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 spectroscopy，FT-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.

关键词

稀土掺杂 / 氧化铟锌 / 纳米粉体 / 共沉淀

Key words

rare earth doping / indium zinc oxide / nanopowders / coprecipitation

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