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Cross‐linking of polybutadiene: correlation between solid‐state 1 H NMR spectroscopy, thermoporosimetry, densimetry and crystallinity measurements
Author(s) -
Pilichowski JeanFrancois,
Liptaj Tibor,
Morel Myriam,
Terriac Emmanuel,
Baba Mohamed
Publication year - 2003
Publication title -
polymer international
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.592
H-Index - 105
eISSN - 1097-0126
pISSN - 0959-8103
DOI - 10.1002/pi.1384
Subject(s) - polybutadiene , macromolecule , elastomer , materials science , polymer , crystallinity , solubility , swelling , solvent , polymer chemistry , chemistry , organic chemistry , copolymer , composite material , biochemistry
T 2 proton NMR relaxation times were used to follow the changes in the macromolecular chain mobility of a chemically (by dicumyl peroxide) cross‐linked polybutadiene matrix. The same phenomenon was also studied by an investigation of the ability of the polymer to crystallize using DSC measurements. The solubility of the elastomer depends on the size of its macromolecular chains. Cross‐linking, leading to an increase in the size of macromolecules, provokes an insolubility of the elastomer. By densimetry measurements, it was possible to follow the changes in the solubility of the polymer up to its gel‐point. Beyond the gel‐point, the swelling solvent, cyclohexane, was used as a textural probe. Using the shift of its solid‐solid thermal transition points, it was possible to calculate the distribution of the distances between the cross‐links as a function of the curing times by thermoporosimetry analysis. Copyright © 2003 Society of Chemical Industry