CN107311222B - CsPb2Br5纳米片的制备方法 - Google Patents
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Abstract
本发明涉及一种可调发光CsPb2Br5纳米片的制备方法及其产品和应用，其制备方法为在氮气保护下，将硬脂酸铯、十八稀和油酸混合，制备油酸铯溶液；另将溴化铅、十八稀、辛胺和油酸混合，加热搅拌，得到PbBr2前驱体溶液；再将油酸铯溶液加入到PbBr2前驱体溶液，混合搅拌后得到CsPb2Br5纳米片。通过调控制备PbBr2前躯体溶液的反应温度在100～140℃，得到不同尺寸的CsPb2Br5纳米片，且光致发光由蓝光逐渐变成绿光。所得CsPb2Br5纳米片可以制备发光二极管、太阳能电池或光电探测器，由本发明制备CsPb2Br5纳米片构造的高单色性绿光LEDs发光效率达到了34.49lm/W。
Description
技术领域
本发明属于纳米材料领域，涉及CsPb2Br5纳米片的制备方法，更涉及这种制备方法得到的产品和应用。
背景技术
无机钙钛矿纳米材料(CsPb2X5，X＝Cl，Br，I)是一种新型的功能材料，在发光二极管、太阳能电池、光电探测器等方面均具有特殊性能，广泛应用于光电器件领域。近几年，CsPb2X5 纳米材料吸引了大量研究人员的关注，特别是对其形貌及应用的研究。例如德国化学会的《应用化学国际版》(Angew.Chem.Int.Ed，2016,55,8328)报道了一种快速离子交换法，成功制备了大量高效发光的CsPb2Br5纳米片；美国化学会的《先进光学材料》(Adv.Opt.Mater，2017, 5,1600788)报道了一种高结晶和强稳定性的CsPb2Br5微米片。然而以上的报道都不涉及到对 CsPb2Br5纳米片形貌进行调控从而实现对其发光性质的调控，以及将其应用于绿光LEDs和光电探测。
发明内容
有鉴于此，本发明通过调控温度来实现对CsPb2Br5纳米片的形貌调控，并进一步利用其构造了高单色性绿光LEDs和稳定的光电探测器。本发明的目的之一在于提供一种可调发光的CsPb2Br5纳米片制备方法，目的之二是提供一种可调发光的CsPb2Br5纳米片，目的之三是提供一种利用这种CsPb2Br5纳米片制备的高单色性绿光LEDs和稳定的光电探测器。
为达到上述目的，本发明提供如下技术方案：
1.可调发光CsPb2Br5纳米片的制备方法，其制备方法步骤如下：
(1)氮气保护下，将硬脂酸铯、十八稀和油酸混合，加热并搅拌，得到油酸铯溶液；
(2)将溴化铅、十八稀、辛胺和油酸混合，加热并搅拌，得到PbBr2前驱体溶液；所述加热为加热至温度100～140℃；
(3)采用热注入法将油酸铯溶液加入到PbBr2前驱体溶液，两者混合搅拌3h，再提纯得到CsPb2Br5纳米片。
进一步，步骤(1)中所述硬脂酸铯物质的量的终浓度为1.5mol/L，十八稀和油酸体积比为20:1～2。
进一步，步骤(1)或步骤(2)中所述搅拌的时间为0.5h，步骤(1)中所述加热温度为140℃。
进一步，步骤(2)中所述溴化铅物质的量的终浓度为0.032mol/L，十八稀、辛胺和油酸体积比为15:1～2:1～2。
进一步，步骤(3)中油酸铯溶液和PbBr2前驱体溶液体积比为1:22～25。
进一步，所述提纯的方法是加入与粗产物等量的甲苯，8000r转速下离心5min，反复4～5 次。
2.由以上任一项所述的制备方法制备的CsPb2Br5纳米片，通过调控制备PbBr2前躯体溶液的反应温度在100～140℃，得到不同尺寸的CsPb2Br5纳米片，且光致发光由蓝光逐渐变成绿光。
进一步，100℃温度条件下制备的CsPb2Br5纳米片光致发光呈蓝光，120℃温度条件下制备的CsPb2Br5纳米片光致发光呈蓝绿光，140℃温度条件下制备的CsPb2Br5纳米片光致发光呈蓝光。
3.制备的CsPb2Br5纳米片在制备发光二极管、太阳能电池或光电探测器中的应用。
进一步，用CsPb2Br5纳米片制备高单色性绿光LEDs。
进一步，用CsPb2Br5纳米片制备光电探测器。
本发明的有益效果在于：1.本发明通过简单的调控温度实现对纳米片形貌的调控，从而使其具有可调的发光性质，在光电器件方面具有广泛的应用前景；2.利用本发明制备的 CsPb2Br5纳米片构造的高单色性绿光LEDs发光效率达到了34.49lm/W.3.利用本发明制备的 CsPb2Br5纳米片构造的光电探测器具有稳定的光响应。
附图说明
为了使本发明的目的、技术方案和有益效果更加清楚，本发明提供如下附图进行说明：
图1为不同温度下合成纳米片的扫描电镜和原子力显微镜图；
图2为CsPb2Br5纳米片Mapping图；
图3为实施例1-3所制备的CsPb2Br5纳米片的光学性质图，其中a是各纳米片的XRD图， b是CsPb2Br5纳米片和CsPbBr3量子点的晶体结构图，c是各纳米片的吸收和荧光图，d是各纳米片的寿命图；
图4为绿光LEDs测试结果；
图5为光电探测结果；
图6为光电探测器的电流-时间曲线；
图7为实施例1-3所制备的CsPb2Br5纳米片荧光颜色图。
具体实施方式
下面将结合附图，对本发明的优选实施例进行详细的描述。实施例中未注明具体条件的实验方法，通常按照常规条件或按照制造厂商所建议的条件。
实施例1 CsPb2Br5的制备
采用热注入方法制备CsPb2Br5纳米片，制备步骤为：
(1)通入氮气且保持机械磁力搅拌的环境下，将625mg硬脂酸铯、10ml十八稀和0.5ml 油酸混合，加热至140℃混合搅拌0.5h，得到油酸铯溶液；
(2)将100mg溴化铅、7.5ml十八稀、0.5ml辛胺和0.5ml油酸混合，加热到100℃并混合搅拌0.5h，得到PbBr2前驱体溶液；
(3)采用热注入法将0.375ml的油酸铯溶液加入到PbBr2前驱体溶液，两者混合搅拌3h，得到粗产物，因粗产物表面存在配体，不能直接使用，要将其进行提纯。提纯方法是加入与粗产物等量的甲苯，8000r转速下离心5min，反复进行4至5次，提纯得到CsPb2Br5纳米片。
实施例2 CsPb2Br5的制备
采用热注入方法制备CsPb2Br5纳米片，制备步骤为：
(1)通入氮气且保持机械磁力搅拌的环境下，将625mg硬脂酸铯、10ml十八稀和0.5ml 油酸混合，加热至140℃混合搅拌0.5h，得到油酸铯溶液；
(2)将100mg溴化铅、7.5ml十八稀、0.5ml辛胺和0.5ml油酸混合，加热到120℃并混合搅拌0.5h，得到PbBr2前驱体溶液；
(3)采用热注入法将0.375ml的油酸铯溶液加入到PbBr2前驱体溶液，两者混合搅拌3h，将粗产物提纯得到CsPb2Br5纳米片。
实施例3 CsPb2Br5的制备
采用热注入方法制备CsPb2Br5纳米片，制备步骤为：
(1)通入氮气且保持机械磁力搅拌的环境下，将625mg硬脂酸铯、10ml十八稀和0.5ml 油酸混合，加热至140℃混合搅拌0.5h，得到油酸铯溶液；
(2)将100mg溴化铅、7.5ml十八稀、0.5ml辛胺和0.5ml油酸混合，加热到140℃并混合搅拌1h，得到PbBr2前驱体溶液；
(3)采用热注入法将0.375ml的油酸铯溶液加入到PbBr2前驱体溶液，两者混合搅拌3h，将粗产物提纯得到CsPb2Br5纳米片。
将实施例1-3制备的CsPb2Br5纳米片分散于甲苯中保存。
图1为实施例1-3不同温度下制备的CsPb2Br5纳米片的扫描电镜和原子力显微镜图；由图1可知，纳米片尺寸在300nm至1um之间，多层纳米片的厚度在10nm至20nm之间；
图2为CsPb2Br5纳米片Mapping图；图3为不同温度下制备的CsPb2Br5纳米片的光学性质图，其中a是各纳米片的XRD图，b是各纳米片的晶格结构图，c是各纳米片的吸收和荧光图，d是各纳米片的寿命图；由图3可知XRD图表明合成的纳米片高度结晶，晶格结构表明在两层Br和Pb离子内有一层Cs离子。吸收和荧光图表面随着温度的升高，纳米片的吸收和荧光发生红移。寿命结果表明温度升高，寿命增加，140℃下合成的纳米片的平均寿命为9.25ns。
图7为实施例1-3不同温度下制备的CsPb2Br5纳米片的荧光照片图，由图7可知，通过调控制备PbBr2前躯体溶液的反应温度在100～140℃，不仅能得到不同尺寸的CsPb2Br5纳米片，且各纳米片的光致发光由蓝光逐渐变成绿光。随着温度的升高，纳米片尺寸逐渐减小，由1μm逐渐减小到300nm，PL发射峰发生红移，从蓝光(467nm)移至绿光(518nm)。100℃温度条件下制备的CsPb2Br5纳米片光致发光呈蓝光，120℃温度条件下制备的CsPb2Br5纳米片光致发光呈蓝光偏绿光，140℃温度条件下制备的CsPb2Br5纳米片光致发光呈绿光。
实施例4 构造高单色性绿光LEDs
在140℃下合成的CsPb2Br5纳米片能够发射窄带绿光，利用其构造高单色性绿光LEDs。采用的方法是用移液枪吸取5μL CsPb2Br5纳米片溶液滴在蓝光InGaN芯片上，并利用光谱仪 PR670测试其发光性质。通过多次涂覆CsPb2Br5纳米片，最终获得半高宽发射光谱峰值为538 nm，半高宽(FWHM)为18nm，色坐标是(0.250，0.690)的高单色性绿光，如图4所示，高单色性绿光LEDs发光效率达到了34.49lm/W.。
实施例5 构造光电探测器
制备的纳米片具有300nm至1μm的尺寸，利用其构造光电探测器，构造方法如下：
吸取20uL的100℃、120℃和140℃温度下制备的CsPb2Br5纳米片溶液分别滴在金叉指电极上，并利用Keithley 4200测试分别其性能，不同温度下制备的CsPb2Br5纳米片所构造的光电探测器都具有稳定的光响应，通过对比，100℃合成的CsPb2Br5纳米片构造的光电探测器上升、下降时间分别为0.426和0.422s，电流变化百分比达到了364％，优于其他温度下合成的纳米片构造的光电探测器，具有较好的性能，结果如图5，图6所示。
最后说明的是，以上优选实施例仅用以说明本发明的技术方案而非限制，尽管通过上述优选实施例已经对本发明进行了详细的描述，但本领域技术人员应当理解，可以在形式上和细节上对其作出各种各样的改变，而不偏离本发明权利要求书所限定的范围。
Claims (9)
1.可调发光CsPb2Br5纳米片的制备方法，其特征在于，制备方法步骤如下：
（1）氮气保护下，将硬脂酸铯、十八稀和油酸混合，加热并搅拌，得到油酸铯溶液；所述硬脂酸铯物质的量的终浓度为1.5mol/L，十八稀和油酸体积比为20:1~2；
（2）将溴化铅、十八稀、辛胺和油酸混合，加热并搅拌，得到PbBr2前驱体溶液；所述加热为加热至温度100~140℃；
（3）采用热注入法将油酸铯溶液加入步骤（2）的PbBr2前驱体溶液 ，两者混合搅拌3h，再提纯得到CsPb2Br5纳米片。
2.根据权利要求1所述的制备方法，其特征在于，步骤（1）或步骤（2）中所述搅拌的时间为0.5h-1h，步骤（1）中所述加热温度为140℃。
3.根据权利要求1所述的制备方法，其特征在于，步骤（2）中所述溴化铅物质的量的终浓度为0.032mol/L，十八稀、辛胺和油酸体积比为15:1~2:1~2，辛胺和油酸体积比1:1。
4.根据权利要求1所述的制备方法，其特征在于，步骤（3）中油酸铯溶液和PbBr2前驱体溶液体积比为1:22~25。
5.由权利要求1~4任一项所述的制备方法制备的CsPb2Br5纳米片，其特征在于，通过调控制备PbBr2前躯体溶液的反应温度在100~140℃，得到不同尺寸的CsPb2Br5纳米片，且光致发光由蓝光逐渐变成绿光。
6.根据权利要求5所述的CsPb2Br5纳米片，其特征在于，100℃温度条件下制备的CsPb2Br5纳米片光致发光呈蓝光，120℃温度条件下制备的CsPb2Br5纳米片光致发光呈蓝绿光，140℃温度条件下制备的CsPb2Br5纳米片光致发光呈绿光。
7.利用权利要求5所述的CsPb2Br5纳米片在制备发光二极管、太阳能电池或光电探测器中的应用。
8.权利要求7所述的应用，其特征在于，用CsPb2Br5纳米片制备高单色性绿光LEDs。
9.权利要求7所述的应用，其特征在于，用CsPb2Br5纳米片制备光电探测器。
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