包覆铕配合物Eu(DBM)3phen的硅胶纳米荧光检测材料的制备

Preparation of Silica Nanomaterials Encapsulated with Europium Complex of Eu(DBM)3phen for Fluorescence Detection

以十六烷基三甲基溴化铵(CTAB)和一种短链氟碳阴离子表面活性剂(Capstone FS-66)作为双模板,通过四乙氧基硅烷(TEOS)和含氯官能团的硅烷偶联剂制备了含氯官能团的大孔径树枝状介孔二氧化硅纳米球(MSNs);利用EuCl3·6H2O、1,10-邻菲啰啉盐酸盐和二苯甲酰甲烷合成铕的配合物Eu(DBM)3phen,然后以MSNs为基质填充Eu(DBM)3phen。为了更好地将Eu(DBM)3phen嵌入到纳米球孔道内,对所制备的介孔纳米球的孔道表面进行聚乙烯亚胺(PEI)修饰;同时为了解决荧光配合物从孔道泄露的问题,在纳米球表面层层自组装吸附多层聚合物,然后包覆一层二氧化硅膜形成核-壳结构。最后将所制备的荧光纳米球与3-氨丙基三乙氧基硅烷反应,使其表面带有氨基,用来嫁接生物分子如抗体等。通过透射电子显微镜(TEM)、荧光光度计和傅里叶红外光谱仪(FTIR)等多种方法对最终合成的纳米球的结构和性能进行了表征。结果表明:本制备的荧光纳米球粒径约为230μm、荧光强度约为2800a.u,1543cm^-1处出现了氨基的弯曲振动峰。

Large bored,twig-like mesoporous silica nanosphenes(abbrv.MSNs)containing Cl-functional group were prepared through the reaction of tetraethoxysilane and a azotizing reagent,Cl-functional group containing silane,taking CTAB and a short-chained fluorocarbon anionic surfactant(Capstone FS-66)as dualtemplates.Fluorescent complex of Eu(DBM)3phen,which was synthesized with EuCl3·6H2O,1,10-phenanthroline hydrochloride and dibenzoylmenthane,was encased into the matrix MSNs,and the surface of bore channels of the MSNs were modified with polyethyleneimine to give a more effective embedding of Eu(DBM)3phen into the bore channels.Furthermore,multilayer polymers were adsorbed on the surface of the nanospheres layer by layer through self-assembly,and then a layer of silica film was encapsulated onto the surface of the nano-spheres to for core-shell structures.Finally,the fluorescent nanospheres were reacted with 3-aminopropyl-triethoxysilane to have amino groups attached on the surfuce,for conjugating with biomolecules,such as anitbodies.The structure and properties of the final product of the nanospheres prepared was characterized by TEM,fluorescence spectrophotometry,FTIR,showing that the fluorescent nanospheres have bore diameters of about 230nm,given fluorescence intensity of about 2800a.u.and bending vibration peak of amino group was observed at 1543cm^-1.