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High-performance 4-nm-resolution X-ray tomography using burst ptychography

Nature volume 632, pages 81–88 (2024)Cite this article

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Abstract

Advances in science, medicine and engineering rely on breakthroughs in imaging, particularly for obtaining multiscale, three-dimensional information from functional systems such as integrated circuits or mammalian brains. Achieving this goal often requires combining electron- and photon-based approaches. Whereas electron microscopy provides nanometre resolution through serial, destructive imaging of surface layers1, ptychographic X-ray computed tomography2 offers non-destructive imaging and has recently achieved resolutions down to seven nanometres for a small volume3. Here we implement burst ptychography, which overcomes experimental instabilities and enables much higher performance, with 4-nanometre resolution at a 170-times faster acquisition rate, namely, 14,000 resolution elements per second. Another key innovation is tomographic back-propagation reconstruction4, allowing us to image samples up to ten times larger than the conventional depth of field. By combining the two innovations, we successfully imaged a state-of-the-art (seven-nanometre node) commercial integrated circuit, featuring nanostructures made of low- and high-density materials such as silicon and metals, which offer good radiation stability and contrast at the selected X-ray wavelength. These capabilities enabled a detailed study of the chip’s design and manufacturing, down to the level of individual transistors. We anticipate that the combination of nanometre resolution and higher X-ray flux at next-generation X-ray sources will have a revolutionary impact in fields ranging from electronics to electrochemistry and neuroscience.

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Fig. 1: Illustration of experimental instabilities and burst data acquisition.
Fig. 2: Burst ptychography data reconstruction workflow.
Fig. 3: Comparison of transistor images obtained by X-ray imaging and electron microscopy.
Fig. 4: Structural analysis of the FinFET transistor layer.
Fig. 5: Quantitative composition characterization of the integrated circuit.

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Data availability

Recorded diffraction patterns, reconstructed ptychographic projections, reconstructed tomograms and accompanying codes are available at https://doi.org/10.16907/33321c7a-f6bf-441e-8ae4-3f4cabd2dc0d.

Code availability

Standalone codes are available at https://doi.org/10.16907/4c56cb87-d73f-402d-96c9-d5e6736fc8a3.

Change history

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Acknowledgements

Tomography experiments were performed at the coherent small-angle X-ray scattering (cSAXS) beamline, located at the Swiss Light Source of the Paul Scherrer Institut in Villigen PSI, Switzerland. We thank S. Stutz for his support with sample preparation; and C. Appel and J. Ihli for discussions regarding quantitative data interpretation. The STEM/EDX analysis and preparation of the pillar-specimen and lamella for electron microscopy was carried out at the Electron Microscopy Facility at PSI. We thank A. Kubec and XRnanotech for support and manufacturing of the aberrated Fresnel zone plates. The work of T.A. is supported by funding from the Swiss National Science Foundation (SNF), project number 200021_196898. N.W.P. has received funding from the European Union’s Horizon 2020 research and innovation programme under the Marie Skłodowska-Curie grant agreement number 884104. G.A. is supported by the European Research Council under the European Union’s Horizon 2020 research and innovation programme, within the Hidden, Entangled and Resonating Order (HERO) project with grant agreement 810451. The transmission electron microscopy/STEM was co-funded by SNF R’Equip Project 206021_177020.

Author information

Author notes

  1. Nicholas W. Phillips

    Present address: Mineral Resources, CSIRO, Clayton, Victoria, Australia

Authors and Affiliations

  1. Paul Scherrer Institute, Villigen, Switzerland

    Tomas Aidukas, Nicholas W. Phillips, Ana Diaz, Emiliya Poghosyan, Elisabeth Müller, Gabriel Aeppli, Manuel Guizar-Sicairos & Mirko Holler

  2. Department of Electrical and Computer Engineering, University of Southern California, Los Angeles, CA, USA

    A. F. J. Levi

  3. Department of Physics, Eidgenössische Technische Hochschule Zürich (ETH Zürich), Zurich, Switzerland

    Gabriel Aeppli

  4. Institute of Physics, École Polytechnique Fédérale de Lausanne (EPFL), Lausanne, Switzerland

    Gabriel Aeppli & Manuel Guizar-Sicairos

  5. Quantum Center, Eidgenössische Technische Hochschule Zürich (ETH Zürich), Zurich, Switzerland

    Gabriel Aeppli

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Contributions

M.H., A.D., M.G.-S., G.A., T.A. and A.F.J.L. conceptualized the project. M.H., N.W.P., M.G.-S. and T.A. carried out the PXCT experiments. T.A., M.H., M.G.-S., N.W.P., G.A. and A.D. interpreted the results. E.M. and E.P. prepared the electron microscopy samples. E.P. collected and analysed the high-resolution STEM and EDX data. T.A. and M.G-.S. developed the computational reconstruction methods and T.A. implemented them into PtychoShelves. T.A. reconstructed the projections and tomograms. T.A. made the figures and videos. All authors contributed to the writing of the paper.

Corresponding authors

Correspondence to Tomas Aidukas or Mirko Holler.

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Extended data figures and tables

Extended Data Fig. 1 Electron microscopy images of the integrated circuit sample.

a,b, Image of the sample prepared using FIB-SEM. The high-resolution image in c was obtained using HAADF STEM. The HAADF STEM image is from a different sample than the one shown in a,b.

Extended Data Fig. 2 Experimental setup geometry and sample scanning stability.

a, Experimental setup geometry used for the ptychographic imaging. The 0.7 μm diameter X-ray beam was created by placing the sample 0.1 mm away from focus (focal length of the Fresnel zone plate is 37.5 mm). Light scattered by the sample propagates through a 0.8 m long evacuated flight tube towards an in-vacuum EIGER detector. b, Average sample scanning stability at every scan position measured by an interferometer operating at 3.5 kHz. The instabilities are plotted as standard deviations from the mean nominal position. During the acquisition of a single projection, the average instability was only up to 4 nm, below the imaging resolution of 4.2 nm.

Extended Data Fig. 3 Burst ptychography data reconstruction pipeline.

a, For computationally efficient burst frame processing, the recorded burst frame area is cropped. b, Next, position refinement is performed on all burst frames to recover the refined positions of the object relative to the probe for each burst frame. In the presence of semi-repeatable instabilities, a low-rank constraint using singular value decomposition (SVD) is imposed to aid convergence of problematic scan areas. c, Once refined positions are identified, the matching burst-frames are summed to increase the SNR of the frames and decrease the computational burden.

Extended Data Fig. 4 Extended depth-of-field tomography using filtered back-propagation.

a, Rendering of the tomogram’s transistor layer, which was reconstructed using the filtered back-propagation tomography algorithm to extend the depth-of-field. This method ensures uniform image quality across the entire volume, as illustrated in b, whereas with conventional back-projection reconstruction image quality notably diminishes beyond a depth of field of 0.5 μm, as demonstrated in c.

Extended Data Fig. 5 Reconstruction quality evaluation between burst and non-burst ptychography.

Comparison between burst ptychography in a and mixed-state ptychography in b shows that the gates and contacts at the transistor layer are well resolved with burst ptychography, which is not the case when using mixed-state ptychography. This discrepancy indicates that the additional probe modes in mixed-state ptychography are trying to account for the unknown instabilities, which were recovered with burst ptychography and are shown for a single scan position in c (taken from Fig. 2). Additionally, the main probe mode power of burst ptychography in d is 93%, whereas for mixed-state ptychography in e it is only 43%.

Extended Data Fig. 6 Integrated circuit elemental composition analysis using EDX.

a, Throughout the IC, the most abundant elements are Cu (for the interconnects) and Si, O for the surrounding dielectric. The concentration of O is higher at the global interconnect layer compared to the other layers, indicating the presence of two dielectric materials which are separated by dashed lines. b, Increased magnification within the non-global layers shows material differences between the interconnect and transistor layers. The element concentration is plotted on a relative scale, in arbitrary units, with respect to each other.

Extended Data Fig. 7 Transistor elemental composition analysis using EDX.

EDX analysis of the transistor layer perpendicular to the fin direction. Source/drain contacts contain mostly Co, while the gates consist of Ti and Al. There is a significant concentration of Si between the interconnects and contacts/gates. The element concentration is plotted on a relative scale, in arbitrary units, with respect to each other.

Extended Data Fig. 8 Resolution analysis using FSC and edge profiles.

a, Fourier shell correlation (FSC) of the reconstructed tomogram showing a pixel-limited half-pitch resolution of 4.2 nm. b, Copper interconnects were used for edge profile analysis in c, which supports the half-pitch resolution estimation by FSC based on the 25-75 edge criterion.

Extended Data Fig. 9 Rendering of the sample’s transistor layer.

Top view of the transistor layer, where the “unit cell” element is repeated throughout the whole layer. See Supplementary Videos 3–4 for a 3D visualization of the transistor layer and the unit cell.

Supplementary information

Supplementary Video 1

Beam instabilities observed in recorded data. This video illustrates the beam instabilities detected within the recorded diffraction patterns of a stationary sample. It shows 23 burst frames, each captured with an 8-ms exposure time.

Supplementary Video 2

Rendering of the integrated circuit. This video presents a reconstructed tomogram rendering, highlighting the internal structure of the integrated circuit.

Supplementary Video 3

Transistor layer rendering. This video showcases the rendered transistor layer, providing an overview of the transistor layout.

Supplementary Video 4

Unit cell of the transistor layer rendering. This video depicts the rendered unit cell of the transistor layer, offering a close-up view of the transistor layer building blocks.

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Aidukas, T., Phillips, N.W., Diaz, A. et al. High-performance 4-nm-resolution X-ray tomography using burst ptychography. Nature 632, 81–88 (2024). https://doi.org/10.1038/s41586-024-07615-6

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