Abstract
Nuclear magnetic resonance (NMR) today probably is the most valuable tool for elucidation of molecular structure, order, and dynamics. For the characterization of macromolecules [1,2], NMR can be divided into two major areas. High-resolution NMR provides detailed information about the chain microstructure in solution. Solid-state NMR allows to characterize the molecular structure and the organization of the macromolecules in the bulk. Special techniques offer to study dynamic aspects over a large range of characteristic rates. Solid-state NMR allows to characterize morphology properties, e.g. chain alignment in oriented polymers [3]. Multidimensional techniques offer fundamental advantages [4] by introducing an additional frequency dimension to increase the spectral resolution and by providing routes to new information, unavailable from 1D spectra even in the limit of high resolution [5]. One aspect to establish structure-property relationships for polymer materials is the characterization of domain sizes in heterogeneous materials. Advanced polymer materials with more than one component are phase separated in most cases. Small domains of only a few nanometers, as well as interfaces between the different phases, are particular difficult to characterize. Here, new solid-state NMR techniques nicely supplement well-established scattering and microscopic methods.
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References
Flory, P.J. (1953) Principles ofPolymer Chemistry, Cornell University Press, Ithaca, NY.
Kroschwith, J.I. (ed.) (1990) Concise Encyclopedia ofPolymer Science and Technology, Wiley, New York.
McBrierty, V.J. and Packer, K.J. (1993) Nuclear Magnetic Resonance of Solid Polymers, Cambridge University Press, Cambridge.
Ernst, E.E., Bodenhausen, G. and Wokaun, A. (1987) Principles of Nuclear Magnetic Resonance in One and Two Dimensions, Oxford University Press, Oxford.
Schmidt-Rohr, K. and Spiess, H.W. (1994) Multidimensional Solid-Stare NMR and Polymers, Academic Press, London.
Komoroski, R.A (ed.) (1986) High Resolution NMR ofSynthetic Polymers in Bulk, VCH, Deerfield Beach, FL.
Bovey, F.A. (1982) Chain Structure and Conformation ofMacromolecules, Academic Press, New York.
Mehring, M. (1983) High Resolution NMR in Solids, Springer Verlag Berlin, Berlin.
Abragam, A (1961) The Principles of Nuclear Magnetism, Oxford University Press, London.
Voelkel, R. (1988) High-Resolution Solid-State 33C-NMRSpectroscopy of Polymers, Angew. Chem. Int. Ed. Engl. 27, 1468–1483.
Aulja, RS., Harris, R.K., Packer, K.J., Prarmeswaran, M., Say, B.J., Bunn, A., and Cudby, M.E.A (1982) Discriminatory Experiments in High-Resolution 13C NMR of Solid Polymers, Polymer Bulletin, 8 253–259.
VanderHart, D.L. (1990) Proton Spin Diffusion as a Tool for Characterizing Polymer Blends, Makromol. Chem., MacromoL Symp. 34, 124–159.
Schmidt-Rohr, K., Clause, J., Bhimich, B., and Spiess, H.W. (1990) Miscibility of Polymer Blends Investigated by ‘H Spin Diffusion and t3C NMR Detection, Magn. Reson. Chem. 28 3–9.
Clauss, J., Schmidt-Rohr, K., and Spiess, H.W. (1993) Determination of domain sizes in heterogeneous polymers by solid state NMR, Acta Polym. 44 1–17.
Spiegel, S., Schmidt-Rohr, K., and Spiess, H.W. (1993) ‘H spin diffusion coefficients of highly mobile polymers, Polymer 34 4566–4569.
Schmidt-Rohr, K., Clauss, J., and Spiess, H.W. (1992) Correlation of Structure, Mobility, and Morphological Information in Heterogeneous Polymer Materials by Two-Dimensional WidelineSeparation NMR Spectrsocopy, Macromolecules 25 3273–3277.
Daniel, J.C. (1985) Latex de particules structurées, Macromol. Chem., Suppl.. 10/11 359–390.
Okubo, M., Katsuta, Y., and Matsumoto, T.J. (1980) Rupture of anomalous composite particles prepared by seeded emulsion polymerization in aging periodPolym. Sci., Polym. Lett. Ed. 18 481–4486.
Okubo, M. (1990) Control of Particle Morphology in Emulsion Polymerization Makromol. Chem., Macromol. Symp. 35/36 307–325.
Okubo, M., Kanaida, K., and Matsumoto, T. (1987) Production of anomalously shaped carboxylated polymer particles by seeded emulsion polymerization, Colloid Polym. Sci. 265 876–881.
Shen, S., El-Aasser, M.S., Dimonie, V.L., Vanderhoff, J.W., and Sudol, E.D. (1991) Preparation and Morphological Characterization of Microscopic Composite Particles, J. Polym. Sci., Polym. Chem. Ed. 29 857–867.
Tembou Nzudie, D., Delmotte, L, and Riess, G. (1991) Magic-angle carbon-13 nuclear magnetic resonance analysis of polybutadiene-poly(methyl methacrylate) core shell latexMakromol. Chem., Rapid Commun. 12 254–458.
Tembou Nzudie, D., Delmotte, L., and Riess, G. (1994) Polybutadiene-poly(methyl methacrylate) core-shell latexes studied by high-resolution solid-state 13C NMR and DSC: Influence of the surface coverage of the polybutadien seed latex and the latex composition on on the interphase formation, Macromol. Chem. Phys. 195 2723–2737.
Nelliappan, V., El-Aasser, M.S., Klein, A., Daniels, E.S., and Roberts, J.E. (1995) Characterization of the Interphase in Poly(divinylbenzene)/Poly(n-butyl acrylate) Core/Shell Latexes by High-Resolution Solid-State NMR Relaxation Studies, J. Appl. Polym. Sci. 58 323–330.
McBrierty, V.J. and Douglass, D.C. (1981), J. Polym. Sci., Macromol. Rev. 16 295–366.
Schmidt-Rohr, K., Clauss, J., and Spiess, H.W. (1992) Correlation of Structure, Mobility, and Morphological Information in Heterogeneous Polymer Materials by 2D Wideline-Separation NMR Spectroscopy, Macromolecules, 25 3273–3277.
Cai, W.Z., Schmidt-Rohr, K., Egger, N., Gerharz, B., and Spiess, H.W. (1993) A solid-state NMR study of microphase structure and segmental dynamics of poly(styrene-b-methylphenylsiloxane) diblock copolymers, Polymer, 34 267–276.
Landfester, K., Boeffel, C., Lambla, M., and Spiess, H.W. (1995) Synthesis and characterization of core-shell latexes with microscopic and solid-state NMR methods, Macromol. Symp. 92 109–116.
Spiegel, S., Landfester, K, Lieser, G., Boeffel, C., Spiess, H.W., and Eidam, N. (1995) Microheterogeneities of core-shell latexes probed by ‘H spin diffusion and transmission electron microscopy, Macromol. Chem. Phys. 196 985–993.
Landfester, K., Boeffel, C., Lambla, M., and Spiess, H.W. (1996) Characterization of interfaces in core-shell polymers by advanced solid-state NMR methods Macromolecules, in press.
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Landfester, K., Spiess, H.W. (1997). Characterization of Particle Morphology by Solid-State NMR. In: Asua, J.M. (eds) Polymeric Dispersions: Principles and Applications. NATO ASI Series, vol 335. Springer, Dordrecht. https://doi.org/10.1007/978-94-011-5512-0_14
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DOI: https://doi.org/10.1007/978-94-011-5512-0_14
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