Characterizing the Core-Shell Architecture of Block Copolymer Nanoparticles with Electron Microscopy: A Multi-Technique Approach

Electron microscopy has proved to be a major tool to study the structure of self-assembled amphiphilic block copolymer particles. These specimens, like supramolecular biological structures, are problematic for electron microscopy because of their poor capacity to scatter electrons and their suscepti...

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Main Authors: Vitalii Tkachenko, Loïc Vidal, Ludovic Josien, Marc Schmutz, Julien Poly, Abraham Chemtob
Format: Article
Language:English
Published: MDPI AG 2020-07-01
Series:Polymers
Subjects:
Online Access:https://www.mdpi.com/2073-4360/12/8/1656
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author Vitalii Tkachenko
Loïc Vidal
Ludovic Josien
Marc Schmutz
Julien Poly
Abraham Chemtob
author_facet Vitalii Tkachenko
Loïc Vidal
Ludovic Josien
Marc Schmutz
Julien Poly
Abraham Chemtob
author_sort Vitalii Tkachenko
collection DOAJ
description Electron microscopy has proved to be a major tool to study the structure of self-assembled amphiphilic block copolymer particles. These specimens, like supramolecular biological structures, are problematic for electron microscopy because of their poor capacity to scatter electrons and their susceptibility to radiation damage and dehydration. Sub-50 nm core-shell spherical particles made up of poly(hydroxyethyl acrylate)–<i>b</i>–poly(styrene) are prepared via polymerization-induced self-assembly (PISA). For their morphological characterization, we discuss the advantages, limitations, and artefacts of TEM with or without staining, cryo-TEM, and SEM. A number of technical points are addressed such as precisely shaping of particle boundaries, resolving the particle shell, differentiating particle core and shell, and the effect of sample drying and staining. TEM without staining and cryo-TEM largely evaluate the core diameter. Negative staining TEM is more efficient than positive staining TEM to preserve native structure and to visualize the entire particle volume. However, no technique allows for a satisfactory imaging of both core and shell regions. The presence of long protruding chains is manifested by patched structure in cryo-TEM and a significant edge effect in SEM. This manuscript provides a basis for polymer chemists to develop their own specimen preparations and to tackle the interpretation of challenging systems.
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spelling doaj.art-6df06562b50a491b9d41fbab9217d0392023-11-20T07:57:23ZengMDPI AGPolymers2073-43602020-07-01128165610.3390/polym12081656Characterizing the Core-Shell Architecture of Block Copolymer Nanoparticles with Electron Microscopy: A Multi-Technique ApproachVitalii Tkachenko0Loïc Vidal1Ludovic Josien2Marc Schmutz3Julien Poly4Abraham Chemtob5Université de Haute-Alsace, CNRS, IS2M UMR7361, F-68100 Mulhouse, FranceUniversité de Haute-Alsace, CNRS, IS2M UMR7361, F-68100 Mulhouse, FranceUniversité de Haute-Alsace, CNRS, IS2M UMR7361, F-68100 Mulhouse, FranceUniversité de Strasbourg, CNRS, ICS UPR22, F-67034 Strasbourg, FranceUniversité de Haute-Alsace, CNRS, IS2M UMR7361, F-68100 Mulhouse, FranceUniversité de Haute-Alsace, CNRS, IS2M UMR7361, F-68100 Mulhouse, FranceElectron microscopy has proved to be a major tool to study the structure of self-assembled amphiphilic block copolymer particles. These specimens, like supramolecular biological structures, are problematic for electron microscopy because of their poor capacity to scatter electrons and their susceptibility to radiation damage and dehydration. Sub-50 nm core-shell spherical particles made up of poly(hydroxyethyl acrylate)–<i>b</i>–poly(styrene) are prepared via polymerization-induced self-assembly (PISA). For their morphological characterization, we discuss the advantages, limitations, and artefacts of TEM with or without staining, cryo-TEM, and SEM. A number of technical points are addressed such as precisely shaping of particle boundaries, resolving the particle shell, differentiating particle core and shell, and the effect of sample drying and staining. TEM without staining and cryo-TEM largely evaluate the core diameter. Negative staining TEM is more efficient than positive staining TEM to preserve native structure and to visualize the entire particle volume. However, no technique allows for a satisfactory imaging of both core and shell regions. The presence of long protruding chains is manifested by patched structure in cryo-TEM and a significant edge effect in SEM. This manuscript provides a basis for polymer chemists to develop their own specimen preparations and to tackle the interpretation of challenging systems.https://www.mdpi.com/2073-4360/12/8/1656core-shellTEMcryo-TEMSEMpositive stainingnegative staining
spellingShingle Vitalii Tkachenko
Loïc Vidal
Ludovic Josien
Marc Schmutz
Julien Poly
Abraham Chemtob
Characterizing the Core-Shell Architecture of Block Copolymer Nanoparticles with Electron Microscopy: A Multi-Technique Approach
Polymers
core-shell
TEM
cryo-TEM
SEM
positive staining
negative staining
title Characterizing the Core-Shell Architecture of Block Copolymer Nanoparticles with Electron Microscopy: A Multi-Technique Approach
title_full Characterizing the Core-Shell Architecture of Block Copolymer Nanoparticles with Electron Microscopy: A Multi-Technique Approach
title_fullStr Characterizing the Core-Shell Architecture of Block Copolymer Nanoparticles with Electron Microscopy: A Multi-Technique Approach
title_full_unstemmed Characterizing the Core-Shell Architecture of Block Copolymer Nanoparticles with Electron Microscopy: A Multi-Technique Approach
title_short Characterizing the Core-Shell Architecture of Block Copolymer Nanoparticles with Electron Microscopy: A Multi-Technique Approach
title_sort characterizing the core shell architecture of block copolymer nanoparticles with electron microscopy a multi technique approach
topic core-shell
TEM
cryo-TEM
SEM
positive staining
negative staining
url https://www.mdpi.com/2073-4360/12/8/1656
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AT ludovicjosien characterizingthecoreshellarchitectureofblockcopolymernanoparticleswithelectronmicroscopyamultitechniqueapproach
AT marcschmutz characterizingthecoreshellarchitectureofblockcopolymernanoparticleswithelectronmicroscopyamultitechniqueapproach
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AT abrahamchemtob characterizingthecoreshellarchitectureofblockcopolymernanoparticleswithelectronmicroscopyamultitechniqueapproach