J. Phys. Chem B 101 (1997) 1950-1960
Spectromicroscopy of Poly(ethylene terephthalate):
Comparison of Spectra and Radiation Damage Rates
In X-ray Absorption and Electron Energy Loss
E.G. Rightor, A. P. Hitchcock,*, H. Ade,§ R. D. Leapman,II S. G. Urquhart,
A. P. Smith,§ G. Mitchell,# D. Fischer^, H. J. ShinO and T. Warwick#
Analytical Sciences, B-1470, Dow Chemical, Freeport, Texas 77541, Department of Chemistry, McMaster University, Hamilton Ontario, Canada L8S 4MI, §Department of Physics, North Carolina State University, Raleigh, North Carolina 27695, IINational Intstitutes of Health, BEIP, NCRR, Bethesda, Maryland 20892, # Analytical Sciences Bldg. 1897, Dow Chemical, Midtown, Michigan 48667, Material Science and Engineering Laboratory, ^National Institute of Standards and Technology, Gaithersburg, Maryland 20899, OPohang Light Source, Pohang, Korea and #Advanced Light Source, Lawrence Berkeley National Lab, Berkeley, California 91420

Received. July 26, 1996, In Final From: November 11, 1990

The C ls and 0 ls X-ray absorption spectra of poly(ethylene terephthalate) (PET) have been recorded using transmission, fluorescence, and electron yield detection. The corresponding electron energy loss spectra (EELS) have been recorded in a scanning transmission electron microscope. 'These results are compared to the C ls and 0 ls spectra of gas phase 1,4-dimethyl terephthalate (the monomer of PET) recorded using EELS. The comparison of monomer and polymer materials in different phases and with different techniques has aided the understanding of the relative strengths and limitations of each technique as well as assisting the spectral interpretation. Good agreement is found in the overall shape and the energies of the spectral features. Relatively minor differences in intensities can be understood in terms of the properties of the individual spectroscopic techniques. The critical dose for radiation damage by 100 keV electrons incident on PET at 100 K is found to be (1.45 ± 0. 15) x 103 eV nm-3. In contrast, the critical dose for radiation damage by 302 eV X-rays incident on PET at 300 K is (1.2 ± 0.6) x 104 eV nm-3. A figure of merit involving the product of critical energy dose and spectral efficiency (as expressed by the appropriate G value) is developed. This indicates that, for near-edge studies involving a 20 eV spectral width, there is ~500-fold advantage of X-ray absorption studies on room temperature PET relative to electron energy loss studies of cooled PET.