功能性纳米Fe_3O_4、TiO_2及其复合结构制备表征及应用
摘要
本论文研究了四氧化三铁、二氧化钛及其复合纳米材料,探索制备各种形貌的低维微纳米材料。通过简单的湿化学方法成功制备出树枝状纳米磁性材料、可回收再利用的光催化薄膜与空心多功能磁载核壳结构光催化剂和药物释放材料。利用透射电镜(TEM)、扫描电镜(SEM)、X射线衍射(XRD)、X射线光电子能谱(XPS)、超导量子干涉仪(SQUID)和紫外-可见光吸收(UV-vis)等多种分析测试手段对这些微结构材料进行表征。结果归纳如下:
1、室温下在玻璃基底上利用模板辅助、气体扩散与表面张力使得晶体生长,再自组装的方法成功得到大面积的树枝状结构Fe_3O_4薄膜。该结构具有超顺磁性。通过NH_3气流动使得玻璃基底上聚乙二醇溶液中的(Fe~(3+)/Fe~(2+)发生反应得到树枝状Fe_3O_4纳米粒子组装结构。该树枝状结构室温下具有超顺磁性性能。并研究了Fe_2+/Fe~(3+)的浓度对Fe_3O_4纳米微粒的形貌产生的影响。该制备方法也是对自然界中严寒情况下玻璃窗户上形成的冰花过程的模拟。
2、利用种子诱导还原方法合成了银/钛酸盐纳米线异质结构,并进一步组装成光催化薄膜。与纯钛酸盐纳米线薄膜相同的是该异质结构银/钛酸盐纳米线薄膜有可折叠,稳定,自支撑等特点,而在光降解水溶液中的甲胺磷和光杀菌活性方面都有明显的增强效果。由于纳米线组成的膜具有易回收再利用的性质。该材料将有可能应用于光催化、消毒、杀菌、环境(水、空气)污染处理等方面。
3、在光催化剂的研究基础之上,将磁性能和光催化相结合。利用溶液法及水热法成功制得空心Fe_3O_4@TiO_2@Ag磁载光催化复合微球,利用水热法形成的氧化钛层纤维化及银的金属特性增强磁载光催化剂的光催化性能。此外该种材料还有可能应用于表面增强拉曼散射(SERS)纳米探针方面。
4、在磁载光催化剂的基础上,利用多种制备核壳材料方法制得空心@Fe_3O_4@空心@TiO_2@CdTe@多孔硅核壳结构,这种将磁性能,量子点荧光性能和多孔硅的缓释性能相结合的新型药物载体有可能应用于肿瘤等疾病治疗药物的释放。
Fe_3O_4, TiO_2 and their composite have been investigated and synthesized in this paper. The synthesis of low-dimensional materials with different morphologies and compositions also was explored. By a simple wet chemical method and hydrothermal method, we successfully synthesized dendritic magnetic nanomaterials, recyclable photocatalytic membrane, magnetic photocatalytic and multifunctional hollow core-shell drug release materials. Transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), superconducting quantum interference device (SQUID) and UV-visible absorption (UV-vis) were used to characterize these mirco- and nano-materials. The results are below:
A method for the growth and self-assembly of Fe_3O_4 nanoparticles that is template assisted, as well as gas diffusion and surface tension controlled, has been developed at room temperature. Well-defined dendrite patterns of Fe_3O_4 nanoparticles were obtained upon ion (Fe~(3+)/Fe~(2+)) entrapment in a polyethylene glycol solution followed by NH3 gas exposure on the surface of an aqueous solution on the glass substrate. This dendrite patterns have superparamagnetic behavior at room temperature. The effects of Fe~(2+)/Fe~(3+) concentration on dendrite patterns of Fe_3O_4 nanoparticles also have been studied. The thus-formed patterns mimic nature’s ice ?owers found on glass windows during frost.
Heteronanostructures of Ag particles on titanate nanofibres were synthesized by a seed induced method, and the hetero-nanofibres were organized into catalytic membrane. The hetero-nanostructure membrane has shown similar character with titanate nanofibre one, such as flexible, stability, and self-supporting properties. The Ag/TiO_2 nanofibre heterostructure films show high activity in photodegradation of methamidophos in aqueous solution and light sterilization. The recycling of nanofibre membranes makes it potentially useful in photocatalyst, catalyzer, antiseptic and the environmental pollution treatment.
Based on the previous studies on photocatalytic, we successfully obtained hollow Fe_3O_4@TiO_2@ Ag composite microspheres using the solution method and hydrothermal method. Disposal of TiO_2 shell by hydrothermal method and Ag was used to develope magnetic photocatalytic’s activity. This kind of material may also be used in Surface enhanced Raman spectroscopy (SERS) nanoprobes et.al.
Hollow@Fe_3O_4@hollow@TiO_2@CdTe@mesoporous silicon core-shell structure was further studied for new drug carrier. This drug carrier which combined magnetic properties, quantum dot fluorescence properties and the controlled-release properties of porous silicon can be controlled to a location and be controlled-release.This drug carrier may be used in drug release of cancer treatment.
1、室温下在玻璃基底上利用模板辅助、气体扩散与表面张力使得晶体生长,再自组装的方法成功得到大面积的树枝状结构Fe_3O_4薄膜。该结构具有超顺磁性。通过NH_3气流动使得玻璃基底上聚乙二醇溶液中的(Fe~(3+)/Fe~(2+)发生反应得到树枝状Fe_3O_4纳米粒子组装结构。该树枝状结构室温下具有超顺磁性性能。并研究了Fe_2+/Fe~(3+)的浓度对Fe_3O_4纳米微粒的形貌产生的影响。该制备方法也是对自然界中严寒情况下玻璃窗户上形成的冰花过程的模拟。
2、利用种子诱导还原方法合成了银/钛酸盐纳米线异质结构,并进一步组装成光催化薄膜。与纯钛酸盐纳米线薄膜相同的是该异质结构银/钛酸盐纳米线薄膜有可折叠,稳定,自支撑等特点,而在光降解水溶液中的甲胺磷和光杀菌活性方面都有明显的增强效果。由于纳米线组成的膜具有易回收再利用的性质。该材料将有可能应用于光催化、消毒、杀菌、环境(水、空气)污染处理等方面。
3、在光催化剂的研究基础之上,将磁性能和光催化相结合。利用溶液法及水热法成功制得空心Fe_3O_4@TiO_2@Ag磁载光催化复合微球,利用水热法形成的氧化钛层纤维化及银的金属特性增强磁载光催化剂的光催化性能。此外该种材料还有可能应用于表面增强拉曼散射(SERS)纳米探针方面。
4、在磁载光催化剂的基础上,利用多种制备核壳材料方法制得空心@Fe_3O_4@空心@TiO_2@CdTe@多孔硅核壳结构,这种将磁性能,量子点荧光性能和多孔硅的缓释性能相结合的新型药物载体有可能应用于肿瘤等疾病治疗药物的释放。
Fe_3O_4, TiO_2 and their composite have been investigated and synthesized in this paper. The synthesis of low-dimensional materials with different morphologies and compositions also was explored. By a simple wet chemical method and hydrothermal method, we successfully synthesized dendritic magnetic nanomaterials, recyclable photocatalytic membrane, magnetic photocatalytic and multifunctional hollow core-shell drug release materials. Transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), superconducting quantum interference device (SQUID) and UV-visible absorption (UV-vis) were used to characterize these mirco- and nano-materials. The results are below:
A method for the growth and self-assembly of Fe_3O_4 nanoparticles that is template assisted, as well as gas diffusion and surface tension controlled, has been developed at room temperature. Well-defined dendrite patterns of Fe_3O_4 nanoparticles were obtained upon ion (Fe~(3+)/Fe~(2+)) entrapment in a polyethylene glycol solution followed by NH3 gas exposure on the surface of an aqueous solution on the glass substrate. This dendrite patterns have superparamagnetic behavior at room temperature. The effects of Fe~(2+)/Fe~(3+) concentration on dendrite patterns of Fe_3O_4 nanoparticles also have been studied. The thus-formed patterns mimic nature’s ice ?owers found on glass windows during frost.
Heteronanostructures of Ag particles on titanate nanofibres were synthesized by a seed induced method, and the hetero-nanofibres were organized into catalytic membrane. The hetero-nanostructure membrane has shown similar character with titanate nanofibre one, such as flexible, stability, and self-supporting properties. The Ag/TiO_2 nanofibre heterostructure films show high activity in photodegradation of methamidophos in aqueous solution and light sterilization. The recycling of nanofibre membranes makes it potentially useful in photocatalyst, catalyzer, antiseptic and the environmental pollution treatment.
Based on the previous studies on photocatalytic, we successfully obtained hollow Fe_3O_4@TiO_2@ Ag composite microspheres using the solution method and hydrothermal method. Disposal of TiO_2 shell by hydrothermal method and Ag was used to develope magnetic photocatalytic’s activity. This kind of material may also be used in Surface enhanced Raman spectroscopy (SERS) nanoprobes et.al.
Hollow@Fe_3O_4@hollow@TiO_2@CdTe@mesoporous silicon core-shell structure was further studied for new drug carrier. This drug carrier which combined magnetic properties, quantum dot fluorescence properties and the controlled-release properties of porous silicon can be controlled to a location and be controlled-release.This drug carrier may be used in drug release of cancer treatment.
引文
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