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Formation of Nanoparticle Ensemble and its Electronic Structure : From Fractal Cluster to Particle Crystal

纳米粒子集合体的形成及其电子结构：从分形簇到粒子晶体

基本信息

批准号：
09304068
负责人：
KIMURA Keisaku
金额：
$ 26.05万
依托单位：
Himeji Institute of Technology
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (A)
财政年份：
1997
资助国家：
日本
起止时间：
1997 至 1999
项目状态：
已结题

项目摘要

During a scheduled period, we have developed a preparation technique enables casting film on quartz or HOPG substrate using high density nanocolloids and observed their structure by STM/AFM which is incorporated in our laboratory. In the last year, we have focused our effort on the formation of gold nanoparticle film together with the confirmation of the size of isolated particles.In addition to the previous preparation method using physical process, a new colloid chemical method was also attempted. It was found that a particle with the smallest size of 1um was prepared when using thiolate as a size controller. A particle whose size is larger than 10nm was formed by the organic reduction method and was fount that the size distribution width is narrow as 15%. The precise surface state of this thiolate-modified particles was determined using various physico-chemical method. In order to aim the particle crystal formation, we have developed a large scale amount synthesis in the order of g using thiol surface modified method. This amount is far from that by the physical dry process in the order of mg. In the final stage of the experiment, particle crystal formation was tested using Au-MSA modified nanoparticles. The regulation parameters tested were content of water/organic solvent, a kind of solvent (methanol, ethanol, 2-propanol),salt concentration, a kind of salt (ammonium sulfate, ammonium chloride), and crystallization temperature. More than several hundreds different conditions were tested using a micro-plating method, well-known in the field of protein chemistry. Unfortunately, a large size crystal formation was not perceived appropriate for the X-ray analysis.The size separation technique such as chromatography or the size-selected precipitation method was remained in a future study to form a three dimensional large size crystal.

在预定的时间内，我们开发了一种制备技术，可以使用高密度纳米胶体在石英或HOPG基底上流延薄膜，并通过我们实验室的STM/AFM观察其结构。去年，我们主要致力于金纳米颗粒薄膜的形成以及分离颗粒尺寸的确认。除了以前使用物理过程的制备方法外，还尝试了新的胶体化学方法。结果发现，当使用硫醇盐作为尺寸控制剂时，制备出最小尺寸为1um的颗粒。通过有机还原法形成尺寸大于10nm的颗粒，发现尺寸分布宽度窄至15%。使用各种物理化学方法测定了这种硫醇盐改性颗粒的精确表面状态。为了实现颗粒晶体形成，我们开发了使用硫醇表面修饰方法的g级大规模合成。这个量与物理干燥法的毫克量级相差甚远。在实验的最后阶段，使用 Au-MSA 修饰的纳米粒子测试了粒子晶体的形成。测试的调节参数为水/有机溶剂含量、溶剂种类(甲醇、乙醇、2-丙醇)、盐浓度、盐种类(硫酸铵、氯化铵)、结晶温度。使用蛋白质化学领域众所周知的微电镀方法测试了数百种不同的条件。不幸的是，大尺寸晶体的形成不适合X射线分析。尺寸分离技术如色谱法或尺寸选择沉淀法仍保留在未来的研究中以形成三维大尺寸晶体。