典型磁性金属及过渡金属氧化物薄膜结构、电磁性能的应变调控
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摘要
利用应变来调控材料宏观物理性质的过程,称其为“应变工程”(strain engineering)。研究表明,应变可以有效调控半导体材料的能带结构、超导体的临界温度、庞磁电阻材料的相分离、铁电体极化状态、铁氧体的共振频率以及多铁体的磁电耦合等物理现象。这些现象本质在于应变通过晶格改变了电荷、轨道、自旋自由度间的竞争及其强关联作用。基于应变调控技术,人们发展了可应变调控的半导体发光二极管、铁氧体微波器件、高灵敏度磁场传感器以及高密度低功耗磁电存储器等新型器件,这些具有极大潜在应用前景的新器件亦将应变调控研究推向了国际前沿。本论文选择该方向,研究应变对过渡金属及其氧化物薄膜材料电磁性质和晶畴结构的调控作用,理解这些材料宏观物理性能和应变的耦合关系,构造并演示一些新型多功能薄膜原型器件(如应变调控的磁电存储器等)。具体地,本论文研究了对尖晶石结构的(001)-Zn0.4Fe2.6O4(ZFO)、钙钛矿结构(011)-La0.67Sr0.33Mn03(LSMO)、多层膜人工纳米结构的磁隧道结(Magnetic Tunnel Junction (MTJ))在压电衬底铌镁钛酸铅(0.7Pb(Mg2/3Nbi/3)O3-0.3PbTiO3(PMN-0.3PT))原位应变作用下电磁性质的变化,获得了薄膜电磁性能等对应变的依赖关系。研究中,采用了高分辨同步辐射X射线衍射技术表征样品的微观结构、晶格应变随衬底外加电场的变化情况。
第一章介绍了应变调控技术的研究背景以及目前存在的主要问题。首先,我们回顾应变工程取得的重要进展；其次,我们介绍了应变工程在多铁性材料研究中的应用,回顾了应变调控磁电性能的研究进展,指出应用复合磁电材料实现应变调控磁电性能的优势所在。最后给出本论文的研究对象、内容以及拟解决的关键科学问题。
第二章简单介绍了应变调控磁性的物理基础,介绍了一些磁性物理的基本概念,给出宏观热力学理论框架下磁电耦合的唯象解释,为论文中的理论分析做准备。
第三章,简要介绍论文工作用到的关键实验技术,包括高质量薄膜制备工艺、同步辐射高分辨X-ray衍射技术、原位电场控制下的磁化强度测量技术以及磁电阻测量平台的软、硬件设计。
第四章,我们选择具有半导体属性的磁性铁氧体Zn2.6Fe0.4O4作为研究对象,开展ZFO薄膜结构和电磁性能的静态(SrTiO3(STO)衬底)和动态应变调控研究。在低温低气压下,利用射频磁控溅射工艺在0.7Pb(Mg1/3Nb2/3)O3-0.3PbTiO3(PMN-0.3PT)上成功生长了极低粗糙度和高外延质量的Zn2.6Fe0.4O4(ZFO)薄膜。我们在ZFO/STO外延薄膜中发现了奇异的应变行为,可能起源于ZFO的V-W生长方式。在ZFO/PMN-0.3PT中,我们发现室温电阻率(调控率-0.1%)和磁化强度(调控率～1.1%)随着应变的增大分别降低和增强。这一结果可能是因为PMN-PT衬底产生的压应变增强了ZFO薄膜中Fe2+和Fe3+的双交换作用所致。该研究成果为应用电场调控磁化强度和电阻率实现多态存储和电写磁读器件提供了实验支持。
第五章,为了增强室温下应变调控剩余磁化强度的力度,我们在[011]取向的PMN-PT上外延生长了La0.67Sr0.33MnO3(LSMO)半金属薄膜。面内各向异性应变的引入可以很好的调控LSMO的剩余磁化强度。我们发现沿着面内[100]和[011]两个方向的剩余磁化强度与电场有着相反的变化关系：沿着[100]方向,剩余磁化强度随着电场增大而减小；沿着[011]方向,剩余磁化强度随着电场增大而增大。这一结果起源于面内各向异性应变作用下易磁化轴从[100]向[011]方向的转动。我们在这一体系中发现了巨大的磁电耦合效应(沿着[100]方向的调控率约-17.9%,沿着[011]方向调控率高达+157%),与国际水平在同一量级上。另外,我们利用衬底诱导的原位应变来调控LSMO的电输运性能,获得了应变调控的非挥发性多电阻态,进而利用脉冲电场实现了多电阻态的写入与擦除。这两方面的结果对于开发新型的电控多态存储器件有着重要的指导意义。
第六章,我们研究了PMN-PT上生长的磁隧道结(MTJ)输运性能。发现应变可以调控MTJ的电阻态,实现了MTJ自由层CoFeB磁化强度的1800翻转,我们认为这一结果起源于应变改变了MTJ自由层的有效磁各向异性。这一结果表明我们向室温下电场写入磁场读出的磁电存储元器件又迈向了重要一步。
"Strain engineering" is a means to manipulating physical properties of films using strain. It is proven that strain is an effective method to tune the band structures of semicondutors, critical temperature of superconductors, phase separation of colossal manganites, polarized states of ferroelectric, resonant frequency of ferrites and magnetoelectric coupling of multiferroics, etc.. The mechanism of these phenomena lies in the strain-tunable competing of charge, orbit, spin and lattice freedoms and strong interactions among them. Consequently, strain engineering is now regarded as an emergent object in condensed matter physics all over the world.
On the other hand, a large amount of promising devices based on the strain engineering have bee proposed, for example, strain-controlled light emitting diode, ferrite microwave devices, high sensitive magnetic field sensors and magnetoelectric memory with high density and low power cost. Therefore, this thesis studies the influences of strain on the electrical and magnetic properties, and crystal structures in metal and oxide films, and show the coupling between properties and strain, and then develops and demonstrates some prototype of novel and multifunctional devices (for example, strain-controlled magnetoelectric memory).
We chose spinel (001)-Zno.4Fe2.604(ZFO) and pervoskite (011)-La2/3Sr1/3MnO3(LSMO) as the typical transition metal oxide films, and artificially nano-structure magnetic tunnel junctions as CoFeB/MgO/CoFeB/Ru/CoFe/IrMn/CoFe multilayers. The in situ strain induced by electric field in0.7Pb(Mg2/3Nbi/3)O3-0.3PbTiO3(PMN-0.3PT) substate is used to tune the strain states in the above films or structures and then we figure out the relationships between properties and strain. The strian in the films as a function of electric field applied to the PMN-0.3PT will be characterized by high resolution sychrotron radiation X-ray diffraction. Combined with the characaterization of the electrical and magnetic properties, we studied systematicially the strain-properties in the above films and provide an effective route to tune the magnetization and transport properties with strain. With the help of strain-property relations, we constructed a non-volatile and multi-state memory by strain through cotrolling polarization switching of the PMN-0.3PT substrates. Our reseach will give a better understandings of the coupling among the intrinsic freedoms, and also contributes to the technique of "straintronics".
In chapter one, we will introduce some backgrounds of strain engineering and problems in this field. The routes of electric-field-controlled magnetization are summarized and we will emphasize the advantages of strain engineering for electric-field-controlled magnetic and electrical properties. At last, the research objects, contents, and key scientific problems will be listed.
In chapter two, we introduce some fundamental physics on for electric-field-controlled magnetization and some physics concepts on magnetism. We will give an interpretation about magnetoelectric coupling in the frame of phenomenological thermodynamics.
In chapter three, some important techniques for sample fabrications and processings, will be introduced, including synchrotron radiation high resolution X-ray diffraction, strain measurements, magnetization measurements under in situ strain and design of magnetoresistance measurement system.
In chapter four, magnetic semiconductor oxide film ZFO was chosen as one typical system for static (on SrTiO3(STO) substrates) and dynamic strain engneering. We observed the anomalous strain states in the ZFO/STO films, originating from the V-W growth mode.(001)-ZFO/PMN-0.3PT epitaxial heterostructures have been investigated to demonstrate the electric-field-controlled resistance and magnetization switching at room temperature. The tunabilitiy of resistance of the ZFO film is about-0.1%under the in-plane strain-0.02%at296K, and the tunabilitiy of magnetization is about1.1%under the in-plane strain-0.11%at296K. A possible microscopic mechanism of the manipulation of resistance and magnetization is the enhancement of hopping amplitude of electrons between mixed-valent Fe2+and Fe3+ions under the electric-field-induced in-plane compressive strain.
In chapter five, for a larger electric-field-controlled remnant magnetization, we choose the (011)-PMN-0.3PT substrate with anisotropic in-plane strain and grow half metallic LSMO expitaxial films on it. A large anisotropic remnant magnetization tunability was observed in multiferroic (011)-LSMO/PMN-0.3PT epitaxial heterostructures. The remnant magnetization along [100] direction was suppressed by an electric field applied to the substrate while the remnant magnetization along [011] was enhanced. The tunabilities of the remnant magnetization along the [100] and [011] directions are about-17.9%and+157%under electric field of+7.27kV/cm, respectively. We also found non-volatile and multi-state resistance in this heterostructures at room temperature. This large anisotropic remnant magnetization tunability and non-volatile resistance states may find potential applications in the electrically written and magnetically read memories.
In chapter six, we studied transportation properties of MTJs/PMN-0.3PT heterostructures. The details of MTJs fabrication and processing procedures are presented. The180°switching of magnetization is observed under in situ strain. We believe that the electric-field-controlled magnetization switching originated from electric-field-induced change of magnetic anisotropy of CoFeB free layer. Our results show that a progressive step towards to electrically written and magnetically read memories.
第一章介绍了应变调控技术的研究背景以及目前存在的主要问题。首先,我们回顾应变工程取得的重要进展；其次,我们介绍了应变工程在多铁性材料研究中的应用,回顾了应变调控磁电性能的研究进展,指出应用复合磁电材料实现应变调控磁电性能的优势所在。最后给出本论文的研究对象、内容以及拟解决的关键科学问题。
第二章简单介绍了应变调控磁性的物理基础,介绍了一些磁性物理的基本概念,给出宏观热力学理论框架下磁电耦合的唯象解释,为论文中的理论分析做准备。
第三章,简要介绍论文工作用到的关键实验技术,包括高质量薄膜制备工艺、同步辐射高分辨X-ray衍射技术、原位电场控制下的磁化强度测量技术以及磁电阻测量平台的软、硬件设计。
第四章,我们选择具有半导体属性的磁性铁氧体Zn2.6Fe0.4O4作为研究对象,开展ZFO薄膜结构和电磁性能的静态(SrTiO3(STO)衬底)和动态应变调控研究。在低温低气压下,利用射频磁控溅射工艺在0.7Pb(Mg1/3Nb2/3)O3-0.3PbTiO3(PMN-0.3PT)上成功生长了极低粗糙度和高外延质量的Zn2.6Fe0.4O4(ZFO)薄膜。我们在ZFO/STO外延薄膜中发现了奇异的应变行为,可能起源于ZFO的V-W生长方式。在ZFO/PMN-0.3PT中,我们发现室温电阻率(调控率-0.1%)和磁化强度(调控率～1.1%)随着应变的增大分别降低和增强。这一结果可能是因为PMN-PT衬底产生的压应变增强了ZFO薄膜中Fe2+和Fe3+的双交换作用所致。该研究成果为应用电场调控磁化强度和电阻率实现多态存储和电写磁读器件提供了实验支持。
第五章,为了增强室温下应变调控剩余磁化强度的力度,我们在[011]取向的PMN-PT上外延生长了La0.67Sr0.33MnO3(LSMO)半金属薄膜。面内各向异性应变的引入可以很好的调控LSMO的剩余磁化强度。我们发现沿着面内[100]和[011]两个方向的剩余磁化强度与电场有着相反的变化关系：沿着[100]方向,剩余磁化强度随着电场增大而减小；沿着[011]方向,剩余磁化强度随着电场增大而增大。这一结果起源于面内各向异性应变作用下易磁化轴从[100]向[011]方向的转动。我们在这一体系中发现了巨大的磁电耦合效应(沿着[100]方向的调控率约-17.9%,沿着[011]方向调控率高达+157%),与国际水平在同一量级上。另外,我们利用衬底诱导的原位应变来调控LSMO的电输运性能,获得了应变调控的非挥发性多电阻态,进而利用脉冲电场实现了多电阻态的写入与擦除。这两方面的结果对于开发新型的电控多态存储器件有着重要的指导意义。
第六章,我们研究了PMN-PT上生长的磁隧道结(MTJ)输运性能。发现应变可以调控MTJ的电阻态,实现了MTJ自由层CoFeB磁化强度的1800翻转,我们认为这一结果起源于应变改变了MTJ自由层的有效磁各向异性。这一结果表明我们向室温下电场写入磁场读出的磁电存储元器件又迈向了重要一步。
"Strain engineering" is a means to manipulating physical properties of films using strain. It is proven that strain is an effective method to tune the band structures of semicondutors, critical temperature of superconductors, phase separation of colossal manganites, polarized states of ferroelectric, resonant frequency of ferrites and magnetoelectric coupling of multiferroics, etc.. The mechanism of these phenomena lies in the strain-tunable competing of charge, orbit, spin and lattice freedoms and strong interactions among them. Consequently, strain engineering is now regarded as an emergent object in condensed matter physics all over the world.
On the other hand, a large amount of promising devices based on the strain engineering have bee proposed, for example, strain-controlled light emitting diode, ferrite microwave devices, high sensitive magnetic field sensors and magnetoelectric memory with high density and low power cost. Therefore, this thesis studies the influences of strain on the electrical and magnetic properties, and crystal structures in metal and oxide films, and show the coupling between properties and strain, and then develops and demonstrates some prototype of novel and multifunctional devices (for example, strain-controlled magnetoelectric memory).
We chose spinel (001)-Zno.4Fe2.604(ZFO) and pervoskite (011)-La2/3Sr1/3MnO3(LSMO) as the typical transition metal oxide films, and artificially nano-structure magnetic tunnel junctions as CoFeB/MgO/CoFeB/Ru/CoFe/IrMn/CoFe multilayers. The in situ strain induced by electric field in0.7Pb(Mg2/3Nbi/3)O3-0.3PbTiO3(PMN-0.3PT) substate is used to tune the strain states in the above films or structures and then we figure out the relationships between properties and strain. The strian in the films as a function of electric field applied to the PMN-0.3PT will be characterized by high resolution sychrotron radiation X-ray diffraction. Combined with the characaterization of the electrical and magnetic properties, we studied systematicially the strain-properties in the above films and provide an effective route to tune the magnetization and transport properties with strain. With the help of strain-property relations, we constructed a non-volatile and multi-state memory by strain through cotrolling polarization switching of the PMN-0.3PT substrates. Our reseach will give a better understandings of the coupling among the intrinsic freedoms, and also contributes to the technique of "straintronics".
In chapter one, we will introduce some backgrounds of strain engineering and problems in this field. The routes of electric-field-controlled magnetization are summarized and we will emphasize the advantages of strain engineering for electric-field-controlled magnetic and electrical properties. At last, the research objects, contents, and key scientific problems will be listed.
In chapter two, we introduce some fundamental physics on for electric-field-controlled magnetization and some physics concepts on magnetism. We will give an interpretation about magnetoelectric coupling in the frame of phenomenological thermodynamics.
In chapter three, some important techniques for sample fabrications and processings, will be introduced, including synchrotron radiation high resolution X-ray diffraction, strain measurements, magnetization measurements under in situ strain and design of magnetoresistance measurement system.
In chapter four, magnetic semiconductor oxide film ZFO was chosen as one typical system for static (on SrTiO3(STO) substrates) and dynamic strain engneering. We observed the anomalous strain states in the ZFO/STO films, originating from the V-W growth mode.(001)-ZFO/PMN-0.3PT epitaxial heterostructures have been investigated to demonstrate the electric-field-controlled resistance and magnetization switching at room temperature. The tunabilitiy of resistance of the ZFO film is about-0.1%under the in-plane strain-0.02%at296K, and the tunabilitiy of magnetization is about1.1%under the in-plane strain-0.11%at296K. A possible microscopic mechanism of the manipulation of resistance and magnetization is the enhancement of hopping amplitude of electrons between mixed-valent Fe2+and Fe3+ions under the electric-field-induced in-plane compressive strain.
In chapter five, for a larger electric-field-controlled remnant magnetization, we choose the (011)-PMN-0.3PT substrate with anisotropic in-plane strain and grow half metallic LSMO expitaxial films on it. A large anisotropic remnant magnetization tunability was observed in multiferroic (011)-LSMO/PMN-0.3PT epitaxial heterostructures. The remnant magnetization along [100] direction was suppressed by an electric field applied to the substrate while the remnant magnetization along [011] was enhanced. The tunabilities of the remnant magnetization along the [100] and [011] directions are about-17.9%and+157%under electric field of+7.27kV/cm, respectively. We also found non-volatile and multi-state resistance in this heterostructures at room temperature. This large anisotropic remnant magnetization tunability and non-volatile resistance states may find potential applications in the electrically written and magnetically read memories.
In chapter six, we studied transportation properties of MTJs/PMN-0.3PT heterostructures. The details of MTJs fabrication and processing procedures are presented. The180°switching of magnetization is observed under in situ strain. We believe that the electric-field-controlled magnetization switching originated from electric-field-induced change of magnetic anisotropy of CoFeB free layer. Our results show that a progressive step towards to electrically written and magnetically read memories.
引文
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