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Development of Nano-Thermal Analysis System with MEMS Technology

利用MEMS技术开发纳米热分析系统

基本信息

批准号：
20360103
负责人：
NAKABEPPU Osamu
金额：
$ 12.48万
依托单位：
Meiji University
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (B)
财政年份：
2008
资助国家：
日本
起止时间：
2008 至 2011
项目状态：
已结题

项目摘要

This project aimed to develop a combined nano-calorimetry system by combining the nano-calorimeter fabricated with the MEMS technology with SEM(Scanning Electron Microscope) or EDXS(Energy dispersive X-ray Spectroscopy). The nano-thermal analysis system has excellent analysis performance in mass and exo-or endothermic reaction measurement with visualization function for nano to microgram sample.Following three techniques have been studied. Minute mass measurement method with mechanical resonance of the micro-cantilever type calorimeter, combination method between the nano-calorimetry and SEM observation, and micromanipulation method for handling the nano-gram level samples.Following results to the mass and thermal analysis of micro-to nano-gram level metal and non-organic samples have been obtained. The cantilever type calorimeter of 260 to 800 micro-meter length with thermal devices such as thermocouple, heater and thermopile was developed with the MEMS technology. Fast temperature sc … More an of 1000 Kelvin per second order is available. Thus, the calorimeter is sensitive to faint exo-and endothermic reaction. The developed calorimeter also can be used in DTA(Differential Thermal Analysis) and DSC(Differential Scanning Calorimetry) modes.As for the mass measurement technology, built-in strain gage detection method has been developed for detecting the mechanical resonance of the nano.calorimeters as well as an optical detection method. The auto-resonance system for the nano-calorimeter was developed with high compactness by the strain gage method and a positive feedback circuit. It was demonstrated that mass and thermal analysis of less than 1 microgram sample ranging from room temperature to 800 degree Celsius are available with the developed system.In the combined nanocalorimetry with the SEM, the compact mass and thermal analysis system was introduced into the compact type SEM of low acceleration voltage type. It was demonstrated that the nanocalorimetry can be performed with observing the sample shape with sub-micrometer resolution. Moreover, another combined analysis investigating chemical species of sample surface is available by using the EDXS with the nanocalorimeter.The micro-manipulation is also important topics for the nanocalorimetry. This research demonstrated controllability of adhesion force between a needle type manipulator and micro-sample with thermal method. In this method, the amount of water on the manipulator tip is controlled with spreading water from capillary in the manipulator and evaporation with heating the tip. As a result, the adhesion force can varies from 1 to 10 micro-Newton level. The possibility in the thermal adhesion control was demonstrated. Less

本项目旨在通过将MEMS技术制造的纳米量热仪与SEM（扫描电子显微镜）或EDXS（能量色散X射线光谱）相结合，开发一种组合式纳米量热系统。纳米热分析系统具有良好的质量分析性能和吸热、放热反应测量性能，并具有纳米级至微米级样品的可视化功能。采用微悬臂梁式量热计的机械共振微量质量测量方法、纳米量热法与SEM观察相结合的方法以及纳米克级样品的显微操作方法，对微米至纳米克级的金属和无机样品进行了质量和热分析，得到了如下结果：利用MEMS技术研制了长度为260 ~ 800 μ m的悬臂梁式量热计，该量热计采用热电偶、加热器和热电堆等热器件。快速温度开关 ...更多信息可获得每秒1000开尔文的量级。因此，量热计对微弱的放热和吸热反应敏感。该量热计还可用于差示热分析（DTA）和差示扫描量热法（DSC）模式。在质量测量技术方面，开发了内置应变片检测方法和光学检测方法，用于检测纳米量热计的机械共振。采用应变片法和正反馈电路，研制了紧凑型纳米量热计自谐振系统。实验结果表明，该系统可对小于1 μ g的样品在室温至800 ℃范围内进行质量和热分析。在与SEM结合的纳米量热法中，将紧凑型质量和热分析系统引入到低加速电压型紧凑型SEM中。结果表明，纳米量热法可以进行观察样品的形状与亚微米分辨率。此外，EDXS与纳米量热仪还可以联合分析样品表面的化学形态，微操作也是纳米量热仪的重要研究课题。本研究以热法验证针式机械手与微样品间附着力之可控制性。在该方法中，操纵器尖端上的水量通过从操纵器中的毛细管扩散水和通过加热尖端蒸发来控制。因此，粘附力可以在1至10微牛顿水平之间变化。证明了热粘附控制的可能性。少