采用溶胶凝胶法与沉淀法相结合的方法,制备Eu^3+∶ZnO1-xSx-SiO2红色发光材料,通过DTA-TG、IR、XRD、TEM、EDS、激发和发射光谱等测试手段,研究材料的结构和发光性能。DTA-TG结果表明,样品在400℃以上,样品结构基本达到稳定状态;IR测试表明,样品中主要存在Si-O-Si键、Zn-S键、Si-O4基团,温度达到800℃时Zn-S键变强,且Si-O-Si三维网络结构的形成有利于Eu^3+的掺杂和发光;1000℃时Si-O4基团发生分裂现象,分为三个峰,同时部分ZnS被氧化为ZnO,该变化破坏了SiO2形成的大的三维网络结构,使Si-O-Si桥氧键断开,形成非桥氧键,此结构不利于Eu^3+的发光,说明800℃时样品的发光性能最好。XRD测试表明,样品属于晶态,主要以ZnO、ZnS、Zn2SiO4的形式存在。TEM和EDS结果表明,样品呈类球状,含有Zn、O、Si、Eu、S元素,其中S的含量约为2.40%(原子分数),说明S被有效地掺入样品中。激发和发射光谱测试表明,在612 nm检测波长下,其最佳激发波长为紫外光395 nm,最佳退火温度为800℃,Eu^3+最佳掺杂量为10%(原子分数),并证明Eu^3+∶ZnO1-xSx-SiO2材料发光强度约是Eu^3+∶ZnO-SiO2发光强度的6倍,说明S的引入可以有效的提高发光性能。
Eu^3+doped ZnO1- xSx- SiO2luminescent materials were synthesized by sol- gel method and precipitation method. The crystal structure and the luminescent properties of the samples were measured and characterized by using the method of DTA- TG,IR,XRD,TEM,EDS and excitation and emission spectra,respectively. DTA- TG shows the samples change into a stable structure when the temperature is above 400 ℃. IR results shows that the samples have formed the chemical bond of Si- O- Si,Zn- S and Si- O4groups. The chemical bond of Zn- S becomes stronger when the temperature is 800 ℃,and the Si- O- Si three- dimensional network structure is beneficial to the doping and luminescence of Eu^3+. Si- O4 group has changed into three sharp peaks when the temperature is 1000 ℃,and a part of ZnS was oxidized to ZnO. The change breaks the three dimensional network structure of SiO2. This phenomenon shows that the Si- O- Si bond was broken and formed non- bridge oxygen bond. This structure has not benefit for doping Eu^3+. The results show that the best temperature is 800 ℃. XRD shows that the samples are crystal material,and composed of ZnO,ZnS and Zn2SiO4. TEM and EDS show that the samples are composed of Zn,O,Si,Eu and S elements,and S content is about 2. 4%( at%),at the same time the samples have spherical morphology. The excitation and emission spectra show that the best excitation wavelength is 395 nm when the wavelength of the monitoring light is 612 nm,the best annealing temperature is 800 ℃,the optimum Eu^3+concentration is 10%,and luminescent intensity of ZnO1- xSx- SiO2Eu^3+is about six times of ZnO- SiO2Eu^3+. The results show that the emission intensity enhances with doping S.