The key optical components of X-ray grating interferometry are gratings, whose profile requirements play the most critical role in acquiring high quality images. The difficulty of etching grating lines with high aspect ratios when the pitch is in the range of a few micrometers has greatly limited imaging applications based on X-ray grating interferometry. A high etching rate with low aspect ratio dependence is crucial for higher X-ray energy applications and good profile control by deep reactive ion etching of grating patterns. To achieve this goal, a modified Coburn–Winters model was applied in order to study the influence of key etching parameters, such as chamber pressure and etching power. The recipe for deep reactive ion etching was carefully fine-tuned based on the experimental results. Silicon gratings with an area of 70 × 70 mm², pitch size of 1.2 and 2 μm were fabricated using the optimized process with aspect ratio α of ~67 and 77, respectively.

The application of superconformal Bi-catalyzed Au electrodeposition for void-free filling of recessed trenches in X-ray gratings used in phase contrast imaging is detailed. Filling of trenches with aspect ratio (height divided by width) up to 55 is demonstrated. Uniform bottom-up filling of patterned trench arrays across 100 mm (4 inch) diameter Si wafer is accomplished using a well-defined hydrodynamic flow field across the wafer surface. The filling process and microstructure are examined by scanning electron microscopy of cross-sectioned specimens. The importance of process optimization, from the design of potential (current) programming to electrolyte pH and concentrations of Na ₃ Au(SO ₃ ) ₂ and Bi ³⁺ , for the filling of high aspect ratio trenches is demonstrated. X-ray phase contrast imaging is used to assay the quality and uniformity of the as-formed gratings as well as demonstrate their application to imaging biological tissue. Successful void-free Au filling of micrometer range pitch, high aspect ratio trenches in Si gratings promises to advance X-ray grating interferometry and its application to X-ray phase contrast imaging.

Refraction-based x-ray imaging can overcome the fundamental contrast limit of computed tomography (CT), particularly in soft tissue, but so far has been constrained to high-dose ex vivo applications or required highly coherent x-ray sources, such as synchrotrons. Here we demonstrate that grating interferometry (GI) is more dose efficient than conventional CT in imaging of human breast under close-to-clinical conditions. Our system, based on a conventional source and commercial gratings, outperformed conventional CT for spatial resolutions better than 263 µm and absorbed dose of 16 mGy. The sensitivity of GI is constrained by grating fabrication, and further progress will lead to significant improvements of clinical CT.

We present a method to produce small pitch gratings for X-ray interferometric imaging applications, allowing the phase sensitivity to be increased and/or the length of the laboratory setup to be minimized. The method is based on fabrication of high aspect ratio silicon microstructures using deep reactive ion etching (Bosch technique) of dense grating arrays and followed by conformal electroplating of Au. We demonstrated that low resistivity Si substrates (<0.01 Ohm·cm) enable the metal seeding layer deposition step to be avoided, which is normally required to initiate the electroplating process. Etching conditions were optimized to realize Si recess structures with a slight bottom tapering, which ensured the void-free Au filling of the trenches. Vapor HF was used to remove the native oxide layer from the Si grating surface prior to electroplating in the cyanide-based Au electrolyte. Fabrication of Au gratings with pitch in the range 1.2–3.0 µm was successfully realized. A substantial improved aspect ratio of 45:1 for a pitch size of 1.2 µm was achieved with respect to the prior art on 4-inch wafer-based technology. The fabricated Au gratings were tested with X-ray interferometers in Talbot–Laue configuration with measured visibility of 13% at an X-ray design energy of 26 keV.

Displacement Talbot lithography can rapidly pattern periodic nanostructures with high depth of focus over large area. Imperfections in the phase mask profile and the stage movement inaccuracies during the exposure cause linewidth variation in every second line of binary gratings. While this beating is barely visible in patterned photoresist, it leads to substantial depth variation when transferred into high aspect ratio silicon structures, because of micro-loading in deep reactive ion etching. A proper scan range compensated the defect, and a beating-free grating with pitch size of 1 μ m and aspect ratio of 54:1 is demonstrated.