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Biomass-derived carbon dots for the initiation of conventional radical and ATRP-based photopolymerization processes

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Abstract

In recent years, there has been increasing interest in using carbon nanodots (CDs) as a component photoinitiator to initiate photopolymerization. These systems support conventional radical photopolymerization and light-mediated atom transfer radical polymerization (photo-ATRP), emphasizing single-component (Type I initiators) and multicomponent systems, which involve at least two reaction partners, specifically, the Type II CD initiator. The latter can function in both photoinduced conventional radical polymerization and photo-ATRP. CDs provide an important advantage by reducing toxicological concerns, as they are nontoxic to cells, and minimizing migration issues typically associated with molecular systems. Here we present two novel photopolymerization methods utilizing biomass-derived CDs as light-sensitive components. The first approach uses biobased furfural to create a Type I CD initiator for photoinduced uncontrolled radical polymerization, which initiates polymerization via homolytic bond cleavage of oxime ester groups attached to the CD surface. The second method employs sodium alginate to generate CDs capable of initiating photoinduced radical polymerization or activating alkyl halides in photo-ATRP processes. Key topics covered in these methods include (1) preparation and characterization of biomass-derived CDs; (2) experimental procedures for CD-assisted photo-induced conventional radical polymerization and photo-ATRP and (3) analysis of the resulting polymers. Preparing and characterizing the CDs takes ~4 d, while photochemical reactions can be conducted within 1 h, depending on requirements. Product separation and analysis take an additional 0.5 h. This protocol is designed for users with experience in polymer chemistry and CD handling.

Key points

  • This Protocol introduces biomass-derived carbon nanodots (CDs) as emerging photoinitiating materials in conventional radical polymerization (Type I and Type II systems) and as photocatalysts for atom transfer radical polymerization-based photopolymerization. The Protocol includes their preparation and characterization, experimental procedures for CD-assisted polymerization and analysis of the resulting polymers focusing on real-time Fourier-transform infrared, photo-differential scanning calorimetry, dynamic mechanical analysis and gel permeation chromatography.

  • Compared with conventional photoinitiators, CDs exhibit notably fewer toxicological responses within the chosen conditions, depending on concentration.

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Fig. 1: General scheme for light-mediated initiation of conventional radical polymerization based on CDs.
Fig. 2: General scheme for the synthesis of Type I CD-PI.
Fig. 3: Mechanism of Type I CDs cleavage.
Fig. 4: Preparation of Type II CDs.
Fig. 5: Mechanism of light-mediated photo-ATRP based on a photocatalytic cycle (modified from ref. 44).
Fig. 6: Preparation of Type I CD initiator.
Fig. 7: Preparation of photopolymerized films comprising Type I CD initiators.
Fig. 8: Preparation of Type II CD initiator and its use to make crosslinked films by photoinitiation following a Type II photoinitiation.
Fig. 9: Analysis of the CDs comprising aldehyde groups on their surface (CDs-CHO).
Fig. 10: Analysis of photopolymerized material and kinetics.
Fig. 11: Characterization of CDs used for ATRP and Type II photoinitiation.
Fig. 12: Photo-DSC of Type II CD-PI.
Fig. 13: GPC of PMMA.

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Data availability

Supporting data for this study can be found in our previous publications42,54 or from the respective corresponding author upon reasonable request. Source data are provided with this paper.

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Acknowledgements

Z.C., X.L. and S.L. acknowledge financial support by the National Key Research and Development Project (grant no. 2024YFD2201503), the National Natural Science Foundation of China (grant no. 32301534), the China Postdoctoral Science Foundation (grant no. 2024M750379) and the Fundamental Research Funds for the Central Universities (grant nos. 2572022CG02, 2572023CT06 and 2572023CT11-04). Furthermore, K.M. gratefully thanks the National Science Foundation of the USA for funding (grant no. NSF CHE 2401112). Moreover, B.S. acknowledges the county of North Rhine Westfalia for financial support of the project REFUBELAS (grant no. 005-1703-0006). In addition, B.S. and V.S. acknowledge the Federal Ministry for Economic Affairs and Climate Action for financial support (B.S.: grant nos. ZF4288703WZ7, KK5297505PA4 and KK5297501TA1 and V.S.: grant nos. KK5297504JN3 and KK5297502BU1).

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  1. These authors contributed equally: Xiongfei Luo, Xue Liu.

Authors and Affiliations

  1. College of Chemistry, Chemical Engineering and Resource Utilization, Northeast Forestry University, Harbin, China

    Xiongfei Luo

  2. Key Laboratory of Bio-based Material Science and Technology Northeast Forestry University, Ministry of Education, Harbin, China

    Xiongfei Luo, Xue Liu, Hongda Guo, Ruiping Li, Min Wang, Xiaotong Li, Shujun Li, Shouxin Liu, Jian Li & Zhijun Chen

  3. Niederrhein University of Applied Sciences Department of Chemistry, Institute for Coatings and Surface Chemistry, Krefeld, Germany

    Veronika Strehmel, Qunying Wang & Bernd Strehmel

  4. Department of Chemistry, Carnegie Mellon University, Pittsburgh, PA, USA

    Gorkem Yilmaz & Krzysztof Matyjaszewski

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Contributions

X. Luo and X. Liu contributed equally to the work regarding writing. H.G. and R.L. performed experiments, investigations, writing of the original draft and data curation. M.W. performed experiments, investigations, writing of original draft and data curation. X.L. performed experiments and investigations. S. Li contributed to writing—review and editing, supervision and acquisition of funding. S. Liu contributed to writing—review and editing. J.L. contributed to writing—review and editing. V.S. contributed to writing—review and editing and funding acquisition. Q.W. performed experiments, investigations, data curation, and writing the original draft and final drafting. G.Y. contributed to writing—review and editing, funding acquisition and conceptualization. K.M. contributed to writing—review and editing, funding acquisition and conceptualization. B.S. contributed to writing—review and editing, funding acquisition, supervision and conceptualization. Z.C. contributed to writing—review and editing, funding acquisition, supervision and conceptualization. All authors contributed extensively to the work presented.

Corresponding authors

Correspondence to Gorkem Yilmaz, Krzysztof Matyjaszewski, Bernd Strehmel or Zhijun Chen.

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Nature Protocols thanks Min Sang Kwon and Weilong Shi for their contribution to the peer review of this work.

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Key references

Kütahya, C. et al. Angew. Chem. Int. Ed. 59, 3166–3171 (2020): https://doi.org/10.1002/anie.201912343

Li, R. et al. Angew. Chem. Int. Ed. 63, e202404454 (2024): https://doi.org/10.1002/anie.202404454

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Luo, X., Liu, X., Guo, H. et al. Biomass-derived carbon dots for the initiation of conventional radical and ATRP-based photopolymerization processes. Nat Protoc (2025). https://doi.org/10.1038/s41596-025-01210-3

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