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Engineering and direct imaging of nanocube self-assembly pathways

Nature Chemical Engineering volume 1, pages 532–541 (2024)Cite this article

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Abstract

Nanoparticle self-assembly offers a scalable and versatile means to fabricate next-generation materials. The prevalence of metastable and nonequilibrium states during the assembly process makes the final structure and function directly dependent upon formation pathways. However, it remains challenging to steer the assembly pathway of a nanoparticle system toward multiple superstructures while visualizing in situ. Here we use liquid-cell transmission electron microscopy to image complete self-assembly processes of gold nanocubes, a model shape-anisotropic nanocolloidal system, into distinct superlattices. Theoretical analysis and molecular dynamics simulations indicate that the electrostatic screening of the medium dictates self-assembly pathways by its effects on the interactions between nanocubes. We leverage this understanding to demonstrate on-the-fly control of assembly behavior through rapid solvent exchange. Our joint experiment–simulation–theory investigation paves the way for elucidating the relationships among building block attributes, assembly pathways and superstructures in nanoscale assembly and opens new avenues for the bottom-up design of reconfigurable and adaptive metamaterials.

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Fig. 1: Charge screening controls the self-assembly phase behavior of gold nanocubes.
Fig. 2: Self-assembly pathway of gold nanocubes into the RB lattice.
Fig. 3: Self-assembly pathway of gold nanocubes into the HR lattice.
Fig. 4: Self-assembly pathway of gold nanocubes into the SQ lattice.
Fig. 5: Solvent-mediated, reversible structural transitions between the SQ and the RB phases.

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The source data for the figures in the main text are available in Supplementary Information.

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Acknowledgements

X.Y. acknowledge support from the US National Science Foundation under grant numbers DMR-2102526 (nanocrystal synthesis) and CBET-2223453 (LCTEM imaging and data analysis). The theory, modeling and simulation work was supported by a CDS&E grant from the National Science Foundation (NSF), Division of Materials Research award no. DMR 2302470 (S.C.G.). Simulation work used NCSA Delta through allocation DMR 140129 from the Advanced Cyberinfrastructure Coordination Ecosystem: Services & Support (ACCESS) program, which is supported by National Science Foundation grant nos. 2138259, 2138286, 2138307, 2137603 and 2138296. Computational resources and services also provided by Advanced Research Computing (ARC), a division of Information and Technology Services (ITS) at the University of Michigan, Ann Arbor. T.D. acknowledges support from the National Science Foundation Graduate Research Fellowship through grant DGE-1256260.

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Author notes

  1. These authors contributed equally: Yaxu Zhong, Timothy C. Moore, Tobias Dwyer.

Authors and Affiliations

  1. Department of Chemistry, Indiana University, Bloomington, IN, USA

    Yaxu Zhong, Alex Butrum-Griffith, Vincent R. Allen, Jun Chen, Yi Wang, Fanrui Cheng & Xingchen Ye

  2. Department of Chemical Engineering, University of Michigan, Ann Arbor, MI, USA

    Timothy C. Moore, Tobias Dwyer & Sharon C. Glotzer

  3. Biointerfaces Institute, University of Michigan, Ann Arbor, MI, USA

    Sharon C. Glotzer

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  1. Yaxu Zhong
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Contributions

Y.Z. and X.Y. designed the experiments. Y.Z., Y.W. and F.C. performed the experiments. Y.Z., T.C.M., T.D., A.B.-G., V.R.A., J.C. and X.Y. analyzed the experimental data. T.C.M., T.D. and S.C.G. designed the theoretical model and performed the simulations. Y.Z., T.C.M, T.D., J.C., S.C.G. and X.Y. wrote the manuscript. S.C.G. and X.Y. supervised the project. All authors discussed the results and commented on the manuscript.

Corresponding authors

Correspondence to Sharon C. Glotzer or Xingchen Ye.

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Nature Chemical Engineering thanks Taylor Woehl, Petra Kral and Ethayaraja Mani for their contribution to the peer review of this work.

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Supplementary information

Supplementary Information

Supplementary Notes 1–10, Table 1, Figs. 1–23, references and captions for Supplementary Movies 1–14.

Supplementary Video 1

Computational self-assembly of gold nanocubes into a SQ lattice. Particles are colored by their orientations. The animation spans a simulation timescale of 8.7 × 105 \(\tau\).

Supplementary Video 2

Computational self-assembly of gold nanocubes into a RB lattice. Particles are colored by their orientations. The animation spans a simulation timescale of 1.38 × 106 \(\tau\).

Supplementary Video 3

Computational self-assembly of gold nanocubes into a HR phase. Particles are colored by their orientations. The animation spans a simulation timescale of 9.8 × 105 \(\tau\).

Supplementary Video 4

Self-assembly of gold nanocubes into the RB lattice. a, Raw LCTEM movie. b–d, LCTEM movie frames with nanocubes colored according to their orientations (b), nanocube centroids colored according to |\({\psi }_{6j}\)| and all nearest-neighbors connected (c) and nanocube centroids colored according to \(|{\phi }_{4j}\)| (d). e,f, Radial distribution function g(r) plots (e) and FFT patterns of LCTEM movie frames (f). g, 2D scatter plots of the order parameters \(|{\psi }_{6j}|\) and \(|{\phi }_{4j}|\). h, Plots of ensemble-averaged local translational and orientational order parameters \(\left({\rm{\langle }}|{\psi }_{6j}|{\rm{\rangle }},\,{\rm{\langle }}|{\phi }_{4j}|{\rm{\rangle }}\right)\) versus time. Dose rate: 14.0 e− Å−2 s−1. The frame rates are 15 fps (15 times faster than real time).

Supplementary Video 5

Movement of a twin boundary in the RB lattice through collective rotation of nanocubes. LCTEM movie frames with nanocubes colored according to their orientations (top) and nanocube centroids colored according to \(|{\psi }_{6j}|\) (bottom). Dose rate: 14.0 e− Å−2 s−1. The frame rates are 5 fps (five times faster than real time).

Supplementary Video 6

Self-assembly of gold nanocubes into the HR lattice. a, Raw LCTEM movie. b–d, LCTEM movie frames with nanocubes colored according to their orientations (b), nanocube centroids colored according to \(\left|{\psi }_{6j}\right|\) and all nearest-neighbors connected (c) and nanocube centroids colored according to \(\left|{\phi }_{4j}\right|\) (d). e,f, Radial distribution function g(r) plots (e) and FFT patterns of LCTEM movie frames (f). g, 2D scatter plots of the order parameters \(\left|{\psi }_{6j}\right|\) and \(\left|{\phi }_{4j}\right|\). h, Plots of ensemble-averaged local translational and orientational order parameters \(\left(\left\langle \left|{\psi }_{6j}\right|\right\rangle ,\,\left\langle \left|{\phi }_{4j}\right|\right\rangle \right)\) versus time. Dose rate: 14.0 e− Å−2 s−1. The frame rates are 15 fps (15 times faster than real time).

Supplementary Video 7

Self-assembly of gold nanocubes into the SQ lattice. a, Raw LCTEM movie. b–d, LCTEM movie frames with nanocubes colored according to their orientations (b), nanocube centroids colored according to \(\left|{\psi }_{4j}\right|\) and all nearest-neighbors connected (c) and nanocube centroids colored according to \(\left|{\phi }_{4j}\right|\) (d). e,f, Radial distribution function g(r) plots (e) and FFT patterns of LCTEM movie frames (f). g, 2D scatter plots of the order parameters \(\left|{\psi }_{4j}\right|\) and \(\left|{\phi }_{4j}\right|\). h, Plots of ensemble-averaged local translational and orientational order parameters \(\left(\left\langle \left|{\psi }_{4j}\right|\right\rangle ,\,\left\langle \left|{\phi }_{4j}\right|\right\rangle \right)\) versus time. Dose rate: 14.0 e− Å−2 s−1. The frame rates are 15 fps (15 times faster than real time).

Supplementary Video 8

Detachment of the SQ superlattice from the Si3N4 window. Dose rate: 14.0 e− Å−2 s−1. The frame rates are 15 fps (15 times faster than real time).

Supplementary Video 9

Vacancy formation and vacancy removal pathways for the HR, RB and SQ superlattices. Dose rate: 14.0 e− Å−2 s−1 for all three movies. The frame rates are 5 fps (real time).

Supplementary Video 10

Solvent-mediated reversible structural transitions between the SQ and the RB phases. a, Raw LCTEM movie. b–d, LCTEM movie frames with nanocubes colored according to their orientations (b), nanocube centroids colored according to \(\left|{\psi }_{6j}\right|\) and all nearest-neighbors connected (c) and nanocube centroids colored according to \(\left|{\phi }_{4j}\right|\) (d). e,f, Radial distribution function g(r) plots (e) and FFT patterns of LCTEM movie frames (f). g, 2D scatter plots of the order parameters \(\left|{\psi }_{6j}\right|\) and \(\left|{\phi }_{4j}\right|\). h, Plots of ensemble-averaged local translational and orientational order parameters \(\left(\left\langle \left|{\psi }_{6j}\right|\right\rangle ,\,\left\langle \left|{\phi }_{4j}\right|\right\rangle \right)\) versus time. Dose rate: 14.0 e− Å−2 s−1. The frame rates are 15 fps (15 times faster than real time).

Supplementary Video 11

Simulated structural transition from the SQ lattice to the RB lattice induced by a change in the screening length. Particles are colored by their orientations. The animation spans a simulation timescale of 2.0 × 105 \(\tau\).

Supplementary Video 12

Simulated structural transition from the RB lattice to the SQ lattice induced by a change in the screening length. Particles are colored by their orientations. The animation spans a simulation timescale of 2.0 × 105 \(\tau\). Note that the time period between snapshots is not constant throughout the movie; the period between snapshots is \(\tau /\updelta t=10\) when \(\tau /\updelta t >\) 1,000, 10,000 when \(\text{1,000}\le \tau /\updelta t < 1\times {10}^{6}\), and 50,000 when \(\tau /\updelta t\ge 1\times {10}^{6}\).

Supplementary Video 13

Melting of the RB lattice induced by changing the solvent from medium-polarity (1:1 v/v octane:butanol) to low-polarity one (4:1 v/v octane:butanol). a, Raw LCTEM movie. b–d, LCTEM movie frames with nanocubes colored according to their orientations (b), nanocube centroids colored according to \(\left|{\psi }_{6j}\right|\) and all nearest-neighbors connected (c) and nanocube centroids colored according to \(\left|{\phi }_{4j}\right|\) (d). e,f, Radial distribution function g(r) plots (e) and FFT patterns of LCTEM movie frames (f). g, 2D scatter plots of the order parameters \(\left|{\psi }_{6j}\right|\) and \(\left|{\phi }_{4j}\right|\). h, Plots of ensemble-averaged local translational and orientational order parameters \(\left(\left\langle \left|{\psi }_{6j}\right|\right\rangle ,\,\left\langle \left|{\phi }_{4j}\right|\right\rangle \right)\) versus time. Dose rate: 14.0 e− Å−2 s−1. The frame rates are 15 fps (15 times faster than real time).

Supplementary Video 14

Structural transition from the SQ to the RB lattice induced by changing the solvent from high-polarity (butanol) to medium-polarity one (1:1 v/v octane:butanol). A different pathway from the one shown in Fig. 5 was observed that involved continuous lattice distortion through collective rotation of AuNCs without losing orientational order. Dose rate: 14.0 e− Å−2 s−1. The frame rates are 15 fps (15 times faster than real time).

Supplementary Data 1

Source images for Figs. 1–5.

Source data

Source Data Fig. 1

Numerical data points for Fig. 1f (makers).

Source Data Fig. 2

Numerical data points for Fig. 2d–h.

Source Data Fig. 3

Numerical data points for Fig. 3c–g.

Source Data Fig. 4

Numerical data points for Fig. 4c,d,e,g,h.

Source Data Fig. 5

Numerical data points for Fig. 5c–g,i,k.

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Zhong, Y., Moore, T.C., Dwyer, T. et al. Engineering and direct imaging of nanocube self-assembly pathways. Nat Chem Eng 1, 532–541 (2024). https://doi.org/10.1038/s44286-024-00102-9

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