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<p>This study investigates the influence of acrylic acid grafted halloysite nanotubes (m-HNTs) on the self-healing performance of natural rubber (NR) composites mediated by ionic supramolecular interactions. Halloysite nanotubes were surface modified with varying acrylic acid contents (2–8 wt%) to overcome their inherent incompatibility with non-polar NR by reducing surface hydroxyl groups and strengthening rubber–filler interfacial interactions. Acrylic acid (AA) grafting further enabled the formation of Zn²⁺ mediated ionic interactions between carboxylic groups on the modified HNTs and zinc thiolate functionalized NR, resulting in additional reversible supramolecular networks. Among the compositions studied, composites containing 6 wt% AA-grafted HNTs exhibited the optimal balance of mechanical strength and healing capability, achieving a tensile strength of 5.56&#xa0;MPa (34.9% improvement) and a healing efficiency of 98.9%, outperforming composites filled with untreated HNTs. Dynamic mechanical, rheological, and fatigue analysis demonstrated that increasing m-HNT content progressively enhanced viscoelastic behavior, large viscoelastic region, and fatigue life. These findings demonstrate that the synergistic reinforcement–healing mechanism overcomes the limitations of conventional HNT systems by employing ionic supramolecular interactions as a robust reinforcement strategy, enabling simultaneous mechanical enhancement and highly efficient self-healing in natural rubber nanocomposites.</p>

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Acid etched halloysite nanotubes as dual-function reinforcement for intrinsic self-healing natural rubber composites

  • 期刊论文

  • 发表日期：

    2026年3月23日

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  • Abdul Rehman,
  • Ayesha Areeba,
  • Wasif Razzaq,
  • Asad ur Rehman Khan,
  • Hanafi Ismail,
  • Raa Khimi Shuib

摘要

This study investigates the influence of acrylic acid grafted halloysite nanotubes (m-HNTs) on the self-healing performance of natural rubber (NR) composites mediated by ionic supramolecular interactions. Halloysite nanotubes were surface modified with varying acrylic acid contents (2–8 wt%) to overcome their inherent incompatibility with non-polar NR by reducing surface hydroxyl groups and strengthening rubber–filler interfacial interactions. Acrylic acid (AA) grafting further enabled the formation of Zn²⁺ mediated ionic interactions between carboxylic groups on the modified HNTs and zinc thiolate functionalized NR, resulting in additional reversible supramolecular networks. Among the compositions studied, composites containing 6 wt% AA-grafted HNTs exhibited the optimal balance of mechanical strength and healing capability, achieving a tensile strength of 5.56 MPa (34.9% improvement) and a healing efficiency of 98.9%, outperforming composites filled with untreated HNTs. Dynamic mechanical, rheological, and fatigue analysis demonstrated that increasing m-HNT content progressively enhanced viscoelastic behavior, large viscoelastic region, and fatigue life. These findings demonstrate that the synergistic reinforcement–healing mechanism overcomes the limitations of conventional HNT systems by employing ionic supramolecular interactions as a robust reinforcement strategy, enabling simultaneous mechanical enhancement and highly efficient self-healing in natural rubber nanocomposites.