Low-temperature sintering and microwave dielectric properties of Mg4Nb2O9 ceramics

The effects of V₂O₅ and Li₂CO₃ on the sinterability and microwave dielectric properties of Mg₄Nb₂O₉ (MN) ceramics were investigated. With addition of 1.5wt% V₂O₅, the dielectric constant (?) and Q·? value of MN ceramics sintered at 1,000 °C are comparable to those of pure MN sintered at 1,400 °C. The good results are because of the enhancement of the density by liquid sintering at the lower temperatures. With the mixtures of V₂O₅ and Li₂CO₃, the sintering temperature of MN was further reduced to 925 °C at the expense of the quality factor (Q·?) value. Typically, ? of 13.7 and Q·? value of 78,000 GHz were obtained for the specimens with mixtures of 1.5wt% V₂O₅ and 1.5wt% Li₂CO₃ and sintered at 925 °C for 5 h.     

Colossal dielectric permittivity of BaTiO3-based nanocrystalline ceramics sintered by spark plasma sintering

In pursuit of high permittivity materials for electronic application, there has been a considerable interest recently in the dielectric properties of various perovskite oxides like calcium copper titanate or lanthanum doped barium titanate. When processed in a particular way, this later material present at ambient temperature and at f?=?1 kHz unusual interesting dielectric properties, a so called “colossal” permittivity value up to several 10⁶ with relatively low dielectric losses. Moreover and contrary to what is classically expected and evidenced for this type of materials, no temperature dependence is observed. This behavior is observed in nanopowders based ceramics. An assumption to explain the observed properties is proposed. These results have important technological applications, since these nanoceramics open a new route to the fabrication of very thin dielectric films.     

Effect of microwave sintering on structural, morphological and dielectric properties of Ba(FeNb)0.5O3 ceramics

Polycrystalline Ba(FeNb)_0.5O₃/BFN ceramics were sintered conventionally and in a microwave (MW) furnace, respectively. Conventional and microwave sintering temperatures were same with different soaking times. Microwave sintering of BFN ceramics showed enhanced grain growth with improved dielectric properties. Highest dielectric constant (~29,913 at 1 kHz) at room temperature (RT) was observed in BFN ceramics sintered in MW furnace for 30 min. At RT, a non-Debye type of dielectric relaxation was observed in both conventionally and MW sintered BFN ceramics. The observed giant dielectric constant of conventionally and MW sintered BFN ceramics was attributed to intrinsic (space charge polarization) and extrinsic (Maxwell-Wagner type polarization) effects, respectively.     

Low temperature sintering and microwave dielectric properties of Ba3Ti5Nb6O28 with B2O3 and CuO additions

The low sintering temperature and the good dielectric properties such as high dielectric constant (ε _r ), high quality factor (Q × f), and small temperature coefficient of resonant frequency (TCF) are required for the application of chip passive components in wireless communication low temperature co-fired ceramics (LTCC). In the present study, the sintering behaviors and dielectric properties of Ba₃Ti₅Nb₆O₂₈ ceramics were investigated as a function of B₂O₃-CuO content. The pure Ba₃Ti₅Nb₆O₂₈ system showed a high sintering temperature (1250^∘C) and had the good microwave dielectric properties: Q × f of 10,600 GHz, ε _r of 37, TCF of −12 ppm/^∘C. The addition of B₂O₃-CuO was revealed to lower the sintering temperature of Ba₃Ti₅Nb₆O₂₈, 900^∘C and to enhance the microwave dielectric properties: Q × f of 32,500 GHz, ε _r of 40, TCF of 9 ppm/^∘C. From the X-ray photoelectron spectroscopy (XPS) and X-ray powder diffraction (XRD) studies, these phenomena were explained in terms of the reduction of oxygen vacancies and the formation of secondary phases having the good microwave dielectric properties.     

Phase compositions and microwave dielectric properties of MgTiO<Subscript>3</Subscript>-based ceramics obtained by reaction-sintering method

MgTiO₃-based microwave dielectric ceramics were prepared successfully by reaction sintering method. The X-ray diffraction patterns of the sintered samples revealed a major phase of MgTiO₃-based and CaTiO₃ phases, accompanied with Mg₂TiO₄ or MgTi₂O₅ determined by the sintering temperature and time. The microwave dielectric properties had a strong dependence of sintering condition due to the different phase compositions and the microstructure characteristics. The ceramics sintered at 1360 °C for 4 h exhibited good microwave dielectric properties: a dielectric constant of 20.3, a high quality factor of 48,723 GHz (at 9GHz), and a temperature coefficient of resonant frequency of ?1.8 ppm/^oC. The obtained results demonstrated that the reaction-sintering process is a simple and effective method to prepare the MgTiO₃-based ceramics for microwave applications.     

Low-temperature sintering of BaTiO3 with Mn-Si-O glass

In order to reduce sintering temperature and prevent adverse dielectric effects, pure BaTiO₃ powder with the addition of Mn-Si-O glass was sintered in the temperature range of 1175–1300°C. Microstructural observation showed that BaTiO₃ grains of the sintered samples only grew from the initial 400 nm to an average of 430 nm between 1175–1275°C for 1 h, or sintered at 1250°C as long as 27 h. Abnormal BaTiO₃ grains are not found in the sintered samples. The microstructure and phase analysis showed that the dielectric properties, tetragonality, and grain growth of BaTiO₃ are closely controlled by the formation of the liquid phase, newly formed Ba₂TiSi₂O₈ grains, and Mn solid solution in BaTiO₃ grains.     

Effect of B2O3 and CuO on the sintering temperature and microwave dielectric properties of the BaTi4O9 ceramics

The effect of B₂O₃ and CuO on the sintering temperature and microwave dielectric properties of BaTi₄O₉ ceramics was investigated. The BaTi₄O₉ ceramics were able to be sintered at 975^∘C when B₂O₃ was added. This decrease in the sintering temperature of the BaTi₄O₉ ceramics upon the addition of B₂O₃ is attributed to the formation of BaB₂O₄ second phase whose melting temperature is around 900^∘C. The B₂O₃ added BaTi₄O₉ ceramics alone were not sintered below 975^∘C, but were sintered at 875^∘C when CuO was added. The formation of BaCu(B₂O₅) second phase could be responsible for the decrease in the sintering temperature of the CuO and B₂O₃ added BaTi₄O₉ ceramics. The BaTi₄O₉ ceramics containing 2.0 mol% B₂O₃ and 5.0 mol% CuO sintered at 900^∘C for 2 h have good microwave dielectric properties of ε_r = 36.3, Q× f = 30,500 GHz and τ_f = 28.1 ppm/^∘C     

Low-temperature dielectric properties of double-perovskite Ca2CoNbO6

Double-perovskite Ca₂CoNbO₆ (CCNO) ceramics were prepared via the solid-state reaction route. Their dielectric properties were investigated as a function of temperature (between 100 and 330?K) in the frequency range from 40?Hz to 10?MHz. Two thermally activated dielectric relaxations were observed with the activation energy around 0.13?eV for the low-temperature relaxation and 0.37?eV for the high-temperature relaxation. Annealing in O₂ and N₂ can remarkably change the dielectric constant, background, relaxation peak intensity and position, etc. These results can be well explained based on the fact that both oxygen and cobalt vacancies coexist in the sample. The low-temperature relaxation was found to be related to the dipolar effect due to the hopping holes, and the high-temperature relaxation was associated with the defect relaxation caused by oxygen and cobalt vacancies.     

Effect of Gd amphoteric substitution on structure and dielectric properties of BaTiO3-based ceramics

BaTiO₃-based ceramics (doped with a small amount of Ni²⁺, Mn²⁺, Nb⁵⁺, Ca²⁺ and Zr⁴⁺) with various Gd₂O₃ concentrations were prepared by the conventional solid-state reaction method. Effects of Gd₂O₃ doping concentrations on the structure and dielectric properties were investigated. It was deduced from XRD patterns that different substitution sites of Gd³⁺ ions could be affected by Gd₂O₃ doping amount. Gd³⁺ tended to occupy Ba-site when Gd₂O₃ concentration was less than 0.25 mol%. With increasing Gd₂O₃ doping amount to 0.3 mol%, Gd³⁺ substituted into both Ba- and Ti-site which contributed to an obvious improvement on dielectric constant of BaTiO₃-based ceramics. Influences of the Gd³⁺ amphoteric substitution on the improvement of the dielectric constant were discussed based on the self-compensation mechanism.     

The sintering behavior and microwave dielectric properties of Mg4(Nb,Sb)2O9 ceramics

The sintering behavior, microstructure and microwave dielectric properties of Mg₄(Nb_2?x Sb _x )O₉ (0?≤?x?≤?2) solid solutions were investigated systematically by X-ray diffraction(XRD), scanning electron microscopy(SEM) and a network analyzer. The solid solutions of Mg₄(Nb_2?x Sb _x )O₉ was formed with x value being no more than 1.6. The dielectric constant (?) of the sintered ceramics decreased from 13.06 to 6.28 with Sb content x from 0 to 1.6. With a substitution of Sb⁵⁺ for Nb⁵⁺ (0.04?≤?x?≤?0.08), the sintering temperature of Mg₄Nb₂O₉ ceramics was decreased from 1400 to 1300 °C without degradation of the Qf values. The optimum microwave dielectric properties of ??～?12.26, Qf?～?168,450 GHz, and τ _f?～??56.4 ppm/°C were obtained in the composition of Mg₄(Nb_1.6Sb_0.4)O₉ sintered at 1300 °C.     

Microwave dielectric properties of B2O3-added Li2MgTiO4 ceramics for LTCC applications

Li₂MgTiO₄ (LMT) ceramics which are synthesized using a conventional solid-state reaction route. The LMT ceramic sintered at 1250°C for 4 h had good microwave dielectric properties. However, this sintering temperature is too high to meet the requirement of low-temperature co-fired ceramics (LTCC). In this study, the effects of B₂O₃ additives and sintering temperature on the microstructure and microwave dielectric properties of LMT ceramics were investigated. The B₂O₃ additive forms a liquid phase during sintering, which decreases the sintering temperature from 1250°C to 925°C. The LMT ceramic with 8 wt% B₂O₃ sintered at 925°C for 4 h was found to exhibit optimum microwave dielectric properties: dielectric constant 15.16, quality factor 64,164 GHz, and temperature coefficient of resonant frequency -28.07 ppm/°C. Moreover, co-firing of the LMT ceramic with 8 wt% B₂O₃ and 20 wt% Ag powder demonstrated good chemical compatibility. Therefore, the LMT ceramics with 8 wt% B₂O₃ sintered at 925°C for 4 h is suitable for LTCC applications.     

Crystallization behavior and microwave dielectric characteristics of ZnO-(La, Nd)2O3-B2O3-based dielectrics

Crystallizable zinc borate glasses modified with different contents of La₂O₃ or Nd₂O₃ were investigated as a potential low loss dielectric with respect to their crystallization behavior and microwave dielectric characteristics. The glasses were admixed with Al₂O₃ filler and fired at 850°C for 30 min in air to prepare low temperature dielectrics. Crystallization behavior and microwave dielectric properties of the resulting samples strongly depended on the relative content of La₂O₃ or Nd₂O₃ in the glass. As a promising result, the composition of 0.15ZnO-0.25Nd₂O₃-0.6B₂O₃ exhibited k?～?6.5 and Q?～?1194 at the resonant frequency of 18.9 GHz. Near zero temperature coefficient of frequency (TCF) was obtained by additional modification of the composition with ～10 wt.% of TiO₂ filler. Crystallization kinetics of the samples was studied based on the differential thermal analysis (DTA) curves obtained with different heating rates. Correlation of the observed dielectric properties to the crystallization behavior is the main subject of this work.     

Phase transformation and microwave dielectric properties of BiPO4 ceramics

Monazite-type compounds, BiPO₄ polymorphs were prepared by the solid-state reaction method. The phase transformation and microwave dielectric properties of sintered ceramics were investigated using the X-ray powder diffraction (XRD) and a network analyzer, respectively. The low-temperature phase of BiPO₄ has monoclinic structure, and was transformed into the high-temperature phase with a slight distortion of monoclinic when it is heated above 600^∘C. The effect of the transformation on the microwave dielectric properties was examined. It was found that the dielectric properties of each phase were significantly different. In particular, the high-temperature phase sintered at 950^∘C has good microwave dielectric properties; the relative dielectric constant (ε _r ) = 22, the quality factor (Q× f) = 32,500 GHz and the temperature coefficient of resonant frequency (τ _f ) = − 79 ppm/ ^∘C.     

Improved giant dielectric properties in microwave flash combustion derived and microwave sintered CaCu 3 Ti 4 O 12 ceramics

The nanocrystals of CaCu3Ti4O12 ceramic were prepared by microwave flash combustion technique. The microwave sintering of powders was optimized to 1025 − 1075 °C for 20 min with heating and cooling rate of 50 °C/min. Microstructural evaluation of sintered sample was carried out using SEM. The dielectric properties were measured in the frequency range 10–2 × 106 Hz and the temperature range 30–100 °C. The CCTO sample sintered at 1075 °C had giant dielectric constant 53,300 at 100 Hz. It was observed that dielectric constant was greatly increased on a slight increase in sintering temperature. Modulus and impedance analysis were performed to explore the observed unusual dielectric response. Grain and grain boundary resistance were observed as 8 Ω and 350,000 Ω, respectively. The grain boundary activation energy for electro-conduction was calculated as 0.65 eV by using the characteristic frequencies in cole-cole plots. It was noticed that the thermally activated charge carriers had long-range mobility.     

Dielectric measurement using non-contact microwave single probe for dielectric materials

A high frequency dielectric measurement method was proposed using a non-contact probe. The microwave reflection intensity was measured for Al₂O₃ and SrTiO₃ substrates at room temperature as a function of distance between sample and probe. The difference of reflection intensity for Al₂O₃ and SrTiO₃ substrates was observed in the region where the distance of 0.2 mm between sample and probe, and it was caused from dielectric permittivities of samples. The reflection coefficient of sample was estimated in comparison with results of electromagnetic simulation. The reflection intensity for Al₂O₃ and SrTiO₃ substrates was transformed to dielectric permittivity at reflection intensity minimum point.     

Low-temperature sintering of Li2O-doped BaTiO3 lead-free piezoelectric ceramics

Low-temperature sintering of BaTiO₃ ceramics using Li₂O as sintering aids was investigated with a special influences of Li₂O content (0–4?mol%) and sintering temperature (1000–1100°C) on crystalline structure and electrical properties. The sinterability of BaTiO₃ ceramics significantly improved by adding Li₂O, whose densification sintering temperature reduced from 1300°C to 1000°C. XRD pattern indicated that BaTiO₃-xLi₂O samples were single phase with a tetragonal symmetry as x?=?0–0.3?mol%, while the samples became an orthorhombic symmetry as x?=?0.5–4?mol%. The densification sintering temperature in which samples showed relative density higher than 90?% decreased with increasing Li₂O content. A maximum d ₃₃ value (200 pC/N) was obtained for the BaTiO₃-0.5?mol%Li₂O sample sintered at 1050°C, which is attributed to a vicinity of the phase transition and the high density. Adding Li₂O not only reduced the sintering temperature but also obtained the acceptable piezoelectric properties, which will make BaTiO₃ become a kind of promising and practical lead-free piezoelectric ceramics.     

Magnetic properties of Ni-Zn ferrites prepared by microwave sintering method

The effect of zinc ion substitution for nickel on structural and magnetic properties of NiZn ferrites is reported. The spinel ferrite system Ni_1-xZn_xFe₂O₄ with x = 0.2, 0.3, 0.4 and 0.5 was prepared by microwave sintering method. The uniaxially pressed samples were sintered at various temperatures such as 900°C, 1000°C and 1100°C for 30 min. X-ray diffraction patterns of the samples indicate the formation of single-phase cubic spinel structure. SEM micrographs show that grain size increases with increasing zinc content and sintering temperature. The elemental composition of these ferrites was analyzed by EDS. Lattice constant increases with increase in zinc content, obeying Vegard’s law. The effect of composition and sintering temperature on initial permeability as the function of frequency and temperature was studied. The initial permeability of NiZn ferrite increases greatly with increasing Zn content and sintering temperature. The dependence of initial permeability with respect to temperature shows the decrease in the Curie point with increase in zinc content, is the normal behavior of ferrites. The relative loss factor (tand

微波烧结与传统烧结合成的NiCuZn铁氧体组织与性能

采用固相合成法制备了Ni Cu Zn铁氧体材料,对比研究了传统烧结与微波烧结工艺对Ni Cu Zn铁氧体材料的致密化行为、显微结构、磁滞回线和直流偏置特性的影响。结果表明,在微波烧结方式中,材料的致密化曲线向低温方向偏移,烧结致密度得到提高,晶粒尺寸显著增大;对比于传统烧结,微波烧结材料的饱和磁感应强度从312m T提高至479m T,起始磁导率从65提升至170,但在叠加直流偏置电流为3A时,磁导率下降幅度从28.5%增至48.4%。     

Abnormal resistivity-temperature characteristics of semiconducting (Ba1-x Pb x )TiO3 materials prepared by microwave sintering

Abstract

(Ba_0.7Pb_0.3)TiO₃ and (Ba_0.4Pb_0.6)TiO₃ materials possessing double critical temperature (T_c ) and single high-T_c in resistivity-temperature (ρ-T) behavior, respectively, were obtained by microwave sintering at 1050°C for 5 minutes. These characteristics were ascribed to the existence of the dual phases with core-shell structure. The cooling-rate control modified the relative magnitude of low-T_c and high-T_c resistivity jumps, without altering the T_c -values. It occurred via the change in relative proportion of the core and shell phases.     

Experimental and numerical studies of dielectric properties of BaTiO/sub 3/-platinum composites at microwave frequencies

The conductor loading method has been used for creating a lossy dielectric material with a desired loss tangent. This method may also be applicable for developing high dielectric constant materials. In this paper, we will present the experimental results of the dielectric properties of BaTiO/sub 3/ and BaTiO/sub 3/ -platinum (BaTiO/sub 3/-Pt) composites. These composite materials were designed to increase the real part of the effective dielectric constant at high frequency. Three different platinum volume fractions were used, 3, 5 and 10%, to make BaTiO/sub 3/-Pt composites, in addition to a pure BaTiO/sub 3/ material. To characterize the BaTiO/sub 3/-Pt composites, microwave frequency measurements were conducted using the waveguide transmission technique. The experimental and numerical results verify that it is possible to increase the dielectric constant using the conductor loading method.