CN115074114A - 一种利用光调控钙钛矿荧光材料颜色变化的方法 - Google Patents
一种利用光调控钙钛矿荧光材料颜色变化的方法 Download PDFInfo
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Abstract
本发明公开了一种利用光调控钙钛矿荧光材料颜色变化的方法,其具体是将钙钛矿纳米晶体与卤代有机物混合,利用光线的分解作用和钙钛矿纳米材料的催化作用,使卤素有机物产生游离的卤素离子,并与离子晶体型的钙钛矿荧光材料发生离子交换,从而使钙钛矿材料产生荧光颜色的变化,同时,通过对所用光线的照射参数进行调整,可以达到精准、快速、宽色域地调控钙钛矿荧光颜色的目的。按本发明方法调控变色的钙钛矿荧光材料具有高的荧光量子产率、很窄的发射峰宽、很宽的变色范围,可实现多波长荧光发射的精准调控,在高密度光存储、防伪材料、紫外线检测等方面具有广阔的应用前景。
Description
技术领域
本发明属于纳米与功能材料领域,具体涉及一种利用光调控钙钛矿荧光材料颜色变化的方法。
背景技术
钙钛矿材料是近年来兴起的一种新型纳米材料,具有优良的光、电性能,在诸多领域如太阳能电池、发光二极管、光电检测器、激光器、荧光材料等有广阔的应用前景。钙钛矿材料是一种离子晶体,可以通过其晶格中所含的卤素离子(如氯离子、溴离子、碘离子)种类及数量的改变实现其荧光颜色的改变。因此,可利用离子交换,通过在钙钛矿发光体系中外加卤素离子,实现对钙钛矿材料荧光颜色的调控。
然而阴离子交换操作通常是将卤化物溶解在极性溶剂中,然后将其添加到纯化的钙钛矿溶液中来进行,这很容易破坏钙钛矿结构并减弱荧光。因此,在离子交换过程中,采用新材料与新方法生成卤化物源,取代手动操作繁琐和侵入性地添加带有极性溶液的卤化物,对从而提高钙钛荧光材料的稳定和变色操作的简便性与可控性具有重要意义。
发明内容
本发明的目的在于提供一种利用光调控钙钛矿荧光材料颜色变化的方法,其操作简单、成本相对低廉,发光量子效率高,可进行多波长荧光连续、精准调控,用途广泛。
为实现上述目的,本发明采用如下技术方案:
一种利用光调控钙钛矿荧光材料颜色变化的方法,其是将钙钛矿纳米晶体与卤代有机物混合均匀后,采用光线进行照射,通过控制照射功率、照射时间及照射次数,以实现所得复合物荧光颜色的变化。
其中,用钙钛矿纳米晶体与卤代有机物的摩尔比m的取值范围为0<m≤10000。
所述钙钛矿纳米晶体为全无机钙钛矿纳米晶体(如CsPbBr3、CsPbI3、CsPbBr1.2I1.8)或有机与无机杂化的钙钛矿纳米晶体(如CH3NH3PbBr3、CH3NH3PbI3、CH3NH3PbBr1.2I1.8),其荧光为绿色、蓝色、红色、无色或其混合色。
所述卤代有机物为氯代、溴代、碘代、氟代有机化合物,其具体可为二氯甲烷、二氯乙烷、二溴甲烷、二溴乙烷、碘仿、四氯化碳中的一种或几种。
所述光线来源于紫外光、可见光或红外光。
进一步的,所述材料具体可以为钙钛矿纳米晶体与卤代有机物的复合材料,也可以是在该复合材料中加入光固化树脂,并通过旋涂、打印或夹心的方法进一步制得的复合薄膜。
本发明钙钛矿-卤代有机物复合物的光控荧光变色范围为绿光到蓝光到紫光,或无色到蓝色到绿色,或从红光到橙光到黄光到绿光到青光到蓝光到紫光,即其可实现全色域多波长连续变化。
本发明的显著优点在于:
本发明采用非离子的卤化有机物作为卤素离子源,利用光线原位照射、定量生成卤素离子,从而达到光调控钙钛矿颜色变化的效果,可用于光学信息的写入。
与传统的光致变色材料相比,本发明方法避免了采用极性溶剂配制卤素离子,并具有更高的荧光量子产率、多波长连续调制的优点,因此在高密度光信息存储、高级防伪和紫外光检测方面具有广阔应用前景。
附图说明
图1为实施例3中绿色钙钛矿荧光复合材料经紫外光照射不同时间(1-20分钟)后的荧光变色情况(A)及荧光光谱变化(B)。
图2为实施例4中红色钙钛矿荧光复合材料经紫外光照射不同时间(1-26分钟)后的荧光变色情况(A)及荧光光谱变化(B)。
图3为实施例5中绿色钙钛矿荧光复合薄膜的制作和紫外光光学信息写入示意图(A)及在不同照射时间(0-15秒)下,在绿色钙钛矿荧光复合薄膜上光学写入的蓝色发射盘状图案(B)。
图4为实施例6中(A)以紫外激光束作为记录笔制作钙钛矿光数据存储器的过程示意图,(B)利用355 nm激光束扫描50次,在绿色钙钛矿荧光复合薄膜上绘制的蓝色荧光圆形图案(a)及通过光纤光谱仪测得的沿X轴(b)和Y轴(c)探测的最大发射波长,(C)在紫外激光扫描不同次数下在钙钛矿薄膜上获得的蓝色荧光圆形图案:(a)5次;(b)10次;(c)15次;(d)20次;(e)30次;(f)40次;(g)50次;(h)60次;(i)70次;(j)80次;(k)90次;(l)100次,(D)355nm激光辐照不同时间下重复制作(n=7)的荧光图案,(E)写入钙钛矿薄膜上的数字信息。
具体实施方式
为了使本发明所述的内容更加便于理解,下面结合具体实施方式对本发明所述的技术方案做进一步的说明,但是本发明不仅限于此。
实施例1
钙钛矿纳米晶体-二氯甲烷复合材料的制备:依次将0.4mmol PbBr2、0.4mmolCsBr和300微升油胺添加到10 mL N,N-二甲基甲酰胺溶液中,经搅拌形成透明前驱体溶液。然后在剧烈搅拌条件下按摩尔比0.0001将400微升前驱体溶液快速注入10毫升二氯甲烷中,得到的绿色荧光钙钛矿纳米晶体-二氯甲烷复合材料。
实施例2
采用0.16 mmol PbBr2、0.16 mmol CsBr、0.24 mmol PbI2、0.24 mmol PbI2替代实施例1中PbBr2和CsBr的使用,以制备摩尔比为0.0001的红色荧光钙钛矿纳米晶体-二氯甲烷复合材料。
实施例3
紫外光调控绿色荧光钙钛矿纳米晶体复合材料变色:用365 nm紫外光手电筒照射实施例1制得的绿色荧光钙钛矿纳米晶体-二氯甲烷复合材料1-20分钟,并实时监测其荧光变化,结果如图1所示。
由图1可见,复合材料的荧光颜色从开始的绿色逐渐过渡到青色、蓝色,最后为紫色,表明其获得了具有不同颜色的荧光钙钛矿纳米晶体复合材料(A);荧光发射光谱测量显示该复合材料的光谱峰宽比较窄,且变色后复合材料的荧光最大发射波长随着紫外线照射时间的延长逐渐紫移,即从518 nm逐渐减少到417 nm(B)。
实施例4
紫外光调控红色荧光钙钛矿纳米晶体复合材料变色:用365 nm紫外光手电筒照射实施例2制得的红色荧光钙钛矿纳米晶体-二氯甲烷复合材料1-26分钟,并实时监测其荧光变化,结果如图2所示。
由图2可见,其获得了经红色-橙色-黄色-绿色-青色-蓝色-紫色依次变化的荧光钙钛矿纳米晶体复合材料(A);荧光发射光谱测量显示该复合材料的光谱峰宽比较窄,且变色后的复合材料的荧光最大发射波长随着紫外线照射时间的延长逐渐紫移,即从635 nm逐渐减少到409 nm (B)。
实施例5
显微镜紫外光束调控绿色荧光钙钛矿纳米晶体复合材料薄膜变色:如图3中(A)所示,将实施例1制得的绿色荧光钙钛矿纳米晶体-二氯甲烷复合材料(PNCs)与紫外光固化树脂(UCR)混合均匀,取一滴于载玻片上,随后盖上盖玻片以形成绿色荧光钙钛矿纳米晶体复合薄膜,利用倒置荧光显微镜产生的紫外光束照射进行照射,以使所得绿色荧光钙钛矿纳米晶体复合薄膜产生荧光变色。如图3中(B)所示,不同照射时间(0-15s)产生从绿光到蓝色逐渐变化的圆形荧光图案。
实施例6
紫外激光光束调控绿色荧光钙钛矿纳米晶体复合材料薄膜变色:如图4中(A)所示,将实施例1制得的绿色荧光钙钛矿纳米晶体-二氯甲烷复合材料(PNCs)与紫外光固化树脂(UCR)混合均匀,取一滴于载玻片上,随后盖上盖玻片以形成绿色荧光钙钛矿纳米晶体复合薄膜,利用计算机控制的355nm紫外线激光束进行扫描,以使所得绿色荧光钙钛矿纳米晶体复合薄膜产生荧光变色。如图4中(B)所示,所产生的蓝色圆形光斑具有清晰的边界(a)和稳定、可重现的波长分布(b、c);如图4中(C)所示,根据紫外激光扫描次数不同(5-100次),绿色荧光钙钛矿纳米晶体复合薄膜产生从绿光到蓝色逐渐变化的圆形荧光图案。同时,如图4中(D)、(E)所示,经重复测试,计算机控制紫外激光束扫描所产生的特定颜色荧光图案具有良好的重现性。
本发明将钙钛矿荧光材料分散于含有卤素原子的有机溶液中,利用光线的分解作用和钙钛矿纳米材料的催化作用,使卤素有机溶剂产生游离的卤素离子,并与离子晶体型的钙钛矿荧光材料发生离子交换,从而使钙钛矿材料产生荧光颜色的变化,且通过对所用光线的照射参数进行调整,可以达到精准、快速、宽色域地调控钙钛矿荧光颜色的目的。因此,按本发明方法调控变色的钙钛矿荧光材料具有高的荧光量子产率、很窄的发射峰宽、很宽的变色范围,可实现多波长荧光发射的精准调控,在高密度光存储,防伪材料,紫外线检测等方面具有广阔的应用前景。
以上所述仅为本发明的较佳实施例,凡依本发明申请专利范围所做的均等变化与修饰,皆应属本发明的涵盖范围。
Claims (5)
1.一种利用光调控钙钛矿荧光材料颜色变化的方法,其特征在于:将钙钛矿纳米晶体与卤代有机物混合均匀后,采用光线进行照射,通过控制照射功率、照射时间及照射次数,以实现所得复合物荧光颜色的变化。
2.根据权利要求1所述的利用光调控钙钛矿荧光材料颜色变化的方法,其特征在于:所用钙钛矿纳米晶体与卤代有机物的摩尔比m的取值范围为0<m≤10000。
3.根据权利要求1或2所述的利用光调控钙钛矿荧光材料颜色变化的方法,其特征在于:所述钙钛矿纳米晶体为全无机钙钛矿纳米晶体或有机与无机杂化的钙钛矿纳米晶体,其荧光为绿色、蓝色、红色、无色或其混合色。
4.根据权利要求1所述的利用光调控钙钛矿荧光材料颜色变化的方法,其特征在于:所述光线来源于紫外光、可见光或红外光。
5.根据权利要求1所述的利用光调控钙钛矿荧光材料颜色变化的方法,其特征在于:所述复合物具体为钙钛矿纳米晶体与卤代有机物的复合材料,或在其复合材料中加入光固化树脂,并通过旋涂、打印或夹心的方法进一步制得的复合薄膜。
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