In situ TEM observation of crack propagation in LiTaO3 particle toughened Al2O3 ceramics

Direct observation of crack propagation in LiTaO₃/Al₂O₃ composite ceramics was carried out using in situ transmission electron microscopy (TEM). Domain switching induced by crack propagation, crack deflection and branching at domain boundaries and ripples similar to the contrasts of 180° domains at the microcrack tip inside LiTaO₃ grains were detected evidently. Domain switching, crack deflection, branching and energy dissipation resulting from the formation of contrasts similar to the 180° domains at the microcrack tip, were proposed as the toughening mechanisms in LiTaO₃/Al₂O₃ ceramics.     

Preparation and thermophysical properties of LaMgAl11O19–Yb3Al5O12 ceramic composites

LaMgAl₁₁O₁₉–Yb₃Al₅O₁₂ ceramic composites were prepared by pressureless sintering process at 1700 °C for 10 h in air. The microstructure and thermophysical properties of the composites were characterized by X-ray diffraction, scanning electron microscopy, high-temperature dilatometer and laser flash diffusivity measurements. LaMgAl₁₁O₁₉–Yb₃Al₅O₁₂ ceramic composites are composed of magnetoplumbite and garnet structures. LaMgAl₁₁O₁₉–Yb₃Al₅O₁₂ ceramic composites exhibit typical linear increase in thermal expansion with the increase of temperature. The measured thermal diffusivity gradually decreases with increasing temperature. Thermal conductivity of LaMgAl₁₁O₁₉–Yb₃Al₅O₁₂ ceramic composites is in the range of 2.6–3.9 W·m⁻¹·K⁻¹ from room temperature to 1200 °C.     

Dielectric properties and microstructures of CaSiO3 ceramics with B2O3 addition

The effects of B₂O₃ additives on the sintering behavior, microstructure and dielectric properties of CaSiO₃ ceramics have been investigated. The B₂O₃ addition resulted in the emergence of CaO–B₂O₃–SiO₂ glass phase, which was advantageous to lower the synthesis temperature of CaSiO₃ crystal phase, and could effectively lower the densification temperature of CaSiO₃ ceramic to as low as 1100 °C. The 6 wt% B₂O₃-doped CaSiO₃ ceramic sintered at 1100 °C possessed good dielectric properties: _r = 6.84 and tan δ = 6.9 × 10⁻⁴ (1 MHz).     

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.     

Preparation of ZrO2/Gd2O3 composite ceramic materials by coprecipitation method

High burnup is a goal for further development of advanced nuclear power in the future. However, along with the increase of burnup, it becomes more diffidult to control reactor reactivity, which affects the operation safety of the nuclear reactor. Al₂O₃/B₄C burnable poison materials widely used in pressurized water reactor currently will not meet the requirements of burnable poison materials in high burnup nuclear power. Because of the better performance of ZrO₂/Gd₂O₃ burnable poison materials than that of Al₂O₃/B₄C, this paper studies the preparation of ZrO₂/Gd₂O₃ composite ceramic materials by the coprecipitation method. The experimental results show that at the sintering temperature of 1500–1650 °C, ZrO₂/Gd₂O₃ composite ceramic grains are small, compact and uniform with the generation of homogeneous solid solution. At 1600 °C, ZrO₂–10%Gd₂O₃ has the highest density and mechanical strength.     

Effect of CeO2 addition on densification and microstructure of Al2O3-YSZ composites

Alumina (Al₂O₃) and alumina-yttria stabilized zirconia (YSZ) composites containing 3 and 5 mass% ceria (CeO₂) were prepared by spark plasma sintering (SPS) at temperatures of 1350-1400 °C for 300 s under a pressure of 40 MPa. Densification, microstructure and mechanical properties of the Al₂O₃ based composites were investigated. Fully dense composites with a relative density of approximately 99% were obtained. The grain growth of alumina was inhibited significantly by the addition of 10 vol% zirconia, and formation of elongated CeAl₁₁O₁₈ grains was observed in the ceria containing composites sintered at 1400 °C. Al₂O₃-YSZ composites without CeO₂ had higher hardness than monolithic Al₂O₃ sintered body and the hardness of Al₂O₃-YSZ composites decreased from 20.3 GPa to 18.5 GPa when the content of ZrO₂ increased from 10 to 30 vol%. The fracture toughness of Al₂O₃ increased from 2.8 MPa m^1/2 to 5.6 MPa m^1/2 with the addition of 10 vol% YSZ, and further addition resulted in higher fracture toughness values. The highest value of fracture toughness, 6.2 MPa m^1/2, was achieved with the addition of 30 vol% YSZ.     

Influence of low concentration of SO2 for selective reduction of NO by C3H8 in lean-exhaust conditions on the activity of Ag/Al2O3 catalyst

The effect of SO₂ for the selective reduction of NO by C₃H₈ on Ag/Al₂O₃ was investigated in the presence of excess oxygen and water vapor. The NO_x conversion decreased permanently even in the presence of a low concentration of SO₂ (0.5–10 ppm) at <773 K. The increase in SO₂ concentration resulted in a large decrease in NO_x conversion at 773 K. However, when the reaction temperature was more than 823 K, the activity of Ag/Al₂O₃ remained constant even in the presence of 10 ppm of SO₂. The sulfate species formed on the used Ag/Al₂O₃ were characterized by a temperature programmed desorption method. The sulfated species formed on silver should mainly decrease the deNO_x activity on the Ag/Al₂O₃. The sulfated Ag/Al₂O₃ was appreciably regenerated by thermal treatment in the deNO_x feed at 873 K. The moderate activity remains at 773 K in the presence of 1 ppm SO₂ for long time by the heat treatment at every 20 h intervals.     

Study on the formation process of Al2O3-TiO2 composite powders

Fine particles of anatase were suspended in solutions of ammonium alum with Al₂O₃/TiO₂ molar ratios from 0.1:1 to 7:1. By spray drying the suspensions and calcining the spray-dried powders, Al₂O₃-TiO₂ composite particles were obtained. The results show that after the spray drying, coatings of ammomium alum are formed on the surface of the anatase particles, leading to composite precursor powders (CCPs) with larger particle sizes. Upon calcining the CCPs, ammomium alum pyrolyzes to amorphous Al₂O₃ and anatase transforms into rutile. Both are mainly responsible for the observed particle size reductions as well as the densification of each composite particle. The in-situ formed α-Al₂O₃ and rutile may have higher reactivities, forming aluminum titanate at 1150 °C, about 130 °C lower than the theoretical temperature for the formation of Al₂TiO₅ by solid reaction. The reaction between α-Al₂O₃ and rutile starts from the interface between the anatase and the alum coating and mainly takes place in the single particles formed by spray drying. The molar ratio of Al₂O₃ to TiO₂ influences the final crystalline phases in the composite powders, but not stoichiometrically.     

Processing and physical properties of Al2O3/aluminum alloy composites

Porous aluminum oxide (Al₂O₃) preforms were formed by sintering in air at 1200 °C for 2 h. A356, 6061, and 1050 aluminum alloys were infiltrated into the preforms by squeeze casting in order to fabricate Al₂O₃/A356, Al₂O₃/6061, and Al₂O₃/1050 composites, respectively, with different volumes of aluminum alloy content. The content of aluminum alloy in the composites was 10–40% by volume. The resistivity of Al₂O₃/A356, Al₂O₃/6061, and Al₂O₃/1050 composites decreased dramatically from 6.41 × 10¹² to 9.77 × 10⁻⁴, 7.28 × 10⁻⁴, and 6.24 × 10⁻⁴ Ω m, respectively, the four-points bending strength increased from 397 to 443, 435.1, 407.2 MPa, respectively, and the deviations were smaller than 2%. From SEM microstructural analysis and TEM bright field images, the pore volume fraction and the relative density of the composites were the most important factors that affected the physical and mechanical properties. The ceramic phase and alloy phase in Al₂O₃/aluminum alloy composites were found to be homogenized and uniformly distributed using electrical and mechanical properties analysis, microstructure analysis, and image analysis.     

Enhancement of oxygen storage capacity by reductive treatment of Al2O3 and CeO2–ZrO2 solid solution nanocomposite

Oxygen storage capacity (OSC) of CeO₂–ZrO₂ solid solution, Ce_xZr_(1−x)O₄, is one of the most contributing factors to control the performance of an automotive catalyst. To improve the OSC, heat treatments were employed on a nanoscaled composite of Al₂O₃ and CeZrO₄ (ACZ). Reductive treatments from 700 to 1000 °C significantly improved the complete oxygen storage capacity (OSC-c) of ACZ. In particular, the OSC-c measured at 300 °C reached the theoretical maximum with a sufficient specific surface area (SSA) (35 m²/g) after reductive treatment at 1000 °C. The introduced Al₂O₃ facilitated the regular rearrangement of Ce and Zr ions in CeZrO₄ as well as helped in maintaining the sufficient SSA. Reductive treatments also enhanced the oxygen release rate (OSC-r); however, the OSC-r variation against the evaluation temperature and the reduction temperature differed from that of OSC-c. OSC-r measured below 200 °C reached its maximum against the reduction temperature at 800 °C, while those evaluated at 300 °C increased with the reduction temperature in the same manner as OSC-c.     

Dielectric and piezoelectric properties of (Ba0.95Ca0.05)(Ti0.88Zr0.12)O3 ceramics sintered in a protective atmosphere

(Ba_0.95Ca_0.05)(Ti_0.88Zr_0.12)O₃ (BCTZ) ceramics have been produced in a protective atmosphere of industrial N₂ gas for potential piezoelectric applications. For comparison, the ceramics were also sintered at 1200–1400 °C in air. The results revealed that the reducing atmosphere of pO₂ = 5 × 10² Pa had no substantial effect on the phase structure or the microstructure of the BCTZ ceramics. The XRD patterns suggested a tetragonal to pseudocubic phase transition at sintering temperatures above 1300 °C in both atmospheres. The nitrogen-sintered BCTZ samples had higher dielectric constants _r but lower electromechanical coupling coefficients k_p than the air-sintered samples. The piezoelectric constant d₃₃ for the BCTZ ceramics was not significantly influenced by the reducing atmosphere of pO₂ = 5 × 10² Pa. The correlation of dielectric and piezoelectric properties of the BCTZ ceramics with the sintering temperature was explained based on a competing mechanism between phase structure and microstructure.     

Electrochemical performance of Li3V2(PO4)3/C cathode material using a novel carbon source

Polyethylene glycol (PEG, mean molecular weight of 10,000) has been used to prepare a Li₃V₂(PO₄)₃/C cathode material by a simple solid-state reaction. The Raman spectra shows that the coating carbon has a good structure with a low I_D/I_G ratio. The images of SEM and TEM show that the carbon is dispersed between the Li₃V₂(PO₄)₃ particles, which improves the electrical contact between the corresponding particles. The electronic conductivity of Li₃V₂(PO₄)₃/C composite is 7.0 × 10⁻¹ S/cm, increased by seven orders of magnitude compared with the pristine Li₃V₂(PO₄)₃ (2.3 × 10⁻⁸ S/cm). At a low discharge rate of 0.28C, the sample presents a high discharge capacity of 131.2 mAh/g, almost achieving the theoretical capacity (132 mAh/g) for the reversible cycling of two lithium. After 500 cycles, the discharge capacity is 123.9 mAh/g with only 5.6% fading of the initial specific capacity. The Li₃V₂(PO₄)₃/C material also exhibits an excellent rate capability with high discharge capacities of 115.2 mAh/g at 1C and 106.4 mAh/g at 5C.     

Comparison of dispersants performance on the suspension Lu2O3:Eu stability and high-density compacts on their basis

The conditions for obtaining a stable Lu₂O₃:Eu³⁺ suspension of spherical particles with a diameter of 100 nm using three dispersants possessing an electrosteric stabilizing effect (Dolapix CE 64, Darvan 821 A, Darvan C-N) have been studied. It has been shown that in colloidal processing of ceramics the packing density and microstructure of green bodies can be controlled by regulating the interactions between ceramic particles in the suspension. The influence of the molecular weight and concentration of the dispersant on the stability of Lu₂O₃:Eu³⁺ suspensions containing 5-10 vol.% of the solid loading has been considered. It has been determined that use of Dolapix CE 64 with a concentration of 1 mass.% in the alkaline pH range allows to obtain suspensions with high stability and low viscosity (∼1.7 сP). Such suspensions were used to produce compacts with a maximum relative density of ∼52% and uniform density distribution by the pressure slip casting method. The obtained compacts were densified into translucent Lu₂O₃:Eu³⁺ ceramics by the vacuum sintering method.     

Effects of CaSiO3 addition on sintering behavior and microwave dielectric properties of Al2O3 ceramics

The effects of CaSiO₃ addition on the sintering behavior and microwave dielectric properties of Al₂O₃ ceramics have been investigated. The addition of CaSiO₃ into Al₂O₃ ceramics resulted in the emergence of Ca₂Al₂SiO₇ and CaAl₂Si₂O₈, which acting as liquid sintering aids can effectively lower the sintering temperature of Al₂O₃ ceramic. The Q × f value of Al₂O₃-CaSiO₃ ceramics decreased with the CaSiO₃ addition increasing because of the lower Q × f value of Ca₂Al₂SiO₇ and CaAl₂Si₂O₈. Compared with the pure CaSiO₃ ceramic, the Al₂O₃-CaSiO₃ ceramic with 20 wt% CaSiO₃ addition possessed good dielectric properties of ?_r = 9.36 and Q × f = 13,678 GHz at the similar sintering temperature.     

Improvement of coke resistance of Ni/Al2O3 catalyst in CH4/CO2 reforming by ZrO2 addition

This work investigates the improvement of Ni/Al₂O₃ catalyst stability by ZrO₂ addition for H₂ gas production from CH₄/CO₂ reforming reactions. The initial effect of Ni addition was followed by the effect of increasing operating temperature to 500–700 °C as well as the effect of ZrO₂ loading and the promoted catalyst preparation methods by using a feed gas mixture at a CH₄:CO₂ ratio of 1:1.25. The experimental results showed that a high reaction temperature of 700 °C was favored by an endothermic dry reforming reaction. In this reaction the deactivation of Ni/Al₂O₃ was mainly due to coke deposition. This deactivation was evidently inhibited by ZrO₂, as it enhances dissociation of CO₂ forming oxygen intermediates near the contact between ZrO₂ and nickel where the deposited coke is gasified afterwards. The texture of the catalyst or BET surface area was affected by the catalyst preparation method. The change of the catalyst texture resulted from the formation of ZrO₂–Al₂O₃ composite and the plugging of Al₂O₃ pore by ZrO₂. The 15% Ni/10% ZrO₂/Al₂O₃ co-impregnated catalyst showed a higher BET surface area and catalytic activity than the sequentially impregnated catalyst whereas coke inhibition capability of the promoted catalysts prepared by either method was comparable. Further study on long-term catalyst stability should be made.     

Microstructure evolution of Al2O3/Al2O3 joint brazed with Ag-Cu-Ti + B + TiH2 composite filler

Al₂O₃/Al₂O₃ joint was achieved using Ag-Cu-Ti + B + TiH₂ composite fillers at 900 °C for 10 min. The evolution mechanism of interface during brazing was discussed. Effects of Ti and B atoms content on microstructure of joints were investigated. Results show that a continuous and compact reaction layer Ti₃(Cu,Al)₃O forms at Al₂O₃/brazing alloy interface. Ti(Cu,Al) precipitates near Ti₃(Cu,Al)₃O layer. In situ synthesized TiB whiskers evenly distribute in Ag and Cu based solid solution. The higher content of B powders in composite fillers increases TiB whiskers content, but decreases the thickness of Ti₃(Cu,Al)₃O layer, while the higher TiH₂ powders content thickens Ti₃(Cu,Al)₃O layer. Ag and Cu based solid solutions become uniform and fine with the increasing of TiB whiskers content. Ti(Cu,Al) intermetallics content increase and they gradually distribute from Al₂O₃ side to the central of brazing alloy, but the content of Cu based solid solution decreases when the TiH₂ content increases.     

Evaluation of sintering stresses of an Al2O3 powder with a self-loading apparatus

The sintering stress of an Al₂O₃ powder, σ_s, is evaluated from an equation σ_s = F_s/ρS_a, where F_s is the uniaxial tensile force necessary to just stop the sintering contraction, ρ is the relative density, and S_a is the cross-sectional area. During densification, σ_s increases to the maximum at a relative density of 85%, and then abruptly decreases. The variation of σ_s in the intermediate sintering stage suggests a simple cubic packing of particles. Densification in the final sintering stage is explained by shrinkage of the pores at the corners where four tetrakaidecahedra meet. The present surface tensions of the Al₂O₃ powder evaluated from the σ_s roughly equal a reported value.     

Rapid consolidation of nanocrystalline Al2O3 reinforced Ni–Fe composite from mechanically alloyed powders by high frequency induction heated sintering

Nano-powders of Ni–Fe and Al₂O₃ were made from NiO and FeAl powders by high-energy ball milling. Nanocrystalline 5Ni_0.6Fe_0.4–Al₂O₃ composite was consolidated by high frequency induction heated sintering (HFIHS) method within 2 min from mechanically alloyed powders of Al₂O₃ and Ni–Fe. The average grain size and mechanical properties of the composite were investigated.     

Mechanical and dielectric properties of short carbon fiber reinforced Al2O3 composites with MgO additive

A series of short-carbon-fiber/Al₂O₃ composites with MgO as sintering additive were fabricated by pressureless sintering process. The effects of short carbon fiber (C_sf) content on the mechanical, dielectric and microwave absorbing properties of the composite were investigated. The results show that the addition of MgO enhances the density, hardness and the flexural strength of the alumina ceramic. However, these mechanical properties of the C_sf/Al₂O₃–MgO composite decrease with increasing C_sf content. Both the real and imaginary parts of the complex permittivity increase with increasing C_sf content in the frequency range of 8.2–12.4 GHz, which is attributed to the increasing electron polarization and associated polarization relaxation, respectively. When the C_sf content is 0.3 wt%, the reflection loss less than −10 dB and the minimum value of −27 dB are obtained with the coating thickness being 1.4 mm. The results indicate that the C_sf/Al₂O₃ with MgO is an excellent candidate for microwave absorbing material with favorable mechanical property.