CN107502337A - 单相磷光体量子点及其白光led芯片的制备方法 - Google Patents
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Abstract
本发明提供了一种单相磷光体量子点及其白光LED芯片的制备方法。本发明将包括一种单相磷光体量子点及其白光LED芯片的制备,包括制备掺杂铜的Cu:InP量子点核(d‑Core),包括制备ZnS屏障(Barrier),包括制备InP量子井(q‑Well),包括制备ZnS壳(Shell),形成Cu:InP/ZnS/InP/ZnS QDs结构单相磷光体量子点,包括将单相磷光体量子点涂覆在蓝光LED芯片上得到单相磷光体量子点白光LED芯片。本发明采用分步合成法、涂覆技术和紫外固化技术实现单相磷光体量子点白光LED芯片的制备。
Description
技术领域
本发明涉及光致发光二极管技术领域,特别涉及一种单相磷光体量子点及其白光LED芯片的制备方法。
背景技术
模拟黑体辐射将磷元素应用于白光LED灯的荧光粉上的做法已被认为是具有高能效的的传统光源替代方案。量子点是具有优异发光特性的半导体纳米材料,由于其高的量子产率、连续可调的荧光发射光谱、优异的摩尔吸收性能,被视为荧光粉的替代物,在照明技术领域有广阔的应用前景。
量子点光致发光二极管是一种以量子点为发光层,以蓝光LED为背光源的新型量子点LED发光器件,与传统光源相对比,量子点光致发光二极管具有更高的转化效率。
但是,目前P元素量子点的稳定性不高,量子产率不稳定。
发明内容
本发明的目的在于提供一种单相磷光体量子点及其白光LED芯片的制备方法。本发明提供的制备方法,方法简单,制备所得的量子点稳定性高,制备所得的光致发光芯片显示指数90以上。
为了实现上述发明目的,本发明提供以下技术方案:本发明提供了单相磷光体量子点及其白光LED芯片的制备方法,包括以下步骤:
(1)制备得到掺杂铜的Cu:InP量子点核(d-Core);
(2)在步骤(1)的Cu:InP量子点核的基础上制备ZnS屏障层(Barrier),得到Cu:InP/ZnS(d-Core/Barrier)结构量子点;
(3)在步骤(2)的Cu:InP/ZnS的基础上制备InP量子井(q-Well),得到Cu:InP/ZnS/InP(d-Core/Barrier/q-Well)结构量子点;
(4)在步骤(3)的Cu:InP/ZnS/InP的基础上制备ZnS壳(Shell),得到Cu:InP/ZnS/InP/ZnS QDs(d-Core/Barrier/q-Well/Shell)结构量子点;
(5)将制备得到的Cu:InP/ZnS/InP/ZnS QDs(d-Core/Barrier/q-Well/Shell)结构单相磷光体量子点涂覆在蓝光LED芯片上制得单相磷光体量子点白光LED芯片。
步骤(1),在单口瓶中加入0.2mmolP(TMS)3、2.4mmol辛胺和1.5mlODE,得到P前驱液;在单口瓶中加入0.2mlODE和0.02mmolCu(Ac)2,得到Cu前驱体;在50ml三口瓶中加入0.4mmolIn(Ac)3、1.2mmolMA和4mlODE;将三口瓶中的混合物在N2气条件下加热到188℃,注入制备好的磷前驱液;将反应温度保持在178℃,有利于InP量子点核充分生长;十分钟后将反应温度降到130℃,注入制备好的铜前驱液;再将反应温度升高到210℃,有利于在InP量子点核中掺杂Cu离子。
步骤(2),将在步骤(1)的反应降温到150℃,逐滴滴加0.08mmol/mlZn(st)2-ODE溶液和0.06mmol/ml S-TOP溶液;将反应温度升高到210℃,保持30分钟,有利于ZnS屏障层的生长;将反应温度降到150℃,再次逐滴滴加0.08mmol/mlZn(st)2-ODE溶液和0.06mmol/mlS-TOP溶液并再次升温到210℃保持30分钟;重复三遍此步骤后将反应温度降到室温,在反应物中加入正己烷和乙醇进行萃取,反复多次,除掉多余的反应物及副产品;加入丙酮、正己烷溶液沉淀、离心、干燥得到Cu:InP/ZnS core/Barrier量子点。
步骤(3),其特征在于,在50ml三口瓶中加入权利要求3中得到的量子点粉末和4mlODE溶液,在N2气环境下加热到100℃,逐滴滴加0.142mmol/ml P (TMS)3-ODE溶液和0.2ml辛胺溶液;迅速升温至120℃,保持5分钟,在降温至80℃,逐滴滴加3mmol/ml MA-ODE溶液和0.142mmol/ml In(MA)3–ODE溶液,将反应升温到178℃,保持30分钟,有利于InP量子井层的生长;将反应温度降为100℃,逐滴滴加0.09mmol/ml P (TMS)3-ODE溶液和0.3ml辛胺溶液;迅速升温至120℃,逐滴滴加3mmol/ml MA-ODE溶液和0.09mmol/ml In(MA)3–ODE溶液;将反应温度升高到220℃,保持30分钟,有利于InP量子井层生长。
步骤(4),将在步骤(3)的反应降温到150℃,逐滴滴加0.08mmol/mlZn(st)2-ODE溶液和0.06mmol/ml S-TOP溶液;
将反应温度升高到210℃,保持30分钟,有利于ZnS壳层的生长;
将反应温度降到150℃,再次逐滴滴加0.08mmol/mlZn(st)2-ODE溶液和0.06mmol/mlS-TOP溶液并再次升温到210℃保持30分钟;
重复三遍此步骤后将反应温度降到室温,在反应物中加入正己烷和乙醇进行萃取,反复多次,除掉多余的反应物及副产品,最终得到Cu:InP/ZnS/InP/ZnS QDs量子点。
步骤(5),沉淀量子点的方法得到Cu:InP/ZnS/InP/ZnS量子点粉末,将量子点粉末于三氯甲烷溶液按质量比1:10配置成混合溶液,加入0.05gPMMA,将配置好的混合溶液涂覆在蓝光芯片上,放置在在紫外灯下2小时,进行紫外固化,得到基于Cu:InP/ZnS/InP/ZnS量子点的白光LED芯片。
本发明的优点是:一种单相磷光体量子点及其白光LED芯片的制备方法。本发明将包括一种单相磷光体量子点及其白光LED芯片的制备,包括制备掺杂铜的Cu:InP量子点核(d-Core),包括制备ZnS屏障(Barrier),包括制备InP量子井(q-Well),包括制备ZnS壳(Shell),形成Cu:InP/ZnS/InP/ZnS QDs结构单相磷光体量子点,包括将单相磷光体量子点涂覆在蓝光LED芯片上得到单相磷光体量子点白光LED芯片。本发明采用分步合成法、涂覆技术和紫外固化技术实现单相磷光体量子点白光LED芯片的制备。
具体实施方式
本发明提供了单相磷光体量子点及其白光LED芯片的制备方法,包括以下步骤:
(1)制备得到掺杂铜的Cu:InP量子点核(d-Core)。
(2)在步骤(1)的Cu:InP量子点核的基础上制备ZnS屏障层(Barrier),得到Cu:InP/ZnS(d-Core/Barrier)结构量子点。
(3)在步骤(2)的Cu:InP/ZnS的基础上制备InP量子井(q-Well),得到Cu:InP/ZnS/InP(d-Core/Barrier/q-Well)结构量子点。
(4)在步骤(3)的Cu:InP/ZnS/InP的基础上制备ZnS壳(Shell),得到Cu:InP/ZnS/InP/ZnS QDs(d-Core/Barrier/q-Well/Shell)结构量子点。
(5)将制备得到的Cu:InP/ZnS/InP/ZnS QDs(d-Core/Barrier/q-Well/Shell)结构单相磷光体量子点涂覆在蓝光LED芯片上制得单相磷光体量子点白光LED芯片。
本发明中,制备方法步骤(1)具体实施步骤为,在单口瓶中加入0.2mmolP(TMS)3、2.4mmol辛胺和1.5mlODE,得到P前驱液。在单口瓶中加入0.2mlODE和0.02mmolCu(Ac)2,得到Cu前驱体。在50ml三口瓶中加入0.4mmolIn(Ac)3、1.2mmolMA和4mlODE。将三口瓶中的混合物在N2气条件下加热到188℃,注入制备好的磷前驱液。将反应温度保持在178℃,有利于InP量子点核充分生长。十分钟后将反应温度降到130℃,注入制备好的铜前驱液。再将反应温度升高到210℃,有利于在InP量子点核中掺杂Cu离子。
本发明中,制备方法步骤(2)具体实施步骤为,将在步骤(1)的反应降温到150℃,逐滴滴加0.08mmol/mlZn(st)2-ODE溶液和0.06mmol/ml S-TOP溶液。将反应温度升高到210℃,保持30分钟,有利于ZnS屏障层的生长。将反应温度降到150℃,再次逐滴滴加0.08mmol/mlZn(st)2-ODE溶液和0.06mmol/ml S-TOP溶液并再次升温到210℃保持30分钟。重复三遍此步骤后将反应温度降到室温。在反应物中加入正己烷和乙醇进行萃取,反复多次,除掉多余的反应物及副产品。加入丙酮、正己烷溶液沉淀、离心、干燥得到Cu:InP/ZnS core/Barrier量子点。
本发明中,制备方法步骤(3)具体实施步骤为,在50ml三口瓶中加入权利要求3中得到的量子点粉末和4mlODE溶液,在N2气环境下加热到100℃,逐滴滴加0.142mmol/ml P(TMS)3-ODE溶液和0.2ml辛胺溶液。迅速升温至120℃,保持5分钟,在降温至80℃。逐滴滴加3mmol/ml MA-ODE溶液和0.142mmol/ml In(MA)3–ODE溶液。将反应升温到178℃,保持30分钟,有利于InP量子井层的生长。将反应温度降为100℃,逐滴滴加0.09mmol/ml P (TMS)3-ODE溶液和0.3ml辛胺溶液。迅速升温至120℃,逐滴滴加3mmol/ml MA-ODE溶液和0.09mmol/ml In(MA)3–ODE溶液。将反应温度升高到220℃,保持30分钟,有利于InP量子井层生长。
本发明中,制备方法步骤(4)具体实施步骤为,采取与权利要求3中一致的方法,在权利要求4中得到的Cu:InP/ZnS/InP(d-Core/Barrier/qWell)量子点的表面包裹一层ZnS壳,修饰量子点表面缺陷,最终得到Cu:InP/ZnS/InP/ZnS QDs (d-Core/Barrier/qWell/Shell)量子点。
本发明中,制备方法步骤(5)具体实施步骤为,根据权利要求3中沉淀量子点的方法得到Cu:InP/ZnS/InP/ZnS (d-core/barrier/q-well/shell)量子点粉末。将量子点粉末于三氯甲烷溶液按质量比1:10配置成混合溶液。加入0.05gPMMA。将配置好的混合溶液涂覆在蓝光芯片上,放置在在紫外灯下2小时,进行紫外固化,得到基于Cu:InP/ZnS/InP/ZnS量子点的白光LED芯片。
Claims (6)
1.单相磷光体量子点及其白光LED芯片的制备方法,包括以下步骤:
(1)制备得到掺杂铜的Cu:InP量子点核;
(2)在步骤(1)的Cu:InP量子点核的基础上制备ZnS屏障层,得到Cu:InP/ZnS结构量子点;
(3)在步骤(2)的Cu:InP/ZnS的基础上制备InP量子井,得到Cu:InP/ZnS/InP结构量子点;
(4)在步骤(3)的Cu:InP/ZnS/InP的基础上制备ZnS壳,得到Cu:InP/ZnS/InP/ZnS QDs结构量子点;
(5)将制备得到的Cu:InP/ZnS/InP/ZnS QDs结构单相磷光体量子点涂覆在蓝光LED芯片上制得单相磷光体量子点白光LED芯片。
2.根据权利要求1所述的单相磷光体量子点及其白光LED芯片的制备方法,其特征在于:
步骤(1),在单口瓶中加入0.2mmolP(TMS)3、2.4mmol辛胺和1.5mlODE,得到P前驱液;
在单口瓶中加入0.2mlODE和0.02mmolCu(Ac)2,得到Cu前驱体;
在50ml三口瓶中加入0.4mmolIn(Ac)3、1.2mmolMA和4mlODE;将三口瓶中的混合物在N2气条件下加热到188℃,注入制备好的磷前驱液;
将反应温度保持在178℃,有利于InP量子点核充分生长;
十分钟后将反应温度降到130℃,注入制备好的铜前驱液;
再将反应温度升高到210℃,有利于在InP量子点核中掺杂Cu离子。
3.根据权利要求1所述的单相磷光体量子点及其白光LED芯片的制备方法,其特征在于:
步骤(2),将在步骤(1)的反应降温到150℃,逐滴滴加0.08mmol/mlZn(st)2-ODE溶液和0.06mmol/ml S-TOP溶液;
将反应温度升高到210℃,保持30分钟,有利于ZnS屏障层的生长;
将反应温度降到150℃,再次逐滴滴加0.08mmol/mlZn(st)2-ODE溶液和0.06mmol/ml S-TOP溶液并再次升温到210℃保持30分钟;
重复三遍此步骤后将反应温度降到室温,在反应物中加入正己烷和乙醇进行萃取,反复多次,除掉多余的反应物及副产品;
加入丙酮、正己烷溶液沉淀、离心、干燥得到Cu:InP/ZnS core/Barrier量子点。
4.根据权利要求1所述的单相磷光体量子点及其白光LED芯片的制备方法,其特征在于:
步骤(3),其特征在于,在50ml三口瓶中加入权利要求3中得到的量子点粉末和4mlODE溶液,在N2气环境下加热到100℃,逐滴滴加0.142mmol/ml P (TMS)3-ODE溶液和0.2ml辛胺溶液;
迅速升温至120℃,保持5分钟,在降温至80℃,逐滴滴加3mmol/ml MA-ODE溶液和0.142mmol/ml In(MA)3–ODE溶液,将反应升温到178℃,保持30分钟,有利于InP量子井层的生长;
将反应温度降为100℃,逐滴滴加0.09mmol/ml P (TMS)3-ODE溶液和0.3ml辛胺溶液;迅速升温至120℃,逐滴滴加3mmol/ml MA-ODE溶液和0.09mmol/ml In(MA)3–ODE溶液;将反应温度升高到220℃,保持30分钟,有利于InP量子井层生长。
5.根据权利要求1所述的单相磷光体量子点及其白光LED芯片的制备方法,其特征在于:
步骤(4),将在步骤(3)的反应降温到150℃,逐滴滴加0.08mmol/mlZn(st)2-ODE溶液和0.06mmol/ml S-TOP溶液;
将反应温度升高到210℃,保持30分钟,有利于ZnS壳层的生长;
将反应温度降到150℃,再次逐滴滴加0.08mmol/mlZn(st)2-ODE溶液和0.06mmol/ml S-TOP溶液并再次升温到210℃保持30分钟;
重复三遍此步骤后将反应温度降到室温,在反应物中加入正己烷和乙醇进行萃取,反复多次,除掉多余的反应物及副产品,最终得到Cu:InP/ZnS/InP/ZnS QDs量子点。
6.根据权利要求1或3所述的单相磷光体量子点及其白光LED芯片的制备方法,其特征在于:
步骤(5),沉淀量子点的方法得到Cu:InP/ZnS/InP/ZnS量子点粉末,将量子点粉末于三氯甲烷溶液按质量比1:10配置成混合溶液,加入0.05gPMMA,将配置好的混合溶液涂覆在蓝光芯片上,放置在在紫外灯下2小时,进行紫外固化,得到基于Cu:InP/ZnS/InP/ZnS量子点的白光LED芯片。
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