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How do layered double hydroxides evolve? First in situ insights into their synthesis processes.

G Doungmo1,2, A F Morais3, D Mustafa3

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This study investigated the crystallization of layered double hydroxides (LDHs) using in situ techniques. Higher reactant concentrations accelerated crystal growth, while increased temperature enhanced crystallite size.

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Area of Science:

  • Materials Science
  • Inorganic Chemistry
  • Crystallography

Background:

  • Layered double hydroxides (LDHs) are crucial materials with applications in catalysis, medicine, and water treatment.
  • The crystallization process of LDHs remains under-investigated, hindering controlled synthesis and optimization.

Purpose of the Study:

  • To investigate the formation dynamics of carbonate-intercalated Mg2+/Al3+ LDHs using in situ characterization.
  • To explore the effects of temperature and reactant concentration on LDH crystallization kinetics and morphology.
  • To provide experimental insights into the nucleation and growth phases of LDH formation.

Main Methods:

  • Utilized a combinatorial multi-modal approach with in situ pH, ion conductivity, and light scattering measurements.
  • Employed synchrotron-based in situ X-ray diffraction (XRD) for real-time structural analysis.
  • Investigated co-precipitation methods under varying temperatures and reactant concentrations.

Main Results:

  • Nuclei formation was indicated by a stable pH due to hydroxyl ion uptake.
  • Crystal growth was detected by light scattering and confirmed by in situ XRD.
  • Increased reactant concentration accelerated crystal growth onset by 70% with minimal impact on crystallite size.
  • Elevated temperatures (up to 65 °C) had a minor effect on kinetics but doubled crystallite size.
  • Reversing reactant addition order led to rapid saturation and formation of ~10 nm crystallites.

Conclusions:

  • In situ characterization provides unprecedented access to LDH formation dynamics.
  • Reactant concentration and temperature are key parameters influencing LDH crystallization kinetics and morphology.
  • Understanding these dynamics enables tailored synthesis of LDHs for specific applications.