<p>This study investigates the fabrication of millimeter-sized spherical porous zirconia (ZrO₂) supports using chitosan as a patterning agent. The process is based on pH inversion, where chitosan, dissolved in acidic conditions (proton donors: HCl, CH₃COOH), undergoes gelation upon exposure to an alkaline coagulation bath (NH₄OH, NaOH). This work systematically evaluates how different combinations of strong and weak proton donors and coagulation baths influence chitosan dissolution, gelation, and the structural properties of the resulting ZrO₂ supports. Results demonstrated that, after aging, washing, and sintering at 800 °C, the proton donor significantly affected dispersion viscosity, impacting composition optimization and granule sphericity, with additional effects arising from proton donor–coagulation bath interactions. Elemental and microstructural analyses highlighted the necessity of washing, particularly for NaOH-based systems, to eliminate irregularities and achieve smooth surfaces comparable to those obtained with NH₄OH-based systems. While proton donor–coagulation bath interactions influenced surface properties, porosity (55.5–58.2%), pore size (0.080–0.092 μm), and compressive strength (1.5–1.8 MPa) remained primarily dictated by sintering conditions. Ultimately, the choice of strong/weak, weak/strong, and weak/weak proton donor–coagulation bath combinations provides greater control over material processing and final properties, offering tunability in porous ZrO₂ fabrication.</p><p></p>

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Comparative study of the effect of strong and weak proton donor and coagulation baths on the properties of millimeter-sized spherical porous ZrO2 supports prepared via chitosan gelation

  • Maria Dolores Sosa Lucio,
  • Eun-Ji Oh,
  • Jang-Hoon Ha,
  • Jongman Lee,
  • Hong-Joo Lee,
  • Seung Hwa Jung,
  • Jun Young Shin,
  • Sang-Chae Jeon,
  • In-Hyuck Song

摘要

This study investigates the fabrication of millimeter-sized spherical porous zirconia (ZrO₂) supports using chitosan as a patterning agent. The process is based on pH inversion, where chitosan, dissolved in acidic conditions (proton donors: HCl, CH₃COOH), undergoes gelation upon exposure to an alkaline coagulation bath (NH₄OH, NaOH). This work systematically evaluates how different combinations of strong and weak proton donors and coagulation baths influence chitosan dissolution, gelation, and the structural properties of the resulting ZrO₂ supports. Results demonstrated that, after aging, washing, and sintering at 800 °C, the proton donor significantly affected dispersion viscosity, impacting composition optimization and granule sphericity, with additional effects arising from proton donor–coagulation bath interactions. Elemental and microstructural analyses highlighted the necessity of washing, particularly for NaOH-based systems, to eliminate irregularities and achieve smooth surfaces comparable to those obtained with NH₄OH-based systems. While proton donor–coagulation bath interactions influenced surface properties, porosity (55.5–58.2%), pore size (0.080–0.092 μm), and compressive strength (1.5–1.8 MPa) remained primarily dictated by sintering conditions. Ultimately, the choice of strong/weak, weak/strong, and weak/weak proton donor–coagulation bath combinations provides greater control over material processing and final properties, offering tunability in porous ZrO₂ fabrication.