烧结温度和CaTiO3添加对不稳定层状Can+1TinO3n+1 (n = 1)陶瓷体系结构与介电性能的影响

doi:10.15541/jim20160426

摘要/Abstract

摘要：

采用固相反应法制备了Ca₂TiO₄+xwt% CaTiO₃(x=0、0.8、1.6和3.2)陶瓷, 并分析了其相组成与结构、显微结构、烧结温度和微波介电性能之间的影响关系。室温XRD晶体结构分析表明: 未掺杂CaTiO₃的Ca₂TiO₄体系主晶相受烧结温度的影响明显, 由1400℃烧结的正交结构CaTiO₃相转变为1420℃烧结的四方结构层状Ca₃Ti₂O₇相。当烧结温度由1420℃升高至1450℃时, 不同含量CaTiO₃掺杂均能使Ca₂TiO₄体系中主晶相的含量和成分发生改变。其中, 1.6wt%~3.2wt%的CaTiO₃掺杂可使Ca₂TiO₄体系获得稳定且含量较高的Ca₃Ti₂O₇相。微波介电性能测试结果显示, 未掺杂的Ca₂TiO₄体系的ε_r、Q×f和τ_f值均在其主晶相发生改变时大幅降低, 分别由1400℃烧结的85.84、10030 GHz和508.87×10^-6/℃降至1420℃烧结的59.04、2340 GHz和93.13×10^-6/℃, 而不同含量的CaTiO₃掺杂则可在一定范围内稳定复相Ca₂TiO₄体系的Q×f值。

关键词: 层状钙钛矿, Ca2TiO4, 微波介电性能, CaTiO3

Abstract:

Ca₂TiO₄+xwt% CaTiO₃ (x=0, 0.8, 1.6 and 3.2) ceramics were prepared by solid state reaction technique. The relation between phase compositions and structures, microstructures, sintering temperatures, and microwave dielectric properties of these ceramic systems were accordingly studied. XRD patterns revealed that the main phase of the undoped CaTiO₃in Ca₂TiO₄ceramic systems was closely related with the sintering temperature, and the crystal phase transited from the orthorhombic CaTiO₃ phase (as sintered at 1400℃) to tetragonal Ca₃Ti₂O₇phase (as sintered at 1420℃). In addition, the CaTiO₃-doping in various amounts resulted in the change of main phase with the sintering temperature increasing from 1420℃ to 1450℃. Wherein, the stability and high-content Ca₃Ti₂O₇phase could be obtained by doping 1.6wt%-3.2wt% CaTiO₃. The microwave dielectric properties test showed that the undoped Ca₂TiO₄multiphase systems got a great reduction in the ε_r, Q×f and τ_f values from 59.04, 2340 GHz and 93.13×10^-6/℃ (as sintered at 1400℃) to 59.04, 2340 GHz and 93.13×10^-6/℃ (as sintered at 1420℃), respectively. Additionally, the various amounts of CaTiO₃-doping could keep the Q×f values stably to some extent for the Ca₂TiO₄ceramic systems.

Key words: layered perovskite, Ca2TiO4, microwave dielectric properties, CaTiO3

中图分类号:

TM277

刘飞, 黄先培, 袁昌来, 陈国华. 烧结温度和CaTiO₃添加对不稳定层状Ca_n₊₁Ti_nO₃_n+₁(n = 1)陶瓷体系结构与介电性能的影响[J]. 无机材料学报, 2017, 32(5): 489-494.

LIU Fei, HUANG Xian-Pei, YUAN Chang-Lai, CHEN Guo-Hua. Influence of Sintering Temperature and CaTiO₃ Doping on Structure and Dielectric Properties for Instability Layered Ca_n₊₁Ti_nO₃_n+₁(n = 1) Ceramics[J]. Journal of Inorganic Materials, 2017, 32(5): 489-494.

图/表 5

图1 不同温度烧结的Ca2TiO4体系及1420℃、1450℃烧结Ca2TiO4+xwt% CaTiO3样品的XRD图谱

Fig. 1 (a) XRD patterns of Ca2TiO4 systems specimens sintered at different temperatures and Ca2TiO4+xwt% CaTiO3 sintered at 1420℃, (b) XRD patterns of Ca2TiO4+xwt% CaTiO3 specimens sintered at 1450℃

图2 在不同温度烧结4 h的Ca2TiO4+ xwt% CaTiO3(x=0、0.8和3.2)样品的背散射图片

Fig. 2 Back scattered electron images of Ca2TiO4+xwt% CaTiO3 (x=0, 0.8 and 3.2) ceramics sintered at different temperatures for 4 h

图3 1400℃烧结4 h的Ca2TiO4陶瓷样品的EDS面扫描图像

Fig. 3 EDS scan images of Ca2TiO4 system ceramics sintered at 1400℃ for 4 h

图4 1450℃烧结4 h的3.2wt%CaTiO3掺杂Ca2TiO4样品表面的EDS区域扫描图谱

Fig. 4 EDS graphs of region‘A’ and region‘B’ from the surface of Ca2TiO4+xwt% CaTiO3 (x=3.2) ceramics sintered at 1450℃ for 4 h

图5 Ca2TiO4+xwt% CaTiO3(x=0、0.8、1.6和3.2)样品的εr、Q×f和τf值随烧结温度的变化

Fig. 5 (a) εr, τf and (b) Q×f values of Ca2TiO4+xwt% CaTiO3 (x=0, 0.8, 1.6 and 3.2) ceramics as functions of sintering temperatures

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烧结温度和CaTiO₃添加对不稳定层状Ca_n₊₁Ti_nO₃_n+₁(n = 1)陶瓷体系结构与介电性能的影响

Influence of Sintering Temperature and CaTiO₃ Doping on Structure and Dielectric Properties for Instability Layered Ca_n₊₁Ti_nO₃_n+₁(n = 1) Ceramics

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