稀土掺杂特殊形貌二氧化钛纳米材料的制备及其发光性能研究
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摘要
由于科技的进步，照明材料已经从过去的煤油灯时代发展到今天五光十色的高性能的电灯照明时代。并且随着人们对物质方面的要求的提高，照明材料的需求也越来越高。基于这些，研究者们加大了对发光材料的研究，制备了更多性能优异的发光材料。TiO_2因其具有优异的性能而常被用作发光材料的基质，展现出良好的应用前景。本文以TiO_2为基质，采用水热法制备了Eu~(3+)掺杂的TiO_2纳米棒、纳米带和纺锤形纳米结构，采用微乳法制备了Eu~(3+)掺杂的TiO_2三维花状结构。利用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线衍射（XRD)、傅里叶红外光谱（FT-IR)、光致发光光谱（PL）等现代分析技术，对发光材料进行了表征,系统研究了材料的形貌对发光性能的影响，并探讨了不同形貌的形成及其对发光性能影响的机理。主要工作有以下几个方面：
1、通过一种简单的水热过程成功合成了钛酸纳米管和纳米带。纳米管是由包含数层的片状结构组成的。纳米管的形成是一个从纳米粒子到纳米片的生长过程，接着纳米片在反应条件提供的驱动力下发生卷曲，最后得到纳米管结构；纳米带的形成是由纳米粒子在一定的实验条件下先形成小的纳米带，最后小的纳米带聚集形成较大的带状结构。
2、采用水热方法成功地制备了Eu~(3+)掺杂和Eu~(3+)/Gd~(3+)共掺的TiO_2纳米带。研究表明，煅烧温度不仅对TiO_2的晶体结构和形貌有很大影响，同时也影响其发光性能。在UV激发下，Eu~(3+)掺杂的TiO_2纳米带显示红光发射。纳米带的发光强度与Gd~(3+)和Eu~(3+)的掺杂浓度有关，发光性质主要取决于Eu~(3+)。
3、通过一步简单水热反应以及随后的煅烧过程成功制备出TiO_2:Eu~(3+)纳米棒。研究发现制得的前驱体为钛酸结构纳米管；煅烧处理后，纳米管转变为纳米棒。最终的TiO_2:Eu~(3+)纳米棒和纳米带由于Eu~(3+)的f-f跃迁在紫外激发下有强的红光发射。
4、通过两步水热过程得到了形貌规则、均一好、分散性好的的TiO_2:Eu~(3+)纺锤形纳米粒子。详细地研究了锐钛矿、钛酸钠和钛酸间的相转化和纺锤形TiO_2纳米粒子可能的形成机理。最终产物TiO_2:Eu~(3+)纺锤形纳米粒子在紫外光激发下显示强的红光发射。
5、成功制备了三种不同形貌的三维花状结构TiO_2纳米颗粒。花状TiO_2晶型为金红石型。对其形成机理进行了简单的分析。荧光光谱研究表明花状结构的发光强度较弱，这主要是由基体的晶型不同引起的。
With the development of the society, people's physical requirements are alsogetting higher and higher. Lighting materials have been already developed from thepast kerosene lamp era to today's resplendent with variegated coloration of highperformance electric lighting Era. It was required that the lighting materials shouldalso be developed with the demand of the people. Therefore, the researchers increasedthe luminescent materials research investment, and found much more luminescentmaterials. TiO_2, as a kind of good matrix, has shown a good application prospect inluminescent materials. In this work, TiO_2was used as matrix, and Eu~(3+)-doped TiO_2nanorods, nanobelts and spindle-shaped nanoparticles were prepared by hydrothermalmethod. In addition, Eu~(3+)ions doped3-dimensional flower-like TiO_2nanoparticleswere fabricated by micro-emulsion method. To study the effects of the morphology onthe luminescent properties, modern analysis techniques including SEM, TEM, XRD,FT-IR and PL were used to investigate the characteristics of these materials. The mainresults of the research work are as follows：
1. Titanate nanotubes and nanobelts were successfully synthesized via a simplehydrothermal process. The TiO_2nanoparticles are grown to nanosheets, finally turnedinto nanotubes structure under the driving force in this process. Nanobelts were alsoformed from the TiO_2nanoparticles under certain experimental conditions. Smallnanobelts were formed, and the small nanobelts bind together to form the finalnanobelt structure. The crystallization rate has great influence on the formation ofmorphology. If the crystallization rate is large enough so that the growth of thenanosheets can be more than the general value, and then they will overlap each other,become hard and difficult to curl, resulting in the formation of nanobelt instead of nanotubes.
2. TiO_2:Eu~(3+)nanobelts have been successfully prepared using the hydrothermalmethod. The XRD results show that anatase-phase TiO_2can be formed attemperatures above300oC, and the optimal calcination temperature is500oC. Underthe UV excitation, TiO_2:Eu~(3+)nanobelts exhibit red emission. The calcinationtemperature has a great influence not only on the crystal structure and morphology,but also on the luminescence properties. It is expected that TiO_2:Eu~(3+)nanobelts can bea potential candidate as the novel semiconductor fluorescence materials.
3. The controllable synthesis of TiO_2:Eu~(3+)nanorods have been successfullyachieved through a simple hydrothermal process followed by the calcination process.The as-obtained precursors have the structure of titanate. The morphology of thenanotubes changed to nanorods after calcination process. The final TiO_2:Eu~(3+)nanorods showed a strong red emission under ultraviolet excitation.
4. Highly uniform TiO_2:Eu~(3+)spindle-shaped nanoparticles were synthesized bytwo-step hydrothermal processes. The width of the nanobelt precursor is about50–200nm and the lengths are about several micrometers. The diameters of the TiO_2:Eu~(3+)spindle shaped nanoparticles are about50–200nm and the lengths about200-1000nm.The phase transformation among the anatase structure, sodium titanate and titanateand the possible formation mechanism were also investigated in detail. The finalproducts of the TiO_2:Eu~(3+)spindle shaped nanoparticles show strong red emissionintensity under ultraviolet excitation, which is due to the lack of inversion symmetryat the Eu~(3+)ions site and depends strongly on the site symmetry in a host crystal. It canbe anticipated that the as-prepared product is a potential candidate as the novelsemiconductor luminescent materials.
5. TiO_2:Eu~(3+)nanorods and spindle-shaped nanoparticles have been synthesized through simple calcination and two-step hydrothermal processes using titanate as theprecursors. Not only the morphologies of the precursors have been changed fromnanotubes to nanorods and spindle-shaped nanoparticles, but also the structures of theprecursors have been transformed into anatase nanostructure. Under UV lightexcitation, the TiO_2:Eu~(3+)nanorods and spindle-shaped nanoparticles exhibit the strongred emission corresponding to the5D0-7F2transition of the Eu~(3+)ions. In addition, theluminescence intensity of the TiO_2:Eu~(3+)nanorods is stronger than that of spindle-shaped nanoparticles, which is due to the defects on the surface of the samples.
6. We have demonstrated a facile route to synthesize3-dimensional flower-likeTiO_2using commercial CTAB as the reacting surfactant and template in the acidsurrounding. The PL spectrums show that the3-dimensional flower-like TiO_2:Eu~(3+)exhibited emission peak centered at around614nm when the excitation wavelength is393nm. However, It was found that the emission intensity of the3-dimensionalflower-like TiO_2:Eu~(3+)is lower than that of the other morphologies TiO_2, which is dueto the matrix can not transfer their energy to rare earth ions, and rare earth ion returnto the excited state by itself. The synthesis of3-dimensional flower like TiO_2:Eu~(3+)crystals in the acid surrounding will provide a new route to other compounds withcontrolled shapes and sizes.
1、通过一种简单的水热过程成功合成了钛酸纳米管和纳米带。纳米管是由包含数层的片状结构组成的。纳米管的形成是一个从纳米粒子到纳米片的生长过程，接着纳米片在反应条件提供的驱动力下发生卷曲，最后得到纳米管结构；纳米带的形成是由纳米粒子在一定的实验条件下先形成小的纳米带，最后小的纳米带聚集形成较大的带状结构。
2、采用水热方法成功地制备了Eu~(3+)掺杂和Eu~(3+)/Gd~(3+)共掺的TiO_2纳米带。研究表明，煅烧温度不仅对TiO_2的晶体结构和形貌有很大影响，同时也影响其发光性能。在UV激发下，Eu~(3+)掺杂的TiO_2纳米带显示红光发射。纳米带的发光强度与Gd~(3+)和Eu~(3+)的掺杂浓度有关，发光性质主要取决于Eu~(3+)。
3、通过一步简单水热反应以及随后的煅烧过程成功制备出TiO_2:Eu~(3+)纳米棒。研究发现制得的前驱体为钛酸结构纳米管；煅烧处理后，纳米管转变为纳米棒。最终的TiO_2:Eu~(3+)纳米棒和纳米带由于Eu~(3+)的f-f跃迁在紫外激发下有强的红光发射。
4、通过两步水热过程得到了形貌规则、均一好、分散性好的的TiO_2:Eu~(3+)纺锤形纳米粒子。详细地研究了锐钛矿、钛酸钠和钛酸间的相转化和纺锤形TiO_2纳米粒子可能的形成机理。最终产物TiO_2:Eu~(3+)纺锤形纳米粒子在紫外光激发下显示强的红光发射。
5、成功制备了三种不同形貌的三维花状结构TiO_2纳米颗粒。花状TiO_2晶型为金红石型。对其形成机理进行了简单的分析。荧光光谱研究表明花状结构的发光强度较弱，这主要是由基体的晶型不同引起的。
With the development of the society, people's physical requirements are alsogetting higher and higher. Lighting materials have been already developed from thepast kerosene lamp era to today's resplendent with variegated coloration of highperformance electric lighting Era. It was required that the lighting materials shouldalso be developed with the demand of the people. Therefore, the researchers increasedthe luminescent materials research investment, and found much more luminescentmaterials. TiO_2, as a kind of good matrix, has shown a good application prospect inluminescent materials. In this work, TiO_2was used as matrix, and Eu~(3+)-doped TiO_2nanorods, nanobelts and spindle-shaped nanoparticles were prepared by hydrothermalmethod. In addition, Eu~(3+)ions doped3-dimensional flower-like TiO_2nanoparticleswere fabricated by micro-emulsion method. To study the effects of the morphology onthe luminescent properties, modern analysis techniques including SEM, TEM, XRD,FT-IR and PL were used to investigate the characteristics of these materials. The mainresults of the research work are as follows：
1. Titanate nanotubes and nanobelts were successfully synthesized via a simplehydrothermal process. The TiO_2nanoparticles are grown to nanosheets, finally turnedinto nanotubes structure under the driving force in this process. Nanobelts were alsoformed from the TiO_2nanoparticles under certain experimental conditions. Smallnanobelts were formed, and the small nanobelts bind together to form the finalnanobelt structure. The crystallization rate has great influence on the formation ofmorphology. If the crystallization rate is large enough so that the growth of thenanosheets can be more than the general value, and then they will overlap each other,become hard and difficult to curl, resulting in the formation of nanobelt instead of nanotubes.
2. TiO_2:Eu~(3+)nanobelts have been successfully prepared using the hydrothermalmethod. The XRD results show that anatase-phase TiO_2can be formed attemperatures above300oC, and the optimal calcination temperature is500oC. Underthe UV excitation, TiO_2:Eu~(3+)nanobelts exhibit red emission. The calcinationtemperature has a great influence not only on the crystal structure and morphology,but also on the luminescence properties. It is expected that TiO_2:Eu~(3+)nanobelts can bea potential candidate as the novel semiconductor fluorescence materials.
3. The controllable synthesis of TiO_2:Eu~(3+)nanorods have been successfullyachieved through a simple hydrothermal process followed by the calcination process.The as-obtained precursors have the structure of titanate. The morphology of thenanotubes changed to nanorods after calcination process. The final TiO_2:Eu~(3+)nanorods showed a strong red emission under ultraviolet excitation.
4. Highly uniform TiO_2:Eu~(3+)spindle-shaped nanoparticles were synthesized bytwo-step hydrothermal processes. The width of the nanobelt precursor is about50–200nm and the lengths are about several micrometers. The diameters of the TiO_2:Eu~(3+)spindle shaped nanoparticles are about50–200nm and the lengths about200-1000nm.The phase transformation among the anatase structure, sodium titanate and titanateand the possible formation mechanism were also investigated in detail. The finalproducts of the TiO_2:Eu~(3+)spindle shaped nanoparticles show strong red emissionintensity under ultraviolet excitation, which is due to the lack of inversion symmetryat the Eu~(3+)ions site and depends strongly on the site symmetry in a host crystal. It canbe anticipated that the as-prepared product is a potential candidate as the novelsemiconductor luminescent materials.
5. TiO_2:Eu~(3+)nanorods and spindle-shaped nanoparticles have been synthesized through simple calcination and two-step hydrothermal processes using titanate as theprecursors. Not only the morphologies of the precursors have been changed fromnanotubes to nanorods and spindle-shaped nanoparticles, but also the structures of theprecursors have been transformed into anatase nanostructure. Under UV lightexcitation, the TiO_2:Eu~(3+)nanorods and spindle-shaped nanoparticles exhibit the strongred emission corresponding to the5D0-7F2transition of the Eu~(3+)ions. In addition, theluminescence intensity of the TiO_2:Eu~(3+)nanorods is stronger than that of spindle-shaped nanoparticles, which is due to the defects on the surface of the samples.
6. We have demonstrated a facile route to synthesize3-dimensional flower-likeTiO_2using commercial CTAB as the reacting surfactant and template in the acidsurrounding. The PL spectrums show that the3-dimensional flower-like TiO_2:Eu~(3+)exhibited emission peak centered at around614nm when the excitation wavelength is393nm. However, It was found that the emission intensity of the3-dimensionalflower-like TiO_2:Eu~(3+)is lower than that of the other morphologies TiO_2, which is dueto the matrix can not transfer their energy to rare earth ions, and rare earth ion returnto the excited state by itself. The synthesis of3-dimensional flower like TiO_2:Eu~(3+)crystals in the acid surrounding will provide a new route to other compounds withcontrolled shapes and sizes.
引文
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