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Particle size and solvent environment significantly impact the thermodynamic stability of polymorphs during grinding. Nanoscale surface effects can reverse stability, demonstrating thermodynamics control in ball-mill experiments.

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Area of Science:

  • Solid-state chemistry and materials science
  • Crystallography and polymorphism
  • Nanomaterials and surface science

Background:

  • Polymorphism, the ability of a solid material to exist in multiple crystalline forms, significantly affects material properties.
  • Ball-milling techniques, including neat grinding (NG) and liquid-assisted grinding (LAG), are used to induce polymorphic transformations.
  • Understanding the thermodynamic stability of polymorphs under different processing conditions is crucial for material design.

Purpose of the Study:

  • To investigate the influence of particle size and solvent environment on the thermodynamic stability of polymorphs during ball-milling.
  • To determine how neat grinding (NG) and liquid-assisted grinding (LAG) affect polymorphic transformations in cocrystals and disulfide compounds.
  • To elucidate the role of nanoscale surface effects and solvent interactions in controlling polymorphic outcomes.

Main Methods:

  • Ball-mill neat grinding (NG) and liquid-assisted grinding (LAG) experiments were performed on two systems: a theophylline:benzamide cocrystal and an aromatic disulfide compound.
  • Controlled LAG experiments with varying solvent volumes and types were conducted to monitor polymorphic conversions.
  • Ex situ diffraction, electron microscopy, and Density Functional Theory with dispersion corrections (DFT-d) were used to analyze particle size, surface stability, and thermodynamic properties.

Main Results:

  • NG converted stable-bulk polymorphs to metastable-bulk polymorphs in both systems.
  • LAG outcomes varied with solvent amount and nature, allowing derivation of polymorph equilibrium curves.
  • Nanoscale particle sizes (tens of nanometers) were achieved, and DFT-d calculations supported findings on solvent-dependent surface stability and crossover sizes.

Conclusions:

  • The study demonstrates a switch in thermodynamic stability of polymorphs at the nanoscale, driven by surface effects influenced by the solvent environment.
  • Surface properties become critical at the nanoscale, potentially reversing the bulk thermodynamic stability order.
  • Equilibrium outcomes of ball-mill NG and LAG experiments are primarily governed by thermodynamics, with surface effects playing a significant role.