单晶钛酸铅纳米结构的可控制备、掺杂、相变与应用研究
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摘要
钙钛矿结构铁电氧化物纳米材料具有优异的物理和化学性能,在高密度存储器、压电纳米发电机和催化等领域有着广阔的应用前景。开展纳米尺度钙钛矿结构铁电氧化物的可控制备,研究其结构与性能间的相互关系,对于这类材料的发展以及应用拓展都具有重要的指导意义。
本文首先简要概述了铁电氧化物的结构特点,重点总结和评述了PbTiO3(PT)及其固溶体铁电纳米材料的制备与性能研究现状。针对一维单晶PT及其固溶体铁电纳米材料的可控制备和尺寸调控等难点问题,本文采用PVA作为表面修饰剂辅助水热法分别首次成功合成出Ba、Fe、Zr掺杂前钙钛矿相PT单晶纳米纤维,并通过固相烧结法获得Ba、Fe、Zr掺杂的四方钙钛矿相PT单晶纳米纤维。此外,采用多种分析测试技术对前钙钛矿相和钙钛矿相Ba、Fe、Zr掺杂PT单晶纳米纤维的铁电性、铁磁性和荧光等性能进行了研究。系统研究了前钙钛矿相PT纳米纤维的相变过程和介孔形成机制。以低维PT铁电纳米材料为载体,分别对其负载Pt和Ti02合成Pt-PT和PT-TiO2复合材料,成功将铁电氧化物纳米材料拓展到CO催化和可见光光催化领域。本文主要研究内容如下：
(1)采用PVA辅助水热法,首次成功制备了一系列具有规则刻面且表面光滑的Ba掺杂前钙钛矿相PT纳米纤维,其直径为100-600nm,长度为13-120gm,纳米纤维长径比高达200,Ba2+在前钙钛矿相PT中的掺杂极限值为5-8mo1%。在生长过程中,PVA分子链通过氢键或化学吸附附着在Ba掺杂前钙钛矿相PT晶核表面,抑制了{001}晶面的生长速率,使其沿[001]方向发生取向生长,从而制备出Ba掺杂前钙钛矿相PT单晶纳米纤维。该纳米纤维在高温热处理后会相变成为单晶Ba掺杂钙钛矿相PT纳米纤维,压电力显微镜研究表明5mol%Ba掺杂PT单晶纳米纤维具有明显的压电铁电性能。
(2)采用PVA辅助水热法,首次成功制备了A位Fe掺杂前钙钛矿相PT单晶纳米纤维,其掺杂极限在2-5mo1%之间,该纳米纤维在高温热处理后相变为B位Fe掺杂的四方钙钛矿相PT纳米纤维。Fe掺杂前钙钛矿相PT纳米纤维的M-H结果表明,未掺杂的样品为典型的抗磁性,Fe掺杂浓度为1mol%时,样品表现为铁磁性,当掺杂含量增加至2mo1%,转变为顺磁性；Fe掺杂钙钛矿相PT纳米纤维的M-H曲线显示,纯PT表现为抗磁性,当掺杂含量为1mol%时,样品为铁磁性,且随着Fe浓度增加至2mo1%时,样品饱和磁化强度基本不变。
(3)采用PVA辅助水热法,首次成功制备了一系列Zr掺杂前钙钛矿相PT纳米纤维,其直径为100-400nm,长度为5-30μm,掺杂极限在15-20mo1%+之间；该纳米纤维在高温热处理后可以转变为Zr掺杂钙钛矿相PT单晶纳米纤维。室温条件下,经325nm激光激发后,Zr掺杂前钙钛矿相PT纳米纤维在绿光和近红外波段都有荧光发光峰,且随着Zr掺杂浓度增加,其发光强度减弱,发光峰位基本不变。
(4)采用高温热处理法,结合In-situ XRD和In-situ TEM等测试手段,系统研究了前钙钛矿相向钙钛矿相PT的相变过程和介孔形成机制。在相变过程中,随着温度的升高,前钙钛矿相晶体结构的ab面首先被打破,产生大量熔化形成的非晶区域,这些区域的出现有效降低了前钙钛矿和钙钛矿相PT晶格不匹配造成的界面能,使其相变过程顺利进行。此外,相变过程中产生的非晶区域结晶成为立方钙钛矿结构时,由于两种结构存在较大的密度差,纳米纤维内部出现孔径为5-10nm的介孔,这种介孔随着温度的升高相互吞并长大,直至迁移至表面、消失；采用短时间热处理并结合快速冷却的方式可以有效保留这些介孔,获得单晶介孔的铁电纳米纤维。
(5)采用浸渍还原法获得Pt-PT纳米纤维,其CO催化结果显示,纯钙钛矿相PT纳米纤维在温度升高至250℃对CO仍无催化作用；开孔Pt/meso-PT样品和闭孔Pt/meso-PT-surf-block样品在温度为85℃时,均可实现对CO的100%转化率,而无孔的Pt-PT样品温度为100℃。通过对比三者的动力学曲线,发现其表观活化能呈递减趋势,介孔Pt/meso-PT纳米纤维的催化活性最高。
(6)采用简单的二次水热法成功合成出不同浓度的PT-TiO2复合纳米材料,研究发现Ti02纳米颗粒与PT纳米片可能发生外延生长,形成异质结结构。有机物光降解研究表明：可见光(λ～420nm)连续辐照3h后,PT-TiO2复合纳米材料对亚甲基蓝(MB)溶液的降解效率接近100%；且随着复合材料中Ti02比例增加,PT-TiO2复合纳米材料的一级反应速率常数从0.0161增加至0.0203min-1。
(7)采用水热法合成了a-FeOOH单晶纳米棒,在氧气和氮气保护下对其进行热处理,分别获得单晶介孔a-Fe2O3和Fe304纳米棒,二者孔径分布范围对应为1-8nm和1-18nm。三种不同结构氧化铁的电化学性能数据显示,在0.1C倍率下,无孔a-FeOOH样品循环性能较差,而具有介孔结构的a-Fe2O3和Fe304单晶纳米棒由于结构稳定性好,比表面积高,在0.1C倍率下充放电50次后,可逆容量分别高于890mAhg-1和840mAhg-1,表现出优异的循环性能。
Perovskite-type ferroelectric oxide nanomaterials demonstrate unique physical and chemical properties, affording versatile potential applications ranging from high-density ferroelectric random access memory, nanogenerators to catalysis. Investigation on the controllable growth of the perovskite nano-ferroelectrics and further building the relationship between the microstructures and properties, are highly desired to develop and expand application for these materials.
In this dissertation, the structure and preparation of ferroelectric nanomaterials has been reviewed firstly. Furthermore, the current situation and main problems on the synthesis and properties of PbTiO3(PT) as well as its solid solutions have been summarized in detail. However, the controllable growth of one-dimensional(ID) single-crystal PT and its solid solutions nanostructures remains a challenge. Thus, single-crystal pre-perovskite PT nanofibers with different dopant such as Ba, Fe and Zr ions were synthesized via a polymer-assisted hydrothermal method. On the basis of the doped pre-perovskite PT nanofibers, single-crystal Ba, Fe and Zr-doped perovskite PT nanofibers have been prepared accordingly via a phase transformation route. Moreover, various measurement methods were employed to study ferroelectricity, ferromagnetism and photoluminescence (PL) properties of the pre-perovskite and perovskite PT nanofibers with Ba, Fe and Zr dopant. In particular, the phase transformation from pre-perovskite PT to perovskite PT, accompanied by the formation of the mesoporosity has been systematically explored. To further investigate the applications of the low-dimensional PT ferroelectrics, the obtained PT nanostructures were loaded by Pt and TiO2nanocrystals, respectively. It is clearly demonstrated that Pt-PT and TiO2-PT composite materials represent fascinating CO catalytic activity and visible-light photocatalytic performances, which could extend the applications of ferroelectric oxides to environment area. The main contents and results are summarized as follows:
(1) Single-crystal Ba-doped pre-perovskite PT nanofibers (0-5mol%) with a diameter of100-600nm and a length of13-120μm have been synthesized by a PVA assisted hydrothermal method. The limited solubility of Ba in pre-perovskite PT was determined to be5-8mol%. During the reaction process. PVA molecule was possibly adsorbed on the Ba-doped pre-perovskite PT nanoparticle via hydrogen bonding or chemical interaction, which limited the growth of certain crystalline planes{110}, leading to the oriented growth of Ba-doped pre-perovskite PT nanofibers along [001] direction. Ba-doped perovskite PT nanofibers have been prepared via a phase transformation of the pre-perovskite ones. And the PFM results confirmed the piezoelectric and ferroelectric properties of5mol%Ba-doped perovskite nanofibers.
(2) Fe-doped pre-perovskite PT single-crystal nanofibers have been synthesized by hydrothermal method, and the limited solubility of Fe in this structure was determined to be2-5mol%. These nanofibers can transform to Fe-doped perovskite PT single-crystal nanofibers. As Fe doping contents increased, M-H results indicated that the pre-perovskite PT nanofibers develop from diamagnetism (without Fe doping) to ferromagnetism(1mol%) and paramagnetism (2mol%). For the Fe-doped perovskite PT nanofibers, the magnetism of the samples developed from diamagnetism (0mol%) to ferromagnetism(1mol%). However, as Fe doping concentration increased to2mol%, the saturation magnetization changed slightly.
(3) Single-crystal Zr-doped pre-perovskite PT nanofibers with a diameter of100-400nm and a length of5-30μm have been synthesized by a PVA assisted hydrothermal method. The limited solubility of Zr in pre-perovskite PT was determined to be15-20mol%. Moreover. these nanofibers can transform into single-crystal perovskite Pb(Zr, Ti)O3(PZT) nanofibers by annealing treatment in air. Zr-doped pre-perovskite PT nanofibers demonstrate strong green and near infrared (NIR) PL emission at room temperature. The green PL intensity is evidently decreased with the Zr doping concentration increased.
(4) The phase transformation from pre-perovskite PT to perovskite PT, accompanied by the formation of the mesopores has been systematically investigated with in-situ XRD and in-situ TEM analysis. During the phase transformation process, ab plane of pre-perovskite PT crystal structure wasdestroyed firstly. accompanied with the appearance of a large number of amorphous regions. These amorphous regions could reduce the interface energy between pre-perovskite PT and perovskite PT, and stimulate the transformation process. In addition, the faceted mesoporeswith a size of5-10nm formed within the entire nanofiber when the amorphous crystallized into the structure of cubic perovskite PT, due to the density difference between pre-perovskite and perovskite PT. When the heating time is long enough, the porous aggregated and moved into the surface of the fibers, and disappeared in the end. accompanied with a complete phase transformation. Therefore, single-crystal mesoporous perovskite PT nanofibers could be obtained by a short time annealing treated and quickly quenched approach.
(5) Pt-PT nanofibers were prepared by an impregnation-reduction method. The catalytic results suggested that pure PT nanofibers almost have no catalytic activity for the oxidation of CO up to250℃. For Pt/meso-PT, Pt/meso-PT-surf-block and Pt/PTsamples, the100%conversion of CO was achieved at-85℃,-85℃and-100℃, respectively. Additionally, the apparent activation energyof these three samples was decreased gradually, indicating that the Pt/meso-PT sample with open porous structure has an improved catalytic performance.
(6) PT-TiO2composite nanomaterials were fabricated by a hydrothermal method. A crystallography epitaxial growth of TiO2on PT may be appeared. The PT-TiO2composite nanomaterials were used to photochemically degrade methylene blue (MB) under visible light(λ-420nm). After3h of irradiation, the degradation rate of MB was closed to100%. The first-order reaction rates of PT-TiO2samples were increased from0.0161to0.0203min-1as increasing the TiO2ratio in the composite materials.
(7) Single-crystal a-FeOOH nanorods were successfully synthesized via a facile hydrothermal method. Mesoporous a-Fe2O3and Fe3O4single-crystal nanorods with a pore size of1-8nm and1-18nm, respectively, could be obtained by calcining these a-FeOOH precursors in different atmosphere. When tested as the anode materials for lithium ion batteries, a-FeOOH sample exhibited a poor electrochemical performance. In contrast, a-Fe2O3and Fe3O4nanorods with the unique mesoporous structure have excellent structural stability and large specific surface area, which could deliver the high reversible capacities of890and840mAhg-1after50cycles at0.1C respectively.
本文首先简要概述了铁电氧化物的结构特点,重点总结和评述了PbTiO3(PT)及其固溶体铁电纳米材料的制备与性能研究现状。针对一维单晶PT及其固溶体铁电纳米材料的可控制备和尺寸调控等难点问题,本文采用PVA作为表面修饰剂辅助水热法分别首次成功合成出Ba、Fe、Zr掺杂前钙钛矿相PT单晶纳米纤维,并通过固相烧结法获得Ba、Fe、Zr掺杂的四方钙钛矿相PT单晶纳米纤维。此外,采用多种分析测试技术对前钙钛矿相和钙钛矿相Ba、Fe、Zr掺杂PT单晶纳米纤维的铁电性、铁磁性和荧光等性能进行了研究。系统研究了前钙钛矿相PT纳米纤维的相变过程和介孔形成机制。以低维PT铁电纳米材料为载体,分别对其负载Pt和Ti02合成Pt-PT和PT-TiO2复合材料,成功将铁电氧化物纳米材料拓展到CO催化和可见光光催化领域。本文主要研究内容如下：
(1)采用PVA辅助水热法,首次成功制备了一系列具有规则刻面且表面光滑的Ba掺杂前钙钛矿相PT纳米纤维,其直径为100-600nm,长度为13-120gm,纳米纤维长径比高达200,Ba2+在前钙钛矿相PT中的掺杂极限值为5-8mo1%。在生长过程中,PVA分子链通过氢键或化学吸附附着在Ba掺杂前钙钛矿相PT晶核表面,抑制了{001}晶面的生长速率,使其沿[001]方向发生取向生长,从而制备出Ba掺杂前钙钛矿相PT单晶纳米纤维。该纳米纤维在高温热处理后会相变成为单晶Ba掺杂钙钛矿相PT纳米纤维,压电力显微镜研究表明5mol%Ba掺杂PT单晶纳米纤维具有明显的压电铁电性能。
(2)采用PVA辅助水热法,首次成功制备了A位Fe掺杂前钙钛矿相PT单晶纳米纤维,其掺杂极限在2-5mo1%之间,该纳米纤维在高温热处理后相变为B位Fe掺杂的四方钙钛矿相PT纳米纤维。Fe掺杂前钙钛矿相PT纳米纤维的M-H结果表明,未掺杂的样品为典型的抗磁性,Fe掺杂浓度为1mol%时,样品表现为铁磁性,当掺杂含量增加至2mo1%,转变为顺磁性；Fe掺杂钙钛矿相PT纳米纤维的M-H曲线显示,纯PT表现为抗磁性,当掺杂含量为1mol%时,样品为铁磁性,且随着Fe浓度增加至2mo1%时,样品饱和磁化强度基本不变。
(3)采用PVA辅助水热法,首次成功制备了一系列Zr掺杂前钙钛矿相PT纳米纤维,其直径为100-400nm,长度为5-30μm,掺杂极限在15-20mo1%+之间；该纳米纤维在高温热处理后可以转变为Zr掺杂钙钛矿相PT单晶纳米纤维。室温条件下,经325nm激光激发后,Zr掺杂前钙钛矿相PT纳米纤维在绿光和近红外波段都有荧光发光峰,且随着Zr掺杂浓度增加,其发光强度减弱,发光峰位基本不变。
(4)采用高温热处理法,结合In-situ XRD和In-situ TEM等测试手段,系统研究了前钙钛矿相向钙钛矿相PT的相变过程和介孔形成机制。在相变过程中,随着温度的升高,前钙钛矿相晶体结构的ab面首先被打破,产生大量熔化形成的非晶区域,这些区域的出现有效降低了前钙钛矿和钙钛矿相PT晶格不匹配造成的界面能,使其相变过程顺利进行。此外,相变过程中产生的非晶区域结晶成为立方钙钛矿结构时,由于两种结构存在较大的密度差,纳米纤维内部出现孔径为5-10nm的介孔,这种介孔随着温度的升高相互吞并长大,直至迁移至表面、消失；采用短时间热处理并结合快速冷却的方式可以有效保留这些介孔,获得单晶介孔的铁电纳米纤维。
(5)采用浸渍还原法获得Pt-PT纳米纤维,其CO催化结果显示,纯钙钛矿相PT纳米纤维在温度升高至250℃对CO仍无催化作用；开孔Pt/meso-PT样品和闭孔Pt/meso-PT-surf-block样品在温度为85℃时,均可实现对CO的100%转化率,而无孔的Pt-PT样品温度为100℃。通过对比三者的动力学曲线,发现其表观活化能呈递减趋势,介孔Pt/meso-PT纳米纤维的催化活性最高。
(6)采用简单的二次水热法成功合成出不同浓度的PT-TiO2复合纳米材料,研究发现Ti02纳米颗粒与PT纳米片可能发生外延生长,形成异质结结构。有机物光降解研究表明：可见光(λ～420nm)连续辐照3h后,PT-TiO2复合纳米材料对亚甲基蓝(MB)溶液的降解效率接近100%；且随着复合材料中Ti02比例增加,PT-TiO2复合纳米材料的一级反应速率常数从0.0161增加至0.0203min-1。
(7)采用水热法合成了a-FeOOH单晶纳米棒,在氧气和氮气保护下对其进行热处理,分别获得单晶介孔a-Fe2O3和Fe304纳米棒,二者孔径分布范围对应为1-8nm和1-18nm。三种不同结构氧化铁的电化学性能数据显示,在0.1C倍率下,无孔a-FeOOH样品循环性能较差,而具有介孔结构的a-Fe2O3和Fe304单晶纳米棒由于结构稳定性好,比表面积高,在0.1C倍率下充放电50次后,可逆容量分别高于890mAhg-1和840mAhg-1,表现出优异的循环性能。
Perovskite-type ferroelectric oxide nanomaterials demonstrate unique physical and chemical properties, affording versatile potential applications ranging from high-density ferroelectric random access memory, nanogenerators to catalysis. Investigation on the controllable growth of the perovskite nano-ferroelectrics and further building the relationship between the microstructures and properties, are highly desired to develop and expand application for these materials.
In this dissertation, the structure and preparation of ferroelectric nanomaterials has been reviewed firstly. Furthermore, the current situation and main problems on the synthesis and properties of PbTiO3(PT) as well as its solid solutions have been summarized in detail. However, the controllable growth of one-dimensional(ID) single-crystal PT and its solid solutions nanostructures remains a challenge. Thus, single-crystal pre-perovskite PT nanofibers with different dopant such as Ba, Fe and Zr ions were synthesized via a polymer-assisted hydrothermal method. On the basis of the doped pre-perovskite PT nanofibers, single-crystal Ba, Fe and Zr-doped perovskite PT nanofibers have been prepared accordingly via a phase transformation route. Moreover, various measurement methods were employed to study ferroelectricity, ferromagnetism and photoluminescence (PL) properties of the pre-perovskite and perovskite PT nanofibers with Ba, Fe and Zr dopant. In particular, the phase transformation from pre-perovskite PT to perovskite PT, accompanied by the formation of the mesoporosity has been systematically explored. To further investigate the applications of the low-dimensional PT ferroelectrics, the obtained PT nanostructures were loaded by Pt and TiO2nanocrystals, respectively. It is clearly demonstrated that Pt-PT and TiO2-PT composite materials represent fascinating CO catalytic activity and visible-light photocatalytic performances, which could extend the applications of ferroelectric oxides to environment area. The main contents and results are summarized as follows:
(1) Single-crystal Ba-doped pre-perovskite PT nanofibers (0-5mol%) with a diameter of100-600nm and a length of13-120μm have been synthesized by a PVA assisted hydrothermal method. The limited solubility of Ba in pre-perovskite PT was determined to be5-8mol%. During the reaction process. PVA molecule was possibly adsorbed on the Ba-doped pre-perovskite PT nanoparticle via hydrogen bonding or chemical interaction, which limited the growth of certain crystalline planes{110}, leading to the oriented growth of Ba-doped pre-perovskite PT nanofibers along [001] direction. Ba-doped perovskite PT nanofibers have been prepared via a phase transformation of the pre-perovskite ones. And the PFM results confirmed the piezoelectric and ferroelectric properties of5mol%Ba-doped perovskite nanofibers.
(2) Fe-doped pre-perovskite PT single-crystal nanofibers have been synthesized by hydrothermal method, and the limited solubility of Fe in this structure was determined to be2-5mol%. These nanofibers can transform to Fe-doped perovskite PT single-crystal nanofibers. As Fe doping contents increased, M-H results indicated that the pre-perovskite PT nanofibers develop from diamagnetism (without Fe doping) to ferromagnetism(1mol%) and paramagnetism (2mol%). For the Fe-doped perovskite PT nanofibers, the magnetism of the samples developed from diamagnetism (0mol%) to ferromagnetism(1mol%). However, as Fe doping concentration increased to2mol%, the saturation magnetization changed slightly.
(3) Single-crystal Zr-doped pre-perovskite PT nanofibers with a diameter of100-400nm and a length of5-30μm have been synthesized by a PVA assisted hydrothermal method. The limited solubility of Zr in pre-perovskite PT was determined to be15-20mol%. Moreover. these nanofibers can transform into single-crystal perovskite Pb(Zr, Ti)O3(PZT) nanofibers by annealing treatment in air. Zr-doped pre-perovskite PT nanofibers demonstrate strong green and near infrared (NIR) PL emission at room temperature. The green PL intensity is evidently decreased with the Zr doping concentration increased.
(4) The phase transformation from pre-perovskite PT to perovskite PT, accompanied by the formation of the mesopores has been systematically investigated with in-situ XRD and in-situ TEM analysis. During the phase transformation process, ab plane of pre-perovskite PT crystal structure wasdestroyed firstly. accompanied with the appearance of a large number of amorphous regions. These amorphous regions could reduce the interface energy between pre-perovskite PT and perovskite PT, and stimulate the transformation process. In addition, the faceted mesoporeswith a size of5-10nm formed within the entire nanofiber when the amorphous crystallized into the structure of cubic perovskite PT, due to the density difference between pre-perovskite and perovskite PT. When the heating time is long enough, the porous aggregated and moved into the surface of the fibers, and disappeared in the end. accompanied with a complete phase transformation. Therefore, single-crystal mesoporous perovskite PT nanofibers could be obtained by a short time annealing treated and quickly quenched approach.
(5) Pt-PT nanofibers were prepared by an impregnation-reduction method. The catalytic results suggested that pure PT nanofibers almost have no catalytic activity for the oxidation of CO up to250℃. For Pt/meso-PT, Pt/meso-PT-surf-block and Pt/PTsamples, the100%conversion of CO was achieved at-85℃,-85℃and-100℃, respectively. Additionally, the apparent activation energyof these three samples was decreased gradually, indicating that the Pt/meso-PT sample with open porous structure has an improved catalytic performance.
(6) PT-TiO2composite nanomaterials were fabricated by a hydrothermal method. A crystallography epitaxial growth of TiO2on PT may be appeared. The PT-TiO2composite nanomaterials were used to photochemically degrade methylene blue (MB) under visible light(λ-420nm). After3h of irradiation, the degradation rate of MB was closed to100%. The first-order reaction rates of PT-TiO2samples were increased from0.0161to0.0203min-1as increasing the TiO2ratio in the composite materials.
(7) Single-crystal a-FeOOH nanorods were successfully synthesized via a facile hydrothermal method. Mesoporous a-Fe2O3and Fe3O4single-crystal nanorods with a pore size of1-8nm and1-18nm, respectively, could be obtained by calcining these a-FeOOH precursors in different atmosphere. When tested as the anode materials for lithium ion batteries, a-FeOOH sample exhibited a poor electrochemical performance. In contrast, a-Fe2O3and Fe3O4nanorods with the unique mesoporous structure have excellent structural stability and large specific surface area, which could deliver the high reversible capacities of890and840mAhg-1after50cycles at0.1C respectively.
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