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北京航空航天大学, 材料物理与化学中心 北京,100083
收稿日期:2008-06-25,
修回日期:2008-10-24,
纸质出版日期:2008-11-20
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谢晶, 万辉, 张俊英, 丛亮, 张巍巍. 不同制备条件对Zn<sub>2</sub>SiO<sub>4</sub>:Mn<sup>2+</sup>粉末发光性能的影响[J]. 发光学报, 2008,29(6): 973-978
XIE Jing, WAN Hui, ZHANG Jun-ying, CONG Liang, ZHANG Wei-wei. Effect of Preparation Condition on the Luminescent Properties of Zn<sub>2</sub>SiO<sub>4</sub>:Mn<sup>2+</sup> Phosphors[J]. Chinese Journal of Luminescence, 2008,29(6): 973-978
谢晶, 万辉, 张俊英, 丛亮, 张巍巍. 不同制备条件对Zn<sub>2</sub>SiO<sub>4</sub>:Mn<sup>2+</sup>粉末发光性能的影响[J]. 发光学报, 2008,29(6): 973-978 DOI:
XIE Jing, WAN Hui, ZHANG Jun-ying, CONG Liang, ZHANG Wei-wei. Effect of Preparation Condition on the Luminescent Properties of Zn<sub>2</sub>SiO<sub>4</sub>:Mn<sup>2+</sup> Phosphors[J]. Chinese Journal of Luminescence, 2008,29(6): 973-978 DOI:
利用溶胶-凝胶法制备了Zn
2
SiO
4
: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Zn
2
SiO
4
:Mn
2+
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N
2
(90%)+H
2
(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 wetresistence
Zn
2
SiO
4
exhibitsmore excellent performance than the sulfides as luminescent hostmaterial. Zn
2
SiO
4
: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 photolumines-centproperties of Zn
2
SiO
4
:Mn
2+
such as calcining temperatures
concentration of Mn
2+
atmosphere of heat treatment
various preparationmethods.However
the pH value of the Zn
2
SiO
4
: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
neutralprotecting and reducing) and calcining temperature on the photo-luminescent intensity of Zn
2
SiO
4
:Mn
2+
phosphor powder.Zn
2
SiO
4
:Mn
2+
phosphors have been prepared via a solgel route.DifferentpH values of the sol resulted in differentgeling time and the sol with pH value lower than 3 could notbe gelatinized.After preheating at 600℃
Zn
2
SiO
4
:Mn
2+
precursorswere calcined in different atmosphere (air
N
2
and mixture of 10% H
2
+90% N
2
) atheating temperature varing from 800℃ to 1100℃.The structure of Zn
2
SiO
4
:Mn
2+
has been characterized by X-ray diffraction (XRD)
which shows thatall the phase of phosphors is with -Zn
2
SiO
4
phase.The phosphor prepared from the sol with pH of 4.34 has the best crystallinity.Scanning electronmicroscope (SEM) is used tomeasure the particle size of the Zn
2
SiO
4
:Mn
2+
phosphors and the mean size of the phosphor obtained from the solwith 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 increaseswith increasing the pH value ofprecursor sol
and themaximum was obtainedwhen the pH value of precursor sol is 4.34.Because the phosphor obtained from the sol with pH value of 4.34 has bestcrystallinity
and its particle size is larger
leading to smaller specific surface area.When the specific surface area is smaller
there are lower defects in the surface ofparticles and fewernonradiative transitions appear.Additionally
the hydrolysis and polyconden-sation reactions of the precursor solwith pH value of 4.34 have been carried throughly and properly
resulting in the well dispersion of the Mn ions.The emission intensity of Zn
2
SiO
4
:Mn
2+
phosphors calcined in themixture of nitrogen and hydrogen is stronger than those of the phosphors calcined in the other heating at mosphere.Reducing atmosphere could easily split Mn-Mn pair and produce large number of is olated Mn ions.With H
2
existing in the heating at mosphere
more Zn ions in cline to be volatilized and more Mn ionswould substitute for Zn ions.There fore
the PL intensity of Zn
2
SiO
4
:Mn
2+
phosphors is the strongestwhen the pH value of the precursor sol is 4.34 and the phosphors are calcined in the mixture of N
2
and H
2
at 900℃.
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