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 ◽  
...  

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.

2019 ◽  
Author(s):  
Barry Reid ◽  
Alberto Alvarez Fernandez ◽  
Benjamin Schmidt-Hansberg ◽  
Stefan Guldin

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.


2019 ◽  
Author(s):  
Barry Reid ◽  
Alberto Alvarez Fernandez ◽  
Benjamin Schmidt-Hansberg ◽  
Stefan Guldin

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.


2007 ◽  
Vol 1027 ◽  
Author(s):  
Do Young Noh ◽  
Ki-Hyun Ryu ◽  
Hyon Chol Kang

AbstractThe transformation of Au thin films grown on sapphire (0001) substrates into nano crystals during thermal annealing was investigated by in situ synchrotron x-ray scattering and ex situ atomic force microscopy (AFM). By monitoring the Au(111) Bragg reflection and the low Q reflectivity and comparing them with ex situ AFM images, we found that polygonal-shape holes were nucleated and grow initially. As the holes grow larger and contact each other, their boundary turns into Au nano crystals. The Au nano crystals have a well-defined (111) flat top surface and facets in the in-plane direction.


2021 ◽  
Vol 54 (6) ◽  
Author(s):  
Roman Pleshkov ◽  
Nikolay Chkhalo ◽  
Vladimir Polkovnikov ◽  
Mikhail Svechnikov ◽  
Maria Zorina

The structures of Cr/Be multilayer mirror interfaces are investigated using X-ray reflectometry, diffuse X-ray scattering and atomic force microscopy. The combination of these methods makes it possible to separate the contributions of roughness and interlayer diffusion/intermixing for each sample. In the range of period thicknesses of 2.26–0.8 nm, it is found that the growth roughness of the Cr/Be multilayer mirrors does not depend on the period thickness and is ∼0.2 nm. The separation of roughness and diffuseness allows estimation of layer material intermixing and the resulting drop in the optical contrast, which is from 0.85 to 0.17 in comparison with an ideally sharp structure.


1999 ◽  
Vol 38 (4) ◽  
pp. 684 ◽  
Author(s):  
Victor E. Asadchikov ◽  
Angela Duparré ◽  
Stefan Jakobs ◽  
Albert Yu. Karabekov ◽  
Igor V. Kozhevnikov ◽  
...  

2000 ◽  
Vol 662 ◽  
Author(s):  
Elizabeth E. Shen ◽  
Hsin-Lung Chen ◽  
Balaji Narasimhan

AbstractThis research examines the microstructure of polyanhydride blends for use in drug delivery devices. Atomic force microscopy (AFM) and small-angle X-ray scattering (SAXS) studies were performed on the homopolymers and blends of the polyanhydrides poly(1,6-carboxyphenoxy hexane) (CPH) and poly(sebacic anhydride) (SA). AFM of the CPH/SA blends 20:80, 50:50, and 80:20 showed distinct patterns indicating spinodal decomposition and phase separation on the micron-scale. Because it has been shown that incorporated drugs will thermodynamically partition into phase-separated domains depending on their hydrophobicity, polyanhydride blends will be able to encapsulate larger bioactive compounds including nucleotides, proteins, and vaccines. Preliminary SAXS studies of the CPH/SA blend systems provide information on the crystalline morphology of the polymer. A peak shift to a lower q from poly(SA) to the blends indicates that the poly(CPH) is incorporated into and causes swelling of the interlamellar amorphous regions of poly(SA).


Nanoscale ◽  
2019 ◽  
Vol 11 (10) ◽  
pp. 4463-4470 ◽  
Author(s):  
Maxim A. Shcherbina ◽  
Oleg V. Borshchev ◽  
Alexandra P. Pleshkova ◽  
Sergei A. Ponomarenko ◽  
Sergei N. Chvalun

Several generations of carbosilane dendrimers with quaterthiophene end groups were studied by X-ray scattering, differential scanning calorimetry, polarizing optical and atomic force microscopy and molecular modelling.


2006 ◽  
Author(s):  
M. L. Zanaveskin ◽  
Yu. V. Grishchenko ◽  
A. L. Tolstikhina ◽  
V. E. Asadchikov ◽  
B. S. Roshchin ◽  
...  

Sign in / Sign up

Export Citation Format

Share Document