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1.
A coating approach for synthesizing 0.9Pb(Mg1/3 Nb2/3 )O3 –0.1PbTiO3 (0.9PMN–0.1PT) and PMN using a single calcination step was demonstrated. The pyrochlore phase was prevented by coating Mg(OH)2 on Nb2 O5 particles. Coating of Mg(OH)2 on Nb2 O5 was done by precipitating Mg(OH)2 in an aqueous Nb2 O5 suspension at pH 10. The coating was confirmed using optical micrographs and zeta-potential measurements. A single calcination treatment of the Mg(OH)2 -coated Nb2 O5 particles mixed with appropriate amounts of PbO and PbTiO3 powders at 900°C for 2 h produced pyrochlore-free perovskite 0.9PMN–0.1PT and PMN powders. The elimination of the pyrochlore phase was attributed to the separation of PbO and Nb2 O5 by the Mg(OH)2 coating. The Mg(OH)2 coating on the Nb2 O5 improved the mixing of Mg(OH)2 and Nb2 O5 and decreased the temperature for complete columbite conversion to ∼850°C. The pyrochlore-free perovskite 0.9PMN–0.1PT powders were sintered to 97% density at 1150°C. The sintered 0.9PMN–0.1PT ceramics exhibited a dielectric constant maximum of ∼24 660 at 45°C at a frequency of 1 kHz. 相似文献
2.
A relaxor ferroelectric material, 0.9Pb(Mg1/3 Nb2/3 )O3 -0.1PbTiO3 (0.9PMN-0.1PT) with a pyrochlore-free phase, was prepared by using one-step calcination in the present study. The 0.9PMN-0.1PT powder with the pure perovskite phase was prepared successfully from a mixture of the PMN precursor and the crystalline PT by heating for 2 h at temperatures greaterthan equal to750°C. The PMN precursor was synthesized by adding an aqueous Mg(NO3 )2 solution, rather than MgO, to the alcoholic slurry of PbO and Nb2 O5 . The 0.9PMN-0.1PT powder sintered to >96% relative density via heat treatment for 2 h at temperatures of 900°-1200°C. The highest room-temperature dielectric constant (epsilonrt ) was 24700 at 1 kHz for the samples that were sintered at 1100°C; however, the samples that were sintered at 900°C still had epsilonrt values of 22600 at 1 kHz. 相似文献
3.
Zhijun Xu Ruiqing Chu Jigong Hao Yanjie Zhang Guorong Li Qingrui Yin Aili Ding 《Journal of the American Ceramic Society》2010,93(1):18-21
Using two-step particle-coating method, pyrochlore-free Pb(Mg1/3 Nb2/3 )O3 (PMN) powders have been successfully synthesized by a single calcination step at a relatively lower calcined temperature of 850°C. The XRD and EDS results confirmed that the Mg–citric acid polymeric complex coatings effectively prevent direct contact between PbO and Nb2 O5 and thus avoid the formation of pyrochlore phase. The coated powders were calcined directly without the ball-milling procedure at 850°C. The pyrochlore-free PMN powders obtained showed uniform and even grain size. The results showed that this method is an attractive method for the synthesis of PMN-based composite powders. 相似文献
4.
The Bi2 O3 –Nb2 O5 –NiO phase diagram at 1100°C was determined by means of solid-state synthesis, X-ray diffraction, and scanning electron microscopy. A ternary eutectic with a melting point below 1100°C was found to exist in the field between NiO, Bi2 O3 , and the end-member of the δBi2 O3 –Nb2 O5 solid solution. The existence of the previously reported Bi3 Ni2 NbO9 phase was disproved. A pyrochlore homogeneity range around Bi1.5 Ni0.67 Nb1.33 O6.25 was determined together with all the phase relations in this phase diagram. 相似文献
5.
Lead-based piezoelectric ceramics typically require sintering temperatures higher than 1000°C at which significant lead loss can occur. Here, we report a double precursor solution coating (PSC) method for fabricating low-temperature sinterable polycrystalline [Pb(Mg1/3 Nb2/3 )O3 ]0.63 -[PbTiO3 ]0.37 (PMN–PT) ceramics. In this method, submicrometer crystalline PMN powder was first obtained by dispersing Mg(OH)2 -coated Nb2 O5 particles in a lead acetate/ethylene glycol solution (first PSC), followed by calcination at 800°C. The crystalline PMN powder was subsequently suspended in a PT precursor solution containing lead acetate and titanium isopropoxide in ethylene glycol to form the PMN–PT precursor powder (second PSC) that could be sintered at a temperature as low as 900°C. The resultant d 33 for samples sintered at 900°, 1000°, and 1100°C for 2 h were 600, 620, and 700 pm/V, respectively, comparable with the known value. We attributed the low sintering temperature to the reactive sintering nature of the present PMN–PT precursor powder. The reaction between the nanosize PT and the submicrometer-size PMN occurred roughly in the same temperature range as the densification, 850°–900°C, thereby significantly accelerating the sintering process. The present PSC technique is very general and should be readily applicable to other multicomponent systems. 相似文献
6.
Dae-Joon Kim Paul F. Becher Camden R. Hubbard 《Journal of the American Ceramic Society》1993,76(11):2904-2908
Tetragonal ZrO2 ( t -ZrO2 ) solid solutions were prepared with addit ons of 2 mol% Y2 O3 plus up to 0.45 mol% Nb2 O5 . The thermal expansion coefficients in both the a- and c -axis lattice directions increased with Nb2 O5 alloying and the thermal expansion in the c -axis direction was greater than that in the a -axis direction over the entire composition range. This anisotropic thermal expansion behavior was related to the 4-fold coordination of Nb5+ with oxygen ions in t -ZrO2 solid solutions in the system ZrO2 –Y2 O3 –Nb2 O5 . The fracture toughness continuously increased with Nb2 O5 alloying and suggested that the c/a axial ratio is a more significant factor than the internal stress that arises from the thermal expansion anisotropy, in the determination of the transformability of t -ZrO2 in this system. 相似文献
7.
Our analysis of the microwave dielectric properties of the δ-Bi2 O3 –Nb2 O5 solid solution (δ-BNss ) showed a continuous increase in permittivity and dielectric losses with an increasing concentration of Nb2 O5 . The only discontinuity was found for the temperature coefficient of resonant frequency, which is negative throughout the entire homogeneity range but reaches a minimum value for the sample with 20 mol% Nb2 O5 . At the same composition there is a discontinuity in the grain size of the δ-BNss ceramics. For the sample containing 25 mol% Nb2 O5 two structural modifications were observed. A single-phase tetragonal Bi3 NbO7 , in the literature referred to as a Type-III phase, is formed in a very narrow temperature range from 850° to 880°C. A synthesis performed below or above this temperature range resulted in the formation of the end member of the δ-BNss homogeneity range. Compared with the δ-BNss the Bi3 NbO7 ceramics exhibit lower microwave dielectric losses, an increased conductivity, and a positive temperature coefficient of resonant frequency. 相似文献
8.
The sintering behavior and surface microstructure of PbNi1/3 Nb2/3 O3 –PbTiO3 –PbZrO3 (PNiNb-PT-PZ) ceramics were investigated. The PNiNb-PT-PZ ceramics with the stoichiometric composition and the addition of excess lead oxide (PbO-rich ceramics) were sintered by liquid-phase sintering in accordance with the solution-reprecipitation mechanism at temperatures below the melting point of PbO. The temperature at which the liquid phase forms fell to near the eutectic point of the PbO–Nb2 O5 and the PbO–TiO2 system (868°C) with the addition of 5 mol% PbO. As the calcination temperature influenced the sinterability of the stoichiometric PNiNb-PT-PZ ceramic, unreacted PbO was considered to be the source of the liquid phase in the sintering of the stoichiometric powder. The secondary phase was observed at the surface of PbO-rich ceramics and was suggested to be a liquid phase expelled from inside the ceramic. A sintering scheme of PNiNb-PT-PZ ceramics was proposed, and the high sinterability of PNiNb-PT-PZ ceramics was attributed to the low formation temperature of the liquid phase. 相似文献
9.
Yang Gong-An Pu Yong-Ping Wang Jin-Fei Chen Xiao-Long Zhuang Yong-Yong 《Journal of the American Ceramic Society》2009,92(8):1891-1894
The influence of La2 O3 doped on the microstructure and dielectric properties, including the phase structure, temperature dependence of permittivity, and the hysteresis loop of BaTiO3 –Nb2 O5 –Fe2 O3 (BTNF) materials has been investigated in X-ray diffraction, SEM, and LCR analyzer, respectively. Experiments revealed that incorporation of proper content of La2 O3 basically soluted in the lattice of BaTiO3 and can control the grain-growth, reduce the dielectric loss of the BTNF materials. The development of microstructure promoted by the additives can result in the improvement of the dielectric constant. When the doping concentration of La2 O3 was 3.846 wt%, the relative dielectric constant of the sample sintered at 1280°C only for 2 h could reach 4308, and improve the dielectric-temperature characteristics markedly. As a result, a novel Y5P can be achieved in the BTNF ceramics, which is very promising for practical use in Y5P multilayer ceramic capacitors. 相似文献
10.
Xia Wang Wei Li Jin-lou Gu Yong-sheng Li Liang Li Jian-lin Shi 《Journal of the American Ceramic Society》2009,92(10):2412-2414
Li2.06 Nb0.18 Ti0.76 O3 powder has been successfully prepared at low temperatures via a facile and manageable, activated pretreatment on the inert raw Nb2 O5 . It is demonstrated that with triethanolamine, citric acid, and hydrogen peroxide, this simple pretreatment process could activate Nb2 O5 efficiently. Pure Li2 TiO3 solid solution phase was thus obtained by calcining the mixture of the activated Nb2 O5 , LiOH·H2 O, and Ti(C4 H9 O)4 at temperatures as low as 650°C, which is about 200°C lower than that of the traditional solid-state method. To the best of our knowledge, this temperature is the lowest one for preparing Li2 TiO3 solid solution. Additionally, the phase transformation and the morphology of the final powder are also discussed. 相似文献
11.
Mark I. Pownceby Keri K. Constanti-Carey Michael J. Fisher-White 《Journal of the American Ceramic Society》2003,86(6):975-980
Subsolidus phase equilibria in the system Fe2 O3 –Al2 O3 –TiO2 were investigated between 1000° and 1300°C. Quenched samples were examined using powder X-ray diffraction and electron probe microanalytical methods. The main features of the phase relations were: (a) the presence of an M3 O5 solid solution series between end members Fe2 TiO5 and Al2 TiO5 , (b) a miscibility gap along the Fe2 O3 –Al2 O3 binary, (c) an α-M2 O3 ( ss ) ternary solid-solution region based on mutual solubility between Fe2 O3 , Al2 O3 , and TiO2 , and (d) an extensive three-phase region characterized by the assemblage M3 O5 +α-M2 O3 ( ss ) + Cor( ss ). A comparison of results with previously established phase relations for the Fe2 O3 –Al2 O3 –TiO2 system shows considerable discrepancy. 相似文献
12.
TAKESHI KIKUCHT 《Journal of the American Ceramic Society》1977,60(3-4):148-150
The subsolidus phase equilibria in the system Bi2 O3 -TiO2 -Nb2 O5 at 1100°C were determined by solid-state reaction techniques and X-ray powder diffraction methods. The system was found to contain 4 ternary compounds, i.e. Bi3 TiNbO9 , Bi7 Ti4 NbO21 , a cubic pyrochlore solid solution having a compositional range of 3Bi2 O3 · x TiO2 (7– x )Nb2 O5 where x ranges from 2.3 to 6.75, and an unidentified phase, 4Bi2 O3 ·11TiO2 ·5Nb2 O5 . 相似文献
13.
Lamrath Abdul Khalam Sherin Thomas Mailadil T. Sebastian 《International Journal of Applied Ceramic Technology》2007,4(4):359-366
The columbites MgNb2 O6 , MgTa2 O6 , and corundum-type Mg4 Nb2 O9 ceramics were prepared by the conventional solid-state ceramic route. The structure and microstructure of the sintered samples were investigated by X-ray diffraction and scanning electron microscopic techniques. The microwave dielectric properties of the samples were measured by the resonance method in the frequency range 4–6 GHz. The dielectric properties have been tailored by forming a solid solution between MgNb2 O6 and MgTa2 O6 and by the substitution of TiO2 for Nb2 O5 in both MgNb2 O6 and Mg4 Nb2 O9 ceramics. The Mg(Nb0.7 Ta1.3 )O6 has ɛr =29, Q u × f =67 800 GHz, and τf =0.8 ppm/°C and the MgO–(0.4)Nb2 O5 –(1.5)TiO2 composition has ɛr =34.5, Q u × f =81 300 GHz, and τf =−2 ppm/°C. 相似文献
14.
The sintering characteristics and the reaction of additives with BaTiO3 (BT) were examined for two materials having Nb-rich composition (Comp.N) and Co-rich composition (Comp.C) to elucidate the relation between the stability of the core–shell microstructure and the Nb/Co ratio in the BT–Nb2 O5 –Co3 O4 system. TEM observation revealed that the concentration gradient of Nb and Co existed in the shell region although Nb and Co macroscopically distributed homogeneously. X-ray diffraction analysis showed that the shell formation preceded the densification and completed at about 1280°C for both Comp.N and Comp.C as determined from differential scanning calorimetry. A diffusion couple experiment disclosed that Co had a larger diffusivity than Nb and that the diffusion of Co was suppressed when the sample was codoped with a sufficient amount of Nb. On the basis of these experimental results, new mechanisms of the formation and collapse of core–shell structure in the BT–Nb2 O5 –Co3 O4 system were proposed. 相似文献
15.
Di Zhou Hong Wang Xi Yao Li-Xia Pang Huan-Fu Zhou 《Journal of the American Ceramic Society》2008,91(1):139-143
The high-energy ball-milling (HEM) method was used to synthesize the compositions of BiNbO4 , Bi5 Nb3 O15 , and Bi3 NbO7 in a Bi2 O3 –Nb2 O5 binary system. Reagent Bi2 O3 and Nb2 O5 were chosen as the starting materials. The X-ray diffraction patterns of the three compositions milled for different times were studied. Only the cubic Bi3 NbO7 phase, Nb2 O5 , and amorphous matters were observed in powders after being milled for 10 h. After heating at proper temperatures the amorphous matters disappeared and the proleptic phases of BiNbO4 and Bi5 Nb3 O15 could be obtained. The Scherrer formula was used to calculate the crystal size and the results of nanopowders are between 10 and 20 nm. The scanning electron microscopy photos of Bi3 NbO7 powders showed drastic aggregation, and the particle size was about 100 nm. The dielectric properties of ceramics sintered from the nanopowders prepared by HEM at 100–1 MHz and the microwave region were measured. Bi3 NbO7 ceramics showed a good microwave permittivity ɛr of about 80 and a Q × f of about 300 at 5 GHz. The triclinic phase of BiNbO4 ceramics reached its best properties with ɛr =24 and Q × f =14 000 GHz at about 8 GHz. 相似文献
16.
The phase diagrams in the Al2 O3 –Cr2 O3 and V2 O3 –Cr2 O3 systems have been assessed by thermodynamic modeling with existing data from the literature. While the regular and subregular solution models were used in the Al2 O3 –Cr2 O3 system to represent the Gibbs free energies of the liquid and solid phases, respectively, the regular solution model was applied to both phases in the V2 O3 –Cr2 O3 system. By using the liquidus, solidus, and/or miscibility gap data, the interaction parameters of the liquid and solid phases were optimized through a multiple linear regression method. The phase diagrams calculated from these models are in good agreement with experimental data. Also, the solid miscibility gap and chemical spinodal in the V2 O3 –Cr2 O3 system were estimated. 相似文献
17.
Jin-Ho Lee Masatomo Yashima Masato Kakihana Masahiro Yoshimura 《Journal of the American Ceramic Society》1998,81(4):894-900
The phase equilibria in the Y2 O3 -Nb2 O5 system have been studied at temperatures of 1500° and 1700°C in the compositional region of 0-50 mol% Nb2 O5 . The solubility limits of the C-type Y2 O3 cubic phase and the YNbO4 monoclinic phase are 2.5 (±1.0) mol% Nb2 O5 and 0.2 (±0.4) mol% Y2 O3 , respectively, at 1700°C. The fluorite (F) single phase exists in the region of 20.1-27.7 mol% Nb2 O5 at 1700°C, and in the region of 21.1-27.0 mol% Nb2 O5 at 1500°C, respectively. Conductivity of the Y2 O3 - x mol% Nb2 O5 system increases as the value of x increases, to a maximum at x = 20 in the compositional region of 0 ≤ x ≤ 20, as a result of the increase in the fraction of F phase. In the F single-phase region, the conductivity decreases in the region of 20-25 mol% Nb2 O5 , because of the decrease in the content of oxygen vacancies, whereas the conductivity at x = 27 is larger than that at x = 25. The conductivity decreases as the value of x increases in the region of 27.5 ≤ x ≤ 50, because of the decrease in the fraction of F. The 20 mol% Nb2 O5 sample exhibits the highest conductivity and a very wide range of ionic domain, at least up to log p O 2 =−20 (where p O 2 is given in units of atm), which indicates practical usefulness as an ionic conductor. 相似文献
18.
Matjaz Valant 《Journal of the American Ceramic Society》2009,92(4):955-958
Dielectric properties of pyrochlores compositions from Bi2 O3 –Nb2 O5 –NiO system were analyzed. The dielectric properties are dominated with a low-temperature relaxation that is typical for Bi-pyrochlores. A vast pyrochlore homogeneity range that exists in this system allowed to correlate characteristics of the observed relaxations with a compositional variations within the A2 O'- and B2 O6 pyrochlore sublattice. It was possible to make a distinction between different influences of the two sublattices, which can be satisfactorily described by the existing relaxation model for Bi3/2 ZnNb3/2 O7 . A new relaxor-like room temperature relaxation was found for Bi1.6 Ni0.57 Nb1.43 O6.55 . 相似文献
19.
The binary system Nb2 O5 — SiO2 has been shown to include an extensive two-liquid region over the range 5 to 80% Nb2 O5 . The minimum temperature of the two-liquid area is 1695°C. A eutectic composition occurs at 95% Nb2 O5 and 1448°C. and another at approximately 5% Nb2 O5 and 1695°C. The experimental results were obtained by the cone-fusion method. 相似文献
20.
Dielectric and piezoelectric properties of 0.02Pb(Y2/3 W1/3 )O3 0.98Pb(Zr0.52Ti0.48)O3 ceramics doped with additives (Nb2 O5 , La2 O3 , MnO2 , and Fe2 O3 ) were investigated. The grain sizes of these ceramics decreased with increasing amounts of additives. For additions of MnO2 and Fe2 O3 , dielectric losses decreased, while for Nb2 O5 and La2 O3 , these values increased. The maximum values of the mechanical quality factor Qm were found to be 956 and 975 for additions of 0.9 wt% Fe2 O3 and 0.7 wt% MnO2 , respectively, but donor dopants (Nb2 O5 and La2 O3 ) did not change the values of Qm . On the other hand, the piezoelectric constant d33 and the electromechanical coupling factor kp decreased with additions of MnO2 and Fe2 O3 , but improved with additions of Nb2 O5 and La2 O3 . 相似文献