利用溶胶-凝胶法制备了Zn2SiO4:Mn^2+粉末,探讨了体系pH值、热处理温度、煅烧气氛对材料结构和发光性能的影响。利用X射线衍射(XRD)、扫描电子显微镜(SEM)、光致发光(PL)谱等分析手段对Zn2SiO4:Mn2+粉末的结构、颗粒大小、形貌、发光性能进行了表征。结果表明:溶胶的pH值影响制备的粉体的结晶性和颗粒大小,当溶胶pH值为4.34时,体系水解缩聚反应充分,所得荧光粉的光致发光强度最强;煅烧气氛显著影响荧光粉的发光强度,前驱体在N2(90%)+H2(10%)的还原气氛下煅烧得到的发光粉发光强度最强;最佳热处理温度为900℃。
Owing to its properties of high-luminescent efficiency, chemical stability and wet-resistence, Zn2SiO4 exhibits more excellent performance than the sulfides as luminescent host material. Zn2SiO4: Mn^2+ (willemite) is an efficient phosphor for plasma display, cathodoluminescent and electroluminecent displays. Over the past few decades, researchers have studied intensely about factors influencing on the photoluminescent properties of Zn2SiO4: Mn^2+ , such as calcining temperatures, concentration of Mn^2+ , atmosphere of heat treatment, various preparation methods. However, the pH value of the Zn2SiO4: Mn^2+ precursor sol also plays an important role in its luminescent properties. Herein, we investigate the effects of pH value of the precursor sol, heating atmosphere (oxidizing, neutral protecting and reducing) and calcining temperature on the photoluminescent intensitv of Zn2 SiO4 : Mn^2+ phosphor powder. Zn2SiO4: Mn^2+ phosphors have been prepared via a sol-gel route. Different pH values of the sol resulted in different geling time and the sol with pH value lower than 3 could not be gelatinized. After pre-heating at 600 ℃, Zn2SiO4: Mn^2+ precursors were calcined in different atmosphere (air, N2 and mixture of 10% H2 + 90% N2 ) at heating temperature varing from 800 ℃ to 1 100 ℃. The structure of Zn2SiO4: Mn^2+ has been characterized by X-ray diffraction (XRD), which shows that all the phase of phosphors is with α-Zn2SiO4 phase. The phosphor prepared from the sol with pH of 4.34 has the best crystallinity. Scanning electron microscope (SEM) is used to measure the particle size of the Zn2SiO4: Mn^2+ phosphors and the mean size of the phosphor obtained from the sol with pH value of 4.34 is about 100 nm, larger than the size of the phosphors obtained from sols with pH values of 5.32 and 6.53. The results of photoluminescent (PL) spectra indicate that the PL intensity of the phosphor increases with increasing the pH value of precursor sol, and the ma