Determination of aluminium nitride or free nitrogen in low carbon steel

Abstract

As the aluminium nitrides play an important role in the manufacturing of steel sheets, a specific methodology was developed based on the thermoelectric power (TEP) technique, in order to determine the AIN nitrogen by an indirect method. The free nitrogen was determined and then the AIN nitrogen was calculated by the difference between the total nitrogen and the free nitrogen. Indeed, it is easier to determine the dissolved nitrogen, the content of which gradually decreases during the AIN precipitation, than the AIN nitrogen. A low carbon aluminium killed steel was employed with 580 ppm of aluminium and 50 ppm of nitrogen. A comparison of the results obtained by TEP with those obtained by other techniques (hot hydrogen extraction, electrochemical dissolution followed by a mineralization, electrochemical dissolution followed by a sodic decomposition and the Beeghly method) was conducted, in order to determine a reliable technique likely to quantify the amount of aluminium nitrides in aluminium killed steels. With these techniques, it is possible to determine either free nitrogen or precipitated nitrogen. From an experimental point of view, the precipitation kinetics of AIN was followed during an annealing performed at 973 K (700 °C) by TEP and then different precipitation states of AIN were investigated to compare the different techniques: three annealing states (when no nitrogen, half the nitrogen and the total nitrogen has precipitated) and two soaking states (1403 and 1523 K). Thus, it was possible to compare states where the AIN precipitates are in various forms (different shapes, crystallographic structures, sizes, distributions in the matrix). This work showed that the quantification by TEP, hot hydrogen extraction and electrochemical dissolution followed by a mineralization seem reliable whereas the Beeghly method gives good results only for the precipitates formed at high temperatures. In contrast, the quantification by electrochemical dissolution followed by a sodic decomposition does not seem reliable.