摘要
本文合成了一系列含氮两性分子化合物、配位聚合物、导电聚合物和CdS纳米材料,并研究了某些两性分子和纳米材料自组装过程,具体研究内容如下：
(1)合成了一个新的二吡啶配体2,2,2,7-二溴-9,9-二(4-吡啶甲基)芴[DBPMF],在此基础上,得到了一个超分子化合物{[DBPMF H2]2+·2[ClO4]-}和三个配位聚合物,分别为[Cd4(DBPMF)6(SCN)8]n(1),[Cu2(DBPMF)2(CH3COO)5·2DMF]n(2)和[Cd(DBPMF)(acac)2]n(3)。在超分子{[DBPMF H2]2+·2[ClO4]-}中,存在N-H···O氢键、C-H···O潜在氢键、C-H···π作用力和π···π堆积作用力。这些作用力中,两种类型的N-H···O氢键连接两个[DBPMFH2]2+阳离子和两个[ClO4]-阴离子,形成了一维链。配合物1中,每个配体均和两个金属Cd2+离子相连,形成了一个既相互交叉,又具有螺旋链状结构的配位聚合物,这个聚合物在沿b轴方向最终形成了一个花形的三维孔洞结构；配合物2中,每个配体也和两个金属Cu2+离子相连,使得配合物单元之间两两相连,形成了以Cu(1)单元与Cu(2)单元分别相连的2种1D链结构；配合物3中,乙酰丙酮镉单元在二吡啶配体的连接下,形成了无限一维链状结构。
(2)研究了所合成的两性分子(E)-3-(4-二甲胺苯基)-1-(4-硝基苯基)丙酮(DMAPNPP)的溶液自组装过程。随着DMAPNPP饱和溶液的温度降低和溶剂挥发,DMAPNPP分子首先从晶核中向外自组装成较薄的带,这些卷曲的带在随后的自组装过程中,不仅充当直接的模板,而且被伸直。这个结果很好的表明,最终所得产物形貌的尺寸能够通过调节两性分子饱和溶液的自组装速度和温度来得到控制。这个过程也为相似两性分子的自组装过程开辟了一个很好的途径。
(3)合成了1-(N-丁基-1,8-萘酰亚胺基-4-yl)-3-(4-甲氧苯基)-5-苯基—吡唑啉(BMPP)分子化合物,并溶液自组装方法得到了BMPP分子的纳米纤维结构,进一步以BMPP分子的纳米纤维为模板通过苯胺原位化学氧化聚合法成功的合成了BMPP/聚苯胺核壳纳米纤维结构,利用乙醇溶液去除BMPP/聚苯胺核壳纳米纤维的BMPP核,得到了具有网状壁结构的聚苯胺纳米管,并研究了所合成BMPP/聚苯胺核壳纳米纤维的光学性能和电化学性能。
(4)采用化学氧化聚合法,以亚硒酸钠为氧化剂,制备了硒/聚吡咯纳米结构。EDS谱图结果显示,产物中有大量的硒,说明产物为硒/聚吡咯复合结构,研究了表面活性剂、反应温度等反应条件对硒/聚吡咯纳米结构的形貌和尺寸的影响。以十六烷基三甲基溴化铵为结构指导剂,在水热条件下,合成的硒/聚毗咯空心微管,微管的直径约为1μm,厚度约为30nm,长度为2-3μm,随着氧化剂亚硒酸钠浓度的增加,微管的厚度逐渐增加,且体系中游离的硒粒子的数量逐渐增多。在无表面活性剂时,产物为纳米颗粒的团聚体。表面活性剂在指导形成硒/聚吡咯空心微管的过程中起了重要的作用。实验研究了反应温度对产物的形貌,当反应温度为15°C时,产物为纳米颗粒。
(5)在十二硫醇的存在下通过硫脲和硝酸镉在乙二胺溶液中在180°C进行溶剂热反应制备出了由CdS纳米棒组成的束状纳米结构,其长度约为几十微米。CdS纳米棒直径和长度分别为50-70nm和数微米。实验发现：十二硫醇加入量的不同对束状CdS纳米结构的形成和CdS纳米棒的表面形貌有重要的影响。并研究了束状CdS结构的光致发光性质,当激发波长在405nm处时,在495nm(2.51eV)和522nm(2.38eV)处出现了两个荧光发射峰。
In this dissertation, a research has been made on synthesizing a supermolecular compound, three coordination polymers, microcosmic self-assembly process of the synthesized some amphiphilic molecules, and assembling nanomaterials. The main results are as follows:
(1) A new bis-pyridine ligand of{2,7-dibromo-9,9-(4-pyridyl-methyl) fluorene [DBPMF]} has been synthesized and characterized. By using this ligand, a supermolecular compound of{[DBPMF H2]2+·2[C1O4]-} and three coordination polymers have been obtained, including [Cd4(DBPMF)6(SCN)8]n(1),[Cu2(DBPMF)2(CH3COO)5·2DMF]n(2) and [Cd(DBPMF)(acac)2]n(3). In the{[DBPMF H2]2+·2[C1O4]-}, four kinds of supermocular interactions of N-H…O hydrogen bond, C-H…O potential hydrogen bond, C-H…π interaction and π…π packing interaction have been found. Among these supermolecular interactions, two types of N-H…O hydrogen bonds join two [DBPMFH2]2+cations and two [ClO4]-anions together to form an one-dimensional chain. In the complex1, each ligand coordinates with two Cd2+ions to construct a coordination polymer with intersectant and helix configuration, which finally presents a flower-like hollow structure along the b axis. In the complex2, each ligand also links with two metal ions of Cu2+which results in the interlinkage of two complex units. Ultimately, two kinds of1D chains have been found, one is based on Cu(1) unit and another is based on Cu(2) unit. In the complex3, each of acetylacetone cadmium(II) unit is combined by the bis-pyridine ligand of [DBPMF] to build an infinite1D chain.
(2) We present investigations on microcosmic self-assembly process of the synthesized amphiphilic molecules (DMAPNPP). During the temperature of the amphiphilic molecules' saturated solution drop and the solvent evaporation, the amphiphilic molecules were firstly assembled into thinner belt-like arms which extending from a core. Secondly, the curled belts did not only served as a template, but also were straight as the subsequently assembly. This conclusion can best illuminate why the size can be controlled by adjust amphiphilic molecules deposition velocity in their saturated solution. And which opens a new venue for conveniently adjusting the self assembly dimension of the similar amphiphilic molecules.
(3)1-(N-butyl-1,8-naphthalimide-4'-yl)-3-(4-methoxyl-phenyl)-5-phenyl-pyrazoline (BMPP)/polyaniline core-shell nanofibers were synthesized by in situ chemical oxidative polymerization of aniline using BMPP nanofibers as template. BMPP/polyaniline core-shell nanofibers exhibited uniform fibrilliar morphology and possessed BMPP nanofiber core and polyaniline shell, which existed in the form of nanoparticles. BMPP nanofibers were fabricated by the modified reprecipitation method with water as poor solvent. After BMPP/polyaniline core-shell nanofibers were washed with ethanol as good solvent to remove BMPP cores, polyaniline nanotubes with netlike structures were obtained. The molecular structures of BMPP/polyaniline nanocables were characterized by Fourier transform infrared spectroscopy and UV-vis spectroscopy, respectively. The core/shell structures of BMPP and polyaniline endowed BMPP/polyaniline core-shell nanofibers good electrochemical properties in comparison with BMPP nanofibers.
(4) Se/polypyrrole nanostructures were successfully synthesized using sodium selenite as initiator by chemical polymerization of pyrrole. EDS spectrum shows that the resulting products is consist of selenium, carbon, and nitrogen, which further conforms the Se/polypyrrole composite structure. The influences of synthetic parameters, such as surfactants, and reaction temperature, on the morphologies and sizes of Se/polypyrrole nanostructures were investigated. Se/polypyrrole hollow microtubes have been obtained using cetyltrimethylammonium bromide (CTAB) as surfactant under hydrothermal conditions. The hollow microtube is about800nm in diameter,30nm in the thickness, and the lengths of2-3um. With the concentration of sodium selenite increased, the thickness of Se/polypyrrole hollow microtubes is gradually increasing, and the separated selenium particles in the system are obtained. However, only Se/polypyrrole nanoparticles are obtained in the absence of CTAB, which shows that CTAB plays an important role in the formation of Se/polypyrrole hollow microtubes. When the reaction is taken at150℃, Se/polypyrrole nanoparticles are obtained.
(5) Bundle-like cadmium sulfide (CdS) nanostructures assembled by high-quality nanorods have been successfully synthesized on a large scale via a facile solvothermal route in a mixed solvent of ethylenediamine and dodecanethiol. The typical lengths of bundle-like CdS nanostructures are several tens of micrometers, and the diameters and lengths of CdS nanorods are about50-70nm and several micrometers, respectively. The influence of the concentration of dodecanethiol on the morphologies of CdS nanostructures has been investigated carefully. Photoluminescence spectra (PL) of CdS nanostructures reveal that the bundle-like CdS nanostructures exhibited two fluorescence emission peaks centered at495nm (2.51eV) and522nm (2.38eV) as the excitation wavelength is405nm.
引文
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