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High Pressure-Based Synthesis of Nanoporous Metal-Organic Framework ZIF-93 Giving Rise to a Phase for Proton
Marta Pérez-Miana1,2, Roberto Fernández de Luis3, Arkaitz Fidalgo-Marijuan3,4
1Instituto de Nanociencia y Materiales de Aragón (INMA), CSIC-Universidad de Zaragoza, Zaragoza 50018, Spain.
ACS Applied Nano Materials
|November 6, 2025
Summary
A novel, high-pressure, solvent-free synthesis yielded ZIF-93_HP, a new zeolitic imidazolate framework phase. This discovery opens avenues for exploring new ZIF materials with unique properties like proton conductivity.
Area of Science:
- Materials Science: Synthesis and characterization of novel nanoporous materials.
- Chemistry: Development of green synthesis methods for metal-organic frameworks.
Background:
- Zeolitic imidazolate frameworks (ZIFs) are a class of metal-organic frameworks with diverse applications.
- Traditional solvothermal synthesis methods can be limited in accessing certain ZIF phases.
- Green chemistry principles encourage the development of solvent-free synthesis routes.
Purpose of the Study:
- To develop a green, solvent-free synthesis for ZIF-93 and explore new phases.
- To investigate the formation of a novel high-pressure ZIF phase, ZIF-93_HP.
- To characterize ZIF-93_HP and evaluate its properties, including proton conductivity.
Main Methods:
- Solvent-free synthesis of ZIF-93_HP using zinc oxide under high pressure (150 MPa) and elevated temperature (110 °C).
- Systematic investigation of synthesis parameters, including NH4NO3 promoter concentration and reaction steps.
- Extensive material characterization using X-ray diffraction, thermogravimetry, electron microscopy, and gas adsorption (N2, CO2).
Main Results:
- Successful synthesis of a new nanoporous ZIF phase, ZIF-93_HP (Zn-(C5N2OH5)2·1.2-(NH4NO3)·(H2O)).
- Optimization of synthesis conditions to maximize ZIF-93_HP yield and prevent conversion to ZIF-93.
- ZIF-93_HP exhibits proton conductivity (3.76 × 10^-3 S/cm) at room temperature and moisture, which decreases with increasing temperature.
- Water washing transforms ZIF-93_HP into ZIF-93, significantly increasing BET surface area from 4 to 181 m²/g.
Conclusions:
- High-pressure, solvent-free synthesis is a powerful method for discovering new ZIF phases inaccessible via traditional methods.
- ZIF-93_HP demonstrates promising proton conductivity, highlighting its potential for specific applications.
- This approach expands the landscape of reticular materials, enabling the discovery of structures with unique properties.
Keywords:
ZIF-93high-pressure synthesismetal−organic frameworksolventless synthesiszeolitic imidazolate framework
