苝四甲酸二酐的真空升华提纯及其光谱测试与分析  

Purification of PTCDA by Vacuum Sublimation and Spectral Test and Analysis

作　　者：张旭[1] 张杰[2] 闫兆文[2] 周星宇[3] 张福甲[2] 

机构地区：[1]兰州文理学院电子信息工程学院,甘肃兰州730000 [2]兰州大学物理科学与技术学院,甘肃兰州730000 [3]兰州大学应用有机化学国家重点实验室,甘肃兰州730000

出　　处：《光谱学与光谱分析》2015年第4期885-888,共4页Spectroscopy and Spectral Analysis

基　　金：甘肃省自然科学基金项目(145RJZA071);甘肃省教育厅科研项目(2013A-133)资助

摘　　要：纯度为9.75%的有机半导体材料苝四甲酸二酐(PTCDA),在其升华点进行了真空升华提纯,其纯度可达99.9%。利用质谱、红外光谱及X光电子能谱对这种高纯材料进行了测试并详细分析了其分子结构、化学键的形成、原子在晶格平衡位置的振动模式、电子的组态和原子的结合能的变化。由红外光谱分析得出,苝四甲酸二酐的分子结构是中央5个C构所组成的苝核基团及位于苝核两端的两个酸酐组成,它们主要以共价键结合。晶格上的C原子在其平衡位置主要以伸缩振动为主。其分子中有大量可以自由移动的π电子;分子间离域大π键的交叠决定了苝四甲酸二酐的导电性能。由XPS谱分析得出,高纯度的苝四甲酸二酐中有结合能不同的两种C原子,结合能分别为:285.3和288.7eV。它们对应于苝环及酸酐上的C原子。另外,有两种类型的O原子,即CO和C—O—C,其结合能分别为531.3和533.1eV。The organic semiconductor 3 ,4 ,9 ,10 perylenetetracarboxylic dianhydride （PTCDA） with the purity of 97.5% was purified by sublimation to 99.9% .The high‐purity PTCDA material was measured by mass spectra ,infrared spectrum and X‐ray photoelectron spectroscopy （XPS） .Detailed analysis revealed its molecular structure ,the forming of chemical bond ,the vibra‐tion modes of atoms in equilibrium lattice position ,electronic configuration and the shift of binding energy of atoms .Based on the infrared spectrum analysis ,the molecular structure of PTCDA is consisting of perylene core group with five Crings and two an‐hydrides located at both ends of perylene core ,which is mainly bonded with covalent bond .The stretching vibration of Catoms in the crystal lattice dominates in their equilibrium positions .The PTCDA molecules have a large number of π electrons which can move freely ;the intermolecular delocalized πbond overlap determines the conductivity of PTCDA .Based on XPS analysis ,it can be found that there exist two kinds of Catoms with different binding energy ：285.3 and 288.7 eV ,respectively ,correspond‐ing to the Catoms in the perylene ring and anhydride .In addition ,there are two kinds of O atoms ,i .e . CO and C—O—C, whose bonding energy is 531.3 and 533.1 eV ,respectively .

关 键 词：质谱 红外光谱 X光电子能谱 离域大π键 原子振动模式 结合能 

分 类 号：O621.1[理学—有机化学]