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Structural Characterization of Mesoporous Thin Film Architectures: A Tutorial Overview.
Alberto Alvarez-Fernandez1, Barry Reid1, Maximiliano J Fornerod1
1Department of Chemical Engineering , University College London , Torrington Place , London WC1E 7JE , United Kingdom.
ACS Applied Materials & Interfaces
|January 22, 2020
Summary
Characterizing mesoporous thin films is challenging. This study provides a tutorial overview comparing techniques like SEM, AFM, GISAXS, and EP for reliable structural evaluation of these advanced materials.
Area of Science:
- Materials Science
- Nanotechnology
- Surface Chemistry
Background:
- Mesoporous thin films offer unique properties like high surface area and tunable pore structures.
- Characterizing these films, especially with small sample volumes, presents significant challenges compared to bulk materials.
- Existing techniques often provide incomplete or inconsistent data on pore morphology, size, and porosity.
Purpose of the Study:
- To provide a comprehensive tutorial for the reliable structural characterization of mesoporous thin films.
- To critically assess and compare various characterization techniques for these materials.
- To offer guidelines for implementing these techniques effectively.
Main Methods:
- Utilized three model mesoporous thin film samples prepared via block copolymer (BCP) coassembly with varying porosity and pore size.
- Employed a side-by-side comparison of multiple techniques: Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM), Grazing Incidence Small-Angle X-ray Scattering (GISAXS), and Ellipsometric Porosimetry (EP).
- Evaluated the advantages and limitations of each technique for structural analysis.
Main Results:
- SEM and AFM provide direct visualization of surface and cross-sectional morphology.
- GISAXS offers insights into pore ordering and structure on the nanoscale.
- Ellipsometric Porosimetry (EP) quantifies porosity and pore size distribution through vapor sorption analysis.
Conclusions:
- No single technique provides a holistic evaluation; a combination is necessary for reliable characterization.
- Guidelines are provided for the optimal implementation of SEM, AFM, GISAXS, and EP for mesoporous thin films.
- This work facilitates accurate structural assessment, crucial for understanding and utilizing these advanced materials.
