蓝光发光性能优异的氧化锌空心微球的制备及表征

doi:10.3724/SP.J.1077.2013.12168

摘要/Abstract

摘要：

本工作采用低温溶剂水浴热法, 以葡萄糖、柠檬酸盐为辅助剂, 首先制备了柠檬酸锌空心微球, 然后在空气气氛中500℃煅烧制得ZnO空心微球。应用XRD、TG-DSC、SEM、TEM、IR对产物的组成、结构以及形貌进行了研究, 研究发现该方法制备的前驱体为直径约为2 μm, 壁厚约为200 nm的空心微球。由前驱体煅烧后得到的ZnO空心微球由粒径为20~30 nm的纳米粒子组装成, 平均直径约为1 μm, 壁厚约为100 nm。此外还采用光致发光光谱仪(PL)对产物的光学性能进行了研究, 结果表明ZnO空心微球在激发波长为325 nm的条件下具有较好的蓝光发光性能, 发光峰位于469 nm处。

关键词: 氧化锌, 空心微球, 奥斯特瓦尔德熟化, 蓝光

Abstract:

With the assistance of glucose and citrate, hollow micro-spheres of zinc citrate were prepared through low-temperature hydrothermal route, and then hollow micro-spheres of ZnO were obtained by calcinating the precursor at 500℃ in air. The composition, structures and morphologies of products were characterized by XRD, TG-DSC, SEM, TEM and IR. It was investigated that the precursor hollow micro-spheres with average diameter of 2 μm and thickness of 200 nm were prepared by the hydrothermal route. ZnO hollow micro-spheres prepared by calcinating the precursor with average diameter of 1 μm and thickness of 100 nm were composed of nanoparticles with diameter of 20-30 nm. The room-temperature photoluminescence property of the sample was studied. Under excitation wavelength of 325 nm, the as-prepared ZnO hollow micro-spheres possess excellent properties of blue emission, locating at 469 nm.

Key words: ZnO, hollow micro-spheres, Ostwald ripening, blue emission

中图分类号:

TQ174

孙勇疆, 王莉, 蒋学会, 陈克正. 蓝光发光性能优异的氧化锌空心微球的制备及表征[J]. 无机材料学报, 2013, 28(2): 184-188.

SUN Yong-Jiang, WANG Li, JIANG Xue-Hui, CHEN Ke-Zheng. Preparation and Characterization of ZnO Hollow Micro-spheres with Excellent Property of Blue Emission[J]. Journal of Inorganic Materials, 2013, 28(2): 184-188.

图/表 7

图1 前驱体(a)及ZnO (b)的XRD图谱

Fig.1 XRD patterns of precursor (a) and ZnO (b)

图2 前驱体及ZnO空心微球的SEM照片

Fig. 2 SEM images of precursor and ZnO hollow micro-spheres (A) SEM images of zinc citrate precursor; (B) High-magnification SEM images of precursor; (C) SEM images of ZnO hollow micro-spheres; (D) High-magnification SEM images of ZnO hollow micro-spheres

图3 前驱体(a)及氧化锌(b)的红外光谱图

Fig. 3 IR spectra of precursor (a) and ZnO (b)

图4 前驱体DSC-TG曲线

Fig. 4 DSC-TG curves of precursor

图5 不同柠檬酸钠浓度获得前驱体产物的SEM照片

Fig. 5 SEM images of precursor prepared with different concentrations of trisodium citrate

图6 不同葡萄糖浓度制备的柠檬酸锌前驱物及ZnO空心微球的SEM照片

Fig. 6 SEM images of zinc citrate precursor and ZnO hollow micro-spheres prepared with different concentrations of glucose (A, B) 0 mol/L; (C, D) 0.15 mol/L; (E, F) 0.25 mol/L Condition: 0.05 mol/L Zn(NO3)2·6H2O; 0.05 mol/L C6H12N4; 0.05 mol/L trisoclium citrate

图7 ZnO空心微球的光致发光光谱

Fig. 7 PL spectrum of ZnO hollow micro-spheres

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