Development of Nano-Thermal Analysis System with MEMS Technology

本项目旨在将采用MEMS技术制造的纳米量热计与扫描电子显微镜(SEM)或能量色散X射线能谱(EDXS)相结合，开发出一种组合的纳米量热仪系统。该纳米热分析系统在质量和放热或吸热反应测量中具有良好的分析性能，具有纳米到微克样品的可视化功能。提出了微悬臂式热量计机械共振的微小质量测量方法、纳量热法与扫描电子显微镜观察相结合的方法、纳米克级样品的微操作处理方法，并对微纳克级金属和非有机样品进行了质量和热分析。利用MEMS技术研制了长度为260~800微米的悬臂式热量计，并配备了热电偶、加热器和热电堆等热器件。快速温度sc…更多1000开尔文每秒的订单可供选择。因此，量热计对微弱的放热和吸热反应很敏感。在质量测量技术方面，发展了内置式应变片检测纳米量热仪机械共振的方法和光学检测方法。采用应变片技术和正反馈电路，研制出高紧凑度的纳米量热计自谐振系统。结果表明，该系统可对室温至800℃范围内小于1微克的样品进行质量和热分析。在纳米量热和扫描电子显微镜的结合中，将紧凑型质量和热分析系统引入到低加速电压型紧凑型扫描电子显微镜中。结果表明，通过观察亚微米分辨率的样品形状，可以进行纳米量热测量。此外，利用EDXS和纳米量热计还可以对样品表面的化学物种进行联合分析。微操作也是纳米量热学的重要课题。本研究用热法证明了针式机械手与微量样品之间粘附力的可控性。在该方法中，通过从机械手中的毛细管中扩散水并在加热机械手尖端时蒸发来控制机械手尖端上的水量。因此，附着力可以从1微牛顿到10微牛顿级别变化。论证了其在热粘着控制中的可行性。较少

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