Effect of CuO Addition on the Microstructure and Electric Properties of Low‐Temperature Sintered 0.25PMN–0.40PT–0.35PZ Ceramics

Low‐temperature sintering of 0.25PMN–0.40PT–0.35PZ ceramics was investigated using CuO as a sintering aid. Effect of CuO on the sinterability, microstructure, and electric properties of 0.25PMN–0.40PT–0.35PZ system was systematically studied. The CuO addition significantly reduced the sintering temperature of 0.25PMN–0.40PT–0.35PZ from 1260°C to 950°C. SEM results indicated that a dense microstructure without any second phase was obtained when the amount of CuO was 0.25 wt%, which gave rise to high values of d₃₃ = 532 pC/N and k_p = 58.4%. A large field‐induced longitudinal strain ~2.28% (at 30 kV/cm) can also be obtained for 0.25 wt% CuO‐added specimens, which shows a great promise for multilayer actuator applications.     

Low‐Temperature Sintering and Electric Properties of Pb0.99(Zr0.95Ti0.05)0.98Nb0.02O3 Ferroelectric Ceramics with CuO Additive

The low‐temperature sintering and electric properties of Pb_0.99(Zr_0.95Ti_0.05)_0.98Nb_0.02O₃ (PZTN 95/5) ferroelectric ceramics with CuO addition was investigated. The CuO addition significantly promoted the densification and reduced the sintering temperature of PZTN 95/5 ceramics by more than 200°C. The 0.2 wt% CuO‐added sample sintered at 1150°C exhibited the optimum relative density of 96.7% and excellent electric properties with values of P_r = 37.80 μC/cm², T_C = 223°C, ε_r = 329, and tan δ = 0.016, which were superior to that of PZTN 95/5 ceramics sintered at 1350°C.     

Low‐Temperature Sintering of Bi0.5(Na,K)0.5TiO3 for Multilayer Ceramic Actuators

We investigated the influence of CuO amount (0.5–3.0 mol%), sintering temperature (900°C–1000°C), and sintering time (2–6 h) on the low‐temperature sintering behavior of CuO‐added Bi_0.5(Na_0.78K_0.22)_0.5TiO₃ (BNKT22) ceramics. Normalized strain (S_max/E_max), piezoelectric coefficient (d₃₃), and remanent polarization (P_r) of 1.0 mol% CuO‐added BNKT22 ceramics sintered at 950°C for 4 h was 280 pm/V, 180 pC/N, and 28 μC/cm², respectively. These values are similar to those of pure BNKT22 ceramics sintered at 1150°C. In addition, we investigated the performance of multilayer ceramic actuators made from CuO‐added BNKT22 in acoustic sound speaker devices. A prototype sound speaker device showed similar output sound pressure levels as a Pb(Zr,Ti)O₃‐based device in the frequency range 0.66–20 kHz. This result highlights the feasibility of using low‐cost multilayer ceramic devices made of lead‐free BNKT‐based piezoelectric materials in sound speaker devices.     

Densification of copper oxide doped alumina toughened zirconia by conventional sintering

The effect of copper oxide doping (0.05–1 wt%) on the densification, microstructure evolution and mechanical characteristics of alumina toughened zirconia (ATZ: 80 wt% Y-TZP + 20 wt% Al₂O₃) ceramic composites was investigated. Green samples were pressureless sintered using a short hold time of 12 min at temperatures varying from 1250 °C to 1500 °C. The incorporation of up to 0.2 wt% copper oxide was beneficial in promoting densification at low sintering temperature and improving the mechanical properties of ATZ without affecting the tetragonal phase stability. It was found that 0.2 wt% copper oxide addition was most efficacious, and the samples could attain a relative density of approximately 92% at 1250 °C, approximately 97% dense at 1350 °C and above 99% dense at 1450–1500 °C. This approach was also accompanied by an improvement in the Vickers hardness (12.7 GPa) and fracture toughness (6.94 MPam^1/2) when consolidated at 1450 °C/12 min. In comparison, the undoped composite exhibited relative densities of approximately 80% at 1250 °C, 87% at 1350 °C and approximately 97%–98% at 1450 °C-1500 °C. However, the study also found that higher dopant levels (0.5 wt% and 1 wt%) was not beneficial because the tetragonal zirconia phase was disrupted upon cooling from sintering, resulting in the monoclinic phase formation. In addition, low densification and poor mechanical properties were obtained.     

Low‐Temperature Preparation of β‐Si3N4 Porous Ceramics with a Small Amount of Li2O–Y2O3

Porous β‐Si₃N₄ ceramics are sintered at 1600°C in N₂ and postheat treated at 1500°C under vacuum using Li₂O and Y₂O₃ as the sintering additives. The partial sintering and phase transformation are promoted at low temperature by the addition of Li₂O. The addition of Y₂O₃ is advantageous for the formation of high aspect ratio β‐Si₃N₄ grains. After postheat treatment, a large amount of intergranular glassy phase is removed, and the Li content in the samples is decreased. By this method, the β‐Si₃N₄ porous ceramic with a porosity of 54.1% and high flexural strength of 110 ± 8.1 MPa can be prepared with a small amount of sintering additives, 0.66 wt% Li₂O and 0.33 wt% Y₂O₃, and it is suitable for high‐temperature applications.     

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.     

Low-temperature sintering of coarse alumina powder compact with sufficient mechanical strength

Coarse alumina powder compacts doped with various amounts of titania and copper oxide were pressurelessly sintered from 900 °C to 1600 °C. Their phase assemblages and microstructural evolution, as well as their properties, were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), differential scanning calorimetry/thermogravimetric (DSC/TG) analysis, and three-point bending and wetting test. The role of TiO₂ and CuO during the sintering is discussed in detail. The experimental results show that the liquid phase from the copper oxide appeared at approximately 1200 °C, so the solid-state reaction between alumina and titania took place at a lower temperature. Such solid state-reaction sintering had a strong impact on the grain growth and greatly promoted the densification of the alumina compact. In addition, the liquid phase inhibited the abnormal grain growth and microcracking. As a result, the coarse alumina powder compacts doped with 5 wt% TiO₂–CuO were fully densified and exhibited sufficient flexural strength (342±21 MPa) when sintered at a temperature of 1450 °C for 2 h.     

CuO improved (Sn,Sb)O2 ceramic anodes for electrochemical advanced oxidation processes

Antimony-doped tin oxide electrodes with CuO as sintering aid are presented as an economical alternative to metal-based electrodes, intended for the electrooxidation process of emerging and recalcitrant organic contaminants in wastewaters. The CuO proportion has been optimized to obtain densified electrodes with a mild thermal cycle (T_max = 1200°C). One of the manufactured electrodes (97.8 mol.% of SnO₂, 1.0 mol.% of Sb₂O₃, and 1.2 mol.% of CuO) was selected for electrochemical characterization from a physical and morphological analysis. The electrochemical behavior of the selected electrode showed that the addition of CuO as sintering aid widens the electrochemical window and increases the electrode “inactivity”, with respect to an (Sn, Sb)O₂ electrode synthesized in the same conditions. In return, the (Sn,Sb,Cu)O₂ electrode presents a significantly lower electrochemical rugosity factor. Moreover, the addition of CuO does not change the oxygen evolution reaction mechanism, but it modifies the kinetic parameters, leading to a larger accumulation of hydroxyl radicals. Consequently, the addition of CuO as sintering aid significantly improves the electrochemical properties of the electrode as an electrochemical advanced oxidation process anode with respect to the (Sn,Sb)O₂ electrode, at the expense of worsening its electrochemical roughness factor. The results of the electrochemical characterization were confirmed by Norfloxacin degradation tests.     

Synthesis of galaxite by sintering at various temperatures and atmospheres

Galaxite has broad application prospects in the field of cement rotary kiln burning zones owing to its excellent properties (high melting point and corrosion resistance). In this study, MnO and α-Al₂O₃ powders were used as raw materials to synthesize galaxite in air, coke bed, or nitrogen at 1500–1600 °C. Their phase compositions and microstructure changes were investigated by XRD and SEM-EDS. The results show that Mn^II(Al, Mn^III)₂O₄ composite spinel were formed in the air at 1500–1600 °C and increased with increasing temperature, whereas only MnAl₂O₄ was formed in the coke bed and nitrogen at 1550 °C. Therefore, the specimens treated at 1600 °C in air exhibited a high density of 3.88 g/cm³, which was similar to those of the specimens sintered in the coke bed and nitrogen at 1550 °C, demonstrating good sintering properties. Furthermore, the number and size of pores gradually decreased, and the bulk density increased as the temperature increased from 1500 °C to 1600 °C in the air.     

Effectively controlling the crystal growth of Cr2O3 using SiO2 as the second phase

The inevitable crystal growth of Cr₂O₃ during sintering causes the generation of cracks, which degrades the high-temperature properties. To solve this, SiO₂ is adopted as the second phase and the specimens are sintered at 1200-1500°C under buried carbon condition. The results show that the addition of approximate 20 wt% SiO₂ can effectively control the crystal growth of Cr₂O₃. The Cr₂O₃ particle size can keep uniform ranging from 4 μm to 12 μm even when the temperature increases to 1500°C. The sintering of Cr₂O₃ mainly follows the defect model, which depends on the reaction temperatures and atmospheres. This work should also contribute to the sintering of other oxide refractories with controlled crystal size for practical application.     

Effect of carbon content on electrical,thermal, and mechanical properties of porous SiC ceramics with B4C and C additives

The electrical, thermal, and mechanical properties of porous SiC ceramics with B₄C-C additives were investigated as functions of C content and sintering temperature. The electrical resistivity of porous SiC ceramics decreased with increases in C content and sintering temperature. A minimal electrical resistivity of 4.6 × 10^?2 Ω·cm was obtained in porous SiC ceramics with 1 wt% B₄C and 10 wt% C. The thermal conductivity and flexural strength increased with increasing sintering temperature and showed maxima at 4 wt% C addition when sintered at 2000 °C and 2100 °C. The thermal conductivity and flexural strength of porous SiC ceramics can be tuned independently from the porosity by controlling C content and sintering temperature. Typical electrical resistivity, thermal conductivity, and flexural strength of porous SiC ceramics with 1 wt% B₄C-4 wt% C sintered at 2100 °C were 1.3 × 10^?1 Ω·cm, 76.0 W/(m·K), and 110.3 MPa, respectively.     

Preparation and mechanical performance of ductile Csf/Al2O3-BN composites,Part 1: Effects of fiber length and sintering temperature

Since its invention, alumina ceramics have been extensively investigated for potential various applications. However, their intrinsic brittle nature is still an insurmountable obstacle when they are applied as structural components. This paper provides a simple routs to prepare ductile alumina based composites with the addition of chopped carbon fiber (C_sf/Al₂O₃-BN). Effects of fiber length and sintering temperature on the microstructure, phase composition, mechanical properties together with fracture behavior were systematically investigated. The results showed that composites with mixed fiber lengths of 12 mm and 1 mm exhibited homogeneous microstructure and striking enhancement in mechanical performances compared with composites with other fiber length. With the increase in sintering temperature from 1500 °C to 1650 °C, interfacial bonding strength increased and interface state converted from mechanical interlocking at 1500 °C into chemical bonding at 1650 °C. Chemical reaction in the composites degraded carbon fiber properties, which resulted in the decrease in mechanical performance of the composites.     

Low‐Cost Silicon Nitride from β‐Silicon Nitride Powder and by Low‐Temperature Sintering

Aiming to manufacture low‐cost silicon nitride components, a low‐cost β powder was chosen as a raw powder and low‐temperature sintering at 1550–1600°C under atmospheric pressure nitrogen was carried out. The silicon nitride from β powder with 5 wt% Y₂O₃ and 5 wt% MgAl₂O₄ additives and sintered at 1600°C for 8 h was successfully densified, and it exhibited moderate strength and toughness of 553 MPa ± 22 and 3.5 MPa m^1/2, respectively. The results indicate that the low‐temperature sintering of the low‐cost β powder has a potential to reduce cost of components.     

Enhanced mechanical strength and bactericidal activity of macro-porous Al2O3 ceramics through the introduction of Cu for membrane support application

Enhancing the mechanical strength of macro-porous ceramics and simultaneously endowing them with bactericidal activity are considered to be beneficial for their application as membrane support materials for water and wastewater treatment. In this study, Cu-containing Al₂O₃ porous ceramics were prepared by powder mixing, cold pressing and subsequent sintering. The microstructures of as-fabricated ceramics consisted of large α-Al₂O₃ particles as matrix, as well as inter-particle NaAlSiO₄, CuAl₂O₄ and CuO phase. With increased sintering temperature from 1430 to 1560 °C, the proportion of band-shaped CuO phase, which exhibited stronger binding tendency with Al₂O₃ than NaAlSiO₄, gradually increased, while that of particle-shaped CuAl₂O₄ phase decreased. Increasing the Cu content from 2 to 8 wt% at a fixed sintering temperature of 1500 °C resulted in the presence of more band-shaped CuO phase in Al₂O₃ matrix which tightly bonded Al₂O₃ particles together. The increase of sintering temperature and Cu content could both lead to enhanced bending strength and reduced porosity, while the later factor showed stronger modulatory effects than the former one. Moreover, the bactericidal rates of Cu-containing Al₂O₃ porous ceramics towards Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus) were found to increase with increased Cu content in a Cu content-dependent manner. Together, the Cu-containing Al₂O₃ porous ceramic added with 8 wt% Cu and sintered at 1500 °C exhibited the highest bending strength and strongest bactericidal activity, which could be a promising candidate material for membrane support application.     

Fabrication and properties of macro-porous SiC using Al2O3–Y2O3–SiO2 as bonding additives

Macro-porous SiC was fabricated without using pore-forming agents by an in situ reaction bonding process. A bonding additive, Al₂O₃–Y₂O₃–SiO₂, with a low melting temperature was mixed with SiC particles and sintered at 1500 °C and 1600 °C for 1 h in Ar. Macro-porous SiC with a porosity of 32.7–45.9%, a pore size of 3.4–4.2 μm, and a relatively narrow and uniform pore size distribution was fabricated by varying the amount of bonding additive. The flexural strength of macro-porous SiC prepared at 1500 °C increased from 47.2 MPa to 71.2 MPa while the porosity decreased from 45.9% to 42.8%, respectively. When the sintering temperature of the macro-porous SiC was increased to 1600 °C, the flexural strengths were significantly reduced to 32.6–35.6 MPa, along with a reduction in porosity and pore size. The permeability of macro-porous SiC prepared at 1500 °C varied from 1.59 × 10^?12 m² to 1.26 × 10^?12 m², depending on the porosity. As the sintering temperature increased from 1500 °C to 1600 °C, the permeability decreased to less than 1.00 × 10^?12 m² because of the reduced porosity and average pore size. The electrical resistivity of macro-porous SiC prepared at 1500 °C and 1600 °C varied from 2.7 × 10⁸ Ω-cm to 1.4 × 10⁹ Ω-cm and from 1.3 × 10⁸ Ω-cm to 1.7 × 10⁹ Ω-cm, respectively, with increasing volume percent of bonding additives. The relatively high electrical resistivity was apparently due to neck bonding phase between SiC particles formed by phases consisting of Y₂Si₂O₇, YAG, and residual Al₂O₃.     

Sintering properties and homogeneity of Ca2+-doped .65Y2O3–.35YCr0.5Mn0.5O3 NTC ceramics

Ceramics suitable for use over a wide temperature and having a negative temperature coefficient (NTC) based on .65Y₂O₃–.35YCr_0.5Mn_0.5O₃-doped with CaO were prepared by applying a solid-state reaction at different temperatures (1500–1650°C). The physical properties and scanning electron microscopy results revealed that dense NTC ceramics could be obtained by sintering at >1550°C. The effect of two different sintering methods on the properties of the NTC ceramics was studied, and the results indicated that the NTC ceramics obtained by employing the two-step sintering method exhibited better properties. The contents of Cr and Mn oxides in the NTC ceramic discs prepared by applying two-step sintering (1600°C) exhibited a decreasing trend from inside to outside. To quantify the diffusion rate, Fick's second law was used, and the diffusion coefficients of Cr and Mn oxides in the NTC ceramics were found to be 5.20 × 10^–5 and 2.36 × 10^–5 cm²/s, respectively. Resistivity and temperature analyses indicated that the resistivity (ρ₂₅), B_25/100, and B_700/1000 of the NTC ceramics were 1.61 × 10⁶ Ω cm, 2367 K, and 2697 K, respectively, which are suitable for a wide temperature range.     

Effect of CeO2 addition on the sintering behavior of pre-synthesized magnesium aluminate spinel ceramic powders

In this work, the effects of 1?wt%, 2?wt%, and 3?wt% CeO₂ as an additive on the sintering behavior of alumina-rich spinel and magnesia-rich spinel powders subjected to sintering at temperatures of 1600?°C, 1650?°C, 1700?°C, and 1750?°C were investigated. The sintering behavior of the ceramics was investigated according to dilatometry measurements, linear shrinkage, bulk density, phase analysis, and microstructure. It was demonstrated that CeO₂ hindered the sintering process in alumina-rich spinel by reacting with Al₂O₃ exsolved from the spinel to form platelet-shaped particles of CeAl₁₁O₁₈ interspersed between the spinel grains. Meanwhile, the presence of CeO₂ promotes the sintering process in magnesia-rich spinel by being distributed in an isolated form among the spinel grains.     

Effect of zirconia content on mechanical and thermal properties of mullite–zirconia composite

Abstract

Mullite–zirconia composites were prepared by adding various zirconia contents in the mullite ranging from 0 to 30 wt-% and sintering at 1400–1600°C for 2 h. The phase composition examined by X-ray diffraction showed that mullite was the major phase combined with developed t-ZrO₂ and m-ZrO₂ phase as a function of zirconia content, especially at 1600°C, wherein m-ZrO₂ predominated. Density increased when the zirconia content and sintering temperature were increased ranging from 2·2 to 3·53 g cm^?3. The morphology of mullite grain showed elongated grains, whereas dispersed zirconia showed equiaxed and intergranular grains. Flexural strength was continuously improved by adding zirconia during the sintering temperature ranging from 1400 to 1500°C, whereas flexural strength was initially improved up to 5 wt-% of zirconia addition and deteriorated with more than 5 wt-% of zirconia content during sintering between 1550 and 1600°C. The maximum strength, 190 MPa, was obtained when sintering mullite with 30 wt-% of zirconia content at 1500°C. The degradation of strength at high sintering temperature may be a result from more occurrence of m-ZrO₂ phase. Thermal expansion of sintered specimens indicated linear change and hysteresis loop change. The hysteresis loop obtained with increased zirconia content resulted in the t–m phase transformation. Martensitic start temperature M_s was determined to be 530°C for 15 wt-% zirconia sintered at 1500°C, implying that the t–m phase transformation occurred.     

Sintering and microstructural study of mullite prepared from kaolinite and reactive alumina: Effect of MgO and TiO2

Mullite ceramic was prepared using kaolinite and synthesized alumina (combustion route) by solid-state interaction process. The influence of TiO₂ and MgO additives in phase formation, microstructural evolution, densification, and mechanical strengthening was evaluated in this work. TiO₂ and MgO were used as sintering additives. According to the stoichiometric composition of mullite (3Al₂O₃·2SiO₂), the raw materials, ie kaolinite, synthesized alumina, and different wt% of additives were wet mixed, dried, and uniaxially pressed followed by sintering at different temperature. 1600°C sintered samples from each batch exhibit enhanced properties. The 1 wt% TiO₂ addition shows bulk density up to 2.96 g/cm³ with a maximum strength of 156.3 MPa. The addition of MgO up to 1 wt% favored the growth of mullite by obtaining a density and strength matching with the batch containing 1 wt% TiO₂. These additives have shown a positive effect on mullite phase formation by reducing the temperature for complete mullitization by 100°C. Both additives promote sintering by liquid phase formation. However, the grain growth, compact microstructure, and larger elongated mullite crystals in MgO containing batch enhance its hardness properties.     

Investigation on properties of Al2O3–SiO2 complex shaped refractory fabricated by layered extrusion forming

As one of the 3D printing methods, layered extrusion forming (LEF) has distinct advantages to form complex configuration ceramics directly. The feasibility of using LEF to make refractory products with complex shapes was explored by this work, using water-based Al₂O₃–SiO₂ ceramic slurry and specially equipped device. By measuring rheological parameters, the effects of binder addition, dispersant addition and volume proportion of the solid portion composed of α-Al₂O₃ ultrafine powder (92 wt%) and silica fume (8 wt%) on rheological behavior of the slurry were investigated. The green body specimens prepared by the LEF were fired at 1400°C–1600 °C for 3h. The influence of firing temperature on phase composition, microstructure, sintering degree and comprehensive properties of the specimens was investigated. At 2.5 wt% addition of aluminum dihydrogen phosphate as binder, 0.2 wt% addition of sodium hexametaphosphate as dispersant and with solid portion between 56 vol% and 58 vol%, required pseudoplastic behavior of the slurry can be achieved, suitable for the LEF. With the increase of heating temperature, mullitization by the reaction between the α-Al₂O₃ ultrafine powder and silica fume becomes stronger and sintering gets enhanced, leading to improved comprehensive properties of the specimens. Fired at 1600 °C, properties in terms of bulk density 3.03g/cm³, cold compressive strength 190.5 MPa and refractoriness under load 1598 °C are achieved. Crucible slag test shows a good resistance to the glass melt corrosion. Good feasibility of fabricating some complex shaped refractory products by LEF as a novel forming approach has been confirmed by the present work.