Development of Microcalorimetry

微量热法的发展

• 批准号: 60303002
• 负责人: SUGA Hiroshi
• 金额: $ 6.46万
• 依托单位: Faculty of Science, Osaka University
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Co-operative Research (A)
• 财政年份: 1985
• 资助国家: 日本
• 起止时间: 1985 至 1987
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-60303002/
• 关键词: microcalorimetry; miniaturization of calorimeter; reaction calorimeter; 非反応系カロリメトリー

Many calorimetric methods owe their accurate data partly to large amount of purified speciman used in the experiments. Recent development in synthesis of new materials and characterization methods necessitated to miniaturize various types of calorimeters for the thermodynamic characterization. It is the purpose of this research project to aim at miniaturization of various kinds of reaction and non-reaction calorimeters for further development of thermoscience without loss of accuracy and precision of the resulting calorimetric data.A low-temperature adiabatic microcalorimeter was developed which made it possible to determine the third law entropy with small amount of specimen less than 1 g. A laser-flash calorimeter was improved so as to produce reliable heat capacity data of solid sample up to 1200 K. A microcalorimeter was built for measuring the heat capacity of a 1- l liquid sample using a light-irradiation ac calorimetric technique. A micro-bomb calorimeter was developed which req … More uired only 10 mg of sample for the determination of enthalpies of combustion of inorganic and organic compounds. A micro-solution calorimeter was improved in a sophisticated way so that the enthalpy of mixing between benzene and perdeuterobenzene was determined with inaccuracy of 1 %. An adiabatic micro-calorimeter for vapor-deposited sample clarified a new aspect of vapor-deposited amorphous material. They showed non-linear enthalpy relaxation phenomennon which started at much lower temperature than those for liquidd-quenched sample. A very low-temperature calorimeter with a dilution refrigerator made it possible to determine the heat capacity of condensed matter down to 20 mK. This clarified many aspects of magnetic material possessing weak interaction among the constituents.These development widen the applicability of the calorimetric experiments to many types of new materials which are possible to prepare only in small quantity, and surely open the door to novel way of thermoscience. Less

许多量热方法的准确数据部分归功于实验中使用了大量的纯化样品。在新材料的合成和表征方法的最新进展中，有必要将各种类型的量热计小型化以进行热力学表征。本研究的目的是为了使各种反应量热计和非反应量热计小型化，在不影响量热数据的准确度和精密度的前提下，进一步发展热科学。研制了一种低温绝热微量热计，它可以在小样品量小于1g的情况下测定第三定律熵。对激光闪光量热计进行了改进，使之能够产生可靠的固体样品在1200K以下的热容数据。利用光辐照交流量热技术，建立了一种用于测量1-L液体样品热容量的微量热计。研制了一种要求…的微弹量热仪此外，只需10毫克样品即可测定无机和有机化合物的燃烧热。对微溶液量热仪进行了改进，使之能准确测定苯与二氢呋喃的混合热值，误差为1%。用于气相沉积样品的绝热微量热计阐明了气相沉积非晶态材料的一个新方面。它们表现出明显的非线性热弛豫现象，其起始温度比液态淬火样品低得多。一种带有稀释冰箱的超低温量热计使测定凝聚态物质的热容到20MK成为可能。这些发展使量热实验的适用范围扩大到许多类型的新材料，这些新材料可能只需要少量的制备，也必将为新的热科学方法打开大门。较少

项目成果

S. Murakawa, T. Wakamatsu, M. Sarai and H. Suga: "A Very Low-temperature Calorimeter with a (^3He + ^4He)Dilution Refrigerator: The Heat Capacity of trans-bis(ethylenediamine) bis(isothiocyanato)nickel(II)" J. Chemical Thermodynamics. 19. 1275-1292 (1987)

S. Murakawa、T. Wakamatsu、M. Sarai 和 H. Suga：“带有 (^3He ^4He) 稀释制冷机的极低温量热计：反式双（乙二胺）双（异硫氰酸）镍的热容量（

T.Matsuo et al.: Thermichimica Acta. 88. 149-158 (1985)

T.Matsuo 等人：Thermichimica Acta。

S. Murakami et al: J. Solution Chemistry. 16. 315-326 (1987)

S. Murakami 等人：J. 溶液化学。

I.Hatta et al.: Japanese J.Applied Physics. 25. L493-L495 (1986)

I.Hatta 等人：日本应用物理学杂志。

H. Uedaira et al: Thermochimica Acta. 123. 183-191 (1988)

H. Uedaira 等人：Thermochimica Acta。