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08:09
A Technique to Functionalize and Self-assemble Macroscopic Nanoparticle-ligand Monolayer Films onto Template-free Substrates
Published on: May 9, 2014
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Self-association during heterogeneous nucleation onto well-defined templates
Samir A Kulkarni1, Cameron C Weber, Allan S Myerson
1Intensified Reaction & Separation Systems, Process & Energy Laboratory, Delft University of Technology , Leeghwaterstraat 44, 2628CA Delft, The Netherlands.
Langmuir : the ACS Journal of Surfaces and Colloids
|September 27, 2014
Summary
Surface templating with self-assembled monolayers (SAMs) influences the crystallization of isonicotinamide and 2,6-dihydroxybenzoic acid polymorphs. Molecular interactions between the molecules and SAMs dictate the specific crystal forms obtained, impacting solid-state properties.
Area of Science:
- Materials Science
- Crystallography
- Physical Chemistry
Background:
- Understanding molecular crystallization is crucial for controlling solid-state properties.
- Self-assembly of molecules in solution and on surfaces plays a significant role in polymorph selection.
- Self-assembled monolayers (SAMs) offer a tunable surface environment for templating crystallization.
Purpose of the Study:
- To investigate how self-assembled monolayers (SAMs) influence the crystallization of isonicotinamide (INA) and 2,6-dihydroxybenzoic acid (DHB) polymorphs.
- To elucidate the interplay between solution self-association and surface templating effects on crystal nucleation and growth.
- To determine the role of solvent and SAM end-group chemistry in directing polymorph crystallization.
Main Methods:
- Crystallization experiments of INA and DHB in various solvents on different SAMs.
- Characterization of polymorphs using X-ray powder diffraction (XRPD) to identify crystal structure and orientation.
- Spectroscopic analysis (Raman spectroscopy) to probe molecular interactions between solutes and SAMs.
Main Results:
- SAMs can direct the crystallization of specific INA polymorphs (form I or II) in ethanol, contrasting with bulk crystallization outcomes.
- In nitrobenzene and nitromethane, INA crystallization on SAMs yielded the same polymorphs as in bulk solution, suggesting minimal template influence.
- For DHB in toluene and chloroform, all studied SAMs consistently nucleated the stable form 2 polymorph, overriding the solvent-mediated preference for metastable form 1 in toluene.
Conclusions:
- The chemical nature of SAMs and their interactions with solute molecules are critical factors in controlling polymorph crystallization.
- Solvent hydrogen-bonding capabilities and solute self-association behavior significantly influence the effectiveness of surface templating.
- SAMs provide a powerful tool for tailoring crystal polymorphs by mediating molecular interactions at the solid-liquid interface.
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