非线性光学PI/SiO_2纳米杂化材料的合成与表征

Synthesis and attribute of nonlinear optical PI/SiO_2 nanometer hybridization material

以含氟的二胺5,5’-(六氟异丙基)-二-(2-氨基苯酚)及二酐3,3’,4,4’-苯四甲酸二酐(BPDA)为单体。首先合成了经酰胺化的主链上带有活性羟基的含氟聚酰亚胺,再通过 Mitsunobu 反应将活性生色分子共价链接到聚酰亚胺的侧链骨架上,合成了二阶非线性光学(NLO)含氟聚酰亚胺,采用溶胶-凝胶(sol-gel)技术,并利用偶联剂 APTES 制备带有发色团的及含有硅氧烷端分子的聚酰胺酸,其中的 Si(OR)_3基经水解、缩合后,与 TEOS 在催化剂作用下反应,经杂化、凝胶后,得到光学透明的具有非线性光学的、热稳定性高的杂化材料。将制得的 NLO 含氟聚酰亚胺/SiO_2杂化材料,采用红外光谱(FT-IR)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X 射线衍射(XRD)、示差扫描量热法(DSC)和热重分析(TGA)性能测试装置对材料的结构、表面形貌、热性能进行了表征。

In this experiment,the fluorine-containing monomers 2,2-Bis (3-amino-4-hydroxyphenyl) hexafluoropropane (6FHP) and 3,3′,4,4′-Bisphenyltetracarboxylic (BPDA) were used.It is a first-step preparation of a preimided hydroxy-containing polyimide,followed by the covalent bonding of an active chromophore onto the backbone of the polyimide via the Mitsunobu reaction.The second-order nonlinear optical (NLO) containing fluorine polyimide was synthesized.Thence,sol-gel technique is adopted,utilizing 3-aminopropyltriethoxysilane (APTES) as a coupling agent,poly (amide acid),containing chromophore and alkoxysilane monomers,is synthesized.Si (OR_3) group is hydrolyzed and condensated.It reacts with TEOS in presence of catalyst,via hybridization,gelatinous.The hybrid material is obtained with optics transparent,nonlinear optical,high thermal stability.NLO fluorine-containing polyimides/silica hybrid material is characterized by the methods of FT-IR spectra,Scanning Electron Microscope (SEM),Transmission Electron Microscope (TEM),X-ray diffraction (XRD),Differential Scanning Calorimetry (DSC) and thermogravimetric analysis (TGA) measuring apparatus to get their surface structure,morphology,thermal performance.