含络合/有机阳离子金属卤化物的合成及发光性质研究

近年来，零维有机-无机杂化金属卤化物因结构可调、光学性质优异等特性引起了科研工作者极大的研究兴趣。这类材料具有晶格软、量子限域效应强和电-声耦合强等特点，呈现出宽光谱发射、大斯托克斯位移、高发光量子产率等光学特征，在照明、显示以及闪烁体等领域展现出广阔的应用前景。最近的研究表明在高维金属卤化物体系中，有机阳离子在调控有机-无机杂化金属卤化物的光电和物理化学性质中起到关键作用。但在零维体系中，无机多面体仅与有限个数的阳离子产生较弱的相互作用（氢键、静电相互作用），阳离子对材料发光的影响较弱，且较软的有机阳离子骨架会带来更多的非辐射跃迁过程淬灭材料的发光，给研究金属卤化物材料的结构-发光性质之间的关系带来了难度。此外，因为阴阳离子键较弱的相互作用，有机阳离子对材料发光性能的改善有限。因此，本论文主要关注具有刚性结构的有机/络合阳离子对金属卤化物材料发光的影响以及对发光热稳定性、远程发光测温性能的改善。研究内容具体如下：

有机-无机杂化Sn基卤化物材料的多激子发射调控：以刚性有机化合物三乙烯二胺（DABCO）为基础，通过选择性的甲基化反应，合成了两种不同结构的有机阳离子（[C₈N₂H₁₈]²⁺，[C₇N₂H₁₆]²⁺），将它们与SnX₂（X=Br，I）共结晶得到了两种具有不同发光性质的零维有机-无机杂化Sn基金属卤化物材料。这两种材料具有不同强度的氢键作用，在强氢键体系中，氢键会诱导产生电荷转移激子，继而引起发光的激发依赖现象，在弱氢键体系中，则保持自陷态激子发光。该工作证明了阴阳离子间的相互作用可以改变材料的发光，这就为进一步改善材料的发光性能提供了一定的理论支持。

高发光热稳定性的Mn基金属卤化物的构筑：利用18-冠醚-6与Pb²⁺离子的尺寸匹配性以及18-冠醚-6自身的强螯合效应，构建了刚性络合阳离子[Pb(C₁₂O₆H₂₄)X]⁺（X = Cl，Br），并将其与MnX₂（X = Cl，Br）共结晶，得到了零维Mn基杂化金属卤化物材料[Pb(C₁₂O₆H₂₄)X]₂[Mn₂X₆]（X = Cl，Br）。其中，[Pb(C₁₂O₆H₂₄)Cl]₂[Mn₂Cl₆]在蓝光（445 nm）激发下，呈现出宽光谱的黄光发射，发光量子产率接近100%。发光机理研究表明黄光发射来源于Mn²⁺的d-d跃迁；图钉状络合阳离子[Pb(C₁₂O₆H₂₄)Cl]⁺中的Pb²⁺存在空配位点，对双核四面体构型阴离子[Mn₂Cl₆]^2-的形成和稳定起到了促进作用；络合阳离子[Pb(C₁₂O₆H₂₄)Cl]⁺自身的结构刚性也增强了材料的结构刚性，减少了分子热振动引起的非辐射跃迁，提高了杂化Mn基金属卤化物材料的发光热稳定性。

高效远程发光测温的Zn/Cd基金属卤化物的构筑：在上一章节的工作基础上，利用刚性络合阳离子[Pb(C₁₂O₆H₂₄)X]⁺（X = Cl，Br）合成了一系列具有不同多面体发光中心的金属卤化物材料。其中多面体的构型包括：双核四面体构型、金字塔构型、八面体构型等；这些材料的发光呈现出宽光谱发射，光谱涵盖了青光（505 nm）到红光（720 nm）区域，具有丰富的结构和发光可调性；此外，基于Zn、Cd两种金属合成的[Pb(C₁₂O₆H₂₄)Br]₂[M₂Br₆]（M = Zn，Cd）金属卤化物在较宽的温度范围（2∆T = 68/74 K）内发光寿命与温度成线性关系，具有潜在的远程发光测温应用，且线性测温范围远高于目前已报道的基于自陷态激子发光有机-无机杂化金属卤化物的测温范围（2∆T = 36 K）。研究发现，结构刚性的络合阳离子减缓了金属卤化物材料随温度升高而引起的声子辅助热辐射过程，拓宽了材料的线性变温区间，提高了远程发光测温性能。

Recently, zero-dimensional organic-inorganic hybrid metal halides (0D HMHs) have attracted great interest owing to their exceptional structural tunability and intriguing emission properties. They typically exhibit broad emissions with large Stokes shift and high photoluminescence quantum yields due to the strong quantum confinement, soft lattice, and strong electron-phonon coupling. These features endow them with wide applications in liquid crystal displays backlighting, illumination, and scintillators. Progresses in recent years have unraveled the important role of the organic cation in determining the optoelectronic and physicochemical properties of high-dimensional HMHs. In 0D HMHs, metal halide polyhedra have weak interactions with limit organic cations. Therefore, their luminescent properties have seldomly been affected by organic cations. Besides, the soft skeletons of organic cations make it difficult to investage the relationships of HMHs’ structure and properties. On the other hand, the enhancement of luminescent properties for HMHs is limited by the weak interactions between organic cations and metal halide polyhedra. The research contents are summarized as follows:

Luminescence regulation of Sn-based HMHs: Two kinds of organic cations based on DABCO were co-crystallized with SnX2 (X=Br, I) to obtain 0D HMHs: (C8N2H18)2SnX6 and (C7N2H16)2SnX6 (X=Br, I). These two types of hybrid tin bromides share similar structural features with different hydrogen bonding interactions between [SnBr6]4- anions and organic cations. Detailed structural analyses and Hirshfeld surface calculations confirm that the enhanced hydrogen bonding interactions are essential to obtain the multiple emissions in (C7N2H16)2SnBr6.

Construction of Mn-based HMHs with high photoluminescence thermal stability: a rigid complex cation was constructed by 18-crown-6 with strong chelating effect and Pb2+, and then co-crystallized with MnX2 (X = Cl, Br) to obtain a 0D Mn-based HMHs [Pb(C12O6H24)X]2[Mn2X6] (X = Cl, Br). Among them, [Pb(C12O6H24)Cl]2[Mn2Cl6] exhibits a broad yellow emission under the excitation of blue light (445 nm), and its photoluminescence quantum yield is near-unity. It was found that the Pb2+ in the pushpin complex cation [Pb(C12O6H24)Cl]+ has an empty coordination site, which plays an important role in promoting the formation and stabilization of the binuclear tetrahedral anion [Mn2Cl6]2-. Meanwhile, the rigidity of the complex cation [Pb(C12O6H24)Cl]+ also greatly enhances the structural rigidity of [Pb(C12O6H24)Cl]2[Mn2Cl6], reduces the non-radiative transitions, and improves the photoluminescence thermal stability.

Construction of HMHs with efficient remote thermometry: Based on complex cations [Pb(C12O6H24)X]+ (X = Cl, Br), a series of HMHs with different metal halide polyhedra were synthesized. The metal halide polyhedra include dimeric tetrahedron, square pyramid, octahedron and so on. The photoluminescence of these HMHs can be tuned from cyan (505 nm) to red (720 nm). More importantly, two kinds of [Pb(C12O6H24)X]2[M2X6] (X = Cl, Br; M = Zn) based on group 12 metals (Zn and Cd) exhibit broad cyan emissions. The lifetimes of [Pb(C12O6H24)Br]2[M2Br6] (M = Zn, Cd) show linear relationships with temperature (93-256 K), which could be used for remote optical thermometry. Compared to other metal halide materials, it is found that the rigidity of complex cations reduces the phonon-assisted nonradiative process and broadens the linear temperature range of Sn-based, Sb-based HMHs.

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