摘要
近年来,由于荧光探针在化学传感、生物检测及光学元件等领域的广泛的需求,荧光纳米材料得到人们前所未有的重视。相比于传统的荧光染料,荧光纳米材料不仅具有较高的荧光强度和优越的光稳定性,而且具有纳米材料特有的量子效应、小尺寸效应等性质,从而可以弥补传统的荧光染料无法克服的缺陷,为化学、物理、医学和生物领域都带来新的发展机遇。目前研究最热、发展最快的当属半导体量子点和碳量子点两类荧光纳米材料。无机半导体量子点由于荧光强、粒径小、光稳定性好,因而倍受人们青睐,所以研究此类量子点的新型制备和表面修饰方法具有重要意义。但是,因为这类量子点含有Cd、Pb、Hg等重金属离子,毒性较大,发展不含毒重金属的新型荧光材料也是当前的发展趋势之一。碳点及有机物聚合物荧光纳米材料由于其较低的生物毒性和稳定的化学性质,已成为人们关注的焦点。本学位论文工作采用新颖的一步光化学合成法制备了高量子产率的水溶性CdTe(S)三元混晶结构的量子点,并通过一步光化学法制备了表面聚合物修饰的CdTe(S)量子点；通过一步溶剂热的方法制备了纯粹的聚合物荧光纳米材料,利用水热法改性炭黑获得了高量子产率的荧光碳纳米材料,并对这些荧光纳米材料的性质进行了系统表征。
本学位论文共分为五章。
第一章：简单介绍了纳米材料的概念,着重介绍了半导体量子点、碳量子点点等荧光纳米材料的发展背景、制备方法、表面修饰及在多个领域的应用。
第二章：通过一步光化学合成法制备了高量子产率的水溶性CdTe(S)量子点,该法只需将氯化镉溶液、新鲜制备的碲氢化钠溶液及巯基乙酸按照一定的比例混合,直接置于500W高压汞灯下照射25分钟,即可制得量子产率高达80%的量子点。所合成的量子点的平均粒径小,约为2.2nm,是一种Cd、S、Te三元混晶结构的量子点。这种一步光化学合成法操作简便快捷,适合大批量合成。
第三章：利用一步光化学合成法制备了聚合物修饰的CdTe(S)量子点,将量子点的合成与聚合物的包覆合为一步,半小时内即可制得量子产率≥74%的聚合物修饰的量子点。并且通过调节反应条件可以方便的改变量子点的荧光颜色,从而制得绿色、黄色、橙色、红色等不同颜色发射的CdTe(S)量子点。本章共分两节,分别为采用一步光化学合成法制备N-(3-二甲氨基丙基)甲基丙烯酰胺(DPMA)聚合物包覆的两性量子点和聚丙烯酸修饰的量子点。我们通过MTT(噻唑蓝)细胞实验和大肠杆菌实验证明聚合物修饰的量子点的生物毒性明显降低。另外,DPMA聚合物修饰的量子点对溶液pH值的响应非常灵敏,从而可以用来检测溶液的pH值。而通过HTB-95637膀胱癌细胞的细胞成像试验可知,丙烯酸修饰的量子点可以吸附在细胞膜上。
第四章：主要以三聚氰胺和二醛类化合物为起始单体,基于西弗碱反应,通过简单的一步溶剂热反应制备了具有强荧光的纯聚合物纳米颗粒。本章共分为两节,第一节主要利用三聚氰胺和乙二醛反应制备了一种发射强烈的近白色荧光的聚合物纳米材料,量子产率为22%。通过调节激发波长,可以改变纳米颗粒的发射光谱,从而发出白色,蓝色,绿色,黄色,橙色和红色等不同颜色的荧光。第二节主要利用三聚氰胺与戊二醛的聚合反应制备了另外一种聚合物纳米材料,可以发出很强的绿色荧光。
第五章：本章主要通过一种经济温和的水热合成法,利用商品化炭黑作为起始原料,乙二醇作为钝化剂,硝酸作为氧化剂,制备了高量子产率(QY=25%)的荧光碳点。此碳点的发射波长随激发波长的红移而不断红移,并发出蓝色、绿色、黄色、橙色、红色等不同颜色的荧光。碳点的纳米颗粒粒径较小,只有2-3nm,可以穿透植物细胞的细胞壁、细胞膜和核膜进入细胞核,从而可以用来特异性标记细胞核。
In recent years, photoluminescent nanomaterials have attracted great attentions due to their wide applications as fluorescent probes in chemical and biological sensors, and in optical elements. Compared with traditional fluorescent dyes, photoluminescent nanomaterials have not only strong fluorescence and good resistance to light bleaching, but also the unique advantages of nanomaterials, such as quantum effects and small size effects, so they can eliminate the shortcomings of traditional fluorescent dyes and bring new development opportunity for the fields including chemistry, physics, biology and medicine. At present, the studies of photoluminescent nanomaterials focus on semiconductor quantum dots and carbon nanodots. Semiconductor quantum dots are extremely popular for their strong fluorescence, small sizes and excellent photostability. Therefore, the research on novel synthetic methods and surface modification protocols of quantum dots has a vital significance. However, the heavy metal ions such as Cd, Pb and Hg in the inorganic quantum dots might be a source of toxicity, development of novel photoluminescent nanomaterials without heavy metals has become a new trend. Therefore, many researchers devote to the exploration of carbon nanodots and organic polymeric photoluminescent nanomaterials owing to their low toxicity and stable chemical property. In this dissertation, novel methods of synthesis, characterization and application of four kinds of photoluminescent nanomaterials were presented. Water soluble alloyed CdTe(S) quantum dots with high quantum yields and surface modified CdTe(S) quantum dots with polymers were successfully prepared via one-step photochemical route. Meanwhile, pure polymeric photoluminescent nanoparticles were synthesized by a single-step sol-thermal method. Carbon nanodots with high quantum yields were prepared by modifying carbon black in a hydrothermal method.
The dissertation consists of five chapters.
Chapter1:The concept of nanomaterials was introduced. The background of development, methods of synthesis, protocols of surface modification and application of nanomaterials were summarized briefly.
Chapter2:A successful synthesis of water soluble CdTe(S) quantum dots with high quantum yields via a mild photochemical route in one step with thioglycolic acid as the stabilizer and sulfur source was described in this chapter. The precursor solution of mixed cadmium chloride, freshly prepared sodium hydrogen telluride and thioglycolic acid was subjected directly to the UV irradiation using a500W high-pressure mercury lamp under the protection of N2. Alloyed CdTeS quantum dots with a smaller particle size (2.2nm) and a high photoluminescence quantum yield (up to80%at room temperature) were formed within25min. The proposed one-step photochemical synthesis is simple and efficient, might be a potential way for the large scale preparation of CdTe(S) quantum dots.
Chapter3:Facile one-step photochemical synthesis of surface modified CdTe(S) quantum dots with polymer was developed in this chapter. The grafting and polymerization of monomers was incorporated with the forming of nanocrystals. The modified CdTe(S) quantum dots with high photoluminescence quantum yield (>74%) were synthesized in30min. CdTe(S) quantum dots with colorful photoluminescence from green and yellow to orange and red can be prepared by adjusting the reaction condition. This chapter includes two sections. Quantum dots coated with N-[3-(Dimethylamino) propyl] methacrylamide (DPMA) polymer and polyacrylate were prepared through one-step photochemical methods. MTT assay and E coli assay reveal that surface modified quantum dots are less toxic than pristine quantum dots. Quantum dots modified with DPMA polymer show a sensitive response to pH, implying their application in the pH measurement. Quantum dots coated with polyacrylate were proved to attach to cell membranes of HTB-95637through cell imaging.
Chapter4:Pure polymeric nanoparticles with high photoluminescence were synthesized by reaction of melamine and dialdehyde based on Schiff base chemistry. This chapter includes two sections. In the first section, near white-light-emitting polymeric nanoparticles with photoluminescence quantum yield of22%were prepared via reaction of melamine and glyoxal. The polymeric nanoparticles show excitation-tunable emission color, that is, the fluorescence varied from white, green, yellow, to red when excitation wavelength shifted from300nm to530nm. The second section describes another polymeric nanomaterial with green photoluminescence through reaction of melamine and glutaraldehyde.
Chapter5:Carbon nanodots with photoluminescence quantum yield of25%were prepared via an economical and mild hydrothermal method using commercial carbon black as the carbon source, nitric acid as the oxidant and glycol as the surface passivation agent. Blue, green, yellow, orange and red fluorescence were observed with the increase of the excitation wavelengths. Carbon dots synthesized in this way could be endocytosed into cell nucleus through cell walls, cell membranes and nuclear membranes readily due to their smaller sizes (2～3nm) and could be used to stain cell nucleus.
引文
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