Microwave dielectric properties of Al2O3 ceramics sintered at low temperature

The sintering behavior, microstructure and microwave dielectric properties of Al₂O₃ ceramics co-doped with 3000ppmCuO₂+6000ppmTiO₂+500ppmMgO (Cu/Ti/Mg) have been investigated. The results show that 1 wt% Cu/Ti/Mg can reduce the sintering temperature of Al₂O₃ ceramics effectively. Samples with relative densities of ≥97% and uniform microstructure can be obtained when sintered at 1150 °C. Higher temperature can further increase the density of the sample, but it inevitably leads to abnormal grain growth. Meanwhile, the investigation results show that the low-firing Al₂O₃ ceramics have good microwave dielectric properties especially high Q × f value. A high Q × f value of 109616 GHz is able to be obtained for the 1150 °C sintered sample. The reason for the low temperature densification, abnormal grain growth behavior and the changing trend of the microwave dielectric properties are discussed in the paper.     

Effect of dual liquid phase sintering aids on the densification and microstructure of low temperature sintered alumina ceramics

Alumina ceramics was prepared by pressureless sintering technology in which a CuO–TiO₂–Bi₂O₃ mixture (0–4.0 wt% Bi₂O₃ and 4.0 wt% CuO and TiO₂) was added as dual liquid phase sintering aids. The phase compositions, microstructural feature, and sintering behaviour of the alumina ceramics were analyzed. The results showed that adding 2.5 wt% Bi₂O₃ to alumina ceramics can increase the contribution rate of initial stage of sintering to the sintering process. The relative density of the sample reached 97.63% after sintering at 1200 °C for 90 min. Measurements from differential scanning calorimetry, with the addition of CuO–TiO₂–Bi₂O_3, demonstrated the formation of two liquid phase points, 827.4 and 936.8 °C. Notably, the solid solution temperature of TiO₂ and Al₂O₃ ceramics diminished thanks to the dual liquid phase sintering aids, and at the same time the activation energy required also dropped from 368.96 to 137.31 kJ/mol. Research indicates that the combined action of dual liquid phase sintering and solid-state reaction sintering has promoted the densification of alumina ceramics during the sintering process while at the same time inhibiting the growth of abnormal grains so that a homogeneous microstructure can be formed.     

Effects of sintering curves on microstructure,physical and mechanical properties and on low temperature degradation of zirconia-toughened alumina

The objective of this work was to study two-step sintering as a means of controlling the microstructure of coarse Al₂O₃ matrix composites containing submicrometric and nanometric inclusions of ZrO₂ ranging from 0–30 wt. % by weight based on commercially available powders and evaluate its hydrothermal degradation as function of a water vapour pressure and its mechanical properties. The results showed that two-step sintering allowed a more efficient microstructural control than single-step sintering, resulting in good mechanical properties. The highest flexural strength was achieved for ZTA samples sintered in two-stage sintering conditions TSS2 with T1 = 1560 °C for 3 h, T2 = 1460 °C for 8 h. The studied composites showed good resistance to hydrothermal degradation compared to composites sintered in single step sintering conditions.     

Effect of Dy2O3 content on microstructure and mechanical properties of zirconia-toughened alumina

In this study, the effect of adding Dy₂O₃ on the microstructure and mechanical properties of zirconia-toughened alumina (ZTA) stabilised by yttrium oxide was investigated. ZTA-Dy₂O₃ composites with different Dy₂O₃ contents (0 wt%, 1 wt%, 2 wt%, 3 wt%, and 4 wt%) were prepared by sintering at 1600 °C for 4 h. The phases and structures of the samples were characterised through X-ray diffraction (XRD) and scanning electron microscopy (SEM). Dy₂O₃ formed a solid solution c-DYZ with YSZ, and an appropriate amount of Dy₂O₃ could refine the grains and contribute to densification. The densities, hardness, flexural strength and toughness all increased and then decreased with increasing Dy₂O₃ content, reaching maximum values of 99.2%, 1741 ± 19 HV, 449 ± 10 MPa and 5.87 ± 0.42 MPa?m^1/2, respectively, at 3 wt% Dy₂O₃ content.     

Electrical conductivity and thermal properties of spark plasma sintered Al2O3-SiC-CNT hybrid nanocomposites

In this study, we report the electrical conductivity and thermal properties of Al₂O₃-SiC-CNT hybrid nanocomposites processed via ball milling (BM) and spark plasma sintering (SPS). The initial powders and consolidated samples were characterized using transmission electron microscopy (TEM) and field emission scanning electron microscopy (FE-SEM), respectively. A multifunction calibrator and a high-resolution digital multimeter were used to measure the electrical conductivity. The thermal properties were measured using a thermal constants analyser. The SiC and CNT-reinforced alumina hybrid nanocomposites exhibited a significant increase in their room-temperature electrical conductivity, which made them suitable for electrical discharge machining. The Al₂O₃-5SiC-2CNTs had a high electrical conductivity value of 8.85 S/m compared to a low value of 6.87×10⁻¹⁰ S/m for the monolithic alumina. The addition of SiC and CNTs to alumina decreased its room-temperature thermal properties. The increase in temperature resulted in a decrease in the thermal conductivity and thermal diffusivity but an increase in the specific heat of the monolithic alumina and the hybrid nanocomposites. These properties were correlated with the microstructure, and possible transport mechanisms were discussed.     

Effect of Bi-substitution on the microstructure and electromagnetic properties of YCaZrVIG with low sintering temperature

Bi substituted YCaZrVIG ferrites, Y_2.3−xBi_xCa_0.7Zr_0.3V_0.2Fe_4.42O₁₂ (x=0.1, 0.25, 0.4, 0.5, 0.75) ferrites were prepared by conventional oxide method. The addition of Bi₂O₃ promoted the sintering performance and lowered the sintering temperature from 1420–1230 °C. However, it also resulted in the formation of minor second phases and the decrease of grain size. With the increase of Bi concentration, the dielectric constant increases linearly and then remains unchanged. The dielectric loss decreased firstly and then increased. The saturation magnetization (4πM_s) almost retained unchanged as the Bi concentration increased except for the sample with 0.75. The coercivity (H_c) decreased firstly and reached the minimum of 1.32 Oe at 0.25, and then rose when x>0.25, which was related to the facility of magnetic domain wall motion and magnetic moment reverse. Moderate addition of Bi also can increase the remanence (B_r) by improving sintering process. Additionally, we got the optimum electromagnetic properties in the samples with x=0.25 at 1230 °C: RD>97%, ε_r=15.7, tan δ_e=2.48×10⁻⁴, H_c=1.32Oe, 4πM_S=1663 Gs, B_r=583.91 Gs.     

Effects of YH2 addition on pressureless sintered AlN ceramics

A new type of non-oxide sintering additive of YH₂ was introduced for the fabrication of AlN ceramics with high thermal conductivity and flexural strength. The effects of YH₂ addition (0–5 wt%) on the phase composition, densification, microstructure, thermal conductivity and flexural strength of pressureless sintered AlN ceramics were investigated and compared with those Y₂O₃-added samples (1–5 wt%). The addition of 1 wt% YH₂ led to an in-situ reduction reaction with oxygen impurities, the formation of Y₂O₃ and finally the formation of yttrium aluminate, which in turn improved densification and microstructure. A high flexural strength (408.69 ± 28.23 MPa) was achieved. The addition of 3 wt% YH₂ increased the average grain size and purified the lattice. All these effects are believed to help achieve a high thermal conductivity of 184.82 ± 1.75 W·m^?1·K^?1. Although the thermal conductivity was close to the value of 3 wt% Y₂O₃-added sample, its strength was much increased to 381.53 ± 43.41 MPa. Meanwhile, it demonstrated a good combination of the thermal conductivity and flexural strength than the values reported in some literature. However, further increasing the YH₂ addition to 5 wt% resulted in a high N/O ratio that inhibited the densification behavior of AlN ceramics. The current study showed that AlN ceramics with excellent thermal and mechanical properties could be obtained by the introduction of a suitable YH₂ additive.     

Effect of MgF2 addition on mechanical properties and thermal conductivity of silicon nitride ceramics

Dense silicon nitride (Si₃N₄) ceramics were prepared using Y₂O₃ and MgF₂ as sintering aids by spark plasma sintering (SPS) at 1650 °C for 5 min and post-sintering annealing at 1900 °C for 4 h. Effects of MgF₂ contents on densification, phase transformation, microstructure, mechanical properties, and thermal conductivity of the Si₃N₄ ceramics before and after heat treatment were investigated. Results indicated that the initial temperature of liquid phase was effectively decreased, whereas phase transformation was improved as increasing the content of MgF₂. For optimized mechanical properties and thermal conductivity of Si₃N₄, optimum value for MgF₂ content existed. Sample with 3 mol.% Y₂O₃ and 2 mol.% MgF₂ obtained optimum flexural strength, fracture toughness and thermal conductivity (857 MPa, 7.4 MPa m^1/2 and 76 W m⁻¹ K⁻¹, respectively). It was observed that excessive MgF₂ reduced the performance of the ceramic, which was caused by the presence of excessive volatiles.     

Microstructure and mechanical properties of cold sintered porous alumina ceramics

New innovative approach to fabricate porous alumina ceramics by cold sintering process (CSP) is presented using NaCl as pore forming agent. The effects of CSP and post-annealing temperature on the microstructure and mechanical strength were investigated. Al₂O₃–NaCl composite with bulk density of 2.92 g/cm³ was compacted firstly using CSP and then a porous structure was formed using post-annealing at 1200°C–1500°C for 30 min. Brazilian test method and Vickers hardness test were used to determine the indirect tensile strength and hardness of the porous alumina, respectively. Meanwhile, the phases and the microstructure were respectively examined using X-ray diffractometer and scanning electron microscope (SEM) complemented by the 3D image analysis with X-ray tomography (XRT). SEM structural and XRT image analysis of cold sintered composite showed a dense structure with NaCl precipitated between Al₂O₃ particles. The NaCl volatization from the composite was observed during the annealing and then complete porous Al₂O₃ structure was formed. The porosity decreased from 48 vol% to 28 vol% with the annealing temperature increased from 1200 °C to 1500 °C, while hardness and mechanical strength increased from 14.3 to 115.4 HV and 18.29–132.82 MPa respectively. The BET analysis also showed a complex pore structure of micropores, mesopores and macropores with broad pore size distribution.     

Effect of Nb2O5 and MgO/Nb2O5 doping on densification,microstructure and wear resistance of alumina

In this paper, the influence of Nb₂O₅ single-doping and MgO/Nb₂O₅ co-doping on the densification, microstructure and wear resistance of Al₂O₃ has been investigated. The results show that Nb₂O₅ single-doping can increase the density of alumina effectively, but excessive Nb₂O₅ will lead to abnormal grain growth. Comparing with Nb₂O₅ single-doping, MgO/Nb₂O₅ co-doping can further increase the density and suppress the abnormal grain growth of the alumina. Meanwhile, the co-doped samples also show much lower wear rates. Typically, when 500 ppm MgO/1000 ppm Nb₂O₅ co-doped, the alumina ceramics has a minimum wear rate of 0.01‰, which is about 1/5 of the alumina ceramics with 1000 ppm Nb₂O₅ single-doped. The inhibiting effect of co-doping on abnormal grain growth and the reasons for the decrease of wear rate are also discussed.     

Influence of injection temperature and pressure on the properties of alumina parts fabricated by low pressure injection molding (LPIM)

The quality of ceramics parts made by powder injection molding (PIM) method is influenced by a range of factors such as powder and binder characteristics, rheological behavior of feedstock, molding parameters and debinding and sintering conditions. In this study, to optimize the molding parameters, the effect of injection temperature and pressure on the properties of alumina ceramics in the LPIM process were thoroughly studied. Experimental tests were conducted on alumina feedstock with 60 vol% powder. Injection molding was carried out at temperatures and pressures of 70–100 °C and 0.1–0.6 MPa respectively. Results showed that increase in injection temperature and pressure and the resulting increase in flow rate leads to the formation of void which impairs the properties of molded parts. The SEM studies showed that injection at temperature of 100 °C results in evaporation of binder components. From the processing point of view, the temperature of 80 °C and pressure of 0.6 MPa seems to be the most suitable condition for injection molding. In addition, the effects of sintering conditions (temperature and time) on the microstructure and mechanical properties are discussed. The best final properties were found using injection molding under the above stated conditions, thermal debinding and sintering at 1700 °C during 3 h.     

Effect of diopside addition on sintering and mechanical properties of alumina

In this paper, diopside was introduced in alumina as a sintering aid and fine structural alumina matrix ceramic materials were fabricated by pressureless sintering. The relative density, hardness, fracture toughness and bending strength of the new fabricated composites were measured. Tribological tests were carried out at a given rotation speed of 160 rpm and in a normal load ranged from 50 to 200 N. The experiment results show that the introduction of diopside can enhance densification rate, which may contribute to the improvement in mechanical properties and result in enhanced wear resistances. The effects of diopside on mechanical properties and microstructures of fine structural alumina matrix ceramic materials were analyzed and discussed.     

Mechanical and thermal properties of spark plasma sintered Al2O3-graphene-SiC hybrid composites

Monolithic Al₂O₃ and Al₂O₃-graphene-SiC hybrid composites were prepared by spark plasma sintering (SPS) under vacuum atmosphere. The results show that the hybrid composites were almost completely dense (>97%). SiC content has a significant effect on the microstructure of the composites. With the increase of SiC content, the average grain size of alumina decreased gradually. The addition of SiC to alumina changed fracture mode from inter-granular fracture to mixed fracture mode of inter-granular fracture and trans-granular fracture. The Al₂O₃-0.4 wt%graphene-5 wt% SiC hybrid composite has the highest bending strength and hardness, which were 57% and 19.22% higher than those of the monolithic alumina, respectively. The room temperature (RT) thermal conductivity of the monolithic Al₂O₃ (25.5 W/m·K) was the highest. The thermal conductivity and thermal diffusivity coefficient of the composites decreased with the increase in temperature, while the specific heat of monolithic alumina and composites increased with the increase in temperature and additives. These properties were related to the microstructure of materials and the possible transport mechanisms were discussed.     

The influence of spinel and magnesia powder bed on mechanical properties of alumina sintered under air and nitrogen atmosphere

ABSTRACT

The aim of the present work was changing the surface properties of alumina ceramic via sintering of samples in spinel MgAl₂O₄ and magnesia MgO powder bed. During sintering nitrogen and air atmosphere were used; and the reference material was sintered at the same conditions but in an alumina powder bed. All samples were sintered to a density higher than 99.2% of theoretical density of alumina. In order to examine samples SEM, EDX and XRD (X-ray diffraction from 18 to 70 °2Theta) analysis were performed together with B3B flexural strength measurement. Results revealed that by sintering of alumina samples in a spinel powder bed pore-free surfaces were prepared, which had a favourable effect on B3B flexural strength. This was ascribed to the high solubility of Al³⁺ in spinel at sintering temperatures, which increases the sintering driving force. A further positive effect on B3B flexural strength was observed when samples were sintered in nitrogen instead of air.     

Effect of sintering temperature on microstructure and mechanical properties of zirconia-toughened alumina machinable dental ceramics

This study investigated the effect of sintering temperature on the microstructure and mechanical properties of dental zirconia-toughened alumina (ZTA) machinable ceramics. Six groups of gelcast ZTA ceramic samples sintered at temperatures between 1100 °C and 1450 °C were prepared. The microstructure was investigated by mercury intrusion porosimetry (MIP), X-ray diffraction (XRD), and scanning electron microscopy (SEM) techniques. The mechanical properties were characterized by flexural strength, fracture toughness, Vickers hardness, and machinability. Overall, with increasing temperature, the relative density, flexural strength, fracture toughness, and Vickers hardness values increased and more tetragonal ZrO₂ transformed into monoclinic ZrO₂; on the other hand, the porosity and pore size decreased. Significantly lower brittleness indexes were observed in groups sintered below 1300 °C, and the lowest values were observed at 1200 °C. The highest flexural strength and fracture toughness of ceramics reached 348.27 MPa and 5.23 MPa m^1/2 when sintered at 1450 °C, respectively. By considering the various properties of gelcast ZTA that varied with the sintering temperature, the optimal temperature for excellent machinability was determined to be approximately 1200–1250 °C, and in this range, a low brittleness index and moderate strength of 0.74–1.19 µm^−1/2 and 46.89–120.15 MPa, respectively, were realized.     

Effect of ZrB2 powders on densification,microstructure, mechanical properties and thermal conductivity of ZrB2-SiC ceramics

With the view to improve the densification behaviour and mechanical properties of ZrB₂-SiC ceramics, three synthesis routes were investigated for the production of ZrB₂, prior to the fabrication of ZrB₂-20 vol. % SiC via spark plasma sintering (SPS). Two borothermal reduction routes, modified with a water-washing stage (BRW) and partial solid solution of Ti (BRS), were utilised, alongside a boro/carbothermal mechanism (BRCR) were utilised to synthesise ZrB₂, as a precursor material for the production of ZrB₂-SiC. It was determined that reduction in the primary ZrB₂ particle size, alongside a diminished oxygen content, was capable of improving densification. ZrB₂-SiC ceramics, with ZrB₂ derived from BRW synthesis, exhibited a favorable combination of high relative density (98.6%), promoting a marked increase in Vickers hardness (21.4 ± 1.7 GPa) and improved thermal conductivity (68.7 W·m^-1K^-1).     

A comparative study of thermal conductivity and thermal emissivity of high temperature solar absorber of ZrO2 /Fe2O3 and Al2O3/CuO ceramics

Oxide ceramics are considered as promising high temperature solar absorber materials. The major aim of this work is the development of a new solar absorber material with promising characteristics, high efficiency and low-cost processing. Hence, this work provides a comparative and inclusive study of densification behavior, microstructure features, thermal emissivity and thermal conductivity values of the two new high temperature solar absorbers of ZrO₂/Fe₂O₃ and Al₂O₃/CuO ceramics. Ceramic composites of ZrO₂/(10–30 wt%) Fe₂O₃ and Al₂O₃/(10–30 wt%) CuO were prepared by pressureless sintering method at a temperature of 1700 °C/2hrs. Identification of the solar to thermal efficiency of the composites was evaluated in terms of their measured thermal emissivity. Thermal efficiency and heat transfer homogeneity were investigated in terms of thermal conductivity and diffusivity measurement. The results showed that both composites exhibited comparable densification behavior, homogenous and harmonious microstructure. However, Al₂O₃/10 wt% CuO composite showed higher thermal and solar to thermal efficiencies than ZrO₂/Fe₂O₃ composites. It gave the lowest and the best thermal emissivity of 0.561 and the highest thermal conductivity of 15.4 W/m. K. These values proved to be the best amongst all those of the most known solar absorber materials made from the expensive SiC and AlN ceramics. Thus, Al₂O₃/CuO composites have succeeded in obtaining outstanding properties at a much lower price than its other competitive materials. These results may strongly identify Al₂O₃/CuO composites as promising high-temperature solar absorber materials instead of ZrO₂ and the other carbide and nitride ceramics.     

Effect of thermal insulation on microstructural homogeneity and onset temperature of flash sintered materials

The present work aimed to reduce the microstructure heterogeneity inherent to flash sintering by using alumina blankets as a thermal insulator around ZnO cylindrical samples during the sintering process, under different electric field conditions. Thermal insulation significantly reduced the flash onset temperature and the grain size heterogeneity. For higher electric fields, a temperature reduction as high as 480 °C was observed, which also led to lower densification. These findings were discussed in terms of changes in the heat loss dynamics coupled with the adsorbed water retention, both promoted by the applied thermal insulation. A model to estimate the temperature at stage III of flash sintering was proposed. The final temperature reached with thermal insulation did not differ significantly from the ones without it. Thus, thermal insulation could represent an alternative route to flash sinter materials with lower furnace temperatures with energy savings up to 78 % and a more homogeneous microstructure.     

Structures and electrical conductivities of Gd3+ and Fe3+ co-doped cerium oxide electrolytes sintered at low temperature for ILT-SOFCs

Gd³⁺ and Fe³⁺ co-doped cerium oxide electrolytes, Ce_0.9Gd_0.1‐xFe_xO_2-δ (x?=?0.00, 0.01, 0.03, 0.05, 0.07, 0.10), were prepared by co-precipitation for ultrafine precursor powders and sintering for densified ceramic pellets. The crystal and microscopic structures were characterized by XRD, FESEM and Raman spectroscopy and their electrical properties were studied by AC impedance spectroscopy and the measurement of single cell's outputs. In comparison with Ce_0.9Gd_0.1O_1.95, the ceramic pellets of Ce_0.9Gd_0.1‐xFe_xO_2-δ with a relative density of 95% can be obtained after sintered at 1000?°C for 5?h, showing a remarkably enhanced sintering performance with a sintering temperature reduction of 500?°C, which might be ascribed to the highly activated migration of constituent species in the cerium oxide lattice doped with Gd³⁺ and Fe³⁺ions. Moreover, the electrical conductivity of Ce_0.9Gd_0.1‐xFe_xO_2-δ can be significantly enhanced depending on the mole fraction x, with Ce_0.9Gd_0.07Fe_0.03O_1.95 exhibiting the highest electrical conductivity of 38 mS/cm at 800?°C, about 36% higher than that of Ce_0.9Gd_0.1O_1.95 electrolyte sintered at 1500?°C for 5?h. So, The Gd³⁺ and Fe³⁺ co-doped cerium oxide would be an excellent candidate electrolyte for ILT SOFCs due to its prominent sintering performance and enhanced electrical conductivity.     

Effects of aligned carbon nanotube microcolumns on mechanical and thermal properties of C/SiC composites prepared by LA-CVI methods

Herein, C/SiC-CNTs composites were prepared by laser assisted chemical vapor infiltration (LA-CVI) method combined with vacuum impregnation. Density, mechanical property and thermal conductivity of as-prepared composites were then investigated by various analytical methods. Scanning electron microscopy (SEM) revealed good dispersion of CNTs in C/SiC-CNTs between composites layers and directional heat transfer channels. This formed unique three-dimensional connected networks, reinforcing multi-scale composites matrix. Average density and bending strength of composites were estimated to 2.35 g cm⁻³ and 598 MPa, respectively, which is 20.5% and 27.2% higher than those of CVI-C/SiC composites. The comparison between theoretical thermal conductivity and experiments revealed that the overall thermal conductivity of LA-CVI-C/SiC-CNTs composites (150.42 W m⁻¹ K⁻¹) was nearly 25 times higher than that of CVI-C/SiC composites.