磁、发光羟基磷灰石的制备与表征
发布时间：2018-01-10 00:33
本文关键词：磁、发光羟基磷灰石的制备与表征 出处：《华北理工大学》2015年硕士论文 论文类型：学位论文
【摘要】：羟基磷灰石(简称HAp)赋予磁、发光性能后,具有跟踪标记和靶向定位功能,在疾病的诊断与分析、靶向药物载体以及细胞的分离和标识等领域展现出广阔的应用前景。采用共沉淀法、阴离子交换法和沉淀包覆法合成了磁、发光HAp,通过X射线衍射仪、场发射扫描电镜、透射电镜、荧光分光光度计和振动样品磁强计等测试手段表征了产物的相组成、显微结构、发光性能和磁性能,主要研究结果如下:以CaCl2和Na2HPO4为原料,CTAB为模板剂,在碱性条件下,采用共沉淀法,制备了分散性良好,粒径为40~100 nm的球形稀土掺杂HAp。在一定掺量内,Gd3+对Tb3+有敏化作用,使Gd3+和Tb3+共掺杂HAp的发光强度增强。随着Gd3+掺量的增加,Gd3+和Tb3+共掺杂HAp的磁化强度明显增强。以碳化法合成的Gd3+和Tb3+共掺杂碳酸钙为模板,在水浴环境中,采用阴离子交换法,获得球形Gd3+和Tb3+共掺杂HAp纳米颗粒。以直接沉淀法合成的粒径为1 um的Gd3+和Eu3+共掺杂碳酸钙为模板,在水热环境中,采用阴离子交换法制备出Gd3+和Eu3+共掺杂HAp微球,粒径为1~4 um。在波长为228 nm的光激发下,Gd3+和Tb3+共掺杂HAp在545 nm处具有较强的绿光发射。在波长为394 nm的光激发下,Gd3+和Eu3+共掺杂HAp的最强发射峰在592 nm处,属于Eu3+的5D0→7F1磁偶极跃迁。以水热法合成Fe3+和Co2+共掺杂HAp为磁性核,采用沉淀包覆法制备了具有核壳结构磁、发光HAp纳米颗粒,粒径为10~60 nm。在波长为352、371和448nm的光激发下,在545 nm处呈现绿色荧光。随着Tb3+掺量的增加,具有核壳结构磁、发光HAp纳米颗粒的发光强度增强,当Tb3+掺量为8 mol%时,达到最大值,继续增加Tb3+掺量,由于发生浓度淬灭,发光强度降低。具有核壳结构磁、发光HAp纳米颗粒具有顺磁性,随着包覆次数的增加,产物的磁化强度降低。
[Abstract]:Hydroxyapatite (Hapatite) is endowed with magnetic and luminescent properties, with tracking and targeting functions in the diagnosis and analysis of diseases. Magnetic and luminescent HAps were synthesized by coprecipitation, anion exchange and precipitation coating methods, and HAps were synthesized by X-ray diffractometer. The phase composition, microstructure, luminescence and magnetic properties of the products were characterized by field emission scanning electron microscopy, transmission electron microscopy, fluorescence spectrophotometer and vibrating sample magnetometer. The main results are as follows: using CaCl2 and Na2HPO4 as raw materials, CTAB was prepared by coprecipitation under alkaline conditions. The spherical rare earth doped HAps with a particle size of 40 ~ 100nm can sensitize Tb3 with a certain amount of Gd3. The luminescence intensity of HAp co-doped with Gd3 and Tb3 increased with the increase of Gd3 content. The magnetization of HAp co-doped with Gd3 and Tb3 was obviously enhanced. Using Gd3 and Tb3 co-doped calcium carbonate synthesized by carbonization as templates, anion exchange method was used in water bath. Spherical Gd3 and Tb3 co-doped HAp nanoparticles were obtained. Gd3 and Eu3 co-doped calcium carbonate with 1 um diameter synthesized by direct precipitation method were used as templates in hydrothermal environment. Gd3 and Eu3 co-doped HAp microspheres were prepared by anion exchange method. The particle size of HAp microspheres was 1 渭 m and the wavelength was 228nm. Gd3 and Tb3 co-doped HAp have strong green emission at 545nm, and the wavelength is 394nm. The strongest emission peak of HAp co-doped with Gd3 and Eu3 is at 592nm, which belongs to 5D0 of Eu3. 鈫，
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