhanced; meanwhile the number of absorption peaks is gradually increased, and the absorption peaks also move toward a thinner thickness. When the nanowires filling ratio was 40?wt%, the minimum reflection loss reached down to ?35.2?dB and the effective absorption (RL?<??10?dB) bandwidth was 1.8?GHz?at a thickness of 1.3?mm. The possible growth mechanism of the worm-like SiC nanowires is that the intermediate reaction gas phases, SiO and CO, were confined in the relatively independent tiny pores of expanded graphite. This resulting in an excessive local gas phase pressure, which causes the nanowire growth direction changes randomly.     

Effects of corrosion in liquid fluoride salt on the tensile strength of domestic SiC fibers

The relationship between the tensile strength of corroded domestic second-generation (2ed-gen) SiC fibers at various temperatures for 500 h in 46.5LiF-11.5NaF-42.0KF (mol. %) eutectic salt and the typical microstructure was studied. Weibull theory was used to analyze the critical defects that caused the tensile fracture, and the microstructure of fibers before and after corrosion was characterized. It is concluded that the decrease of tensile strength after corrosion at 800 °C is caused by the surface injury of fibers, which led to the shift of critical defects from the internal defects of virgin fibers to surface defects. Moreover, corrosion at higher temperature accelerates the corrosion process and dissolve the surface O-contained layer thoroughly. This shifts the critical defects back to the internal defects and will be helpful for the recovery of tensile strength of corroded fibers at the higher temperature.     

Effect of Co addition on microstructural and mechanical properties of WC–B4C–SiC composites

In this study, the effect of Co addition on microstructural and mechanical properties of WC-B₄C–SiC composites sintered by spark plasma sintering (SPS) method was investigated. For this purpose, three batches of WC-B₄C–SiC with different contents of Co (10 vol%, 15 vol%, and 20 Vol %) were sintered at 1400 °C. The results of X-ray diffraction (XRD) analysis of the samples indicated the formation of W₂B₅, W₃CoB₃ as well as the remained C phases and unreacted SiC phase. It was observed that by increasing the Co content, the amount of W₂B₅ phase reduces and W₃CoB₃ and C contents increase. Therefore, W₂B₅ peaks were not detected in the sample containing 20vol% Co. Relative density values above 97% were obtained for all the composites. However, a decrease was observed in relative density by increasing the Co content in the composites. The highest flexural strength (510 ± 42 MPa), fracture toughness (10.34 ± 0.82 MPa m^1/2), and hardness (20.63 ± 0.75 GPa) were also obtained for the sample containing 10vol% Co compared to the other samples. In addition, Transgranular fracture of SiC as well as pulling out of W₃CoB₃ and W₂B₅ particles were observed in the fracture surface micrographs of the samples. The presence of micro-cracks in the SiC grains, fracture of W₃CoB₃ grains, and crack deflection was reported as dominant toughening mechanisms.     

Centimeter-scale low-damage micromachining on single-crystal 4H–SiC substrates using a femtosecond laser with square-shaped Flat-Top focus spots

Femtosecond (fs) lasers have been proved to be reliable tools for high-precision and high-quality micromachining of ceramic materials. Nevertheless, fs laser processing using a single-mode beam with a Gaussian intensity distribution is difficult to obtain large-area flat and uniform processed surfaces. In this study, we utilize a customized diffractive optical element (DOE) to redistribute the laser pulse energy from Gaussian to square-shaped Flat-Top profile to realize centimeter-scale low-damage micromachining on single-crystal 4H–SiC substrates. We systematically investigated the effects of processing parameters on the changes in surface morphology and composition, and an optimal processing strategy was provided. Mechanisms of the formation of surface nanoparticles and the removal of surface micro-burrs were discussed. We also examined the distribution of subsurface defects caused by fs laser processing by removing a thin surface layer with a certain depth through chemical mechanical polishing (CMP). Our results show that laser-induced periodic surface structures (LIPSSs) covered by fine SiO₂ nanoparticles form on the fs laser-processed areas. Under optimal parameters, the redeposition of SiO₂ nanoparticles can be minimized, and the surface roughness Sa of processed areas reaches 120 ± 8 nm after the removal of a 10 μm thick surface layer. After the laser processing, micro-burrs on original surfaces are effectively removed, and thus the average profile roughness Rz of 2 mm long surface profiles decreases from 920 ± 120 nm to 286 ± 90 nm. No visible micro-pits can be found after removing ~1 μm thick surface layer from the laser-processed substrates.