Comparison among different sintering routes for preparing alumina-YAG nanocomposites

Al₂O₃-YAG (50 vol.%) nanocomposite powders were prepared by wet-chemical synthesis and characterized by DTA-TG, XRD and TEM analyses. Amorphous powders were pre-heated at different temperatures (namely 600 °C, 800 °C, 900 °C and 1215 °C) and the influence of this thermal treatment on sintering behavior, final microstructure and density was investigated. The best performing sample was that pre-calcined at 900 °C, which yields dense bodies with a micronic/slightly sub-micronic microstructure after sintering at 1600 °C. A pre-treatment step to induce controlled crystallisation of the amorphous powder as well as a fast sintering procedure for green compacts, were also performed as a comparison.Finally, the previously stated thermal pre-treatment of the amorphous product was coupled to an extensive mechanical activation performed by wet planetary/ball milling. This procedure was highly effective in lowering the densification temperature, so that fully dense Al₂O₃-YAG composites, with a mean grain size smaller than 200 nm, were obtained by sintering in the temperature range 1370–1420 °C.     

Compositional inhomogeneity and segregation in (K0.5Na0.5)NbO3 ceramics

In this report, the effects of the calcination temperature of (K_0.5Na_0.5)NbO₃ (KNN) powder on the sintering and piezoelectric properties of KNN ceramics have been investigated. KNN powders are synthesized via the solid-state approach. Scanning electron microscopy and X-ray diffraction characterizations indicate that the incomplete reaction at 700 °C and 750 °C calcination results in the compositional inhomogeneity of the K-rich and Na-rich phases while the orthorhombic single phase is obtained after calcination at 900 °C. During the sintering, the presence of the liquid K-rich phase due to the lower melting point has a significant impact on the densification, the abnormal grain growth and the deteriorated piezoelectric properties. From the standpoint of piezoelectric properties, the optimal calcination temperature obtained for KNN ceramics calcined at this temperature is determined to be 800 °C, with piezoelectric constant d₃₃=128.3 pC/N, planar electromechanical coupling coefficient k_p=32.2%, mechanical quality factor Q_m=88, and dielectric loss tan δ=2.1%.     

Nano-sized BaSnO3 powder via a precursor route: Comparative study of sintering behaviour and mechanism of fine and coarse-grained powders

Preparation of a very fine BaSnO₃ powder by calcination of a barium tin 1,2-ethanediolato complex precursor and its sintering behaviour are described herein. A rate controlled calcination process to 820 °C leads to a nm-sized BaSnO₃ powder with a specific surface area of S = 15.1 m²/g (d_av. = 55 nm). The powder has a slightly larger cell parameter of a = 412.22(7) pm compared to the single crystal value, which decreases with increasing calcination temperature and reaches the reference value above 1000 °C. The sintering behaviour is compared between fine and coarse-grained BaSnO₃ powders. Corresponding powder compacts of the nano-sized BaSnO₃ achieve a relative density of 90% after sintering at 1600 °C for 1 h and at 1500 °C and a soaking time of 30 h, whereas coarse-grained powder compacts reach only 80% of the relative density at 1650 °C (10 h). Furthermore, the shrinkage mechanisms of fine and coarse-grained powder compacts have been investigated and are discussed.     

Electrochemical performance of La2NiO4+δ cathode for intermediate-temperature solid oxide fuel cells

The application of the La₂NiO_4+δ (LNO), one of the Ruddlesden–Popper series materials, as a cathode material for intermediate temperature solid oxide fuel cells is investigated in detail. LNO is synthesized via a complex method using ethylenediaminetetraacetic acid (EDTA) and citric acid. The effect of the calcination temperature of the LNO powder and the sintering temperature of the LNO cathode layer on the anode-supported cell, Ni–YSZ/YSZ/GDC/LNO, is characterized in view of the charge transfer resistance and the mass transfer resistance. Charge transfer resistance was not significantly affected by calcination and sintering temperature when the sintering temperature was not lower than the calcination temperature. Mass transfer resistance was primarily governed by the sintering temperature. The unit cell with the LNO cathode sintered at 1100 °C with 900 °C-calcined powder presented the lowest polarization resistance for all the measured temperatures and exhibited the highest fuel cell performances, with values of 1.25, 0.815, 0.485, and 0.263 W cm⁻² for temperatures of 800, 750, 700, and 650 °C, respectively.     

Effect of calcination temperature on the fabrication of transparent lutetium titanate by spark plasma sintering

Transparent lutetium titanate (Lu₂Ti₂O₇) bodies were fabricated by spark plasma sintering using Lu₂O₃ and TiO₂ powders calcined from 700 °C to 1200 °C. No solid-state reaction was identified after calcination at 700 °C, whereas single-phase Lu₂Ti₂O₇ powder was prepared at 1100 and 1200 °C. The calcination at 700 °C promoted densification at the early stages of sintering, whereas residual pores at grain boundaries resulted in Lu₂Ti₂O₇ bodies with low transparency. Low-density and opaque Lu₂Ti₂O₇ bodies formed owing to the coarsening of the powder calcined at 1200 °C. The Lu₂Ti₂O₇ body sintered using the powder calcined at the moderate temperature of 1100 °C had a density of 99.5% with the highest transmittances of 41% and 74% at wavelengths of 550 nm and 2000 nm, respectively.     

Dielectric properties of nano-sized Ba0.7Sr0.3TiO3 powders prepared by spray pyrolysis

Nano-sized Ba_0.7Sr_0.3TiO₃ powders are prepared by post-treatment of the precursor powders with hollow and thin wall structure at temperatures between 900 and 1100 °C. Ethylenediaminetetraacetic acid and citric acid improve the hollowness of the precursor powders prepared by spray pyrolysis. The mean sizes of the powders post-treated at temperatures of 900, 1000 and 1100 °C are 42, 51 and 66 nm, respectively. The densities of the Ba_0.7Sr_0.3TiO₃ pellets obtained from the powders post-treated at 900, 1000 and 1100 °C are each 5.36, 5.55 and 5.38 g cm^?3 at a sintering temperature of 1300 °C. The pellet obtained from the powders post-treated at 1000 °C has higher maximum dielectric constant than those obtained from the powders post-treated at 900 and 1100 °C.     

SrCo0.9Sc0.1O3−δ perovskite hollow fibre membranes for air separation at intermediate temperatures

SrCo_0.9Sc_0.1O₃ (SCSc) perovskite powders with sub-micron particle size were synthesized by a modified Pechini method combined with a post-treatment of sintering and ball-milling. From the prepared powders, the SCSc hollow fibre membranes with asymmetric structure and gas-tight property were fabricated by spinning a polymer solution containing 58.4 wt% SCSc followed by sintering at 1200 °C for 5 h. The oxygen permeation properties of the obtained SCSc fibres were measured under air/He gradients at 500–800 °C. This showed the oxygen flux of 1 mL cm^?2 min^?1 at 750 °C and 4.41 mL cm^?2 min^?1 at 900 °C. Modeling analysis reveals that the oxygen permeation process is predominated by oxygen surface exchange kinetics with an activation energy of 95.0 kJ mol^?1. The SCSc membranes showed excellent oxygen permeation performance while exhibiting high structural and permeating stability at intermediate temperatures (500–800 °C).     

Thermoelectric Ca0.9Yb0.1MnO3−δ grain growth controlled by spark plasma sintering

n-Type Ca_0.9Yb_0.1MnO_3?δ thermoelectric (TE) powders were prepared by solid state synthesis (SSS) and co-precipitation method (Cop). The bulk TE materials were consolidated using conventional sintering (CS) and spark plasma sintering (SPS) respectively. The shrinkage behavior, as well as the sample densification strongly depends on the starting particle size. Consequently, the bulk samples from normal powder (SSS) and nano-powder (Cop) were prepared with similar density by using different sintering temperatures, of 1400 °C and 1200 °C, then 1200 and 950 °C for CS and SPS respectively. Such a decrease (up to 200 °C) of the sintering temperature is a consequent progress in terms of engineering for applications. Another advantage of the co-precipitation process compared to the conventional solid state synthesis is that, due to the small particle sizes and the decreased sintering temperature, grain growth was limited and TE properties were enhanced. The interest of the SPS process was also evidenced and we are presenting here the structural and microstructural investigations. In addition, the thermoelectric properties of samples prepared with two different processes were studied with the figure of merit of 0.18 at 750 °C.     

Facile synthesis of LaAlO3 and Eu(II)-doped LaAlO3 powders by a solid-state reaction

Lanthanum aluminate (LaAlO₃) powder was prepared by a solid-state reaction between lanthanum(III) carbonate fluoride (LaFCO₃) and alumina (Al₂O₃) powders at elevated temperatures, and characterized by powder X-ray diffraction (XRD), ²⁷Al magic-angle spinning nuclear magnetic resonance spectroscopy, and scanning electron microscopy. The formation temperature (1000 °C) of LaAlO₃ was much lower than that in other solid-state reactions. The Eu(II)-doped LaAlO₃ powder was prepared by calcination of a mixture of Eu(III)-doped LaFCO₃ and Al₂O₃ in a nitrogen atmosphere and characterized by powder XRD, and photoluminescence and X-ray photoelectron spectroscopy. The intensity of blue emission due to Eu(II) ions in the LaAlO₃ powder increased with increasing calcination temperature up to 1200 °C but decreased with further increases in temperature. The origin of the Eu(II) ions was explained by the thermal decomposition of EuF₃.     

Thermal behavior of the nonstoichiometric lithium niobate powders synthesized via a combustion method

Lithium niobate (Li_xNb_1?xO_3+δ) powders with various compositions are prepared via combustion synthesis. The thermal properties, crystal structure, and surface morphology of the as-prepared lithium niobate powders are characterized by thermogravimetric and differential thermal analyses (TG/DTA), powder X-ray diffraction (XRD), and scanning electron microscopy (SEM). When the calcination temperature reached 900 °C, the secondary phases Li₃NbO₄ and LiNb₃O₈ were observed. The lithium concentration before 900 °C was 40–43%. The lattice parameters increased slightly with decreasing concentration of lithium ions. When the calcination temperature was higher than 900 °C, the major Li_0.91NbO₃ phase and the minor LiNbO₃ phase coexisted in the nonstoichiometric lithium niobate with 43% lithium content.     

Fabrication of Lu2O3:Eu transparent ceramics using powder consisting of mono-dispersed spheres

Mono-dispersed spherical Lu₂O₃:Eu (5 mol%) powders for transparent ceramics fabrication were synthesized by urea-based homogeneous precipitation technique. The effects of the doped-Eu³⁺ on the synthesis of Lu₂O₃:Eu particles were investigated in detail. The results show that the doping of Eu³⁺ ions into Lu system can significantly decrease the particle size of the resultant precursor spheres. Owing to the sequential precipitation in Lu/Eu system, there are compositional gradients within each of the resultant precursor spheres. Well dispersed, homogeneous and spherical/near spherical Lu₂O₃:Eu powders were obtained after calcination at 600–1000 °C for 4 h. The powder calcined at 600 °C shows better sintering behavior and can be densified into transparent ceramic after vacuum sintering at 1700 °C for 5 h. The luminescence properties of the obtained Lu₂O₃:Eu powder and transparent ceramic were also studied.     

Synthesis and characterization of nanometric gadolinia powders by room temperature solid-state displacement reaction and low temperature calcination

Nanometric-sized gadolinia (Gd₂O₃) powders were obtained by applying solid-state displacement reaction at room temperature and low temperature calcination. The XRD analysis revealed that the room temperature product was gadolinium hydroxide, Gd(OH)₃. In order to induce crystallization of Gd₂O₃, the subsequent calcination at 600 ∼ 1200 °C of the room temperature reaction products was studied. Calculation of average crystallite size (D) as well as separation of the effect of crystallite size and strain of nanocrystals was performed on the basic of Williamson-Hall plots. The morphologies of powders calcined at different temperatures were followed by scanning electron microscopy. The pure cubic Gd₂O₃ phase was made at 600 °C which converted to monoclinic Gd₂O₃ phase between 1400° and 1600 °C. High-density (96% of theoretical density) ceramic pellet free of any additives was obtained after pressureless sintering at 1600 °C for 4 h in air, using calcined powder at 600 °C.     

PVA assisted coprecipitation synthesis and characterization of MgFe2O4 nanoparticles

Single phase magnesium ferrite (MgFe₂O₄) nanoparticles were prepared by the coprecipitation method followed by calcination at 700 °C for 1 h. The effects of polyvinyl alcohol (PVA) agent on the structural, microstructure, magnetic properties and AC magnetically induced heating characteristics of MgFe₂O₄ nanoparticles were investigated. The structure and cation distributions investigated by X-ray diffraction method showed single phase MgFe₂O₄ powders had partially inverse spinel structure in which the inversion coefficient increased by adding more PVA. The small particle size and narrow size distribution of the coprecipitated MgFe₂O₄ powders characterized by scanning electron microscopy were achieved using PVA agent. Magnetic properties of MgFe₂O₄ nanoparticles studied by vibrating sample magnetometry showed ferrimagnetic characteristics with the highest saturation magnetization and coercivity of 24.6 emu/g and 17 Oe, respectively. The coprecipitated MgFe₂O₄ nanoparticles assisted by PVA exhibited the lower AC heating temperature of 5.6 °C and specific loss power of 2.4 W/g in comparison with 6.1 °C and 2.7 W/g for the powders coprecipitated without using PVA.     

Far infrared and microstructural studies of mechanically activated nickel manganite

Nickel manganite powder synthesized by calcination of a stoichiometric mixture of manganese (MnO Aldrich 99.9%) and nickel oxide (NiO Merck, 99.5%) containing 0.5 wt% CoO and Fe₂O₃, was additionally mechanically activated in a high energy planetary ball mill for 5–60 min. The resulting powders were uniaxially pressed into disc shape pellets and then sintered for 60 min at 900 °C, 1050 °C and 1200 °C. Morphological changes of the obtained nickel manganite ceramics induced by mechanical activation were monitored using scanning electron microscopy, while changes in structural characteristics were followed using X-ray powder diffraction. Room temperature far infrared reflectivity spectra for all sintered samples were recorded in the frequency range between 50 cm^?1and 1200 cm^?1. The observed spectra for all samples showed the presence of the same oscillators, but their intensities depended on the sintering temperature and the time of mechanical acivation. Transversal and longitudinal optical modes were calculated for six ionic oscillators (four strong, and two shoulders) belonging to the nickel manganite partially inverse spinel structure.     

Preparation and characterization of LnMgAl11O19 (Ln=La,Nd, Gd) ceramic powders

Lanthanide hexaaluminate powders of LaMgAl₁₁O₁₉ (LMA), NdMgAl₁₁O₁₉ (NMA) and GdMgAl₁₁O₁₉ (GMA) were synthesized via the solid state reaction or sol–gel and calcination method. The LMA and NMA powders synthesized by the sol–gel and calcination method at 1600 °C for 8 h exhibit a single hexaaluminate phase with magnetoplumbite structure; however, the GMA powder synthesized by the sol–gel and calcination method at 1600 °C for 8 h contains both a hexaaluminate phase and a small amount of second phase GdAlO₃ with a perovskite structure. The powders synthesized by the solid state reaction method at 1500 °C for 4 h have a small particle size of 1–3 μm, and a large specific surface area and a good uniformity. The powders synthesized by the sol–gel and calcination method at 1600 °C for 8 h have a particle size of 5–20 μm, and exhibit to a certain extent agglomeration.     

Influence of heat treatment of powder mixture on the microstructure and optical transmission of Nd:YAG transparent ceramics

Transparent Nd:YAG ceramics were fabricated by solid-state reactive sintering of Y₂O₃, α-Al₂O₃ and Nd₂O₃ powders with TEOS and MgO as sintering aids. The powders were ball-milled, dried, sieved and calcined at different temperatures. Samples sintered at 1745 °C for 10 h were utilized to observe the microstructure and the optical transmission. It is found that heat treatments of the powder mixtures above 600 °C for 1 h are necessary to remove the carbon contamination but below 800 °C for 4 h can avoid strong aggregation of the powder. So there is a room for heat-treatment, between 600 °C and 800 °C that can obtain Nd:YAG ceramics with almost pore-free microstructures and high transparency. Highly transparent Nd:YAG ceramic with 84.3% in-line transmission at 1064 nm was fabricated by sintering the 800 °C-1 h-heat-treated powder mixture at 1745 °C for 50 h. Even at wavelength of 400 nm, the transmittance of the sample reached 82.9% and the optical scattering coefficient was as low as 0.71% cm⁻¹.     

Copper-doped BaZrO3 crucibles for YBCO single crystal growth

The corrosion resistance of BaZrO₃ to molten barium cuprates is controlled by secondary phases, and requires high chemical and phase purity, as well as high density for sustained flux containment. The high sintering temperatures required for solid-state derived powders is a significant obstacle inhibiting more widespread use of high density BaZrO₃. We have investigated the use of Cu²⁺ doping to enable practical sintering temperatures whilst still producing corrosion resistant ceramics. Low levels of copper addition (0.2 wt.% CuO equiv.) produced densities of >97% theoretical using sintering temperatures as low as 1400 °C, as long as the dopant was added after all powder calcination steps, i.e. immediately before forming/sintering. Corrosion resistance at 0.2 wt.% CuO equiv. was equal to un-doped materials fabricated using the same powder processing method.     

Crystallization behavior and sintering of cordierite synthesized by an aqueous sol–gel route

The purpose of the research was to investigate crystallization behavior and sintering of cordierite synthesized by a low-price aqueous sol–gel route starting from silicic acid and magnesium and aluminum salts. Viscous sintering of the gel occurred in the temperature range of 800–850 °C, followed by μ-cordierite crystallization at about 900 °C, which proves the homogeneity of the gel. Decreasing of μ-cordierite crystallinity in a wide temperature range prior to commencing of α-cordierite crystallization at about 1200 °C indicates reconstructive type of μ- → α-cordierite transformation. The transformation was fully completed at 1350 °C. The value of the Avrami parameter indicates that μ-cordierite crystallization was controlled by surface or interface nucleation, which implies that viscous sintering occurred in the primary gel particles, which leads to shrinkage, and thereafter nucleation occurred on the surface or interface of the particles. The overall activation energy of μ-cordierite crystallization was 382.0 kJ/mol. The sinterability of the powder obtained by calcination at 1300 °C, where well-crystallized α-cordierite was formed, was better than that of the powder obtained by calcination at 850 °C, where the most intensive shrinkage occurred before the onset of crystallization of μ-cordierite.     

Highly transparent AlON ceramics sintered from powder synthesized by carbothermal reduction nitridation

Aluminum oxynitride (AlON) powders were synthesized by the carbothermal reduction and nitridation process using commercial γ-Al₂O₃ and carbon black powders as starting materials. And AlON transparent ceramics were fabricated by pressureless sintering under nitrogen atmosphere. The effects of ball milling time on morphology and particle size distribution of the AlON powders, as well as the microstructure and optical property of AlON transparent ceramics were investigated. It is found that single-phase AlON powder was obtained by calcining the γ-Al₂O₃/C mixture at 1550 °C for 1 h and a following heat treatment at 1750 °C for 2 h. The AlON powder ball milled for 24 h showed smaller particles and narrower particle size distribution compared with the 12 h one, which was benefit for the improvement of optical property of AlON transparent ceramics. With the sintering aids of 0.25 wt% MgO and 0.04 wt% Y₂O₃, highly transparent AlON ceramics with in-line transmittance above 80% from visible to infrared range were obtained through pressureless sintering at 1850 °C for 6 h.     

Poly(N-isopropylacrylamide) assisted microwave synthesis of magnesium aluminate spinel oxide for production of highly transparent films by hot compression

Magnesium aluminate spinel oxides have been prepared via poly(N-isopropylacrylamide) assisted microwave technique. The prepared MgAl₂O₄ powders showed a crystalline cubic structure with spinel phase after calcination at 600 °C only. The poly(N-isopropylacrylamide) amount showed a high effect on the crystallite size and the densification behavior of MgAl₂O₄. The increase of the amount of poly(N-isopropylacrylamide) reduced the sintering temperature of MgAl₂O₄ from 1400 °C to 1050 °C. The hot-pressed of MgAl₂O₄ powders in the presence of 3 wt% of poly(N-isopropylacrylamide) exhibited a full density at sintering temperature 1100 °C in 15 min only. The sintered films showed high transparency (81 ± 2%) in the wavelength range 500–1000 nm.