铁酸铋高性能多铁陶瓷材料的制备与研究
摘要
多铁材料因同时具有铁电性、铁磁性甚至铁弹性而引起了人们广泛的关注它具有多方面的应用前景,是当前材料领域研究中的前沿热点之一BiFeO3(BFO)是一种单相多铁材料,它具备高的居里温度(Tc～1100K)和奈尔温度(TN～643K),是少数在室温下同时具有铁电性和铁磁性的多铁材料之一。理论计算表明BFO具有大的自发极化值。此外,BFO中的铁电序和铁磁序的相互作用将产生磁电耦合效应。对BFO材料的研究,不仅具有重要的物理意义,有助于认识多铁材料多铁性共存的物理机制,而且对研制新型信息存储器件、自旋电子器件、磁电耦合传感器件等方面具有潜在的应用前景。
然而,目前对于BFO的研究还有待深入,对BFO多铁性共存的物理机制还有待进一步深入认识,在制备性能优良的单相BFO陶瓷和薄膜以满足器件应用的要求等方面,还存在不少亟待解决的关键问题,有许多研究工作要做。因此,本文主要从以下几方面开展了BFO陶瓷和薄膜的制备及其性能的研究工作并取得了一些创新性成果。
1.针对铁酸铋存在的问题,为有效减小其漏电流,高价离子Ti的引入成为很多科研工作者研究的热点,使用快速液相烧结的方法成功制备了以钙钛矿相为主晶相的掺Ti陶瓷BiFe0.9Ti0.05O3、BiFe0.9Ti0.1O3和BiFeO3, Ti的掺入不仅提高了铁酸铋的烧结温度,同时也抑制了铁酸铋陶瓷表面颗粒的液化现象,使其晶粒减小提高了陶瓷样品的致密度和烧结收缩率,XRD分析结果表明,钛的掺入引起了BiFeO3的晶格产生变化。
2.在计量掺杂的基础上,通过制备非计量掺钛的陶瓷样品BiFe0.9Ti0.05O3.研究在引入高价Ti离子的同时引入铁空位Vfem,深入探讨铁酸铋体系的导电机理,实验结果发现相比铁酸铋,计量掺钛样品的漏电流密度降低了4个数量级,而非计量掺钛却降低了9个数量级,电阻率高达1014Ω cm,在低频100Hz损耗仅有0.015,结果说明了电子在金属离子Fe2+和Fe3+之间的跃迁所引起的漏导可以通过Ti掺杂和Fe空位的引入而得到有效的抑制。在非计量掺钛的样品中观测到改善的铁电性,其Pr为0.23μC/cm2。铁磁数据的测量结果显示,铁空位Vmfe的引入并未明显改变其体系的螺旋磁结构。
3.采用固相合成法制备了Dy掺杂与Dy和Ti共掺杂的BFO(BDFTO)陶瓷,XRD测试结果显示，样品的主品相为钙钛矿相,虽然有少量杂相存在,但并没有探测到Dy3Fe5012相和菱面体结构相。相比单掺Dy的样品，共掺样品BDFTO表现出高的电阻率(1013Ωcm),改善的铁电性¨(Pr～0.25μC/cm2)和铁磁性(Ms～1emu/g)。该研究结果表明,在BFO体系中Ti和Dy的协同效应是引起该体系性能提高的可能机制,值得进一步深入研究。
4.为有效提高BFO体系的铁磁性和研究Ti与稀上元素共掺杂对该体系性能的影响和调制作用,使用固相烧结法制备了Ho掺杂以及Ho和Ti共掺杂的BFO(BHFTO)陶瓷。XRD测试结果显示,有少量杂相Bi12(Bi0.5Fe0.5)O19.5和Bi46Fe2O12,但样品主晶相为钙钛矿相。SEM测试结果显示,在单掺Ho的基础上引入Ti离子后,样品的颗粒小(1μm)而均匀且致密度明显提高,烧结线收缩率达到了13%。样品有极高的电阻率(1014Ωcm)和在100Hz下损耗仅为0.02,,共掺杂样品并未有明显的介电弥散现象。铁电性和铁磁性的改善表明A/B位共掺杂技术是同时改善提高BFO陶瓷的铁电性和铁磁性的有效方法
Multiferroic materials, simultaneously possessing the properties of ferroelectricity, ferromagnetism and even ferroelasticity, have aroused much attention in recent years. As a prospective candidate for potential applications in many aspects, multiferroic materials have been one of the most focused research fields at present.BiFeO3(BFO) is a single-phase multiferroic material with a high Curie temperature(Tc～1100K) and a high Neel temperature (TN～643K). It is one of the fewmultiferroic materials exhibiting both ferroelectric and ferromagnetic properties at room temperature. Theoretical calculations indicated that large polarization could be achieved in BFO. Moreover, interaction between the ferroelectric and ferromagnetic orders will lead to the effect of magnetoelectric (ME) coupling. The research on BFO material has not only the theoretical importance for understanding the physical mechanism of the coexistence of the ferroelectric and ferromagnetic properties, but also the importance for potential applications in novel devices of information storages,spintronics, ME sensor etc.
However, much work has to be done to understand the physical mechanisms of the coexistence of the multiferroic properties of the BFO, and to solve the key problems emerged in the preparation of pure BFO ceramic and thin film with satisfied high quality for various novel device applications. Therefore, this dissertation focuses on the study of the preparations and properties of BFO based ceramics and thin films in the following aspects and some original novel results had been obtained as follows:
1. Ti substitution for Fe has been proven effective to reduce the leakage current in BFO. Undoped BFO, Ti doped BiFe0.9Ti0.05O3and BiFe0.9Ti0.1O3ceramics were prepared by a rapid liquid phase sintering technique. The introduction of Ti not only raises the sintering temperature but also suppresses the appearance of liquid phases. The ceramic sintering shrinkage and density of the samples are also improved. XRD analysis results show that Ti-doping induces some subtle changes in BFO lattice.
2. The nominal nonstoichiometric Ti doped ceramics BiFe0.9Ti0.05O3were prepared in order to introduce some Fe vacancy and probe the conduction mechanism of BFO. The leakage current of BiFeo.9Tio.05O3is decreased by nine orders of magnitude from that of BiFeO3. With an ultrahigh electrical resistivity, over1014Ωcm, BiFe0.9Ti0.05O3ceramic displays an especially low dielectric loss,0.015at100Hz, a remanent polarization Pr of0.23μC/cm2and a remanent magnetization Mr of0.13emu/g at room temperature. It is proposed that the Fe-deficiency in BiFeo.9Ti0.05O3decreases the amount of Fe2+and leads to the ultrahigh electrical resistivity. However the result of ferromagnctism presents that the introduction of Fe vacancy can not effectively cause the change of spatially modulated spin structure.
3. Bi0.9Dy0.1Fe0.95O3and Bi0.9Dy0.1Fe0.9Ti0.05O3ceramics of high rhombohedral perovskite phase content were prepared and compared, which shows that Ti-doping leads to not only a great increase in electrical resistivity but also a further dramatic magnetization enhancement in addition to that induced by Dy-doping. With a high electrical resistivity around1×10Ωcm and a remanent polarization Pr of0.25μC/cm2, Bio.9Dyo.1Fco.9Tio.05O3ceramics sintered at960°C display a saturation magnetization Ms of lemu/g, which is three times as much as that of Bi0.9Dy0.1Fe0.95O3sintered at900°C. It is proposed that there exist some synergistic action between Ti and Dy in Bi0.9Dy0.1Fe0.9Ti0.05O3which gives rise to additional magnetization enhancement in BiFeO3.
4. In order to improve the fcrromagnetism of BFO and study the effect of eodoping of Ti and rare earth elements on the properties of BFO, Bio.9Hoo.1Fco.95O3and Bi0.9Ho0.1Fe0.9Ti0.05O3ceramics were prepared through conventional solid-state-reaction. X-ray diffraction indicated that both ceramics were of a high rhombohedral perovskite phase content and contained minor impurities phases such as Bi12(Bi0.5Fe0.5)O19.5and Bi46Fe2O12. Microstructural analyses showed that the grains of Bi0.9Ho0.1Fe0.9Ti0.05O3ceramics were much smaller than those of Bi0.9Ho0.1Fe0.95O3. Bi0.9Ho0.1Fe0.9Ti0.05O3ceramics showed a electrical resistivity over1×1014Qcm at room temperature, a very low. dielectric loss of0.02at100Hz, magnetic hysteresis loop with a remnant magnetization2Mrof～0.485emu/g, both much higher than those of Bi0.9Ho0.1Fe0.95O3. It was proposed that the defect subsystem of BiFeO3is responsible for the improvements and attention should be paid to tailor the defect subsystem through adopting nonstoichiometric compositions and codoping of multiple elements.
然而,目前对于BFO的研究还有待深入,对BFO多铁性共存的物理机制还有待进一步深入认识,在制备性能优良的单相BFO陶瓷和薄膜以满足器件应用的要求等方面,还存在不少亟待解决的关键问题,有许多研究工作要做。因此,本文主要从以下几方面开展了BFO陶瓷和薄膜的制备及其性能的研究工作并取得了一些创新性成果。
1.针对铁酸铋存在的问题,为有效减小其漏电流,高价离子Ti的引入成为很多科研工作者研究的热点,使用快速液相烧结的方法成功制备了以钙钛矿相为主晶相的掺Ti陶瓷BiFe0.9Ti0.05O3、BiFe0.9Ti0.1O3和BiFeO3, Ti的掺入不仅提高了铁酸铋的烧结温度,同时也抑制了铁酸铋陶瓷表面颗粒的液化现象,使其晶粒减小提高了陶瓷样品的致密度和烧结收缩率,XRD分析结果表明,钛的掺入引起了BiFeO3的晶格产生变化。
2.在计量掺杂的基础上,通过制备非计量掺钛的陶瓷样品BiFe0.9Ti0.05O3.研究在引入高价Ti离子的同时引入铁空位Vfem,深入探讨铁酸铋体系的导电机理,实验结果发现相比铁酸铋,计量掺钛样品的漏电流密度降低了4个数量级,而非计量掺钛却降低了9个数量级,电阻率高达1014Ω cm,在低频100Hz损耗仅有0.015,结果说明了电子在金属离子Fe2+和Fe3+之间的跃迁所引起的漏导可以通过Ti掺杂和Fe空位的引入而得到有效的抑制。在非计量掺钛的样品中观测到改善的铁电性,其Pr为0.23μC/cm2。铁磁数据的测量结果显示,铁空位Vmfe的引入并未明显改变其体系的螺旋磁结构。
3.采用固相合成法制备了Dy掺杂与Dy和Ti共掺杂的BFO(BDFTO)陶瓷,XRD测试结果显示，样品的主品相为钙钛矿相,虽然有少量杂相存在,但并没有探测到Dy3Fe5012相和菱面体结构相。相比单掺Dy的样品，共掺样品BDFTO表现出高的电阻率(1013Ωcm),改善的铁电性¨(Pr～0.25μC/cm2)和铁磁性(Ms～1emu/g)。该研究结果表明,在BFO体系中Ti和Dy的协同效应是引起该体系性能提高的可能机制,值得进一步深入研究。
4.为有效提高BFO体系的铁磁性和研究Ti与稀上元素共掺杂对该体系性能的影响和调制作用,使用固相烧结法制备了Ho掺杂以及Ho和Ti共掺杂的BFO(BHFTO)陶瓷。XRD测试结果显示,有少量杂相Bi12(Bi0.5Fe0.5)O19.5和Bi46Fe2O12,但样品主晶相为钙钛矿相。SEM测试结果显示,在单掺Ho的基础上引入Ti离子后,样品的颗粒小(1μm)而均匀且致密度明显提高,烧结线收缩率达到了13%。样品有极高的电阻率(1014Ωcm)和在100Hz下损耗仅为0.02,,共掺杂样品并未有明显的介电弥散现象。铁电性和铁磁性的改善表明A/B位共掺杂技术是同时改善提高BFO陶瓷的铁电性和铁磁性的有效方法
Multiferroic materials, simultaneously possessing the properties of ferroelectricity, ferromagnetism and even ferroelasticity, have aroused much attention in recent years. As a prospective candidate for potential applications in many aspects, multiferroic materials have been one of the most focused research fields at present.BiFeO3(BFO) is a single-phase multiferroic material with a high Curie temperature(Tc～1100K) and a high Neel temperature (TN～643K). It is one of the fewmultiferroic materials exhibiting both ferroelectric and ferromagnetic properties at room temperature. Theoretical calculations indicated that large polarization could be achieved in BFO. Moreover, interaction between the ferroelectric and ferromagnetic orders will lead to the effect of magnetoelectric (ME) coupling. The research on BFO material has not only the theoretical importance for understanding the physical mechanism of the coexistence of the ferroelectric and ferromagnetic properties, but also the importance for potential applications in novel devices of information storages,spintronics, ME sensor etc.
However, much work has to be done to understand the physical mechanisms of the coexistence of the multiferroic properties of the BFO, and to solve the key problems emerged in the preparation of pure BFO ceramic and thin film with satisfied high quality for various novel device applications. Therefore, this dissertation focuses on the study of the preparations and properties of BFO based ceramics and thin films in the following aspects and some original novel results had been obtained as follows:
1. Ti substitution for Fe has been proven effective to reduce the leakage current in BFO. Undoped BFO, Ti doped BiFe0.9Ti0.05O3and BiFe0.9Ti0.1O3ceramics were prepared by a rapid liquid phase sintering technique. The introduction of Ti not only raises the sintering temperature but also suppresses the appearance of liquid phases. The ceramic sintering shrinkage and density of the samples are also improved. XRD analysis results show that Ti-doping induces some subtle changes in BFO lattice.
2. The nominal nonstoichiometric Ti doped ceramics BiFe0.9Ti0.05O3were prepared in order to introduce some Fe vacancy and probe the conduction mechanism of BFO. The leakage current of BiFeo.9Tio.05O3is decreased by nine orders of magnitude from that of BiFeO3. With an ultrahigh electrical resistivity, over1014Ωcm, BiFe0.9Ti0.05O3ceramic displays an especially low dielectric loss,0.015at100Hz, a remanent polarization Pr of0.23μC/cm2and a remanent magnetization Mr of0.13emu/g at room temperature. It is proposed that the Fe-deficiency in BiFeo.9Ti0.05O3decreases the amount of Fe2+and leads to the ultrahigh electrical resistivity. However the result of ferromagnctism presents that the introduction of Fe vacancy can not effectively cause the change of spatially modulated spin structure.
3. Bi0.9Dy0.1Fe0.95O3and Bi0.9Dy0.1Fe0.9Ti0.05O3ceramics of high rhombohedral perovskite phase content were prepared and compared, which shows that Ti-doping leads to not only a great increase in electrical resistivity but also a further dramatic magnetization enhancement in addition to that induced by Dy-doping. With a high electrical resistivity around1×10Ωcm and a remanent polarization Pr of0.25μC/cm2, Bio.9Dyo.1Fco.9Tio.05O3ceramics sintered at960°C display a saturation magnetization Ms of lemu/g, which is three times as much as that of Bi0.9Dy0.1Fe0.95O3sintered at900°C. It is proposed that there exist some synergistic action between Ti and Dy in Bi0.9Dy0.1Fe0.9Ti0.05O3which gives rise to additional magnetization enhancement in BiFeO3.
4. In order to improve the fcrromagnetism of BFO and study the effect of eodoping of Ti and rare earth elements on the properties of BFO, Bio.9Hoo.1Fco.95O3and Bi0.9Ho0.1Fe0.9Ti0.05O3ceramics were prepared through conventional solid-state-reaction. X-ray diffraction indicated that both ceramics were of a high rhombohedral perovskite phase content and contained minor impurities phases such as Bi12(Bi0.5Fe0.5)O19.5and Bi46Fe2O12. Microstructural analyses showed that the grains of Bi0.9Ho0.1Fe0.9Ti0.05O3ceramics were much smaller than those of Bi0.9Ho0.1Fe0.95O3. Bi0.9Ho0.1Fe0.9Ti0.05O3ceramics showed a electrical resistivity over1×1014Qcm at room temperature, a very low. dielectric loss of0.02at100Hz, magnetic hysteresis loop with a remnant magnetization2Mrof～0.485emu/g, both much higher than those of Bi0.9Ho0.1Fe0.95O3. It was proposed that the defect subsystem of BiFeO3is responsible for the improvements and attention should be paid to tailor the defect subsystem through adopting nonstoichiometric compositions and codoping of multiple elements.
引文
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