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Closed-Loop Controlled Photopolymerization of Hydrogels

  • Manjot Singh
    Manjot Singh
    Department of Industrial and Systems Engineering, Virginia Tech, Blacksburg, Virginia 24061, United States
    More by Manjot Singh
  • Junru Zhang
    Junru Zhang
    Department of Industrial and Systems Engineering, Virginia Tech, Blacksburg, Virginia 24061, United States
    More by Junru Zhang
  • Keturah Bethel
    Keturah Bethel
    Department of Chemical and Biomolecular Engineering, Clemson University, Clemson, South Carolina 29634, United States
  • Yang Liu
    Yang Liu
    Macromolecules Innovation Institute, Virginia Tech, Blacksburg, Virginia 24061, United States
    More by Yang Liu
  • Eric M. Davis
    Eric M. Davis
    Department of Chemical and Biomolecular Engineering, Clemson University, Clemson, South Carolina 29634, United States
  • Haibo Zeng
    Haibo Zeng
    Department of Electrical and Computer Engineering, Virginia Tech, Blacksburg, Virginia 24061, United States
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  • Zhenyu Kong
    Zhenyu Kong
    Department of Industrial and Systems Engineering, Virginia Tech, Blacksburg, Virginia 24061, United States
    More by Zhenyu Kong
  • , and 
  • Blake N. Johnson*
    Blake N. Johnson
    Department of Industrial and Systems Engineering, Virginia Tech, Blacksburg, Virginia 24061, United States
    Macromolecules Innovation Institute, Virginia Tech, Blacksburg, Virginia 24061, United States
    Department of Materials Science and Engineering, Virginia Tech, Blacksburg, Virginia 24061, United States
    Department of Chemical Engineering, Virginia Tech, Blacksburg, Virginia 24061, United States
    *Email: [email protected]. Fax: 540-231-3322.
Cite this: ACS Appl. Mater. Interfaces 2021, 13, 34, 40365–40378
Publication Date (Web):August 20, 2021
https://doi.org/10.1021/acsami.1c11779
Copyright © 2021 American Chemical Society

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    Abstract

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    Here, we present a closed-loop controlled photopolymerization process for fabrication of hydrogels with controlled storage moduli. Hydrogel crosslinking was associated with a significant change in the phase angle of a piezoelectric cantilever sensor and established the timescale of the photopolymerization process. The composition, structure, and mechanical properties of the fabricated hydrogels were characterized using Raman spectroscopy, scanning electron microscopy (SEM), and dynamic mechanical analysis (DMA). We found that the storage moduli of photocured poly(ethylene glycol) dimethacrylate (PEGDMA) and poly(N-isopropylacrylamide) (PNIPAm) hydrogels could be controlled using bang-bang and fuzzy logic controllers. Bang-bang controlled photopolymerization resulted in constant overshoot of the storage modulus setpoint for PEGDMA hydrogels, which was mitigated by setpoint correction and fuzzy logic control. SEM and DMA studies showed that the network structure and storage modulus of PEGDMA hydrogels were dependent on the cure time and temporal profile of UV exposure during photopolymerization. This work provides an advance in pulsed and continuous photopolymerization processes for hydrogel engineering based on closed-loop control that enables reproducible fabrication of hydrogels with controlled mechanical properties.

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    Cited By

    This article is cited by 7 publications.

    1. Hai-Tao Ren, Da-Shuai Li, Chao-Chen Cai, Ting-Ting Li, Ching-Wen Lou, Jia-Horng Lin, Xu Han. Facile Photopolymerization of High-Molecular-Weight Polyaniline Composites Induced by g-C3N4 at Room Temperature for Trace Fe Ion Sensors. Macromolecules 2023, 56 (23) , 9509-9522. https://doi.org/10.1021/acs.macromol.3c01970
    2. Yang Liu, Junru Zhang, Yujing Zhang, Hu Young Yoon, Xiaoting Jia, Maren Roman, Blake N. Johnson. Accelerated Engineering of Optimized Functional Composite Hydrogels via High-Throughput Experimentation. ACS Applied Materials & Interfaces 2023, 15 (45) , 52908-52920. https://doi.org/10.1021/acsami.3c11483
    3. Hao Sun, Shen Shen, Liangliang Zhu. Photo-stimuli-responsive Organic Room-Temperature Phosphorescent Materials. ACS Materials Letters 2022, 4 (9) , 1599-1615. https://doi.org/10.1021/acsmaterialslett.2c00392
    4. Yang Liu, Keturah Bethel, Manjot Singh, Junru Zhang, Rana Ashkar, Eric M. Davis, Blake N. Johnson. Comparison of Bulk- vs Layer-by-Layer-Cured Stimuli-Responsive PNIPAM–Alginate Hydrogel Dynamic Viscoelastic Property Response via Embedded Sensors. ACS Applied Polymer Materials 2022, 4 (8) , 5596-5607. https://doi.org/10.1021/acsapm.2c00634
    5. Ezgi Kucukdeger, Blake N. Johnson. Closed-loop controlled conformal 3D printing on moving objects via tool-localized object position sensing. Journal of Manufacturing Processes 2023, 89 , 39-49. https://doi.org/10.1016/j.jmapro.2023.01.020
    6. Junru Zhang, Yang Liu, Durga Chandra Sekhar.P, Manjot Singh, Yuxin Tong, Ezgi Kucukdeger, Hu Young Yoon, Alexander P. Haring, Maren Roman, Zhenyu (James) Kong, Blake N. Johnson. Rapid, autonomous high-throughput characterization of hydrogel rheological properties via automated sensing and physics-guided machine learning. Applied Materials Today 2023, 30 , 101720. https://doi.org/10.1016/j.apmt.2022.101720
    7. Xinyue Guo, Huanv Mao, Chunyan Bao, Decheng Wan, Ming Jin. Fused carbazole–coumarin–ketone dyes: high performance and photobleachable photoinitiators in free radical photopolymerization for deep photocuring under visible LED light irradiation. Polymer Chemistry 2022, 13 (22) , 3367-3376. https://doi.org/10.1039/D2PY00466F

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