The effect of nano-Cr2O3 on solid-solution assisted sintering of MgO refractories

The effect of Cr₂O₃ particle size on the densification of magnesia refractories was investigated. Magnesia grains (<45 μm) were mixed with 2 wt% of micro-Cr₂O₃ (2 μm) and nano-Cr₂O₃ particles (10–20 nm) and sintered at 850–1450 °C, for 5 h in air. The progress of the densification and phase evolution of samples was studied with the support of X-ray diffraction phase analysis (XRD), Fourier transformer infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). It was shown that the densification of magnesia was enhanced by reducing the particle size of the added chromia to the range of 20 nm. According to the phase analysis results, the higher dissolution rate of Cr₂O₃ in MgO in the MgO–Cr₂O₃ system was responsible for the faster densification of nano-Cr₂O₃ containing mixes.     

Influence of magnesia on sintering stress of alumina

The sintering stress and the densification of MgO-doped Al₂O₃ were measured with a self-loading apparatus and a thermomechanical analyzer, respectively. The densification started at 950 °C and finished at about 1450 °C. The measured surface tensions were 0.7–0.8 N m⁻¹ in the intermediate sintering stage but drastically decreased to 0.2 N m⁻¹ in the final stage of sintering.     

High-pressure sintered yttria stabilized zirconia ceramics

Fast densification of 8YSZ ceramics under a high pressure of 4.5 GPa was carried out at different temperatures (800, 1000, 1450 °C), by which a high relative density above 92% could be obtained. FT-Raman spectra indicate that the 8YSZ underwent a phase transition from partially tetragonal to partially cubic phase as temperatures increase from 1000 to 1450 °C when sintering under high pressure. The electrical properties of the samples under different high-pressure sintering conditions were measured by complex impedance method. The total conductivity of 0.92 × 10⁻² S cm⁻¹ at 800 °C has been obtained for 8YSZ under high pressure at 1450 °C, which is about 200 °C lower than that of the samples prepared by conventional pressureless sintering.     

Sintering of Al2O3-SiC composite from sol-gel method with MgO, TiO2 and Y2O3 addition

Al₂O₃-SiC composite ceramics were prepared by pressureless sintering with and without the addition of MgO, TiO₂ and Y₂O₃ as sintering aids. The effects of these compositional variables on final density and hardness were investigated. In the present article at first α-Al₂O₃ and β-SiC nano powders have been synthesized by sol-gel method separately by using AlCl₃, TEOS and saccharose as precursors. Pressureless sintering was carried out in nitrogen atmosphere at 1600 °C and 1630 °C. The addition of 5 vol.% SiC to Al₂O₃ hindered densification. In contrast, the addition of nano MgO and nano TiO₂ to Al₂O₃-5 vol.% SiC composites improved densification but Y₂O₃ did not have positive effect on sintering. Maximum density (97%) was achieved at 1630 °C. Vickers hardness was 17.7 GPa after sintering at 1630 °C. SEM revealed that the SiC particles were well distributed throughout the composite microstructures. The precursors and the resultant powders were characterized by XRD, STA and SEM.     

Two-step sintering of fine alumina–zirconia ceramics

This work investigates the feasibility to the fabrication of high density of fine alumina–5 wt.% zirconia ceramics by two-step sintering process. First step is carried out by constant-heating-rate (CHR) sintering in order to obtain an initial high density and a second step is held at a lower temperature by isothermal sintering aiming to increase the density without obvious grain growth. Experiments are conducted to determine the appropriate temperatures for each step. The temperature range between 1400 and 1450 °C is effective for the first step sintering (T₁) due to its highest densification rate. The isothermal sintering is then carried out at 1350–1400 °C (T₂) for various hours in order to avoid the surface diffusion and improve the density at the same time. The content of zirconia provides a pinning effect to the grain growth of alumina. A high ceramic density over 99% with small alumina size controlled in submicron level (0.62–0.88 μm) is achieved.     

Densification and characterization of SiO2B2O3CaOMgO glass/Al2O3 composites for LTCC application

A glass/ceramic composite using lead-free low melting glass (SiO₂B₂O₃CaOMgO glass) with Al₂O₃ fillers was investigated. X-ray diffraction analysis revealed that the anorthite and cordierite phase appeared in the sintered composites. The dilatometric analysis showed that the onset of shrinkage took place at ∼624 °C for all the samples and the onset temperature was independent on the content of glass. The low melting glass significantly promoted densification of the composites and lowered the sintering temperature to ∼875 °C. The addition of 50 wt% glass sintered at 875 °C showed ε_r of 7.3, tan δ of 1.15×10⁻³, TEC of 5.41 ppm/°C, thermal conductivity of 3.56 W/m °C, and flexural strength of 184 MPa. The results showed that the SiO₂B₂O₃CaOMgO glass/Al₂O₃ composites were strong potential candidates for low temperature cofired ceramic substrate applications.     

Transparent polycrystalline MgAl2O4 ceramic fabricated by spark plasma sintering: Microwave dielectric and optical properties

The optical properties and microwave dielectric properties of transparent polycrystalline MgAl₂O₄ ceramics sintered by spark plasma sintering (SPS) through homemade nanosized MgAl₂O₄ powders at temperatures between 1250 °C and 1375 °C are discussed. The results indicate that, with increasing sintering temperatures, grain growth and densification occurred up to 1275 °C, and above 1350 °C, rapid grain and pore growth occurred. The in-line light transmission increases with the densification and decreases with the grain/pore growth, which can be as high as 70% at the wavelength of 550 nm and 82% at the wavelength of 2000 nm, respectively. As the sintering temperature increases, Q×f and dielectric constant ε_r values increase to maximum and then decrease respectively, while τ_f value is almost independent of the sintering temperatures and remains between −77 and −71 ppm/°C. The optimal microwave dielectric properties (ε_r=8.38, Q×f=54,000 GHz and τ_f=−74 ppm/°C) are achieved for transparent MgAl₂O₄ ceramics produced by spark plasma sintering at 1325 °C for 20 min.     

Low temperature sintering of barium titanate based ceramics with high dielectric constant for LTCC applications

The sintering temperature of BaTiO₃ powder was reduced to 900 °C due to the ZnO-B₂O₃-Li₂O-Nb₂O₅-Co₂O₃ addition. Excellent densification was achieved after sintering at 900 °C for 2 h. The low sintering temperature of newly developed capacitor materials allows a co-firing with pure silver electrodes. The dielectric constant and the temperature stability of the dielectric constant are strongly correlated with the composition of the ZnO-B₂O₃-Li₂O additives. A high dielectric constant up to 3000 and a dielectric loss less than 0.024 were measured on multilayer capacitors sintered at 900 °C with silver inner electrodes.     

Preparation of AlON ceramics via reactive spark plasma sintering

Al₂O₃ and AlN powder mixtures were used to synthesise AlON ceramics using the reactive spark plasma sintering (SPS) method at temperatures between 1400 and 1650 °C for 15-45 min at 40 MPa under N₂ gas flow. AlON phase formation was initiated in the samples sintered above 1430 °C, according to the X-ray analysis. The complete transformation of the initial phases (Al₂O₃ and AlN) into AlON was observed in the samples that were spark plasma sintered at 1650 °C for 30 min at 40 MPa. A high spark plasma sintering temperature together with a low heating rate produced a greater amount of AlON formation at a constant process time. The densification, microstructure and mechanical properties of the produced ceramics were analysed. The highest hardness value was recorded to be 16.7 GPa, and the fracture toughness of the sample with the highest AlON ratio was measured to be 3.95 MPa m^1/2.     

Low-temperature preparation and microwave dielectric properties of ZBS glass–Al2O3 composites

The preparation and microwave dielectric properties of ZnAl₂O₄-based glass–ceramic composites were investigated. Using zinc borosilicate (ZBS) glass and Al₂O₃, glass–ZnAl₂O₄ composites with high quality factor was successfully prepared at temperatures below 950 °C. The linear shrinkage for 50 vol% ZBS glass–ZnAl₂O₄ composite showed a steep increase up to 650 °C and a plateau between 700 °C and 950 °C, implying that one-stage densification process occurred. The crystallization of ZnAl₂O₄ was observed above 700 °C and an insufficient densification occurred due to the consumption of the glass. As the sintering temperature increased, the quality factor (Q × f₀) showed an increase with an S-type curve whereas the dielectric constant was almost constant. The formation of ZnAl₂O₄ might correspond to the increase of Q × f₀; a high value of 17,757 GHz (1415 at 12.6 GHz) was obtained for the specimen sintered at 900 °C.     

Formation, densification, and selected mechanical properties of hot pressed Al4SiC4, Al4SiC4 with 30 vol.% WC, and Al4SiC4 with 30 vol.% TiC

Powders of Al₄C₃ and SiC were combined by high-energy milling to produce Al₄SiC₄, Al₄SiC₄ + 30 vol.% TiC, and Al₄SiC₄ + 30 vol.% WC. Five different temperatures were used to hot press the constituents. XRD, SEM, relative density, and hardness measurements showed that formation of single-phase Al₄SiC₄ occurred at 1450 °C and full densification (99%) was achieved at 1500 °C. Both of these temperatures are lower than previously reported. Adding TiC and WC increases hardness, while WC improves densification (99.5%).     

Low temperature sintering of CCTO using P2O5 as a sintering aid

Recent work on CCTO is directed towards decreasing its dissipation factor and further raising its dielectric constant by using different dopants. Also attempts have been made to lower its sintering temperature by adding different sintering aids so as to save energy and use low-cost electrodes (Ag–Pd or base metal) for making multilayer capacitors. Normally, CCTO needs a processing temperature of 1100 °C and above for densification. We report the formation of dense CCTO ceramics at a temperature as low as 1000 °C by adding P₂O₅ as a sintering aid. The samples showed dielectric constant value as high as 40,000, though the dissipation factor values remained high like those reported for pure CCTO.     

Sintering high purity,magnesia with additions of hafnium dioxide

Conclusions The introduction of hafnium dioxide into high-purity active magnesia accelerates its sintering and with 0.1–0.3 mol % HfO₂ a ceramic with an apparent density of 99–100% of the theoretical (3.56–3.63 g/cm³) can be obtained after firing at 1300–1400°C. The optimum quantity of HfO₂ additive is close to 0.25 mol %.The calcination temperature of the mixture of magnesium hydroxide and additive obtained by precipitation from a solution of MgCl₂ and Hf(SO₄)₂ with ammonia, and the fabrication pressure do not greatly affect the final density of the ceramics.Sintering of spectrally pure MgO containing 0.25 mol. % HfO₂ begins at 950°C, then the apparent density grows rapidly with rise in firing temperature, approaching 3.40 g/cm² at 1100°C. Selective recrystallization at these low temperatures is slow and sintering is not accompanied by a substantial grain growth. At 1300°C and higher firing temperatures densification of the ceramics approaches the limit in several minutes.The mechanism of the transfer of substance during the sintering of these specimens is volume self-diffusion from the grain boundaries to the surfaces of the bridges formed between them. The energy of activation of this process [3.9 eV (6.2 × 10^–16 J) in the 1000–1300°C range] and the coefficient of self-diffusion for MgO calculated in accordance with this (6 × 10^–14 cm²/sec at 1100°C) correspond to existing data on the diffusion of magnesium into MgO.With the incorporation of 0.25 mol. % HfO₂ in less pure magnesia obtained from chemically pure MgCl₂, sintering is little different from the sintering of spectrally pure MgO, but the limiting apparent density of the ceramics in this case is somewhat lower-of the order of 99% of the theoretical.     

The phase structure and electric properties of low-temperature sintered (K,Na)NbO3-based piezoceramics modified by CuO

0.25 wt% CuO-doped (Li,K,Na)(Nb,Ta)O₃–AgSbO₃ lead-free piezoceramics with pure perovskite structure were successfully prepared at a sintering temperature below 1000 °C. The sintering temperature of KNN-based piezoceramics was effectively reduced by about 100 °C due to the enhanced densification process induced by the addition of CuO. Besides, the acceptable sintering temperature window was broadened by the addition of CuO. It is found that the CuO-doped samples show slightly higher tetragonal–orthorhombic phase transition point (T_T−O) but a lower Curie point (T_c), compared to undoped ones. The KNN-based piezoceramics became “hard” as CuO was added, supported by an increase of Q_m. Fairly good electrical properties of d₃₃^*=383 pm/V, ε_r=860, Q_m=188 and T_c=215 °C could be obtained in dense CuO-modified KNN-based piezoceramics sintered at 970 °C, demonstrating promising potential in practical applications.     

Densification and microstructure evolution of Cr,Nd:YAG transparent ceramics for self-Q-switched laser

Transparent 0.1 at.% Cr, 1.0 at.% Nd:YAG ceramics were fabricated by solid-state reaction and vacuum sintering using commercial Y₂O₃, α-Al₂O₃, Cr₂O₃ and Nd₂O₃ as raw materials. CaO and tetraethoxysilane (TEOS) were used as charge compensator and sintering aid, respectively. The powders were mixed in ethanol and doped with TEOS, dried and pressed. Pressed samples were sintered from 1450 to 1800 °C for 10 h. The relative density increased from 68.8% to 99.4% at the sintering temperature from 1450 to 1700 °C. Grain size increased with increase of sintering temperature and obvious grain growth occurred between 1650 and1700 °C. For the Cr,Nd:YAG ceramics sintered at 1750 and 1800 °C for 10 h, nearly pore-free microstructures with average particle size of ∼10 μm were obtained. The optical transmittance of the 1800 °C sintered sample was ∼70% in the infrared wavelength.     

Effect of sintering temperature on the microstructure and mechanical properties of ZrO2-3 mol%Y2O3 sol–gel films

The microstructural evolution and mechanical properties of ZrO₂-3 mol%Y₂O₃ films were investigated as a function of the sintering temperature in the range from 100 °C to 1500 °C, using a battery of characterization techniques including X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and nanoindentation. It was found that the crystallization occurs at temperatures close to 300 °C. A gradual increase in the grain and crystallite sizes is observed as the sintering temperature increases up to 1000 °C, and above this sintering temperature the tendency changes abruptly with a rapid increase in these values. Although Young's modulus of the coatings did not change with sintering temperature, a slight decrease was observed in the hardness values above 1000 °C which is attributed to microstructure coarsening. Finally, a slight degradation of the films occurs above 1300 °C, which is due to the occurrence of a process of grain spheroidization.     

Ultraviolet irradiated ozone treatment of a metal catalyst for the large-scale synthesis of single-walled carbon nanotubes with small, uniform diameters

Large-scale synthesis of single-walled carbon nanotubes with small diameters and narrow distribution was performed using catalytic decomposition of C₂H₂ at 800 °C by introducing an ultraviolet irradiated ozone (UV-ozone) treatment on an as-prepared Fe-Mo/MgO catalyst (APC). The UV-ozone treatment effectively suppressed metal migration and the agglomeration of the Fe-Mo catalyst on the MgO support material at high temperature (800 °C). During UV-ozone treatment, active oxygen species were adsorbed onto the APC and generated hydroxyl groups. The hydroxyl groups prevented the formation of large catalytic metal nanoparticles at 800 °C by acting as a surfactant. We also investigated whether the Mo species prevented the metal sintering of iron species into the MgO lattice.     

Pressureless sintering of silicon carbide ceramics containing zirconium diboride

SiC-5 wt.% ZrB₂ composite ceramics with 10 wt.% Al₂O₃ and Y₂O₃ as sintering aids were prepared by presureless liquid-phase sintering at temperature ranging from 1850 to 1950 °C. The effect of sintering temperature on phase composition, sintering behavior, microstructure and mechanical properties of SiC/ZrB₂ ceramic was investigated. Main phases of SiC/ZrB₂ composite ceramics are all 6H-SiC, 4H-SiC, ZrB₂ and YAG. The grain size, densification and mechanical properties of the composite ceramic all increase with the increase of sintering temperatures. The values of flexural strength, hardness and fracture toughness were 565.70 MPa, 19.94 GPa and 6.68 MPa m^1/2 at 1950 °C, respectively. The addition of ZrB₂ proves to enhance the properties of SiC ceramic by crack deflection and bridging.     

Effect of Y2O3 additive on conventional and microwave sintering of mullite

Mullite has become a strong candidate material for advanced structural and functional ceramics. Much interest has recently focused on sintering aids for mullite. The aim of this study was to evaluate the effect of Y₂O₃ as a sintering aid in the conventional and microwave sintering of mullite. To accomplish this study, a highly pure industrial mullite was used. Mullite with and without Y₂O₃ was pressed under a cold isostatic pressure of 200 MPa. Samples were sintered conventionally at 1400, 1450, 1500, 1550 and 1600 °C for 2 h and microwave-sintered for up to 40 min using a large range of power. The microstructure and physical properties of the microwave-sintered samples were compared to those of the conventionally sintered samples. The results showed that Y₂O₃ improved the densification of mullite bodies in the conventional and microwave sintering processes, but high densifications were achieved in just a few minutes when Y₂O₃ was used with microwave processing.     

Effect of manganese oxide on the sintered properties and low temperature degradation of Y-TZP ceramics

The sinterability of yttria-tetragonal zirconia polycrystals (Y-TZP) containing small amounts of MnO₂ as sintering aid was investigated over the temperature range of 1250–1500 °C. Sintered samples were evaluated to determine bulk density, Young's modulus, Vickers hardness and fracture toughness. In addition, the tetragonal phase stability of selected samples was evaluated by subjecting the samples to hydrothermal ageing in superheated steam at 180 °C/10 bar for up to 24 h. The results showed that the addition of MnO₂, particularly ≥0.3 wt% was effective in aiding densification, improving the matrix stiffness and hardness when compared to the undoped Y-TZP sintered at temperatures below 1350 °C. On the other hand, the fracture toughness of Y-TZP was unaffected by MnO₂ addition except for the 1 wt% MnO₂-doped Y-TZP samples sintered above 1400 °C. The hydrothermal ageing resistance of Y-TZP was significantly improved with the additions of MnO₂ in the Y-TZP matrix.