Quantitative Chemical Speciation of Multi-Phase Polymers Using Zone Plate x-ray Microscopy

Phase segregation is important in determining the properties of many complex polymers, including polyurethanes. Achieving a better understanding of the links between formulation, chemical nature of segregated phases, and physical properties, has the potential to aid development of improved polymers....

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Bibliographic Details
Published in:Microscopy and microanalysis 1998-07, Vol.4 (S2), p.808-809
Main Authors: Hitchcock, A.P., Urquhart, S.G., Ade, H., Rightor, E.G., Lidy, W.
Format: Article
Language:English
Subjects:
Analytical chemistry
Chemical analysis
Chemical speciation
Developments in Measuring Polymer Microstructures
Image acquisition
Microscopes
Physical properties
Polymers
Polyurethane
Polyurethane resins
Quantitative analysis
Radiation damage
Spatial analysis
Spatial discrimination
Spatial resolution
Speciation
Spectra
Urea
X ray microscopy
Zone plates
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Summary:Phase segregation is important in determining the properties of many complex polymers, including polyurethanes. Achieving a better understanding of the links between formulation, chemical nature of segregated phases, and physical properties, has the potential to aid development of improved polymers. However, the sub-micron size of segregated features precludes detailed chemical analysis by most existing methods. Zone-plate based, scanning transmission X-ray microscopes (STXM) at NSLS and ALS provide quantitative chemical analysis (speciation) of segregated polymer phases at ∼50 nm spatial resolution. Image sequences acquire much more data with less radiation damage, than spot spectra. After alignment, they provide high quality near edge spectra, and thus quantitative analysis, at full spatial resolution. Fig. 1 shows an image and spectra acquired with the NSLS STXM of a macro-phase segregated TDI polyurethane. Spectral decomposition using model polymer spectra is used to measure the local urea, urethane and polyether content.
ISSN:1431-9276
1435-8115
DOI:10.1017/S1431927600024168