CN114958368B - 一种二维手性有机-无机杂化钙钛矿晶体及其制备方法和用途 - Google Patents

一种二维手性有机-无机杂化钙钛矿晶体及其制备方法和用途 Download PDF

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CN114958368B
CN114958368B CN202210657386.8A CN202210657386A CN114958368B CN 114958368 B CN114958368 B CN 114958368B CN 202210657386 A CN202210657386 A CN 202210657386A CN 114958368 B CN114958368 B CN 114958368B
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罗军华
官倩文
刘希涛
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Abstract

本发明涉及一种二维手性有机‑无机杂化钙钛矿晶体及其制备方法和用途。一种二维手性有机‑无机杂化钙钛矿晶体：化学式为(R)‑(BPEA)FAPbBr4·H2O和(S)‑(BPEA)FAPbBr4·H2O，分子式是C9H18Br5N3OPb；其中，S‑BPEA是(S)‑(‑)‑1‑(4‑溴苯基)乙胺，R‑BPEA是(R)‑(+)‑1‑(4‑溴苯基)乙胺,FA是甲脒。本发明的二维手性有机‑无机杂化钙钛矿晶体制备成的光学器件在激光照射下能产生蓝色左旋或右旋的圆偏振光。

Description

一种二维手性有机-无机杂化钙钛矿晶体及其制备方法和 用途
技术领域
本发明属于功能晶体材料领域中的人工晶体材料领域，具体涉及一种二维手性有机-无机杂化钙钛矿晶体及其制备方法和用途。
背景技术
圆偏振发光(CPL)在3D显示器、液晶显示器、数据存储和光通信设备中的潜在应用价值引起了极大的关注。传统上，CPL是由线性偏振片和四分之一波片产生的，这会造成光损失，进一步限制了CPL的发展。最近，二维手性有机-无机杂化钙钛矿晶体直接发射左旋和右旋CPL，有效降低光损失，在手性光学领域展现出巨大潜力。将多种手性阳离子引入卤化物钙钛矿构筑结构多样的二维手性有机-无机杂化钙钛矿晶体有助于实现多色的CPL。众所周知，红色、绿色和蓝色(RGB)是光的三基色，将这三种颜色以任意比例混合可以得到自然界的任何一种颜色。目前，二维手性有机-无机杂化钙钛矿晶体中的红色和绿色圆偏振光取得了重大进展。但是，蓝色CPL材料作为RGB的重要颜色之一，在二维手性有机-无机杂化钙钛矿晶体中很稀缺，限制了CPL显示器的发展。二维手性有机-无机杂化钙钛矿晶体具有结构多样性、化学稳定性和性能可调等优点。调整手性卤化物钙钛矿的结构来实现高效蓝色CPL是最常用和有效的方法。
因此基于结构多样、性能可调的手性有机-无机杂化钙钛矿材料构筑蓝色圆偏振光材料具有重要的理论和实际价值。
发明内容
本发明提供一种二维手性有机-无机杂化钙钛矿晶体及其制备方法和用途。本发明的二维手性有机-无机杂化钙钛矿晶体制备成的光学器件在激光照射下能产生蓝色左旋或右旋的圆偏振光。本发明的二维手性有机-无机杂化钙钛矿晶体制备成的光学器件在激光照射下能产生蓝色左旋或右旋的圆偏振光。
本发明的技术方案如下：
方案一)
一种二维手性有机-无机杂化钙钛矿晶体：化学式为(R)-(BPEA)FAPbBr4·H2O和(S)-(BPEA)FAPbBr4·H2O，分子式是C9H18Br5N3OPb；
其中，S-BPEA是(S)-(-)-1-(4-溴苯基)乙胺，R-BPEA是(R)-(+)-1-(4-溴苯基)乙胺,FA是甲脒。
一种二维手性有机-无机杂化钙钛矿晶体属于单斜晶系，空间群为P21。
一种二维手性有机-无机杂化钙钛矿晶体，所述的(R)-(BPEA)FAPbBr4·H2O晶胞参数为：α＝90°，β＝93.2930(10)°，γ＝90°，/>Z＝2；
所述的(S)-(BPEA)FAPbBr4·H2O晶胞参数为： α＝90°，β＝93.004(4)°，γ＝90°，/>Z＝2。
一种二维手性有机-无机杂化钙钛矿晶体的制备方法，包括以下步骤：
称取(R)-(+)-1-(4-溴苯基)乙胺或者(S)-(-)-1-(4-溴苯基)乙胺与Pb(Ac)2·3H2O和醋酸甲脒置于烧杯中，再向烧杯中加入HBr水溶液，加热到100～130℃并搅拌至得到黄色澄清溶液；
然后将得到的溶液密封并于室温下静置2小时以上，即得到所述的二维手性有机-无机杂化钙钛矿晶体；
所述的(R)-(+)-1-(4-溴苯基)乙胺或者(S)-(-)-1-(4-溴苯基)乙胺与Pb(Ac)2·3H2O和醋酸甲脒的摩尔比为1：3：2；
所述的Pb(Ac)2·3H2O与HBr的摩尔比为1：(8～20)。
进一步地，所述的HBr水溶液中HBr的质量分数为47～48％。
方案三)
一种二维手性有机-无机杂化钙钛矿晶体的用途，所述的手性有机-无机杂化钙钛矿晶体用于制备圆偏振发光器件，能应用在发光领域。
X射线单晶衍射的结果表明：所述的手性有机-无机杂化钙钛矿晶体用于制备圆偏振发光器件的分子式为C9H18Br5N3OPb，结构简式为(R)-(BPEA)FAPbBr4·H2O或(S)-(BPEA)FAPbBr4·H2O。其中，S-BPEA是(S)-(-)-1-(4-溴苯基)乙胺，R-BPEA是(R)-(+)-1-(4-溴苯基)乙胺,FA是甲脒)分子式是C9H18Br5N3OPb。在室温下(R)-(BPEA)FAPbBr4·H2O和(S)-(BPEA)FAPbBr4·H2O晶体属于单斜晶系，空间群为P21。所述晶体R构型的(R)-(BPEA)FAPbBr4·H2O晶胞参数为： α＝90°，β＝93.2930(10)°，γ＝90°，/>Z＝2。所述晶体S构型的(S)-(BPEA)FAPbBr4·H2O晶胞参数为：/> α＝90°，β＝93.004(4)°，γ＝90°，/> Z＝2。
较之前的现有技术，本发明具有以下有益效果：本发明制备了一种二维手性有机-无机杂化钙钛矿晶体，本发明的二维手性有机-无机杂化钙钛矿晶体可以用于制备能产生蓝色左旋或者右旋的圆偏振光的器件。利用波长为375nm的激发光照射该单晶晶体，测试其发光性能，当激发光照射该晶体时，该晶体发出明显的蓝色光。该结果表明本发明手性有机-无机杂化钙钛矿晶体用来制作蓝色圆偏振发光器件具有潜在的应用价值。
附图说明
图1是本发明实施例1制备的(R)-(BPEA)FAPbBr4·H2O晶体照片。
图2是本发明实施例2制备的(S)-(BPEA)FAPbBr4·H2O晶体照片。
图3是本发明的(R)-(BPEA)FAPbBr4·H2O晶体结构堆积图。
图4是本发明的(S)-(BPEA)FAPbBr4·H2O晶体结构堆积图。
图5是本发明的(R)-(BPEA)FAPbBr4·H2O晶体的紫外可见吸收光谱。
图6是本发明的(S)-(BPEA)FAPbBr4·H2O晶体的紫外可见吸收光谱。
图7是本发明的(R)-(BPEA)FAPbBr4·H2O和(S)-(BPEA)FAPbBr4·H2O晶体的吸收光谱和圆二色性光谱。
图8是本发明中的(R)-(BPEA)FAPbBr4·H2O和(S)-(BPEA)FAPbBr4·H2O晶体的圆偏振发光的不对称因子。
图9是本发明中的(R)-(BPEA)FAPbBr4·H2O和(S)-(BPEA)FAPbBr4·H2O晶体的圆偏振发光光谱。
具体实施方式
下面结合具体实施例对本发明进一步阐述
实施例1
一种二维手性有机-无机杂化钙钛矿晶体的制备方法，包括以下步骤：
称取(R)-(+)-1-(4-溴苯基)乙胺与Pb(Ac)2·3H2O和醋酸甲脒置于烧杯中，再向烧杯中加入HBr水溶液，加热到120℃并搅拌至得到黄色澄清溶液；
然后将得到的溶液密封并于室温下静置2小时以上，即得到所述的二维手性有机-无机杂化钙钛矿晶体；(如图1所示)。
所述的(R)-(+)-1-(4-溴苯基)乙胺与Pb(Ac)2·3H2O和醋酸甲脒的摩尔比为1：3：2；
所述的Pb(Ac)2·3H2O与HBr的摩尔比为1：8。
所述的HBr水溶液中HBr的质量分数为47％。
化学反应式为
R/S-BPEA+Pb(Ac)2·3H2O+FAAc+4HBr→
(R/S)-(BPEA)FAPbBr4·H2O+2H2O+3HAc
实施例2
一种二维手性有机-无机杂化钙钛矿晶体的制备方法，包括以下步骤：
称取(S)-(-)-1-(4-溴苯基)乙胺与Pb(Ac)2·3H2O和醋酸甲脒置于烧杯中，再向烧杯中加入HBr水溶液，加热到100℃并搅拌至得到黄色澄清溶液；
然后将得到的溶液密封并于室温下静置2小时以上，即得到所述的二维手性有机-无机杂化钙钛矿晶体；(如图2所示)。
所述的(S)-(-)-1-(4-溴苯基)乙胺与Pb(Ac)2·3H2O和醋酸甲脒的摩尔比为1：3：2；
所述的Pb(Ac)2·3H2O与HBr的摩尔比为1：20；
所述的HBr水溶液中HBr的质量分数为47％。
实施例3
一种二维手性有机-无机杂化钙钛矿晶体的制备方法，包括以下步骤：
称取(S)-(-)-1-(4-溴苯基)乙胺与Pb(Ac)2·3H2O和醋酸甲脒置于烧杯中，再向烧杯中加入HBr水溶液，加热到130℃并搅拌至得到黄色澄清溶液；
然后将得到的溶液密封并于室温下静置2小时以上，即得到所述的二维手性有机-无机杂化钙钛矿晶体；
所述的(S)-(-)-1-(4-溴苯基)乙胺与Pb(Ac)2·3H2O和醋酸甲脒的摩尔比为1：3：2；
所述的Pb(Ac)2·3H2O与HBr的摩尔比为1：10；
所述的HBr水溶液中HBr的质量分数为47％。
X射线单晶衍射的结果表明：上述实施例1-3均能制备分子式为C9H18Br5N3OPb的化合物，结构简式为(R)-(BPEA)FAPbBr4·H2O或(S)-(BPEA)FAPbBr4·H2O。其中，S-BPEA是(S)-(-)-1-(4-溴苯基)乙胺，R-BPEA是(R)-(+)-1-(4-溴苯基)乙胺,FA是甲脒。在室温下(R)-(BPEA)FAPbBr4·H2O和(S)-(BPEA)FAPbBr4·H2O晶体属于单斜晶系，空间群为P21。所述晶体R构型的(R)-(BPEA)FAPbBr4·H2O晶胞参数为： α＝90°，β＝93.2930(10)°，γ＝90°，/>Z＝2。所述晶体S构型的(S)-(BPEA)FAPbBr4·H2O晶胞参数为：/> α＝90°，β＝93.004(4)°，γ＝90°，/> Z＝2。
从图3、4中可以看出，(R)-(BPEA)FAPbBr4·H2O和(S)-(BPEA)FAPbBr4·H2O采用如下的结构：(R)-(BPEA)FAPbBr4·H2O和(S)-(BPEA)FAPbBr4·H2O均呈现出稀有的(110)方向的波浪形无机骨架。有机阳离子层((S)-(-)-1-(4-溴苯基)乙胺或者(R)-(+)-1-(4-溴苯基)乙胺,甲脒和H2O)和无机层交错堆积构成二维杂化钙钛矿结构，而且有机层部分和无机层部分构成天然的量子阱。
由于手性化合物R构型和S构型的化合物虽然在晶型、空间的排列方式、熔点、旋光度等物理性质有差异，但其对普通光吸收相同。将实施例1制得的手性有机-无机杂化钙钛矿晶体(R)-(BPEA)FAPbBr4·H2O通过紫外可见吸收光谱对(R)-(BPEA)FAPbBr4·H2O的光学吸收进行分析。如图5所示，(R)-(BPEA)FAPbBr4·H2O的吸收截止边为435nm。根据Tauc公式可以推导出该化合物的光学带隙值为2.85eV。如图6所示，(S)-(BPEA)FAPbBr4·H2O的吸收截止边为435nm。根据Tauc公式可以推导出该化合物的光学带隙值为2.89eV
由于手性化合物R构型和S构型的化合物虽然在晶型、空间的排列方式、熔点、旋光度等物理性质有差异，但其普通荧光性能相同。因此基于(R)-(BPEA)FAPbBr4·H2O晶体，在紫外光的激发下，测试其荧光光谱。结果表明，(R)-(BPEA)FAPbBr4·H2O具有405nm和427nm的蓝色发射峰。由于手性阳离子的引入，(R)-(BPEA)FAPbBr4·H2O和(S)-(BPEA)FAPbBr4·H2O选择性的发左旋光和右旋光。随后的CPL测试也证明了(R)-(BPEA)FAPbBr4·H2O和(S)-(BPEA)FAPbBr4·H2O，两者实现了稀有的蓝光圆偏振光，不对称因子高达±8.4×10-3，(R)-(BPEA)FAPbBr4·H2O选择性发右旋光，(S)-(BPEA)FAPbBr4·H2O选择性发左旋光。该结果不仅揭示了(R)-(BPEA)FAPbBr4·H2O和(S)-(BPEA)FAPbBr4·H2O晶体的半导体性能，而且表明该材料能够用于制作发光器件，表明材料在发光领域具有潜在的应用价值。
本发明不仅限于上述实施例，凡是依据本发明上述实施例所作出的替换和变更，都在本发明保护范围之内。

Claims (4)

1.一种二维手性有机-无机杂化钙钛矿晶体，其特征在于：所述的一种二维手性有机-无机杂化钙钛矿晶体的化学式为(R)-(BPEA)FAPbBr4·H2O或(S)-(BPEA)FAPbBr4·H2O，分子式是C9H18Br5N3OPb；
其中，S-BPEA是(S)-(-)-1-(4-溴苯基)乙胺，R-BPEA是(R)-(+)-1-(4-溴苯基)乙胺,FA是甲脒；
所述的二维手性有机-无机杂化钙钛矿晶体属于单斜晶系，空间群为 P21；
所述的(R)-(BPEA)FAPbBr4·H2O晶胞参数为：a = 5.8741(2) Å，b = 8.4349(3) Å，c =19.4900(6) Å，α = 90 °，β = 93.2930(10) °，γ = 90 °，V = 964.09(6) Å3，Z = 2；
所述的(S)-(BPEA)FAPbBr4·H2O晶胞参数为：a = 5.8906(7) Å，b = 8.4638(8) Å，c =19.515(2) Å，α = 90 °，β = 93.004(4) °，γ = 90 °，V = 971.63(18) Å3，Z = 2。
2.根据权利要求1所述的二维手性有机-无机杂化钙钛矿晶体的制备方法，其特征在于：包括以下步骤：
称取(R)-(+)-1-(4-溴苯基)乙胺或者(S)-(-)-1-(4-溴苯基)乙胺，与Pb(Ac)2·3H2O和醋酸甲脒一起置于烧杯中，再向烧杯中加入HBr 水溶液，加热到100~130℃并搅拌至得到黄色澄清溶液；
然后将得到的溶液密封并于室温下静置2小时以上，即得到所述的二维手性有机-无机杂化钙钛矿晶体；
所述的(R)-(+)-1-(4-溴苯基)乙胺或者(S)-(-)-1-(4-溴苯基)乙胺与Pb(Ac)2·3H2O和醋酸甲脒的摩尔比为 1：3：2；
所述的Pb(Ac)2·3H2O与HBr的摩尔比为1：(8~20)。
3.根据权利要求 2所述的二维手性有机-无机杂化钙钛矿晶体的制备方法，其特征在于：所述的HBr水溶液中HBr的质量分数为47~48%。
4.根据权利要求1所述的二维手性有机-无机杂化钙钛矿晶体的用途，其特点在于：所述的二维手性有机-无机杂化钙钛矿晶体用于制备圆偏振发光器件。
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