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Measurement of hydrogen concentration in steels by laser-induced breakdown spectroscopy (LIBS)
(2021)
Current efforts to achieve lightweight construction and the required reduction in CO2 emissions and an increase in energy and resource efficiency call for the increasing use of high-strength fine-grain structural steels. However, as the strength of higher-strength fine-grain structural steels increases, so do the associated joining challenges. Particular attention must be paid to hydrogen-assisted cold cracking. The influence of hydrogen reveals itself less in the strength but has a significant effect on the deformability [1, 2]. The degradation of the material properties can lead to zero ductility, where the values of the yield strengths coincide with the tensile strengths.
Laser-induced breakdown spectroscopy (LIBS) is a spectroscopic technique that can be used to determine elemental compositions without pre-treatment of the samples. Short, high-energy laser pulses ablate a small volume (< 0.1 mm3) of the examined material and ionize it to form a plasma. The decaying plasma emits element-specific light. This light is spectroscopically analysed and allows to detect qualitatively the present elements and to quantify them with help of a standardization routine. The simple experimental set-up and the fast, nearly non-destructive analysis procedure characterize the LIBS analysis. The LIBS method allows a time and spatially resolved in situ measurement of steel components in use.
Even low hydrogen concentrations (~ 1 wt.-ppm) in steel can be measured with the LIBS method and can be quantified with help of certified reference materials. The results are compared with results gained with the well-established carrier gas hot extraction method.
The KorroPad indicator test was invented at the Federal Institute for Materials Research and Testing to detect stainless-steel surfaces susceptible to pitting corrosion. The KorroPad indicator test is thus an interesting alternative for manufacturers, processors, users and researchers to time consuming exposition experiments and complex electrochemical investigations, which are normally used to reveal surface-related processing errors resulting in reduced pitting corrosion resistance. Furthermore, the KorroPad indicator test can be used to visualize alloy- and microstructure-related factors causing susceptibility to pitting corrosion. The detection limit of the KorroPad indicator test was characterized in this work using reference alloys with different chromium content (5 % to 18 %). The alloy-specific detection limit was shifted successfully to higher chromium content by increasing the concentrations of NaCl and K3[Fe(CN)6]. The modified KorroPads can now be used to establish an alloy-specific quality control regarding the pitting corrosion resistance of different stainless steel grades.
Nickel-free, nitrogen alloyed austenitic stainless-steels, with about 19 wt.-% Mn and 0,8 wt. % N, are an interesting alternative to classic CrNi austenitic stainless steels due to their superior mechanical properties (Rm > 900 MPa, A5 > 50 %, Av > 350 J) in the solution annealed condition. The formation of chromium-rich nitrides during suboptimal heat treatment, processing or application leads to an inhomogeneous distribution of alloying elements in the microstructure, which reduces the corrosion resistance. Consequently, an accurate knowledge of the sensitization behavior is indispensable for the use of nickel-free, high-nitrogen austenitic stainless steels. The relationship between artificial aging, phase formation and corrosion resistance was investigated on the alloys X8CrMnN18-19 (1.3815) and X8CrMnMoN18-19-2 (1.4456), both alloyed with 0,8 wt.-% Nitrogen, in the present work. The microstructural evolution was studied by LM and SEM while the corrosion resistance was characterized with the electrochemical potentiodynamic reactivation (EPR) and the KorroPad indicator-test. Both alloys showed increased corrosion susceptibility within critical aging parameters. Finally, a sensitization diagram was described successfully for both alloys showing the positive effect of molybdenum.
The copper alloyed stainless steel 1.4542 (X5CrNiCuNb16-4) is used in different areas due to its good mechanical properties and corrosion resistance. Strength and corrosion re-sistance can be adjusted by the heat treatment, which is of importance for the application of this alloy. The mechanical properties (strength and hardness) are attributed to the dispersive precipitation of the copper rich ε–Phase. The additional precipitation of chromium carbides can reduce the corrosion resistance. Different ageing states were produced to investigate the precipitation behaviour with various methods. Furthermore, the influence of cold-rolling on the precipitation behaviour was studied in comparison to a solution annealed state without deformation. The microstructure was studied by SEM and the variations of hardness and magnetic proportion were characterised. The electrochemical potentiodynamic reactivation (EPR) was used to determine the corrosion resistance and detect chromium depletion in all heat-treated states. The results show that a work hardening accelerates the precipitation rate, while ageing at 600 °C reduces the corrosion re-sistance due to chromium depletion.
In the context of a research project carried out by BAM, nine different steel alloys were exposed to maritime environmental conditions at the German Island of Helgoland over a period of five years and their corrosion behavior was compared and evaluated. In order to evaluate the influence of a possible concentration of corrosion specific crucial air constituents on the investigated steel grades, a series of sample surfaces were freely exposed to the we ather while other samples were protected from direct rain in a covered area. The parallel investigation of four different surface finishes (cold rolled, dry grinded, electro-polished, blasted) of the respective alloys also made it possible to take account of the specific influences and features of the surface finish during the material comparison. On the basis of the results of the natural exposure tests, conclusions were drawn about the influence of the alloy composition, the surface finish and the exposure time under maritime conditions. The samples of the three investigated duplex alloys exhibited the best corrosion resistance under the given maritime environmental conditions over the five-year period, both with and without crevice geometry. Likewise, the molybdenum alloy ferrite 1.4521 could achieve comparable corrosion resistance as the austenitic standard materials 1.4301 and 1.4404. The results on the freely exposed surfaces showed, that due to the washing effect the influence of the exposure time on the corrosion of the samples is low while the particular surface finish has a great influence on the overall corrosion behavior of the stainless steels. Thus, the electro-polished surfaces showed few signs of corrosion while the blasted surfaces exhibited very poor corrosion behavior. In the case of the covered specimens, the respective material-specific corrosion resistance as well as the exposure time have a significant influence on the corrosion behavior while the surface finishes were of marginal importance.