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The crystal structure of lanthanum-modified lead magnesium niobates having composition (Pb1− x La x ) (Mg(1+ x )/3 -Nb(2− x )/3 )O3 with X = 0 to 1 was investigated by X-ray powder diffraction. It was found that the fundamental reflections from perovskite structure remain in the whole range of composition. The superlattice reflections from the A(B'1/2 -B"1/2 )O3 ordered structure are also well preserved for La content greater than 50 at.%; however, a series of extra peaks of mixing indices appears, with intensities gradually enhanced with the increase of La content. For the complete substitution of Pb by La, a splitting of some reflections can be observed in the diffraction pattern. The results indicate that the crystal structure evolves continuously with the La content, from disordered cubic perovskite of space group Pm 3 m for X = 0, to ordered cubic perovskite of space group Fm 3 m for X = 0.5, distorted cubic perovskite of space group Pa 3 for 0.5 < X < 0.9, and finally to a rhombohedral perovskite, possibly belonging to the space group R 3 , for X ≥ 0.9. In the evolution of structure, a linear reduction of the lattice constant of the perovskite cell from 4.048 to 3.964 Å was observed. 相似文献
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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
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Twenty hours of mechanical activation of mixed oxides at room temperature led to the formation of Pb(Mg1/3 Nb2/3 )O3 (PMN) in excess PbO. The crystallinity of the activation-derived perovskite PMN phase was further established when the activated PMN–PbO phase mixture was subjected to calcination at 800°C. Pyrochlores, such as Pb3 Nb4 O13 and Pb2 Nb2 O7 , were not observed as transitional phases on mechanical activation and subsequent calcination, although 50% excess PbO was deliberately added. The perovskite PMN phase was recovered by washing off excess PbO using acetic acid solution at room temperature. It was sintered to a relative density of 98.9% of theoretical at 1200°C for 1 h and the sintered PMN exhibited a dielectric constant of ∼14 000 at 100 Hz and a Curie temperature of −11°C. 相似文献
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P. Ravindranathan Sridhar Komarneni Rustum Roy 《Journal of the American Ceramic Society》1990,73(4):1024-1025
Lead magnesium niobate (PMN), Pb(Mg1/3 Nb2/3 )O3 , with perovskite structure has been prepared using structurally diphasic PMN gels. The diphasic gels were made using various concentrations of perovskite PMN seeds. The unseeded gel calcined at 775°C for 2 h gave ∼98% of perovskite PMN phase. The use of 1% PMN perovskite seed not only led to a pure perovskite phase but also lowered the crystallization temperature of these gels by about 75°C. These results show that isostructural seeding helps to lower the crystallization temperature of perovskite PMN phase. 相似文献
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Edward M. Sabolsky Gary L. Messing Susan Trolier-McKinstry 《Journal of the American Ceramic Society》2001,84(11):2507-2513
Single-crystal layers of 0.65Pb(Mg1/3 Nb2/3 )O3 ·0.35PbTiO3 (PMN-35PT) were grown heteroepitaxially on {001}-BaTiO3 template crystals. A {001}-BaTiO3 crystal was embedded in a fine-grained matrix of PMN-35PT containing excess PbO and heated between 950° and 1150°C for 0–5 h. The initial growth of the PMN-35PT on the {001} surface and the growth of the matrix grains both displayed a t 1/3 dependence which is characteristic of diffusion-controlled growth. Growth was limited to ∼100–150 μm due to the significantly reduced driving force at longer times because of matrix coarsening and porosity evolution. 相似文献
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Effect of Grain Coalescence on the Abnormal Grain Growth of Pb(Mg1/3 Nb2/3 )O3 -35 mol% PbTiO3 Ceramics
Ui-Jin Chung Jong-Keuk Park Nong-Moon Hwang Ho-Yong Lee Doh-Yeon Kim 《Journal of the American Ceramic Society》2002,85(4):965-968
Abnormal grain growth (AGG), which occurred during the heat treatment of Pb(Mg1/3 Nb2/3 )O3 -35 mol% PbTiO3 (PMN-35PT) with excess PbO, was investigated. AGG has been suggested to be the consequence of grain coalescence that results in the formation of Σ3 coincidence site lattice and low angle grain boundaries. Because of reentrant edges appearing at the ends of these boundaries, the coarsening rate of grains was significantly enhanced and AGG occurred. 相似文献
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Wen Gong Jing-Feng Li Xiangcheng Chu Longtu Li 《Journal of the American Ceramic Society》2004,87(6):1031-1034
Lead magnesium niobium titanate (PMNT) thin films with a composition near the morphotropic phase boundary were prepared on conventional Pt(111)/Ti/SiO2 /Si substrates using a modified sol-gel process. A PbO seeding layer was introduced to the interface between the PMNT layer and the substrate to enhance the [001]-preferential orientation of the PMNT film. Single-phase perovskite PMNT films with highly [001]-preferential orientation were obtained at reduced annealing temperatures compared with the PMNT films directly deposited on the same substrates. The dielectric and ferroelectric properties of the prepared PMNT films were evaluated as a function of annealing temperature. 相似文献
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Ui-Jin Chung Jong-Keuk Park Nong-Moon Hwang Ho-Yong Lee Doh-Yeon Kim 《Journal of the American Ceramic Society》2002,85(12):3076-3080
Pb(Mg1/3 Nb2/3 )O3 -35 mol% PbTiO3 (PMN-35PT) specimens with a 5 mol% excess PbO were prepared by excessive heat treatment at 1150°C to induce abnormal grain growth. Through electron backscatter diffraction analysis and the observation of a three-dimensional morphology, the abnormally grown PMN-35PT grains were found to be twinned crystals with penetration characteristics. The morphology of the PMN-35PT twinned crystal was crystallographically analyzed. The abnormal grain growth of PMN-35PT is suggested to be due to preferential growth at the reentrant angles formed by twins. 相似文献
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Polarization reversal and domain dynamics were investigated in 0.7Pb(Mg1/3 Nb2/3 )O3 ·0.3PbTiO3 using a method of current transients. Investigations were performed as a function of applied electric field. The kinetics of the transients were modeled to a stretched exponential-type function. 相似文献
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Palaniappan Ravindranathan Sridhar Komarneni Amar S. Bhalla Rustum Roy 《Journal of the American Ceramic Society》1991,74(12):2996-2999
A solution sol-gel method has been developed to prepare 0.9Pb(Mg1/3 Nb2/3 )O3 -0.1PbTiO3 (0.9PMN-0.1PT) ceramics. During the processing the gel first converted to cubic pyrochlore phase at a calcination temperature of 600°C followed by the formation of pure perovskite phase at 775°C. The ceramics sintered at 1250°C for 4 h showed ≈98% of the theoretical density. The room-temperature dielectric constant of the pellets sintered at 1250°C showed a maximum value of 25035 at 1 kHz. Sintering studies at different temperatures revealed that the dielectric constant increased with increasing grain size in these ceramics. 相似文献
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Lead zinc niobate–lead magnesium niobate–lead titanate (PZN–PMN–PT) ceramic powders of perovskite structure have been prepared via a mechanochemical processing route. A single-phase perovskite powder of ultrafine particles in the nanometer range was successfully synthesized when a MZN powder (columbite precursor) was mechanically activated for 10 h together with mixed lead and titanium oxides. The following steps are involved when the ternary oxide mixture is subjected to an increasing degree of mechanical activation. First, the starting materials are significantly refined in particle size as a result of the continuous deformation, fragmentation and then partially amorphized at the initial stage of mechanical activation. This is followed by the formation of perovskite nuclei and subsequent growth of these nuclei in the activated oxide matrix with increasing activation time. When calcined at various temperatures in the range of 500–800°C, pyrochlore phase was not detected by XRD phase analysis in the mechanochemically synthesized powder. Only a minor amount (∼2%) of pyrochlore phase was observed when the calcination temperature was raised to 850°C. The PZN–PMN–PT derived from the mechanochemically synthesized powder can be sintered to ∼98% relative density at a sintering temperature of 950°C. The PZN–PMN–PT sintered at 1100°C for 1 h exhibits a dielectric constant of ∼18 600 and a dielectric loss of 0.015 at the Curie temperature of 112°C when measured at a frequency of 0.1 kHz, together with a d 33 value of 323 ×10−12 pC/N. 相似文献
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John Gerard Fisher Min-Soo Kim Ho-Yong Lee Suk-Joong L. Kang 《Journal of the American Ceramic Society》2004,87(5):937-942
Abnormal grain growth in Pb(Mg1/3 Nb2/3 )O3 –35 mol% PbTiO3 (PMN-35PT) ceramics doped with Li2 O and PbO has been investigated. Replacing the PbO dopant with up to 2 mol% Li2 O caused an increase in the number of abnormal grains. For the composition containing 2 mol% Li2 O and 6 mol% PbO, the amount of abnormal grain growth decreased with increasing sintering temperature. Single crystals of ∼6 mm × 6 mm × 2 mm thickness were grown from the 2 mol% Li2 O, 6 mol% PbO-containing composition via the templated grain growth method. Grain growth behavior with temperature is explained in terms of the effect of Li2 O on interface-reaction-controlled grain growth and the critical driving force. 相似文献
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Jong-Keuk Park Ui-Jin Chung Nong M. Hwang Doh-Yeon Kim 《Journal of the American Ceramic Society》2001,84(12):3057-3059
The effect of spark plasma sintering (SPS) on the densification behavior of Pb(Mg1/3 Nb2/3 )O3 –PbTiO3 ceramics has been investigated. Specimens with a density of >99% of the theoretical density (TD) were obtained using SPS treatment at 900°C. Through normal sintering at 1200°C, however, the density of the specimen was only ∼92% of TD. 相似文献
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Microencapsulation of ceramic powders using metalloorganic stearate soaps was investigated as an economical means to increase solid-state reactivity of multicomponent mixtures. The specific system investigated was lead magnesium niobate (PMN); however, the process may be applicable to a wide range of other compositions. The physical and chemical characteristics of the unfired powder mixtures and reactivity during subsequent calcination were studied as a function of batch composition and mixing method. Batch composition was varied by molar substitution of magnesium stearate for magnesium carbonate. Mixing method was investigated by comparing a dry-mixing technique developed for particle coating (mechanofusion) with conventional wet ball milling. Both mixing processes resulted in surface coating of the ceramic particles by the stearate soap. In addition, the mechanofusion process produced densely packed spherical granules of coated particles (multicored microcapsules) in the 50- to 200-μm range. Solid-state reactivity was measured in terms of perovskite phase yield, increased yields being indicative of a more reactive mixture. The highest perovskite yields (95 to 98 vol%) were achieved at 100 mol% substitution of magnesium stearate for magnesium carbonate, independent of mixing method. However, when magnesium stearate was only partially substituted for magnesium carbonate, the mechanofusion process produced consistently higher perovskite yields than did ball milling. Compared to conventional mixed-oxide processing, the increased reactivity of the microencapsulated mixtures can be attributed to higher chemical activity of the metallo-organic precursor, finer scale of mixing achieved by particle coating, and a further reduction in segregation scale due to the dense intragranule packing of multicore microcapsules. 相似文献
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(Na1/2 La1/2 )(Mg1/3 Nb2/3 )O3 undergoes a series of phase transitions that involve cation order on the A- and B-sites of the parent perovskite structure. At high temperatures both sites contain a random distribution of cations; below 1275°C a 〈111〉 layering of Mg and Nb leads to the formation of a 1:2 ordered structure with a monoclinic supercell. A second transition was observed at 925°C, where the Na and La cations order onto alternate A-site positions along the 〈001〉 direction of the parent subcell. By quenching samples from above 1275°C to preserve the disorder on the B-site, a fourth variant of this compound was obtained by inducing A-site order through a subsequent anneal at 900°C. Although the changes in structure do not produce significant alterations in the relative permittivity (ɛr ∼ 35), they do have a significant effect on the value of the temperature coefficient of the capacitance. 相似文献
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The effects of lead content on the structure and electrical properties of Pb((Zn1/3 Nb2/3 )0.5 (Zr0.47 Ti0.53 )0.5 )O3 ceramics were investigated. Specimens with various lead concentrations were prepared by the conventional oxide-mixing method. When the lead concentration was slightly less than the stoichiometric amount, a large amount of pyrochlore phase was formed along with the perovskite phase. On the other hand, excessive amounts of lead led to the formation of PbO on the surface of the specimen. These second phases were seriously detrimental to electromechanical properties. The highest piezoelectric properties were observed when an excess of 1 mol% lead was added. By optimizing the specimen composition, excellent piezoelectric and dielectric properties ( k p = 0.7, d 33 = 490 pC/N, and ɛm = 15000) were obtained. 相似文献
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Marina Villegas Amador C. Caballero Carlos Moure Pedro Durán José F. Fernández Robert E. Newnham 《Journal of the American Ceramic Society》2000,83(1):141-46
Pb(Zn1/3 Nb2/3 )O3 -based ceramics have been prepared by two different processing methods: conventional (PZN-C) and reaction-sintering (PZN-RS). The conventionally prepared PZN-based ceramics densified at lower temperatures (950°C) than the reaction-sintered samples (1100°C), but the perovskite/pyrochlore ratio was always higher in PZN-RS. The presence of a substantial amount of pyrochlore phase in PZN-C ceramics caused a decrease in the electrical properties. The maximum dielectric constant values in PZN-C ceramics were 10%–15% lower than those of PZN-RS, despite a similar average grain size, 7 ± 0.2 μm. The temperature of the maximum of the dielectric constant ( T max ) was lower than that expected from the mixing rule because of the possible formation of Ba–Nb clusters. The higher chemical homogeneity in PZN-RS ceramics is the main reason for the higher dielectric constant, T max and electromechanical response, as well as for the lower difference between T max and the depolarization temperature ( T d ) and the lower diffusiveness parameter (δ). 相似文献
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Seiji Shinohara Jong-Gab Baek Tetsuhiko Isobe Mamoru Senna 《Journal of the American Ceramic Society》2000,83(12):3208-3210
Phase-pure perovskite Pb(Zn x Mg1– x )1/3 Nb2/3 O3 solid solution (PZ x M1– x N) is obtained for x ≦ 0.7 by heating a milled stoichiometric mixture of PbO, Mg(OH)2 , Nb2 O5 , and 2ZnCO3 ·3Zn(OH)2 ·H2 O at 1100°C for 1 h. Percent perovskite ( f P ) with respect to total crystalline phase decreases with increasing temperature of subsequent heating then increases to 900°C for the mixtures where x ≦ 0.8 and milled for 3 h. For mixtures with x = 0.9 and x = 1, f P decreases monotonically. Curie temperature increases almost linearly with increasing x up to x = 0.7. The maximum dielectric constant at 1 kHz is 2×104 and 1.7×104 for the mixture with x = 0.4 and x = 0.7, respectively. The stabilization mechanism of strained perovskite is discussed. 相似文献