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Determination of microphase structure and scale and scale of mixing in poly‐ε‐caprolactone (PCL)/poly(vinyl chloride) (PVC) blend by high‐resolution solid‐state 13 C‐NMR spectroscopy with magic angle spinning and cross polarization
Author(s) -
Kwak S.Y.
Publication year - 1994
Publication title -
journal of applied polymer science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.575
H-Index - 166
eISSN - 1097-4628
pISSN - 0021-8995
DOI - 10.1002/app.1994.070531312
Subject(s) - magic angle spinning , vinyl chloride , spin diffusion , materials science , solid state nuclear magnetic resonance , spectroscopy , caprolactone , nuclear magnetic resonance spectroscopy , polymer , polymer blend , analytical chemistry (journal) , polymer chemistry , polymerization , nuclear magnetic resonance , chemistry , diffusion , thermodynamics , composite material , copolymer , organic chemistry , physics , quantum mechanics
High‐resolution solid‐state, pulsed Fourier‐transform (FT) 13 C‐nuclear magnetic resonance (NMR) spectroscopy with magic angle spinning (MAS) and cross polarization (CP) was applied to a mechanical blend of poly‐ε‐caprolactone (PCL) and poly(vinyl chloride) (PVC) with 50/50 weight ratio (%) whose composition results in very complex morphology and phase structure in the solid state. Proton spin‐lattice relaxation times, T 1 ( 1 H) and T 1ρ ( 1 H), were used as a probe to determine the microphase structure, the degree of homogeneity in terms of the domain size, and the state of mixing of the blend. In particular, T 1ρ ( 1 H) was shown to be able to distinguish the separated domains at a level of a few nanometers; the scale of mixing was evaluated from the approximation based on spin‐diffusion phenomenon to be ∼ 4.7 nm below which two polymers were partially mixed and above which they were homogeneously mixed. Treatment of the T 1ρ ( 1 H) data with two exponential decay functions resulted in a resolution of individual T 1ρ ( 1 H) into rigid and mobile components, from which more detailed information on the phase structure and state of mixing were obtained. © 1994 John Wiley & Sons, Inc.