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合成了标题配合物,测定了其晶体在80~385 K温度范围的等压摩尔热容,低温区间的绝热量热和差示扫描量热均发现配合物在220K和245K附近存在固-固相转变,推测其机理可能是配合物中高氯酸根的重取向运动不同阶段所造成;根据实验热容数据和热力学公式,计算出配合物在80~385 K温度区域内相对于298.15K的标准热力学函数[HT-H298.15]和[ST-S298.15],根据热容测定数据计算出该相变的焓变和熵变。用热重法检测了配合物的热稳定性并推测其热分解机理。这两个低温区相变过程的发现,使开发此类配合物作为新低温相变材料成为可能。
The title complex was synthesized and the isothermal molar heat capacity of the crystal at 80 ~ 385 K was measured. The adiabatic calorimetry and differential scanning calorimetry (DSC) showed that there was a solid-solid phase near 220K and 245K It is speculated that the mechanism may be caused by different stages of reorientation of perchlorate in the complex. Based on the experimental heat capacity data and the thermodynamic formula, the standard thermodynamic function of the complex in the temperature range of 80 ~ 385 K relative to 298.15 K [HT-H298.15] and [ST-S298.15], the enthalpy change and entropy change of this phase change were calculated from the heat capacity measurement data. The thermogravimetric method was used to determine the thermal stability of the complex and the mechanism of its thermal decomposition. The discovery of these two phase transitions in the low temperature region makes it possible to develop such complexes as new low temperature phase change materials.