Hydrogen trapping and de-trapping behavior was investigated for steels with and without V. The de-trapping of hydrogen is very slow while the trapping presumably proceeds rapidly for steels containing VC precipitates. The activation energy for de-trapping is in the range of 33 to 35 kJ/mol. The trapped-hydrogen content and diffusible-hydrogen content in the steady state increase with increasing hydrogen entry rate into the steel. The density of hydrogen trapping sites decides the maximum trapped-hydrogen content; 9 ppm for 1 % V steel tempered at peak secondary hardening temperature. Analysis of hydrogen embrittlement cracking tests in terms of hydrogen contents such as the critical hydrogen content should be performed on the specimens with uniform hydrogen distribution and must consider the nature of hydrogen whether it is trapped or diffusible.
A computer model was developed to simulate the thermal desorption flux of hydrogen from steel specimens by an explicit finite difference method, which is convergent and stable for all time increment. The influences of experimental parameters, e.g. ramp rate, specimen size and duration of exposure at ambient temperature etc., on the desorption spectrum, concentration profile of hydrogen in the lattice and fractional occupancy at the trapping sites, were studied assuming that the major trapping sites were dislocations. The increase in ramp rate caused a marked shift in the desorption peak to a higher temperature, whilst the increase in the specimen size shifted the peak to higher temperatures to a moderate extent. The duration of exposure may have a considerable influence on the thermal desorption spectra when the desorption peak is associated with a lower binding energy trap site.
Thermal desorption analyses (TDA) were conducted in high strength martensitic steels containing carbon from 0.33 to 1.0 mass pct, which were charged with hydrogen at 1223 K (950°C) under hydrogen of one atmospheric pressure and quenched to room temperature. In 0.33C steel, which had the highest M s temperature, only one desorption peak was observed around 373 K (100°C), whereas two peaks, one at a similar temperature and the other around and above 573 K (300°C), were observed in the other steels, the height of the second peak increasing with carbon content. In 0.82C steel, both peaks disappeared during exposure at room temperature in 1 week, whereas the peak heights decreased gradually over 2 weeks in specimens electrolytically charged with hydrogen and aged for varying times at room temperature. From computer simulation, by means of the McNabb-Foster theory coupled with theories of carbon segregation, these peaks are likely to be due to trapping of hydrogen in the strain fields and cores of dislocations, and presumably to a lesser extent in prior austenite grain boundaries. The results also indicate that carbon atoms prevent and even expel hydrogen from trapping sites during quenching and aging in these steels.
Resistance to hydrogen embrittlement of low alloy steels was evaluated based on their critical hydrogen content and critical stress. Constant load test (CLT), Slow Strain Rate Test (SSRT) and Conventional Strain Rate Test (CSRT) were carried out using JIS-SCM435 and V-added steels in six laboratories. It was confirmed that the same test results were obtained in different laboratories under the same test conditions. Furthermore, the relationships between diffusible hydrogen content and nominal fracture stress obtained by means of CLT and SSRT were similar to each other. In CSRT, the nominal fracture stress was higher than that in CLT and SSRT under the same absorbed hydrogen content in the specimens. In SSRT and CSRT, fracture surfaces showed Quasi-cleavage mode under small hydrogen content, while they showed Inter-granular fracture under large hydrogen content. In order to compare the three methods considering the concentration of hydrogen in stress field, locally accumulated hydrogen content under the same fracture stress is calculated. The locally accumulated hydrogen under the same applied stress, in other words, critical hydrogen content to hydrogen embrittlement, is the following order; SSRT < CLT < CSRT in JIS-SCM435, and CSRT < CLT ≒ SSRT in V-added steels.
Transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) enable the visualization of three-dimensional (3D) microstructures ranging from atomic to micrometer scales using 3D reconstruction techniques based on computed tomography algorithms. This 3D microscopy method is called electron tomography (ET) and has been utilized in the fields of materials science and engineering for more than two decades. Although atomic resolution is one of the current topics in ET research, the development and deployment of intermediate-resolution (non-atomic-resolution) ET imaging methods have garnered considerable attention from researchers. This research trend is probably not irrelevant due to the fact that the spatial resolution and functionality of 3D imaging methods of scanning electron microscopy (SEM) and X-ray microscopy have come to overlap with those of ET. In other words, there may be multiple ways to carry out 3D visualization using different microscopy methods for nanometer-scale objects in materials. From the above standpoint, this review paper aims to (i) describe the current status and issues of intermediate-resolution ET with regard to enhancing the effectiveness of TEM/STEM imaging and (ii) discuss promising applications of state-of-the-art intermediate-resolution ET for materials research with a particular focus on diffraction contrast ET for crystalline microstructures (superlattice domains and dislocations) including a demonstration of in situ dislocation tomography.
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