前钙钛矿、钙钛矿氧化物纳米结构的可控制备、微结构和性能研究
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摘要
低维钙钛矿结构氧化物,尤其是一维钙钛矿氧化物,因其在铁电非挥发性存储器(FeRAM)、压电纳米发电机和压电纳米传感器等方面的潜在应用而备受关注。开展一维钙钛矿纳米材料的可控制备、微结构与性能的研究对于发现新现象、拓展新应用具有重要的理论意义和实际价值。
本文首先简要综述了钙钛矿结构氧化物的结构特点与研究现状,并重点总结和评述了一维钙钛矿铁电氧化物纳米结构的制备及性能研究。在这一方面,实验研究明显滞后于相关的理论研究,其主要原因在于一维钙钛矿铁电氧化物单晶纳米结构的可控制备仍是一个挑战。针对这一问题,本文首次通过高分子辅助水热方法合成出尺寸可控前钙钛矿相PbTiO3(PT)单晶纳米纤维,并通过固态相变获得尺寸可控的钙钛矿相PT单晶纳米纤维；通过高分子辅助水热／溶剂热法合成出Fe掺杂钙钛矿相PT类单晶自组装超结构。通过多种分析测试方法对前钙钛矿、钙钛矿相PT单晶纳米纤维的铁电性及其尺寸效应、Fe掺杂PT自组装超结构的铁磁性等进行了深入的研究；对前钙钛矿相PT单晶纳米纤维的生长模型、固态相变模型展开了讨论。主要研究内容如下：
(1)利用高分子辅助水热法,通过调节水热过程中反应物前躯体浓度Pb/Ti的摩尔比值(提高Pb的加入量)成功实现了前钙钛矿相PT单晶纳米纤维的尺寸可控制备。纳米纤维的直径从平均约90nm到15nm,且伴随着尺寸的减小纤维长径比从120减小到40。水热系统中较高的Pb浓度提高了晶体成核量,而前钙钛矿相的大量成核则降低了晶核生长的驱动力,从而限制了晶体的生长,引起尺寸的减小
(2)紫外可见吸收谱(UV)和荧光光谱(PL)研究表明前钙钛矿相PT纳米纤维光学带隙约为3.10eV,而PL发光位置为绿光波段(-550nm)和近红外波段(～900nm),且随尺寸无明显变化。其可能的机制是光激发后的电子和空穴分别形成Ti4+和Pb2+相关的自俘获激子(STE)态复合发光,而两个波段发光都没有明显的尺寸效应说明一维柱状的晶体结构起到重要作用。动态接触式静电力显微镜(DC-EFM)研究表明前钙钛矿相PT单晶纳米纤维的铁电性随尺寸的减小而降低。
(3)通过前钙钛矿相PT纳米纤维空气中退火处理成功制备了不同尺寸的钙钛矿相PT单晶纳米纤维,其直径范围为85nm至15nm,长径比约为105至37。XRD、差热分析(DTA)、二次谐波(SHG)及压电力显微镜(PFM)等研究表明钙钛矿相PT单晶纳米纤维的铁电性随直径的减小而降低,且平均直径为15nm的纤维中仍然存在铁电性,这一结论在直径为13nm的单根纤维中得到了证实。
(4)研究揭示了前钙钛矿结构水热合成实验条件,如矿化剂种类、矿化剂浓度、水热温度、水热时间、添加剂等,对产物物相及形貌的影响规律。利用SEM、HRTEM等手段研究了前钙钛矿相PT单晶纳米纤维的生长过程并提出了可能的取向聚集生长机制：前钙钛矿相PT晶核在PVA中羟基(-OH)的吸附作用下生长为直径约4nm-6nm,长度约50nm-200nm的生长基元,这些基元再通过空间取向聚集的方式生长成为前钙钛矿相PT单晶纳米纤维,取向聚集模型的驱动力可能是晶体的表面能及静电力。
(5)利用DTA、XRD、原位TEM等分析方法对前钙钛矿-钙钛矿结构的相变过程展开了深入研究,并提出表面及界面诱导的虚拟熔化-结晶-晶核取向聚集生长的相变模型。前钙钛矿相晶体在表面能及界面上缺陷的驱动下,产生大量虚拟熔化的无序非晶区域,这些无序结构的出现降低了钙钛矿结构形核的动力学势垒并生成钙钛矿相PT晶核,钙钛矿相晶粒通过取向聚集的方式生长为单晶纳米纤维。前钙钛矿-钙钛矿结构相变温度有着随纤维直径的减小而升高的趋势,这可能是由于尺寸的减小降低了虚拟熔化形成的驱动力。
(6)以稀磁半导体的掺杂研究为指导,利用高分子辅助水热/溶剂热法成功制备了高度(001)取向的钙钛矿相PT类单晶自组装超结构及Fe掺杂钙钛矿相PT类单晶自组装超结构。利用XRD、SEM、TEM等手段对其进行了表征并研究了PT自组装超结构的生长机制。利用MPMS研究了铁掺杂钙钛矿PT纳米结构的室温铁磁性,并提出大量增加的晶界界面提高了产生铁磁性的F色心交换作用,从而提高了其室温铁磁性。
Low-dimensional perovskite oxides, in particular, one-dimensional perovskite oxides have received extensive attention due to their promising potential applications in non-volatile ferroelectric memory (FeRAM), piezoelectric nanogenerators and piezoelectric nanosensors. Therefore, researches on controllable synthesis, microstructure and properties of one-dimensional (ID) perovskite nanomaterials should be of great significance both theoretically and practically in discovering new phenomena and exploring novel applications.
In this dissertation, the characteristics crystal structure and the current status of researches of the perovskite oxides were reviewed firstly. And then the present studies concerning the preparation and properties of1D perovskite ferroelectric oxide nanomaterials have been summarized and commented in detail. However, the controllable preparation of single crystal nanostructures of1D perovskite ferroelectric oxide remains a challenge. In this perspective, experimental exploration has lagged far behind theoretical ones. Focusing on this problem, we report, for the first time, a polymer-assisted hydrothermal synthesis of single-crystal pre-perovskite PbTiO3(PT) nanofibers with a controllable size, and based on which single-crystal perovskite PT nanofibers have been prepared via a solid phase transformation route. Single-crystal like Fe-doped perovskite PT superstructure have been successfully synthesized through a self-assembly mechanism by the similar polymer-assisted hydrothermal/solvothermal method. By employing a variety of characterization methods, comprehensive and in-depth investigations on the ferroelectric property and size effect of single-crystal pre-perovskite/perovskite ferroelectric PT nanofibers and the ferromagnetic property of single-crystal like superstructure of Fe-doped perovskite PT are carried out systematically. Consequently, constructive and insightful discussions were concentrated on a growth model of the single-crystal pre-perovskite PT nanofibers and its solid phase transformation. The main contents are listed as follows:
(1). Size-controlled synthesis of single-crystal pre-perovskite PT nanofibers was achieved through a polymer-assisted hydrothermal method by adjusting the precursor concentration of Pb/Ti molar ratio in the reactants during the hydrothermal process (increasing the added amount of Pb). The diameter of the as-prepared PT nanofibers decreased from an average size of～90nm to～15nm, accompanying with a reduction of aspect ratio from120and40. It has been found that the decrease in the size of the nanofibers can be attributed to the relatively higher Pb concentration during the hydrothermal process which significantly limited the number of crystal nucleation of the pre-perovskite oxides and undermined the driving force for the growth of pre-perovskite nucleates, leading to the decrease of size thus of the nanofibers.
(2). UV-visible absorption spectroscopy (UV) and fluorescence spectra (PL) studies have shown that the pre-perovskite PT nanofibers possess an optical band-gap of～3.10eV, and corresponding PL emission located at the green light band (-550nm) and near infrared band (～900mn), where significant change of the emission the diameter of the nanofibers decreased. A possible mechanism underlying this photo excitation phenomenon can be attributed to the recombination of Ti4+and Pb2+related self-trapping excitons (STE) that formed from the optical excitation generated electrons and holes. We suggested that the1D columnar crystal structure of the pre-perovskite plays a key role in the size independence of the two-band luminescence phenomenon. Dynamic contact type electrostatic force microscopy (DC-EFM) studies revealed that the ferroelectric properties of the single-crystal nanofibers of pre-perovskite PT decrease with the diameter.
(3). Perovskite PT nanofibers with a diameter ranging from85nm to15nm and aspect ratio of about105-37were successfully prepared by annealing the corresponding pre-perovskite nanofibers in air. X-ray diffraction (XRD), differential thermal analysis (DTA), second harmonic generation (SHG) and piezoelectric force microscopy (PFM) were employed to investigate the ferroelectric property of the single-crystal nanofibers of perovskite PT. The results demonstrate the decrease of the ferroelectricity with perovskite PT nanofiber size and the existence of ferroelectricity in perovskite PT nanofiber with a diameter as low as15nm. This was further confirmed by the fact that ferroelectricity still remains in a single perovskite PT nanofiber with a diameter of～13nm.
(4). The effect of experimental conditions in the hydrothermal process, such as the type of mineralizer, mineralizer concentration, reaction temperature, reaction time and additives have been studies comprehensively on the formation of the resulting products and their morphology evolution. SEM and HRTEM were employed to investigate the growth process of pre-perovskite PT single crystal nanofibers, on the basis of which a possible growth mechanism via an oriented aggregation process was proposed. It is found that pre-perovskite PT nuclei developed into the growing units with diameter of about4nm-6nm and length of about50nm-200nm by the adsorption of hydroxyl (-OH) in PVA firstly. And then the growing units grew into the single-crystal nanofibers of pre-perovskite PT by orientation attachment. The driving force for the orientation attachment growth model could be the surface energy and static electric force existed in the system.
(5). In-depth research into the phase transformation process from pre-perovskite structure to perovskite one was conducted by using DTA, XRD and in-situ TEM. On the basis of these experiments, we propose a surface-and interface-induced virtual melting-crystallization-nuclei oriented attachment growth procedure to model this phase transformation process. Large-scale of disordered amorphous regions by virtual melting were formed in pre-perovskite, resulting from the surface energy and the interfacial defects, which reduces the apparent kinetic energy barrier and the formation of perovskite PT nuclei. And then the single-crystal perovskite PT nanofibers were formed by the oriented attachment growth of the perovskite nanocrystals. The phase transformation temperature from pre-perovskite structure to perovskite structure increases with the decrease of the diameter size of the pre-perovskite nanofibers, which could be due to the decrease of virtual melting driving force resulting from the size reduction of PT pre-perovskite nanofibers.
(6). Under the guidance of rare magnetic semiconductor, self-assembled single-crystal like superstructure of perovskite PT and Fe-doped perovskite PT with a high (001) orientation were successfully prepared via a polymer-assisted hydrothermal/solvothermal method. The growth mechanism of the self-assembled superstructure was explored by using XRD、SEM、TEM. MPMS was employed to study ferromagnetism of Fe-doped perovskite PT nanostructures. A significant increase in the grain boundary interfaces could increase F-color centers generating ferromagnetic exchange interaction, thereby improving its ferromagnetism.
本文首先简要综述了钙钛矿结构氧化物的结构特点与研究现状,并重点总结和评述了一维钙钛矿铁电氧化物纳米结构的制备及性能研究。在这一方面,实验研究明显滞后于相关的理论研究,其主要原因在于一维钙钛矿铁电氧化物单晶纳米结构的可控制备仍是一个挑战。针对这一问题,本文首次通过高分子辅助水热方法合成出尺寸可控前钙钛矿相PbTiO3(PT)单晶纳米纤维,并通过固态相变获得尺寸可控的钙钛矿相PT单晶纳米纤维；通过高分子辅助水热／溶剂热法合成出Fe掺杂钙钛矿相PT类单晶自组装超结构。通过多种分析测试方法对前钙钛矿、钙钛矿相PT单晶纳米纤维的铁电性及其尺寸效应、Fe掺杂PT自组装超结构的铁磁性等进行了深入的研究；对前钙钛矿相PT单晶纳米纤维的生长模型、固态相变模型展开了讨论。主要研究内容如下：
(1)利用高分子辅助水热法,通过调节水热过程中反应物前躯体浓度Pb/Ti的摩尔比值(提高Pb的加入量)成功实现了前钙钛矿相PT单晶纳米纤维的尺寸可控制备。纳米纤维的直径从平均约90nm到15nm,且伴随着尺寸的减小纤维长径比从120减小到40。水热系统中较高的Pb浓度提高了晶体成核量,而前钙钛矿相的大量成核则降低了晶核生长的驱动力,从而限制了晶体的生长,引起尺寸的减小
(2)紫外可见吸收谱(UV)和荧光光谱(PL)研究表明前钙钛矿相PT纳米纤维光学带隙约为3.10eV,而PL发光位置为绿光波段(-550nm)和近红外波段(～900nm),且随尺寸无明显变化。其可能的机制是光激发后的电子和空穴分别形成Ti4+和Pb2+相关的自俘获激子(STE)态复合发光,而两个波段发光都没有明显的尺寸效应说明一维柱状的晶体结构起到重要作用。动态接触式静电力显微镜(DC-EFM)研究表明前钙钛矿相PT单晶纳米纤维的铁电性随尺寸的减小而降低。
(3)通过前钙钛矿相PT纳米纤维空气中退火处理成功制备了不同尺寸的钙钛矿相PT单晶纳米纤维,其直径范围为85nm至15nm,长径比约为105至37。XRD、差热分析(DTA)、二次谐波(SHG)及压电力显微镜(PFM)等研究表明钙钛矿相PT单晶纳米纤维的铁电性随直径的减小而降低,且平均直径为15nm的纤维中仍然存在铁电性,这一结论在直径为13nm的单根纤维中得到了证实。
(4)研究揭示了前钙钛矿结构水热合成实验条件,如矿化剂种类、矿化剂浓度、水热温度、水热时间、添加剂等,对产物物相及形貌的影响规律。利用SEM、HRTEM等手段研究了前钙钛矿相PT单晶纳米纤维的生长过程并提出了可能的取向聚集生长机制：前钙钛矿相PT晶核在PVA中羟基(-OH)的吸附作用下生长为直径约4nm-6nm,长度约50nm-200nm的生长基元,这些基元再通过空间取向聚集的方式生长成为前钙钛矿相PT单晶纳米纤维,取向聚集模型的驱动力可能是晶体的表面能及静电力。
(5)利用DTA、XRD、原位TEM等分析方法对前钙钛矿-钙钛矿结构的相变过程展开了深入研究,并提出表面及界面诱导的虚拟熔化-结晶-晶核取向聚集生长的相变模型。前钙钛矿相晶体在表面能及界面上缺陷的驱动下,产生大量虚拟熔化的无序非晶区域,这些无序结构的出现降低了钙钛矿结构形核的动力学势垒并生成钙钛矿相PT晶核,钙钛矿相晶粒通过取向聚集的方式生长为单晶纳米纤维。前钙钛矿-钙钛矿结构相变温度有着随纤维直径的减小而升高的趋势,这可能是由于尺寸的减小降低了虚拟熔化形成的驱动力。
(6)以稀磁半导体的掺杂研究为指导,利用高分子辅助水热/溶剂热法成功制备了高度(001)取向的钙钛矿相PT类单晶自组装超结构及Fe掺杂钙钛矿相PT类单晶自组装超结构。利用XRD、SEM、TEM等手段对其进行了表征并研究了PT自组装超结构的生长机制。利用MPMS研究了铁掺杂钙钛矿PT纳米结构的室温铁磁性,并提出大量增加的晶界界面提高了产生铁磁性的F色心交换作用,从而提高了其室温铁磁性。
Low-dimensional perovskite oxides, in particular, one-dimensional perovskite oxides have received extensive attention due to their promising potential applications in non-volatile ferroelectric memory (FeRAM), piezoelectric nanogenerators and piezoelectric nanosensors. Therefore, researches on controllable synthesis, microstructure and properties of one-dimensional (ID) perovskite nanomaterials should be of great significance both theoretically and practically in discovering new phenomena and exploring novel applications.
In this dissertation, the characteristics crystal structure and the current status of researches of the perovskite oxides were reviewed firstly. And then the present studies concerning the preparation and properties of1D perovskite ferroelectric oxide nanomaterials have been summarized and commented in detail. However, the controllable preparation of single crystal nanostructures of1D perovskite ferroelectric oxide remains a challenge. In this perspective, experimental exploration has lagged far behind theoretical ones. Focusing on this problem, we report, for the first time, a polymer-assisted hydrothermal synthesis of single-crystal pre-perovskite PbTiO3(PT) nanofibers with a controllable size, and based on which single-crystal perovskite PT nanofibers have been prepared via a solid phase transformation route. Single-crystal like Fe-doped perovskite PT superstructure have been successfully synthesized through a self-assembly mechanism by the similar polymer-assisted hydrothermal/solvothermal method. By employing a variety of characterization methods, comprehensive and in-depth investigations on the ferroelectric property and size effect of single-crystal pre-perovskite/perovskite ferroelectric PT nanofibers and the ferromagnetic property of single-crystal like superstructure of Fe-doped perovskite PT are carried out systematically. Consequently, constructive and insightful discussions were concentrated on a growth model of the single-crystal pre-perovskite PT nanofibers and its solid phase transformation. The main contents are listed as follows:
(1). Size-controlled synthesis of single-crystal pre-perovskite PT nanofibers was achieved through a polymer-assisted hydrothermal method by adjusting the precursor concentration of Pb/Ti molar ratio in the reactants during the hydrothermal process (increasing the added amount of Pb). The diameter of the as-prepared PT nanofibers decreased from an average size of～90nm to～15nm, accompanying with a reduction of aspect ratio from120and40. It has been found that the decrease in the size of the nanofibers can be attributed to the relatively higher Pb concentration during the hydrothermal process which significantly limited the number of crystal nucleation of the pre-perovskite oxides and undermined the driving force for the growth of pre-perovskite nucleates, leading to the decrease of size thus of the nanofibers.
(2). UV-visible absorption spectroscopy (UV) and fluorescence spectra (PL) studies have shown that the pre-perovskite PT nanofibers possess an optical band-gap of～3.10eV, and corresponding PL emission located at the green light band (-550nm) and near infrared band (～900mn), where significant change of the emission the diameter of the nanofibers decreased. A possible mechanism underlying this photo excitation phenomenon can be attributed to the recombination of Ti4+and Pb2+related self-trapping excitons (STE) that formed from the optical excitation generated electrons and holes. We suggested that the1D columnar crystal structure of the pre-perovskite plays a key role in the size independence of the two-band luminescence phenomenon. Dynamic contact type electrostatic force microscopy (DC-EFM) studies revealed that the ferroelectric properties of the single-crystal nanofibers of pre-perovskite PT decrease with the diameter.
(3). Perovskite PT nanofibers with a diameter ranging from85nm to15nm and aspect ratio of about105-37were successfully prepared by annealing the corresponding pre-perovskite nanofibers in air. X-ray diffraction (XRD), differential thermal analysis (DTA), second harmonic generation (SHG) and piezoelectric force microscopy (PFM) were employed to investigate the ferroelectric property of the single-crystal nanofibers of perovskite PT. The results demonstrate the decrease of the ferroelectricity with perovskite PT nanofiber size and the existence of ferroelectricity in perovskite PT nanofiber with a diameter as low as15nm. This was further confirmed by the fact that ferroelectricity still remains in a single perovskite PT nanofiber with a diameter of～13nm.
(4). The effect of experimental conditions in the hydrothermal process, such as the type of mineralizer, mineralizer concentration, reaction temperature, reaction time and additives have been studies comprehensively on the formation of the resulting products and their morphology evolution. SEM and HRTEM were employed to investigate the growth process of pre-perovskite PT single crystal nanofibers, on the basis of which a possible growth mechanism via an oriented aggregation process was proposed. It is found that pre-perovskite PT nuclei developed into the growing units with diameter of about4nm-6nm and length of about50nm-200nm by the adsorption of hydroxyl (-OH) in PVA firstly. And then the growing units grew into the single-crystal nanofibers of pre-perovskite PT by orientation attachment. The driving force for the orientation attachment growth model could be the surface energy and static electric force existed in the system.
(5). In-depth research into the phase transformation process from pre-perovskite structure to perovskite one was conducted by using DTA, XRD and in-situ TEM. On the basis of these experiments, we propose a surface-and interface-induced virtual melting-crystallization-nuclei oriented attachment growth procedure to model this phase transformation process. Large-scale of disordered amorphous regions by virtual melting were formed in pre-perovskite, resulting from the surface energy and the interfacial defects, which reduces the apparent kinetic energy barrier and the formation of perovskite PT nuclei. And then the single-crystal perovskite PT nanofibers were formed by the oriented attachment growth of the perovskite nanocrystals. The phase transformation temperature from pre-perovskite structure to perovskite structure increases with the decrease of the diameter size of the pre-perovskite nanofibers, which could be due to the decrease of virtual melting driving force resulting from the size reduction of PT pre-perovskite nanofibers.
(6). Under the guidance of rare magnetic semiconductor, self-assembled single-crystal like superstructure of perovskite PT and Fe-doped perovskite PT with a high (001) orientation were successfully prepared via a polymer-assisted hydrothermal/solvothermal method. The growth mechanism of the self-assembled superstructure was explored by using XRD、SEM、TEM. MPMS was employed to study ferromagnetism of Fe-doped perovskite PT nanostructures. A significant increase in the grain boundary interfaces could increase F-color centers generating ferromagnetic exchange interaction, thereby improving its ferromagnetism.
引文
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