S3DXRD evolved from box-beam 3DXRD, which was pioneered by Henning Friis Poulsen, a physicist at the Technical University of Denmark (DTU). The technique involves placing a large, 2D area detector close to a rotating sample, and collecting thousands of diffraction spots from different crystal planes while being scanned by a nanofocused X-ray beam.

Although the essential hardware for S3DXRD has been at ID11 for several years, the beamline recently had a diffractometer upgrade that allows the scanning of larger samples, with 25 times faster acquisition overall. With the addition of some custom data-analysis code, says James Ball, an ID11 postdoc, “we’re now routinely producing very high-quality grain maps within a few hours of collection.” This is particularly relevant to components made by additive manufacturing (AM), because the microstructures are so complex, Ball adds. “I would say this sets a new standard for how to analyse AM materials with S3DXRD.”

For the study, a group led by Yunhui Chen at RMIT University in Melbourne, Australia, produced a nickel superalloy via an AM technique known as directed energy deposition, in which a laser forms components according to a digital design, melting metal powder as it is deposited layer by layer. The technique is particularly useful in the repair of high-value engineering components, but the fast solidification – 1000 times faster than traditional alloy manufacturing – can result in an uneven structure, with long grains crossed by a honeycomb network of microscopic cell walls, and dotted with carbides in a primary cubic metal phase. In collaboration with scientists at the University of Cambridge and the University of Birmingham in the UK, and the University of Kassel in Germany, Ball and other ESRF scientists used S3DXRD to non-destructively map the orientation, strain, and stress of a sample of the alloy, tracking more than 37,000 individual carbides alongside 82 nickel grains at 200 nm resolution.

The results showed that the carbides cluster along the cell walls, where elements such as titanium and niobium accumulate during the rapid cooling. Unlike the surrounding metal, these regions form internal stress patterns that could change the mechanical properties of the material. According to Ball, the findings offer manufacturers new insights into how printing conditions shape internal architecture, potentially showing how to improve the durability of AM superalloy components.

“We’re really starting to establish ourselves in the AM community,” says Ball. “One could imagine many types of experiments – for example, evaluating choices of processing parameters in terms of the resultant residual strain fields. S3DXRD data is very rich and we’re only scratching the surface of what we can extract, even from old datasets. We’re working hard to push the field even further.”

The technique goes beyond AM, however, being applicable to any study involving the mapping of crystalline orientation or strain in bulk materials. There is also the possibility of in situ experiments during tensile deformation, nano-indentation and heating or cooling, as well as complementary data from dark-field X-ray microscopy (DFXM), which images a single diffraction spot from a single crystal grain at high spatial resolution. “The ideal experiment uses both: S3DXRD to capture mesoscale information about an entire layer of a sample, and then DFXM to ‘zoom in’ to image dislocation structures at the highest resolutions,” says Ball.

Whatever the application, however, the message is that S3DXRD has come of age, he says. “Instead of looking at chemistry, crystal orientations or residual strains separately, we can now see all three at once.”

Reference:

Ball, J.A.D., Collins, D.M., Tang, Y.T. et al. Revealing 3D strain and carbide architectures in additively manufactured Ni superalloys. Nat Commun (2026). https://doi.org/10.1038/s41467-026-77198-5

Text by Jon Cartwright

Top image: Reconstructed S3DXRD volume, γ phase, coloured by grain-averaged orientations (IPF-Z) showing the columnar as-printed microstructure.