Low-temperature densification sintering and properties of CaAl2Si2O8 ceramics with MeO·2B2O3 (Me=Ca,Sr, Ba)

Dense CaAl2Si2O8 ceramics were prepared via a two-step sintering process at temperatures below 1000°C. First, pre-sintered CaAl2Si2O8 powders containing small amounts of other crystal phases were obtained by sintering a mixture of calcium hydroxide and kaolin powders at 950°C for 6 h. Subsequently, the combination of the pre-sintered ceramic powders with MeO·2B2O3 (Me=Ca, Sr, Ba) flux agents enabled the low-temperature densification sintering of the CaAl2Si2O8 ceramics at 950°C. The sintering behavior and phase formation of the CaAl2Si2O8 ceramics were investigated in terms of the addition of the three MeO·2B2O3 flux agents. Furthermore, alumina and quartz were introduced into the three flux agents to investigate the sintering behaviors, phase evolvements, microstructures, and physical properties of the resulting CaAl2Si2O8 ceramics. The results showed that, because of their low-melting characteristics, the MeO·2B2O3 (Me=Ca, Sr, Ba) flux agents facilitated the formation of the CaAl2Si2O8 ceramics with a dense microstructure via liquid-phase sintering. The addition of alu-mina and quartz to the flux agents also strongly affected the microstructures, phase formation, and physical properties of the CaAl2Si2O8 ce-ramics.     

单斜相SrAl2Si2O8陶瓷的烧结及其对Sr的固化

Monoclinic SrAl₂Si₂O₈ ceramics for Sr immobilization were prepared by a liquid-phase sintering method. The sintering temperature, mineral phase composition, microstructure, flexural strength, bulk density, and Sr ion leaching characteristics of the SrAl₂Si₂O₈ ceramics were investigated. A crystalline monoclinic SrAl₂Si₂O₈ phase formed through liquid-phase sintering at 1223 K. The introduction of four flux agents (B₂O₃, CaO·2B₂O₃, SrO·2B₂O₃, and BaO·2B₂O₃) to the SrAl₂Si₂O₈ ceramics not only reduced the densification temperature and decreased the volatilization of Sr during high-temperature sintering but also impacted the mechanical properties of the ceramics. Product consistency tests showed that the leaching concentration of Sr ions in the sample with flux agent B₂O₃ was the lowest, whereas that of Sr ions in the sample with flux agent BaO·2B₂O₃ was the highest. These results show that the leaching concentration of Sr ions depends largely on the amorphous phase in the ceramics. Meanwhile, the formation of mineral analog ceramics containing Sr is an important factor to improve Sr immobilization.     

Bioactivity analysis of the Ta(Ⅴ) doped SiO_2–Ca O–Na_2O–P_2O_5 ceramics prepared by solid state sintering method

The main objective of the study was to control the degradation rate of material at a higher degradation rate improving the chemical stability of the material. Ta is known to have good chemical resistance, biocompatibility and show no adverse biological response. In the present study, Si O_2–Na_2O–Ca O–P_2O_5 bioceramics with different Ta_2O_5 contents was prepared by solid state sintering method at 1000 °C. The as-sintered ceramics were subjected to immersion studies in stimulated body fluid(SBF) for 21 days under static condition and characterized by XRD, FTIR, SEM, and AAS. The findings of the research indicate that the addition of Ta_2O_5 controlled degradability, and all samples showed sufficient bioactivity.     

Novel approaches to produce Al2O3– TiC/TiCN– Fecomposite powders directly from ilmenite

Al2O3 –TiC/TiCN–Fe composite powders were successfully prepared directly from ilmenite at 1300–1400℃.The effects of Al/C ratio,sintering atmosphere,and reaction temperature and time on the reaction products were investigated.Results showed that the nitrogen atmosphere was bene cial to the reduction of ilmenite and the formation of Al2O3 –TiC/TiCN–Fe composite powders.When the reaction temperature was between 600 and 1100℃,the intermediate products,TiO2,Ti3O5 and Ti4O7 were found,which changed to TiC or TiCN at higher temperature.Al/C ratio was found to affect the reaction process and synthesis products.When Al addition was 0.5 mol,the Al2O3 phase did not appear.The content of carbon in TiCN rose when the reaction temperature was increased.     

Effects of AlN on the densification and mechanical properties of pressureless-sintered SiC ceramics

In the present work, Si C ceramics was fabricated with Al N using B_4 C and C as sintering aids by a solid-state pressureless-sintered method. The effects of Al N contents on the densification, mechanical properties, phase compositions, and microstructure evolutions of as-obtained Si C ceramics were thoroughly investigated. Al N was found to promote further densification of the Si C ceramics due to its evaporation over 1800 °C,transportation, and solidification in the pores resulted from Si C grain coarsening. The highest relative density of 99.65% was achieved for Si C sample with 15.0 wt% Al N by the pressureless-sintered method at 2130 °C for 1 h in Ar atmosphere. Furthermore, the fracture mechanism for Si C ceramics containing Al N tended to transfer from single transgranular fracture mode to both transgranular fracture and intergranular fracture modes when the sample with 30.0 wt% Al N sintered at 1900 °C for 1 h in Ar. Also, Si C ceramics with 30.0 wt% Al N exhibited the highest fracture toughness of 5.23 MPa m~(1/2) when sintered at 1900 °C.     

Effects of Yb^3＋ codoping on visible and near infrared emissions of Er^3＋-Yb^3＋ codoped Al2O3 powders by the sol-gel method

The 0.1 mol% Er^3＋ and 0-2 mol% Yb^3＋ codoped Al2O3 powders were prepared by the sol-gel method, and the phase structure, including only two crystalline types of doped Al2O3 phase, γ-（Al,Er, Yb）2O3 and θ-（Al,Er, Yb）2O3, was detected at the sintering temperature of 1000℃. The visible and near infrared emissions properties depended strongly on the Yb^3＋ codoping, and the corresponding maximal peak intensities centered at about 523, 545, 660 and 1533 nm were obtained respectively for the 0.1 mol% Er^3＋ and 0.5 mol% Yb^3＋ codoped Al2O3 powders, which were composed of θ-（Al,Er,Yb）2O3 and a small amount of γ-（Al,Er, Yb）2O3 phases. The two-photon absorption process was responsible for the visible up-conversion emissions, and the one-photon absorption process was involved in the near infrared emissions of the Er^3＋-yb^3＋ codoped Al2O3 powders.     

Manufacture of biomorphic Al2O3 ceramics using filter paper as template

Biomorphic Al2O3 ceramics were prepared through the surface sol-gel process with filter papers as bio-templates. The filter papers were infiltrated with γ-AlOOH sol and subsequently sintered in air at high temperatures to produce the biomorphic Al2O3 ceramics. The results show that the final materials have a hierarchical structure originated from the morphology of cellulose paper. The sintering temperatures exhibit a strong effect on the surface pore-size distribution of obtained Al2O3 ceramics. Differential scanning calorimeter, scanning electron microscopy, X-ray diffraction and BET analysis were employed to characterize the microstructure, morphology and phase compositions of the final products.     

The development of Bi Fe O3-based ceramics

The multiferroic properties of Bi Fe O3-based ceramics were improved through optimizing their sintering method and doping with certain rare earth elements in pure Bi Fe O3. Some methods, especially liquid-phase sintering method has largely decreased the densities of oxygen vacancies and Fe2in Bi Fe O3-based ceramics, and thus their resistivity became high enough to measure the saturated polarization and the large piezoelectric d33 coefficient under the high electric field of [150 k V/cm. Besides,multiferroic properties were improved through the rare earth elements’ doping in pure Bi Fe O3. Magnetization commonly increases with the proportional increase of Nd,La, Sm and Dy contents up to ＊30 %, while ferroelectric phase can transform to paraelectric phase at a certain proportion. An improved magnetoelectric coupling was often observed at ferroelectric phase with a relatively large proportion. Besides, an enhanced piezoelectric coefficient is expected in Bi Fe O3-based ceramics with morphotropic phase boundaries as they are already observed in thin epitaxial Bi Fe O3 films.     

Mineral-phase evolution and sintering behavior of MO–SiO_2–Al_2O_3–B_2O_3 (M = Ca,Ba) glass-ceramics by low-temperature liquid-phase sintering

In this work, network former SiO_2 and network intermediate Al_2O_3 were introduced into typical low-melting binary compositions CaO·B_2O_3, CaO·2B_2O_3, and BaO·B_2O_3 via an aqueous solid-state suspension milling route. Accordingly, multiple-phase aluminosilicate glass-ceramics were directly obtained via liquid-phase sintering at temperatures below 950°C. On the basis of liquid-phase sintering theory, mineral-phase evolutions and glass-phase formations were systematically investigated in a wide MO–SiO_2–Al_2O_3–B_2O_3(M = Ca, Ba) composition range. The results indicate that major mineral phases of the aluminosilicate glass-ceramics are Al_(20)B_4O_(36), CaAl_2Si_2O_8, and BaAl_2Si_2O_8 and that the glass-ceramic materials are characterized by dense microstructures and excellent dielectric properties.     

Effect of B2O3 on the aqueous tape casting and microwave properties of Li2O–Nb2O5–TiO2 ceramics

The effect of B2O3 addition on the aqueous tape casting, sintering, microstructure and microwave dielectric properties of Li2O-Nb2O5-TiO2 ceramics has been investigated. The tape casting slurries exhibit a typical shear-thinning behavior without thixotropy, but the addition of B2O3 increases the viscosity of the slurries significantly. It was found that doping of B2O3 can decrease the tensile strength, strain to failure and density of the green tapes. The sintering temperature could be lowed down to 900℃ with the addition of 2 wt% B2O3 due to the liquid phase effect. No secondary phase is observed. The addition of B2O3 does not induce much degradation on the microwave dielectric properties. Optimum microwave dielectric properties of εr 67, Q×f 6560 GHz are obtained for Li2O-Nb2O5-TiO2 ceramics containing 2 wt% B2O3 sintered at 900 1C. It represents that the ceramics could be promising for multilayer low-temperature co-fired ceramics (LTCC) application.     

Near-infrared to visible up-conversion emissions of Er^3＋ doped Al2O3 powders derived from the sol-gel method

The Er3 doped Al2O3 powders were prepared by the sol-gel method using the aluminium isopropoxide [Al(OC3H7)3]-derived Al2O3 sols with addition of the erbium nitrate [Er(NO3)3.5H2O]. The different phase structure, including three crystalline types of (Al,Er)2O3 phases, γ, θ, α, and two Er-Al-O phases, ErAlO3 and Al10Er6O24, was obtained with the 1 mol% Er3 doped Al2O3 powders at the different sintering temperatures of 600―1200℃. The green and red up-conversion emissions centered at about 523, 545 and 660 nm, corresponding respectively to the 2H11/2, 4S3/2→4I15/2 and 4F9/2→4I15/2 transitions of Er3 , were detected by a 978 nm semiconductor laser diodes excitation. The phase structure and OH content had evident influence on the up-conversion emissions intensity. The maximum intensities of both the green and red emissions were obtained respectively for the Er3 doped Al2O3 powders sintered at 1200 ℃, which was composed mainly of α-(Al,Er)2O3, less of ErAlO3 and Al10Er6O24 phases, and with the least OH content. The two-photon absorption up-conversion process was involved in the green and red up-conversion emissions of the Er3 doped Al2O3 powders.     

Effect of SiO2 addition on the dielectric properties and microstructure of BaTiO3-based ceramics in reducing sintering

The effect of SiO₂ doping on the sintering behavior, microstructure, and dielectric properties of BaTiO₃-based ceramics has been investigated. Silica was added to the BaTiO₃-based powder prepared by the solid state method with 0.075mol%, 0.15mol%, and 0.3mol%, respectively. The SiO₂-doped BaTiO₃-based ceramic with high density and uniform grain size were obtained, which were sintered in reducing atmosphere. A scanning electron microscope, X-ray diffraction, and LCR meter were used to determine the microstructure as well as the dielectric properties. SiO₂ can form a liquid phase belonging to the ternary system of BaO-TiO₂-SiO₂, leading to the formation of BaTiO₃ ceramics with high density at a lower sintering temperature. The SiO₂-doped BaTiO₃-based ceramics can be sintered to a theoretical density higher than 95% at 1220℃ with a soaking time of 2 h. The dielectric constants of the sample with 0.15mol% SiO₂ addition sintered at 1220℃ is about 9000. Doping with a small amount of silica can improve the sintering and dielectric properties of BaTiO₃-based ceramics.     

Effects of Yb～(3 ) codoping on visible and near infrared emissions of Er～(3 )-Yb～(3 ) codoped Al_2O_3 powders by the sol-gel method

The 0.1 mol% Er3 and 0―2 mol% Yb3 codoped Al2O3 powders were prepared by the sol-gel method,and the phase structure,including only two crystalline types of doped Al2O3 phase,γ-(Al,Er,Yb)2O3 and θ-(Al,Er,Yb)2O3,was detected at the sintering temperature of 1000℃. The visible and near infrared emissions properties depended strongly on the Yb3 codoping,and the corresponding maximal peak intensities centered at about 523,545,660 and 1533 nm were obtained respectively for the 0.1 mol% Er3 and 0.5 mol% Yb3 codoped Al2O3 powders,which were composed of θ-(Al,Er,Yb)2O3 and a small amount of γ-(Al,Er,Yb)2O3 phases. The two-photon absorption process was responsible for the visible up-conversion emissions,and the one-photon absorption process was involved in the near infrared emissions of the Er3 -Yb3 codoped Al2O3 powders.     

Phase modification and dielectric properties of a cullet-paper ash-kaolin clay-based ceramic

Novel ceramics from waste material made of (x) paper ash-(80-x) cullet-20 kaolin clay (10wt% ≤ x ≤ 30wt%) were successfully synthesized using a conventional solid-state reaction technique. Energy-dispersive X-ray analysis confirmed the presence of Si, Ca, Al, and Fe in the waste material for preparing these ceramics. The influence of the cullet content on the phase structures and the dielectric properties of these ceramics were systematically investigated. The impedance spectra were verified in the range from 1 Hz to 10 MHz at room temperature. The phase of the ceramics was found to primarily consist of wollastonite (CaSiO₃), along with minor phases of γ-dicalcium silicate (Ca₂SiO₄) and quartz (SiO₂). The sample with a cullet content of 55wt% possessed the optimum wollastonite structure and exhibited good dielectric properties. An increase of the cullet content beyond 55wt% resulted in a structural change from wollastonite to dicalcium silicate, a decrease in dielectric constant, and an increase in dielectric loss. All experimental results suggested that these novel ceramics from waste are applicable for electronic devices.>     

Effects of chelating agents on the sol-gel synthesis of nano-zirconia:Comparison of the Pechini and sugar-based methods

This study focused on the comparison of the Pechini and sugar-based combustion synthesis methods to produce nano-zirconia. Zirconium hydroxide was utilized as metal precursor and citric acid, sucrose, and fructose were used as chelating agents, followed by calcination at 500, 600, and 700°C in air, respectively. Characterization was conducted by thermal analysis, specific surface area measurement, Fourier transform infrared spectroscopy, X-ray diffraction, and scanning and transmission electron microscopy. When sucrose and citric acid were used as chelating agents during synthesis, mixtures of monoclinic and tetragonal phases were formed after calcination at 600 and 700°C. In the fructose samples, the tetragonal structure was the unique characterized phase. The tetragonal parameters in the fructose samples were determined using the diffraction data and the lattice parameter ratio was proven to increase with the temperature increase. Compared with the citrate and sucrose samples, the largest specific surface area(27 m2·g-1) and smallest particle size(39.1 nm) were obtained for the fructose sample after calcination at 700°C. The study revealed the formation of single-phase stabilized tetragonal zirconia using fructose as chelating agent after calcination at 500°C, and the presence and formation mechanism of stabilized tetragonal phase were also discussed on the basis of the X-ray and electron diffraction studies.     

Effect of Sintering on Grain Boundary Microstructure and Electrical Properties of CaCu_3Ti_4O_(12) Ceramics

CaCu3Ti4O12 ceramic with a giant dielectric constant was synthesized by sol-gel method and sintered in three different sintering conditions: 1 035 ℃ for 48 h, 1 080 ℃ for 3 h and 48 h. The phase of the ceramics, the element distribution, the valance state of Ti ions at grain boundaries, and the electrical properties were characterized via X-ray diffraction(XRD), energy dispersive X-ray analysis(EDAX), X-ray photoelectron spectroscopy(XPS), electrical conduction and dielectric measurement. The results demonstrate that the grain-boundary microstructure and the electrical properties are influenced by sintering conditions: 1 By raising sintering temperature, the Cu-rich and Ti-poor grain boundary was formed and grain resistivity was decreased. 2 By prolonging sintering time, the content of Ti3+ near the grain boundary increased, leading to the decrease of the grain-boundary resistivity and the increase of the activation energy at grain boundary. The ceramic, sintering at 1 080 ℃ for 48 h, exhibited a small grain resistivity(60.5 *cm), a large grain-boundary activation energy(0.42 e V), and a significantly enhanced dielectric constant(close to 1×105 at a low frequency of 1×103 Hz). The results of electrical properties accord with the internal boundary layer capacitor model for explaining the giant dielectric constant observed in Ca Cu3Ti4O12 ceramics.     

A TEM study on the microstructure of spark plasma sintered ZrB_2-based composite with nano-sized SiC dopant

Sintering behavior of ZrB_2 ceramic with nano-sized SiC dopant was studied. ZrB_2-25 vol% nano-sized SiC was selected as the starting mixture to fabricate the composite. The manufacturing process was accomplished at 1800℃ for 5 min under 25 MPa via spark plasma sintering(SPS). The as-sintered sample reached a relative density of 99%. Besides the initial phases, namely ZrB_2 and SiC, the high-resolution X-ray diffraction(HRXRD) was used to study the formation of an in-situ ZrC phase. The possible chemical interactions during the ZrC phase formation were scrutinized. The microstructure of the composite was studied by the field emission scanning electron microscopy(FESEM) and transmission electron microscopy(TEM). Elemental analysis through FESEM evaluations revealed the formation of amorphous phases, rich in Zr, C, Si, B, and O elements, which was in harmony with the thermodynamical assessments. TEM studies endorsed the formation of such phases, containing a glassy bed of Si–B–O with ZrC and C islands dispersed therein.     

Densification behavior of mechanically milled Cu–8 at% Cr alloy and its mechanical and electrical properties

Synthesis and consolidation behavior of Cu–8 at%Cr alloy powders made by mechanical alloying with elemental Cu and Cr powders,and subsequently,compressive and electrical properties of the consolidated alloys were studied.Solid solubility of Cr in Cu during milling,and subsequent phase transformations during sintering and heat treatment of sintered components were analyzed using X-ray diffraction,scanning electron microscopy and transmission electron microscopy.The milled powders were compacted applying three different pressures(200 MPa,400 MPa and 600 MPa)and sintered in H2atmosphere at 900 1C for 30 min and at 1000 1C for 1 h and 2 h.The maximum densification(92.8%)was achieved for the sample compacted at 600 MPa and sintered for 1000 1C for 2 h.Hardness and densification behavior further increased for the compacts sintered at 900 1C for 30 min after rolling and annealing process.TEM investigation of the sintered compacts revealed the bimodal distribution of Cu grains with nano-sized Cr and Cr2O3precipitation along the grain boundary as well as in grain interior.Pinning of grain boundaries by the precipitates stabilized the fine grain structure in bimodal distribution.     

Synthesis and characterization of Cr2AlC with nanolaminated particles

In this work, we reported the large-scale and low cost synthesis of high purity Cr2 AlC powders with nanolaminated particles by pressureless sintering. The chemical reactions involved in synthesizing Cr2 AlC had been studied and discussed. The results showed that the Al contents in the starting materials and sintering temperatures had significant effects on the synthesis and purity of Cr2 AlC. The obtained high purity Cr2 AlC powders were stable up to at least 1400 °C. The Cr2 AlC powders consisted of nanolaminated particles, the size of which was tunable by adjusting sintering time. The present synthesized nanolaminated Cr2 AlC powders would be an excellent reinforcement material for metal matrix composites.     

Preparation of Ln3-xEuxS4 （Ln=Ce,Pr, and Nd） ceramics by pressureless sintering

The preparation of ternary rare earth sulfides of Ln3-xEuxS4 （Ln = Ce, Pr, and Nd） ceramics was investigated, and the effect of Eu substitution on Ln3-xEuxS4 ceramics was also studied. Ln3-xEuxS4 powders were synthesized by the sulfurization of their oxide powders using carbon disulfide gas. Ln3-xEuxS4 ceramics were sintered by pressure-less sintering method. All pressureless sintered Ln3-xEuxS4 ceramics crystallized in y-phase. It was found that Eu substitution could improve the density of Ln3-xEuxS4 ceramics. Furthermore, Eu substitution might narrow the optical band gaps of Ln3-xEuxS4 ceramics.