CN110054628A - 一种水稳定杂化铅碘钙钛矿材料及其应用 - Google Patents
一种水稳定杂化铅碘钙钛矿材料及其应用 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 47
- DXZHSXGZOSIEBM-UHFFFAOYSA-M iodolead Chemical compound [Pb]I DXZHSXGZOSIEBM-UHFFFAOYSA-M 0.000 title claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 12
- -1 2,2 bipyridine cations Chemical class 0.000 claims abstract description 8
- CTZCWZWQIAUFCB-UHFFFAOYSA-N 1-ethyl-2-(1-ethylpyridin-1-ium-2-yl)pyridin-1-ium Chemical compound CC[N+]1=CC=CC=C1C1=CC=CC=[N+]1CC CTZCWZWQIAUFCB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 239000013078 crystal Substances 0.000 claims description 5
- 150000002892 organic cations Chemical class 0.000 claims description 5
- 230000002708 enhancing effect Effects 0.000 claims description 4
- 230000002209 hydrophobic effect Effects 0.000 claims description 4
- 150000001449 anionic compounds Chemical class 0.000 claims description 2
- 229910001412 inorganic anion Inorganic materials 0.000 claims description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-M iodide Chemical compound [I-] XMBWDFGMSWQBCA-UHFFFAOYSA-M 0.000 claims description 2
- 229940006461 iodide ion Drugs 0.000 claims description 2
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 230000029936 alkylation Effects 0.000 abstract 1
- 238000005804 alkylation reaction Methods 0.000 abstract 1
- 238000011065 in-situ storage Methods 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical group N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 1
- IKUCKMMEQAYNPI-UHFFFAOYSA-N [Pb].CN.[I] Chemical compound [Pb].CN.[I] IKUCKMMEQAYNPI-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000001450 anions Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical group [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000035755 proliferation Effects 0.000 description 1
- ROSDSFDQCJNGOL-UHFFFAOYSA-N protonated dimethyl amine Natural products CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 1
- 230000005588 protonation Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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- C07D—HETEROCYCLIC COMPOUNDS
- C07D471/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00
- C07D471/12—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00 in which the condensed system contains three hetero rings
- C07D471/14—Ortho-condensed systems
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Abstract
本发明公开了一种有机‑无机杂化铅碘钙钛矿材料及其用途。所述的杂化铅碘钙钛矿结构式为(1,1'‑diethyl‑[2,2'‑bipyridine]‑1,1'‑diium)Pb3I8，该材料由双乙基化的2,2联吡啶阳离子和无机(Pb3I8)2–阴离子构成。有机组分由2,2联吡啶阳离子原位烷基化生成，无机部分(Pb3I8)可以看成是由三核簇(Pb3I14)通过共用六个Pb‑I键连接而形成的一维链，具有新颖的Geiser堆积符号3(1/2,–1/2)(1/2,1/2)。该杂化材料具有优异的水、光和热稳定性和光电转换性能，可作为一种光电探测器的备选材料。
Description
技术领域
本发明涉及无机-有机杂化铅碘钙钛矿领域，尤其涉及一种水稳定铅碘杂化钙钛矿材料(1,1'-diethyl-[2,2'-bipyridine]-1,1'-diium)Pb3I8与其光电转换应用。
背景技术
近年来电子信息产品迅速普及和推广，已成为个人日常生活中必不可少的一类工具；而光电器件在日常生产、生活所用电子产品，如笔记本电脑、智能手机、太阳能电池、相机中具有核心地位。随着电子产品的迭代升级，对光电器件和光电材料的需求不仅越来越大，而且要求也越来越多；因此探索新型的光电材料，增强其物化性能具有极其重要的现实意义。
光敏探测器是一种基于光电效应，在外界紫外光或可见光照射下，可以产生光生电子和空穴，进而产生光生电流的器件。它基于光电效应而工作，是半导体材料的重要应用之一；要求材料的带隙值必须小于等于入射光子的能量。
与传统纯无机或有机材料而言，有机-无机杂化钙钛矿材料集合了无机和有机材料各自的优点于一身，不但具有低廉的价格和优异的光电性能，而且具有容易成膜，可制备柔性器件的优势。在此领域，有机-无机杂化铅碘钙钛矿类材料，如甲胺铅碘由于具有合适的带隙吸收，高的载流子迁移率，宽的光响应范围以及低的激子结合能等引起了广泛的研究关注，在太阳能电池、光敏探测器等方面有了极大的研究进展。杂化铅碘钙钛矿具有类似于钙钛矿矿石的AMX3的分子式。其中，A为半径较大的阳离子，如甲胺、二甲胺阳离子，M为金属离子，X为卤素原子。结构中，二价金属离子M占据体心位置与6个相距最近的卤素阴离子形成MX6八面体；这些八面体通过共顶点连接形成三维框架结构；有机阳离子则填充在由八个八面体形成的空洞当中，形成完整的钙钛矿晶体结构。该类结构中A，M和X位置都有宽泛的选择度，容忍因子t处于0.81-1.11范围内，八面体因数处于0.44-0.90范围内。当t位于0.89-1.0范围之间时，钙钛矿晶体具有立方相结构，t值越小，对称度越低，会发生相变形成四方或斜方相晶系。杂化钙钛矿结构中，不仅有机阳离子的大小会影响容忍因子，而且外界温度也会影响容忍因子，温度变化可能会导致有机阳离子的无序取向或流动性改变，从而发生结构相变。
目前已经报道的杂化铅碘钙钛矿光敏材料大多基于质子化的有机胺为阳离子，此类材料最大的不足是对水、光和热不稳定；因此，合成稳定性增强的杂化铅碘光敏材料是这一领域亟待解决的关键问题。
本发明以疏水烷基化联吡啶分子构筑水稳定性增强的有机-无机杂化铅碘钙钛矿材料，该材料在300-600 nm范围内表现出较强的光学吸收能力，而且具有较高的光电响应系数，在光敏探测器件、光电转化和太阳能电池领域具有重要的应用前景。
发明内容
本发明的目的在于提供一种有机-无机杂化铅碘钙钛矿材料，该材料由强疏水的烷基化芳香族阳离子和新颖的无机(Pb3I8) 2–阴离子构成，该材料表现出增强的水、热和光稳定性，克服了传统有机胺类阳离子调控的铅碘钙钛矿材料具有的稳定性差的问题；因此具有稳定性强，光响应系数高，循环性好等优势。
本发明的技术方案包括以下内容：
1. 一种水稳定有机-无机杂化铅碘钙钛矿材料(1,1'-diethyl-[2,2'-bipyridine]-1,1'-diium)Pb3I8，该杂化物结晶于单斜晶系，P21/n空间群，单胞参数为a=7.83埃，b=22.90埃，c=18.30埃，α=90度，β=95.0度，γ=90度，材料单晶体的颜色为黄色，晶体结构特征为由烷基化的吡啶阳离子和无机(Pb3I8)2–阴离子通过分子间作用力堆积而成；有机阳离子为N-双烷基化的+2价2,2联吡啶阳离子；无机阴离子(Pb3I8)2–可以看成是由(Pb3I14)三核簇通过共用六个Pb-I键连接而形成的一维链，具有全新的Geiser堆积符号3(1/2, –1/2)(1/2, 1/2)；每个(Pb3I14)簇由三个共边连接的(PbI6)八面体形成，结构中每一个铅离子都是采取PbI6的八面体型配位模式；碘离子则采取端基或桥连的模式。
2. 如项1所述的水稳定有机-无机杂化铅碘钙钛矿材料的用途，其特征在于：该化合物具有优异的稳定性和光电转换性能，作为一种光电探测器的备选材料。
本发明的有益效果为该杂化铅基钙钛矿材料由疏水烷基化阳离子构筑而成，得到的材料含有结构新颖的无机铅碘阴离子，杂化材料不仅有优异的光电转换性能而且具有增强的水、热和光稳定性，可用于光敏器件的制作。
附图说明
图1为有机-无机杂化铅碘钙钛矿材料的分子结构图。
图2为有机-无机杂化铅碘钙钛矿材料分子中一维阴离子链结构图。
图3为有机-无机杂化铅碘钙钛矿材料的紫外可见吸收光谱图。在300-600 nm的范围内该材料表现出良好的光学吸收，带隙为2.1 eV。
图4为有机-无机杂化铅碘钙钛矿材料刚合成，100%湿度气氛内放置60天后，太阳光照射60天后的粉末衍射花样，均与单晶模拟衍射结果完全吻合，说明材料具有优异的稳定性。
图5为有机-无机杂化铅碘钙钛矿材料在黑暗和500 W氙灯照射下的I-V曲线。明显地，当施加可见光照射后，材料表现出增强的电流密度，材料的on/off比值接近2。
图6为有机-无机杂化铅碘钙钛矿材料的光电响应循环性效果图。材料表现出良好的光电响应循环性，在5个循环后，无明显衰减。
图7有机-无机杂化铅碘钙钛矿材料的光响应时间。该材料的响应和衰减时间分别为120 ms和300 ms。
具体实施方式
（1）(1,1'-diethyl-[2,2'-bipyridine]-1,1'-diium)Pb3I8的合成
将0.115 g PbI2和0.078 g 2,2联吡啶加入25 mL的聚四氟乙烯内胆中，加入1 mL HI和4 mL乙醇，然后将聚四氟乙烯内胆放入不锈钢反应釜中，旋紧后放在190 ℃烘箱加热。在此温度下恒温六天后，自然冷却至室温，得红色柱状晶体，即为目标铅碘杂化材料。
（2）水和光稳定性测试
将30毫克充分研磨的(1,1'-diethyl-[2,2'-bipyridine]-1,1'-diium)Pb3I8粉末放置于100%湿度气氛容器或太阳光照射下，60天后，收集样品直接进行粉末衍射表征。
（3）光电响应及循环性测试
将5毫克充分研磨的(1,1'-diethyl-[2,2'-bipyridine]-1,1'-diium)Pb3I8粉末分散在0.5毫升乙醇中，加入40微升Nafion溶液，超声处理三十分钟，将3.5微升分散液滴涂在叉指电极上，重复五次成膜，40摄氏度真空干燥四小时后分别在黑暗和500 W氙灯的照射下进行线性伏安扫描。
Claims (2)
1.一种水稳定有机-无机杂化铅碘钙钛矿材料(1,1'-diethyl-[2,2'-bipyridine]-1,1'-diium)Pb3I8，该材料结晶于单斜晶系，P21/n空间群，单胞参数为a=7.83埃，b=22.90埃，c=18.30埃，α=90度，β=95.0度，γ=90度，材料单晶体的颜色为黄色，晶体结构特征为由疏水的芳香杂环阳离子和无机(Pb3I8)2–阴离子通过分子间作用力堆积而成；有机阳离子为N-双烷基化的2,2联吡啶阳离子；无机阴离子(Pb3I8)2–可以看成是由(Pb3I14)三核簇通过共用六个Pb-I键连接形成的一维链，具有全新的Geiser堆积符号3(1/2, –1/2)(1/2, 1/2)；每个(Pb3I14)簇由三个共边连接的(PbI6)八面体形成，结构中每一个铅离子都是采取PbI6的八面体型配位模式；碘离子则采取端基或桥连的模式。
2.如项1所述的稳定性增强的有机-无机杂化铅碘钙钛矿材料的用途，其特征在于：该化合物具有优异的稳定性和光电转换性能，作为一种光电探测器的备选材料。
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| CN110552065A (zh) * | 2019-09-19 | 2019-12-10 | 华中科技大学 | 一种链状碘化物材料及其制备与应用 |
| CN110590647A (zh) * | 2019-10-10 | 2019-12-20 | 济南大学 | 一种水稳定锑碘基杂化钙钛矿及其合成与应用 |
| CN113979926A (zh) * | 2021-08-17 | 2022-01-28 | 中国计量大学 | 一种基于碘化铋和吡啶鎓离子的电荷转移盐类钙钛矿半导体材料 |
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2019
- 2019-03-25 CN CN201910225505.0A patent/CN110054628B/zh not_active Expired - Fee Related
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| GUANG-NING LIU ET AL.: ""A comparison study of aliphatic and aromatic structure directing agents influencing the crystal and electronic structures, and properties of iodoplumbate hybrids: water induced structure conversion and visible light photocatalytic properties"", 《DALTON TRANS.》 * |
| GUANG-NING LIU ET AL.: ""Constructing moisture-stable hybrid lead iodine semiconductors based on hydrogen-bond-free and dual-iodine strategies"", 《J. MATER. CHEM. C》 * |
| TANLAI YU ET AL.: ""Hydrogen bonds and steric effects induced structural modulation of three layered iodoplumbate hybrids from nonperovskite to perovskite structure"", 《DALTON TRANS.》 * |
| XIAN-HUA ZENG ET AL.: ""Polymeric Iodoplumbate Templated by Photochemically Active Coordination Cation [Ru(phen)3]2+: Structure and Properties of a Bimetallic Inorganic–organic Hybrid"", 《J CLUST SCI》 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110552065A (zh) * | 2019-09-19 | 2019-12-10 | 华中科技大学 | 一种链状碘化物材料及其制备与应用 |
| CN110552065B (zh) * | 2019-09-19 | 2020-11-24 | 华中科技大学 | 一种链状碘化物材料及其制备与应用 |
| CN110590647A (zh) * | 2019-10-10 | 2019-12-20 | 济南大学 | 一种水稳定锑碘基杂化钙钛矿及其合成与应用 |
| CN110590647B (zh) * | 2019-10-10 | 2022-09-20 | 济南大学 | 一种水稳定锑碘基杂化钙钛矿及其合成与应用 |
| CN113979926A (zh) * | 2021-08-17 | 2022-01-28 | 中国计量大学 | 一种基于碘化铋和吡啶鎓离子的电荷转移盐类钙钛矿半导体材料 |
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| CN110054628B (zh) | 2022-01-28 |
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