The effect of a controlled oxygen admixture to a plasma nitrocarburizing process using active screen technology and an active screen made of carbon was investigated to control the carburizing potential within the plasma-assisted process. Laser absorption spectroscopy was used to determine the resulting process gas composition at different levels of oxygen admixture using O2 and CO2, respectively, as well as the long-term trends of the concentration of major reaction products over the duration of a material treatment of ARMCO® iron. The short-term studies of the resulting process gas composition, as a function of oxygen addition to the process feed gases N2 and H2, showed that a stepwise increase in oxygen addition led to the formation of oxygen-containing species, such as CO, CO2, and H2O, and to a significant decrease in the concentrations of hydrocarbons and HCN. Despite increased oxygen concentration within the process gas, no oxygen enrichment was observed in the compound layer of ARMCO® iron; however, the diffusion depth of nitrogen and carbon increased significantly. Increasing the local nitrogen concentration changed the stoichiometry of the ε-Fe3(N,C)1+x phase in the compound layer and opens up additional degrees of freedom for improved process control.
The work is devoted to the development of laser absorption spectroscopy (LAS) of plasma-assisted processes for application under industrial conditions. The interpretation of the LAS measurements was revised by taking into consideration the temperature gradient along the absorption path, which is unavoidable in a reactor for thermochemical treatment. The revision is based on the measurement of HCN, NH3, H2O and CO molecular lines in an industrial-scale, active screen plasma nitrocarburizing (ASPNC) reactor with a steel active screen (AS). It shows that an effective temperature determined from Doppler broadening could be assigned to each measured spectral line. The effective temperature does not only reflect the temperature gradients along the line-of-sight but also the line strength dependence on temperature for the specific spectroscopic transition. Lower limit estimates of the molecular densities are proposed based on the determined effective temperatures under the assumption of a Boltzmann distribution of the population density over the molecular levels at any local volume of the reactor. For a more accurate interpretation of LAS data of plasma-assisted processes, the spatial distribution of the temperature along line-of-sight has to be known and needs to be taken into account to obtain the molecular densities.
In principle, the plasma nitriding of Al based substrates is a well-known process, though it remains extremely challenging from both the technological point of view and the aspect of stress loading conditions. In order to improve the latter, a duplex treatment consisting of plasma nitriding and subsequent surface remelting using electron beam technology was employed. The focus of this paper (part I) was on the characterisation of the initial microstructure after plasma nitriding. This should create the basis for a better understanding of the processes taking place or changes in the subsequent duplex treatment. This was done with the help of high-resolution imaging and analysis tools in the scanning and transmission electron microscope as well as XPS analyses. Special attention was paid to the nitriding mechanism at the interface as a function of the local microstructural constituents of the hypereutectic Al alloy substrate (Al solid solution, primary silicon, and intermetallic phases). While the main part of the nitride layer formed consisted of AlN and small fractions of pure Al in the diffusion paths, other nitrides and oxides could also be detected in the area of the interface.
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