环保型BaTiO_3基陶瓷介质的掺杂与介电性能的研究
摘要
本文以具有钙钛矿结构的BaTiO_3基陶瓷作为研究对象,分别研究了Sm_2O_3掺杂对(BaxSr1-x)TiO_3、Ba(Sn_xTi_(1-x))O_3和Ba(ZrxTi1-x)O_3陶瓷微观结构与介电性能的影响,以及Y_2O_3和NiO掺杂对(Ba_xSr1-x)TiO_3陶瓷微观结构与介电性能的影响。通过对试样微观结构和介电特性的研究,揭示了Sm_2O_3、Y_2O_3和NiO在BaTiO_3基陶瓷中的掺杂机理。研究结果发现:
Sm_2O_3和Y_2O_3在(Ba_xSr_(1-x))TiO_3陶瓷中,随着掺杂量的增加,Sm~(3+)和Y~(3+)有一个优先取代位置,也就是在它们掺杂的起始阶段,Sm~(3+)和Y~(3+)主要进入晶格A位位置,而在其掺杂量超过某个量之后,则以进入晶格B位位置为主,这种优先取代结果导致试样晶胞参数a随掺杂量的增加先减小后增大,试样介电常数先增大后减小。两者都能使试样介电损耗得到改善,尤其是当Y~(3+)掺杂量为1.0 mol%时,试样介电损耗降低到0.0015。两者掺杂结果的显著不同在于Y~(3+)掺杂使试样表现出了弥散相变特性,而Sm~(3+)掺杂却没有。
当NiO被添加到(BaxSr1-x)TiO_3陶瓷中时,只有一少部分Ni~(2+)离子进入晶格的B位取代Ti4+离子,导致试样晶格参数轻微增加,之后NiO主要在晶界附近聚集,形成BST/NiO复合材料。试样介电常数随NiO掺杂量的增加而下降,介电温谱显示含Ni试样具有弥散相变特性,且随掺杂量的增加,效果越明显,这也使试样介电温谱得到了很大改善。
Sm_2O_3的加入并不改变BTS10和BZT20陶瓷的主晶相结构,与空白试样相比,掺杂微量Sm~(3+)会使晶粒尺寸下降。随着Sm_2O_3掺杂量的增加,BTS10和BZT20陶瓷试样介电常数先增大后减小,当试样介电常数最大时,其介电损耗也最高。BTS10和BZT20陶瓷试样Tm和Sm_2O_3掺杂量之间的变化规律大致相似,不同点在于BTS10陶瓷的Tm在Sm_2O_3掺杂起始阶段并不改变。
掺杂Sm_2O_3的BTS10和BZT20陶瓷试样均具有弥散相变特性,但二者有两点明显不同,其一,BTS10空白试样本身并不具有弥散相变特性,而BZT20空白试样即具有弥散相变特性。其二,随Sm_2O_3掺杂量的增加,BTS10陶瓷试样弥散特性一致增强,而BZT20陶瓷试样弥散特性却是先变弱后增强。这种差别说明,在Sm_2O_3掺杂起始阶段,一部分Sm~(3+)进入了BTS10陶瓷晶格B位位置,而在BZT20陶瓷中却没有,而两者试样Tm在Sm_2O_3掺杂起始阶段变化的差异性也说明了这一点。
The effects of Sm_2O_3, Y_2O_3 and NiO on microstructure and dielectric properties in BaTiO_3-based ceramics are investigated, respectively. Based on the effects of Sm~(3+), Y~(3+), and Ni~(2+) on the microstructure and dielectric properties, the substitution mechanism of Sm~(3+), Y~(3+), and Ni~(2+) in BaTiO_3-based ceramics is also investigated and discussed, respectively. The research achievements are as follows:
There is an alternation of substitution preference of Sm~(3+) and Y~(3+) for the host cations in perovskite lattice, that is, Sm~(3+) and Y~(3+) enter the A site in perovskite lattice at first, then they enter the B site when the additive amount of Sm~(3+) and Y~(3+) exceed some value. Owing to the substitution preference, the crystal cell a and dielectric constant rise at first, if the amount continues increasing, they will decrease. Both Sm~(3+) and Y~(3+) can improve the dissipation factor, especially, the optimized dissipation factor is 0.0015 for 1.0 mol%-Y~(3+)-doped samples, making it a superior candidate material for applications. There is an obvious distinction for the effects on dielectric properties between Sm~(3+) and Y~(3+), that is, the Y~(3+), not Sm~(3+), makes the BST ceramics exhibit the diffuse phase transition.
It is also found that Ni~(2+) can enter the B site in ABO_3 perovskite at first, making the crystal cell a rise, whereafter, Ni~(2+) ions most segregate on the grain boundaries to inhabit the grain growth, forming the BST/NiO composites. Due to the decrease of grain size and the impurity, the dielectric constants are decreased. It is concluded that the diffuse phase transition is linked to the adulteration of Ni~(2+), and the diffuse phase transition increases with the doping level increasing, leading to that the peaks of dielectric constants become slower and flatter.
The results indicate that the crystal structures are perovskite phase for all of the examined samples in BTS10 and BZT20 ceramics, however, contrasting to the blank sample, the grain size of the sample with Sm_2O_3 addition is decreased. Owing to the substitution of Sm~(3+), the dielectric constant rises at first, if the amount continues increasing, it will decrease, in the mean time, the dissipation factor also comes to its maximum when the dielectric constant is the highest. The relation between Tm and the concentration of Sm_2O_3 has some similarity except that Tm does not move in BTS10 ceramics at first, resulting from a handful of Sm~(3+) entering into the B site.
All of the samples exhibit the diffuse phase transition with Sm_2O_3 addition, however, there are two obvious distinction among BTS10 and BZT20 ceramics. First, the blank sample of BTS10 has no diffuse phase transition in nature, the samples of BTS10 can exhibit diffuse phase transition only when the Sm~(3+) ions are added, on the contrary, the blank sample of BZT20 possesses the diffuse phase transition in nature. Second, the diffuse phase transition congruously increases with the level of the Sm~(3+) doping increasing in BTS10 ceramics, however, the diffuse phase transition lowers in the beginning in BZT20 ceramics, if the amount continues increasing, it will increase, which demonstrated that a handful of Sm~(3+) ions have entered into the B site in BTS10 ceramics but not in BZT20 ceramics in the beginning, proved by the distinction of the relation between Tm and the concentration of Sm_2O_3 at first.
Sm_2O_3和Y_2O_3在(Ba_xSr_(1-x))TiO_3陶瓷中,随着掺杂量的增加,Sm~(3+)和Y~(3+)有一个优先取代位置,也就是在它们掺杂的起始阶段,Sm~(3+)和Y~(3+)主要进入晶格A位位置,而在其掺杂量超过某个量之后,则以进入晶格B位位置为主,这种优先取代结果导致试样晶胞参数a随掺杂量的增加先减小后增大,试样介电常数先增大后减小。两者都能使试样介电损耗得到改善,尤其是当Y~(3+)掺杂量为1.0 mol%时,试样介电损耗降低到0.0015。两者掺杂结果的显著不同在于Y~(3+)掺杂使试样表现出了弥散相变特性,而Sm~(3+)掺杂却没有。
当NiO被添加到(BaxSr1-x)TiO_3陶瓷中时,只有一少部分Ni~(2+)离子进入晶格的B位取代Ti4+离子,导致试样晶格参数轻微增加,之后NiO主要在晶界附近聚集,形成BST/NiO复合材料。试样介电常数随NiO掺杂量的增加而下降,介电温谱显示含Ni试样具有弥散相变特性,且随掺杂量的增加,效果越明显,这也使试样介电温谱得到了很大改善。
Sm_2O_3的加入并不改变BTS10和BZT20陶瓷的主晶相结构,与空白试样相比,掺杂微量Sm~(3+)会使晶粒尺寸下降。随着Sm_2O_3掺杂量的增加,BTS10和BZT20陶瓷试样介电常数先增大后减小,当试样介电常数最大时,其介电损耗也最高。BTS10和BZT20陶瓷试样Tm和Sm_2O_3掺杂量之间的变化规律大致相似,不同点在于BTS10陶瓷的Tm在Sm_2O_3掺杂起始阶段并不改变。
掺杂Sm_2O_3的BTS10和BZT20陶瓷试样均具有弥散相变特性,但二者有两点明显不同,其一,BTS10空白试样本身并不具有弥散相变特性,而BZT20空白试样即具有弥散相变特性。其二,随Sm_2O_3掺杂量的增加,BTS10陶瓷试样弥散特性一致增强,而BZT20陶瓷试样弥散特性却是先变弱后增强。这种差别说明,在Sm_2O_3掺杂起始阶段,一部分Sm~(3+)进入了BTS10陶瓷晶格B位位置,而在BZT20陶瓷中却没有,而两者试样Tm在Sm_2O_3掺杂起始阶段变化的差异性也说明了这一点。
The effects of Sm_2O_3, Y_2O_3 and NiO on microstructure and dielectric properties in BaTiO_3-based ceramics are investigated, respectively. Based on the effects of Sm~(3+), Y~(3+), and Ni~(2+) on the microstructure and dielectric properties, the substitution mechanism of Sm~(3+), Y~(3+), and Ni~(2+) in BaTiO_3-based ceramics is also investigated and discussed, respectively. The research achievements are as follows:
There is an alternation of substitution preference of Sm~(3+) and Y~(3+) for the host cations in perovskite lattice, that is, Sm~(3+) and Y~(3+) enter the A site in perovskite lattice at first, then they enter the B site when the additive amount of Sm~(3+) and Y~(3+) exceed some value. Owing to the substitution preference, the crystal cell a and dielectric constant rise at first, if the amount continues increasing, they will decrease. Both Sm~(3+) and Y~(3+) can improve the dissipation factor, especially, the optimized dissipation factor is 0.0015 for 1.0 mol%-Y~(3+)-doped samples, making it a superior candidate material for applications. There is an obvious distinction for the effects on dielectric properties between Sm~(3+) and Y~(3+), that is, the Y~(3+), not Sm~(3+), makes the BST ceramics exhibit the diffuse phase transition.
It is also found that Ni~(2+) can enter the B site in ABO_3 perovskite at first, making the crystal cell a rise, whereafter, Ni~(2+) ions most segregate on the grain boundaries to inhabit the grain growth, forming the BST/NiO composites. Due to the decrease of grain size and the impurity, the dielectric constants are decreased. It is concluded that the diffuse phase transition is linked to the adulteration of Ni~(2+), and the diffuse phase transition increases with the doping level increasing, leading to that the peaks of dielectric constants become slower and flatter.
The results indicate that the crystal structures are perovskite phase for all of the examined samples in BTS10 and BZT20 ceramics, however, contrasting to the blank sample, the grain size of the sample with Sm_2O_3 addition is decreased. Owing to the substitution of Sm~(3+), the dielectric constant rises at first, if the amount continues increasing, it will decrease, in the mean time, the dissipation factor also comes to its maximum when the dielectric constant is the highest. The relation between Tm and the concentration of Sm_2O_3 has some similarity except that Tm does not move in BTS10 ceramics at first, resulting from a handful of Sm~(3+) entering into the B site.
All of the samples exhibit the diffuse phase transition with Sm_2O_3 addition, however, there are two obvious distinction among BTS10 and BZT20 ceramics. First, the blank sample of BTS10 has no diffuse phase transition in nature, the samples of BTS10 can exhibit diffuse phase transition only when the Sm~(3+) ions are added, on the contrary, the blank sample of BZT20 possesses the diffuse phase transition in nature. Second, the diffuse phase transition congruously increases with the level of the Sm~(3+) doping increasing in BTS10 ceramics, however, the diffuse phase transition lowers in the beginning in BZT20 ceramics, if the amount continues increasing, it will increase, which demonstrated that a handful of Sm~(3+) ions have entered into the B site in BTS10 ceramics but not in BZT20 ceramics in the beginning, proved by the distinction of the relation between Tm and the concentration of Sm_2O_3 at first.
引文
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