scholarly journals Tuning Pore Dimensions of Mesoporous Inorganic Films by Homopolymer Swelling

2019 ◽  
Author(s):  
Barry Reid ◽  
Alberto Alvarez Fernandez ◽  
Benjamin Schmidt-Hansberg ◽  
Stefan Guldin
Keyword(s):  
Pore Size ◽  
Grazing Incidence ◽  
X Ray ◽  
Force Microscopy ◽  
X Ray Scattering ◽  
Atomic Force ◽  
Inorganic Films ◽  
Micelle Size ◽  
Poly Ethylene Oxide ◽  
Poly Ethylene

The functionality and applications of mesoporous inorganic films are closely linked to their mesopore dimensions. For material architectures derived from block copolymer (BCP) micelle co-assembly, the pore size is typically manipulated by changing the molecular weight corresponding to the pore-forming block. However, bespoke BCP synthesis is often a costly and time-consuming process. An alternative method for pore size tuning involves the use of swelling agents, such as homopolymers (HPs), which selectively interact with the core-forming block to increase the micelle size in solution. In this work, poly(isobutylene)-block-poly(ethylene oxide) (PIB-b-PEO) micelles were swollen with poly(isobutylene) HP in solution and co-assembled with aluminosilicate sol with the aim of increasing the resulting pore dimensions. An analytical approach implementing spectroscopic ellipsometry (SE) and ellipsometric porosimetry (EP) alongside the more commonly used atomic force microscopy (AFM) and small angle x-ray scattering in transmission (SAXS) and grazing-incidence (GISAXS) modes enabled to study the material evolution from solution processing through to the manifestation of the mesoporous inorganic film after BCP removal. In-depth SE/EP analysis evidenced an increase of over 40% in mesopore diameter with HP swelling and a consistent scaling of the overall void volume and number of pores. Importantly, our analytical tool-box enabled us to study the effect of swelling on the connecting necks between adjacent pores, with observed increases as high as ≈35%, knowledge of which is crucial to sensing, electrochemical and other mass transfer-dependent applications.

scholarly journals Tuning Pore Dimensions of Mesoporous Inorganic Films by Homopolymer Swelling

2019 ◽  
Author(s):  
Barry Reid ◽  
Alberto Alvarez Fernandez ◽  
Benjamin Schmidt-Hansberg ◽  
Stefan Guldin
Keyword(s):  
Pore Size ◽  
Grazing Incidence ◽  
X Ray ◽  
Force Microscopy ◽  
X Ray Scattering ◽  
Atomic Force ◽  
Inorganic Films ◽  
Micelle Size ◽  
Poly Ethylene Oxide ◽  
Poly Ethylene

The functionality and applications of mesoporous inorganic films are closely linked to their mesopore dimensions. For material architectures derived from block copolymer (BCP) micelle co-assembly, the pore size is typically manipulated by changing the molecular weight corresponding to the pore-forming block. However, bespoke BCP synthesis is often a costly and time-consuming process. An alternative method for pore size tuning involves the use of swelling agents, such as homopolymers (HPs), which selectively interact with the core-forming block to increase the micelle size in solution. In this work, poly(isobutylene)-block-poly(ethylene oxide) (PIB-b-PEO) micelles were swollen with poly(isobutylene) HP in solution and co-assembled with aluminosilicate sol with the aim of increasing the resulting pore dimensions. An analytical approach implementing spectroscopic ellipsometry (SE) and ellipsometric porosimetry (EP) alongside the more commonly used atomic force microscopy (AFM) and small angle x-ray scattering in transmission (SAXS) and grazing-incidence (GISAXS) modes enabled to study the material evolution from solution processing through to the manifestation of the mesoporous inorganic film after BCP removal. In-depth SE/EP analysis evidenced an increase of over 40% in mesopore diameter with HP swelling and a consistent scaling of the overall void volume and number of pores. Importantly, our analytical tool-box enabled us to study the effect of swelling on the connecting necks between adjacent pores, with observed increases as high as ≈35%, knowledge of which is crucial to sensing, electrochemical and other mass transfer-dependent applications.

Nanometer surface gratings on Si(100) characterized by x-ray scattering under grazing incidence and atomic force microscopy

1997 ◽  
Vol 81 (3) ◽  
pp. 1212-1216 ◽  
Author(s):  
T. H. Metzger ◽  
K. Haj-Yahya ◽  
J. Peisl ◽  
M. Wendel ◽  
H. Lorenz ◽  
...  
Keyword(s):  
Atomic Force Microscopy ◽  
Grazing Incidence ◽  
X Ray ◽  
Force Microscopy ◽  
X Ray Scattering ◽  
Atomic Force ◽  
Ray Scattering

scholarly journals Characterization of the shape and line-edge roughness of polymer gratings with grazing incidence small-angle X-ray scattering and atomic force microscopy

2016 ◽  
Vol 49 (3) ◽  
pp. 823-834 ◽  
Author(s):  
Hyo Seon Suh ◽  
Xuanxuan Chen ◽  
Paulina A. Rincon-Delgadillo ◽  
Zhang Jiang ◽  
Joseph Strzalka ◽  
...  
Keyword(s):  
Atomic Force Microscopy ◽  
Grazing Incidence ◽  
Line Edge Roughness ◽  
X Ray ◽  
Force Microscopy ◽  
X Ray Scattering ◽  
Atomic Force ◽  
Edge Roughness ◽  
Average Shape ◽  
Polymer Gratings

Grazing-incidence small-angle X-ray scattering (GISAXS) is increasingly used for the metrology of substrate-supported nanoscale features and nanostructured films. In the case of line gratings, where long objects are arranged with a nanoscale periodicity perpendicular to the beam, a series of characteristic spots of high-intensity (grating truncation rods, GTRs) are recorded on a two-dimensional detector. The intensity of the GTRs is modulated by the three-dimensional shape and arrangement of the lines. Previous studies aimed to extract an average cross-sectional profile of the gratings, attributing intensity loss at GTRs to sample imperfections. Such imperfections are just as important as the average shape when employing soft polymer gratings which display significant line-edge roughness. Herein are reported a series of GISAXS measurements of polymer line gratings over a range of incident angles. Both an average shape and fluctuations contributing to the intensity in between the GTRs are extracted. The results are critically compared with atomic force microscopy (AFM) measurements, and it is found that the two methods are in good agreement if appropriate corrections for scattering from the substrate (GISAXS) and contributions from the probe shape (AFM) are accounted for.

scholarly journals Molecular and Structure–Properties Comparison of an Anionically Synthesized Diblock Copolymer of the PS-b-PI Sequence and Its Hydrogenated or Sulfonated Derivatives

Polymers ◽  
2021 ◽  
Vol 13 (23) ◽  
pp. 4167
Author(s):  
Nikolaos Politakos ◽  
Ioannis Moutsios ◽  
Gkreti-Maria Manesi ◽  
Konstantinos Artopoiadis ◽  
Konstantina Tsitoni ◽  
...  
Keyword(s):  
Chemical Modification ◽  
Diblock Copolymer ◽  
Film Structure ◽  
X Ray ◽  
Force Microscopy ◽  
Annealing Temperatures ◽  
X Ray Scattering ◽  
Atomic Force ◽  
Poly Ethylene ◽  
Structure Properties

An approach to obtaining various nanostructures utilizing a well-studied polystyrene-b-poly(isoprene) or PS-b-PI diblock copolymer system through chemical modification reactions is reported. The complete hydrogenation and partial sulfonation to the susceptible carbon double bonds of the PI segment led to the preparation of [polystyrene-b-poly(ethylene-alt-propylene)] as well as [polystyrene-b-poly(sulfonated isoprene-co-isoprene)], respectively. The hydrogenation of the polyisoprene block results in enhanced segmental immiscibility, whereas the relative sulfonation induces an amphiphilic character in the final modified material. The successful synthesis of the pristine diblock copolymer through anionic polymerization and the relative chemical modification reactions were verified using several molecular and structural characterization techniques. The thin film structure–properties relationship was investigated using atomic force microscopy under various conditions such as different solvents and annealing temperatures. Small-angle X-ray scattering was employed to identify the different observed nanostructures and their evolution upon thermal annealing.

Growth of thermally stable crystalline C60 films on flat-lying copper phthalocyanine

2016 ◽  
Vol 4 (3) ◽  
pp. 1028-1032 ◽  
Author(s):  
Terry McAfee ◽  
Aubrey Apperson ◽  
Harald Ade ◽  
Daniel B. Dougherty
Keyword(s):  
Copper Phthalocyanine ◽  
Grazing Incidence ◽  
Thermally Stable ◽  
X Ray ◽  
Force Microscopy ◽  
Cupc Film ◽  
X Ray Scattering ◽  
Atomic Force ◽  
Stable Growth ◽  
C60 Films

We observe thermally stable growth of fcc(111) films of fullerene-C60 on top of crystalline, flat-lying, CuPc film structures on graphite using combined grazing incidence wide-angle X-ray scattering and atomic force microscopy.

scholarly journals Bicontinuous Gyroid Phase of a Water-Swollen Wedge-Shaped Amphiphile: Studies with In-Situ Grazing-Incidence X-ray Scattering and Atomic Force Microscopy

Materials ◽  
2021 ◽  
Vol 14 (11) ◽  
pp. 2892
Author(s):  
Kseniia N. Grafskaia ◽  
Azaliia F. Akhkiamova ◽  
Dmitry V. Vashurkin ◽  
Denis S. Kotlyarskiy ◽  
Diego Pontoni ◽  
...  
Keyword(s):  
Atomic Force Microscopy ◽  
Environmental Conditions ◽  
Grazing Incidence ◽  
X Ray ◽  
Force Microscopy ◽  
X Ray Scattering ◽  
Atomic Force ◽  
Double Gyroid ◽  
Ray Scattering

We report on formation of a bicontinuous double gyroid phase by a wedge-shaped amphiphilic mesogen, pyridinium 4′-[3″,4″,5″-tris-(octyloxy)benzoyloxy]azobenzene-4-sulfonate. It is found that this compound can self-organize in zeolite-like structures adaptive to environmental conditions (e.g., temperature, humidity, solvent vapors). Depending on the type of the phase, the structure contains 1D, 2D, or 3D networks of nanometer-sized ion channels. Of particular interest are bicontinuous phases, such as the double gyroid phase, as they hold promise for applications in separation and energy. Specially designed environmental cells compatible with grazing-incidence X-ray scattering and atomic force microscopy enable simultaneous measurements of structural parameters/morphology during vapor-annealing treatment at different temperatures. Such in-situ approach allows finding the environmental conditions at which the double gyroid phase can be formed and provide insights on the supramolecular structure of thin films at different spatial levels.

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