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

Published online by Cambridge University Press:  02 July 2020

A.P. Hitchcock ,
S.G. Urquhart ,
H. Ade ,
E.G. Rightor  and
W. Lidy
A.P. Hitchcock
Affiliation:
BIMR, McMaster University, Hamilton ON Canada, L8S 4M1
S.G. Urquhart
Affiliation:
Physics, North Carolina State University, Raleigh, NC27895
H. Ade
Affiliation:
Physics, North Carolina State University, Raleigh, NC27895
E.G. Rightor
Affiliation:
Dow Chemical, B-1470, 2301 N. Brazosport Blvd, Freeport, TX77541
W. Lidy
Affiliation:
Dow Chemical, B-1470, 2301 N. Brazosport Blvd, Freeport, TX77541
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Extract

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.

Type
Developments in Measuring Polymer Microstructures
Information
Microscopy and Microanalysis , Volume 4 , Issue S2: Proceedings: Microscopy & Microanalysis '98, Microscopy Society of America 56th Annual Meeting, Microbeam Analysis Society 32nd Annual Meeting, Atlanta, Georgia July 12-16, 1998 , July 1998 , pp. 808 - 809
Copyright
Copyright © Microscopy Society of America

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References

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6. We thank Chris Jacobsen for developing and assisting us with stacks; and Tony Warwick. NSLS & ALS are operated by Dept. of Energy (DE-AC03-76SF00098).Google Scholar