Study on Ultraminiature Thermal Analysis Device and its Thermal Analysis Method

本研究的目的是将微型气桥加热器、样品架和温度传感器单片制作，研究原始加热方法及其控制系统，研究理论热方程与实验数据对比得出物理量的推导方法，研究量热评价，开发从低温到高温均可测量的热分析装置。研究有机和无机材料的实际热分析评价，研究磁性材料的热分析，从初始和时间相关的热变化中识别各种样品的初始质量和时间相关的质量变化，从理论上研究这些现象，制作一个方便的超微型热分析装置，并构建原始热分析系统的基础。并建立了可变b常数电路的晶体管热敏电阻作为一个tem . More温度传感器。本研究的结果如下：1)对微加热器和样品架的尺寸和形状、热电偶材料和蚀刻工艺进行了研究和评价，发现从再现的角度来看，Au和Ni薄膜组合作为热电偶是最好的。2)制作了适用于传感部分的温度扫描控制系统，并采用恒功率速率扫描的个人电脑驱动器进行了演示。3)为了验证和评价微分法对时间的影响，建立了一种无需参考样品就能得到升温速率曲线的新方法。4)建立了水等样品的初始质量评价方法，得到了水样的焓值。5)提出了双极型和MOSFET型的晶体管热敏电阻来测量衬底的绝对温度，并在理论上进行了考虑，并证明了能够与小型化的热分析传感器单片集成。6)部分冷却系统，使用温度控制系统与珀尔帖装置相结合，控制样品架的温度从低温到高温。7)对一些样品（包括从冰到蒸汽的水）的热分析可以在30秒内完成。如上所述，我们已经明确了一个指导方针，以实现热分析系统的高速，低功耗，非常高的灵敏度，非常少量的样品。除了对磁性材料进行评价外，基本达到了本研究的目的。少

The purpose of this study is to fabricate a micro-air-bridge heater, a sample holder and a temperature sensor monolithically, to investigate original heating method and its control system, to investigate the deduction method of physical quantities obtained from comparison between theoretical thermal equations and experimental data, to investigate calorimetric evaluations, to develop the thermal analysis device measurable from low to high temperature, to investigate actual thermal analytical evaluations of organic and inorganic materials, to investigate the magnetic materials thermal analytically, to identify the initial mass and time dependent change of the mass of various samples from initial and time dependent thermal variations, to investigate these phenomena theoretically, to fabricate a handy ultraminiature thermal analysis device and to construct the basis of the original thermal analysis system, and to establish the variable B-constant circuits for transistor-thermistor as a tem … More perature sensor. Results of this study are as follows:1) Suitable size and shape for microheater and sample holder, materials of thermocouple and etching process are investigated and evaluated, and it is found that combination of Au and Ni film as a thermocouple are the best for this purpose from the point of view of reproduction. 2) Control system for temperature scanning suitable to the sensing portion is made and is demonstrated by personal computer drive adopting the constant-power-rate scanning. 3) A new method to get a heating-rate curve without the reference-sample is established in order to confirm and to evaluate the differentiation method with respect to time. 4) Evaluation method of initial mass of a sample such as water is established, and the enthalpy of the water sample is obtained. 5) Transistor-thermistors of both bipolar type and MOSFET type are proposed to measure the absolute temperature of the substrate, and are considered theoretically, and are demonstrated to be able to be monolithically integrated with a miniaturized thermal analysis sensor. 6) Partial cooling system to control the temperature of the sample-holder from low to high temperature is performed using the temperature control system combined with a Peltier device. 7) It is demonstrated that thermal analysis for some samples including water from ice to vapor is carried out within 30 seconds. As mentioned above, we have clarify a guide-line to achieve the thermal analysis system with high speed, lower power consumption, very high sensitivity for very small quantity of sample. The purpose of this basic study is successfully achieved, except evaluation of the magnetic materials. Less