Abstract
A 29Si and 27Al magic angle spinning nuclear magnetic resonance study is reported for differently synthesized mullites. The 29Si MAS NMR spectra of all samples are essentially identical. They consist of a main resonance at -86.8 ppm, a shoulder around -90 ppm and a second resonance at -94.2 ppm. The main resonance is interpreted as being due to a sillimanite-type geometry around Si and the second one is tentatively assigned to a Si environment typical for mullite. The 27Al MAS NMR spectra of sinter- and fused-mullite measured at different Larmor frequencies revealed clearly the presence of three distinct Al sites in mullite, i.e. of octahedral (M1), tetrahedral (M2) and distorted tetrahedral (Al*) sites.
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References
Alemany LB, Kirker GW (1986) First observation of 5-coordinate aluminum by MAS 27Al NMR in well-characterized solids. J Am Chem Soc 108:6158–6162
Angel RJ, Prewitt CT (1986) Crystal structure of mullite: A re-examination of the average structure. Am Mineral 71:1476–1482
Bertram UC, Heine V, Jones IL, Price GD (1990) Computer modeling of Al/Si ordering in sillimanite. Phys Chem Minerals 17:326–333
Blinc R (1981) Magnetic Resonance and Relaxation in Structural Incommensurate Systems. Phys Rep 79:331–398
Burnham CW (1963) Refinement of the crystal structure of sillimanite. Z Kristallogr 115:127–148
Burnham CW (1964) Crystal structure of mullite. Carnegie Inst. Wash. Year Book 63:223–227
Cameron WE (1977) Mullite: A substituted alumina. Am Mineral 62:747–755
Cruickshank MC, Dent Glasser LS, Barri SAI, Poplett IJF (1986) Penta-coordinated aluminum: a solid state 27Al NMR study. J Chem Soc D 23–24
Dec SF, Maciel GE (1990) High-speed MAS NMR of quadrupolar nuclides at high magnetic fields. J Magn Reson 87:153–159
Engelhardt G, Michel D (1987) High-resolution solid-state NMR of silicates and zeolites. Wiley, New York
Holm JL, Kleppa OJ (1966) The thermodynamic properties of the aluminium silicates. Am Mineral 51:1608–1622
Lippmaa E, Samoson A, Mägi M (1986) High-resolution 27Al NMR of Aluminosilicates. J Am Chem Soc 108:1730–1735
McConnell JDC, Heine V (1985) Incommensurate structure and stability of mullite. Phys Rev B 31:6140–6143
Merwin LH, Sebald A, Scifert F (1989) The Incommensurate-commensurate Phase Transition in Akermanite, Ca2MgSi2O7, Observed by in-situ 29Si MAS NMR spectroscopy. Phys Chem Minerals 16:752–756
Morimoto N (1990) Modulated structure and vacancy ordering in mullite. Ceram Trans 6:115–124
Rocha J, Klinowski J (1990) 29Si and 27Al Magic-Angle-Spinning NMR studies of the thermal transformation of kaolinite. Phys Chem Minerals 17:179–186
Saalfeld H (1979) The domain structure of 2∶1 mullite (2Al2O3 1SiO2). N Jb Mineralogie Abh 134:306–316
Saalfeld H, Guse W (1981) Structure refinement of 3∶2 mullite (3Al2O3 2SiO2). N Jb Mineralogie Mh 145–150
Sanz J, Madami A, Serratosa JM, Moya JS and Aza S (1988) Aluminum-27 and Silicon-29 Magic-Angle-Spinning Nuclear Magnetic Resonance Study of the Kaolinite-Mullite Transformation. J Am Ceramic Soc 10:C418–421
Schneider H (1986) Formation, properties, and high-temperature behavior of mullite. Habilitation Faculty of Chemistry, University of Münster 1–148
Schneider H (1990) Transition metal distribution in mullite. Adv Ceram Trans 6:135–158
Sheriff BL, Grundy HD (1988) Calculations of 29Si MAS NMR chemical shift from silicate mineral structure. Nature 332:819–820
Turner GL, Kirkpatrick RJ, Risbud SH, Oldfield E (1987) Multinuclear magic-angle sample spinning nuclear magnetic resonance spectroscopic studies of crystalline and amorphous ceramic materials. Am Ceram Soc Bull 66:656–663
Yasumori A, Iwasaki M, Kawazoe H, Yamane M, Nakamura Y (1990) Nuclear magnetic resonance study of the structure of aluminosilicate gel and glass. Phys Chem Glass 31:1–9
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Merwin, L.H., Sebald, A., Rager, H. et al. 29Si and 27Al MAS NMR spectroscopy of mullite. Phys Chem Minerals 18, 47–52 (1991). https://doi.org/10.1007/BF00199043
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DOI: https://doi.org/10.1007/BF00199043