氧化锌纳米结构的制备及光学、磁学、光催化性质研究
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摘要
氧化锌(ZnO)是一种重要的直接带隙半导体材料,禁带宽度3.37eV激子束缚能60meV。由于其宽的带隙、高的激子束缚能、优良的压电性质、大的比表面积和作为半导体的特点,纳米氧化锌在紫外激光器件、光电探测器、日用化工、医药卫生、环境保护等领域具有广阔的应用前景。研究表明,氧化锌纳米结构的性质随相应的制备方法、实验条件表现出很大的差异性。本文重点关注氧化锌纳米结构光致发光、光催化和磁学性质的探讨,并通过相应的实验手段分析了其微观机理,取得了如下重要的实验结果。
1在ZnO纳米晶中引入缺陷发光中心是制备强的可见光发光ZnO纳米材料的关键。考虑到Mg2+和Zn2+离子半径比较接近和ZnO两性化合物的特点,我们采用共沉淀法在低温条件下制备了Mg掺杂ZnO纳米晶并系统地研究了Mg掺杂对ZnO纳米晶结构、形貌和光致发光性质的影响。实验发现Mg掺杂增强了ZnO纳米晶的绿光发光,当Mg掺杂浓度为20%时,纳米晶的量子产率达到了22.8%。EPR、XRD、Uv-Vis等实验数据表明Mg掺杂在ZnO纳米晶中引入了锌空位(Vzn)和镁填隙(IMg)缺陷,理论分析表明,ZnO纳米晶强的可见光发光来自电子在对应缺陷能级和ZnO价带问的跃迁。
2 ZnO纳米颗粒的磁学性质随制备条件表现出很大的差异性。为探究缺陷对ZnO纳米颗粒磁学性质的影响,我们采用共沉淀法制备了纯的和不同掺杂比例的Mg、Co掺杂ZnO纳米颗粒,对其做了不同条件的退火处理,探究了掺杂比例、退火条件对其磁学性质的影响。实验发现纯的、Mg掺杂的ZnO纳米颗粒表现出弱的铁磁性,而Co掺杂和Mg、Co共掺杂的ZnO纳米颗粒却表现出顺磁性,氮气条件退火后的Mg掺杂ZnO纳米颗粒表现出较强的铁磁性。理论分析表明,ZnO纳米颗粒的铁磁性与氧缺陷有关,Co2+离子3d电子的非铁磁性交换相互作用强于该实验体系下锌空位、氧空位等缺陷铁磁性交换作用。
3人的比表面积、少的表面基团是提高ZnO光催化活性的要点,为此我们探索采用简易的煅烧法制备了ZnO纳米颗粒并探究了煅烧条件对其光催化性质的影响,实验发现600℃煅烧条件下制备的ZnO纳米颗粒C轴择优取向生长最佳,这种特殊的结构有比较大的(0001)(0001)表面积,具有最佳的光催化活性,光催化效果也最好。
Znic oxide is a kind of direct bandgap semiconductor whose bandgap is 3.37ev and exciton-banding energy is 60mev. According to its wide bandgap, high exciton-banding energy, fine pizoelectrical property and large specific area, nanosized ZnO has great potential application in ultraviolet lasers, optoelectronic detectors, chemical industry, medical science, environmental protection and so on. Generally, property of ZnO nanomaterial show great difference according to different fabrication method and experimental conditions. In this paper, we focused our attention on photoluminescent, photocatalytic and magnetic property of ZnO nanomaterial. By experiment and theoretical analysis, we get important conclusions as follows:
1. To prepare strong visible light emitting ZnO namomaterials, we should introduce luminescent vacancies into ZnO nanocrystals. Ionic radius of Mg2+is close to Zn2+and ZnO is amphoteric compound, so we prepared Mg doped ZnO nanocrystals by co-precipitation at low temperature. Convertion of its shape, structure and photoluminescent property by Mg doping is studied. In our investigation, a direct relationship between inhanced green luminescence and Mg doping is detected. When the doping concentration achieves 20%, the quantum yield (QY) of Mg doped ZnO NCs is about 22.8%. From detections by EPR, XRD and Uv-Vis, we found Mg doping introduced VZn and IMg vacancies into ZnO nanocrystals, theoretical analysis demonstrate the inhanced visible luminescence originate from radiative transition between energy levels of the vacancies and valence band of ZnO nanocrystals.
2. Magnetic property of ZnO nanocrystals varied by experimental condition, in order to investigate role of vacancies in magnetic ZnO NCs, we prepared pure and Mg/Co doped ZnO NCs and investigated magnetic property of them. The samples were prepared by co-precipitation method and annealed in air and N2. We studied variation of magnetic property of the samples with doping concentration and annealing condition. Strangely, pure and Mg dopd ZnO nanocrystals were weakly ferromagnetic but Co doped, Co/Mg co-doped ZnO nanocrystals were paramagnetic. Theoretical and experimental analysis demonstrate the ferromagnetism of pure ZnO NCs may stem from Vo vancancy, paramagnetic interaction of Co2+.ions in our samples was stronger than feeromagnetic interactions of vacancies.
3. Large surface area, less perssad on the surface is important to inhance photocatalytic property of ZnO NCs. So, we tried to prepare ZnO nanoplates by a simple combustion method and studied its photocatalytic property. The experimental results demonstrate when calcined at 600℃, the as-prepared nanoplates get better C-axis orientation and lead to bigger (0001), (0001) surface area. The as-prepared nanoplates showed good photocatalysis to methyl orange.
1在ZnO纳米晶中引入缺陷发光中心是制备强的可见光发光ZnO纳米材料的关键。考虑到Mg2+和Zn2+离子半径比较接近和ZnO两性化合物的特点,我们采用共沉淀法在低温条件下制备了Mg掺杂ZnO纳米晶并系统地研究了Mg掺杂对ZnO纳米晶结构、形貌和光致发光性质的影响。实验发现Mg掺杂增强了ZnO纳米晶的绿光发光,当Mg掺杂浓度为20%时,纳米晶的量子产率达到了22.8%。EPR、XRD、Uv-Vis等实验数据表明Mg掺杂在ZnO纳米晶中引入了锌空位(Vzn)和镁填隙(IMg)缺陷,理论分析表明,ZnO纳米晶强的可见光发光来自电子在对应缺陷能级和ZnO价带问的跃迁。
2 ZnO纳米颗粒的磁学性质随制备条件表现出很大的差异性。为探究缺陷对ZnO纳米颗粒磁学性质的影响,我们采用共沉淀法制备了纯的和不同掺杂比例的Mg、Co掺杂ZnO纳米颗粒,对其做了不同条件的退火处理,探究了掺杂比例、退火条件对其磁学性质的影响。实验发现纯的、Mg掺杂的ZnO纳米颗粒表现出弱的铁磁性,而Co掺杂和Mg、Co共掺杂的ZnO纳米颗粒却表现出顺磁性,氮气条件退火后的Mg掺杂ZnO纳米颗粒表现出较强的铁磁性。理论分析表明,ZnO纳米颗粒的铁磁性与氧缺陷有关,Co2+离子3d电子的非铁磁性交换相互作用强于该实验体系下锌空位、氧空位等缺陷铁磁性交换作用。
3人的比表面积、少的表面基团是提高ZnO光催化活性的要点,为此我们探索采用简易的煅烧法制备了ZnO纳米颗粒并探究了煅烧条件对其光催化性质的影响,实验发现600℃煅烧条件下制备的ZnO纳米颗粒C轴择优取向生长最佳,这种特殊的结构有比较大的(0001)(0001)表面积,具有最佳的光催化活性,光催化效果也最好。
Znic oxide is a kind of direct bandgap semiconductor whose bandgap is 3.37ev and exciton-banding energy is 60mev. According to its wide bandgap, high exciton-banding energy, fine pizoelectrical property and large specific area, nanosized ZnO has great potential application in ultraviolet lasers, optoelectronic detectors, chemical industry, medical science, environmental protection and so on. Generally, property of ZnO nanomaterial show great difference according to different fabrication method and experimental conditions. In this paper, we focused our attention on photoluminescent, photocatalytic and magnetic property of ZnO nanomaterial. By experiment and theoretical analysis, we get important conclusions as follows:
1. To prepare strong visible light emitting ZnO namomaterials, we should introduce luminescent vacancies into ZnO nanocrystals. Ionic radius of Mg2+is close to Zn2+and ZnO is amphoteric compound, so we prepared Mg doped ZnO nanocrystals by co-precipitation at low temperature. Convertion of its shape, structure and photoluminescent property by Mg doping is studied. In our investigation, a direct relationship between inhanced green luminescence and Mg doping is detected. When the doping concentration achieves 20%, the quantum yield (QY) of Mg doped ZnO NCs is about 22.8%. From detections by EPR, XRD and Uv-Vis, we found Mg doping introduced VZn and IMg vacancies into ZnO nanocrystals, theoretical analysis demonstrate the inhanced visible luminescence originate from radiative transition between energy levels of the vacancies and valence band of ZnO nanocrystals.
2. Magnetic property of ZnO nanocrystals varied by experimental condition, in order to investigate role of vacancies in magnetic ZnO NCs, we prepared pure and Mg/Co doped ZnO NCs and investigated magnetic property of them. The samples were prepared by co-precipitation method and annealed in air and N2. We studied variation of magnetic property of the samples with doping concentration and annealing condition. Strangely, pure and Mg dopd ZnO nanocrystals were weakly ferromagnetic but Co doped, Co/Mg co-doped ZnO nanocrystals were paramagnetic. Theoretical and experimental analysis demonstrate the ferromagnetism of pure ZnO NCs may stem from Vo vancancy, paramagnetic interaction of Co2+.ions in our samples was stronger than feeromagnetic interactions of vacancies.
3. Large surface area, less perssad on the surface is important to inhance photocatalytic property of ZnO NCs. So, we tried to prepare ZnO nanoplates by a simple combustion method and studied its photocatalytic property. The experimental results demonstrate when calcined at 600℃, the as-prepared nanoplates get better C-axis orientation and lead to bigger (0001), (0001) surface area. The as-prepared nanoplates showed good photocatalysis to methyl orange.
引文
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