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Topochemical Modulations from 1D Iron Fluoride Precursor to 3D Frameworks.

Arindam Ghosh1,2,3, Dereje Bekele Tekliye4, Emily E Foley5

  • 1New Chemistry Unit, Bangalore, Jakkur 560064, India.

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|July 22, 2024
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Summary

Researchers developed a new topochemical method to create diverse 3D iron fluoride frameworks from a 1D precursor. This approach offers greater control over structural dimensionality and connectivity in inorganic materials.

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Area of Science:

  • Materials Science
  • Inorganic Chemistry
  • Solid-State Chemistry

Background:

  • Topochemical reactions are key for modifying inorganic structures but have limitations in controlling structural connectivity and dimensionality.
  • Existing methods often restrict the ability to tune the architecture of extended inorganic materials.

Purpose of the Study:

  • To introduce a novel bottom-up topochemical strategy for synthesizing diverse three-dimensional (3D) iron fluoride frameworks.
  • To explore the formation mechanism and influencing factors of these 3D frameworks derived from a one-dimensional (1D) precursor.

Main Methods:

  • Utilized a one-dimensional (1D) iron(III) fluoride trihydrate (FeF3·3H2O) precursor.
  • Performed topochemical reactions with various iodide-based reagents (AI; A+ = Na+, K+, NH4+) under controlled conditions (concentration, temperature, duration).
  • Analyzed products using X-ray diffraction, nuclear magnetic resonance, and Mössbauer spectroscopy; employed density functional theory (DFT) calculations.

Main Results:

  • Successfully synthesized diverse 3D iron fluoride phases including hexagonal tungsten bronze (HTB)-type AFeF3, weberite-Na1.95Fe2F7, tetragonal tungsten bronze (TTB)-K0.58FeF3, and pyrochlore-NH4Fe2F6.
  • Demonstrated that varying the molar ratio of AI:IF influences the resulting crystal structure.
  • DFT calculations confirmed the thermodynamic stability of the formed iron fluoride phases, with kinetics playing a crucial role in achieving high purity for weberite and HTB phases.

Conclusions:

  • Established a versatile topochemical bottom-up approach to tailor 3D iron fluoride frameworks from a 1D precursor.
  • Highlighted the importance of both thermodynamic and kinetic factors in controlling the outcome of topochemical reactions.
  • This work expands the possibilities for designing complex inorganic structures with tunable dimensionality and connectivity.