Densification mechanism and microstructure characteristics of nano- and micro- crystalline alumina by high-pressure and low temperature sintering

Fully dense ceramics with retarded grain growth can be attained effectively at relatively low temperatures using a high-pressure sintering method. However, there is a paucity of in-depth research on the densification mechanism, grain growth process, grain boundary characterization, and residual stress. Using a strong, reliable die made from a carbon-fiber-reinforced carbon (C_f/C) composite for spark plasma sintering, two kinds of commercially pure α-Al₂O₃ powders, with average particle sizes of 220 nm and 3 μm, were sintered at relatively low temperatures and under high pressures of up to 200 MPa. The sintering densification temperature and the starting threshold temperature of grain growth (T_sg) were determined by the applied pressure and the surface energy relative to grain size, as they were both observed to increase with grain size and to decrease with applied pressure. Densification with limited grain coarsening occurred under an applied pressure of 200 MPa at 1050 °C for the 220 nm Al₂O₃ powder and 1400 °C for the 3 μm Al₂O₃ powder. The grain boundary energy, residual stress, and dislocation density of the ceramics sintered under high pressure and low temperature were higher than those of the samples sintered without additional pressure. Plastic deformation occurring at the contact area of the adjacent particles was proved to be the dominant mechanism for sintering under high pressure, and a mathematical model based on the plasticity mechanics and close packing of equal spheres was established. Based on the mathematical model, the predicted relative density of an Al₂O₃ compact can reach ～80 % via the plastic deformation mechanism, which fits well with experimental observations. The densification kinetics were investigated from the sintering parameters, i.e., the holding temperature, dwell time, and applied pressure. Diffusion, grain boundary sliding, and dislocation motion were assistant mechanisms in the final stage of sintering, as indicated by the stress exponent and the microstructural evolution. During the sintering of the 220 nm alumina at 1125 °C and 100 MPa, the deformation tends to increase defects and vacancies generation, both of which accelerate lattice diffusion and thus enhance grain growth.     

Recent advances in carbon nanotubes-based microwave absorbing composites

With the blossom of information industry, electromagnetic wave technology shows increasingly potential in many fields. Nevertheless, the trouble caused by electromagnetic waves has also drawn extensive attention. For instance, electromagnetic pollution can threaten information safety in vital fields and the normal function of delicate electronic devices. Consequently, electromagnetic pollution and interference become an urgent issue that needs to be addressed. Carbon nanotubes (CNTs) have become a potential candidate to deal with these problems due to many advantages, such as high dielectric loss, remarkable thermodynamic stability, and low density. With the appearance of climbing demands, however, the carbon nanotubes combining various composites have shown greater prospects than the single CNTs in microwave absorbing materials. In this short review, recent advances in CNTs-based microwave absorbing materials were comprehensively discussed. Typically, we introduced the electromagnetic wave absorption mechanism of CNTs-based microwave absorbing materials and generalized the development of CNTs-based microwave absorbers, including CNTs-based magnetic metal composites, CNTs-based ferrite composites, and CNTs-based polymer composites. Ultimately, the growing trend and bottleneck of CNTs-based composites for microwave absorption were analyzed to provide some available ideas to more scientific workers.     

Achieving fabrication of highly transparent Y2O3 ceramics via air pre-sintering by deionization treatment of suspension

An easy albeit quite effective deionization suspension treatment was adopted to alleviate the detrimental effects related to the hydrolysis of Y₂O₃ in an aqueous medium. Fabrication of highly transparent Y₂O₃ ceramics with a fine grain size via air pre-sintering and post–hot isostatic pressing (HIP) treatment without using any sintering additive was achieved using the treated suspensions. The hydrolysis issue of Y₂O₃ powder in an aqueous medium was effectively alleviated by using deionization treatment, and a well-dispersed suspension with a low concentration of dissolved Y³⁺ species was obtained. The dispersed suspensions were consolidated by the centrifugal casting method, and the green bodies derived from the suspension of 35.0 vol% solid loading showed an improved homogeneity with a relative density of 52.1%. Fully dense Y₂O₃ transparent ceramic with high transparency was obtained by pre-sintering consolidated green compacts at a low temperature of 1400°C for 16 h in air followed by a post-HIP treatment at 1550°C for 2 h under 200 MPa pressure. The sample had a fine average grain size of 690 nm. The in-line transmittance of the sample reached 83.3% and 81.8% at 1100 nm and 800 nm, respectively, very close to the theoretical values of Y₂O₃.     

Highly oriented α-Al2O3 transparent ceramics shaped by shear force

Alumina platelets were arranged horizontally in submicron alumina particles by shear force in the flow of slurries during casting. The obtained alumina green bodies with platelets were pressureless-sintered in vacuum, producing ceramics with thoroughly oriented grains and high transmittance. The effects of sintering parameters on the densification, microstructure evolution, and orientation degree of alumina ceramics were investigated and discussed. The results showed that the densification, grain size, orientation degree, and in-line transmittance were increased with increasing sintering temperature. The enhancement of orientation degree was mainly coherent with grain growth. The grain-oriented samples exhibited a much higher in-line transmittance (at 600 nm) of 61 % than that of the grain random sample (29 %). Moreover, the transmission remained a high level in the ultraviolet range (<300 nm).     

Susceptor-assisted fast microwave sintering of TiN reinforced SiAlON composites in a single mode cavity

In the present study, 17 wt % TiN reinforced α-β SiAlON composites were sintered at low temperature by susceptor-assisted microwave heating. The effect of TiN addition on dielectrical properties of starting powders, as well as the influence of sintering temperature on phase evolution, microstructure development and mechanical properties of α/β-SiAlON-TiN composites were investigated. The obtained results showed that TiN addition increased the microwave absorbing properties which is reflected in the peak sintering temperature. Thus, the α:β ratio decreased and mechanical properties were improved, especially the fracture toughness of the composites. Furthermore, an estimate of energy consumption during microwave assisted sintering at the laboratory scale is presented. As a result, the highest values for relative density (97.1%), Vickers hardness (13.35 ± 0.47 GPa), and fracture toughness (7.52 ± 0.54 MPa m^1/2) were obtained by microwave sintering for 30 min at 1300 °C.     

Structural dependence of microwave dielectric properties in ilmenite-type Mg(Ti1-xNbx)O3 solid solutions by Rietveld refinement and Raman spectra

Mg(Ti_1-xNb_x)O₃ (x = 0–0.09) ceramics were prepared by the conventional solid-state reaction method. The phase composition, sintering characteristics, microstructure and dielectric properties of Ti⁴⁺ replacement by Nb⁵⁺ in the formed solid solution Mg(Ti_1-xNb_x)O₃ (x = 0–0.09) ceramics were systematically studied. The structural variations and influence of Nb⁵⁺ doping in Mg(Ti_1-xNb_x)O₃ were also systematically investigated by X-ray diffraction and Raman spectroscopy, respectively. X-ray diffraction and its Rietveld refinement results confirmed that Mg(Ti_1-xNb_x)O₃ (x = 0–0.09) ceramics crystallised into an ilmenite-type with R-3 (148) space group. The replacement of the low valence Ti⁴⁺ by the high valence Nb⁵⁺ can improve the dielectric properties of Mg(Ti_1-xNb_x)O₃ (x = 0–0.09). This paper also studied the different sintering temperatures for Mg(Ti_1-xNb_x)O₃ (x = 0–0.09) ceramics. The obtained results proved that 1350 °C is the best sintering temperature. The permittivity and Q × f initially increased and then decreased mainly due to the effects of porosity caused by the sintering temperature and the doping amount of Nb₂O₅, respectively. Furthermore, the increased Q × f is correlated to the increase in Ti–O bond strength as confirmed by Raman spectroscopy, and the electrons generated by the oxygen vacancies will be compensated by Nb⁵⁺ to a certain extent to suppress Ti⁴⁺ to Ti³⁺, which was confirmed by XPS. The increase in τ_f from ?47 ppm/°C to ?40.1 ppm/°C is due to the increment in cell polarisability. Another reason for the increased τ_f is the reduction in the distortion degree of the [TiO₆] octahedral, which was also confirmed by Raman spectroscopy. Mg(Ti_0.95Nb_0.05)O₃ ceramics sintered at 1350 °C for 2 h possessed excellent microwave dielectric properties of ε_r = 18.12, Q × f = 163618 GHz and τ_f = ?40.1 ppm/°C.     

Optimized microwave absorption properties by tailoring the morphology of carbon coated TiC nanoparticles by N2 pressure

Increasing the dielectric loss capacity plays an important role in enhancing the electromagnetic absorption performance of materials. It remains a challenge to simultaneously introduce multiple types of dielectric losses in the material. In this work, we show that the atomic and interfacial dipole polarizations can be simultaneously enhanced by substituting N species into both carbon coating layers and bulk TiC lattices of a core-shell TiC@C material. Additionally, substitution of N species results more exposed TiC(111) facets and refines the TiC grain sizes in the bulk material, which is beneficial for enhancing the scattering of the external electromagnetic waves. The maximum reflection loss of the N substituted TiC@C material is measured as ?47.1 dB with an effective absorbing bandwidth of 4.83 GHz at 1.9 mm, which illustrates a valuable way to further tuning the electromagnetic absorption performance of this type of materials.     

Effect of microwave sintering on the microstructure and mechanical properties of AA7075/B4C/ZrC hybrid nano composite fabricated by powder metallurgy techniques

AA7075 + 6%B4C+3%ZrC nano hybrid composite was successfully fabricated, with nano reinforcements composition in AA7075 alloy selected based on previous investigation, to achieve better mechanical performance. Two different sintering techniques, namely conventional and microwave, were implemented to determine the effect on microstructural and mechanical properties. Microstructural investigation was performed with the help of W-SEM. Tensile, compression, and hardness were measured with the help of UTM and Vickers microhardness machine. Porosity was calculated by using Archimedes principle. It was observed that the added nano ZrC particles formed agglomerates and the B₄C particles were distributed homogenously. Composites processed by microwave sintering showed excellent mechanical properties compared to the conventionally sintered composites. No intermetallic compounds were detected in microwave sintered composites through XRD analysis, indicating strong and clean interface bonds between matrix and reinforcement particles. High strain to fracture value of 12.24% was noted in microwave sintered nano hybrid composite, while it was 6.12% for conventional sintered one. Fractography revealed no peeling action of reinforcements from the matrix material, and the mode of failure was brittle. It was concluded that, while fabricating nano range hybrid composites, the implementation of advanced sintering technique (microwave sintering) with low sintering temperatures and low sintering times with internal heat generations, helps in eliminating defects that may develop because of high surface energies of nano range reinforcements.     

Fabrication of Nd-doped Ni–Zn ferrite/multi-walled carbon nanotubes composites with effective microwave absorption properties

The electromagnetic materials are featured by good magnetic permeability and dielectric constant characteristics, which are of significant importance in solving the pollution problem of electromagnetic. In this study, after the complete of the use of sol-gel method, argon gas was then introduced for calcination, and eventually a new type of MWCNTs/Ni_0.5Zn_0.5Nd_0.04Fe_1.96O₄ composites was synthesized after the above mentioned procedures. The synthesized MWCNTs were able to be adsorbed on the surface of Ni_0.5Zn_0.5Nd_0.04Fe_1.96O₄ and could form a good conductive work of 3D. Also, the effect of additional MWCNTs on microwave absorption properties of MWCNTs/Ni_0.5Zn_0.5Nd_0.04Fe_1.96O₄ composites were also observed in this study. The results indicate that the additional MWCNTs function to significantly improve the microwave absorption property of MWCNTs/Ni_0.5Zn_0.5Nd_0.04Fe_1.96O₄. Through altering the amount of MWCNTs, the microwave attenuation performance and impedance matching coefficient of this electromagnetic materials can be effectively improved. The S2 sample presented a minimum reflection loss of ?35.05 dB when its thickness reached 1.6 mm, meanwhile, the effective absorption bandwidth achieved 4.55 GHz. The prepared composites perform well in microwave absorption, which can attribute to the reasonable ratio of composites as well as its interaction with both of the magnetic and dielectric components. This research paved the way for novel ideas to be put in the electromagnetic absorption materials with high-efficient.     

A thermal perspective of flash sintering: The effect of AC current ramp rate on microstructure evolution

In flash sintering experiments, the thermal history of the sample is key to understanding the mechanisms underlying densification rate and final properties. By combining robust temperature measurements with current-ramp-rate control, this study examined the effects of the thermal profile on the flash sintering of yttria-stabilized zirconia, with experiments ranging from a few seconds to several hours. The final density was maximized at slower heating rates, although processes slower than a certain threshold led to grain growth. The amount of grain growth observed was comparable to a similar conventional thermal process. The bulk electrical conductivity correlated with the maximum temperature and cooling rate. The only property that exhibited behavior that could not be attributed to solely the thermal profile was the grain boundary conductivity, which was consistently higher than conventional in flash sintered samples. These results suggest that, during flash sintering, athermal electric field effects are relegated to the grain boundary.