几种ABO_3型稀土锰铁氧化物的水热合成及其磁性研究
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摘要
ABO3型复合氧化物对A位和B位离子半径与价态具有相当大的容忍性，有利于材料掺杂改性与新体系合成。其中，ABO3型Mn、Fe基稀土复合氧化物因其丰富的磁、电等物理性质和优异的物理效应，如巨磁阻效应和多铁性等，而成为当前功能材料和凝聚态物理领域的研究热点之一。目前，人们就此开展的研究主要建立在高温合成的基础上，但许多已显示或具有潜在优异物理效应的ABO3型Mn、Fe基稀土复合氧化物属亚稳相，高温合成法难以制备高质量的单相晶体产物，影响了研究进展。水热合成为制备亚稳相开辟了一条新的途径。本文选择具有磁阻效应或多铁性的四个ABO3型Mn、Fe基稀土复合氧化物体系为研究对象，采用水热技术合成了各体系单相晶体产物，特别是一些亚稳相；对合成条件与产物晶体结构、化学组成、元素价态、微观形貌和磁、电性质进行了表征和研究。
A位掺杂正交锰酸钇是磁阻效应研究中的一个典型体系，其电荷有序相及E型反铁磁对称交换收缩引起的铁电性也正成为多铁性研究中的热点。本文采用水热技术合成了正交Y1-xCaxMnO3（x=0，0.07，0.55和0.65）四个单相产物，实现了在0≤x0.25和0.5≤x≤0.75范围内合成正交单相Y1-xCaxMnO3的突破。产物均为正交单相，具有规整的形貌和良好的结晶状态。Y1-xCaxMnO3（x=0）和Y1-xCaxMnO3（x=0.07）显示类自旋玻璃行为；Y1-xCaxMnO3（x=0.55）显示明显的电荷有序、反铁磁转变和类自旋玻璃行为；Y1-xCaxMnO3（x=0.65）显示非常强的电荷有序信号和反铁磁转变，但未显示类自旋玻璃特征，低温磁化强度剧烈增加，表明体系中存在Dzialoshinsky-Moriya各向异性超交换作用。Y1-xCaxMnO3（x=0.65）在4K时显示了明显的磁滞行为，表明样品在低温下存在较强的局域短程铁磁作用。Y1-xCaxMnO3（x=0.55和0.65）显示了半导体输运性质和小磁阻效应，电导机制符合高相关电子变程跳跃模型。
稀土正铁氧体（RFeO3）因其潜在的室温多铁性而成为多铁性材料研究中的又一亮点。本文采用水热技术合成了系列稀土正铁氧体RFeO3（R=Pr~Lu）单相产物，并对其合成条件与晶体结构、微观形貌和磁相变进行了系统的表征和研究。产物均为正交单相，具有规整的形貌和良好的结晶状态，晶体成核与生长受沉淀-溶解机制控制。通过磁性测量表征了Fe3+的反铁磁转变、自旋重取向转变、磁化强度反转及R3+的磁有序转变等磁相变。与传统合成方法相比，水热合成样品的磁特性表现出一定的不同之处，特别是传统非自旋重取向化合物EuFeO3和LuFeO3显现了自旋重取向迹象。
正交TbMnO3、DyMnO3和HoMnO3具有较强的磁电耦合作用，引起了广泛关注。B位掺杂会引起MnO6八面体结构变化和交换作用变化，进而影响材料的性质，对研究其多铁性具有一定的启发。本文采用水热技术合成了B位锰、铁双掺杂的稀土复合氧化物RMn0.5Fe0.5O3（R=Tb，Dy和Ho）。分析表明，产物是符合化学计量比、结晶状态良好、形貌规整的正交单相化合物，B位元素均为+3价。磁性分析给出了三个样品的反铁磁转变温度和自旋重取向温区。TbFe0.5Mn0.5O3显示了磁化强度反转，高磁场能够扭转磁化强度方向，自旋重取向开始及停止温度与外磁场强度呈线性关系。TbFe0.5Mn0.5O3和DyFe0.5Mn0.5O3在低温下显现了稀土离子的反铁磁转变。三个试样在2K和300K下均显示一定的弱铁磁性。
六方RMnO3具有几何铁电性，是研究较多的多铁性材料之一，但其反铁磁转变温度亟待提高。本文采用水热技术合成了Fe掺杂的六方稀土锰氧化物RMn1-xFexO3（R=Er，Tm，Yb和Lu；x=0，0.1，0.3和0.5）。结构分析显示，ErMnO3和RMn1-xFexO3（R=Tm，Yb和Lu；x=0，0.1，0.3和0.5）均为六方单相，ErMn1-xFexO3（x=0.1，0.3和0.5）为正交和六方混相。Fe掺杂使沿c轴方向的Mn-O键拉长，a-b面内的Mn-O键缩短，晶格参数c增大而a减小。Fe掺杂有效提高了产物的反铁磁转变温度TN，且提高程度与Fe掺杂量x基本呈线性关系。
ABO3-type composite oxides show great tolerance for A-and B-site ions in theaspects of ionic radius and valence. It provides probability and convenience fordoping modification of existing materials and synthesis of new materials. Thereinto,ABO3-type rare-earth manganates and ferrites have become a research focus in thefields of materials and condensed matter physics because of their richmagnetic/electric properties and especially the excellent physical effects such asgiant magnetoresistance, multiferroics, etc. At present, the reaserch therein is mostlybased on high-temperature synthesis. But many outstanding candidates aremetastable phases, which are hard to form or form into the pure phase in hightemperatatures, thus hindering the reaserch progress. Hydrothermal synthesisprovides probability for synthesizing varieties of metastable phases. In this work,four series ABO3-type rare-earth manganates and ferrites were chosen as researchobject, hydrothermal technique was used to synthesize pure-phased samples, and thecrystal structures, chemical compositions, valence states, morphologies, magneticproperties, etc. were studied.
Four pure-phased orthorhombic Y1-xCaxMnO3(x=0,0.07,0.55and0.65)samples with fine crystallization and morphologies were successfully synthesizedvia the low-temperature hydrothermal technique. Y1-xCaxMnO3(x=0) andY1-xCaxMnO3(x=0.07) show the behavior of spin glass. Y1-xCaxMnO3(x=0.55)shows obvious charge-ordering, antiferromagnetic transition and the behavior ofspin glass. Y1-xCaxMnO3(x=0.65) shows strong signals of charge ordering andantiferromagnetic transition, but no behavior of spin glass. Drastic increase ofmagnetization at low temperatures was observed in Y1-xCaxMnO3(x=0.65),suggesting the existence of Dzialoshinsky-Moriya anisotropic superexchange.Obvious magnetic hysteresis was observed in Y1-xCaxMnO3(x=0.65) at4K,suggesting the existence of strong local short-range ferromagnetic interaction.Y1-xCaxMnO3(x=0.55) and Y1-xCaxMnO3(x=0.65) show the charge transportbehavior of semiconductors and a small magnetoresistance, and the electricconduction mechanism accords with the variable range hopping mode of thehighly-correlated electrons.
Pure-phased metastable rare-earth orthoferrites RFeO3(R=Pr, Nd, Sm, Eu, Gd,Tb, Dy, Ho, Er, Tm, Yb and Lu) with fine crystallization and morphologies were successfully synthesized via the low-temperature hydrothermal technique. Thefactors that affect the formation of target products such as media alkalinity, reactiontemperature and time etc. were fully studied, and optimum routes were concluded.The crystal structures, morphologies were characterized, and the crystal nucleationand growth mechanism were analyzed. The magnetic properties, including Fe3+antiferromagnetic transition, spin reorientation, spin glass transition, magnetizationreversal, Re3+antiferromagnetic transition, etc., were characterized and discussed.Compared with samples synthesized by solid state sintering in literatures, thesamples in this work show some difference in the magnetic properties, for example,spin reorientation was observed in EuFeO3and LuFeO3.
Pure-phased orthorhombic RMn0.5Fe0.5O3(R=Tb, Dy and Ho) weresuccessfully synthesized via the low-temperature hydrothermal technique. Thecrystal structures, morphologies, chemical compositions and valences, magneticproperties etc. were analyzed. Magnetization reversal was observed inTbFe0.5Mn0.5O3. A high magnetic field can reverse the magnetization direction, andthe spin reorientation temperature has a linear relation with the magnetic fieldintensity. Re3+antiferromagnetic transition was observed in TbFe0.5Mn0.5O3andDyFe0.5Mn0.5O3at low temperatures. The three samples show residual magnetism at2K and300K.
Hexagonal RMn1-xFexO3(R=Er, Tm, Yb and Lu; x=0,0.1,0.3and0.5) weresuccessfully synthesized via the low-temperature hydrothermal technique. Structuralanalysis shows that the samples of ErMnO3and RMn1-xFexO3(R=Tm, Yb and Lu;x=0,0.1,0.3and0.5) are all pure hexagonal phase, but the samples of ErMn1-xFexO3(x=0.1,0.3and0.5) comprise hexagonal phase and orthorhombic phase. Fe dopingstretches the Mn-O bond along the c axis and shortens the Mn-O bond in the a-bplane, thus leading increase of c and decrease of a. The ferromagnetictransformation TNwas elevated by Fe doping and a linear relation was observedbetween ΔTNand Fe doping x.
A位掺杂正交锰酸钇是磁阻效应研究中的一个典型体系，其电荷有序相及E型反铁磁对称交换收缩引起的铁电性也正成为多铁性研究中的热点。本文采用水热技术合成了正交Y1-xCaxMnO3（x=0，0.07，0.55和0.65）四个单相产物，实现了在0≤x0.25和0.5≤x≤0.75范围内合成正交单相Y1-xCaxMnO3的突破。产物均为正交单相，具有规整的形貌和良好的结晶状态。Y1-xCaxMnO3（x=0）和Y1-xCaxMnO3（x=0.07）显示类自旋玻璃行为；Y1-xCaxMnO3（x=0.55）显示明显的电荷有序、反铁磁转变和类自旋玻璃行为；Y1-xCaxMnO3（x=0.65）显示非常强的电荷有序信号和反铁磁转变，但未显示类自旋玻璃特征，低温磁化强度剧烈增加，表明体系中存在Dzialoshinsky-Moriya各向异性超交换作用。Y1-xCaxMnO3（x=0.65）在4K时显示了明显的磁滞行为，表明样品在低温下存在较强的局域短程铁磁作用。Y1-xCaxMnO3（x=0.55和0.65）显示了半导体输运性质和小磁阻效应，电导机制符合高相关电子变程跳跃模型。
稀土正铁氧体（RFeO3）因其潜在的室温多铁性而成为多铁性材料研究中的又一亮点。本文采用水热技术合成了系列稀土正铁氧体RFeO3（R=Pr~Lu）单相产物，并对其合成条件与晶体结构、微观形貌和磁相变进行了系统的表征和研究。产物均为正交单相，具有规整的形貌和良好的结晶状态，晶体成核与生长受沉淀-溶解机制控制。通过磁性测量表征了Fe3+的反铁磁转变、自旋重取向转变、磁化强度反转及R3+的磁有序转变等磁相变。与传统合成方法相比，水热合成样品的磁特性表现出一定的不同之处，特别是传统非自旋重取向化合物EuFeO3和LuFeO3显现了自旋重取向迹象。
正交TbMnO3、DyMnO3和HoMnO3具有较强的磁电耦合作用，引起了广泛关注。B位掺杂会引起MnO6八面体结构变化和交换作用变化，进而影响材料的性质，对研究其多铁性具有一定的启发。本文采用水热技术合成了B位锰、铁双掺杂的稀土复合氧化物RMn0.5Fe0.5O3（R=Tb，Dy和Ho）。分析表明，产物是符合化学计量比、结晶状态良好、形貌规整的正交单相化合物，B位元素均为+3价。磁性分析给出了三个样品的反铁磁转变温度和自旋重取向温区。TbFe0.5Mn0.5O3显示了磁化强度反转，高磁场能够扭转磁化强度方向，自旋重取向开始及停止温度与外磁场强度呈线性关系。TbFe0.5Mn0.5O3和DyFe0.5Mn0.5O3在低温下显现了稀土离子的反铁磁转变。三个试样在2K和300K下均显示一定的弱铁磁性。
六方RMnO3具有几何铁电性，是研究较多的多铁性材料之一，但其反铁磁转变温度亟待提高。本文采用水热技术合成了Fe掺杂的六方稀土锰氧化物RMn1-xFexO3（R=Er，Tm，Yb和Lu；x=0，0.1，0.3和0.5）。结构分析显示，ErMnO3和RMn1-xFexO3（R=Tm，Yb和Lu；x=0，0.1，0.3和0.5）均为六方单相，ErMn1-xFexO3（x=0.1，0.3和0.5）为正交和六方混相。Fe掺杂使沿c轴方向的Mn-O键拉长，a-b面内的Mn-O键缩短，晶格参数c增大而a减小。Fe掺杂有效提高了产物的反铁磁转变温度TN，且提高程度与Fe掺杂量x基本呈线性关系。
ABO3-type composite oxides show great tolerance for A-and B-site ions in theaspects of ionic radius and valence. It provides probability and convenience fordoping modification of existing materials and synthesis of new materials. Thereinto,ABO3-type rare-earth manganates and ferrites have become a research focus in thefields of materials and condensed matter physics because of their richmagnetic/electric properties and especially the excellent physical effects such asgiant magnetoresistance, multiferroics, etc. At present, the reaserch therein is mostlybased on high-temperature synthesis. But many outstanding candidates aremetastable phases, which are hard to form or form into the pure phase in hightemperatatures, thus hindering the reaserch progress. Hydrothermal synthesisprovides probability for synthesizing varieties of metastable phases. In this work,four series ABO3-type rare-earth manganates and ferrites were chosen as researchobject, hydrothermal technique was used to synthesize pure-phased samples, and thecrystal structures, chemical compositions, valence states, morphologies, magneticproperties, etc. were studied.
Four pure-phased orthorhombic Y1-xCaxMnO3(x=0,0.07,0.55and0.65)samples with fine crystallization and morphologies were successfully synthesizedvia the low-temperature hydrothermal technique. Y1-xCaxMnO3(x=0) andY1-xCaxMnO3(x=0.07) show the behavior of spin glass. Y1-xCaxMnO3(x=0.55)shows obvious charge-ordering, antiferromagnetic transition and the behavior ofspin glass. Y1-xCaxMnO3(x=0.65) shows strong signals of charge ordering andantiferromagnetic transition, but no behavior of spin glass. Drastic increase ofmagnetization at low temperatures was observed in Y1-xCaxMnO3(x=0.65),suggesting the existence of Dzialoshinsky-Moriya anisotropic superexchange.Obvious magnetic hysteresis was observed in Y1-xCaxMnO3(x=0.65) at4K,suggesting the existence of strong local short-range ferromagnetic interaction.Y1-xCaxMnO3(x=0.55) and Y1-xCaxMnO3(x=0.65) show the charge transportbehavior of semiconductors and a small magnetoresistance, and the electricconduction mechanism accords with the variable range hopping mode of thehighly-correlated electrons.
Pure-phased metastable rare-earth orthoferrites RFeO3(R=Pr, Nd, Sm, Eu, Gd,Tb, Dy, Ho, Er, Tm, Yb and Lu) with fine crystallization and morphologies were successfully synthesized via the low-temperature hydrothermal technique. Thefactors that affect the formation of target products such as media alkalinity, reactiontemperature and time etc. were fully studied, and optimum routes were concluded.The crystal structures, morphologies were characterized, and the crystal nucleationand growth mechanism were analyzed. The magnetic properties, including Fe3+antiferromagnetic transition, spin reorientation, spin glass transition, magnetizationreversal, Re3+antiferromagnetic transition, etc., were characterized and discussed.Compared with samples synthesized by solid state sintering in literatures, thesamples in this work show some difference in the magnetic properties, for example,spin reorientation was observed in EuFeO3and LuFeO3.
Pure-phased orthorhombic RMn0.5Fe0.5O3(R=Tb, Dy and Ho) weresuccessfully synthesized via the low-temperature hydrothermal technique. Thecrystal structures, morphologies, chemical compositions and valences, magneticproperties etc. were analyzed. Magnetization reversal was observed inTbFe0.5Mn0.5O3. A high magnetic field can reverse the magnetization direction, andthe spin reorientation temperature has a linear relation with the magnetic fieldintensity. Re3+antiferromagnetic transition was observed in TbFe0.5Mn0.5O3andDyFe0.5Mn0.5O3at low temperatures. The three samples show residual magnetism at2K and300K.
Hexagonal RMn1-xFexO3(R=Er, Tm, Yb and Lu; x=0,0.1,0.3and0.5) weresuccessfully synthesized via the low-temperature hydrothermal technique. Structuralanalysis shows that the samples of ErMnO3and RMn1-xFexO3(R=Tm, Yb and Lu;x=0,0.1,0.3and0.5) are all pure hexagonal phase, but the samples of ErMn1-xFexO3(x=0.1,0.3and0.5) comprise hexagonal phase and orthorhombic phase. Fe dopingstretches the Mn-O bond along the c axis and shortens the Mn-O bond in the a-bplane, thus leading increase of c and decrease of a. The ferromagnetictransformation TNwas elevated by Fe doping and a linear relation was observedbetween ΔTNand Fe doping x.
引文
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