CN103887391B - 一种内含掺杂量子点的硫化锌薄膜交流电致发光器件及其制备方法 - Google Patents
一种内含掺杂量子点的硫化锌薄膜交流电致发光器件及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种薄膜交流电致发光器件及其制备方法,具体涉及一种内含掺杂半导体量子点的硫化锌薄膜交流电致发光器件及其制备方法。本发明的薄膜交流电致发光器件包括依次设置的ITO导电玻璃层(5)、第一绝缘层(4)、发光层(3)、第二绝缘层(2)、金属电极层(1)。所述发光层(3)为硫化锌溶胶与掺杂半导体量子点混合,采用硫化锌溶胶与掺杂半导体量子点混合制备的发光层(3)可以提高导电性能,有效增强掺杂半导体量子点的发光效率。同时在以硫化锌溶胶与掺杂半导体量子点混合薄膜为发光层(3)的薄膜电致发光器件制备中,控制发光层的厚度也变得相对容易。
Description
技术领域
本发明涉及一种薄膜交流电致发光器件及其制备方法,具体涉及一种内含掺杂半导体量子点的硫化锌薄膜交流电致发光器件及其制备方法。
背景技术
目前,薄膜交流电致发光器已经应用于高分辨的平板显示器。薄膜交流电致发光器件具有抗击穿能力强,寿命更长,低功率高亮度等优点。薄膜式电致发光显示器(TFEL)与液晶显示器(LCD)相比,具有无需背光源,发光强度高,响应速度快等优点;与阴极射线显示器(CRT)相比,具有能耗低,且发光效率高,视角广等优点;与等离子体显示器(PDP)相比,也具有造价低廉,使用安全,寿命长等优点。
TFEL器件要求制备的发光层致密度高、缺陷少以防止在高压下出现电击穿现象,影响发光器件的效率和使用寿命。传统的TFEL器件的发光层的上、下设置有绝缘层,绝缘层采用高介电常数的绝缘介质,从而使发光层有了上下绝缘层的保护,同时增加ZnS或ZnO等半导体材料作为电子产生或传输层,从而提高荧光粉的电激发效率。另外,麻省理工学院(MIT)的研究者成功研制了以硫化锌半导体层与掺杂量子点层交替结构为功能层的交流电致发光器件。但是,硫化锌半导体层与掺杂量子点层采用的是交替结构,工艺比较复杂,且无法实现对掺杂量子点的有效激发,从而难以实现掺杂量子点的最佳发光性能。而传统以ZnS:Mn为发光层的薄膜交流电致发光器件是通过真空沉积的方法实现的,该方法需要高真空,高纯度的原材料等严苛要求,无法实现广泛应用。
发明内容
本发明的目的是提供一种内含掺杂半导体量子点的硫化锌薄膜交流电致发光器件及其制备方法,器件发光层采用硫化锌和掺杂半导体量子点混合薄膜。该方法可以提高TFEL器件发光层的导电性能,提高载流子的密度,增强掺杂半导体量子点的激发效率,提高器件发光效率。同时工艺简单,控制发光层的厚度也变得相对容易。
本发明的一种薄膜交流电致发光器件,包括依次设置的ITO导电玻璃层、第一绝缘层、发光层、第二绝缘层和金属电极层,所述发光层为硫化锌溶胶凝胶与掺杂半导体量子点CdS:Mn/ZnS混合的薄膜。
所述的金属电极层的材料为金、铝或银中的一种。
所述的第一绝缘层和第二绝缘层的材料为Ta2O5、SiO2、Al2O3或TiO2中的一种。
本发明的一种薄膜交流电致发光器件的制备方法,包括以下几个步骤:
1.)在ITO导电玻璃上制备第一绝缘层;
2.)合成CdS核,然后在120℃吸附Mn,250℃分别注入S/ODE、ZnSt2/ODE,反应生成ZnS壳,得到CdS:Mn/ZnS掺杂半导体量子点;
3.)将转水后的油性掺杂半导体量子点放入硫化锌溶胶凝胶中,用旋涂成膜的方法在第一绝缘层上均匀成膜,然后在100℃~200℃惰性气体环境中退火处理,形成发光层薄膜;
4.)在发光层上制备第二绝缘层,最终形成薄膜交流电致发光器件。
所述的金属电极层的材料为金、铝或银中的一种。
所述的第一绝缘层和第二绝缘层的材料为Ta2O5、SiO2、Al2O3或TiO2中的一种。
在上述制备CdS:Mn/ZnS掺杂半导体量子点时,通过控制Mn的含量,使掺杂粒子Mn的发光强度与CdS的本征发光相当,可以直接制备出发出白光的CdS:Mn/ZnS掺杂半导体量子点。使用该量子点制备出的硫化锌(ZnS)与掺杂半导体量子点CdS:Mn/ZnS混合薄膜的TFEL器件可以实现白色发光。
相较于传统ACTFEL器件,本发明工艺简单,成本低,而且本发明的发光层是由掺杂半导体量子点与ZnS溶胶凝胶混合,从而实现液相制备掺杂半导体量子点与ZnS混合发光层。使得ZnS材料可以在高电场下产生丰富的电子,电子在电场的加速下高速撞击掺杂半导体量子点,从而有效激发掺杂半导体量子点,显著提高掺杂半导体量子点的激发效率,因此能显著提高器件的发光效率。但是ZnS溶胶凝胶并不是影响器件发光与否的关键,关键在掺杂半导体量子点,ZnS溶胶凝胶只起到提高器件发光效率的作用,因此ZnS溶胶凝胶与掺杂半导体量子点的用量比例关系可以在很大的范围内进行选择。
附图说明
图1为具体实施方式1中得到的CdS的吸收和荧光谱,其中虚线为吸收光谱,实线为荧光谱;
图2为具体实施方式1中得到的CdS:Mn/ZnS半导体量子点纳米材料的吸收和荧光谱,其中虚线为吸收光谱,实线为荧光谱;
图3为CdS:Mn/ZnS半导体量子点的透射电镜(TEM)图;
图4为薄膜交流电致发光器件的结构示意图;
图中:金属电极层1、第二绝缘层2、发光层3、第一绝缘层4、ITO导电玻璃层5、交流电6。
具体实施方式
实施例1
本器件的制备包括以下几个步骤:
(1)制备第一绝缘层
首先对ITO导电玻璃层5进行超声清洗,烘干。在ITO电极上通过电子束热蒸发的方法镀上Ta2O5绝缘层,即为第一绝缘层4。
(2)制备硫化锌溶胶凝胶
把醋酸锌(Zn(CH3COO)2 2H2O)溶液和乙二胺(En)在烧杯中搅拌均匀,加入少量盐酸。之后,再边搅拌边加入硫代乙酰胺。最后,加入少量盐酸,得到ZnS溶胶凝胶。
(3)制备掺杂半导体量子点CdS:Mn/ZnS
采用Growth-doping方法合成CdS:Mn/ZnS。首先在三颈烧瓶中Ar气环境下将Cd的前驱CdO和Oleic acid、ODE搅拌除气15min,230℃下注入S的前驱反应5min,提纯离心后得到CdS量子点。取一定量的CdS量子点、油胺和ODE于50ml的三颈烧瓶,除气后的混合物加热到120℃。在此温度下注入MnSt2/ODE反应30分钟。温度升至250℃稳定后,先后注入S/ODE、ZnSt2/ODE,反应30分钟形成ZnS壳层。降温到60℃以下,多次提纯并离心得到掺杂半导体量子点CdS:Mn/ZnS。
(4)掺杂半导体量子点CdS:Mn/ZnS水相转换
取上述制备的CdS:Mn/ZnS掺杂半导体纳米材料溶于少量CHCl3,加入巯基丙酸至溶液浑浊,将浑浊液超声2小时出现絮状沉淀物。用CHCl3反复提纯3次得到沉淀,加入少量去离子水和四甲基氢氧化铵至沉淀溶解。将水相CdS:Mn/ZnS溶于少量去离子水中。
(5)制备发光薄膜
然后将制备好的硫化锌溶胶凝胶与掺杂半导体量子点CdS:Mn/ZnS的混合溶液在Ta2O5绝缘层上旋涂成膜,形成发光层3,旋涂成膜后的玻璃片在氩气中100℃退火,膜厚控制在100nm。
(6)制备第二绝缘层
在发光层3上通过电子束蒸发的方法制备Ta2O5绝缘层,即为第二绝缘层2。
(7)制备金属电极层
在第二绝缘层2上镀上Al电极,形成金属电极层1后最终得到薄膜交流电致发光器件。
实施例2
本实施例与实施例1基本相同,不同之处在于:成膜后的玻璃片在氩气中150℃退火,膜厚控制在500nm。
实施例3
本实施例与实施例1基本相同,不同之处在于:成膜后的玻璃片在氩气中200℃退火,膜厚控制在1000nm。
取实施例1所得的CdS和CdS:Mn/ZnS半导体量子点纳米材料进行吸收和荧光谱试验得到图1和图2,从图1可以看出CdS的吸收峰和荧光发射峰明显,说明CdS核已形成,可用于进一步合成CdS:Mn/ZnS半导体量子点。图2,可以看出:CdS:Mn/ZnS半导体量子点的吸收和荧光峰明显,说明CdS:Mn/ZnS半导体量子点已经形成,可用于制备薄膜。
取实施例1所得的CdS:Mn/ZnS半导体量子点纳米材料进行透射电镜试验得到图3,从图3中可以看出:CdS:Mn/ZnS半导体量子点已经形成,且粒径均匀分布(平均直径为7nm),晶格明显。
Claims (6)
1.一种薄膜交流电致发光器件,包括依次设置的ITO导电玻璃层(5)、第一绝缘层(4)、发光层(3)、第二绝缘层(2)和金属电极层(1),其特征在于:所述发光层(3)为硫化锌溶胶与掺杂半导体量子点CdS:Mn/ZnS混合的薄膜。
2.根据权利要求1所述的薄膜交流电致发光器件,其特征在于:所述的金属电极层(1)的材料为金、铝或银。
3.根据权利要求1所述的薄膜交流电致发光器件,其特征在于:所述的第一绝缘层(4)和第二绝缘层(2)的材料为Ta2O5、SiO2、Al2O3或TiO2。
4.一种如权利要求1中所述的薄膜交流电致发光器件的制备方法,其特征在于:所述制备方法包括以下几个步骤:
1.)在ITO导电玻璃层(5)上制备第一绝缘层(4);
2.)合成CdS核,然后在120℃吸附Mn,250℃分别注入S/ODE、ZnSt2/ODE,反应生成ZnS壳,得到CdS:Mn/ZnS掺杂半导体量子点;
3.)将转水后的油性掺杂半导体量子点放入硫化锌溶胶凝胶中,用旋涂成膜的方法在第一绝缘层上均匀成膜,然后在100℃~200℃惰性气体环境中退火处理,得到发光层(3),发光层(3)的膜厚为100-1000nm;
4.)在发光层(3)上制备第二绝缘层(2);
5.)在第二绝缘层(2)上制备金属电极层(1),最终形成薄膜交流电致发光器件。
5.根据权利要求4所述的薄膜交流电致发光器件的制备方法,其特征在于:所述的金属电极层(1)的材料为金、铝或银。
6.根据权利要求4所述的薄膜交流电致发光器件的制备方法,其特征在于:所述的第一绝缘层(4)和第二绝缘层(2)的材料为Ta2O5、SiO2、Al2O3或TiO2。
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