几种氧（硫）化物纳米材料的制备及发光性质的研究
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摘要
纳米发光材料是非常重要的一类材料，在照明、显示、荧光探测、光电器件等领域有广泛的应用前景。在本论文中我们以几种典型的二元氧化物、复合氧化物、硫化物纳米材料为基质，采用不同的合成方法、控制产物的形貌，通过引入不同的激活离子，系统地研究了其发光性质，以寻求具有高性能的新型发光材料。
在第一章中，我们对纳米材料的基本概念、纳米材料的制备方法、纳米材料的结构和特性作了简单的介绍。并对发光理论、纳米发光材料的研究现状作了简要介绍。
在第二章中，我们以ZrO_2和Eu_2O_3为研究对象，研究了其制备过程和发光特性。采用沉淀法在400、500、600℃的热处理温度下，制备了粒径在3.8-6nm的ZrO_2纳米晶。并首次在其中引入了Pb~(2+)、Dy~(3+)，研究了它们的发光特点。观察到了Pb~(2+)位于630nm的红光发射和Dy~(3+)位于480nm和575nm的蓝光和黄光发射。发光中心间的交叉弛豫引发了浓度猝灭现象，pb2~(2+)和Dy~(3+)的最佳掺杂摩尔浓度值分别为5％和2％。产物中残余的氯离子对发光强度有很大的影响，由热处理温度的升高引起的氯离子含量的减少导致了发光强度的减弱。以Er~(3+)为共激活剂对ZrO_2：Mn~(2+)纳米晶中Mn~(2+)的发光进行敏化。由于Er~(3+)→Mn~(2+)间的能量传递，使得Mn~(2+)的发光强度大大增强。但由于两种离子间的能量传递具有相互竞争性，随Er~(3+)浓度的增加将导致发光的浓度猝灭。Er~(3+)的最佳掺杂浓度为0.3％。首次采用燃烧法以Ca~(2+)为稳定剂合成了ZrO_2纳米晶。通过改变Ca~(2+)的掺杂浓度，观察到了单斜相、四方相、立方相的相转变。在制得的纳米晶中掺入了探针离子Eu~(3+)观察到了Eu~(3+)由相变过程而导致的不同的发光现象。首次采用液相回流制备了Eu_2O_3的前躯体并通过热处理得到了梭形的具有介孔结构的Eu_2O_3。在制备过程中，采用分步加入尿素的方法，调节尿素的加入量和回流时间，得到了不同尺寸和纵横比的梭形介孔结构。小角X射线散射(SAXS)和N_2吸附的结果证实了产物具有介孔结构。高分辨电镜(HRTEM)测试表明孔壁是由Eu_2O_3纳米晶组成，且孔的分布是无序的。在梭形Eu_2O_3介孔结构的形成过程中，表面活性剂聚乙二醇(PEG)既作为反应调节剂、结构导向剂又作为软模板，起了重要的作用。发光测试表明Eu_2O_3介孔结构具有良好的红光发光特性。
Nanoscaled luminescent materials have found wide applications in many fields, such as display, illumination, photo-electronic devices. In order to explore novel luminescent systems with high efficiency, in this thesis, we chose and synthesized several oxide/sulfide nanomaterials via different methods and studied their luminescent properties systemically by introducing different dopant ions as well as their morphology-dependent optical properties.
In Chapter 1, we briefly introduced the conceptions, the preparation methods, the unique structural characteristic and properties of nanomaterials. Also, we introduced the corresponding theory of the luminescent nanomaterials.
In Chapter 2, we studied the preparation and luminescent properties of nanocrystalline ZrO_2 and Eu_2O_3. A simple precipitation method has been employed for the synthesis of ZrO_2 nanocrystals. By introducing Pb~(2+) and Dy~(3+) ions into ZrO_2, we firstly studied the luminescent properties of the doped system. Red emission at 630nm of Pb~(2+) and blue (480nm) and yellow emission (575nm) of Dy~(3+) can be observed. Because of the cross-relaxation process of luminescent centers, luminescent quenching occurs with the increase of the dopant concentrations. The optimal values for Pb~(2+) and Dy~(3+) are 5% and 2%, respectively. With increasing calcining temperature, the content of chlorine in the host decreases rapidly for evaporation, which induces the decrease of the luminescent intensity. Er~(3+) was introduced as a co-activator ion into the ZrO_2: Mn~(2+) nanocrystals. Due to the energy transfer of Er~(3+)→Mn~(2+), the emission intensity of Mn~(2+) was increased greatly. By adjusting the concentration of the dopant, the optimal value for Er~(3+) was determined to be 0.3%. By using Ca~(2+) as a stabilizer, we synthesized ZrO_2 nanocrystals at a relatively lower temperature (400℃) via a combustion process. The phase transformation from monoclinic (m) to
在第一章中，我们对纳米材料的基本概念、纳米材料的制备方法、纳米材料的结构和特性作了简单的介绍。并对发光理论、纳米发光材料的研究现状作了简要介绍。
在第二章中，我们以ZrO_2和Eu_2O_3为研究对象，研究了其制备过程和发光特性。采用沉淀法在400、500、600℃的热处理温度下，制备了粒径在3.8-6nm的ZrO_2纳米晶。并首次在其中引入了Pb~(2+)、Dy~(3+)，研究了它们的发光特点。观察到了Pb~(2+)位于630nm的红光发射和Dy~(3+)位于480nm和575nm的蓝光和黄光发射。发光中心间的交叉弛豫引发了浓度猝灭现象，pb2~(2+)和Dy~(3+)的最佳掺杂摩尔浓度值分别为5％和2％。产物中残余的氯离子对发光强度有很大的影响，由热处理温度的升高引起的氯离子含量的减少导致了发光强度的减弱。以Er~(3+)为共激活剂对ZrO_2：Mn~(2+)纳米晶中Mn~(2+)的发光进行敏化。由于Er~(3+)→Mn~(2+)间的能量传递，使得Mn~(2+)的发光强度大大增强。但由于两种离子间的能量传递具有相互竞争性，随Er~(3+)浓度的增加将导致发光的浓度猝灭。Er~(3+)的最佳掺杂浓度为0.3％。首次采用燃烧法以Ca~(2+)为稳定剂合成了ZrO_2纳米晶。通过改变Ca~(2+)的掺杂浓度，观察到了单斜相、四方相、立方相的相转变。在制得的纳米晶中掺入了探针离子Eu~(3+)观察到了Eu~(3+)由相变过程而导致的不同的发光现象。首次采用液相回流制备了Eu_2O_3的前躯体并通过热处理得到了梭形的具有介孔结构的Eu_2O_3。在制备过程中，采用分步加入尿素的方法，调节尿素的加入量和回流时间，得到了不同尺寸和纵横比的梭形介孔结构。小角X射线散射(SAXS)和N_2吸附的结果证实了产物具有介孔结构。高分辨电镜(HRTEM)测试表明孔壁是由Eu_2O_3纳米晶组成，且孔的分布是无序的。在梭形Eu_2O_3介孔结构的形成过程中，表面活性剂聚乙二醇(PEG)既作为反应调节剂、结构导向剂又作为软模板，起了重要的作用。发光测试表明Eu_2O_3介孔结构具有良好的红光发光特性。
Nanoscaled luminescent materials have found wide applications in many fields, such as display, illumination, photo-electronic devices. In order to explore novel luminescent systems with high efficiency, in this thesis, we chose and synthesized several oxide/sulfide nanomaterials via different methods and studied their luminescent properties systemically by introducing different dopant ions as well as their morphology-dependent optical properties.
In Chapter 1, we briefly introduced the conceptions, the preparation methods, the unique structural characteristic and properties of nanomaterials. Also, we introduced the corresponding theory of the luminescent nanomaterials.
In Chapter 2, we studied the preparation and luminescent properties of nanocrystalline ZrO_2 and Eu_2O_3. A simple precipitation method has been employed for the synthesis of ZrO_2 nanocrystals. By introducing Pb~(2+) and Dy~(3+) ions into ZrO_2, we firstly studied the luminescent properties of the doped system. Red emission at 630nm of Pb~(2+) and blue (480nm) and yellow emission (575nm) of Dy~(3+) can be observed. Because of the cross-relaxation process of luminescent centers, luminescent quenching occurs with the increase of the dopant concentrations. The optimal values for Pb~(2+) and Dy~(3+) are 5% and 2%, respectively. With increasing calcining temperature, the content of chlorine in the host decreases rapidly for evaporation, which induces the decrease of the luminescent intensity. Er~(3+) was introduced as a co-activator ion into the ZrO_2: Mn~(2+) nanocrystals. Due to the energy transfer of Er~(3+)→Mn~(2+), the emission intensity of Mn~(2+) was increased greatly. By adjusting the concentration of the dopant, the optimal value for Er~(3+) was determined to be 0.3%. By using Ca~(2+) as a stabilizer, we synthesized ZrO_2 nanocrystals at a relatively lower temperature (400℃) via a combustion process. The phase transformation from monoclinic (m) to
引文
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