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Small Angle X-Ray Scattering on Poly(Ethylene-Methacrylic Acid) Lead and Lead Sulfide Ionomers

Published online by Cambridge University Press:  21 February 2011

Benjami Chu ,
Dan O. Wu  and
Walter Mahler
Benjami Chu*
Affiliation:
Department of Chemistry, State University of New York at Stony Brook, Long Island, NV1Y1 794–3400
Dan O. Wu
Affiliation:
Department of Chemistry, State University of New York at Stony Brook, Long Island, NV1Y1 794–3400
Walter Mahler
Affiliation:
Central Research & Development Department, Experimental Station, E.l. du Pont de Nemours & Co., Inc., Wilmington, DE 19880-0328
*
author to whom all correspondence should be addressed
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Abstract

The morphology of ionomers, e.g., poly(ethylene-methacrylic acid) (EMA) lead salts (EMA/Pb) and lead sulfide compounds (EMA/PbS), has been studied by using the techniques of small angle x-ray scattering (SAXS), anomalous SAXS (ASAXS), wide angle x-ray scattering (WAXS), and differential scanning calorimetry (DSC). EMA/Pb containing less than 5 wt% of lead exhibited two characteristic SAXS peaks which corresponded to the lamellar structure of the partially crystalline polymer matrix and the ionic structure of the lead aggregates that were present in the amorphous regions. The lead aggregates were not distributed uniformly and increased in packing density with increasing lead content. Both DSC and WAXS showed that the crystalline phase was present for all EMA/Pb samples and that the crystallinity decreased slightly with increasing lead content. ASAXS near the L3 absorption edge of lead permitted the extraction of the scattered intensity of lead ions from the SAXS patterns of the superimposed crystalline and ionic structures. Correlation function analysis revealed that the ionic aggregates of the EMA/Pb containing 5 wt% of lead could be described by a liquid-like model with a short range order of 2-4 nm. EMA/PbS samples were made by a reaction of EMA/Pb ionomers with hydrogen sulfide. Instead of an ionic peak as shown by EMA/Pb samples, the SAXS patterns of EMA/PbS showed a broad diffraction peak located at the same q value as the lamellar peak of the EMA in acid form. The (lamellar) peak could be attributed to the interference between the PbS crystallites in the neighboring lamellae.

Type
Research Article
Information
MRS Online Proceedings Library (OPL) , Volume 171: Symposium O – Polymer Based Molecular Composites , 1989 , 237
Copyright
Copyright © Materials Research Society 1990

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References

REFERENCES

[1] Rees, R.W. and Vaughan, D.J., Polym. Prepr.Am. Chem. Soc. Div. Polym. Chem., 6, 287 (1965).Google Scholar
[2] Wilson, F.C., Longworth, R. and Vaughan, D.J., Polym. Prepr., Amer. Chem. Soc. Div. Polym. Chem., 9, 505 (1968).Google Scholar
[3] Longworth, R. and Vaughan, D.J., Nature (London), 218, 85 (1968); and Polym. Prepr., Amer. Chem. Soc. Div. Polym. Chem., 9, 525 (1968).Google Scholar
[4] Longworth, R., in Ionic Polymer, edited by Holliday, L. (Halsted-Wiley, New York, 1975).Google Scholar
[5] Max, C.L., Caulfield, D.F., and Cooper, S.L., Macromolecules, 6, 344 (1973).Google Scholar
[6] Earnest, T.R. Jr., and MacKnight, W.J., Macomolecules, 10, 206 (1977) and J. Polym. Sci., Polym. Phys. Ed., 16, 143 (1978)Google Scholar
[7] MacKnight, W. J., Taggart, W.P., and Stein, R.S., J. Polym. Sci., Polym. Symp., 45, 113 (1974).Google Scholar
[8] Kao, J., Stein, R.S., MacKnight, W.J., Taggart, W.P., and Cargill, G.S., Macromolecules, 7, 95 (1974).Google Scholar
[9] Earnest, T.R. Jr., Ph.D Thesis, University of Massachusetts, (1978)Google Scholar
[10] MacKnight, W.J. and Earnest, T.R., J. Polym. Sc: Macrom. Rev., 16, 41 (1981).Google Scholar
[11] Yarusso, D.J., Cooper, S.L., Polymer, 26, 371 (1985) and Macromolecules, 16, 1871 (1983).Google Scholar
[12] Tadano, K., Hirasawa, E., Yamamoto, H., and Yano, S., Macomolecules, 22, 226 (1989).Google Scholar
[13] Mahler, W., J. Inorg. Chem., 27, 436 (1988).Google Scholar
[14] Stuhrmann, H. B., Adv. Polym. Sci., 67, 123 (1985).Google Scholar
[15] Phillips, J.C. and Hodgson, K.O., in Synchrotron Radiation Research, edited by Winick, H. and Doniach, S., (Plenum, New York, 1980) and Acta Cryst., A36, 856 (1980).Google Scholar
[16] Miake-Lye, R.C., Doniach, S., and Hodgson, K.O., Biophys. J., 41, 287 (1983).Google Scholar
[17] Goudeau, P., Fontaine, A., Naudon, A., and Williams, C.E., J. Appl. Cryst., 12, 19 (1986).Google Scholar
[18] Simon, J.P., Lyon, O., and Fontaine, D. de, J. Appl. Cryst., 18, 230 (1985).Google Scholar
[19] Ding, Y.S., Hubbard, S.R., Hodgson, K.O., Register, R.A., and Cooper, S.L., Macromolecules, 21, 1698 (1988).Google Scholar
[20] Register, R.A. and Cooper, S.L., to be published in Macromolecules.Google Scholar
[21] Chu, B., Phillips, J.C., Wu, D.Q., in Polymer Research at Synchrotron Radiation Sources, edited by Russel, T.P. and Goland, A.N., report no. BNL51847, Brookhaven National Laboratory, Upton, NY (1986) p.126 and J.C. Phillips, K.J. Baldwin, W.F. Lehnert, A.D. LeGrand, C.T. Prewitt, Nucl. Instrum. and Methods in Phys. Res., A246, 182 (1986).Google Scholar
[22] Chu, B., Wu, D.O., and Wu, C., Rev. Sci. Instrum., 581(7), 1158 (1987).Google Scholar
[23] Chu, B., Wu, D.Q., and Howard, R., Rev. Sci. instrum., 60(10), 3224 (1989).Google Scholar
[24] Fujimura, M., Hashimoto, T., and Kawai, H., Macromolecules, 14, 1309 (1981) and 15, 136 (1982).Google Scholar
[25] Chu, B., Wu, D.O., MacKnight, W.J., Wu, C., Phillips, J.C., LeGrand, A., Lantman, C.W., and Lundberg, R.D., Macromolecules, 21, 523 (1988).Google Scholar
[26] Wu, D.O., Phillips, J.C., Lundberg, R.D., MacKnight, W.J., and Chu, B., Macromolecules, 22, 992 (1989).Google Scholar
[27] Song, H., Stein, R.S., Wu, D.O., Ree, M., Phillips, J.C., LeGrand, A., Chu, B., Macromolecules, 21, 1180 (1988) and H. Song, D.Q. Wu, M. Satkowski, R.S. Stein, and B. Chu, Macromolecule, in press.Google Scholar
[28] Wu, D.O., Chu, B., and Mahler, W., to be submitted to Macromolecules.Google Scholar
[29] Debye, P. and Bueche, A.M., J. Appl. Phys., 20, 299 (1949) and H. Brumberger and P. Debye, J. Phys. Chem., 61, 1623 (1957).Google Scholar
[30] Porod, G., in Small Angle X-ray Scattering, edited by Glatter, O., Kratky, O., (Academic Press, London 1982)Google Scholar
[31] Williams, C.E., in Structure and Properties of lonomers, edited by Pineri, M. and Eisenberg, A., (D. Reidel Publishing Co., Dordrecht 1987).Google Scholar
[32] Wu, D.O., Chu, B., Lundberg, R.D., and MacKnight, W.J., manuscript in preparation.Google Scholar