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稀土掺杂氧化铟锌纳米粉体制备及其微观组织调控

Preparation and microstructure control of rare earth doped indium zinc oxide nanopowders

  • 摘要: 共沉淀法可实现金属离子原子级均匀混合,有效改善粉体组分偏析,提升掺杂均匀性。以非掺杂氧化铟锌(indium zinc oxide,IZO)为研究对象,采用共沉淀工艺制备In、Zn原子比1:1的IZO纳米粉体,探究沉淀终止pH与煅烧温度对粉体物相、形貌的影响,确定最优共沉淀工艺参数。在此基础上制备PrIZO、NdIZO、TbIZO稀土元素掺杂纳米粉体,稀土元素(Pr、Nd、Tb)、In、Zn原子比为0.01:1.00:1.00。通过热重-示差扫描量热法(thermogravimetric-differential scanning calorimeter,TG-DSC)剖析不同元素掺杂前驱体的热分解、物相转变与晶化过程。借助X射线衍射(X-ray diffraction,XRD)分析前驱体及煅烧粉体的物相结构。利用扫描电子显微镜(scanning electron microscope,SEM)和透射电子显微镜(transmission electron microscope,TEM)表征粉体微观形貌与粒径特征,并结合能谱分析(energy disperse spectroscopy,EDS)和傅里叶变换红外光谱(Fourier transform infrared spectroscopyFT-IR)验证粉体元素组成与分散均匀性。结果表明,稀土掺杂可有效调控IZO粉体的热行为、结晶性能与微观形貌,最终成功制备出粒径均匀、分散性良好、球形度优异的IZO及稀土掺杂IZO纳米粉体,明确了稀土元素掺杂对IZO前驱体及煅烧粉体物相结构及微观形貌的调控规律。

     

    Abstract: The coprecipitation method enables the atomic-level homogeneous mixing of metal ions, effectively mitigating powder composition segregation and enhancing doping uniformity. The non-doped indium zinc oxide (IZO) nanopowders were synthesized by coprecipitation with In:Zn atomic ratio of 1:1 in this study, the effects of final precipitation pH and calcination temperature on phase composition and morphology were investigated, and the optimal process parameters were established. Subsequently, the rare-earth-doped PrIZO, NdIZO, and TbIZO nanopowders were prepared with rare earth (Pr, Nd, Tb):In:Zn atomic ratio of 0.01:1.00:1.00. Thermogravimetric-differential scanning calorimeter (TG-DSC) was adopted to analyze the thermal decomposition, phase transformation, and crystallization behavior of the precursors. Phase structure and composition of both precursors and calcined powders were characterized by X-ray diffraction (XRD). The scanning electron microscope (SEM) and transmission electron microscope (TEM) were utilized to examine the micro-morphology and particle size distribution, while the elemental composition and distribution were verified by energy disperse spectroscopy (EDS) and Fourier transform infrared spectroscopy (FT-IR). The results demonstrate that, the rare earth doping effectively modulates the thermal behavior, crystallization, and microstructure of IZO powders. Uniform, the well-dispersed and high-sphericity doped IZO nanopowders are successfully fabricated, and the influencing mechanism of rare earth elements on the structural and microscopic properties of IZO precursors and calcined powders is clarified.

     

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