Bottom-up Au electroplating of high-aspect-ratio Si-based X-ray microgratings

High-aspect-ratio Au microgratings are critical optical components for grating based X-ray interferometry, which we recently demonstrated to be more dose efficient than conventional computer tomography in imaging of human breast under close-to-clinical condition. High quality dense gratings (50% duty cycle) on large area (4-inch wafers at least) are needed for this medical application. Silicon-based manufacturing allows high precision pattern definition by lithographic techniques and high-aspect-ratio silicon template fabrication by pattern transfer methods such as deep reactive ion etching . Uniform and voids-free gold filling of the high aspect ratio silicon trenches is the final step of our grating microfabrication. 

The electrolytes [1-3] used for Au bottom-up-fill (BUF) are simple and nontoxic, containing Na3Au(SO3)2, Na2SO3, and micromolar concentrations of Bi3+ additiveA typical BUF goes through an incubation period, Bi-activated local deposition at the bottom, sustained bottom-up filling, and self-passivation [1-2]. High-aspect-ratio void-free Au BUF can be realized by controlling the solution concentration and pH, as well as the plating potential. Au BUF can also be realized in bent gratings attached to curved holders, reducing the elastic strains with respect to planar gratings bent to the same radius [3]. 

We systematically investigated the process reproducibility and the filling quality. Void-free BUF of high-aspect-ratio gratings is challenging because deposition on the sidewalls can happen during active filling, causing truncated BUF. Electroplating parameters need to be adjusted in accord with the feature dimensions. We successfully filled Au microgratings with various feature sizes with pitch ranging from 1 [4] to 5 µm [3], and we are challenging ourselves with uniform filling in more extreme structures (submicron pitch and aspect ratio higher than 100) and larger wafer sizes (up to 8-inch wafer scale).

Left: Schematic representation of the electroplating 3-electrode configuration; right: scanning electron microscopic images of cleaved high-aspect-ratio Si-based Au microgratings (Au has brighter contrast than Si)
References
  1. D. Josell, Z. Shi, K. Jefimovs, L. Romano, J. Vila-Comamala, T.P. Moffat, Pushing the Limits of Bottom-Up Gold Filling for X-ray Grating Interferometry, Journal of The Electrochemical Society 167(13) (2020) 132504.
  2. D. Josell, Z. Shi, K. Jefimovs, V.A. Guzenko, C. Beauchamp, L. Peer, M. Polikarpov, T.P. Moffat, Bottom-Up Gold Filling in New Geometries and Yet Higher Aspect Ratio Gratings for Hard X-ray Interferometry, Journal of The Electrochemical Society 168(8) (2021) 082508.
  3. D. Josell, D. Raciti, T. Gnaupel-Herold, A. Pereira, V. Tsai, Q. Yu, L. Chen, M. Stauber, M. Rawlik, M. Stampanoni, T.P. Moffat, L. Romano, Bottom-up Gold Filling of Trenches in Curved Wafers, Journal of The Electrochemical Society 171(3) (2024) 032502.
  4. C. Organista, R. Tang, Z. Shi, K. Jefimovs, D. Josell, L. Romano, S. Spindler, P. Kibleur, B. Blykers, M. Stampanoni, M.N. Boone, Implementation of a dual-phase grating interferometer for multi-scale characterization of building materials by tunable dark-field imaging, Scientific Reports 14(1) (2024) 384.
Collaboration
  • Dr. Konstantins Jefimovs, Paul Scherrer Institute, 5232 Villigen, Switzerland
  • Dr. Martin Stauber, GratXray, PARK innovAARE, 5234 Villigen, Switzerland
  • Dr. Daniel Josell, NIST, Gaithersburg, Maryland 20899, USA
Funding
  • SwissLOS Lottery Fund of Kanton Aargau
  • SNF R’Equip 189662 (SiDRY)
  • SNF R’Equip 177036 (DTL)
Contact
Dr. Liyang Chen, liyang.chen@psi.ch
Dr. Lucia Romano, lucia.romano@psi.ch, +41 56 310 56 88