LuFe_2O_4及LuFeO_3基陶瓷的结构与多铁性
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摘要
由于其丰富的物理内涵与诱人的潜在应用,同时具有磁性与铁电性的多铁性材料正越来越受到广泛关注。本学位论文系统研究了LuFe2O4与LuFeO3基陶瓷的晶体结构、介电、铁电及磁学性能,并探讨其可能的多铁性机制,获得如下主要结论：
采用真空反应烧结法可控制备出致密的单相LuFe2O4陶瓷,其在室温下为菱方结构,空间群是R3m。LuFe2O4陶瓷在175-275K间存在一个激活能为0.29eV的类Debye介电弛豫,可归结于Fe2+与Fe3+离子之间的电子涨落作用。LuFe2O4陶瓷的亚铁磁转变温度为250K,温度约216K时发生玻璃态转变。室温下存在的非线性磁滞回线说明LuFe2O4在奈耳温度以上存在一定的弱铁磁性。LuFe2O4陶瓷经磁化处理后的介电常数在室温附近有明显下降,显示了明显的磁介电效应。然而,由于漏电流较大,LuFe2O4陶瓷在室温下难以测出可信的电滞回线。
通过Mg2+置换Fe2+得到LuFeMgO4,其晶体结构与LuFe2O4-一致。LuFeMgO4陶瓷的反铁磁转变温度为27K,远低于LuFe2O4的磁转变温度,这可归结为非磁性的Mg2+离子置换磁性的Fe2+离子后引起的磁稀释作用。在Fe-O双层中Fe和O原子为非完全共面排列,导致LuFeMgO4在10K时出现宏观净磁化。LuFeMgO4陶瓷在240-420K温度范围内存在一个明显的介电弛豫,主要源于Fe2+与Fe3+离子之间的电荷跃迁。由于Mg2+离子的存在阻碍了电子的传递,其激活能的值比LuFe2O4要略大。经氧气氛热处理后介电弛豫受到明显的抑制,表明氧空位对LuFeMgO4陶瓷的介电弛豫有非常重要的影响。
通过Cu2+置换Fe2+得到LuFeCuO4,其晶体结构与LuFe2O4及LuFeMgO4类似。LuFeCuO4陶瓷在250-415K间存在一个明显的介电弛豫,其激活能为0.37eV,与LuFe2O4及LuFeMgO4中介电弛豫的激活能较为接近,说明Fe3+/Fe2+及Fe3+/Cu2+离子之间的有序作用对LuFeCuO4的介电行为有重要影响。在LuFe2O4、 LuFeCuO4及LuFeMgO4中,随着二价离子自旋磁矩的降低,磁转变温度逐渐下降,在LuFeCuO4陶瓷中,其反铁磁转变温度为57K。与LuFe2O4相比,LuFeCuCU陶瓷剩余极化较弱,表明Cu2+离子抑制了体系的铁电性。在室温下,LuFeCuO4陶瓷具有显著的磁介电效应,在磁场12kOe,频率10kHz下介电常数变化～7%。
LuFeO3在室温下为正交扭转的钙钛矿结构,空间群为Pbnm。LuFeO3陶瓷在140-250K及350-500K温度范围内存在两个明显的类Debye介电弛豫,其激活能分别为0.21eV及0.76eV。低温介电弛豫可能源自体系中Fe2+和Fe3+离子之间的电荷跃迁,而高温介电弛豫则与氧空位等缺陷密切相关。LuFeO3陶瓷的反铁磁转变温度为628K,低于该温度时可观测到弱铁磁性的存在,这是由于Fe自旋结构的排列存在一定的倾斜。在室温下,LuFeO3陶瓷具有明显的电滞回线,且其电极化在经过磁化处理后有明显的增大,表明磁性与铁电性之间可能存在耦合作用。室温下可观察到LuFeO3陶瓷中微弱的磁介电效应,进一步说明了其多铁性的存在。
LuFe0.95Mn0.05O3陶瓷在室温下的晶体结构与LuFeO3一致。在360-530间存在与LuFeO3中的高温介电弛豫相似的介电弛豫,主要源自氧空位的贡献。与LuFeO3相比,LuFe0.95Mn0.05O3陶瓷在室温下的铁电性有一定程度的削弱,说明了Fe2+和Fe3+电荷有序对LuFeO3铁电性的贡献以及Mn置换对电荷有序的破坏作用。LuFe0.95Mn0.05O5陶瓷的反铁磁转变温度为601K,比LuFeO3略低,这是由于Mn3+-O-Mn3+以及Fe3+-O-Mn3+反铁磁交换作用比Fe3+-O-Fe3+交换作用弱。低温下,具有强各向异性能的Mn3+离子对体系的磁各向异性占主导作用,导致LuFe0.95Mn0.05O3在温度约108K时发生自旋重取向。
Recently, multiferroic materials that combine at least two ferroic parameters have attracted remarkable interest due to the rich physical contents and the great potential applications in smart and multifunctional devices. In the present thesis, the crystal structure, dielectric, ferroelectric and magnetic properties of LuFe2O4and LuFeO3-based ceramics were investigated systematically. Moreover, the possible multiferroic characteristics in these ceramics were discussed. The following primary conclusions were obtained.
Single-phase LuFe2O4could be obtained under vacuum environment and the crystal structure was identified to be rhombohedral in space group R3m. An obvious dielectric relaxation with activation energy of0.29eV was observed between175K and275K, which was ascribed to the electron hopping between Fe2+and Fe3+ions. The Neel temperature of the present ceramics was-250K, and a re-entrant spin glass transition was indicated at-216K. The nonlinear M-H hysteresis loop indicated weak ferromagnetic characteristics at room temperature. Meanwhile, a remarkable decrease appeared in the dielectric constant of the as-magnetized sample, implying the magnetodielectric effect in the LuFe2O4ceramics. No convincing ferroelectric hysteresis could be obtained in LuFe2O4ceramics at room temperatrure, which might be caused by high leakage.
LuFeMgO4, which was isomorphous to LuFe2O4, was indentified to be antiferromagnetic with a Neel temperature of27K. The slim hysteresis loop measured at10K demonstrated the weak ferromagnetic or ferrimagnetism ordering in LuFeMgO4ceramics, which might be attributed to the canting angle in Fe moment. An obvious Debye-type dielectric relaxation with an activation energy of0.35eV was observed between240and420K. The replacement of Mg2+caused the suppression of electron transfer, resulting a larger activation energy than that of LuFe2O4. The dielectric relaxation could be strongly suppressed by oxygen annealing, indicating that oxygen vacancies played an essential role in the dielectric response of LuFeMgO4ceramics.
The crystal structure of LuFeCuO4was similar with those of LuFe2O4and LuFeMgO4. An obvious dielectric relaxation with activation energy0.37eV was observed between250and415K, which could be ascribed to the electron hopping between the ions on Fe sites. With the decrease of spin moments of the divalent ions, the values of TN became smaller in the order of LuFe2O4, LuFeCuO4(TN～57K) and LuFeMgO4. A P-E hysteresis loop was observed in LuFeCuO4ceramics at150K, and the replacement of Cu2+resulted in the weaker ferroelectricity than LuFe2O4. At room temperature, remarkable magnetodielectric response (～7%) was observed in LuFeCuO4ceramics.
LuFeO3was identified to be an orthorhombically distorted perovskite structure with space group Pbnm. Two Debye-type dielectric relaxations were observed in LuFeO3ceramics. The low temperature relaxation was originated from the electron hopping between Fe2+and Fe3+ions, while the high temperature relaxation was related with oxygen vacancies. The Neel temperature for LuFeO3was628K, and the weak ferromagnetic characteristics owing to the canting angle of magnetic spins were detected at room temperature. Obvious ferroelectric loops were observed at room temperature, and the values of electric polarization increased with an applied external magnetic field. Meanwhile, room-temperature magnetodielectric effect was detected, and LuFeO3was expected as a promising candidate for new multiferroic materials.
In LuFeO3, partially substituting Mn for Fe did not change the crystal structure. The low temperature dielectric relaxation was suppressed and only one dielectric anomaly around360-530K was observed in LuFe0.95Mn0.05O3ceramics. The smaller polarization compared with LuFeO3suggested the important role of electron hopping between Fe2-and Fe3+ions in ferroelectricity. The results of thermal analysis indicated that the Neel temperature decreased with Mn-substitution, which could be ascribed to the weaker Fe3+-O-Mn3+and Mn3+-O-Mn3+exchange interactions compared with Fe3+-O-Fe3+interaction. Due to the strong anisotropy of Mn3+ions, a spin reorientation transition could be induced in LuFeo.95Mno.05O3.
采用真空反应烧结法可控制备出致密的单相LuFe2O4陶瓷,其在室温下为菱方结构,空间群是R3m。LuFe2O4陶瓷在175-275K间存在一个激活能为0.29eV的类Debye介电弛豫,可归结于Fe2+与Fe3+离子之间的电子涨落作用。LuFe2O4陶瓷的亚铁磁转变温度为250K,温度约216K时发生玻璃态转变。室温下存在的非线性磁滞回线说明LuFe2O4在奈耳温度以上存在一定的弱铁磁性。LuFe2O4陶瓷经磁化处理后的介电常数在室温附近有明显下降,显示了明显的磁介电效应。然而,由于漏电流较大,LuFe2O4陶瓷在室温下难以测出可信的电滞回线。
通过Mg2+置换Fe2+得到LuFeMgO4,其晶体结构与LuFe2O4-一致。LuFeMgO4陶瓷的反铁磁转变温度为27K,远低于LuFe2O4的磁转变温度,这可归结为非磁性的Mg2+离子置换磁性的Fe2+离子后引起的磁稀释作用。在Fe-O双层中Fe和O原子为非完全共面排列,导致LuFeMgO4在10K时出现宏观净磁化。LuFeMgO4陶瓷在240-420K温度范围内存在一个明显的介电弛豫,主要源于Fe2+与Fe3+离子之间的电荷跃迁。由于Mg2+离子的存在阻碍了电子的传递,其激活能的值比LuFe2O4要略大。经氧气氛热处理后介电弛豫受到明显的抑制,表明氧空位对LuFeMgO4陶瓷的介电弛豫有非常重要的影响。
通过Cu2+置换Fe2+得到LuFeCuO4,其晶体结构与LuFe2O4及LuFeMgO4类似。LuFeCuO4陶瓷在250-415K间存在一个明显的介电弛豫,其激活能为0.37eV,与LuFe2O4及LuFeMgO4中介电弛豫的激活能较为接近,说明Fe3+/Fe2+及Fe3+/Cu2+离子之间的有序作用对LuFeCuO4的介电行为有重要影响。在LuFe2O4、 LuFeCuO4及LuFeMgO4中,随着二价离子自旋磁矩的降低,磁转变温度逐渐下降,在LuFeCuO4陶瓷中,其反铁磁转变温度为57K。与LuFe2O4相比,LuFeCuCU陶瓷剩余极化较弱,表明Cu2+离子抑制了体系的铁电性。在室温下,LuFeCuO4陶瓷具有显著的磁介电效应,在磁场12kOe,频率10kHz下介电常数变化～7%。
LuFeO3在室温下为正交扭转的钙钛矿结构,空间群为Pbnm。LuFeO3陶瓷在140-250K及350-500K温度范围内存在两个明显的类Debye介电弛豫,其激活能分别为0.21eV及0.76eV。低温介电弛豫可能源自体系中Fe2+和Fe3+离子之间的电荷跃迁,而高温介电弛豫则与氧空位等缺陷密切相关。LuFeO3陶瓷的反铁磁转变温度为628K,低于该温度时可观测到弱铁磁性的存在,这是由于Fe自旋结构的排列存在一定的倾斜。在室温下,LuFeO3陶瓷具有明显的电滞回线,且其电极化在经过磁化处理后有明显的增大,表明磁性与铁电性之间可能存在耦合作用。室温下可观察到LuFeO3陶瓷中微弱的磁介电效应,进一步说明了其多铁性的存在。
LuFe0.95Mn0.05O3陶瓷在室温下的晶体结构与LuFeO3一致。在360-530间存在与LuFeO3中的高温介电弛豫相似的介电弛豫,主要源自氧空位的贡献。与LuFeO3相比,LuFe0.95Mn0.05O3陶瓷在室温下的铁电性有一定程度的削弱,说明了Fe2+和Fe3+电荷有序对LuFeO3铁电性的贡献以及Mn置换对电荷有序的破坏作用。LuFe0.95Mn0.05O5陶瓷的反铁磁转变温度为601K,比LuFeO3略低,这是由于Mn3+-O-Mn3+以及Fe3+-O-Mn3+反铁磁交换作用比Fe3+-O-Fe3+交换作用弱。低温下,具有强各向异性能的Mn3+离子对体系的磁各向异性占主导作用,导致LuFe0.95Mn0.05O3在温度约108K时发生自旋重取向。
Recently, multiferroic materials that combine at least two ferroic parameters have attracted remarkable interest due to the rich physical contents and the great potential applications in smart and multifunctional devices. In the present thesis, the crystal structure, dielectric, ferroelectric and magnetic properties of LuFe2O4and LuFeO3-based ceramics were investigated systematically. Moreover, the possible multiferroic characteristics in these ceramics were discussed. The following primary conclusions were obtained.
Single-phase LuFe2O4could be obtained under vacuum environment and the crystal structure was identified to be rhombohedral in space group R3m. An obvious dielectric relaxation with activation energy of0.29eV was observed between175K and275K, which was ascribed to the electron hopping between Fe2+and Fe3+ions. The Neel temperature of the present ceramics was-250K, and a re-entrant spin glass transition was indicated at-216K. The nonlinear M-H hysteresis loop indicated weak ferromagnetic characteristics at room temperature. Meanwhile, a remarkable decrease appeared in the dielectric constant of the as-magnetized sample, implying the magnetodielectric effect in the LuFe2O4ceramics. No convincing ferroelectric hysteresis could be obtained in LuFe2O4ceramics at room temperatrure, which might be caused by high leakage.
LuFeMgO4, which was isomorphous to LuFe2O4, was indentified to be antiferromagnetic with a Neel temperature of27K. The slim hysteresis loop measured at10K demonstrated the weak ferromagnetic or ferrimagnetism ordering in LuFeMgO4ceramics, which might be attributed to the canting angle in Fe moment. An obvious Debye-type dielectric relaxation with an activation energy of0.35eV was observed between240and420K. The replacement of Mg2+caused the suppression of electron transfer, resulting a larger activation energy than that of LuFe2O4. The dielectric relaxation could be strongly suppressed by oxygen annealing, indicating that oxygen vacancies played an essential role in the dielectric response of LuFeMgO4ceramics.
The crystal structure of LuFeCuO4was similar with those of LuFe2O4and LuFeMgO4. An obvious dielectric relaxation with activation energy0.37eV was observed between250and415K, which could be ascribed to the electron hopping between the ions on Fe sites. With the decrease of spin moments of the divalent ions, the values of TN became smaller in the order of LuFe2O4, LuFeCuO4(TN～57K) and LuFeMgO4. A P-E hysteresis loop was observed in LuFeCuO4ceramics at150K, and the replacement of Cu2+resulted in the weaker ferroelectricity than LuFe2O4. At room temperature, remarkable magnetodielectric response (～7%) was observed in LuFeCuO4ceramics.
LuFeO3was identified to be an orthorhombically distorted perovskite structure with space group Pbnm. Two Debye-type dielectric relaxations were observed in LuFeO3ceramics. The low temperature relaxation was originated from the electron hopping between Fe2+and Fe3+ions, while the high temperature relaxation was related with oxygen vacancies. The Neel temperature for LuFeO3was628K, and the weak ferromagnetic characteristics owing to the canting angle of magnetic spins were detected at room temperature. Obvious ferroelectric loops were observed at room temperature, and the values of electric polarization increased with an applied external magnetic field. Meanwhile, room-temperature magnetodielectric effect was detected, and LuFeO3was expected as a promising candidate for new multiferroic materials.
In LuFeO3, partially substituting Mn for Fe did not change the crystal structure. The low temperature dielectric relaxation was suppressed and only one dielectric anomaly around360-530K was observed in LuFe0.95Mn0.05O3ceramics. The smaller polarization compared with LuFeO3suggested the important role of electron hopping between Fe2-and Fe3+ions in ferroelectricity. The results of thermal analysis indicated that the Neel temperature decreased with Mn-substitution, which could be ascribed to the weaker Fe3+-O-Mn3+and Mn3+-O-Mn3+exchange interactions compared with Fe3+-O-Fe3+interaction. Due to the strong anisotropy of Mn3+ions, a spin reorientation transition could be induced in LuFeo.95Mno.05O3.
引文
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