Effects of dopants with various valences on densification behavior and phase composition of a ZrO2–SiO2 nanocrystalline glass-ceramic

Effects of dopants with different valences on the densification behavior and phase composition of a ZrO₂–SiO₂ nanocrystalline glass-ceramic (NCGC) during pressureless sintering were investigated in this study. The raw powder of Ca²⁺, La³⁺, Ce⁴⁺ and Ta⁵⁺ ions doped ZrO₂–SiO₂ (referred to as Ca-ZS, La-ZS, Ce-ZS, Ta-ZS, respectively) and pure ZrO₂–SiO₂ (PZS) sample were synthesized by sol-gel method, followed by pressureless sintering. Compared with the PZS sample, doping of Ca²⁺ and La³⁺ ions significantly promoted the densification of the NCGCs. The “densification promotion” effect was attributed to the formation of oxygen vacancies and the decrease of SiO₂ viscosity due to doping of aliovalent cations. The dopants with various valences showed significant effects on the phase compositions of the NCGCs during sintering. Doping of Ca²⁺ ion accelerated the reaction kinetics between ZrO₂ nanocrystallites and amorphous SiO₂ to yield ZrSiO₄. The La³⁺ ion acted as destabilizer of t-ZrO₂, which resulted in a rapid tetragonal (t) to monoclinic (m) ZrO₂ phase transformation during sintering, while in the Ta⁵⁺ and Ce⁴⁺ ions doped sample, the phase transformation occurred gradually. All the doping ions increased the lattice parameters and the volume of t-ZrO₂ unit cell, while the effects of the doping ions on the lattice parameters of m-ZrO₂ unit cell were more complex.     

Stacking behavior of the close-packed Ta-atom planes and its effects on formation of “hybrid grains” in TaC0.66-0.7 ceramics

In previous works, it was found hard to synthesize “phase pure” ζ-Ta₄C_3-z at relatively low temperatures even by prolonged heating, though ζ-Ta₄C_3-z was believed stable till decomposition at ~2130°C. When the samples were subjected to TEM, vast richness of locally disordered structures in close relation with stacking of the close-pacted Ta-atom planes was observed. Although kinetic factors including diffusion of C atoms/vacancies and re-stacking of the Ta-atom planes explain the densely disordered structures, the richness of local disorders is a scenario that shows cohabitant of the cubic, rhombohedral, and hexagonal structures in a single grain, i.e. formation of a “hybrid grain” consisted of the three symmetries, indicating a transitional or intermediate stage before complete formation of the final phase of rhombohedral ζ-Ta₄C_3-z. This time tantalum carbide ceramics TaC_x with C:Ta atomic ratios x = 0.66 and 0.7 were prepared by reaction hot pressing of TaC and Ta powder mixtures. 5–30 mol% Cu/Ag additives and heat treatments were used to reproduce “hybrid grains” to facilitate further TEM and HRTEM observations on the disordered hybrid grains to argue for the transitional/intermediate stage. The cohabitant cubic, rhombohedral, and hexagonal structures in single grains may also help explain the difficulty in identification of the various phases by XRD in the transitional/intermediate stage of ζ-Ta₄C_3-z reaction. Microstructural evolution and fracture toughness of the composites were also investigated.     

Effect of pyrolysis temperature on the mechanical evolution of SiCf/SiC composites fabricated by PIP

Three types of SiC_f/SiC composites with a four-step three-dimensional SiC fibre preform and pyrocarbon interface fabricated via precursor infiltration and pyrolysis at 1100 °C, 1300 °C, and 1500 °C were heat-treated at 1300 °C under argon atmosphere for 50 h. The effects of the pyrolysis temperature on the microstructural and mechanical properties of the SiC_f/SiC composites were studied. With an increase in the pyrolysis temperature, the SiC crystallite size of the as-fabricated composites increased from 3.4 to 6.4 nm, and the flexural strength decreased from 742 ± 45 to 467 ± 38 MPa. After heat treatment, all the samples exhibited lower mechanical properties, accompanied by grain growth, mass loss, and the formation of open pores. The degree of mechanical degradation decreased with an increase in the pyrolysis temperature. The composites fabricated at 1500 °C exhibited the highest property retention rates with 90% flexural strength and 98% flexural modulus retained. The mechanism of the mechanical evolution after heat treatment was revealed, which suggested that the thermal stability of the mechanical properties is enhanced by the high crystallinity of the SiC matrix after pyrolysis at higher temperatures.     

Compressive strength and microstructure of alkali-activated fly ash/slag binders at high temperature

This paper reports the results of the compressive strength and microstructure of various alkali-activated binders at elevated temperatures of 300 and 600 °C. The binders were prepared by alkali-activated low calcium fly ash/ground granulated blast-furnace slag at ratios of 100/0, 50/50, 10/90 and 0/100 wt.%. Specimens free of loading were heated to a pre-fixed temperature by keeping the furnace temperature constant until the specimens reached a steady state. Then the specimen was loaded to failure while hot. XRD, SEM and FTIR techniques were used to investigate the microstructural changes after the thermal exposure. The fly ash-based specimen shows an increase in strength at 600 °C. On the other hand, the slag-based specimen gives the worst high-temperature performance particularly at a temperature of 300 °C as compared to ordinary Portland cement binder. This contrasting behaviour of binders is due to their different binder formulation which gives rise to various phase transformations at elevated temperatures. The effects of these transformations on the compressive strength are discussed on the basis of experimental results.     

Improving weld formability by a novel dual-rotation bobbin tool friction stir welding

A novel dual-rotation bobbin tool friction stir welding (DBT-FSW) was developed, in which the upper shoulder (US) and lower shoulder (LS) have different rotational speeds. This process was tried to weld 3.2 mm thick aluminum-lithium alloy sheets. The metallographic analysis and torque measurement were carried out to characterize the weld formability. Experimental results show that compared to conventional bobbin tool friction stir welding, the DBT-FSW has an excellent process stability, and can produce the defect-free joints in a wider range of welding parameters. These can be attributed to the significant improvement of material flow caused by the formation of a staggered layer structure and the unbalanced force between the US and LS during the DBT-FSW process.     

Influence of CeO2 addition on the microstructure and mechanical properties of Zirconia-toughened alumina (ZTA) composite prepared by spark plasma sintering

In this study, zirconia-toughened alumina (ZTA) samples with different amounts of CeO₂ were prepared by the spark plasma sintering method. The phase composition and microstructure of the samples were examined by X-ray diffraction, scanning electron microscopy, and energy-dispersive X-ray spectroscopy. The addition of CeO₂ results in grain refinement and density increase; moreover, CeO₂ stabilises the high-temperature metastable phase. As the amount of CeO₂ reaches 7 wt%, a new CeAl₁₁O₁₈ phase appears. The Vickers hardness, modulus, and fracture toughness of the samples depend to a large extent on the grain size, relative density, and existence of the second phase. Among the composites, that with 5 wt% CeO₂ shows the best performance with the highest values of relative density, Vickers hardness, and fracture toughness: 96.51%, 1688 HV, and 9.91 MPa.√m, respectively.     

Effect of Al2O3 particles on mechanical and tribological properties of Al–Mg dual-matrix nanocomposites

This article aims to manufacture homogenous dual-matrix Al–Mg/Al₂O₃ nanocomposite from their raw materials and give insight into the correlation between powder morphology, crystallite structure and their mechanical and tribological properties. Al–Mg dual-matrix reinforced with micro/nano Al₂O₃ particles was manufactured by a novel double high-energy ball milling process followed by a cold consolidation and sintering. Microstructure and phase composition of the prepared samples were characterized using FE-SEM, EDS and XRD inspections. Mechanical and wear properties were characterized using compression and sliding wear tests. The results showed that a milling of Mg with Al₂O₃ particles in an initial step before mixing with Al has the beneficial of well dispersion of Al₂O₃ nanoparticles in Al–Mg dual matrix. The Al–Mg dual matrix reinforced with nano-size Al₂O₃ showed 3.29-times smaller crystallite size than pure Al. Moreover, the hardness and compressive strength are enhanced by adding nano-size Al₂O₃ with Al–Mg dual matrix composite while the ductility is maintained relatively high. Additionally, the wear rate of this composite was reduced by a factor of 2.7 compared to pure Al. The reduced crystallite size, the dispersion of Al₂O₃ nanoparticles and the formation of (Al–Mg)_ss were the main improvement factors for mechanical and wear properties.     

Joining ZTA ceramic by using Dy2O3-Al2O3-SiO2 glass ceramic filler

In this paper, a novel Dy₂O₃-Al₂O₃-SiO₂ (DAS) glass ceramic was designed and prepared for joining zirconia toughened alumina (ZTA) ceramic. The crystallization, thermal expansion behavior and wetting behavior of the DAS glass filler were studied. The effect of cooling rate and joining temperature on the microstructure and flexural strength of joints was investigated. The results show that slow cooling rate (15 °C/min) leads to crystallization of brazing seam, which causes the formation of pores in the joints due to the large density difference between the glass and the crystalline phases. The dissolution of ZrO₂ from ZTA substrate into the filler during joining process improves the mismatch of the coefficient of thermal expansion (CTE) between the brazing seam and substrate. The maximum flexural strength of 535 MPa is obtained when the joining temperature and cooling rate are 1475 °C and 50 °C/min, respectively.     

Microstructure evolution and grain growth mechanisms of h-BN ceramics during hot-pressing

Pure h-BN ceramic specimens were prepared by hot-pressing under different sintering temperatures and pressures using ball milled h-BN powders composed of amorphous and nanocrystalline BN. Microstructures and thermal conductivities of these h-BN ceramic specimens were characterized and measured. Higher sintering pressure is more favorable to the preferred orientation growth of plate-like h-BN grains along the pressure direction, forming microstructures where the c-axes of h-BN grains are preferentially oriented perpendicular to the pressure direction. However, such microstructures can only be obtained at appropriate sintering temperature. Thermal conductivities of h-BN ceramic specimens are strongly related to their microstructures, especially the grain orientation. Growth mechanisms of h-BN grains were investigated. There is multi-area co-growth phenomenon around the grain boundaries composed of the basal planes of h-BN grains, which results in the formation of stacking faults in the as-grown h-BN grains.     

Micromechanical properties and microstructural evolution of Amosic-3 SiC/SiC composites irradiated by silicon ions

In this work, Amosic-3 SiC/SiC composites were irradiated to 10 dpa and 115 dpa with 300 keV Si ions at 300 °C. To evaluate its irradiation behaviour and investigate the underlying mechanism, nanoindentation, AFM, Raman and electron microscopy were utilized. Nanoindentation showed that although micromechanical properties declined after irradiation, hardness and Young’s modulus were maintained better under 115 dpa. AFM manifested differential swelling among PyC interface, fiber and matrix and SEM showed irradiation-induced partial interface debonding, which are both more obvious under 115 dpa. TEM revealed the generation and proliferation of amorphous regions, which is according with the decline and broadening of peaks in Raman spectra. The material was almost completely amorphous after irradiated to 10 dpa while recrystallization occurred under 115 dpa. All results mentioned above contribute to the decline of hardness and Young’s modulus and may explain why the micromechanical degradation was more significant under 10 dpa.