Crystallographic characterization of steel microstructure using neutron diffraction.

Applications of neutron diffraction to microstructure evaluation of steel investigated by a project commissioned by the Innovative Structural Materials Association are summarized. The volume fraction of austenite (γ) for a 1.5Mn-1.5Si-0.2C steel was measured by various techniques including backscatter electron diffraction (EBSD) and X-ray diffraction. It is recommended to measure volume fraction and texture simultaneously using neutron diffraction. The γ reverse transformation was in situ monitored using dilatometry, EBSD, X-ray diffraction and neutron diffraction. The γ reversion kinetics showed excellent agreements between dilatometry and neutron diffraction, whereas the γ formation started at higher temperatures in EBSD and X-ray diffraction measurements. Such discrepancy is attributed to the change in chemical compositions at the specimen surface by heating; Mn and C concentrations were decreased with heating. Phase transformations from γ upon cooling were monitored, which enabled us to elucidate the changes in lattice parameters of ferrite (α) and γ affected by not only thermal contraction but also transformation strains, thermal misfit strains and carbon enrichment in γ in the above hypoeutectoid steel. Pearlitic transformation started after the carbon enrichment reached approximately 0.76 mass% and contributed to diffraction line broadening. Martensitic transformation with or without ausforming at 700°C was monitored for a medium carbon low alloyed steel. Dislocation density after ausforming was determined using the convolutional multiple whole profile fitting method for 10 s time-sliced data. The changes in γ and martensite lattice parameters upon quenching were tracked and new insights on internal stresses and the axial ratio of martensite were obtained.

Neutron Bragg-edge transmission imaging for microstructure and residual strain in induction hardened gears.

A time-of-flight Bragg-edge neutron transmission imaging was used to investigate the microstructure and strain distributions in a gear hardened by a newly developed two-step induction-heating method: precursor (Sample 1) and final product (Sample 2). The edge-position and edge-broadening were determined and mapped with high spatial resolution, which enabled us to confirm the two-dimensional distributions of the microstructure and residual strain. A deep hardened layer was made for Sample 1 in which martensite was formed on the entire teeth and the outer peripheral portion of the gear body. Sample 2 was subjected to double induction-hardening, where a tempered martensite was formed as the thermal refined microstructure between a fine-grained martensite at the tooth surface and a ferrite-pearlite microstructure at the core. The relationship between edge-broadening and the Vickers hardness described by a linear equation was employed to derive the elastic residual strain. The residual strain map for Sample 2 revealed that a steep compressive strain was introduced into the fine-grained martensite at the tooth surface by the super rapid induction-heating and quenching process. The reversal of tension was speculated to occur below 2 mm from the tooth tip, and the strain was almost zero in the core region.

High stereographic resolution texture and residual stress evaluation using time-of-flight neutron diffraction.

Neutron diffraction texture measurements provide bulk averaged textures with excellent grain orientation statistics, even for large-grained materials, owing to the probed volume being of the order of 1 cm3. Furthermore, crystallographic parameters and other valuable microstructure information such as phase fraction, coherent crystallite size, root-mean-square microstrain, macroscopic or intergranular strain and stress, etc. can be derived from neutron diffractograms. A procedure for combined high stereographic resolution texture and residual stress evaluation was established on the pulsed-neutron-source-based engineering materials diffractometer TAKUMI at the Materials and Life Science Experimental Facility of the Japan Proton Accelerator Research Center, through division of the neutron detector panel regions. Pole figure evaluation of a limestone standard sample with a well known texture suggested that the precision obtained for texture measurement is comparable to that of the established neutron beamlines utilized for texture measurement, such as the HIPPO diffractometer at the Los Alamos Neutron Science Center (New Mexico, USA) and the D20 angle-dispersive neutron diffractometer at the Institut Laue-Langevin (Grenoble, France). A high-strength martensite-austenite multilayered steel was employed for further verification of the reliability of simultaneous Rietveld analysis of multiphase textures and macro stress tensors. By using a texture-weighted geometric mean micromechanical (BulkPathGEO) model, a macro stress tensor analysis with a plane stress assumption showed a rolling direction-transverse direction (RD-TD) in-plane compressive stress (about -330 MPa) in the martensite layers and an RD-TD in-plane tensile stress (about 320 MPa) in the austenite layers. The phase stress partitioning was ascribed mainly to the additive effect of the volume expansion during martensite transformation and the linear contraction misfit between austenite layers and newly transformed martensite layers during the water quenching process.