钛酸盐纳米管的结构稳定性和光学特性研究
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摘要
由于钛酸盐纳米管具有强的可见光吸收因而在太阳能利用方面将有潜在的应用前景而备受人们广泛的关注。水热法合成钛酸盐纳米管具有操作简单,成本低、产量高等优点因此引起了研究者广泛的兴趣。人们经过十多年的时间,对钛酸盐纳米管的组成、形成机理和物理化学性能进行了大量的研究,但是到目前为止,研究者对其形成机理、可见光吸收等特殊光电性质的来源、结构稳定性等方面的认识尚不清楚,因此本论文对这些方面开展了如下研究:
在第二章中我们从热力学的角度系统地研究了煅烧温度对钛酸盐纳米管形貌、结构稳定性和光学性能的影响,发现钛酸钠纳米管是热力学稳定的,而钛酸纳米管是热力学不稳定的。通过控制合适的干噪过程可以实现纳米管在可见光区的强吸收和发射,并且纳米管具有特殊的吸收带是与其特定能级相联系的。纳米管这种特殊的光电性质是由钛酸盐独特的管状结构和缺陷决定的。发现钛酸纳米管在高温时向锐钛矿结构转变,相转变的机制是由于纳米管在热力学条件下层间和层内进行脱水,正交结构遭到破坏后结构进行重新排列而导致的。
在第三章中我们从动力学的角度研究了纳米管在不同pH值和不同的酸浓度条件下形貌、结构稳定性和光学性能的变化规律。结果表明在稀酸和水洗这种温和的条件下管状结构并没有遭到破坏,可见光激发后纳米管随着pH值的减小荧光强度增加。这种特殊的光电性质来源于束缚单电子的氧空位。而在浓酸的作用下,管状结构遭到了严重的破坏,动力学不稳定使其结构进行重新排列由正交结构转变为锐钛矿结构。同时通过控制合适的后处理条件我们可以获得结构稳定的在可见区具有强的光吸收的钛酸盐一维纳米材料。
为了深入研究钛酸盐纳米管的相变机制和其可见区的光吸收和发射的来源,在第四章中我们开展了高压下钛酸盐纳米管的结构相转变研究,以期为揭示钛酸盐纳米管结构相转变的本质和更深入的理解管状结构形成的机理和特殊光电性质的来源提供直接的实验证据。在第四章中我们对钛酸钠纳米管的高压结构相变进行了研究,利用高压拉曼和高压X射线衍射实验手段分析证明在我们所研究的压力范围内纳米管发生了两次结构相转变:一个是在压力小于5 GPa时发生了向纤铁矿结构(H0.7Ti1.825□0.175O4·H2O)的转变;另一个是当压力超过16.7 GPa时发生了向无定型的转变,同时纳米管发生了坍塌。钛酸盐纳米管的结构相转变属于不可逆相变,恢复到常压时高压亚稳相纤铁矿结构可以保持,Ti-O键在钛酸盐纳米管的结构相转变中扮演着十分重要的角色。
The titanate nanotubes have been attracted widely attention due to their strong absorption in the visible light region and potential application on the utilization of the solar energy. The titanate nanotubes prepared by the hydrothermal method have growing interest due to their simple operation, cheap fabrication and high yield. In the past decade, much research has been done on the composition, formation mechanism and physical and chemical properties. But so far, it is not clear that formation mechanism, the origin of specific photoelectric properties in the visible light region and structural stability. Our main investigation can be summarized as follows:
We systemically studied the effect of the calcination temperature on the morphology, structural stability and optical properties of the titanate nanotubes from the thermodynamics degree. The results show that the sodium titanate nanotubes were thermally stable at T﹤600℃. But the titanic acid nanotubes were thermally unstable. It can be realized that the nanotubes have stronger absorption and emission in the visible light region by controlling the appropriate desiccation process. The three absorption peaks located at 515,575 and 675 nm, respectively.These specific absorption bands are in relation to the special energy levels. The specific photoelectric properties are determinated by the unique tubular structures and oxygen vacancies defects.We found that the titanic acid nanotubes transformed from orthorhombic to anatase at higher temperature.The mechanism of phase transition is that the dehydration of intralayered and interlayered groups in the titanate nanotubes under the thermodynamics conditions.After the orthorhombic structure was destroyed, the structure rearranged to form anatase lattice.
We systemically studied the effect of the post treatment on the structure and optical properties of the titanate nanotubes from the dynamics degree.The results show that the photoluminescence intensity increases and the peak position shifts to shorter wavelength with the decrease of pH values under the visible light excitation. XPS results have verified that the specific optical properties are in relation to the elements under the different chemical environment.We further revealed that the formation mechanism of the nanotubes and the mechanism of the phase transition from the orthorhombic structure to anatase were controlled by the morphology change induced by the surface chemistry. At the same time we could obtain one-dimentional titanate materials by controlling the appropriate post treatment conditions, which has the structural stability and stronger absorption in the visible light region.
In order to further investigate the formation mechanism of the nanotubes and the origin of specific photoelectric properties, we studied high pressure structural phase transitions of the sodium titanate nanotubes.In-situ high-pressure Raman and X-ray powder diffraction results show that two structural phase transitions were observed in the sodium titanate nanotubes in our pressure range. One is the phase transitions from the orthorhombic structure to lepidocate structure under the pressure of 5 GPa; the other is the phase transitions from lepidocate structure to the amorphous phase above the pressure of 16.7 GPa. At the same time the collapse of the tubular structure occurs. The structural phase transitions of the titanate nanotubes are irreversible. The high pressure metastable phase– the lepidocate structure can remain when the pressure recovers to ambient pressure. It demonstrates that Ti-O bonds play the important role in the structural phase transition of the titanate nanotubes.
在第二章中我们从热力学的角度系统地研究了煅烧温度对钛酸盐纳米管形貌、结构稳定性和光学性能的影响,发现钛酸钠纳米管是热力学稳定的,而钛酸纳米管是热力学不稳定的。通过控制合适的干噪过程可以实现纳米管在可见光区的强吸收和发射,并且纳米管具有特殊的吸收带是与其特定能级相联系的。纳米管这种特殊的光电性质是由钛酸盐独特的管状结构和缺陷决定的。发现钛酸纳米管在高温时向锐钛矿结构转变,相转变的机制是由于纳米管在热力学条件下层间和层内进行脱水,正交结构遭到破坏后结构进行重新排列而导致的。
在第三章中我们从动力学的角度研究了纳米管在不同pH值和不同的酸浓度条件下形貌、结构稳定性和光学性能的变化规律。结果表明在稀酸和水洗这种温和的条件下管状结构并没有遭到破坏,可见光激发后纳米管随着pH值的减小荧光强度增加。这种特殊的光电性质来源于束缚单电子的氧空位。而在浓酸的作用下,管状结构遭到了严重的破坏,动力学不稳定使其结构进行重新排列由正交结构转变为锐钛矿结构。同时通过控制合适的后处理条件我们可以获得结构稳定的在可见区具有强的光吸收的钛酸盐一维纳米材料。
为了深入研究钛酸盐纳米管的相变机制和其可见区的光吸收和发射的来源,在第四章中我们开展了高压下钛酸盐纳米管的结构相转变研究,以期为揭示钛酸盐纳米管结构相转变的本质和更深入的理解管状结构形成的机理和特殊光电性质的来源提供直接的实验证据。在第四章中我们对钛酸钠纳米管的高压结构相变进行了研究,利用高压拉曼和高压X射线衍射实验手段分析证明在我们所研究的压力范围内纳米管发生了两次结构相转变:一个是在压力小于5 GPa时发生了向纤铁矿结构(H0.7Ti1.825□0.175O4·H2O)的转变;另一个是当压力超过16.7 GPa时发生了向无定型的转变,同时纳米管发生了坍塌。钛酸盐纳米管的结构相转变属于不可逆相变,恢复到常压时高压亚稳相纤铁矿结构可以保持,Ti-O键在钛酸盐纳米管的结构相转变中扮演着十分重要的角色。
The titanate nanotubes have been attracted widely attention due to their strong absorption in the visible light region and potential application on the utilization of the solar energy. The titanate nanotubes prepared by the hydrothermal method have growing interest due to their simple operation, cheap fabrication and high yield. In the past decade, much research has been done on the composition, formation mechanism and physical and chemical properties. But so far, it is not clear that formation mechanism, the origin of specific photoelectric properties in the visible light region and structural stability. Our main investigation can be summarized as follows:
We systemically studied the effect of the calcination temperature on the morphology, structural stability and optical properties of the titanate nanotubes from the thermodynamics degree. The results show that the sodium titanate nanotubes were thermally stable at T﹤600℃. But the titanic acid nanotubes were thermally unstable. It can be realized that the nanotubes have stronger absorption and emission in the visible light region by controlling the appropriate desiccation process. The three absorption peaks located at 515,575 and 675 nm, respectively.These specific absorption bands are in relation to the special energy levels. The specific photoelectric properties are determinated by the unique tubular structures and oxygen vacancies defects.We found that the titanic acid nanotubes transformed from orthorhombic to anatase at higher temperature.The mechanism of phase transition is that the dehydration of intralayered and interlayered groups in the titanate nanotubes under the thermodynamics conditions.After the orthorhombic structure was destroyed, the structure rearranged to form anatase lattice.
We systemically studied the effect of the post treatment on the structure and optical properties of the titanate nanotubes from the dynamics degree.The results show that the photoluminescence intensity increases and the peak position shifts to shorter wavelength with the decrease of pH values under the visible light excitation. XPS results have verified that the specific optical properties are in relation to the elements under the different chemical environment.We further revealed that the formation mechanism of the nanotubes and the mechanism of the phase transition from the orthorhombic structure to anatase were controlled by the morphology change induced by the surface chemistry. At the same time we could obtain one-dimentional titanate materials by controlling the appropriate post treatment conditions, which has the structural stability and stronger absorption in the visible light region.
In order to further investigate the formation mechanism of the nanotubes and the origin of specific photoelectric properties, we studied high pressure structural phase transitions of the sodium titanate nanotubes.In-situ high-pressure Raman and X-ray powder diffraction results show that two structural phase transitions were observed in the sodium titanate nanotubes in our pressure range. One is the phase transitions from the orthorhombic structure to lepidocate structure under the pressure of 5 GPa; the other is the phase transitions from lepidocate structure to the amorphous phase above the pressure of 16.7 GPa. At the same time the collapse of the tubular structure occurs. The structural phase transitions of the titanate nanotubes are irreversible. The high pressure metastable phase– the lepidocate structure can remain when the pressure recovers to ambient pressure. It demonstrates that Ti-O bonds play the important role in the structural phase transition of the titanate nanotubes.
引文
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