摘要
镧系配合物由于具有非常完美的发光行为,如发射谱带窄、色纯度高、荧光寿命长、量子产率高以及发射光谱范围覆盖可见和近红外光区等特点,在发光材料领域独树一帜。然而,纯的配合物往往具有光稳定性及热稳定性差的缺点,限制了其在很多领域的应用。将镧系配合物引入到基质中可以改善它们的稳定性及机械加工性能。根据基质材料的不同,杂化材料可分为无机基质、有机基质及无机/有机复合基质的杂化材料。这些杂化材料往往既具有主体基质良好的稳定性和机械加工性能,又具有镧系配合物独特的发光性能,在光学器件领域(LED照明、光纤维、光学放大器及激光等)及生命分析领域(细胞及组织成像、生命金属离子的追踪和检测等)等方面具有重要的应用价值。
本课题组一直致力于镧系配合物杂化发光材料的设计、组装及性能研究。为了发展镧系配合物杂化发光材料组装的新途径以及探讨材料主客体相互作用对其光物理性质和稳定性的影响,在课题组已有工作基础上,我们设计了一系列β-二酮配体镧系配合物,并通过次键力(氢键、静电作用或范德华力)或化学键合作用(共价接枝或配位作用)将其负载到无机基质、无机/有机复合基质或有机基质中,组装出有望应用于生物细胞成像、LED白光器件、光学放大器和气相荧光传感器等领域的新型镧系配合物杂化发光材料。研究表明,主体基质与客体配合物分子之间的相互作用对其光物理性质和稳定性均有明显的调制作用。取得的研究成果为新型镧系配合物发光材料的设计组装提供了新思路和新途径,对稀土功能材料的设计应用具有重要的理论意义及一定的应用价值。
本论文共分为四部分：
第一章：简要概述了镧系配合物杂化发光材料的研究进展。
第二章：镧系配合物＠无机基质杂化发光材料的组装。
以江苏盱眙产凹凸棒石粘土(Atta)和二氧化硅颗粒为基质,分别以3-氨基丙基-三乙氧基硅烷(APTES)和3-氨丙基-甲基-二乙氧基硅烷(ATMDES)为偶联剂,通过配体交换反应将镧系配合物共价接枝于无机基质表面,组装出镧系配合物＠粘土基质的杂化发光材料。通过对发光材料的组成及光物理性质分析,筛选出了最优化的组合Atta-APTES-cpa-Eu(DBM)3,该材料表现出更长的荧光寿命及更高的相对荧光强度。值得一提的是,通过材料的组装,获得了能够被可见光(398nm)激发的镧系杂化发光材料Atta-APTES-cpa-Eu(DBM)3。细胞成像和细胞毒性实验研究表明,该材料有望应用于医疗诊断。
将一系列带有不同末端基的酰胺型β-二酮配体镧系配合物共价接枝于溶胶凝胶体系中,制备出一系列发射绿色和红色荧光的镧系配合物溶胶凝胶杂化材料。光物理性研究表明,配体以苯环为末端基的杂化材料体系中存在更加有效的分子内能量传递效率、更长的荧光寿命以及更高的量子产率,推测一个稳定的共轭体系的存在为能量转移过程提供了有利的条件。
第三章：镧系配合物＠无机／有机复合基质杂化发光材料的组装。
无机基质的杂化材料具有良好的稳定性,但机械加工性能差,在无机基质中引入廉价的有机高分子基质,得到混合基质的杂化材料可以有效改善材料的机械加工性能。以凹凸棒石粘土为基质、3-氯丙基-三乙氧基硅烷为偶联剂,通过加入1-甲基咪唑形成离子液型凹凸棒石,进而通过离子交换反应引入β-二酮镧系配合物,组装出新型镧系配合物[C4mim][Ln(TTA)4]＠凹凸棒石的离子液型杂化材料,并通过加入高分子PMMA形成无机／有机复合基质的发光薄膜,进一步探讨主客体相互作用对杂化材料光物理性质的影响,为实现材料器件化应用提供理论依据。
通过溶胶凝胶法,将β-二酮配体的镧系配合物引入到Si02凝胶及Si02/有机聚合物的复合基质中。通过对杂化材料光物理性质的研究发现,有机聚合物的配位作用及主客体间相互作用对镧系配合物的能量传递产生了一定的影响。
第四章：镧系配合物＠有机基质杂化发光材料的组装。
以一个质子敏感的酰胺型β-二酮作为光敏化剂,通过添加固定含量的铽盐及铕盐以及高分子PVP形成一个杂化前驱体,并首次通过改变前驱体中碱的浓度以及激发波长,得到了一系列包含白光发射在内的全发光荧光薄膜材料。传统的多色发光材料的荧光调控是通过改变配体以及镧系离子的含量来实现的。这种薄膜对酸碱气体有荧光发射响应。由于其具有良好的稳定性、可循环性以及快响应性,有望应用于酸碱气体的荧光传感器。
The lanthanide complexes have excellent photoluminescent properties, such as sharp emission spectra for high color purity, broad emission bands covering the visible to near infrared region, a wide range of lifetimes, and high luminescence quantum efficiencies. However, the factors such as poor stabilities under high temperature or moisture conditions and low mechanical strength limit their practical use. In order to circumvent these drawbacks, lanthanide complexes have been incorporated into the matrices to constitute hybrid materials. The solid matrices could be divided into inorganic, organic and mixed matrices. The potential of these hybrid materials relies on exploiting the synergy between the intrinsic characteristics of host matrices (versatile shaping and patterning, excellent optical quality, high stabilities under high temperature or moisture conditions photosensitivity) and the luminescence features of trivalent lanthanide ions. These properties have attracted much attention for a wide variety of applications in the fields of lighting devices (light-emitting diodes (LED), optical fibers, optical amplifiers, lasers), and biomedical analysis (medical diagnosis and cell imaging).
Our group is dedicated to the design and assembly of functional lanthanide-based hybrid materials. In order to assemble novel lanthanide-based materials and elucidate the effect of interactions between host and guest on the photophysical behaviors and stabilities of the materials, we designed and synthesized a series of β-diketonated lanthanide complex based materials on the basic of the previous studies. The lanthanide complexes were incorporated into inorganic matrix, inorganic-organic mixed matrix or organic matrix by weak interactions (such as hydrogen bonding, van der Waals forces, or weak static effects) or strong interactions (such as covalent or coordinate bond). The assembly of these materials would be applied to cell imaging white-light light-emitting diodes (LED), optical amplifiers and vapoluminescent sensor. It is found that the host-guest interactions have distinctive modulation effects on the photophysical behaviors and stabilities of the hybrid materials. The research results of this dissertation might have theoretical and practical significance for the design of functional lanthanide-based hybrid materials.
The dissertation includes following four chapters:
Chapter1:A brief review of investigation progress of lanthanide-based hybrid materials was summarized.
Chapter2:Lanthanide complexes based inorganic matrices hybrid materials were assembled.
Attapulgite (so-called palygorskite) is a hydrated magnesium aluminium silicate present in nature as a fibrillar silicate clay mineral. We discuss the preparation and luminescence of a europium complex covalently attached to attapulgite and SiO2nanoparticals, grafting the europium complexes with two alkoxide structures, APTES and APMDES. The composites display more efficient emission and improved lifetime in comparison with the isolated complexes, due to interactions of the complexes with the matrixes. The most efficient emission of Atta-APTES-cpa-Eu(DBM)3among the composites results from the uniformly structured ternary europium complexes.
The development of sol-gel derived hybrid materials have been of widespread interest in materials science. Highly luminescent Eu(Ⅲ) and Tb(Ⅲ) complexes with a kind of amide-type β-diketone ligands, emitting in the green and red visible spectral regions upon UV irradiation, respectively, have been covalently bonded to the silica gels upon acidic hydrolysis and by using tetraethylorthosilicate as a silica source. The hybrids assembled by the ligand containing aromatic end group exhibited more effective intramolecular energy transfer, longer luminescence lifetimes and higher quantum efficiency. The above photoluminescence features indicated that the existence of a suitable conjugated system should allow a better energy transfer.
Chapter3:Lanthanide complexes based inorganic-organic mixed matrices hybrid materials were assembled.
Polymers are always incorporated into inorganic matrix to constitute inorganic-organic mixed matrix due to their several attractive features including mechanical strength, flexibility, and controllable cost. We assembled the ionic liquid-type lanthanide complexes onto attapulgite (atta). First, atta was anchored by1-propyl-3-methylimidazolium groups. Then we could prepare an immobilized analogue of the complex [C4mim][Ln(TTA)4] by an ion exchange route. The luminescence behaviors of the hybrid materials were investigated. The results of this work would have potential significance for the design and assembly of the luminescent lanthanide materials for high performance luminescence application.
We also embedded a new terbium β-diketonate complex into silica gel and SiO2/polymer matrices containing the long organic carbon chains and inorganic network (Si-O-Si) through sol-gel process to assemble the hybrid polymeric materials, Tb-L xerogel and Polymer-Tb-L xerogels. As the data suggested, the polymeric hybrid materials in comparison with the isolated complex possess higher unit mass luminescence intensities and exposure durability. The polymers containing carbonyl groups are supposed to conduce to the energy transfer progress and the hydrogen bonding between the host and guest may affect the ligand-to-metal energy transfer.
Chapter4:Lanthanide complexes based organic matrices hybrid materials were assembled.
The full-color photoluminescence materials including a white-light-emitting film were designed and fabricated facilely with a fixed-component Ln-based (Ln=Tb and Eu) polymer hybrid doped with an amide-type β-diketonated ligand. The tunable photoluminescence emissions were achieved by changing the amounts of the hydroxides of the polymer hybrid as well as excitation wavelength, rather than varying the relative concentrations of the lanthanide ions and ligand. The film with good stability, sensitivity, reversibility, and quick response triggered by base-acid vapor would be available as a vapoluminescent indicator.
引文
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