The martensitic transformation in a high carbon steel was studied by a new experimental approach focusing on the nucleation and growth as well as the variant pairing of the early-formed martensite. A mixed microstructure with tempered early-formed martensite and fresh later-formed martensite was achieved by a heat treatment with an isothermal hold below the martensite start temperature. In-situ high-energy X-ray diffraction showed no further transformation of austenite to ferrite/martensite during the isothermal hold. The tempered early-formed martensite was characterized with a combination of light optical microscopy and local tetragonality determination by electron backscatter diffraction. The characterization allowed qualitative as well as quantitative analysis of the tempered early-formed martensite with regard to the prior austenite grain boundaries (PAGB) and variant pairing. The early-formed martensite was shown to grow predominantly along the PAGBs and clustering was observed indicating an autocatalytic nucleation mechanism. The variant pairing of the early-formed martensite had a stronger plate character compared to the later-formed martensite.

A novel approach for the correlation of local martensite tetragonality determined by electron backscatter diffraction and carbon distribution by atom probe tomography (APT) is presented. The two methods are correlated by site-specific sample preparation for APT based on the local tetragonality. This approach is used to investigate the local carbon distribution in high carbon steel with varying local martensite tetragonality. Regions with low tetragonality show clear agglomeration of carbon based on statistical nearest neighbour (NN) analysis, while regions with high tetragonality show only small elongated agglomerations of carbon and no significant clustering using NN analysis. The APT average bulk carbon content shows no quantitative difference between regions with low and high tetragonality, indicating that no significant long-range diffusion of carbon has taken place.

The impact of cooling rate during high-pressure gas quenching on the fatigue performance of low-pressure carburized spur gears was studied for steel grades 20MnCr5 and 17NiCrMo6-4. The results show an increased fatigue limit by 10 to 11% when applying a slower cooling rate for both steel grades. Moreover, for 20MnCr5 the slower cooled gears show an increase in compressive residual stresses by 130 MPa compared to the faster cooling, although no significant difference was observed for 17NiCrMo6-4. It is also seen that the cooling rate affects the core hardness for both steel grades, while other properties like surface hardness, case-hardness depth and martensite variant pairing were unaffected. The results for the retained austenite content and average martensite unit size show no clear effect of the cooling rate. The possible influence of different carbon distributions after quenching for the two used cooling rates on the carbide precipitation and fatigue limit is discussed.

The martensitic transformation was studied by in situ and ex situ experiments in two high-carbon, 0.54 and 0.74 wt pct C, steels applying three different cooling rates, 15 °C/s, 5 °C/s, and 0.5 °C/s, in the temperature range around Ms, to improve the understanding of the evolution of martensite tetragonality c/a and phase fraction formed during the transformation. The combination of in situ high-energy X-ray diffraction during controlled cooling and spatially resolved tetragonality c/a determination by electron backscatter diffraction pattern matching was used to study the transformation behavior. The cooling rate and the different Ms for the steels had a clear impact on the martensitic transformation with a decrease in average tetragonality due to stronger autotempering for a decreasing cooling rate and higher Ms. A slower cooling rate also resulted in a lower fraction of martensite at room temperature, but with an increase in fraction of autotempered martensite. Additionally, a heterogeneous distribution of martensite tetragonality was observed for all cooling rates.