CN114686987B - 一种二维有机-无机杂化双钙钛矿半导体晶体及其制备方法和用途 - Google Patents
一种二维有机-无机杂化双钙钛矿半导体晶体及其制备方法和用途 Download PDFInfo
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Abstract
本发明涉及一种二维有机‑无机杂化双钙钛矿半导体晶体及其制备方法和用途。一种有机‑无机杂化双钙钛矿半导体晶体，所述的无机‑有机杂化半导体材料的化学式为(C6H5CH2NH3)4AgBiBr8。本发明制备了一种有机‑无机杂化双钙钛矿半导体晶体，本发明的有机‑无机杂化双钙钛矿半导体晶体制备成平面光电导探测器可实现对本征吸收光谱的高灵敏度探测。利用波长为405nm的激光照射该单晶晶体探测器件，测试其光电响应。当入射光的功率密度为50.9mW/cm2时，该晶体器件表现出明显的光电导效应，光电流和暗电流的比值可以达到1.8×103。该结果表明该材料用作光电导探测器件具有潜在的应用价值。
Description
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，具体涉及一种二维有机-无机杂化双钙钛矿半导体晶体及其制备方法和用途。
背景技术
近年来，以铅碘甲胺(CH3NH3PbI3)为代表的有机-无机杂化钙钛矿材料，具有诸多优异的光电物理性能，成为光电功能材料领域的研究热点。其中，体块有机-无机杂化钙钛矿半导体由于载流子迁移率高，载流子扩散距离长，以及可采用低成本的溶液法生长，在光电二极管(LED)，太阳能电池，光电探测器等光电器件中展现了巨大潜力。然而，稳定性较差以及铅元素的毒性等问题制约了这类三维杂化钙钛矿材料大规模的生产和应用。因此合成绿色、稳定的有机-无机杂化钙钛矿化合物是目前光电材料研究领域重要的研究课题。以铅卤素钙钛矿材料为骨架模型，采用异价离子取代的方法，如选择一价金属和三价金属离子取代Pb2+,构筑有机-无机杂化双钙钛矿化合物是一个设计新型绿色、稳定杂化钙钛矿材料的可行方案。与此同时，引入大尺寸芳香胺阳离子，利用降维策略，组装二维有机-无机杂化双钙钛矿，提高其稳定性，并且二维层状的结构具有独特的量子阱效应，可提高材料的激子结合能，促进光生电子和空穴的快速分离。
因此基于芳香胺构筑稳定性高和光电性能优异的有机-无机杂化双钙钛矿半导体材料，并基于其高质量单晶光电器件具有重要的理论和实际价值。
发明内容
本发明的第一个目的在于提供一种二维有机-无机杂化双钙钛矿半导体晶体。
本发明的第二个目的在于提供一种有机-无机杂化双钙钛矿半导体晶体的制备方法。
本发明的第三个目的在于提供一种有机-无机杂化双钙钛矿半导体晶体的用途。
本发明的技术方案如下：
方案一)
一种有机-无机杂化双钙钛矿半导体晶体，所述的无机-有机杂化半导体材料的化学式为(C6H5CH2NH3)4AgBiBr8。
进一步地，所述的有机-无机杂化双钙钛矿半导体晶体属于单斜晶系，空间群为P21/c。
进一步地，所述晶体的晶胞参数为： α＝90°，β＝90.052(3)°，γ＝90°，/>Z＝2。
方案二)
一种有机-无机杂化双钙钛矿半导体晶体的制备方法，包括以下步骤：
称取苄胺、Ag2O和Bi2O3并置于烧杯中，再向烧杯中加入HBr水溶液，加热到126～130℃并搅拌至得到黄色澄清溶液；
然后将得到的溶液密封放入55℃-60℃的烘箱中，以0.8～1(℃/天的速率冷却至室温，即得到所述的有机-无机杂化双钙钛矿半导体；
所述的苄胺、Ag2O和Bi2O3的摩尔比为(4～8)：(1～2)：1；
所述的Ag2O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)
一种有机-无机杂化双钙钛矿半导体的用途，所述的有机-无机杂化双钙钛矿半导体(C6H5CH2NH3)4AgBiBr8能应用在光电导探测器领域。
X射线单晶衍射的结果表明：该化合物的分子式为C28H40AgBiBr8N4，结构简式为(C6H5CH2NH3)4AgBiBr8。其中，C6H5CH2NH3代表苄铵离子。在室温下(C6H5CH2NH3)4AgBiBr8晶体属于单斜晶系，空间群为P21/c。该化合物的晶胞参数为α＝90°，β＝90.052(3)°，γ＝90°，Z＝2，单胞体积为/>
较之前的现有技术，本发明具有以下有益效果：本发明制备了一种有机-无机杂化双钙钛矿半导体晶体，本发明的有机-无机杂化双钙钛矿半导体晶体制备成平面光电导探测器可实现对本征吸收光谱的高灵敏度探测。利用波长为405nm的激光照射该单晶晶体探测器件，测试其光电响应。当入射光的功率密度为50.9mW/cm2时，该晶体器件表现出明显的光电导效应，光电流和暗电流的比值(Iph/Idark)可以达到1.8×103。该结果表明该材料用作光电导探测器件具有潜在的应用价值。
附图说明
图1是本发明中实施例2(C6H5CH2NH3)4AgBiBr8晶体的照片
图2是本发明中(C6H5CH2NH3)4AgBiBr8晶体的晶体结构堆积图
图3是本发明中(C6H5CH2NH3)4AgBiBr8的紫外可见吸收光谱
图4是本发明中(C6H5CH2NH3)4AgBiBr8晶体的光电导性能
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
制备有机-无机杂化双钙钛矿半导体晶体(C6H5CH2NH3)4AgBiBr8
采用降温结晶法合成晶体(C6H5CH2NH3)4AgBiBr8，化学反应式为
8C6H5CH2NH2+Ag2O+Bi2O3+8HBr→
2(C6H5CH2NH3)4AgBiBr8+4H2O
称取苄胺(2×10-3mol)、氧化银(0.5×10-3mol)、氧化铋(0.5×10-3mol)溶于10mL的氢溴酸(质量分数为48％)中，加热到126℃并搅拌至得到黄色澄清溶液。然后将得到的溶液自然冷却至室温，得到黄色片状微晶，过滤、烘干，即得到所述的有机-无机杂化双钙钛矿半导体晶体(C6H5CH2NH3)4AgBiBr8。
实施例2
有机-无机杂化双钙钛矿半导体晶体(C6H5CH2NH3)4AgBiBr8的制备
将苄胺(4×10-3mol)、氧化银(1×10-3mol)、氧化铋(1×10-3mol)溶于30mL的氢溴酸(质量分数为48％)中，加热搅拌到130℃并搅拌至得到黄色澄清溶液。将得到的溶液密封好置于60℃的烘箱中，设定降温速率1℃/天。待烘箱温度降到30℃时，溶液析出尺寸为8×4×1mm3的黄色片状晶体(如图1所示)，即(C6H5CH2NH3)4AgBiBr8晶体。
经X射线单晶衍射分析，本实施例制备的(C6H5CH2NH3)4AgBiBr8晶体室温下属于单斜晶系P21/c空间群，晶胞参数为 α＝90°，β＝90.052(3)°，γ＝90°，/>Z＝2。
从图2中可以看出，(C6H5CH2NH3)4AgBiBr8采用如下的结构：有机阳离子层(C6H5CH2NH3 +)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。(C6H5CH2NH3)4AgBiBr8中含有两种八面体：AgBr6和BiBr6八面体。AgBr6和BiBr6八面体有序排列，相互连接形成二维无机层。对于有机部分，C6H5CH2NH3 +的N-H与邻近八面体上的卤素阴离子Br-会形成N-H···Br氢键。
实施例3
将苄胺(4×10-3mol)、氧化银(0.5×10-3mol)、氧化铋(0.5×10-3mol)溶于30mL的氢溴酸(质量分数为47％)中，加热搅拌至到127℃并搅拌至得到黄色澄清溶液。将得到的溶液密封好置于55℃的烘箱中，设定降温速率1℃/天。待烘箱温度降到30℃时，溶液析出晶体。
将实施例2制得的有机-无机杂化双钙钛矿半导体晶体(C6H5CH2NH3)4AgBiBr8通过紫外可见吸收光谱对(C6H5CH2NH3)4AgBiBr8的光学吸收进行分析。如图3所示，(C6H5CH2NH3)4AgBiBr8的吸收截止边为538nm。根据Tauc公式可以推导出该化合物的光学带隙值为2.25eV。
基于(C6H5CH2NH3)4AgBiBr8单晶制成的平面电极采用405nm激光为激发光源研究了其光电导行为。图4显示了(C6H5CH2NH3)4AgBiBr8在黑暗中和光照下的电流-电压(I-V)曲线。结果表明，在10V偏压下，(C6H5CH2NH3)4AgBiBr8的暗电流(Idark)为2.1×10-13A，说明其单晶的结晶质量高，固有载流子密度低。当光照强度为50.9mW/cm2时，(C6H5CH2NH3)4AgBiBr8的光电流(Iph)急剧增加至3.8×10-10A，得到Iph/Idark的值为1.8×103。该结果不仅揭示了(C6H5CH2NH3)4AgBiBr8晶体的半导体性能，而且表明该材料能够用于制作光电导探测器件，表明材料在集成光电功能器件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 (2)
1.一种有机-无机杂化双钙钛矿半导体晶体的制备方法，其特征在于：包括以下步骤：
称取苄胺、Ag2O和Bi2O3并置于烧杯中，再向烧杯中加入HBr 水溶液，加热到126~130℃并搅拌至得到黄色澄清溶液；
然后将得到的溶液密封放入55℃-60℃的烘箱中，以0.8~1（℃/天的速率冷却至室温，即得到所述的有机-无机杂化双钙钛矿半导体；
所述的苄胺、Ag2O和Bi2O3的摩尔比为 (4~8)：(1~2)：1；
所述的Ag2O与HBr的摩尔比为1：(8~20)；
所述的无机-有机杂化半导体材料的化学式为(C6H5CH2NH3)4AgBiBr8；所述的有机-无机杂化双钙钛矿半导体晶体属于单斜晶系，空间群为 P21/c；所述晶体的晶胞参数为：a =8.0614(6) Å，b = 32.683(3) Å，c = 8.1092(7) Å，α = 90 °，β = 90.052(3) °，γ = 90°，V = 2136.5(3) Å3，Z = 2。
2.根据权利要求1所述的有机-无机杂化双钙钛矿半导体晶体的制备方法，其特征在于：所述的HBr水溶液中HBr的质量分数为47~48%。
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| CN107248538A (zh) * | 2017-05-25 | 2017-10-13 | 华中科技大学 | 一种双钙钛矿晶体的后处理方法及应用 |
| US20180290897A1 (en) * | 2015-09-02 | 2018-10-11 | Oxford University Innovation Limited | Double perovskite |
| CN109369725A (zh) * | 2018-09-20 | 2019-02-22 | 西安交通大学 | 一种无铅杂化二维双钙钛矿材料及制备方法 |
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| US20180290897A1 (en) * | 2015-09-02 | 2018-10-11 | Oxford University Innovation Limited | Double perovskite |
| CN107248538A (zh) * | 2017-05-25 | 2017-10-13 | 华中科技大学 | 一种双钙钛矿晶体的后处理方法及应用 |
| CN109369725A (zh) * | 2018-09-20 | 2019-02-22 | 西安交通大学 | 一种无铅杂化二维双钙钛矿材料及制备方法 |
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| Exploring Unprecedented Room-Temperature Ferroelectric of Two-Dimensional Metal Halide Double Perovskite with X-ray-Sensitive Merits;Wuqian Guo et al.;《RESEARCH ARTICLE》;20201231;第1-6页 * |
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