Skip to main content

Thank you for visiting nature.com. You are using a browser version with limited support for CSS. To obtain the best experience, we recommend you use a more up to date browser (or turn off compatibility mode in Internet Explorer). In the meantime, to ensure continued support, we are displaying the site without styles and JavaScript.

  • Original Article
  • Published:

Study on the deformation and fracture of epoxy monoliths through mechanical tensile and compressive tests and X-ray CT imaging

Polymer Journal volume 56, pages 529–540 (2024)Cite this article

Subjects

Abstract

As porous polymer materials with continuous epoxy skeletons and pores, epoxy monoliths are used as column fillers in HPLC, separators in lithium-ion batteries, and precursor polymers for monolith adhesion and co-continuous network polymer fabrication. Due to their unique mechanical properties and fracture behavior, epoxy monoliths can incur large deformation and are different from the bulk thermoset of epoxy resins that exhibit hard and brittle features. In this study, we prepared an epoxy monolith using 2,2’-bis(4’-glycidyloxaphenyl)propane (BADGE) and tripropylene glycol diglycidyl ether (TPGD) as epoxy resins, 4,4’-methylenebis(cyclohexylamine) (BACM) as a crosslinker, and poly(ethylene glycol) (PEG) as a porogen, and TPGD-induced effects on the pore structure and properties of the obtained monoliths were investigated. To clarify the relationship between the pore structure and the mechanical properties of the monolith, scanning electron microscopy (SEM) observations and tensile and compression tests were performed. In addition, X-ray CT imaging nondestructively revealed a change in the inner porous structure of the monolith after a large deformation occurred under various compression conditions. We clarified the effects of the TPGD addition on the monolith structure and the mechanical properties with tensile and compressive deformation.

This is a preview of subscription content, access via your institution

Access options

Buy this article

  • Purchase on Springer Link
  • Instant access to full article PDF
Buy now

Prices may be subject to local taxes which are calculated during checkout

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7
Fig. 8
Fig. 9
Fig. 10

Similar content being viewed by others

References

  1. Petrie EM. Handbook of adhesives and sealants. 2nd ed. New York: McGrow-Hill; 2007.

    Google Scholar 

  2. Sprenger S. Epoxy resins modified with elastomers and surface-modified silica nanoparticles. Polymer. 2013;54:4790–7.

    Article  CAS  Google Scholar 

  3. Jin F-L, Li X, Park S-J. Synthesis and application of epoxy resins: a review. J Ind Eng Chem. 2015;29:1–11.

    Article  CAS  Google Scholar 

  4. Mashouf Roudsari G, Mohanty AK, Misra M. Green approaches to engineer tough biobased epoxies: a review. ACS Sustain Chem Eng. 2017;5:9528–41.

    Article  CAS  Google Scholar 

  5. Kumar S, Krishnan S, Samal SK, Mohanty S, Nayak SK. Toughening of petroleum based (DGEBA) epoxy resins with various renewable resources based flexible chains for high performance applications: a review. Ind Eng Chem Res. 2018;57:2711–26.

    Article  CAS  Google Scholar 

  6. Ahmadi Z. Nanostructured epoxy adhesives: a review. Prog Org Coat. 2019;135:449–53.

    Article  CAS  Google Scholar 

  7. Wei H, Xia J, Zhou W, Zhou L, Hussain G, Li Q, et al. Adhesion and cohesion of epoxy-based industrial composite coatings. Comp B. 2020;193:108035.

    Article  CAS  Google Scholar 

  8. Shundo A, Yamamoto S, Tanaka K. Network formation and physical properties of epoxy resins for future practical applications. JACS Au. 2022;2:1522.

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  9. Kinloch AJ. Mechanics and mechanisms of fracture of thermosetting epoxy polymers. Adv Polym Sci. 1985;72:45–67.

    Article  CAS  Google Scholar 

  10. Chikhi N, Fellahi S, Bakar M. Modification of epoxy resin using reactive liquid (ATBN) rubber. Eur Polym J. 2001;38:251–64.

    Article  Google Scholar 

  11. Kishi H, Matsuda S, Imade J, Shimoda Y, Nakagawa T, Furukawa Y. The effects of the toughening mechanism and the molecular weights between cross-links on the fatigue resistance of epoxy polymer blends. Polymer. 2021;223:123712.

    Article  CAS  Google Scholar 

  12. Tanaka N, Kobayashi H, Nakanishi K, Minakuchi H, Ishizuka N. Monolithic LC columns. Anal Chem. 2001;73:420A–9A.

    Article  CAS  PubMed  Google Scholar 

  13. Aoki H, Tanaka N, Kubo T, Hosoya K. Polymer-based monolithic columns in capillary format tailored by using controlled in situ polymerization. J Sep Sci. 2009;32:341–58.

    Article  CAS  PubMed  Google Scholar 

  14. Nguyen AM, Irgum K. Epoxy-based monoliths. A novel hydrophilic separation material for liquid chromatography of biomolecules. Chem Mater. 2006;18:6308–15.

    Article  CAS  Google Scholar 

  15. Tsujioka N, Ishizuka N, Tanaka N, Kubo T, Hosoya K. Well-controlled 3D skeletal epoxy-based monoliths obtained by polymerization induced phase separation. J Polym Sci Part A Polym Chem. 2008;46:3272–81.

    Article  CAS  Google Scholar 

  16. Sakakibara K, Kagata H, Ishizuka N, Sato T, Tsujii Y. Fabrication of surface skinless membranes of epoxy resin-based mesoporous monoliths toward advanced separators for lithium-ion batteries. J Mater Chem A. 2017;5:6866–73.

    Article  CAS  Google Scholar 

  17. Uehara F, Matsumoto A. Metal-resin bonding mediated by epoxy monolith layer. Appl Adhes Sci. 2016;4:18.

    Article  Google Scholar 

  18. Sugimoto Y, Nishimura Y, Uehara F, Matsumoto A. Dissimilar materials bonding using epoxy monolith. ACS Omega. 2018;3:7532–41.

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  19. Sakata N, Takeda Y, Kotera S, Suzuki Y, Matsumoto A. Interfacial structure control and three-dimensional X-ray imaging of an epoxy monolith bonding system with surface modification. Langmuir. 2020;36:10923–32.

    Article  CAS  PubMed  Google Scholar 

  20. Tominaga R, Nishimura Y, Suzuki Y, Takeda Y, Kotera M, Matsumoto A. Co-continuous network polymes using epoxy monolith for the design of tough materials. Sci Rep. 2021;11:1431.

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  21. Tominaga R, Takeda Y, Kotera M, Suzuki Y, Matsumoto A. Non-destructive observation of internal structures of epoxy monolith and co-continuous network polymer using X-ray CT imaging for elucidation of their unique mechanical features and fracture mechanism. Polymer. 2022;263:125433.

    Article  CAS  Google Scholar 

  22. Maire E, Withers PJ. Quantitative X-ray tomography. Inter Mater Rev. 2014;59:1–43.

    Article  CAS  Google Scholar 

  23. Garcea SC, Wang Y, Withers PJ. X-ray computed tomography of polymer composites. Comp Sci Technol. 2018;156:305–19.

    Article  CAS  Google Scholar 

  24. Mi Y, Zhou W, Li Q, Zhang D, Zhang R, Ma G, et al. Detailed exploration of structure formation of an epoxy-based monolith with three-dimensional bicontinuous structure. RSC Adv. 2015;5:55419.

    Article  CAS  Google Scholar 

  25. Nakanishi K, Tanaka N. Sol-gel with phase separation. Hierarchically porous materials optimized for high-performance liquid chromatography separations. Acc Chem Res. 2007;40:863–73.

    Article  CAS  PubMed  Google Scholar 

  26. Svec F. Porous polymer monoliths: amazingly wide variety of techniques enabling their preparation. J Chromatogr A 2010;1217:902–24.

    Article  CAS  PubMed  Google Scholar 

  27. Watanabe M, Takeda Y, Maruyama T, Ikeda J, Kawai M, Mitsumata T. Chain structure in a cross-linked polyurethane magnetic elastomer under a magnetic field. Int J Mol Sci. 2019;20:2879.

    Article  CAS  PubMed  PubMed Central  Google Scholar 

Download references

Author information

Authors and Affiliations

  1. Department of Applied Chemistry, Graduate School of Engineering, Osaka Metropolitan University, 1‐1, Gakuen‐cho, Naka‐ku, Sakai, Osaka, 599‐8531, Japan

    Kazuma Aragishi, Yasuhito Suzuki & Akikazu Matsumoto

  2. Advanced Analysis Research Department, X‐Ray Research Laboratory, Rigaku Corporation, 3‐9‐12, Matsubara‐cho, Akishima, Tokyo, 196‐8666, Japan

    Yoshihiro Takeda

Authors
  1. Kazuma Aragishi
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Yoshihiro Takeda
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Yasuhito Suzuki
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Akikazu Matsumoto
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding authors

Correspondence to Yasuhito Suzuki or Akikazu Matsumoto.

Ethics declarations

Conflict of interest

The authors declare no competing interests.

Additional information

Publisher’s note Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Supplementary information

Rights and permissions

Springer Nature or its licensor (e.g. a society or other partner) holds exclusive rights to this article under a publishing agreement with the author(s) or other rightsholder(s); author self-archiving of the accepted manuscript version of this article is solely governed by the terms of such publishing agreement and applicable law.

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Aragishi, K., Takeda, Y., Suzuki, Y. et al. Study on the deformation and fracture of epoxy monoliths through mechanical tensile and compressive tests and X-ray CT imaging. Polym J 56, 529–540 (2024). https://doi.org/10.1038/s41428-023-00872-8

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1038/s41428-023-00872-8

Search

Advanced search

Quick links