Stoichiometric Pb(Mg1/3Nb2/3)O3 perovskite ceramics produced by reaction-sintering process

Stoichiometric lead magnesium niobate, Pb(Mg_1/3Nb_2/3)O₃ (PMN), perovskite ceramics produced by reaction-sintering process were investigated. Without calcination, a mixture of PbO, Nb₂O₅, and Mg(NO₃)₂ was pressed and sintered directly. Stoichiometric PMN ceramics of 100% perovskite phase were obtained for 1, 2, and 4 h sintering at 1250 and 1270 °C. PMN ceramics with density 8.09 g/cm³ (99.5% of theoretical density 8.13 g/cm³) and K_max 19,900 under 1 kHz were obtained.     

Preparation of polycrystalline BaTi2O5 by pressureless sintering

Polycrystalline BaTi₂O₅ (BT₂) was prepared by pressureless sintering in air using BaCO₃ and TiO₂ as starting materials. XRD results of the calcined powder showed BaCO₃ and TiO₂ reacted completely after being calcined above 950 °C, showing a mixture of BaTiO₃ (BT), BT₂, BaTi₄O₉ and Ba₄Ti₁₃O₃₀. A small amount of ZrO₂ (less than 0.1 wt%) was effective to prepare BT₂ in a single phase and the second phase of BT and B₆T₁₇ increased with ZrO₂ content. BT₂ sintered body in a single phase was obtained at 1175-1300 °C when ZrO₂ content was 0.08 wt%. The maximum permittivity of BT₂ sintered body was 340 at the Curie temperature (T_c) of 463 °C and the frequency of 100 kHz.     

Ferroelectric and piezoelectric properties of tungsten substituted SrBi2Ta2O9 ferroelectric ceramics

Tungsten substituted samples of compositions SrBi₂(W_xTa_1−x)₂O₉ (x = 0.0, 0.025, 0.050, 0.075, 0.10 and 0.20) were synthesized by solid-state reaction method and studied for their microstructural, electrical conductivity, ferroelectric and piezoelectric properties. The X-ray diffractograms confirm the formation of single phase layered perovskite structure in the samples with x up to 0.05. The temperature dependence of dc conductivity vis-à-vis tungsten content shows a decrease in conductivity, which is attributed to the suppression of oxygen vacancies. The ferroelectric and piezoelectric studies of the W-substituted SBT ceramics show that the remanent polarization and d₃₃ values increases with increasing concentration of tungsten up to x ≤ 0.05. Such compositions with low conductivity and high P_r values should be excellent materials for highly stable ferroelectric memory devices.     

(5 − x)BaO-xMgO-2Nb2O5 ceramics prepared using a reaction-sintering process

(5 − x)BaO-xMgO-2Nb₂O₅ (x = 0.5 and 1; 5MBN and 10MBN) microwave ceramics prepared using a reaction-sintering process were investigated. Without any calcinations involved, the mixture of BaCO₃, MgO, and Nb₂O₅ was pressed and sintered directly. MBN ceramics were produced after 2-6 h of sintering at 1350-1500 °C. The formation of (BaMg)₅Nb₄O₁₅ was a major phase in producing 5MBN ceramics, and the formation of Ba(Mg_1/3Nb_2/3)O₃ was a major phase in producing 10MBN ceramics. As CuO (1 wt%) was added, the sintering temperature dropped by more than 150 °C. We produced 5MBN ceramics with these dielectric properties: ?_r = 36.69, Qf = 20,097 GHz, and τ_f = 61.1 ppm/°C, and 10MBN ceramics with these dielectric properties: ?_r = 39.2, Qf = 43,878 GHz, and τ_f = 37.6 ppm/°C. The reaction-sintering process is a simple and effective method for producing (5 − x)BaO-xMgO-2Nb₂O₅ ceramics for applications in microwave dielectric resonators.     

Photocatalytic properties of TiO2-P2O5 glass ceramics

Binary TiO₂-P₂O₅ glasses with 69 mol% and 76 mol% TiO₂ were prepared and converted into glass ceramics by heat-treatments. XRD measurements show that the main crystalline phases precipitated in the glass ceramics are anatase-type TiO₂ crystals or (TiO)₂P₂O₇ crystals, depending on the concentration of titanium constituent. Photocatalytic activities of the glass ceramics were evaluated by the decomposition of methylene blue (MB) and measuring the water contact angle. It is found that the glass ceramics containing anatase crystals exhibit both photocatalytic oxidation activity and highly photo-induced hydrophilicity under UV irradiation with intensity of 1.0 mW/cm².     

Low-temperature performance of Al4B2O9 nanowires

In this paper we report on the synthetic investigation of single-crystalline aluminum borate (Al₄B₂O₉) nanowires in large scale by a direct calcination of a precursor powder made of Na₂B₄O₇·10H₂O and Al (NO₃)₃·9H₂O at a low temperature of 850 °C. The nanowires, with the diameter of 20-40 nm and the length up to several micrometers, possess smooth surfaces and uniform sizes along the entire wire. The growth mechanism of the nanowires is attributed to a solid-liquid-solid process, which controls the nanowire morphology.     

Thermal shock resistance of the porous Al2O3/ZrO2 ceramics prepared by gelcasting

Porous Al₂O₃/ZrO₂ ceramics with porosity varying from 6% to 50% were fabricated by gelcasting using polystyrene (PS) as pore-forming agent. The effects of sintering temperature on porosity, strength as well as pore size were investigated. The flexural strength of these porous ceramics at room temperature significantly decreases as the porosity increases. Thermal shock resistance of these ceramics was improved by increasing the porosity. Both the critical difference temperature (ΔT_c) and residual strength of high porosity ceramics were higher than those of low porosity ceramics. These improvements can be attributed to the pores in the specimens which relax the thermal shock stress and arrest the propagation of microcracks effectively, which is confirmed by XRD analysis of specimens which encountered different thermal shock temperature difference.     

Synthesis and characterization of nanocrystalline MgAl2O4 spinel via sucrose process

Nanocrystalline MgAl₂O₄ spinel powder was synthesized using metal nitrates and a polymer matrix precursor composed of sucrose and polyvinyl alcohol (PVA). The precursor and the calcined powders were characterized by simultaneous thermal analysis (STA), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). According to XRD results, the inceptive formation temperature of spinel via this technique was between 600 and 700 °C. The calcined powder at 800 °C for 2 h has faced shaped morphology and its crystallite size is in the range of 8-12 nm. Further studies also showed that the amount of polymeric matrix to metal ions has significant influence on the crystallite size of synthesized magnesium aluminate spinel powder.     

Synthesis and characterization of nanosized SrBi2Ta2O9 powder by a novel sol-gel process

Chemically homogeneous SrBi₂Ta₂O₉ (SBT) sol was synthesized using ethoxy tantalum, strontium acetate, and bismuth subnitrate as starting materials, methoxyethylene as a solvent and acetic acid (HOAc) as a catalyst. Single-phased perovskite phase SBT ferroelectric ultrafine powder was obtained after the dried gel was treated at 350°C for 30 min and calcined at 800°C for 1 h. FT-IR, XRD, TEM and TG-DTA were employed to investigate the transformation processes of sol to gel and gel to ultrafine SBT powder. Acetic acid not only acts as an acid catalyst, but also changes the alkoxide precursor as a ligand at a molecular level. Bidentate acetates replace OR groups and are directly bounded to the tantalum, leading to the formation of Ta (OR)_x(OAc)_5−x. The perovskite SBT phase formed via intermediate phase Bi₃TaO₇ and a Bi-deficient pyrocholore phase.     

Structural and impedance properties of KBa2V5O15 ceramics

The polycrystalline sample of KBa₂V₅O₁₅ ceramics was prepared by a mixed oxide method at low temperature (i.e., at 560 °C). The formation of the compound was confirmed using an X-ray diffraction technique at room temperature. Scanning electron micrograph of the material showed uniform grain distribution on the surface of the sample. Detailed studies of dielectric properties of the compound as a function of temperature at different frequencies suggest that the compound has a dielectric anomaly of ferroelectric to paraelectric type at 323 °C, and exhibits diffuse phase transition. Electrical properties of the material were analyzed using a complex impedance technique. The Nyquists plot showed the presence of both grain (>10³ Hz) and the grain boundary (<10³ Hz) effects in the material. Studies of electrical conductivity over a wide temperature range suggest that the compound exhibits the negative temperature coefficient of resistance behavior. The ac conductivity spectrum was found to obey Jonscher's universal power law.     

Electronic characterization of alkali ruthenium hollandites: KRu4O8, RbRu4O8 and Cs0.8Li0.2Ru4O8

Transport, specific heat, and magnetic measurements have been performed on three alkali hollandites: KRu₄O₈, RbRu₄O₈, and a newly synthesized Cs analog, Cs_0.8Li_0.2Ru₄O₈, which was determined to have space group I4/m (#87) and lattice parameters, a = 10.0850(4) and c = 3.12180(20). In contrast to the ruthenium perovskites, which display a wide range of electrical and magnetic behavior, the alkali hollandites are simple paramagnetic metals.     

Crystal structures of CdTi2O4(OH)2 and LaTiSbO6

The crystal structures of two PbSb₂O₆-type compounds containing titanium, CdTi₂O₄(OH)₂ and LaTiSbO₆ were refined by X-ray powder diffraction data. For both compounds structure refinements with the space group were successful and the R-factors were R_WP = 6.46% and R_P = 4.90% for CdTi₂O₄(OH)₂ and R_WP = 9.55% and R_P = 7.17% for LaTiSbO₆. These crystal structures were the same as that of the typical PbSb₂O₆-type compound in spite of the existence of protons in the interlayer or two different metal ions in the layer.     

Processing, dielectric properties and impedance characteristics of Na0.5Bi0.5Cu3Ti4O12 ceramics

Na_0.5Bi_0.5Cu₃Ti₄O₁₂ (NBCTO) ceramics were prepared by conventional solid-state reaction method. The phase structure, microstructure and dielectric properties of NBCTO ceramics sintered at various temperatures with different soaking time were investigated. Pure NBCTO phase could be obtained with increasing the temperature and prolonging the soaking time. High dielectric permittivity (13,495) and low dielectric loss (0.031) could be obtained when the ceramics were sintered at 1000 °C for 7.5 h. The ceramics sintered at 1000 °C for 7.5 h also showed good temperature stability (−4.00 to −0.69%) over a large temperature range from −50 to 150 °C. Complex impedances results revealed that the grain was semiconducting and the grain boundaries was insulating. The grain resistance (R_g) was 12.10 Ω cm and the grain boundary resistance (R_gb) was 2.009 × 10⁵ Ω cm when the ceramics were sintered at 1000 °C for 7.5 h.     

Preparation, structure and dielectric properties of Ba4LaMNb3O15 (M = Ti, Sn ) ceramics

Two new cation-deficient hexagonal perovskites Ba₄LaMNb₃O₁₅ (M = Ti, Sn) ceramics were prepared by high temperature solid-state reaction route. The phase and structure of the ceramics were characterized by X-ray diffraction, scanning electron microscopy (SEM). The microwave dielectric properties of the ceramics were studied using a network analyzer. The Ba₄LaTiNb₃O₁₅ has high dielectric constant of 52, high quality factors (Q) 3500 (at 4.472 GHz), and temperature variation of resonant frequency (τ_f) +93 ppm °C⁻¹ at room temperature; Ba₄LaSnNb₃O₁₅ has dielectric constant of 39 with high Q value of 2510 (at 5.924 GHz), and τ_f −29 ppm °C⁻¹.     

Microstructure and microwave dielectric characteristics of (1 − x)Ba(Zn1/3Ta2/3)O3-xBaTi4O9 ceramics

(1 − x)Ba(Zn_1/3Ta_2/3)O₃-xBaTi₄O₉ (0.1 ≤ x ≤ 0.85) composites are prepared by mixing 1150 °C-calcined BaTi₄O₉ with 1150 °C-calcined Ba(Zn_1/3Ta_2/3)O₃ powders. The crystal structure, microwave dielectric properties and sinterabilites of the (1 − x)Ba(Zn_1/3Ta_2/3)O₃-xBaTi₄O₉ ceramics have been investigated. X-ray diffraction patterns reveal that BaTi₄O₉, ordered and disordered Ba(Zn_1/3Ta_2/3)O₃ phases exist independently over the whole compositional range. The sintering temperatures of (1 − x)Ba(Zn_1/3Ta_2/3)O₃-xBaTi₄O₉ ceramics are about 1240 - 1320 °C and obviously lower than those of Ba(Zn_1/3Ta_2/3)O₃ ceramics. The dielectric constants (?_r) and the temperature coefficient of resonant frequency (τ_f) of (1 − x)Ba(Zn_1/3Ta_2/3)O₃-xBaTi₄O₉ ceramics increase with the increase of BaTi₄O₉ content. Nevertheless, the bulk densities and the quality values (Q × f) of (1 − x)Ba(Zn_1/3Ta_2/3)O₃-xBaTi₄O₉ ceramics increase with the increase of Ba(Zn_1/3Ta_2/3)O₃ content. The results are attributed to the higher density and quality value of Ba(Zn_1/3Ta_2/3)O₃ ceramics, the better grain growth, and the densification of sintered specimens added a small BaTi₄O₉ content. The (1 − x)Ba(Zn_1/3Ta_2/3)O₃-xBaTi₄O₉ ceramic with x = 0.1 sintered at 1320 °C exhibits a ?_r value of 31.5, a maximum Q × f value of 68500 GHz and a minimum τ_f value of 4.1 ppm/°C.     

Sintering and dielectric properties of 0.88Al2O3-0.12TiO2 microwave ceramics by glass addition

The microwave characteristics and the microstructures of 0.88Al₂O₃-0.12TiO₂ with various amounts of MgO-CaO-SiO₂-Al₂O₃ (MCAS) glass sintered at different temperatures have been investigated. The sintering temperature can be lowered to 1300 °C by the addition of MCAS glass. The densities, dielectric constants (ε_r) and quality values (Q×f) of the MCAS-added 0.88Al₂O₃-0.12TiO₂ ceramics decrease with the increase of MCAS glass content. The temperature coefficients of the resonant frequency (τ_f) are shifted to more negative values as the MCAS content or the sintering temperatures increase. The change of the crystalline phases of Al₂TiO₅ phase and rutile-TiO₂ phase has profound effects on the microwave dielectric properties of the MCAS-added Al₂O₃-TiO₂ ceramics. As sintered at 1250 °C, 0.88Al₂O₃-0.12TiO₂ ceramics with 2 wt.% MCAS glass addition exists a ε_r value of 8.63, a Q×f value of 9578 and a τ_f value of +5 ppm/°C.     

Synthesis and photoluminescence properties of SrLu2O4:Eu superfine phosphor

Superfine powder SrLu₂O₄:Eu³⁺ was synthesized with a precursor prepared by an EDTA - sol-gel method at relatively low temperature using metal nitrate and EDTA as starting materials. The heat decomposition mechanism of the precursor, formation process of SrLu₂O₄:Eu³⁺and the properties of the particles were investigated by thermo-gravimetric (TG) - differential thermal analysis (DTA), X-ray diffraction (XRD), transmission electron microscopy (TEM) and photoluminescence (PL) analyses. The results show that pure SrLu₂O₄:Eu³⁺ superfine powder has been produced after the precursor was calcinated at 900 °C for 2 h and has an elliptical shape and an average diameter of 80-100 nm. Upon excitation with 250 nm light, all the SrLu₂O₄:Eu³⁺ powders show red and orange emissions due to the 4f-4f transitions of Eu³⁺ ions. The highest photoluminescence intensity at 610 nm was found at a content of about 6 mol% Eu³⁺. Splitting of the ⁵D₀-⁷F₁ emission transition revealed that the Eu³⁺ ions occupied two nonequivalent sites in the crystallite by substituting Lu³⁺ ions.     

Preparation of polycrystalline BaTi2O5 ferroelectric ceramics

Polycrystalline BaTi₂O₅ (BT₂) was prepared by solid state sintering in air using BaCO₃ and TiO₂ as starting materials. A rod-like BT₂ sintered bodies in a single phase were obtained above 1025 °C by adding 5 wt.% B₂O₃. The densification of BT₂ sintered bodies decreased with increasing sintering temperature. The maximum permittivity of BT₂ sintered body was 640 at the Curie temperature (T_c) of 461 °C and the frequency of 100 kHz. The addition of B₂O₃ was effective to obtain BT₂ in a single phase at low temperatures with elongated microstructure and to improve the permittivity, indicating the formation of preferred orientation at low temperature was related with liquid-phase sintering mechanism.     

Preparation of LiMn2O4 thin films by aqueous solution deposition

Cathode material LiMn₂O₄ thin films were prepared by aqueous solution deposition using lithium acetate and manganese acetate as starting materials. The structures, morphologies, and the first discharge specific capacity of the thin films were investigated as a function of annealing temperature and time. The cycling properties of the thin films were also examined. The results show that LiMn₂O₄ thin films prepared by this method are homogenous and crack-free. The thin film annealed at 750°C for 30 min has good rechargeability. The capacity loss per cycle is about 0.05% after being cycled 100 times.     

Synthesis by an ionic liquid-assisted method and optical properties of nanoflower Y2O3

Flower-like Y₂O₃ nano-/microstructured phosphors without metal activators have successfully been fabricated by an ionic liquid (IL)-assisted method involving temperature (600 °C) annealing. In this paper, the effect of IL concentration on the morphology of the product has been investigated. The IL plays a crucial role in the formation of various morphologies of Y₂O₃. The structural and morphological features of the obtained samples have been characterized by means of X-ray powder diffraction (XRD) analysis, photoluminescence spectra (PL), Fourier-transform infrared (FT-IR) spectra and X-ray photoelectron spectra (XPS). The photoluminescence spectra of the products exhibit an intense bluish-white emission (ranging from 405 to 430 nm and centered at 418 nm). The luminescent mechanisms have been ascribed to the carbon impurities in the Y₂O₃ host. The effect of the ILs cation and the counter anions on the Y₂O₃ morphology of these nanostructures was studied experimentally. It was observed that Y₂O₃ morphology and PL of these nanostructures were strongly influenced by the type of cation and anion. As the length of the subsidiary chain of cation section of IL (imidaziole ione) reduces, the thickness of the nano-sheets increases. It is expected that the present method may easily be extended to similar nano-/microstructures of other oxide materials. Such investigations are currently underway.