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Application of Small‐Angle X‐Ray Scattering as a Tool for the Structural Analysis of Industrial Polymer Dispersions
Author(s) -
Bolze Joerg,
Ballauff Matthias,
Kijlstra Johan,
Rudhardt Daniel
Publication year - 2003
Publication title -
macromolecular materials and engineering
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.913
H-Index - 96
eISSN - 1439-2054
pISSN - 1438-7492
DOI - 10.1002/mame.200390046
Subject(s) - small angle x ray scattering , materials science , dispersity , polymer , scattering , particle (ecology) , emulsion polymerization , monomer , particle size , dynamic light scattering , particle size distribution , analytical chemistry (journal) , chemical engineering , polymer chemistry , chemical physics , composite material , optics , chromatography , nanoparticle , nanotechnology , chemistry , physics , oceanography , engineering , geology
Small‐angle X‐ray scattering (SAXS) was applied for the structural analysis of an industrial polymer dispersion in water (synthetic latex). For the preparation of the spherical latex particles under investigation, butadiene, styrene, and acrylic acid were used as monomers in a seeded emulsion polymerization process. The product is widely being used as a film‐forming agent for coatings in the paper‐making industry. It is demonstrated that by measuring the SAXS curves at different contrasts the overall particle size, mass density, polydispersity, and degree of heterogeneity can be estimated with a good accuracy, even without the necessity of a detailed fitting procedure. In particular, one obtains information about the spatial distribution of the various monomer units within the particles. Five isoscattering points could be observed in the contrast variation measurements and the scattering curves at all contrasts could be modeled with a fully consistent set of fit parameters. It is thus safe to conclude that the contrast agent sucrose does not affect the particle structure. A quantitative fitting of the experimental data set revealed that a significant amount of the poly(acrylic acid) is preferentially located in a thin shell of ca. 2 nm thickness around the core of the particles, that is mainly formed by poly(styrene‐ co ‐butadiene). The obtained results are fully consistent with additional measurements of the particle mass density, of the hydrodynamic particle radius by dynamic light scattering, and of the particle surface charge by potentiometric titration. It is concluded that SAXS is a highly useful tool for characterizing the structure of industrial latexes.SAXS data of a BAYSTAL® latex measured at various contrasts, the weight fraction of sucrose in the dispersion medium is given in the legend.