氧化铁基异质结构纳米材料的制备及光电性质研究
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摘要
光电功能材料铁基氧化物及其复合物,具有较好的光电性质,可以应用到光催化、太阳电池及光电子器件等领域。它们优异的光电活性是与光生电荷的迁移行为密切相关的。因此,研究材料的微观的光生电荷载流子的行为特性对于其在光电领域的应用是十分必要的。本论文的工作主要是探讨了光电材料的光生电荷行为特性所表现出来的光电性质与光电活性的关系。首先利用表面光电压技术、Kelvin探针技术及瞬态光电压技术研究了一维有序的α-Fe_2O_3纳米棒阵列结构区别于体相α-Fe_2O_3的特殊的光电性质,证明了α-Fe_2O_3纳米棒阵列结构的量子尺寸效应。然后在这种阵列结构的基础上,与TiO_2构筑成具有异质界面的FTO/TiO_2/Fe_2O_3复合材料电极结构,比较了复合材料电极与单层α-Fe_2O_3纳米棒阵列电极的光电催化活性,测试结果表明复合材料料电极具有较好的光电催化降解染料的活性,同时探讨了复合材料电极相对于单层薄膜电极光生电荷运动行为的变化。最后,设计制备了α-Fe_2O_3纳米粒子包覆锐钛矿型TiO_2微米棒的异质结构复合物粉体,测试了其可见光催化降解有机染料的活性,说明了异质结构复合物优于单独的α-Fe_2O_3和TiO_2微米棒的光催化活性,并利用表面光伏技术证明了材料的光电活性与其本身的光电压性质的内在关系。
Nanomaterials with photoelectric properties are applied to the photocatalysis, solar cell, biological sensor and photoelectric device, etc., following the development of the technology. Iron oxide attracts much attention for its special photoelectric properties among the various nanomaterials. Iron oxide with low band gap of 2.2 eV could absorb most of visible light. Moreover, iron oxide has many morphologies and it will appear some new photoelectric properties for iron oxide with particular structure and dimension. At the same time, poor conductivity, facility to recombine for electron-hole pairs in iron oxide are inhibiting its promising applications. In recent years, many approaches against its drawbacks have been made to improve the photoelectric properties. Among these methods, more efforts have been focused on the polycrystalline heterostructures based on the iron oxide. For this heterogeneous structural material, we could not only utilize the virtues of the iron oxide, but also accelerate the separation of the electons and holes under the influence of heterojunction between two different materials, which could promote the photoelectric activity of the materials. Therefore, the behaviors of photogenerated charges, including the generation, separation, transportation and recombination of the photoexcited charge carriers, directly determine the photoelectric performance of the materials. The surface photovoltage (SPV) technique is a well-suitable and more direct method to characterize the behavior of the photoinduced charges.
In this thesis, we studied the photoelectric properties of theα-Fe_2O_3 nanorod array that are different from the bulk Fe_2O_3 by Kelvin probe system, SPV technique and the transient photovoltage (TPV) technique at first. And then the FTO/TiO_2/Fe_2O_3 two-layered film electrode was prepared based on the FTO/Fe_2O_3 film eldctrode. We compared the photocatalytic activity of the two electrodes and discussed the behaviors of the photogenerated charge carriers at the FTO/TiO_2/Fe_2O_3 two-layered film electrode. At last, we synthesized the Fe_2O_3/TiO_2 composites by coating TiO_2 microrods with Fe_2O_3 nanoparticles and tested the photocatalytic activity of the heterogeneous composites. The relationship between the photocatalytic activity and the photoelectric properties was demonstrated by the SPV and TPV spectra.
The main results of this paper are illustrated as follows:
1. Anα-Fe_2O_3 nanorod array was prepared by the hydrothermal method, and we have studied the photoelectric property and the kinetics of this structure by the SPV and the TPV technology. When theα-Fe_2O_3 nanorod array is excited from the surface, the SPV response takes place only in the ultraviolet region where the photonic energy is much larger than the bulk band gap and exhibits a quantum size effect. The photogenerated electrons transfer to the nanorod surface as a result of the high density of surface states. When the light is incident from the interface between the substrate and the nanorod array, the SPV response extends from ultraviolet to visible region due to the influence of the built-in field at the interface between the substrate and the bottom of the nanorod array, which corresponds to the band-to-band transition and exhibits the bulk property of theα-Fe_2O_3. The photogenerated charges of theα-Fe_2O_3 nanorod array are prone to separate and also to recombine upon illumination. From the comparison of photovoltage properties between theα-Fe_2O_3 nanorod array and theα-Fe_2O_3 nanorod powders, we could find the SPV spectra of theα-Fe_2O_3 nanorod powders only reflect the properties of bulk Fe_2O_3. These results on the behaviors of the photogenerated charge transfer at the surface and the interface of theα-Fe_2O_3 nanorod array could reflect the photoelectric activity of this material. So the information provided in this chapter may provide useful supports for the practical application ofα-Fe_2O_3 nanorod array in solar cell, photocatalysis and sensors.
2. Based on the Fe_2O_3 nanorod array, we prepared the FTO/TiO_2/Fe_2O_3 two-layered film electrode which had the heterogeneous structure. We tested the photoelectric activity by degrading orangeⅡvia combined electro-oxidation and photocatalysis and studied the photoelectric properties of the FTO/TiO_2/Fe_2O_3 two-layered film electrode by electrochemical system, the SPV and the TPV systems. The influences of the hetero-interface between the Fe_2O_3 and TiO_2 on the behaviors of photoexcited charges were discussed. We could obtain the conclusions as follows. The working electrode could generate more photogenerated charges under the excitation of the visible light. The photoelectric activity of the working electrode could be improved by combining the applied electric field on the base of visible light irradiation. Compared the experimental results of photoelectric catalytic (PEC) degradation of organic dye, the PEC activity of the FTO/TiO_2/Fe_2O_3 two-layered film electrode was superior to the FTO/Fe_2O_3 single-layered film electrode. From the TPV and SPV spectra, we could observe that the photogenerated electrons and holes were easier to separate and difficult to recombination under the effect of the hetero-interface in the FTO/TiO_2/Fe_2O_3 two-layered film electrode. Therefore, these results could provide useful information for the application of those two electrodes in photoelectric device.
3. The Fe_2O_3/TiO_2 hetero-structural composites with three mass ratios (Fe_2O_3 vs. TiO_2) by Fe_2O_3 nanoparticles covered TiO_2 microrods were prepared. The photocatalytic experimental results revealed that the Fe_2O_3/TiO_2 composites with hetero-structure were more active than the corresponding bare Fe_2O_3 or bare TiO_2 in the photodegradation of orange II under visible light illumination. Furthermore, the higher the mass ratio of Fe_2O_3 vs. TiO_2 is, the better the photocatalytic activity is for the composites. By comparing the photovoltaic property of pure Fe_2O_3 with that of Fe_2O_3/TiO_2 heterogeneous composites, we observed that the hetero-interface between Fe_2O_3 and TiO_2 imposed an important influence on the behaviors of photogenerated charge carriers. Moreover, the characteristics of the photogenerated charges were associated with the photocatalytic activity. With respect to the pure Fe_2O_3, the photoexcited electrons and holes of the Fe_2O_3/TiO_2 composites were prone to separate under the effect of interfacial electric field under visible light irradiation, which resulted in the enhanced photocatalytic activity of Fe_2O_3/TiO_2 hetero-structural composites. The quantity of the Fe_2O_3 coated on the TiO_2 microrods influenced the interfacial electric field and thus the transfer behaviors of the photogenerated charges, as revealed by the SPS and TPV characterizations. As a result, the photodegrading rates towards orange II were distinct from each other for the Fe_2O_3/TiO_2 composites with different mass ratios. Therefore, the results presented in this work may provide well-suitable and more direct methods to evaluate the photoelectric activities of the advanced materials for practical application such as photocatalysis.
Nanomaterials with photoelectric properties are applied to the photocatalysis, solar cell, biological sensor and photoelectric device, etc., following the development of the technology. Iron oxide attracts much attention for its special photoelectric properties among the various nanomaterials. Iron oxide with low band gap of 2.2 eV could absorb most of visible light. Moreover, iron oxide has many morphologies and it will appear some new photoelectric properties for iron oxide with particular structure and dimension. At the same time, poor conductivity, facility to recombine for electron-hole pairs in iron oxide are inhibiting its promising applications. In recent years, many approaches against its drawbacks have been made to improve the photoelectric properties. Among these methods, more efforts have been focused on the polycrystalline heterostructures based on the iron oxide. For this heterogeneous structural material, we could not only utilize the virtues of the iron oxide, but also accelerate the separation of the electons and holes under the influence of heterojunction between two different materials, which could promote the photoelectric activity of the materials. Therefore, the behaviors of photogenerated charges, including the generation, separation, transportation and recombination of the photoexcited charge carriers, directly determine the photoelectric performance of the materials. The surface photovoltage (SPV) technique is a well-suitable and more direct method to characterize the behavior of the photoinduced charges.
In this thesis, we studied the photoelectric properties of theα-Fe_2O_3 nanorod array that are different from the bulk Fe_2O_3 by Kelvin probe system, SPV technique and the transient photovoltage (TPV) technique at first. And then the FTO/TiO_2/Fe_2O_3 two-layered film electrode was prepared based on the FTO/Fe_2O_3 film eldctrode. We compared the photocatalytic activity of the two electrodes and discussed the behaviors of the photogenerated charge carriers at the FTO/TiO_2/Fe_2O_3 two-layered film electrode. At last, we synthesized the Fe_2O_3/TiO_2 composites by coating TiO_2 microrods with Fe_2O_3 nanoparticles and tested the photocatalytic activity of the heterogeneous composites. The relationship between the photocatalytic activity and the photoelectric properties was demonstrated by the SPV and TPV spectra.
The main results of this paper are illustrated as follows:
1. Anα-Fe_2O_3 nanorod array was prepared by the hydrothermal method, and we have studied the photoelectric property and the kinetics of this structure by the SPV and the TPV technology. When theα-Fe_2O_3 nanorod array is excited from the surface, the SPV response takes place only in the ultraviolet region where the photonic energy is much larger than the bulk band gap and exhibits a quantum size effect. The photogenerated electrons transfer to the nanorod surface as a result of the high density of surface states. When the light is incident from the interface between the substrate and the nanorod array, the SPV response extends from ultraviolet to visible region due to the influence of the built-in field at the interface between the substrate and the bottom of the nanorod array, which corresponds to the band-to-band transition and exhibits the bulk property of theα-Fe_2O_3. The photogenerated charges of theα-Fe_2O_3 nanorod array are prone to separate and also to recombine upon illumination. From the comparison of photovoltage properties between theα-Fe_2O_3 nanorod array and theα-Fe_2O_3 nanorod powders, we could find the SPV spectra of theα-Fe_2O_3 nanorod powders only reflect the properties of bulk Fe_2O_3. These results on the behaviors of the photogenerated charge transfer at the surface and the interface of theα-Fe_2O_3 nanorod array could reflect the photoelectric activity of this material. So the information provided in this chapter may provide useful supports for the practical application ofα-Fe_2O_3 nanorod array in solar cell, photocatalysis and sensors.
2. Based on the Fe_2O_3 nanorod array, we prepared the FTO/TiO_2/Fe_2O_3 two-layered film electrode which had the heterogeneous structure. We tested the photoelectric activity by degrading orangeⅡvia combined electro-oxidation and photocatalysis and studied the photoelectric properties of the FTO/TiO_2/Fe_2O_3 two-layered film electrode by electrochemical system, the SPV and the TPV systems. The influences of the hetero-interface between the Fe_2O_3 and TiO_2 on the behaviors of photoexcited charges were discussed. We could obtain the conclusions as follows. The working electrode could generate more photogenerated charges under the excitation of the visible light. The photoelectric activity of the working electrode could be improved by combining the applied electric field on the base of visible light irradiation. Compared the experimental results of photoelectric catalytic (PEC) degradation of organic dye, the PEC activity of the FTO/TiO_2/Fe_2O_3 two-layered film electrode was superior to the FTO/Fe_2O_3 single-layered film electrode. From the TPV and SPV spectra, we could observe that the photogenerated electrons and holes were easier to separate and difficult to recombination under the effect of the hetero-interface in the FTO/TiO_2/Fe_2O_3 two-layered film electrode. Therefore, these results could provide useful information for the application of those two electrodes in photoelectric device.
3. The Fe_2O_3/TiO_2 hetero-structural composites with three mass ratios (Fe_2O_3 vs. TiO_2) by Fe_2O_3 nanoparticles covered TiO_2 microrods were prepared. The photocatalytic experimental results revealed that the Fe_2O_3/TiO_2 composites with hetero-structure were more active than the corresponding bare Fe_2O_3 or bare TiO_2 in the photodegradation of orange II under visible light illumination. Furthermore, the higher the mass ratio of Fe_2O_3 vs. TiO_2 is, the better the photocatalytic activity is for the composites. By comparing the photovoltaic property of pure Fe_2O_3 with that of Fe_2O_3/TiO_2 heterogeneous composites, we observed that the hetero-interface between Fe_2O_3 and TiO_2 imposed an important influence on the behaviors of photogenerated charge carriers. Moreover, the characteristics of the photogenerated charges were associated with the photocatalytic activity. With respect to the pure Fe_2O_3, the photoexcited electrons and holes of the Fe_2O_3/TiO_2 composites were prone to separate under the effect of interfacial electric field under visible light irradiation, which resulted in the enhanced photocatalytic activity of Fe_2O_3/TiO_2 hetero-structural composites. The quantity of the Fe_2O_3 coated on the TiO_2 microrods influenced the interfacial electric field and thus the transfer behaviors of the photogenerated charges, as revealed by the SPS and TPV characterizations. As a result, the photodegrading rates towards orange II were distinct from each other for the Fe_2O_3/TiO_2 composites with different mass ratios. Therefore, the results presented in this work may provide well-suitable and more direct methods to evaluate the photoelectric activities of the advanced materials for practical application such as photocatalysis.
引文
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