An experimental heat treatment chamber and control system were developed to perform in-situ X-ray diffraction experiments during low-pressure carburizing (LPC) processes. Results from the experimental chamber and industrial furnace were compared, and it was proven that the built system is reliable for LPC experiments. In-situ X-ray diffraction investigations during LPC treatment were conducted at the German Electron Synchrotron Facility in Hamburg Germany. During the boost steps, carbon accumulation and carbide formation was observed at the surface. These accumulation and carbide formation decelerated the further carbon diffusion from atmosphere to the sample. In the early minutes of the diffusion steps, it is observed that cementite content continue to increase although there is no presence of gas. This effect is attributed to the high carbon accumulation at the surface during boost steps which acts as a carbon supply. During quenching, martensite at higher temperature had a lower c/a ratio than later formed ones. This difference is credited to the early transformation of austenite regions having lower carbon content. Also, it was noticed that the final carbon content dissolved in martensite reduced compared to carbon in austenite before quenching. This reduction was attributed to the auto-tempering effect.
In situ X‐ray diffraction experiments during low‐pressure carburizing processes are performed at the German Electron Synchrotron Facility, Beamline P07, in Hamburg, Germany, with a specially developed process chamber. Microstructural evolution is precisely analyzed based on diffraction data, and several process parameters are varied. The investigations focus on boost and diffusion steps in which carbon donor gas interacts with the hot steel surface and carbon atoms diffuse through the sample. An increased process temperature leads to higher carbon absorption during the boost step, especially at the early stages of the process. Regardless of process parameters, austenite saturation is reached in a few seconds. Therefore, longer boost step duration and/or a higher acetylene amount does not directly increase the carbon profile; instead, this would only increase the amount of carbides formed on the surface, which would contribute to the carbon profile by dissolution in the following steps. Therefore, shorter and a high number of boost steps are recommended for high efficiency. The cementite formation rate shows a similar trend with austenite saturation. It is very fast at the beginning and then stays almost constant. Therefore, introducing acetylene to the furnace after that point has no positive effect on the carburization.
Low-pressure carburizing (LPC) is a recipe-controlled process for surface layer hardening. These recipes are mainly based on experience and contain the process parameters used to achieve the desired hardening result. The process parameters influence the chemical gradients which have set in the boundary layer, the local microstructure and the depth distribution of the process-induced residual stresses. Within the scope of this work, a systematic parameter study and advanced characterization was carried out to quantify the influence of these process parameters on the resulting material state. The varied parameters include the carburizing temperature, the hardening temperature, the quenching rate as well as the number of repetitions and durations of the carburizing cycles’ steps. The results obtained should help to extend the fundamental process understanding of the LPC process. The analyses showed that the retained austenite content and its depth profile change significantly for certain process parameter variations, reaching contents of up to 45 vol% in the near-surface region. The differences regarding the residual stress states of the case-hardened samples can first and foremost be related to the formation of varying depth distributions of the retained austenite.
In situ X-ray diffraction investigations during low pressure carburizing (LPC) processes were performed with a specially developed process chamber at the German Electron Synchrotron Facility (DESY) in Hamburg, Germany. Carbon saturation in austenite was reached in less than 20 seconds for all processes with different parameters and carbides formed at the surface. Therefore, the direct contribution of carbon donor gas to the carbon profile after 20 seconds was reduced to very low levels. After that point, further supply of carbon donor gas increased the amount of carbides formed at the surface, which will contribute to the carbon profile indirectly by dissolution in the following diffusion steps. During quenching, martensite at higher temperatures had a lower c/a ratio than later formed ones. This difference is credited to self-tempering effects and reordering of carbon atoms within the martensite lattice.
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