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Dark-field TEM imaging of stacking domains

Created 11 days ago

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Dark-field transmission electron microscopy (DF-TEM) images a sample using only electrons diffracted into a chosen Bragg reflection, selected by an aperture in the diffraction plane. For bilayers it provides direct, large-area maps of stacking domains and domain walls with nanometre resolution [1; 2].

How it distinguishes domains. For Bernal bilayer graphene, the first-order $\{10\bar10\}$ reflections have intensities that differ between AB and BA when the sample is tilted, so AB and BA appear light and dark. Second-order $\{2\bar1\bar10\}$ reflections are insensitive to AB vs BA but darken where the stacking deviates — at walls — and each of the three reflections highlights walls with a particular Burgers-vector direction (the wall is invisible when $\mathbf g\cdot\Delta\mathbf u=0$ modulo $2\pi$) [1, Fig. 1c-d].

What it revealed. Triangular networks of AB/BA domains in CVD bilayer graphene, the shear/tensile character of walls, topological nodes, and — through in-situ heating to 1000–1200 °C and beam exposure — soliton motion, straightening and pairwise annihilation [1, Fig. 4].

Successors. DF-TEM of twisted bilayers established the angle-dependent reconstruction crossover [3]; atomic-resolution STEM resolves wall structure; 4D-STEM Bragg interferometry quantifies local stacking, rotation and strain [4; 5]. Complementary probes include conductive and piezoresponse AFM [6] and STM.

Limits. Contrast is influenced by out-of-plane corrugation and by additional layers; samples must be suspended and electron-transparent, and high beam doses can move walls.

Also known as: DF-TEM, dark-field electron microscopy

References

  1. Alden et al. (2013). Strain solitons and topological defects in bilayer graphene. PNAS 110, 11256. https://arxiv.org/abs/1304.7549
  2. Brown et al. (2012). Twinning and twisting of tri- and bilayer graphene. Nano Lett. 12, 1609. https://doi.org/10.1021/nl204547v
  3. Yoo et al. (2019). Atomic and electronic reconstruction at the van der Waals interface in twisted bilayer graphene. Nat. Mater. 18, 448. https://arxiv.org/abs/1804.03806
  4. Kazmierczak et al. (2021). Strain fields in twisted bilayer graphene. Nat. Mater. 20, 956. https://arxiv.org/abs/2008.09761
  5. Van Winkle et al. (2023). Rotational and dilational reconstruction in transition metal dichalcogenide moiré bilayers. Nat. Commun. 14, 2989. https://arxiv.org/abs/2212.07006
  6. McGilly et al. (2020). Visualization of moiré superlattices. Nat. Nanotechnol. 15, 580. https://doi.org/10.1038/s41565-020-0708-3

Explanation-DAG node dftem · from: alden2013, yoo2019, weston2022 · Alden et al. 2013, Methods; Article copied from v05_woods2014 (dftem); Article copied from v18_wang2022fe (dftem)