Development of Nano-Thermal Analysis System with MEMS Technology

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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