| 题名 | 燃烧合成纳米颗粒制备表征平台与应用探索 |
| 作者 | 岳仁亮 |
| 学位类别 | 博士 |
| 答辩日期 | 2012-06-01 |
| 授予单位 | 中国科学院研究生院 |
| 导师 | 陈运法 |
| 关键词 | 燃烧合成 纳米颗粒 过程表征 |
| 其他题名 | Exploring Characterization Instrument and Application of Nanoparticles by Flame Synthesis |
| 学位专业 | 化学工程 |
| 中文摘要 | 摘要燃烧合成是纳米颗粒制备的常用方法，其反应速度快，容易大规模生产，但产物的可调控性有待提高，因此亟待加强对颗粒形成机理的认识，燃烧合成机理研究的关键在于制备过程表征。本文重点研制了燃烧合成纳米颗粒的表征平台，并开展一些典型纳米颗粒的应用探索。研制了燃烧合成系统，可更好研究纳米颗粒在火焰中的形成过程，通过研制相应设备和集成仪器，建立了制备过程表征平台。结合燃烧合成疏水纳米氧化硅、铝掺杂纳米氧化锌、球形纳米氧化铝等系列纳米颗粒，表征其制备工艺参数，研究其合成调控技术和机理，为燃烧合成高附加值纳米颗粒及工艺放大奠基技术基础。研制了燃烧合成纳米颗粒的装置，系统集成了供气系统、燃烧系统、收集系统，燃烧系统可进行气相进料、液相进料，液相进料中根据压力雾化喷嘴、气体雾化喷嘴、超声波雾化喷雾的特点设计研制了助燃气体控制管路。燃烧合成装置能够制备纳米氧化硅、铝掺杂纳米氧化锌、球形纳米氧化铝等纳米颗粒，装置长期运行稳定，并且具备小批量制备能力，具有较好的实用性。研制了燃烧合成的过程表征平台，平台能原位表征喷雾液滴的粒度、浓度、速度，原位表征燃烧合成火焰场的温度，能够结合研制的在线高温取样稀释器，实时表征火焰中颗粒的浓度、粒度，并可收集后进行形貌分析，能够实时表征纳米颗粒的表面官能团、成分等，通过制备过程表征平台的集成应用，可高效研究燃烧合成纳米颗粒的机制及调控技术。燃烧合成纳米氧化硅，重点探索纳米氧化硅表面官能团作用机制。研究了纳米氧化硅制备的调控技术，通过在反应器中加入支路氩气进行了精确调控颗粒粒径，研究发现随着支路氩气流量的增大，纳米氧化硅的颗粒有小变大，颗粒粒径变大前是亲水氧化硅，表面含有大量羟基，颗粒粒径变大后，颗粒是疏水纳米氧化硅，通过红外、热重、扫描、透视电镜、荧光光谱仪、核磁共振等系列分析，确定了疏水性样品的结构，研究表明疏水性颗粒表面存在甲基基团，分析了疏水性二氧化硅纳米颗粒的形成可能机理，实现了一步法燃烧合成疏水性纳米氧化硅，相关结果未见文献报道，实现了同一反应器燃烧合成亲水纳米氧化硅和疏水纳米氧化硅的调控，探索了其形成机理和表面官能团作用机制，对于燃烧合成纳米颗粒调控具有指导意义。燃烧合成铝掺杂纳米氧化锌，重点研究铝掺杂纳米氧化锌及其导电性能，分析燃烧合成纳米氧化物的掺杂工艺及调控技术。研究了制备过程中的反应条件，通过Al掺杂制备了纳米导电氧化锌，表征了其导电性能，制备的导电纳米氧化锌粒度均匀，导电性能良好，具备了应用条件。燃烧合成球形纳米氧化铝，重点研究球形纳米氧化铝的制备，分析研究燃烧合成球形金属氧化物的工艺和调控技术。研究了制备工艺及对球形纳米氧化铝制备的影响因素，探索了其制备的机理，表征了其在节能灯中爬升时间等性能，测试表明具有良好的应用前景。 |
| 英文摘要 | Abstract The paper focused on the formation process, application and apparatus of flame synthesized nanoparticles according to the technical characteristics and development tendency during nanoparticles preparation. The devices were established by developing interface equipments and integrated equipment for the research of nanoparticles preparation process in the flame. Meanwhile the technological parameters during preparation of silica dioxide, zinc oxide, conductive zinc oxide, alumina and sphere alumina were characterized and the preparation process and possible mechanism were also studied. And this work lays the foundation for high added-value novel materials and process scales up by flame synthesis. Nanoparticles of silica dioxide, zinc oxide and alumina can be prepared by the flame synthesis apparatus, which can apply to continuous production and show long-term stability and good practicability. Besides, granularity, concentration, speed and flame field temperature of the spraying droplets can be characterized by the device of process characterization. The granularity, concentration and morphology after collection of the particles in flame, surface functional groups and compositions of the nanoparticles can also be characterized in the aid of on-line high temperature sampling diluter. Mechanism and regulating technology of flame synthesis were studied efficiently through in-situ characterization. Control of particle size in a large range was investigated via silica dioxide nanoparticles by flame synthesis and one-step synthesis of hydrophobic silica dioxide nanoparticles was achieved through controlling flame parameters. Domestic and international patents have been applied and the relevant results of the field had not been reported until now. Besides, the properties of hydrophobic silica dioxide nanoparticles were characterized and the structure of hydrophobic samples was confirmed, which showed the presence of methyl groups on the surface of hydrophobic silica dioxide nanoparticles. The formation mechanism of hydrophobic silica dioxide nanoparticles was also analyzed. Moreover, controlling of the flame synthesized nanoparticles of hydrophilic and hydrophobic silica dioxide was realized using the same reactor and their formation mechanism and function mechanism of surface functional group were explored, which make important sense to flame synthesis. As refer to Al-doped ZnO, the effects of precursor concentration and flame structure in the preparation on the topographic and dispersing property of zinc oxide were analyzed by the flame-made zinc oxide nanoparticles and technological parameters were confirmed. Conductive property was characterized by exploring the effects of Al-dopant concentration on conductive powders and the particle size of zinc oxide was uniform. Conductive tests suggest lower resistivity and application prospect. In the preparation of nano-Al2O3, especially spherical nano-Al2O3, the process control was adjusted to investigate the effect of parameters on morphology and properties of products. The raw materials were aluminium precursors and sphere alumina nanoparticles were prepared through process and precursor ratio control. Further, the formation mechanism during gas phase synthesis was presumed according to the above experimental results. The sol of nano-Al2O3 exhibited superior stability during CFLs test, and application prospect was indicated by the test of climbing time in CFLs. |
| 语种 | 中文 |
| 公开日期 | 2013-09-25 |
| 内容类型 | 学位论文 |
| 源URL | [http://ir.ipe.ac.cn/handle/122111/1799]  |
| 专题 | 过程工程研究所_研究所（批量导入） |
| 推荐引用方式 GB/T 7714 | 岳仁亮. 燃烧合成纳米颗粒制备表征平台与应用探索[D]. 中国科学院研究生院. 2012. |
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