Skip to main content Accessibility help
×
Home
Hostname: page-component-78bd46657c-2pqp7 Total loading time: 0.135 Render date: 2021-05-09T23:03:03.560Z Has data issue: true Feature Flags: { "shouldUseShareProductTool": true, "shouldUseHypothesis": true, "isUnsiloEnabled": true, "metricsAbstractViews": false, "figures": false, "newCiteModal": false, "newCitedByModal": true }

X-ray Microscopy of Polymeric Materials

Published online by Cambridge University Press:  15 February 2011

H. Adel
Affiliation:
Dept. of Physics, North Carolina State University, Raleigh, NC 27695–8202
B. Hsiao
Affiliation:
Experimental Station, DuPont, Wilmington, DE 19880–0302
G. Mitchell
Affiliation:
Analytical Science Laboratory, Dow Chemical, Midland, MI 48667
E. Rightor
Affiliation:
Texas Polymer Center, B-1470, Dow Chemical, Freeport, TX 77541
A. P. Smith
Affiliation:
Dept. of Physics, North Carolina State University, Raleigh, NC 27695–8202
R. Cieslinski
Affiliation:
Experimental Station, DuPont, Wilmington, DE 19880–0302
Get access

Abstract

We describe how the scanning transmission x-ray microscope at Brookhaven National Laboratory can be used to investigate the bulk characteristics of polymeric materials with chemical sensitivity at a spatial resolution of about 50 nm. We present examples ranging from unoriented multiphase polymers to highly oriented Kevlar fibers. In the case of oriented samples, a dichroism technique is used to determine the orientation of specific chemical bonds. Extension of the technique to investigate surfaces of thick samples is discussed.

Type
Research Article
Copyright
Copyright © Materials Research Society 1995

Access options

Get access to the full version of this content by using one of the access options below.

References

1. For a review of the established methods and developments over the last decade, see X-ray Microscopy, Schmahl, G. and Rudolf, D., eds. (Springer, Berlin, 1984), X-ray Microscopy II, D. Sayre, M. Howells, J. Kirz, and H. Rarback, eds. (Springer, Berlin, 1988), and X-ray Microscopy III, A. Michette, G. Morrison, and C. Buckley, eds. (Springer, Berlin 1992).CrossRefGoogle Scholar
2. Kirz, J., Burge, R., and Rarback, H., Ann. NY. Acad. Sci 342, 135147 (1980), J. Kirz, H. Ade, M. Howells, C. Jacosen, K. H. Ko, S. Lindaas, I. Macnulty, D. Sayre, S. Williams, and X. Zhang, Rev. Sci. Instrum. 63, 557–563 (1992).CrossRefGoogle Scholar
3. Ade, H., Zhang, X., Cameron, S., Costello, C., Kirz, J., and Williams, S., Science 258, 972 (1992).CrossRefGoogle Scholar
4. Ade, H., Smith, A. P., Cameron, S., Cieslinski, R., Hsiao, B., Mitchell, G., Rightor, E. (to be printed in Polymer, 36, (1995)).CrossRefGoogle Scholar
5. see, for example, Stöhr, J., NEXAFS Spectroscopy (Springer, Berlin, 1992) and references therein. F. Sette, J. Stöhr, and A. P. Hitchcock, J. Chem. Phys. 81, 4906 (1984), D. A. Outka et al., Phys. Rev. Lett. 59, 1321 (1987), C. Tourillon at al., Surface Science 201, 171 (1988).CrossRefGoogle Scholar
6. See, for example, Transmission Electron Energy Loss Spectrometry in Materials Science, Disko, M. M., Ahn, C. C., and Fultz, B., eds. (TMS, Warrendale, PA, 1992).Google Scholar
7. Rarback, H. et al., J. X-ray Sci. Technol. 2, 274 (1992).CrossRefGoogle Scholar
8. Anderson, E. and Kern, D., in X-ray Microscopy III, eds. Michette, A., Morrison, G., and Buckley, C., eds. (Springer, Berlin 1992).Google Scholar
9. Jacobsen, C., Williams, S., Anderson, E., Brown, M. T., Buckley, C. J., Kern, D., Kirz, J., Rivers, M., and Zhang, X., Optics Comm. 86, 351 (1991).CrossRefGoogle Scholar
10. Zhang, X., Jacobsen, C., and Williams, S., Proc. SPIE, 1741, 251259 (1992).CrossRefGoogle Scholar
11. The absolute energy calibration is not known to better than about 0.5 eV for these data. Energies quoted to a “precision” better than 0.5 eV are therefore only relevant in the context of energy differences within the short time of the same experiment and sample. Since NEXAFS imaging and micro-spectroscopy are new operating modes of the XI-STXM, in the beginning we did not have the necessary procedures in place to easily calibrate the monochromator with sufficient energy resolution. In addition, during acquisition of the spectra of Figs. 2 and 4, the X 1A monochromator did not have a linear energy scale.Google Scholar
12. for previous EELS work of PET and molecular analoques see Hitchcock, A. P. and Urquhart, S. G. and Rightor, E. G., J. Phys. Chem. 96, 8736 (1992). and E. Rightor et al., Microbeam Analysis 2, S264 (1993). A PET NEXAFS spectrum without spatial resolution is also presented in the latter reference.CrossRefGoogle Scholar
13. Armisted, J., Wilkes, G., and Turner, R., J. Appl. Pol. Sci., 35, 601 (1988). D. Okamoto, E. O'Connelki, S. Cooper, T. Root and references therein, J. Polym. Sci., 31, 1163 (1993).CrossRefGoogle Scholar
14. Urquhart, S. G., Hitchcock, A. P., Leapman, R. D., Priester, R. D., and Rightor, E. G. (submitted to J. Polym. Sci. B: Polymer Physics).Google Scholar
15. Urquhart, S. G., Hitchcock, A. P., Priester, R. D., and Rightor, E. G. (submitted to J. Polym. Sci. B: Polymer Physics).Google Scholar
16. Ade, H. and Hsiao, B., Science 262, 14271429 (1993).CrossRefGoogle Scholar
17. Yang, H. H., Aromatic High Strength Fibers (Wiley-Interscience Pub., New York, 1989).Google Scholar
18. Zhang, X. (private communication).Google Scholar
19. Buckley, C. J., Foster, G. F., Burge, R. E., Ali, S. Y., Scotchford, C. A., Kirz, J., and Rivers, M. L., Rev. Sci. Instrum. 63, 588590, (1992).CrossRefGoogle Scholar
20. Cody, G. (private communication).Google Scholar
21. Tonner, B. and Harp, G., Rev. Sci. Instr. 59, 853 (1988), G. R. Harp, Z. L. Han, and B.P. Tonner, J.Vac.Sci. Technol. A 8, 2566 (1990), J. Stohr, Y. Wu, B. D. Hermsmeier, M. B. Samant, G. R. Harp, S. Koranda, D. Dunham, B. P. Tonner, Science 259, 658 (1993).CrossRefGoogle Scholar
22. Ade, H., Kirz, J., Hulbert, S., Johnson, E., Anderson, E., and Kern, D., Appl. Phys. Lett. 56, 18411843 (1990), H. Ade, Nucl. Instr. Method. in Phys. Res. A 319, 311–319 (1992).CrossRefGoogle Scholar

Send article to Kindle

To send this article to your Kindle, first ensure no-reply@cambridge.org is added to your Approved Personal Document E-mail List under your Personal Document Settings on the Manage Your Content and Devices page of your Amazon account. Then enter the ‘name’ part of your Kindle email address below. Find out more about sending to your Kindle. Find out more about sending to your Kindle.

Note you can select to send to either the @free.kindle.com or @kindle.com variations. ‘@free.kindle.com’ emails are free but can only be sent to your device when it is connected to wi-fi. ‘@kindle.com’ emails can be delivered even when you are not connected to wi-fi, but note that service fees apply.

Find out more about the Kindle Personal Document Service.

X-ray Microscopy of Polymeric Materials
Available formats
×

Send article to Dropbox

To send this article to your Dropbox account, please select one or more formats and confirm that you agree to abide by our usage policies. If this is the first time you use this feature, you will be asked to authorise Cambridge Core to connect with your <service> account. Find out more about sending content to Dropbox.

X-ray Microscopy of Polymeric Materials
Available formats
×

Send article to Google Drive

To send this article to your Google Drive account, please select one or more formats and confirm that you agree to abide by our usage policies. If this is the first time you use this feature, you will be asked to authorise Cambridge Core to connect with your <service> account. Find out more about sending content to Google Drive.

X-ray Microscopy of Polymeric Materials
Available formats
×
×

Reply to: Submit a response


Your details


Conflicting interests

Do you have any conflicting interests? *