Effect of sintering temperature on the properties of modified mechanical alloyed CaCu3Ti4O12

This paper presents the effects of calcination time and sintering temperature on the properties of CaCu(3)Ti(4)O(12). Electroceramic material of CaCu(3)Ti(4)O(12) was prepared using a modified mechanical alloying technique that covers several processes, which are preparation of raw material, mixing and ball milling for 5 hours, calcination, pellet forming and, sintering. The objective of this modified technique is to enable the calcination and sintering processes to be carried out at a shorter time and lower temperature. The x-ray diffraction (XRD) analysis result shows that a single-phase of CaCu(3)Ti(4)O(12) was completely formed by calcination at 750 degrees C for 12 hours. Meanwhile, the grain size of a sample sintered at 1050 degrees C for 24 hours is extremely large, in the range of 20-50 mum obtained from field emission scanning electron microscopy (FESEM) images. The dielectric constant value of 14,635 was obtained at 10 kHz by impedance (LCR) meter in the sintered sample at 1050 degrees C. However, the dielectric constant value of samples sintered at 900 and 950 degrees C is quite low, in the range of 52-119.     

Sintering characteristics and crystallization for sol–gel-derived powders for low-dielectric and low-temperature sintering ceramics

Samples in the MgO–Al₂O₃–SiO₂ system were prepared by the sol–gel technique. The coalescence, sintering characteristics, and crystallization were investigated by X-ray diffraction, thermal analysis, and scanning electron microscopy. The dielectric properties and density were measured with an impedance analyzer. Results demonstrated that the obtained cordierite powders synthesized with the sol–gel method distribute uniformly and its effective size is 474 nm. The glass powder could be sintered at 950 °C, and the polymorphic modification cordierite detected in the sintered sample was only stable hexagonal -phase. The sintering densification process was performed mainly in the temperature range from 800 °C to 930 °C, and follows the viscous floating principle. The dielectric constant of the sintered body is 4.2 and its dielectric loss is lower than 0.001 at high frequency (1.5 GHz).     

Synthesis of cordierite and cordierite-ZrSiO4 composite by colloidal processing

Cordierite powder of high purity and cordierite-ZrO₂ composite powder were synthesized by colloidal processing. Cordierite was synthesized by calcining a precursor gel obtained by gelation and coprecipitation of AlOOH sol, SiO₂ sol and Mg(NO₃)₂. The calcination temperature affected the constituent phases in the powders. The phase assemblage in calcined powder affected the sintering conditions. The optimum sintering temperature of the powder with cordierite single phase was 1440–1450 °C when it was calcined at 1270 °C. The sintered body had a dense microstructure with submicrometre grains. Addition of ZrO₂ sol resulted in reaction with cordierite to form mostly ZrSiO₄ at the sintering temperature. Several properties of cordierite and cordierite-ZrSiO₄ composite, such as thermal expansion coefficient, bending strength, dielectric constant and insulation properties at high temperature, were investigated. Thermal expansion and electric properties were degraded by an increasing amount of ZrO₂ additive, whereas the bending strength was improved by the addition of ZrO₂.     

Sintering Behavior and Microwave Dielectric Properties of MgTiO3 Ceramics Doped with B2O3 by Sol-Gel Method

The B2O3-doped MgTiO3 powders and ceramics have been prepared by sol-gel method using Mg(NO3)2·6H2O, Ti(C4H9O)4 and H3BO3 as the starting materials. The sintering behavior and microwave dielectric properties of ceramics prepared from powders with different particle sizes were investigated. The gels were calcined at 650, 700, 750, 800, 850 and 900 C and the derived particle sizes of powders were 20-30 nm, 30-40 nm, 40-60 nm, 60-90 nm, 90-120 nm and 120-150 nm, respectively. The nanoparticles with the size of 30-60 nm benefited the sintering process with high surface energy whereas nanoparticles with the size of 20-30 nm damaged the microwave dielectric properties due to the pores in the ceramics. The addition of B2O3 used as a liquid sintering aid reduced the sintering temperature of MgTiO3 ceramic, which was supposed to enter the MgTiO3 lattice and resulted in the formation of (MgTi)2(BO3)O phase. The B2O3-doped MgTiO3 ceramic sintered at 1100 C and prepared from the nanoparticles of 40-60 nm had compact structure and exhibited good microwave dielectric properties: εr=17.63, Q × f=33,768 GHz and τ f= 48×10 6 C 1.     

微波烧结对PLZT陶瓷电学性能的影响

采用部分共沉淀法制备锆钛酸铅镧(PLZT)粉体, 分别用普通马弗炉和微波马弗炉进行烧结成瓷, 对比分析不同烧结方法对PLZT陶瓷的晶体结构、微观形貌和电学性能的影响。结果表明: 微波烧结和常规烧结均成功制备出钙钛矿相PLZT陶瓷。采用微波烧结得到的PLZT陶瓷样品比常规烧结的晶粒细小, 尺寸更均匀, 孔洞较少; 在电学性能相近时, 微波烧结温度远低于常规烧结, 且保温时间远小于常规烧结。在1000℃进行微波烧结, 陶瓷的介电常数ε_r和压电常数d₃₃最大, ε_r为2512, d33为405 pC/N, 此时, 剩余极化强度为16.5 kV/cm, 矫顽场为8.2μC/cm²; 在1250℃常规烧结, 陶瓷的介电常数最大, 为2822, 压电常数最大, 为508 pC/N, 剩余极化强度为21.6 kV/cm, 矫顽场为9.6μC/cm²。     

溶胶-凝胶法制备堇青石纳米粉体及表征

以硝酸镁、硝酸铝和正硅酸乙酯为原料,按照堇青石化学计量配比,用溶胶-凝胶法配合回流制备堇青石粉体,通过差热分析、X射线衍射、扫描电镜等分析测试方法,对所制备粉体进行分析和表征.结果表明,在不添加任何助剂的情况下,可制得粒度均匀的堇青石粉体,平均粒径约为100 nm;压片后的坯样经1 056℃烧结,可获得以α-堇青石为主晶相的陶瓷材料,致密度为98.6％,且具有较低的介电常数和介电损耗(ε=3.94,tg δ=0.001 6,1 GHz),可用作高频片感介质材料.     

Microwave dielectric properties and microstructures of MgTa2O6 ceramics with CuO addition

The effect of CuO addition on the microstructures and the microwave dielectric properties of MgTa₂O₆ ceramics has been investigated. It is found that low level-doping of CuO (up to 1 wt.%) can significantly improve the density of the specimens and their microwave dielectric properties. Tremendous sintering temperature reduction can be achieved due to the liquid phase effect of CuO addition observed by scanning electronic microscopy (SEM). The sintered samples exhibit excellent microwave dielectric properties, which depend upon the liquid phase and the sintering temperature. With 0.5 wt.% CuO addition, MgTa₂O₆ ceramic can be sintered at 1400 °C and possesses a dielectric constant (_r) of 28, a Q × f value of 58000 GHz and a temperature coefficient of resonant frequency (τ_f) of 18 ppm/°C.     

(Ba1-xSrx)La4Ti4O15（x=0.8～0.95）陶瓷的微结构及微波介电性能研究

采用固相反应法制备了(Ba1-xSrx)La4Ti4O15(x=0.8~0.95)复合体系微波介质陶瓷,并对其进行物相组成、晶体结构分析以及微波介电性能的研究.研究结果表明,(Ba1-xSrx)La4Ti4O15陶瓷主晶相为SrLa4Ti4O15,并伴随有第二相SrLa8Ti9O15.SEM观察表明,Ba0.2Sr0.8La4Ti4O15陶瓷内部微观结构致密,晶粒尺寸在10~20μm之间,晶界清晰.随着x值逐渐增大,(Ba1-xSrx)La4Ti4O15陶瓷中晶粒形态发生变化,气孔增多.在x=0.8时,(Ba1-xSrx)La4Ti4O15陶瓷具有优良的微波介电性能,即εr=40.86,Q×f≈62806 GHz,τf=20×10 6/℃.随着Ba2+的含量逐渐增加,该陶瓷的介电常数εr单调上升,品质因子Q×f值增加,说明适量的Ba2+替代Sr2+能改善陶瓷的微波介电性能.     

Influence of lead oxide addition on LnTiTaO<Subscript>6</Subscript> (Ln = Ce,Pr and Nd) microwave ceramics

The effect of PbO addition on the structural, processing and microwave dielectric properties of LnTiTaO₆ (Ln = Ce, Pr and Nd) ceramics are reported. Conventional solid state ceramic route was used for the preparation of samples. Phase pure LnTiTaO₆ (Ln = Ce, Pr and Nd) ceramics are prepared at a calcination temperature of 1300°C. The samples are sintered at optimized temperatures. Addition of PbO reduces the sintering temperature. The crystal structure of the materials was analysed using X-ray diffraction techniques and the surface morphology of the sintered samples was analysed using scanning electron microscopy. The dielectric constant at microwave frequency range decreases for higher PbO addition for all the samples but the quality factor improves on small PbO addition. The thermal stability of resonant frequency was also improved with PbO addition on all the systems. A number of samples with improved microwave dielectric properties were obtained on all the systems suitable for practical applications.     

Piezoelectric ceramics with high dielectric constants for ultrasonic medical transducers

Complex system ceramics Pb(Sc(1/2)Nb(1/2))O3-Pb(Mg(1/3)Nb(2/3))O3-Pb(Ni(1/2)Nb(1/2))O3-(Pb0.965,Sr0.035) (Zr,Ti)O3 (PSN-PMN-PNN-PSZT abbreviated PSMNZT) have been synthesized by the conventional technique, and dielectric and piezoelectric properties of the ceramics have been investigated for ultrasonic medical transducers. High capacitances of the transducers are desired in order to match the electrical impedance between the transducers and the coaxial cable in array probes. Although piezoelectric ceramics that have high dielectric constants (epsilon33t/epsilon0 > 5000, k'33 < 70%) are produced in many foundries, the dielectric constants are insufficient. However, we have reported that low molecular mass B-site ions in the lead-perovskite structures are important in realizing better dielectric and piezoelectric properties. We focused on the complex system ceramics PSMNZT that consists of light B-site elements. The maximum dielectric constant, epsilon33T/epsilon0 = 7, 200, was confirmed in the ceramics, where k'33 = 69%, d33 = 940 pC/N, and T(c) = 135 degrees C were obtained. Moreover, pulse-echo characteristics were simulated using the Mason model. The PSMNZT ceramic probe showed echo amplitude about 5.5 dB higher than that of the conventional PZT ceramic probe (PZT-5H type). In this paper, the electrical properties of the PSMNZT ceramics and the simulation results for pulse-echo characteristics of the phased-array probes are introduced.     

Effect of microwave sintering on the structural, optical and electrical properties of BaTiO3 nanoparticles

BaTiO₃ nanoparticles were prepared by high energy ball milling and subjected to conventional and microwave post sintering at 1,000 °C. From the powder X-ray diffraction results, the synthesized material exhibits strong tetragonality with large c/a ratio. Scanning electron microscope results show the formation of tetragonal shaped BaTiO₃ crystals in the nanometer scale and a significant reduction in the particle size for the microwave sintered sample. The reduced d-spacing of 1.741 Å with high crystallinity for the microwave sintered material is revealed by high resolution transmission electron microscopy analysis. Ultraviolet–visible spectroscopy studies confirm the higher optical band gap (E_g) of 4.157 eV for the microwave sintered sample. Microwave sintered sample shows a very high dielectric constant of ε_r = 4,445 with a low dielectric loss as tan δ = 0.0961. Microwave sintered sample exhibit a high polarization maximum of 73 μC/mm² with reduced coercivity to be 0.293 kV/mm.     

Characteristics of Ba6−3x Nd8+2x Ti18O54 microwave dielectric ceramics derived from ethylenediaminetetraacetic acid precursor

ceramic powders were synthesized by the sol-gel method using ethylenediaminetetraacetic acids as chelating agent. Various techniques were used to characterize the precursors, powders and sintered ceramics. The microwave dielectric properties of ceramics sintered at different temperatures were also measured. Well-crystallized powders with about 80 nm particle size were obtained by calcination of the pulverized resins at 900 °C for 3 h in air. The (x=2/3) ceramics sintered at 1340 °C for 3 h had excellent microwave dielectric characteristics: =87.1, Qf=8710 GHz.     

Enhanced tunable characteristics of the Na0.5Bi0.5TiO3-NaTaO3 relaxor-type system

We have investigated the voltage-tunable characteristics of the Na(0.5)Bi(0.5)TiO(3)-NaTaO(3) homogeneity region, for which samples were prepared using a conventional solid-state reaction. The highest value of the relative tunability (n(r)) was obtained for the sample with 5 mol% of NaTaO(3), i.e., 47% at 1 MHz and a 70 kV/cm dc bias field. This sample also showed the highest value of the dielectric losses (tan delta) and temperature coefficient of the dielectric constant (tau(epsilon)), i.e., 0.05 and 4478 ppm/K, respectively. As the concentration of NaTaO(3) increased up to 90 mol% n(r), tan delta, and tau(epsilon) gradually decreased toward 22%, 0.0002 and -899 ppm/K, respectively. The dielectric constant of the samples varied in a similar manner between 662 and 130. At microwave frequencies, the dielectric losses of the samples substantially increased due to their relaxor-type nature. The lowest value was obtained for the samples with 90 mol% of NaTaO(3), i.e., 0.002. The tunable characteristics of the samples are related to the ferroelectric and dielectric properties, and it appears that the dielectric tunability of the Na(0.5)Bi(0.5)TiO(3)-NaTaO(3) system originates from its relaxor-type behavior.     

Characterization of nanostructured PZT prepared by chemical routes

Nanostructured, crystalline Pb(Zr0.52Ti0.48)O3 (crystallite size 8-10 nm) ceramic powders were synthesized at low temperature by the hydroxide co-precipitation and aqueous solution method (water bath technique). The phase and surface morphology characterizations were carried out by XRD, SEM, and TEM analyses. XRD powder pattern exhibited the presence of a major tetragonal and a minor rhombohedral crystalline phase indicating the mixed phase composition in both the samples. SEM-EDS analysis revealed good homogeneity of the materials. From evolution of the Raman spectra the spectroscopic signature of the corresponding phases was determined. Detailed dielectric measurements (between 30 degrees C to 500 degrees C) were obtained to analyze a complete set of impedance-related functions such as dielectric constant (epsilon), loss factor (tan delta), dielectric modulus (M), and conductivity (sigma). Similar to the normal ferroelectric (FE) materials, the dielectric constant (epsilon) of synthesized PZTs was found to be increasing gradually with temperature and attains a maxima (epsilonmax) at the Curie temperature (Tc). The peaks in the dielectric constant plots are attributed to the phase transition associated with the change from tetragonal to rhombohedral structures. The higher dielectric constant of the PZT prepared by hydroxide co-precipitation make it more suitable for various applications.     

Effect of glass additions on the sintering behaviors and electrical microwave properties of BaO–Nd2O3–Sm2O3–TiO2 ceramics

The effect of Al₂O₃-doped silica glass (AS-glass) addition on the structure and dielectric properties of the BaO–Nd₂O₃–Sm₂O₃–TiO₂ (BNST) microwave materials was investigated. This BNST material has a dielectric constant (k) of 80 and a quality factor (Q×f) of 6000 GHz when sintered at 1350 °C for 2 h. Both the microstructure and the microwave dielectric characteristics were determined as a function of the sintering temperature and glass content. A Q×f as high as 8700 GHz was achieved in ceramics added with 20 wt % glass, however, the k value drops to 30. The high Q×f value is attributed to the improved densification of the dielectric when glass is added. Results of X-ray diffraction experiments indicate that glass addition enhances the growth in the longitudinal direction of the columnar crystal and a preferred (0 0 2) orientation. The presence of columnar structure plays an important role in the improvement of the microwave dielectric properties.     

Piezoelectric properties of (K,Na)NbO3 thin films deposited on (001)SrRuO3/Pt/MgO substrates

(K(x),Na(1-x))NbO(3) (KNN) thin films were deposited on (001)SrRuO(3)/(001)Pt/(001)MgO substrates by RF-magnetron sputtering, and their piezoelectric properties were investigated. The x-ray diffraction measurements indicated that the KNN thin films were epitaxially grown with the c-axis orientation in the perovskite tetragonal system. The lattice constant of the c-axis increased with increasing concentrations of potassium. The KNN thin films showed typical ferroelectric behavior; the relative dielectric constant epsilon(r) was 270 to approximately 320. The piezoelectric properties were measured from the tip displacement of the KNN/MgO unimorph cantilevers; the transverse piezoelectric coefficient epsilon*(31) (= d(31)/s(E)(11)) of KNN (x = 0) thin films was calculated to be -0.9 C/m(2). On the other hand, doping of potassium caused an increase in the piezoelectric properties, and the KNN (x = 0.16) films showed a relatively large transverse piezoelectricity of epsilon*(31) = -2.4 C/m(2).     

Microwave and photoluminesent characterizations of (Ca<Subscript>2</Subscript>Mg<Subscript>3</Subscript>)(X<Subscript>1.75</Subscript>Sb<Subscript>0.25</Subscript>)TiO<Subscript>12</Subscript> [X = Nb and Ta] ceramics

(Ca₂Mg₃)(X_1.75Sb_0.25)TiO₁₂ [X = Nb and Ta] ceramics are prepared through the conventional solid-state route. The samples are calcined at 1,100 and 1,180 °C, and are sintered at 1,250 and 1,375 °C. The substitution of Sb decreases the calcination and sintering temperatures of pure (Ca₂Mg₃)(Nb/Ta)₂TiO₁₂. The structure of the samples is analyzed using X-ray diffraction method. The microstructure of the sintered pellet is studied using scanning electron microscopy. The dielectric properties such as dielectric constant (ε_r), quality factor (Q_uxf) and temperature coefficient of resonant frequency (τ_f) are measured in the microwave frequency region. By Sb substitution, thermal stability is achieved, with the increase in dielectric constant, without much change in the quality factor. The materials have intense emission lines in the wavelength region 500–700 nm. The compositions have good microwave dielectric properties and photoluminescence and hence are suitable for dielectric resonator and ceramic laser applications.     

Microwave synthesis and sintering characteristics of CaCu<Subscript>3</Subscript>Ti<Subscript>4</Subscript>O<Subscript>12</Subscript>

CaCu₃Ti₄O₁₂ (CCTO) was synthesized and sintered by microwave processing at 2·45 GHz, 1·1 kW. The optimum calcination temperature using microwave heating was determined to be 950°C for 20 min to obtain cubic CCTO powders. The microwave processed powders were sintered to 94% density at 1000°C/60 min. The microstructural studies carried out on these ceramics revealed the grain size to be in the range 1–7 μm. The dielectric constants for the microwave sintered (1000°C/60 min) ceramics were found to vary from 11000–7700 in the 100 Hz–00 kHz frequency range. Interestingly the dielectric loss had lower values than those sintered by conventional sintering routes and decreases with increase in frequency.     

Li2CO3-B2O3-V2O5掺杂ZnO-TiO2陶瓷低温烧结的研究

以Li2CO3、B2O3和V2O53种常见的低熔点氧化物为烧结助剂,用传统固相法制备了Li2CO3-B2O3-V2O5掺杂的ZnO-TiO2微波介质陶瓷,并利用XRD、SEM等研究了ZnO-TiO2陶瓷的烧结行为、物相组成、显微结构特征及微波介电性能等。结果表明,当掺入3%(质量分数)Li2CO3-B2O3-V2O5时,在840℃烧结2h可制备出体积密度为4.99g/cm3的ZnO-TiO2陶瓷,达到理论密度的96.5%以上,εr、Q.f、τf分别约为24、22900GHz、-4×10-6/℃。     

掺ZBS玻璃低温烧结ZnNb2O6微波介质陶瓷的研究

研究了ZnO-B2 O3-SiO2(ZBS)玻璃料对ZnNb2O6微波介质陶瓷烧结特性和介电性能的影响.结果表明,ZBS玻璃料形成的液相加速了颗粒间的传质,促进了烧结,能使ZnNb2O6陶瓷的烧结温度有效地降低至950℃.随着ZBS含量的增加,样品中出现了第二相,且气孔被包裹在晶粒内部难以逃脱出来,导致样品的缺陷和损耗增加,从而降低介电性能.掺杂1%ZBS的ZnNb2O6陶瓷在950℃保温4h,能获得优异的综合介电性能:ε=23.56、Q·f=18482GHz、τf=-28.8×10￣6/℃.