具有钙钛矿结构多铁材料的高温高压合成及性质研究
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摘要
由于铁电有序以及铁磁有序的共存使得多铁性材料具有丰富的物理性质。同时上述两种有序之间的磁电耦合效应也使得材料能通过外加电场控制其磁化，或通过外加磁场调节其自发极化，从而使其具有广阔的应用前景。虽然多铁材料在发现之初就受到人们的广泛关注，但早期合成的单相多铁材料的磁电耦合效应非常弱，以至于无法在器件中实际应用。近些年随着在具有钙钛矿结构的稀土锰酸盐TbMnO3和TbMn2O5中发现了强的磁电耦合效应后，人们又再次将目光投入到具有强磁电耦合效应的稀土锰酸盐上。由于实际应用的要求，多铁材料在室温以上应该同时具有强的铁电极化强度和强的磁化强度以外，还应该具有强的自发极化与自发磁化之间的耦合。但遗憾的是至今为止，还没有任何一种材料能符合这些要求。目前已知的多铁材料多数为反铁磁材料。因此寻找在室温以上具有强磁电耦合效应的单相多铁材料仍是亟待解决的难题。
被广泛研究的强磁电耦合多铁材料—正交结构的TbMnO3具有27K的铁电转变温度和41K的反铁磁转变温度。TbMnO3属于Pnma空间群，其中的Mn3+离子的电子构型为t2g3eg1。TbMnO3中ab面内自旋铁磁排列，而沿着c轴方向的ab面间自旋反铁磁排列。这两种相互作用间的竞争导致了ab面内自旋失措，进而引起自发极化。因此在o-TbMnO3中磁性和铁电性之间有着十分紧密的关联，即较强的耦合。
另外一种研究较多的正交稀土锰酸盐o-YMnO3具有21K的铁电转变温度和42K的反铁磁温度。如何大幅的提高这类材料的磁和铁电转变温度，是非常有意义的课题。人们做出了非常多的尝试，很遗憾的是转变温度的提升并不显著。这是由于之前的掺杂工作都集中在A位掺杂，即以其他稀土离子掺杂取代A位的Tb3+或Y3+离子。这样做的好处就是最小程度的破坏或改变o-TbMnO3及o-YMnO3的磁结构，从而保护铁电极化不被破坏。近几年的研究表明在B位掺杂Mn4+离子或Cr3+离子不一定会破坏铁电极化，也就是说精心挑选的B位掺杂离子不会破坏铁电极化，这为提高o-YMnO3的转变温度带来了希望。
另外，六方YbFeO3薄膜也表现出了非常好的磁电耦合效应以及强的铁电极化强度，其剩余极化率高达10μC/cm2。随着对其研究的深入人们发现其铁电起源与以下两个因素密切相关，P63cm空间群带来的六方相结构中FeO平面两侧不对称性和5dz2(Yb)-2pz(OA)相互作用。通常情况下，YbFeO3块体材料属于正交Pnma空间群，目前为止有关六方YbFeO3的合成及其多铁性质表征尚无报道。因此本论文设计了一系列新的多铁材料，通过在具有六方结构的InFeO3中掺杂引入Yb离子提供六方晶体结构的几何环境。由于Yb离子的随机取代可以破坏P63/mmc空间群中FeO平面两侧的对称性，同时提供5dz2(Yb)-2pz(OA)之间的相互作用。
本论文通过高压助熔剂方法首次合成制备了具有正交结构的YFe0.5Mn0.5O3（YFMO）和YCr0.5Mn0.5O3（YCMO）。通过X-射线衍射等表征手段确定了其晶体结构。通过磁性测试、介电温谱和电滞回线测试证明了YFMO是多铁材料，其反铁磁转变温度为328K。YCMO为亚铁磁材料，磁转变温度为74K。通过介电温谱的测试发现YCMO样品存在类似弛豫铁电体特有的介电弛豫行为。铁电测试却发现YCMO不存在铁电极化。这一结果也从实验上证明了正交稀土锰酸盐铁电极化只出现在反铁磁材料中这一推论。
通过高温固相法将Yb离子引入六方InFeO3，为Yb5dz2-O2pz杂化轨道提供了六方晶体结构的几何环境。磁化率曲线的测试以及10K及100K下的磁滞回线证明样品为具有倾斜铁磁性的反铁磁材料，反铁磁转变温度即奈尔温度约为150K。双波法测试得到的电滞回线证明了In0.8Yb0.2FeO3的铁电性质。通过对In0.8Yb0.2FeO3结构的讨论得出Yb离子在FeO面两侧的不对称分布造成了微弱的宏观铁电极化的结论。这样的结果为未来多铁材料的设计，尤其是六方稀土铁酸盐块体多铁材料的设计提供新的思路与方法。
Single-phase multiferroic material is a class of single-phase compounds which hasboth ferroelectric and magnetic properties. Firstly, multiferroic materials have bothferroelectric and magnetic properties; secondly, there may be coupling effects betweenferroelectric and magnetic properties, which can achieve the mutual regulation offerroelectric and magnetic materials.
Normally, multiferroic materials are categorized into two different classesdepending on the origin of the ferroelectric properties. The first class called properferroelectrics is exemplified by BiFeO3, BiMnO3and Bi2NiMnO6, which are typicalmultiferroic materials universal with both relative high ferroelectric Curie temperatureand high magnetic Curie temperature. However, this class of materials generally showweak magnetoelectric coupling, because of the different origins of anti/ferromagneticand ferroelectric orderings that FM desires transition metals with unpaired3d electronsand unfilled3d orbital, whereas FE polarization requires transition metals with filled3dorbital. Members of the second class known as improper ferroelectrics have broughtbetter magnetoelectric coupling effect, exemplified by orthorhombic RMnO3(R=Tb-Luand Y) and GdFeO3.
Orthorhombic RMnO3(o-RMnO3) has attracted great research interests owing tothe strong coupling between magnetic ordering and ferroelectric ordering. Themagnetoelectric is useful for storing information in a memory device. Usually the operating temperature is too low to meet the practical applications. Although manystudies have been carried out, the finding of new multiferroics with higher transitiontemperatures is still lacking. Previous studies have mostly focused on doping at therare-earth site to increase the magnetic transition temperature while protecting theferroelectric properties at the same time. Unfortunately, the multiferroic properties haveyet witnessed any significant improvement as desired. Recent reports suggest that asmall quantity of Cr3+doping at Mn3+sites significantly enhances the FM component ofthe samples although the AFM order is dominant. Furthermore, the newdouble-perovskite compound Tb0.5Ca0.5MnO3treated as Mn4+doping at Mn3+siteshowed a high ferroelectric transition temperature at about270K. These are excitingsignals that the carefully chosen atoms doping at the B site may effectively improve themultiferroic peoperties while avoide limination of the FE polarization.
The most widely studied in RMnO3(R=Tb-Lu and Y) is o-TbMnO3, withantiferromagnetic (AFM) ordering at41K and ferroelectric ordering at27K. Anothertypical improper ferroelectric, albeit less studied because of the extraordinary conditionssuch as high-pressure sintering required during synthesis, othorhombic YMnO3(o-YMnO3) is an orthorhombic distorted perovskite (ABO3) in Pnma (No.62) spacegroup. And o-YMnO3shows antiferromagnetic ordering at about42K and ferroelectricordering at21K. Compared with TbMnO3, o-YMnO3is a less complex material to bestudied because the Y3+ion is nonmagnetic. The substitution of the3d5ion Fe3+and3d3ion Cr3+in o-YMnO3gives Fe3+-O-Mn3+(e2-O-1) and Cr3+-O-Mn3+(0gegeg-O-)interaction, thus improving antiferromagnetic transition temperature withoutsignificantly changing the structures. Furthermore, YCrO3is also a multiferroic materialwith antiferromagnetic order at140K and ferroelectric order at437K. Fascinatingproperties are thus expected through the introducing of Cr3+into o-YMnO3. But thedoping product of o-YMnO3, especially high-quality single phase product was barelyreported in the past years. This fact also suggests that it’s difficult to substitute Mn or Yions by other elements in o-YMnO3. The high-quality samples may lead to moreaccurate magnetism and dielectric test results. So the lacking of high-quality samples limited the research of this kind of materials.
The Hexagonal YbFeO3thin-film shows good ferroelectric properties at Curietemperature of470K. The remanent polarizarion is as large as10μC/cm2. To understandthe reason why this material can exhibit ferroelectric polarization reported in theliterature, two very important factors can not be ignored—the absence of mirror-plane ofhexagonal structure of P63cm and the empty5dz2(Yb)-2pz(OA) interaction. The bulkmaterial of YbFeO3belongs to the Pnma space group, in general, while no hexagonalstructure YbFeO3bulk material have been reported. To obtain multiferroic properties inthe bulk material, we designed and synthesized a series compands of Yb ions dopedInFeO3. First, InFeO3has a hexagonal structure. Though InFeO3belongs to the P63/mmcspace group which has a mirror-plane, the random presence of Yb ions makes anonmirror symmetry for Yb ions. Second, this system also has an empty5dz2(Yb)-2pz(OA) interaction of Yb ions. Otherwise, indium-based perovskite have been reported asan multiferroic near room temperature. So good multiferroic is expected in theIn1-xYbxFeO3.
The highly pure crystals of Y2FeMnO6(YFMO) and Y2CrMnO6(YCMO) havebeen firstly synthesized using flux method under high temperature of1573K and highpressure of6GPa. Both YFMO and YCMO have orthorhombic structures in space groupPnma. The temperature-dependent magnetization and the nonlinear M-H hysteresisloops of both materials indicate that an antiferromagnetic transition occurs at Néeltemperature of328K for YFMO, and a ferrimagnetic transition occurs at74K forYCMO. YFMO is a relaxor ferroelectric in which three dielectric relaxations wereobserved at245K,328K and358K, respectively. The first relaxation process is due toMaxwell-Wagner polarization at the grain boundary whereas the second and the thirdrelaxation behaviours arise from the beginning and the ending of antiferromagneticordering, respectively. The presence of the dielectric anomaly near TNindicates themagnetoelectric effect. Ferroelectric hysteresis loops and PUND (positive-up&negative-down) pulse data reveal weak ferroelectric behaviors of YFMO at77K.Otherwise one dielectric constant anomaly has been found for YCMO at about390K.But no ferroelectric polarization was observed in YCMO.
A new series of multiferroic materials In1-xYbxFeO3(0.1≤x≤0.3) with giantdielectric constant were firstly prepared. The substitution of Yb ions for In induced theweak ferroelectric properties of this system. Dielectric measurement shows that thedielectric property is closely related to the crystal structures. The crystallize in spacegroup P63/mmc similarly to InFeO3. The increase in the Yb content leads to anincrement in a and reduction in c parameters. Magnetic measurements show thatIn0.8Yb0.2FeO3has antiferromagnetic transition temerature at about150K. And onedielectric constant change has been fund for In0.8Yb0.2FeO3at about553K.
被广泛研究的强磁电耦合多铁材料—正交结构的TbMnO3具有27K的铁电转变温度和41K的反铁磁转变温度。TbMnO3属于Pnma空间群，其中的Mn3+离子的电子构型为t2g3eg1。TbMnO3中ab面内自旋铁磁排列，而沿着c轴方向的ab面间自旋反铁磁排列。这两种相互作用间的竞争导致了ab面内自旋失措，进而引起自发极化。因此在o-TbMnO3中磁性和铁电性之间有着十分紧密的关联，即较强的耦合。
另外一种研究较多的正交稀土锰酸盐o-YMnO3具有21K的铁电转变温度和42K的反铁磁温度。如何大幅的提高这类材料的磁和铁电转变温度，是非常有意义的课题。人们做出了非常多的尝试，很遗憾的是转变温度的提升并不显著。这是由于之前的掺杂工作都集中在A位掺杂，即以其他稀土离子掺杂取代A位的Tb3+或Y3+离子。这样做的好处就是最小程度的破坏或改变o-TbMnO3及o-YMnO3的磁结构，从而保护铁电极化不被破坏。近几年的研究表明在B位掺杂Mn4+离子或Cr3+离子不一定会破坏铁电极化，也就是说精心挑选的B位掺杂离子不会破坏铁电极化，这为提高o-YMnO3的转变温度带来了希望。
另外，六方YbFeO3薄膜也表现出了非常好的磁电耦合效应以及强的铁电极化强度，其剩余极化率高达10μC/cm2。随着对其研究的深入人们发现其铁电起源与以下两个因素密切相关，P63cm空间群带来的六方相结构中FeO平面两侧不对称性和5dz2(Yb)-2pz(OA)相互作用。通常情况下，YbFeO3块体材料属于正交Pnma空间群，目前为止有关六方YbFeO3的合成及其多铁性质表征尚无报道。因此本论文设计了一系列新的多铁材料，通过在具有六方结构的InFeO3中掺杂引入Yb离子提供六方晶体结构的几何环境。由于Yb离子的随机取代可以破坏P63/mmc空间群中FeO平面两侧的对称性，同时提供5dz2(Yb)-2pz(OA)之间的相互作用。
本论文通过高压助熔剂方法首次合成制备了具有正交结构的YFe0.5Mn0.5O3（YFMO）和YCr0.5Mn0.5O3（YCMO）。通过X-射线衍射等表征手段确定了其晶体结构。通过磁性测试、介电温谱和电滞回线测试证明了YFMO是多铁材料，其反铁磁转变温度为328K。YCMO为亚铁磁材料，磁转变温度为74K。通过介电温谱的测试发现YCMO样品存在类似弛豫铁电体特有的介电弛豫行为。铁电测试却发现YCMO不存在铁电极化。这一结果也从实验上证明了正交稀土锰酸盐铁电极化只出现在反铁磁材料中这一推论。
通过高温固相法将Yb离子引入六方InFeO3，为Yb5dz2-O2pz杂化轨道提供了六方晶体结构的几何环境。磁化率曲线的测试以及10K及100K下的磁滞回线证明样品为具有倾斜铁磁性的反铁磁材料，反铁磁转变温度即奈尔温度约为150K。双波法测试得到的电滞回线证明了In0.8Yb0.2FeO3的铁电性质。通过对In0.8Yb0.2FeO3结构的讨论得出Yb离子在FeO面两侧的不对称分布造成了微弱的宏观铁电极化的结论。这样的结果为未来多铁材料的设计，尤其是六方稀土铁酸盐块体多铁材料的设计提供新的思路与方法。
Single-phase multiferroic material is a class of single-phase compounds which hasboth ferroelectric and magnetic properties. Firstly, multiferroic materials have bothferroelectric and magnetic properties; secondly, there may be coupling effects betweenferroelectric and magnetic properties, which can achieve the mutual regulation offerroelectric and magnetic materials.
Normally, multiferroic materials are categorized into two different classesdepending on the origin of the ferroelectric properties. The first class called properferroelectrics is exemplified by BiFeO3, BiMnO3and Bi2NiMnO6, which are typicalmultiferroic materials universal with both relative high ferroelectric Curie temperatureand high magnetic Curie temperature. However, this class of materials generally showweak magnetoelectric coupling, because of the different origins of anti/ferromagneticand ferroelectric orderings that FM desires transition metals with unpaired3d electronsand unfilled3d orbital, whereas FE polarization requires transition metals with filled3dorbital. Members of the second class known as improper ferroelectrics have broughtbetter magnetoelectric coupling effect, exemplified by orthorhombic RMnO3(R=Tb-Luand Y) and GdFeO3.
Orthorhombic RMnO3(o-RMnO3) has attracted great research interests owing tothe strong coupling between magnetic ordering and ferroelectric ordering. Themagnetoelectric is useful for storing information in a memory device. Usually the operating temperature is too low to meet the practical applications. Although manystudies have been carried out, the finding of new multiferroics with higher transitiontemperatures is still lacking. Previous studies have mostly focused on doping at therare-earth site to increase the magnetic transition temperature while protecting theferroelectric properties at the same time. Unfortunately, the multiferroic properties haveyet witnessed any significant improvement as desired. Recent reports suggest that asmall quantity of Cr3+doping at Mn3+sites significantly enhances the FM component ofthe samples although the AFM order is dominant. Furthermore, the newdouble-perovskite compound Tb0.5Ca0.5MnO3treated as Mn4+doping at Mn3+siteshowed a high ferroelectric transition temperature at about270K. These are excitingsignals that the carefully chosen atoms doping at the B site may effectively improve themultiferroic peoperties while avoide limination of the FE polarization.
The most widely studied in RMnO3(R=Tb-Lu and Y) is o-TbMnO3, withantiferromagnetic (AFM) ordering at41K and ferroelectric ordering at27K. Anothertypical improper ferroelectric, albeit less studied because of the extraordinary conditionssuch as high-pressure sintering required during synthesis, othorhombic YMnO3(o-YMnO3) is an orthorhombic distorted perovskite (ABO3) in Pnma (No.62) spacegroup. And o-YMnO3shows antiferromagnetic ordering at about42K and ferroelectricordering at21K. Compared with TbMnO3, o-YMnO3is a less complex material to bestudied because the Y3+ion is nonmagnetic. The substitution of the3d5ion Fe3+and3d3ion Cr3+in o-YMnO3gives Fe3+-O-Mn3+(e2-O-1) and Cr3+-O-Mn3+(0gegeg-O-)interaction, thus improving antiferromagnetic transition temperature withoutsignificantly changing the structures. Furthermore, YCrO3is also a multiferroic materialwith antiferromagnetic order at140K and ferroelectric order at437K. Fascinatingproperties are thus expected through the introducing of Cr3+into o-YMnO3. But thedoping product of o-YMnO3, especially high-quality single phase product was barelyreported in the past years. This fact also suggests that it’s difficult to substitute Mn or Yions by other elements in o-YMnO3. The high-quality samples may lead to moreaccurate magnetism and dielectric test results. So the lacking of high-quality samples limited the research of this kind of materials.
The Hexagonal YbFeO3thin-film shows good ferroelectric properties at Curietemperature of470K. The remanent polarizarion is as large as10μC/cm2. To understandthe reason why this material can exhibit ferroelectric polarization reported in theliterature, two very important factors can not be ignored—the absence of mirror-plane ofhexagonal structure of P63cm and the empty5dz2(Yb)-2pz(OA) interaction. The bulkmaterial of YbFeO3belongs to the Pnma space group, in general, while no hexagonalstructure YbFeO3bulk material have been reported. To obtain multiferroic properties inthe bulk material, we designed and synthesized a series compands of Yb ions dopedInFeO3. First, InFeO3has a hexagonal structure. Though InFeO3belongs to the P63/mmcspace group which has a mirror-plane, the random presence of Yb ions makes anonmirror symmetry for Yb ions. Second, this system also has an empty5dz2(Yb)-2pz(OA) interaction of Yb ions. Otherwise, indium-based perovskite have been reported asan multiferroic near room temperature. So good multiferroic is expected in theIn1-xYbxFeO3.
The highly pure crystals of Y2FeMnO6(YFMO) and Y2CrMnO6(YCMO) havebeen firstly synthesized using flux method under high temperature of1573K and highpressure of6GPa. Both YFMO and YCMO have orthorhombic structures in space groupPnma. The temperature-dependent magnetization and the nonlinear M-H hysteresisloops of both materials indicate that an antiferromagnetic transition occurs at Néeltemperature of328K for YFMO, and a ferrimagnetic transition occurs at74K forYCMO. YFMO is a relaxor ferroelectric in which three dielectric relaxations wereobserved at245K,328K and358K, respectively. The first relaxation process is due toMaxwell-Wagner polarization at the grain boundary whereas the second and the thirdrelaxation behaviours arise from the beginning and the ending of antiferromagneticordering, respectively. The presence of the dielectric anomaly near TNindicates themagnetoelectric effect. Ferroelectric hysteresis loops and PUND (positive-up&negative-down) pulse data reveal weak ferroelectric behaviors of YFMO at77K.Otherwise one dielectric constant anomaly has been found for YCMO at about390K.But no ferroelectric polarization was observed in YCMO.
A new series of multiferroic materials In1-xYbxFeO3(0.1≤x≤0.3) with giantdielectric constant were firstly prepared. The substitution of Yb ions for In induced theweak ferroelectric properties of this system. Dielectric measurement shows that thedielectric property is closely related to the crystal structures. The crystallize in spacegroup P63/mmc similarly to InFeO3. The increase in the Yb content leads to anincrement in a and reduction in c parameters. Magnetic measurements show thatIn0.8Yb0.2FeO3has antiferromagnetic transition temerature at about150K. And onedielectric constant change has been fund for In0.8Yb0.2FeO3at about553K.
引文
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