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Related Experiment Videos

Polymorph selectivity under nanoscopic confinement.

Jeong-Myeong Ha1, Johanna H Wolf, Marc A Hillmyer

  • 1The Department of Chemical Engineering and Materials Science and the Department of Chemistry, University of Minnesota, 421 Washington Avenue SE, Minneapolis, Minnesota 55455-0431, USA.

Journal of the American Chemical Society
|March 18, 2004
PubMed
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Nanoporous materials enable selective crystallization of anthranilic acid (AA) and ROY polymorphs. Size constraints within ultrasmall pores control nucleation and polymorph selection, offering a new method for controlling crystalline forms.

Area of Science:

  • Materials Science
  • Crystallization Science
  • Nanotechnology

Background:

  • Polymorphism, the ability of a solid material to exist in multiple crystalline forms, significantly impacts material properties.
  • Controlling crystallization to selectively produce desired polymorphs remains a significant challenge in materials science.
  • Anthranilic acid (AA) and ROY (5-methyl-2-[(2-nitrophyenyl)amino]-3-thiophenecarbonitrile) are model compounds for studying polymorphic behavior.

Purpose of the Study:

  • To investigate the effect of nanoporous confinement on the crystallization and polymorphism of AA and ROY.
  • To explore the potential of nanoporous glass and polymer matrices for achieving polymorph selectivity.
  • To understand the role of pore size and material matrix in governing nucleation and crystal form.

Main Methods:

Related Experiment Videos

  • Crystallization experiments using nanoporous glass beads and polymer monoliths (p-PCHE) with controlled pore sizes.
  • Melt crystallization and solution evaporation techniques.
  • Characterization of polymorphs using single-crystal X-ray diffraction and other analytical methods.

Main Results:

  • Selective crystallization of metastable polymorph II of AA in nanopores (<23 nm), with selectivity increasing as pore size decreases.
  • Selective crystallization of the yellow (Y) ROY polymorph in 30-nm p-PCHE pores during solution evaporation.
  • Selective crystallization of the red (R) ROY polymorph from the melt within p-PCHE pores, contrasting with external crystallization.
  • Formation of amorphous ROY in p-PCHE pores, subsequently crystallizing to R nanocrystals upon heating.

Conclusions:

  • Nanoporous materials, including glass and polymers, can effectively control polymorph selectivity during crystallization.
  • Critical size constraints imposed by ultrasmall pores are key factors governing nucleation and polymorph selection.
  • This approach offers a promising new strategy for controlling polymorphism and discovering novel crystalline forms in various organic solids.