典型的铁磁、铁电氧化物薄膜界面分析与界面控制方法的研究
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摘要
钙钛矿结构的铁电氧化物薄膜和尖晶石结构的铁磁氧化物薄膜因其独特的电、磁学特性和宽广的应用前景受到了材料科学界的广泛关注，成为近年来介质氧化物薄膜研究的热点。在这类复杂结构的氧化物薄膜生长与应用中，存在着大量的表面、界面效应。由于理论研究和实验条件的制约，与界面相关的一些重要物理现象和机理仍不清楚，尤其是界面形成、界面动力学过程以及微结构控制等问题在一定程度上阻碍了介质氧化物薄膜器件的高速发展。本论文采用激光分子束外延生长技术，围绕几种典型的铁电、铁磁氧化物薄膜生长动力学原理以及界面控制方法，对氧化物薄膜的界面结构进行了较为系统的研究，并对界面应力、取向生长改善薄膜电、磁性能方面做了探索性的工作。
首先，论文系统的研究了CoFe_2O_4(CFO)薄膜生长行为及其界面微结构特性。利用激光分子束外延技术(LMBE)，通过对CFO薄膜生长的原位反射高能电子衍射(RHEED)监测发现生长温度和沉积速率共同决定了层状、层岛混合和岛状三种生长模式的转变。通过优化薄膜生长工艺参数实现对CFO铁磁氧化物薄膜生长模式的有效控制，并绘制出CoFe_2O_4／SrTiO_3(STO)体系生长模式相图。根据RHEED强度振荡曲线，利用Arrhenius理论模型分析了CFO／SrTiO_3(STO)异质外延生长中界面粒子弛豫过程，计算得到CFO表面和界面粒子迁移活化能分别为0．6eV和1．6eV，证明界面粒子需克服晶格失配造成的晶格扭结势垒Es而表现出更大的界面迁移活化能。通过透射电子显微镜(TEM)观察到不同生长模式下界面微结构的差异。在STO单晶基片上650℃，1．25(?)／sec岛状生长的CFO薄膜厚度超过临界厚度(5nm)将产生塑性形变形成失配位错，位错的Burgers矢量为a〈010〉，密度为1．25×10~8m~(-1)。实测位错密度值略小于理论计算值2×10~8m~(-1)，这表明部分失配应力以弹性应变的方式残留于薄膜内；而在同样温度下，以0．5(?)／sec沉积速率层状外延生长的CFO薄膜通过弹性应变方式释放失配应力，厚度超过15nm仍未观察到明显的失配位错形成。研究表明CFO外延薄膜界面的微结构由弹性应变和塑性形变共同决定。
在界面微结构特性研究的基础上，利用界面应力调制CFO异质外延薄膜的微结构并对其性能展开了深入的探讨。采用LMBE技术系统研究了正／负失配下CFO薄膜的应力释放行为以及应变CFO薄膜的磁化特性。研究表明不同界面应力导致CFO薄膜异质外延生长过程中产生非对称界面生长现象，即张应力通过弹性应变使薄膜晶胞畸变，逐层释放应变；压应力通过改变薄膜界面结构来释放应力。通过应力调制作用，首次在应变的CFO／STO体系中得到明显的磁晶各向异性。垂直方向([001])和水平方向([100]／[010])的剩余磁化强度(Mr)分别为190 emu／cm~3和150emu／cm~3，垂直与水平方向的矫顽场差异达到3倍以上。另一方面，利用界面应力调制BaTiO_3(BTO)／CFO／Nb-STO异质外延薄膜微结构，深入的研究了界面应力对复合异质薄膜铁电、铁磁性能的影响。首次通过X射线倒易空间扫描图精确获得BTO／CFO内晶格常数，并利用晶格常数方法计算得到随BTO厚度变化的残余应力分布状态，初步建立了多元氧化物异质外延薄膜有序结构中应力分布及弛豫模型。电性能测试表明BTO／CFO／STO异质外延体系中张应力的释放有利于铁电性的恢复。
其次，采用激光脉冲沉积方法，从界面热力学角度系统研究了Pb(Zr_(1-x)Ti_x)O_3(PZT)铁电薄膜在不同氧化物基片上取向外延生长行为及其界面特性。利用界面双晶外延生长机理实现了PZT薄膜在MgO(100)基片以(110)面取向外延生长。另外，从晶化动力学角度系统研究了后退火工艺中界面反应对PZT多晶薄膜择优取向生长的影响。通过改变升温速率有效控制PZT薄膜在界面异质成核并以(111)面择优生长，绘制出择优取向生长相图，并研究了不同取向PZT薄膜的电性能差异。
最后，采用LMBE技术，以STO缓冲层实现BTO铁电薄膜在GaAs基片上c向外延生长，并对这种大晶格失配体系的界面控制方法进行了深入研究。根据近重位点阵生长机理，STO晶格通过面内45°旋转以减小与GaAs晶格失配。TEM界面研究发现这种非共格界面生长关系造成STO出现高位错密度界面层，且位错延伸至BTO内导致性能退化。首次利用临界厚度效应生长低于临界厚度的STO弹性应变界面层，获得STO缓冲层最优生长厚度为12-16ML之间。此时BTO受到STO缓冲层面内压应力，在均匀应变的STO表面以层状模式外延生长形成应变异质结，从而在原子尺度改善了BTO／STO／GaAs异质结界面结构。电性能测试表明Pt／BTO／STO／GaAs应变异质结表现出良好的极化特性，2Pr为6．5μC／cm~2，±5V偏压下漏电流低于4×10~(-6)A／cm~2，较文献报道同类GaAs基异质结有显著提升，达到器件应用要求。
Owing to their versatile ferroelectric and magnetic function and wide application,the oxidethin films with peroviskite and spinel structure have attracted much attention,and became thekey point in the electronic material studies recently.In the growth and application of thecomplex oxide thin films,it is inevitable that the surface and interface affect the electronicsystems.Due to the limit of the theoretical and experimental condition,the related theory andmechanism of the interface is still lacking including the growth mechanism and dynamics ofinterface and the control of the interface microstructure.Especially when the thickness of thefilms reaches the nanometer level,the unclear problems has become noticeable,which hasstrongly prevented the development of these functional oxide films.In this dissertation,basedon the epitaxial growth mechanism and dynamic of oxide thin film and the method of theinterface control,the interface microstructure and its effect on the physical properties offerroelectric and ferromagnetic films has been systematically studied by experiments with theLaser Molecular Beam Epitaxy techniques (LMBE),including the interface strain modulation,growth orientation and their effects on the electric and magnetic properties.
Firstly,the growth behavior and interface microstrucutre of CFO thin film grown byLMBE with an in-situ reflective high energy electron diffraction (RHEED) were systematicallystudied.It was found that the layer-by-layer,island and Strnaski-Krastanov (layer-by-layer plusisland) growth modes were determined by the growth temperature and deposition rate.Therefore,the growth modes of CFO could be precisely controlled by varying the depositionparameters and hence the growth mode map of the CFO/STO was obtained as a function of thesubstrate temperature for various laser repetition rates.On the other hand,the process ofinterface relaxation was analysised according to the RHEED oscillation and the activity energyfor the particle migration both at surface and interface of the CFO films were calculated to be0.6 eV and 1.6 eV by the Arrhenius theory,respectively.It proves that the particles at interfaceneed more activity energy for migration than these at surface due to the high lattice distortionbarrier (Es) induced by the lattice mismatch.In order to reveal the difference of interfacestructure between the films with island or layer-by-layer growth mode,the TEM technique wasemployed to investigate the cross-sectional characteristic of the CFO films.It was found that theCFO epitaxially grown on STO substrate at the temperature of 650℃and deposition rate of1.25(?)/sec exhibited island growth mode.The misfit dislocations with Burgers vector a<010> occured when the CFO thickness exceeded the critical thickness about 5nm.The misfit densityof the dislocation could be measured to be 1.25×10~8m~(-1),which was less than the value of2×10~8m~(-1) by theoretical calculation.Actually,part of lattice mismatch stress was released bylattice strain;while the CFO grown on STO substrate at the same temperature and depositionrate of 0.5(?)/sec exhibited layer-by-layer growth mode.It was noted that any misfit dislocationcould be observed even in the CFO film with thickness beyond 15nm,which suggested that thelattice mismatch stress in CFO film was released by lattice strain.Therefore,the interfacemicrostructure of CFO film was mainly determined by the lattice strain and dislocation energy.
Based on the study of the interface microstructure,we extensively studied the influence ofthe interface-stress modulation on the microstructure and physical properties of theseheteroepitaxial CFO thin films.First,the stress relaxation and its effects on the magnetism ofthe CFO were systematically studied in the CFO thin films epitaxially grown under the tensileand compressive stress induced by substrates.An asymmetrical growth behavior due to interfacestress was found during the heteroepitaxial growth of the CFO,which could be described thatthe tensile stress was relaxed by changing the lattice constant,while the compressive stress wasrelaxed by changing the interface structure.By stress modulation,a strong magnetic anisotropywas obtained in the compressive strained CFO heteroepitaxial film.The remanent magnetism(Mr) in the vertical ([001]) and parallel ([100]/[010]) direction of compressive strained CFOfilm was measured to be 190 emu/cm~3 and 150 emu/cm~3,respectively.Besides,the coercivemagnetic field (Hc) in the vertical direction was three times that in parallel direction.Furthermore,we systematically studied the influence of stress modulation on the microstructureand the physical properties including ferroelectric and magnetic properties in heteroeptaxiallygrown BaTiO_3(BTO)/CFO/Nb-STO films.The lattice parameters were precisely obtained byX-ray Reciprocal Space Mapping and the residual stress was calculated using the latticeparameter method.A residual stress theoretical model about the relaxation mechanisms of stressin complex oxide heteroepitaxial films with ordered structure was put forward for bettercomprehension of the dependence between thickness and stress.Furthermore,the electricalmeasurement results show that the ferroelectric properties were enhanced with the relaxation ofthe tensile stress in BTO/CFO/STO heteroepitaxial system.
Secondly,based on the principle of interface thermodynamics,the oriented growthbehavior of the Pb(Zr_(1-x)Ti_x)O_3 (PZT) films epitaxially grown by pulsed laser depositiontechnique were systematically studied.According to bicrystalline epitaxial growth mechanism atinterface,the (110)-oriented PZT ferroelectric films were epitaxially grown on MgO(100) substrates.On the other hand,the hetero-nuclear PZT polycrystalline film with (111)-texturecould be obtained by precisely controlling the heating rate.Therefore,the textured growth mapof the polycrystalline PZT was obtained as a function of the substrate temperature for vaviousheating rates.The electrical properties of the texture PZT films were also measured.
Finally,the c-oriented BTO ferroelectric thin films were successfully epitaxially grown onGaAs substrate by using LMBE technique via STO as buffer layer.The interface control methodwas extensively studied in the large lattice mismatch system.According to the NearlyCoincidence Site Lattice (NSCL) theory,the lattice mismatch was reduced by the 45°rotation ofthe STO lattice.The interface was investigated by TEM technique.It was found that theinterface with high density of misfit dislocation in noncoincidence-site growth caused thedegradation of the electrical properties.By inserting a strained interfacial buffer layer of STObelow the critical thickness,a well ordered interface at atomic scale could be obtained in thestrained BTO/STO/GaAs heterostructure.The favor thickness of STO buffer should becontrolled between 12-16 monolayers.The BTO was grown on STO buffer in layer-by-layergrowth mode with an in-plane compressive strain induced by the STO.Compared with thesimilar heterostructure grown on GaAs,The strained Pt/BTO/STO/GaAs heterostructre exhibitsexcellent electrical performance with a 2Pr of 6.5μC/cm~2 and leakage current below4×10~(-6)A/cm~2 at the voltage bias of±5V,which is suitable for device application.
首先，论文系统的研究了CoFe_2O_4(CFO)薄膜生长行为及其界面微结构特性。利用激光分子束外延技术(LMBE)，通过对CFO薄膜生长的原位反射高能电子衍射(RHEED)监测发现生长温度和沉积速率共同决定了层状、层岛混合和岛状三种生长模式的转变。通过优化薄膜生长工艺参数实现对CFO铁磁氧化物薄膜生长模式的有效控制，并绘制出CoFe_2O_4／SrTiO_3(STO)体系生长模式相图。根据RHEED强度振荡曲线，利用Arrhenius理论模型分析了CFO／SrTiO_3(STO)异质外延生长中界面粒子弛豫过程，计算得到CFO表面和界面粒子迁移活化能分别为0．6eV和1．6eV，证明界面粒子需克服晶格失配造成的晶格扭结势垒Es而表现出更大的界面迁移活化能。通过透射电子显微镜(TEM)观察到不同生长模式下界面微结构的差异。在STO单晶基片上650℃，1．25(?)／sec岛状生长的CFO薄膜厚度超过临界厚度(5nm)将产生塑性形变形成失配位错，位错的Burgers矢量为a〈010〉，密度为1．25×10~8m~(-1)。实测位错密度值略小于理论计算值2×10~8m~(-1)，这表明部分失配应力以弹性应变的方式残留于薄膜内；而在同样温度下，以0．5(?)／sec沉积速率层状外延生长的CFO薄膜通过弹性应变方式释放失配应力，厚度超过15nm仍未观察到明显的失配位错形成。研究表明CFO外延薄膜界面的微结构由弹性应变和塑性形变共同决定。
在界面微结构特性研究的基础上，利用界面应力调制CFO异质外延薄膜的微结构并对其性能展开了深入的探讨。采用LMBE技术系统研究了正／负失配下CFO薄膜的应力释放行为以及应变CFO薄膜的磁化特性。研究表明不同界面应力导致CFO薄膜异质外延生长过程中产生非对称界面生长现象，即张应力通过弹性应变使薄膜晶胞畸变，逐层释放应变；压应力通过改变薄膜界面结构来释放应力。通过应力调制作用，首次在应变的CFO／STO体系中得到明显的磁晶各向异性。垂直方向([001])和水平方向([100]／[010])的剩余磁化强度(Mr)分别为190 emu／cm~3和150emu／cm~3，垂直与水平方向的矫顽场差异达到3倍以上。另一方面，利用界面应力调制BaTiO_3(BTO)／CFO／Nb-STO异质外延薄膜微结构，深入的研究了界面应力对复合异质薄膜铁电、铁磁性能的影响。首次通过X射线倒易空间扫描图精确获得BTO／CFO内晶格常数，并利用晶格常数方法计算得到随BTO厚度变化的残余应力分布状态，初步建立了多元氧化物异质外延薄膜有序结构中应力分布及弛豫模型。电性能测试表明BTO／CFO／STO异质外延体系中张应力的释放有利于铁电性的恢复。
其次，采用激光脉冲沉积方法，从界面热力学角度系统研究了Pb(Zr_(1-x)Ti_x)O_3(PZT)铁电薄膜在不同氧化物基片上取向外延生长行为及其界面特性。利用界面双晶外延生长机理实现了PZT薄膜在MgO(100)基片以(110)面取向外延生长。另外，从晶化动力学角度系统研究了后退火工艺中界面反应对PZT多晶薄膜择优取向生长的影响。通过改变升温速率有效控制PZT薄膜在界面异质成核并以(111)面择优生长，绘制出择优取向生长相图，并研究了不同取向PZT薄膜的电性能差异。
最后，采用LMBE技术，以STO缓冲层实现BTO铁电薄膜在GaAs基片上c向外延生长，并对这种大晶格失配体系的界面控制方法进行了深入研究。根据近重位点阵生长机理，STO晶格通过面内45°旋转以减小与GaAs晶格失配。TEM界面研究发现这种非共格界面生长关系造成STO出现高位错密度界面层，且位错延伸至BTO内导致性能退化。首次利用临界厚度效应生长低于临界厚度的STO弹性应变界面层，获得STO缓冲层最优生长厚度为12-16ML之间。此时BTO受到STO缓冲层面内压应力，在均匀应变的STO表面以层状模式外延生长形成应变异质结，从而在原子尺度改善了BTO／STO／GaAs异质结界面结构。电性能测试表明Pt／BTO／STO／GaAs应变异质结表现出良好的极化特性，2Pr为6．5μC／cm~2，±5V偏压下漏电流低于4×10~(-6)A／cm~2，较文献报道同类GaAs基异质结有显著提升，达到器件应用要求。
Owing to their versatile ferroelectric and magnetic function and wide application,the oxidethin films with peroviskite and spinel structure have attracted much attention,and became thekey point in the electronic material studies recently.In the growth and application of thecomplex oxide thin films,it is inevitable that the surface and interface affect the electronicsystems.Due to the limit of the theoretical and experimental condition,the related theory andmechanism of the interface is still lacking including the growth mechanism and dynamics ofinterface and the control of the interface microstructure.Especially when the thickness of thefilms reaches the nanometer level,the unclear problems has become noticeable,which hasstrongly prevented the development of these functional oxide films.In this dissertation,basedon the epitaxial growth mechanism and dynamic of oxide thin film and the method of theinterface control,the interface microstructure and its effect on the physical properties offerroelectric and ferromagnetic films has been systematically studied by experiments with theLaser Molecular Beam Epitaxy techniques (LMBE),including the interface strain modulation,growth orientation and their effects on the electric and magnetic properties.
Firstly,the growth behavior and interface microstrucutre of CFO thin film grown byLMBE with an in-situ reflective high energy electron diffraction (RHEED) were systematicallystudied.It was found that the layer-by-layer,island and Strnaski-Krastanov (layer-by-layer plusisland) growth modes were determined by the growth temperature and deposition rate.Therefore,the growth modes of CFO could be precisely controlled by varying the depositionparameters and hence the growth mode map of the CFO/STO was obtained as a function of thesubstrate temperature for various laser repetition rates.On the other hand,the process ofinterface relaxation was analysised according to the RHEED oscillation and the activity energyfor the particle migration both at surface and interface of the CFO films were calculated to be0.6 eV and 1.6 eV by the Arrhenius theory,respectively.It proves that the particles at interfaceneed more activity energy for migration than these at surface due to the high lattice distortionbarrier (Es) induced by the lattice mismatch.In order to reveal the difference of interfacestructure between the films with island or layer-by-layer growth mode,the TEM technique wasemployed to investigate the cross-sectional characteristic of the CFO films.It was found that theCFO epitaxially grown on STO substrate at the temperature of 650℃and deposition rate of1.25(?)/sec exhibited island growth mode.The misfit dislocations with Burgers vector a<010> occured when the CFO thickness exceeded the critical thickness about 5nm.The misfit densityof the dislocation could be measured to be 1.25×10~8m~(-1),which was less than the value of2×10~8m~(-1) by theoretical calculation.Actually,part of lattice mismatch stress was released bylattice strain;while the CFO grown on STO substrate at the same temperature and depositionrate of 0.5(?)/sec exhibited layer-by-layer growth mode.It was noted that any misfit dislocationcould be observed even in the CFO film with thickness beyond 15nm,which suggested that thelattice mismatch stress in CFO film was released by lattice strain.Therefore,the interfacemicrostructure of CFO film was mainly determined by the lattice strain and dislocation energy.
Based on the study of the interface microstructure,we extensively studied the influence ofthe interface-stress modulation on the microstructure and physical properties of theseheteroepitaxial CFO thin films.First,the stress relaxation and its effects on the magnetism ofthe CFO were systematically studied in the CFO thin films epitaxially grown under the tensileand compressive stress induced by substrates.An asymmetrical growth behavior due to interfacestress was found during the heteroepitaxial growth of the CFO,which could be described thatthe tensile stress was relaxed by changing the lattice constant,while the compressive stress wasrelaxed by changing the interface structure.By stress modulation,a strong magnetic anisotropywas obtained in the compressive strained CFO heteroepitaxial film.The remanent magnetism(Mr) in the vertical ([001]) and parallel ([100]/[010]) direction of compressive strained CFOfilm was measured to be 190 emu/cm~3 and 150 emu/cm~3,respectively.Besides,the coercivemagnetic field (Hc) in the vertical direction was three times that in parallel direction.Furthermore,we systematically studied the influence of stress modulation on the microstructureand the physical properties including ferroelectric and magnetic properties in heteroeptaxiallygrown BaTiO_3(BTO)/CFO/Nb-STO films.The lattice parameters were precisely obtained byX-ray Reciprocal Space Mapping and the residual stress was calculated using the latticeparameter method.A residual stress theoretical model about the relaxation mechanisms of stressin complex oxide heteroepitaxial films with ordered structure was put forward for bettercomprehension of the dependence between thickness and stress.Furthermore,the electricalmeasurement results show that the ferroelectric properties were enhanced with the relaxation ofthe tensile stress in BTO/CFO/STO heteroepitaxial system.
Secondly,based on the principle of interface thermodynamics,the oriented growthbehavior of the Pb(Zr_(1-x)Ti_x)O_3 (PZT) films epitaxially grown by pulsed laser depositiontechnique were systematically studied.According to bicrystalline epitaxial growth mechanism atinterface,the (110)-oriented PZT ferroelectric films were epitaxially grown on MgO(100) substrates.On the other hand,the hetero-nuclear PZT polycrystalline film with (111)-texturecould be obtained by precisely controlling the heating rate.Therefore,the textured growth mapof the polycrystalline PZT was obtained as a function of the substrate temperature for vaviousheating rates.The electrical properties of the texture PZT films were also measured.
Finally,the c-oriented BTO ferroelectric thin films were successfully epitaxially grown onGaAs substrate by using LMBE technique via STO as buffer layer.The interface control methodwas extensively studied in the large lattice mismatch system.According to the NearlyCoincidence Site Lattice (NSCL) theory,the lattice mismatch was reduced by the 45°rotation ofthe STO lattice.The interface was investigated by TEM technique.It was found that theinterface with high density of misfit dislocation in noncoincidence-site growth caused thedegradation of the electrical properties.By inserting a strained interfacial buffer layer of STObelow the critical thickness,a well ordered interface at atomic scale could be obtained in thestrained BTO/STO/GaAs heterostructure.The favor thickness of STO buffer should becontrolled between 12-16 monolayers.The BTO was grown on STO buffer in layer-by-layergrowth mode with an in-plane compressive strain induced by the STO.Compared with thesimilar heterostructure grown on GaAs,The strained Pt/BTO/STO/GaAs heterostructre exhibitsexcellent electrical performance with a 2Pr of 6.5μC/cm~2 and leakage current below4×10~(-6)A/cm~2 at the voltage bias of±5V,which is suitable for device application.
引文
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