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首页> 外文会议>The 3rd International Symposium on Material Chemistry in Nuclear Environment (Material Chemistry '02 MC'02) Mar 13-15, 2002 Tsukuba >STUDY ON SYNTHESIS TECHNIQUE AND THERMAL ANALYSIS OF Na-Fe COMPLEX OXIDES
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STUDY ON SYNTHESIS TECHNIQUE AND THERMAL ANALYSIS OF Na-Fe COMPLEX OXIDES

机译：钠铁复合氧化物的合成技术及热分析的研究

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摘要

As a coolant of Fast Breeder Reactors, sodium reacts with oxygen and moisture in air at elevated temperature. And it is known that structural material is damaged by its by-products. Although the reliable thermodynamic data of Na-Fe complex oxides was needed in order to clarify the corrosion mechanism and to examine the technique of corrosion protection, each data is different by researchers. In this study, synthesis technique of high purity Na_4FeO_3 as one of Na-Fe complex oxides under low oxygen potential has been established in order to get reliable thermodynamic data. For synthesis, the following reaction was used; 2Na_2O + FeO = Na_4FeO_3 (ΔH_(298)K=104.49kJ/mol) in a sealed up vessel at 873K for 100h. Na_2O reagent used was refined at 973K for about 1h in vacuum, where impurity (Na_2O_2) in the reagent was decomposed. In order to keep low oxygen potential in the vessel, mixture of Na_2O and FeO was filled up in the vessel by applying vibration. X-ray diffraction patterns were taken in nitrogen environment to identify the reaction product, and it was confirmed that pure Na_4FeO_3 crystal was obtained. In addition, thermal analysis of the samples has been performed by using a differential scanning calorimeter to determine the melting point and to check a possibility of another phase transformation. The sealed up sample holder made of platinum was used for the analyses. From the analyses, the melting point of Na_4FeO_3 was determined to be 1,008+-15K.
机译：钠作为快速繁殖反应堆的冷却剂，在高温下会与空气中的氧气和水分发生反应。众所周知，结构材料会被其副产品损坏。尽管需要用Na-Fe复合氧化物的可靠热力学数据来阐明腐蚀机理和检验腐蚀防护技术，但研究人员对每种数据都有所不同。为了获得可靠的热力学数据，本研究建立了在低氧势下作为Na-Fe复合氧化物之一的高纯度Na_4FeO_3的合成技术。为了合成，使用以下反应；在密闭容器中于873K加热2h_2O + FeO = Na_4FeO_3（ΔH_（298）K = 104.49kJ / mol）100h。将所用的Na_2O试剂在973K真空中精制约1小时，其中试剂中的杂质（Na_2O_2）分解。为了保持容器中的低氧势，通过施加振动将Na_2O和FeO的混合物填充在容器中。在氮气环境下拍摄X射线衍射图谱以鉴定反应产物，并证实获得了纯的Na_4FeO_3晶体。另外，已经通过使用差示扫描量热仪进行样品的热分析以确定熔点并检查另一相变的可能性。使用由铂制成的密封样品架进行分析。通过分析，确定Na_4FeO_3的熔点为1,008 + -15K。

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