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Metal-halide porous framework superlattices

Nature volume 638, pages 418–424 (2025)Cite this article

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Abstract

The construction of superlattices with a spatial modulation of chemical compositions allows for the creation of artificial materials with tailorable periodic potential landscapes and tunable electronic and optical properties1,2,3,4,5. Conventional semiconductor superlattices with designable potential modulation in one dimension has enabled high-electron-mobility transistors and quantum-cascade lasers. More recently, a diverse set of superlattices has been constructed through self-assembly or guided assembly of multiscale building units, including zero-dimensional nanoclusters and nanoparticles6,7, one-dimensional nanorods and nanowires8,9, two-dimensional nanolayers and nanosheets10,11,12,13, and hybrid two-dimensional molecular assemblies14,15,16,17. These self-assembled superlattices feature periodic structural modulation in two or three dimensions, but often lack atomic precision owing to the inevitable structural disorder at the interfaces between the constituent units. Here we report a one-pot synthesis of multi-dimensional single-crystalline superlattices consisting of periodic arrangement of zero-, one- and two-dimensional building units. By exploiting zirconium (IV) metal–organic frameworks as host templates for directed nucleation and precise growth of metal-halide sublattices through a coordination-assisted assembly strategy, we synthesize a family of single-crystalline porous superlattices. Single-crystal X-ray crystallography and high-resolution transmission electron microscopy clearly resolve the high-order superlattice structure with deterministic atomic coordinates. Further treatment with selected amine molecules produces perovskite-like superlattices with highly tunable photoluminescence and chiroptical properties. Our study creates a platform of high-order single-crystalline porous superlattices, opening opportunities to tailor the electronic, optical and quantum properties beyond the reach of conventional crystalline solids.

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Fig. 1: Structural characterizations of multi-dimensional PbI2@MOF superlattices.
Fig. 2: Monitoring of the intermediates during the stepwise growth.
Fig. 3: Low-dose cryogenic HR-TEM images of PbI2@MOF superlattices.
Fig. 4: Preparation and optical characterizations of amine-modified perovskite-like PbI2@MOFs superlattices.

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Data availability

Additional single-crystal structures, crystallographic information, powder X-ray diffraction data, high-resolution transmission electron microscopy, scanning electron microscopy and energy-dispersive X-ray spectroscopy data, gas-sorption data, Raman spectra, Fourier transform infrared spectra, diffuse reflectance ultraviolet–visible spectra, X-ray photoelectron spectra, ultrafast transient absorption spectra, electrochemical measurements, optical properties, and theoretical calculations are available in Supplementary Information. The X-ray crystallographic structures reported in this article have been deposited at the Cambridge Crystallographic Data Centre (CCDC) with deposition numbers CCDC 2325593, 2325596–2325598, 2325600–2325609, 2325611, 2325612, 2369934–2369944 and 2377565. Source data are provided with this paper.

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Acknowledgements

We thank the staff from BL17B beamlines of the National Facility for Protein Science in Shanghai (NFPS) at the Shanghai Synchrotron Radiation Facility, for assistance during data collection; and D. Yuan from Fujian Institute of Research on the Structure of Matter for his help with X-ray diffraction analysis. This work was financially supported by the National Key Basic Research Program of China (grants 2021YFA1200402 (Y.C.), 2021YFA1501501 (Y.C.), 2022YFA1503302 (Yan Liu), 2021YFA1200302 (Yan Liu) and 2022YFE0113800 (Y. Zhu)), the National Nature Science Foundation of China (grants 22331007 (Y.C.), 22225111 (Yan Liu), 22122505 (Y. Zhu), 21771161 (Y. Zhu) and 22075250 (Y. Zhu)), and the Key Project of Basic Research of Shanghai (22JC1402000 (Y.C.)).

Author information

Authors and Affiliations

  1. School of Chemistry and Chemical Engineering, Frontiers Science Center for Transformative Molecules and State Key Laboratory of Metal Matrix Composites, Shanghai Jiao Tong University, Shanghai, People’s Republic of China

    Wenqiang Zhang, Hong Jiang, Meng Sun, Enping Du, Wei Gong, Jinqiao Dong, Yan Liu & Yong Cui

  2. Center for Electron Microscopy, State Key Laboratory Breeding Base of Green Chemistry Synthesis Technology and College of Chemical Engineering, Zhejiang University of Technology, Hangzhou, People’s Republic of China

    Yikuan Liu & Yihan Zhu

  3. School of Optical and Electronic Information and Wuhan National Laboratory for Optoelectronics, Huazhong University of Science and Technology, Wuhan, People’s Republic of China

    Yue Hu & Dehui Li

  4. Department of Chemical and Biomolecular Engineering, National University of Singapore, Singapore, Singapore

    Athulya Surendran Palakkal & Jianwen Jiang

  5. Hefei National Research Center for Physical Sciences at the Microscale, Synergetic Innovation Center of Quantum Information and Quantum Physics and Department of Chemical Physics, School of Chemistry and Materials Science, University of Science and Technology of China, Hefei, Anhui, People’s Republic of China

    Yujie Zhou & Qun Zhang

  6. Hefei National Laboratory, University of Science and Technology of China, Hefei, Anhui, People’s Republic of China

    Qun Zhang

  7. Department of Chemistry and Biochemistry and California Nanosystems Institute, University of California, Los Angeles, Los Angeles, CA, USA

    Xiangfeng Duan

Authors
  1. Wenqiang Zhang
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Contributions

Y.C. and X.D. conceived the research. Y.C. supervised the project. W.Z., H.J. and W.G. designed and performed the synthesis experiments. Y. Zhu and Yikuan Liu performed the HR-TEM measurements. W.Z., D.L. and Y.H. performed the Raman, photoluminescence and circularly polarized luminescence measurements. Y. Zhou and Q.Z. performed the ultrafast transient absorption measurements. W.Z., M.S. and E.D. performed the SC-XRD, Brunauer–Emmett–Teller, FTIR and other measurements. X.D. and Y.C. advised on the interpretation of results. A.S.P. and J.J. performed the theoretical computation work. W.Z., J.D., Yan Liu, X.D. and Y.C. wrote and revised the paper. All authors were involved in the data analyses and paper preparation.

Corresponding authors

Correspondence to Yihan Zhu, Yong Cui or Xiangfeng Duan.

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Nature thanks Masahide Takahashi, Yupeng Zhang and the other, anonymous, reviewer(s) for their contribution to the peer review of this work.

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Extended data figures and tables

Extended Data Fig. 1 Structural characterizations of PbBr2@NU-1000 superlattice.

Single-crystal structures of PbBr2@NU-1000 viewed along c-axis (001 facet) (a) and b-axis (100 facet) (b). Yellow, green, orange, grey and red spheres represent Zr, Pb, Br, C and O atoms, respectively. H atoms are omitted for clarity. c, PXRD patterns of the simulated MOF NU-1000 and PbBr2@NU-1000 from SC-XRD data and experimental PbBr2@NU-1000.

Extended Data Fig. 2 Structural characterizations of 0D PbBr2@NU-600 superlattice.

a,b, Single-crystal structures of MOF NU-600 (a) and PbBr2@NU-600 (b) viewed along c-axis (001 facet). c, PXRD patterns of the simulated MOF NU-600 and PbBr2@NU-600 from SC-XRD data and experimental PbBr2@NU-600. Dotted line circled shown the enlarged detail structures. The diameter of the hollow quasi-spherical Pb-based clusters is about 18.96 Å. Yellow, green, orange, grey and red spheres represent Zr, Pb, Br, C and O atoms, respectively. H atoms are omitted for clarity.

Extended Data Fig. 3 Structural characterizations of 0D NiBr2@PCN-700 superlattice.

a,b, Single-crystal structures of NiBr2@PCN-700 viewed along c-axis (001 facet) (a) and b-axis (010 facet) (b). Yellow, light blue, orange, grey and red spheres represent Zr, Ni, Br, C and O atoms, respectively. H atoms are omitted for clarity. c, PXRD patterns of the simulated MOF PCN-700 and NiBr2@PCN-700 from SC-XRD data and experimental NiBr2@PCN-700.

Extended Data Fig. 4 Structural characterizations of 1D PbBr2@PCN-700 superlattice.

a, Single-crystal structures of MOF PCN-700 viewed along c-axis (001 facet). b,c, Single-crystal structures of PbBr2@PCN-700 viewed along c-axis (001 facet) (b) and b-axis (010 facet) (c). Yellow, green, orange, grey and red spheres represent Zr, Pb, Br, C and O atoms, respectively. H atoms are omitted for clarity. d, PXRD patterns of the simulated MOF PCN-700 and PbBr2@PCN-700 from SC-XRD data and experimental PbBr2@PCN-700.

Extended Data Fig. 5 Structural characterizations of 2D PbBr2@PCN-606 superlattice.

a, Single-crystal structures of MOF PCN-606 viewed along c-axis (001 facet). b,c, Single-crystal structures of PbBr2@PCN-606 viewed along c-axis (001 facet) (b) and b axis (010 facet) (c). Yellow, green, orange, grey and red spheres represent Zr, Pb, Br, C and O atoms, respectively. H atoms are omitted for clarity. d, PXRD patterns of the simulated MOF PCN-606 and PbBr2@PCN-606 from SC-XRD data and experimental PbBr2@PCN-606.

Extended Data Fig. 6 Structural characterizations of 0D NU-600⊃PbI2 superstructure.

a,b, Single-crystal structures of NU-600⊃PbI2 viewed along c-axis (010 facet) (a) and a-axis (100 facet) (b). c, PXRD patterns of the simulated MOF NU-600 and NU-600⊃PbI2 from SC-XRD data and experimental NU-600⊃PbI2. SC-XRD reveals that the PbI2 units, stabilized by the supramolecular interactions (H···I distance of 3.42-3.56 Å and I···π distance of 3.60 Å) with the channel surfaces, decompose readily in DMF to yield the pristine PCN-700 single crystals. Yellow, green, orange, violet, grey, red and white spheres represent Zr, Pb, Br, I, C, O and H atoms, respectively.

Extended Data Fig. 7 Structural characterizations of 1D PCN-700⊃PbI2 superstructure.

a,b, Single-crystal structures of PCN-700⊃PbI2 viewed along a-axis (100 facet) (a) and c-axis (001 facet) (b). c, PXRD patterns of the simulated MOF PCN-700 and PCN-700⊃PbI2 from SC-XRD data and experimental PCN-700⊃PbI2. SC-XRD reveals that the PbI2 units, stabilized by the supramolecular interactions (H···I distance of 3.69-3.85 Å) with the channel surfaces, decompose readily in DMF to produce the pristine PCN-700 single crystals. Yellow, green, violet, grey, red and white spheres represent Zr, Pb, I, C, O and H atoms, respectively.

Extended Data Fig. 8 Single-crystal structures of 1D PbI2 nanorods.

a,b, Partial structures of 1D PbI2 nanorods viewed along a-axis (100 facet) (a) and b-axis (010 facet) (b). Coordination of N, N-Dimethylformamide (DMF) molecules to lead atoms creates a protective layer on the sides of one-dimensional PbI2 rods, thus limiting the formation of 2D PbI2 sheets. The DMF-protected 1D PbI2 nanorods readily decompose and dissolve in DMF. Green, violet, grey, teal, red and white spheres represent Pb, I, C, N, O and H atoms, respectively.

Extended Data Fig. 9 Electronic band structures.

a-c, Mott-Schottky (MS) plots of MOF PCN-606 (a), PbI2@PCN-606 (b) and S-MBA/PbI2@PCN-606 (c). d, Schematic illustration of these samples. VB and CB stand for the valence and conduction bands, respectively.

Supplementary information

Supplementary Information

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Supplementary Video 1

Time-dependent photoluminescence of the amine-modified ammonium hydroxide/PbI2@PCN-606 superlattice.

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Zhang, W., Jiang, H., Liu, Y. et al. Metal-halide porous framework superlattices. Nature 638, 418–424 (2025). https://doi.org/10.1038/s41586-024-08447-0

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