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High-brightness transition metal-sensitized lanthanide near-infrared luminescent nanoparticles

Nature Photonics (2024)Cite this article

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Abstract

The demand for near-infrared (700–1,700 nm) materials in optical communications, laser sources and biological imaging applications has led to extensive research on lanthanide-doped nanoparticles, owing to their nanostructure modulation and interface property tunability. However, the low molar extinction coefficient of conventional lanthanide sensitizers limits the brightness of lanthanide near-infrared nanoparticles for applications in low-power excitation scenarios. Here we introduce Na3CrF6, a new crystalline nanoparticle that serves as both sensitizer and host for high-brightness near-infrared emission from lanthanide activators (Er3+, Tm3+, Yb3+ or Nd3+). We demonstrate an increase in brightness of up to 370 times compared with the most intense conventional lanthanide-sensitized nanoparticles. This discovery is also validated for other lanthanide-doped nanoparticles sensitized with low-cost transition metals (Mn2+ or Ni2+). Our transition metal-based nanoparticles represent a powerful toolbox to enable high signal-to-noise-ratio labelling and imaging with low-power excitation sources such as white light-emitting diode or persistent luminescence materials. This work paves the way for next-generation high-brightness near-infrared luminescence systems, suited for a wide range of low-illumination excitation applications.

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Fig. 1: Characterization of Na3CrF6:X.
Fig. 2: Spectroscopic evidence for the sensitization mechanism of Na3CrF6:X.
Fig. 3: Controlled structures and compositions of transition metal-sensitized lanthanide hybrid nanostructures.
Fig. 4: CLNP for multiplexed encryption and in vivo bioimaging.
Fig. 5: Non-invasive dual-channel high-contrast bioimaging using PL as an internal excitation source.

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The experimental data supporting the findings of this study are available within the article. Source data are provided with this paper.

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Acknowledgements

This work was supported by the National Key R&D Program of China (grant no. 2023YFB3507100, F.Z.), National Natural Science Foundation of China (NSFC; 22088101, F.Z.), New Cornerstone Science Foundation through the XPLORER PRIZE, the Research Program of Science and Technology Commission of Shanghai Municipality (21142201000 and 22JC1400400, F.Z.), and the Innovation Program of Shanghai Municipal Education Commission (2023ZKZD08, F.Z.). We thank Y. Ma (ShanghaiTech University) for help with the atomically resolved STEM measurements.

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Authors and Affiliations

  1. Department of Chemistry, State Key Laboratory of Molecular Engineering of Polymers, Laboratory of Advanced Materials, Shanghai Key Laboratory of Molecular Catalysis and Innovative Materials and iChem, Fudan University, Shanghai, People’s Republic of China

    Jiang Ming, Ying Chen, Han Miao, Yong Fan, Shangfeng Wang, Zihan Chen, Zhenhao Guo, Zhixiu Guo, Luyin Qi, Xusheng Wang, Baofeng Yun, Peng Pei, Haisheng He, Hongxin Zhang, Yun Tang, Dongyuan Zhao & Fan Zhang

  2. School of Materials Science and Engineering, East China University of Science and Technology, Shanghai, People’s Republic of China

    Han Miao

  3. Department of Applied Biology & Chemical Technology, The Hong Kong Polytechnic University, Hong Kong, Hung Hom, Kowloon, People’s Republic of China

    Gary Ka-Leung Wong

  4. Institut des Sciences Chimiques et Ingénierie, École Polytechnique Fédérale de Lausanne, Lausanne, Switzerland

    Jean-Claude G. Bünzli

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Contributions

J.M. and F.Z. conceived and designed the experiments. J.M., Zhenhao Guo, Zhixiu Guo, L.Q., Z.C., H.M. and X.W. synthesized the nanoparticles and conducted the characterization of CLNPs. J.M., P.P., H.Z., Y.F. and F.Z. discussed the energy transfer mechanism of CLNPs. J.M., Zhenhao Guo, Zhixiu Guo and L.Q. built the in vitro NIR imaging system. J.M., Y.C., Y.F., B.Y. and H.H. conducted the in situ gastric tumour imaging in mice. F.Z., Y.F., J.M., D.Z., S.W., Y.T., G.K.-L.W. and J.-C.G.B. analysed the results, figures and Supplementary Information. J.M., H.M. and F.Z. wrote the paper. All authors contributed to discussing and editing the paper.

Corresponding author

Correspondence to Fan Zhang.

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Extended data

Extended Data Fig. 1 Physical properties of Na3CrF6 and other host matrixes.

a-c, The XRD patterns of Na3CrF6:Er (a), α-NaErF4 (b) and β-NaErF4 (c), respectively. d-i, k-space (d, e, and f) and R-space (g, h, and i) EXAFS fitting results of Na3CrF6:Er, α-NaErF4 and β-NaErF4, respectively. j-l, Raman spectrum of Na3CrF6 (j), α-NaYF4 (k) and β-NaYF4 (l). m, The DFT calculation of Na or Cr in Cr2Na6F6 replaced by Er.

Source data

Extended Data Fig. 2 Optimize the doping concentration of Yb3+, Nd3+, Er3+, and Tm3+ in Na3CrF6:X nanoparticles.

a, Schematic for the synthesis of Na3CrF6:X (X = Yb3+, Nd3+, Er3+, and Tm3+) nanoparticles. Insets: The optical photograph of Na3CrF6:Er nanoparticles. b-e, TEM images for Na3CrF6:Yb (3.5 mol%) (b), Na3CrF6:Nd (5.6 mol%) (c), Na3CrF6:Er (4.2 mol%) (d), and Na3CrF6:Tm (4.1 mol%) (e) nanoparticles, respectively. f-i, Typical emission and excitation spectra of Na3CrF6:Yb (3.5 mol%) (f), Na3CrF6:Nd (5.6 mol%) (g), Na3CrF6:Er (4.2 mol%) (h), and Na3CrF6:Tm (4.1 mol%) (i) nanoparticles, respectively. j-m, Influence of activator concentration on the luminescence intensity of Yb3+ (j), Nd3+ (k), Er3+ (l), and Tm3+ (m) in Na3CrF6:X nanoparticles, respectively. All measurements were performed three times. The data are shown as the mean ± s.d. n-q, The relationship of Yb3+ (n), Nd3+ (o), Er3+ (p), and Tm3+ (q) concentration for ICP-OES tested and fed in the synthesis of Na3CrF6:X (X = Yb3+, Nd3+, Er3+, and Tm3+) nanoparticles, respectively. Scale bar: 100 nm. All measurements were performed three times. The data are shown as the mean ± s.d.

Source data

Extended Data Fig. 3 Luminescence decay curves of Cr3+ and X3+ (X = Er, Tm, Yb, and Nd) in CLNP and calculation of energy transfer efficiency.

a-b, Luminescence decay curves of Na3CrF6:Er nanoparticles measured at 776 nm (a) and 1,540 nm (b) with different Er3+ doping percentage under 655 nm laser excitation. c, The energy transfer efficiency of Na3CrF6:Er nanoparticles from Cr3+ to Er3+ in different Er3+ doping percentage. d-e, Luminescence decay curves of Na3CrF6:Tm measured at 1,050 nm (d) and 1,438 nm (e) with different Tm3+ doping percentage under 655 nm laser excitation. f, The energy transfer efficiency of Na3CrF6:Tm nanoparticles from Cr3+ to Tm3+ in different Tm3+ doping percentage. g-h, Luminescence decay curves of Na3CrF6:Yb measured at 776 nm (g) and 1,000 nm (h) with different Yb3+ doping percentage under 655 nm laser excitation. i, The energy transfer efficiency of Na3CrF6:Yb nanoparticles from Cr3+ to Yb3+ in different Yb3+ doping percentage. j-k, Luminescence decay curves of Na3CrF6:Nd measured at 776 nm (j) and 1,056 nm (k) with different Nd3+ doping percentage under 655 nm laser excitation. l, The energy transfer efficiency of Na3CrF6:Nd nanoparticles from Cr3+ to Nd3+ in different Nd3+ doping percentage. All measurements were performed three times. The data are shown as the mean ± s.d.

Source data

Extended Data Fig. 4 Comparison of the luminescence intensity for CLNP and DSNP of similar size.

a-d, TEM images of Na3CrF6:Er (4.2 mol%) and α-NaYbF4:Er/Ce (2/2 mol%) (a), Na3CrF6:Tm (4.1 mol%) and α-NaYbF4:Tm (8 mol%) (b), Na3CrF6:Nd (5.6 mol%) and β-NaYF4:Nd (5 mol%) (c), and Na3CrF6:Yb (3.5 mol%) and β-NaYF4:Yb (20 mol%) (d), respectively. The size distribution of the particles is shown in the top right of the corresponding TEM images. Scale bar: 200 nm. e-h, Luminescence emission spectra of Na3CrF6:Er (4.2 mol%, excitation: 655 nm) and α-NaYbF4:Er/Ce (2/2 mol%, excitation: 980 nm) (e), Na3CrF6:Tm (4.1 mol%, excitation: 655 nm) and α-NaYbF4:Tm (8 mol%, excitation: 980 nm) (f), Na3CrF6:Nd (5.6 mol%, excitation: 655 nm) and β-NaYF4:Nd (5 mol%, excitation: 808 nm) (g), and Na3CrF6:Yb (3.5 mol%, excitation: 655 nm) and β-NaYF4:Yb (20 mol%, excitation: 980 nm) (h) under corresponding laser excitation with same concertation (0.01 mmol mL-1) and power densities (7 mW cm-2), respectively. Right: Corresponding comparison of the intensity integral area intensity is lebeled in the spectra. i-l, Power dependence comparison of Na3CrF6:Er (4.2 mol%) and α-NaYbF4:Er/Ce (2/2 mol%) (i), Na3CrF6:Tm (4.1 mol%) and α-NaYbF4:Tm (8 mol%) (j), Na3CrF6:Nd (5.6 mol%) and β-NaYF4:Nd (5 mol%) (k), Na3CrF6:Yb (3.5 mol%) and β-NaYF4:Yb (20 mol%) (l) nanoparticles, respectively.

Source data

Extended Data Fig. 5 TRPL spectrum of CLNPs under 655 nm laser.

a, TRPL spectrum of Na3CrF6: Yb (3.5 mol%) under 655 nm laser excitation. b, TRPL kinetics analysis of Na3CrF6: Yb (3.5 mol%) at two characteristic emission peaks (776 nm and 1,000 nm). c, TRPL spectrum of Na3CrF6:Yb (3.5 mol%) at different time delays from 0.1 to 5 ms. d, TRPL spectrum of Na3CrF6: Nd (5.6 mol%) under 655 nm laser excitation. e, TRPL kinetics analysis of Na3CrF6: Nd (5.6 mol%) at four characteristic emission peaks (770 nm, 878 nm, 1,056 nm, and 1,322 nm). f, TRPL spectrum of Na3CrF6:Nd (5.6 mol%) at different time delays from 0.1 to 0.7 ms. g, TRPL spectrum of Na3CrF6: Tm (4.1 mol%) under 655 nm laser excitation. h, TRPL kinetics analysis of Na3CrF6: Tm (4.1 mol%) at four characteristic emission peaks (776 nm, 800 nm, 1,438 nm, and 1,622 nm). i, TRPL spectrum of Na3CrF6:Tm (4.1 mol%) at different time delays from 0.225 to 5 ms. The gray dotted line shows the difference in time at the characteristic emission peaks.

Source data

Extended Data Fig. 6 Characterization of core-shell structured α-NaLnF4@Na3CrF6 NPs.

a-l, TEM images (left) and XRD patterns (right) of α-NaLnF4 (Ln = Y (a), Pr (b), Nd (c), Eu (d), Gd (e), Tb (f), Dy (g), Ho (h), Er (i), Tm (j), Yb (k), and Lu (l)) core before (top left) and after (bottom left) the Na3CrF6 shell coated. Scale bar: 50 nm.

Extended Data Fig. 7 Synthesis and characterization of core-shell CLNP.

a, Schematic of synthesis of core-shell CLNP. b-d, Atomically resolved STEM of α-NaYF4@Na3CrF6 nanoparticles (b), scale bar: 5 nm, normalized gray values of the shell (c, Na3CrF6) and core (d, α-NaYF4) extracted from atomically resolved STEM for the selected area. e, The corresponding XRD patterns of core (α-NaYF4) and core-shell (α-NaYF4@Na3CrF6) nanoparticles. f-i, The power dependence comparison of α-NaYF4:10 mol% Er@Na3CrF6 under 655 nm and 980 nm laser excitation from 1,400-1,650 nm (f), α-NaYF4: 5 mol% Tm@Na3CrF6 under 655 nm and 808 nm laser excitation from 1,300-1,750 nm (g), α-NaYF4: 5 mol% Yb@Na3CrF6 under 655 nm and 980 nm laser excitation from 980-1,200 nm (h), and α-NaYF4: 10 mol% Nd@Na3CrF6 under 655 nm and 808 nm laser excitation from 1,020-1,400 nm (i), respectively.

Source data

Extended Data Fig. 8 The energy transfer process in the core-shell α-NaYF4:X@Na3CrF6(X = 5 mol% Nd, 3 mol% Yb, 5 mol% Er, and 3 mol% Tm)@Na3CrF6 NPs.

a-d, TRPL spectrum of α-NaYF4:Nd(5 mol%)@Na3CrF6 (a), α-NaYF4:Yb(3 mol%)@Na3CrF6 (b), α-NaYF4:Er(5 mol%)@Na3CrF6 (c) and α-NaYF4:Tm(3 mol%)@Na3CrF6 (d) under 655 nm laser excitation. e-h, TRPL kinetics analysis of α-NaYF4:Nd(5 mol%)@Na3CrF6 (e) at four characteristic emission peaks (778 nm, 868 nm, 1,048 nm and 1,318 nm), α-NaYF4:Yb(3 mol%)@Na3CrF6 (f) at two characteristic emission peaks (774 nm and 974 nm), α-NaYF4:Er(5 mol%)@Na3CrF6 (g) at three characteristic emission peaks (778 nm, 978 nm and 1,532 nm) and α-NaYF4:Tm(3 mol%)@Na3CrF6 (h) at three characteristic emission peaks (778 nm, 1,438 nm and 1,622 nm). i-l, TRPL spectra at different time delays of α-NaYF4:Nd(5 mol%)@Na3CrF6 (i) from 0.1425 to 0.56 ms, α-NaYF4:Yb(3 mol%)@Na3CrF6 (j) from 0.07 to 0.25 ms, α-NaYF4:Er(5 mol%)@Na3CrF6 (k) from 0.145 to 0.485 ms and α-NaYF4:Tm(3 mol%)@Na3CrF6 (l) from 0.1325 to 0.75 ms. m-p, Schematic of energy transfer process from Cr3+ to Nd3+ (m) in α-NaYF4:Nd(5 mol%)@Na3CrF6, Cr3+ to Yb3+ (n) in α-NaYF4:Yb(3 mol%)@Na3CrF6, Cr3+ to Er3+ (o) in α-NaYF4:Er(5 mol%)@Na3CrF6, and Cr3+ to Tm3+ (p) in α-NaYF4:Tm(3 mol%)@Na3CrF6.

Source data

Extended Data Fig. 9 The biocompatibility of DSNP-CLNP hybrid nanoparticles and Na3CrF6:Er.

a-b, Cell viabilities of Mouse Forestomach Carcinoma cells incubated with DSNP-CLNP (a) and Na3CrF6:Er (b) for 24 hours, n = 5 independent experiments. c, H&E staining of visceral organs (heart, liver, spleen, lung, and kidney), obtained at 24 h post-injection of Tris (400 μL, control group), DSNP-CLNP or Na3CrF6:Er (1 mg mL-1, 400 μL) via the tail vein. d-e, Biodistribution of DSNP-CLNP-cRGD (d) and Na3CrF6:Er-cRGD (e) in 615 mice with the subcutaneous tumour model and in situ gastric tumour model, respectively. n = 3 independent experiments. These results indicated that DSNP-CLNP and Na3CrF6:Er have biocompatibility and low toxicity. The data are shown as the mean ± s.d. However, given the biosafety of nanomaterials, long-term biotoxicity has to be further evaluated.

Source data

Extended Data Fig. 10 Physicochemical properties of CLNP for biological imaging.

a, Schematic of DSNP-CSNP heterogeneous structure. b, TEM image of DSNP-CLNP hybrid nanoparticles. c, Luminescence image and the merge with the bright-field image of the ex vivo tumor. d, H&E staining results of the removed tumour. Scale bar: 500 μm. The normal (N) and tumour (T) regions selected are marked in the figures. e, NIR-II images of tumour in a living mouse under WLED or 980 nm laser exaction with different power densities. Tumour regions (T) and normal regions (N) are marked in the figure. f, The tumour region signals in NIR-II imaging under WLED or 980 nm laser exaction with different power densities. g, The normal region signals in NIR-II imaging under WLED or 980 nm laser exaction with different power densities. h, Schematic of dual-channel in vivo luminescence imaging of in situ gastric tumour model. i, H&E staining results of the removed tumour. Scale bar: 500 μm. The tumour regions are marked in the figures. j, Relative luminescence intensity of Na3CrF6:Er (4.2 mol%) in cyclohexane, H2O, and Na3CrF6:Er (4.2 mol%)-cRGD in H2O. k, The persistence luminescence power densities as a function of time. l, The relative luminescence intensity of the Na3CrF6:Er at different pH. Incubation time: 10 min. Excitation: 655 nm for Na3CrF6:Er. m, The relative luminescence intensity of Na3CrF6:Er at different time. Incubation pH:1.0. Excitation: 655 nm for Na3CrF6:Er. The data are shown as the mean ± s.d. (n = 3).

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Ming, J., Chen, Y., Miao, H. et al. High-brightness transition metal-sensitized lanthanide near-infrared luminescent nanoparticles. Nat. Photon. (2024). https://doi.org/10.1038/s41566-024-01517-9

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