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  • 1
    Electronic Resource
    Electronic Resource
    Oxford [u.a.] : International Union of Crystallography (IUCr)
    Acta crystallographica 51 (1995), S. 2694-2696 
    ISSN: 1600-5759
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1432-2021
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Notes: Abstract The 29-Si NMR spectra of natural and synthetic leucites (KAlSi2O6) are found to contain a number of resonances which are interpreted in terms of the known structure of low-temperature (tetragonal) leucite. Computer simulation of the spectra suggests that the most distorted tetrahedral lattice site T 1 contains a higher proportion of Al than the other two tetrahedral sites. The occurrence of some ordering of the tetrahedral Si and Al in leucite is confirmed by Mossbauer studies of synthetic iron-containing leucites, including the fully ferric end-member KFeSi2O6, in which the three tetrahedral sites can be distinguished. On replacement of about half this Fe by Al, the most distorted of these sites is lost from the spectrum, reflecting the preference of Al for this site. A linear relationship is found between the unit cell dimensions of all these leucites and their iron content.
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Journal of thermal analysis and calorimetry 38 (1992), S. 2053-2065 
    ISSN: 1572-8943
    Keywords: calcination ; high temperature reactions ; kaolinite ; kinetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Strukturelle Veränderungen bei der Dehydroxylierung von Kaolinit wurden durch die Anwendung einer Blitz-Kalzination untersucht, um kinetisch eingefrorene Kalzinationsprodukte zu erhalten. Der Prozentsatz der Dehydroxylierung wurde durch Veränderung der Verweilzeit im Ofen, durch Ofentemperatur und/oder Heizgeschwindigkeit modifiziert. Diese Kalzinationsbedingungen beeinflußten zwar die Reaktionskinetik, aber die Produkte hingen nur vom Ausmaß der Dehydroxylierung ab. Abweichungen bei Lage und Enthalpie der endothermen Umwandlung zu Metakaolinit und die exotherme Hochtemperaturreaktion von Metakaolinit wurden mittels DSC der Blitz-Kalzinationsprodukte verfolgt und in Beziehung zur Thermogravimetrie gebracht. 27Al Magic-Angle-Spinning NMR Spektren bei hohen magnetischen Feldstärken und Drehgeschwindigkeiten erlauben es, die Reaktion von Kaolinit zu verfolgen und liefern neue Informationen über die Natur der bei der Dehydroxylierung gebildeten Substanzen.
    Notes: Abstract The structural changes occurring during the dehydroxylation of kaolinite have been followed using flash calcination to produce kinetically frozen calcines. The percentage of dehydroxylation was varied by changing the furnace residence time or temperature and/or heating speed. These calcination conditions affected the reaction kinetics, but the products depended only on the extent of dehydroxylation. Changes in the position and enthalpy of the endothermic transformation to metakaolinite and the high temperature exothermic reaction of metakaolinite have been followed using Differential Scanning Calorimetry of the flash calcines and related to Thermogravimetry. 27Al magic-angle-spinning NMR spectra, at high magnetic fields and spin rates, enabled the reaction of kaolinite to be monitored and provides new information on the nature of the species formed in the course of dehydration.
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  • 4
    Electronic Resource
    Electronic Resource
    Springer
    Journal of materials science 4 (1985), S. 163-166 
    ISSN: 1573-4811
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
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  • 5
    Electronic Resource
    Electronic Resource
    Springer
    Journal of materials science 22 (1987), S. 3265-3275 
    ISSN: 1573-4803
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract Only very slight changes are observed in the29Si and27Al solid-sate magic-angle spinning NMR spectra of a montmorillonite containing almost equal numbers of octahedral aluminium and magnesium ions when its interlayer water is driven off by heating. The29Si NMR spectra are unaffected by dehydroxylation which begins at ∼ 450° C, but the27Al spectra show a decrease in total intensity, possibly due to the formation of 5-coordinated aluminium, with a slight increase in the intensity of the tetrahedral aluminium resonance. On the basis of these results, a structural model is proposed for the dehydroxylate phase and its formation mechanism is discussed. The destruction of the dehydroxylate X-ray pattern at ∼ 850° C and the subsequent recrystallization of the high-temperature products (β-quartz, enstatite and high-cordierite at ∼ 1100° C;β-cristobalite, enstatite and sapphirine at ∼ 1200° C) is accompanied by changes in the silicon and aluminium NMR spectra and in the57Fe Mbssbauer spectra which are fully consistent with the known structural features of these phases.
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  • 6
    ISSN: 1573-4803
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract Studies of two muscovites of different iron contents, using solid-state NMR with magic-angle-spinning (MAS) combined with X-ray powder diffraction, thermal analysis and57Fe Mössbauer spectroscopy, suggest that dehydroxylation occurs by a homogeneous rather than an inhomogeneous mechanism, forming a dehydroxylate in which the aluminium is predominantly 5-coordinate. On further decomposition at about 1100° C, the tetrahedral layer and interlayer K+ form a feldspar-like phase similar to leucite (KAISi2O6), the remainder forming a spinel, which, contrary to previous suggestions, appears to contain little silicon. Further heating induces the formation of mullite (AI6Si2OP13), and, in the higher-iron sample, corundum (α-Al2O3), in addition to the feldspar-like phase. The presence of the iron impurity enhances the recrystallization reactions and promotes the conversion of mullite to corundum, which eventually becomes the sole aluminous product in the high-iron sample. In samples fired to higher temperatures, only the tetrahedral aluminium resonance is detectable by27AI NMR, probably because most of the iron is located in either the mullite or corundum phases, in which it broadens the octahedral aluminium resonance beyond detection.
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  • 7
    Electronic Resource
    Electronic Resource
    Springer
    Journal of materials science 12 (1993), S. 1696-1698 
    ISSN: 1573-4811
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Type of Medium: Electronic Resource
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  • 8
    ISSN: 1573-4803
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract Phase formation in kaolinite heated at 1200°C in eight different reaction atmospheres in the presence and absence of carbon has been studied by solid-state magic angle spinning nuclear magnetic resonance (MAS NMR) and X-ray powder diffraction. Mullite (3Al2O3-2SiO2) and amorphous SiO2 are the principal products in all atmospheres. The amount of mullite formed is generally greater under vacuum and in reducing atmospheres, but the precise effect of the atmosphere is also modified by the presence of carbon. Vacuum and reducing atmospheres generally produce mullites of alumina: silica composition nearer 3∶2 than 2∶1 (estimated from unit cell measurements) and containing a higher proportion of Al*, i.e. tetrahedral aluminium associated with an oxygen defect (estimated by 27AlNMR measurements). The result of most significance to sialon formation is the detection by 29Si NMR of silicon oxynitride formation at 1200°C in systems containing either nitrogen or ammonia, in the presence of carbon. The preferential formation of Si-O-N bonds at such an early stage of the reaction under carbothermal conditions was confirmed by thermodynamic calculations, which also clarify other details of the complex interactions between the aluminosilicate, carbon, and the various gas atmospheres.
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  • 9
    Electronic Resource
    Electronic Resource
    Springer
    Journal of materials science 29 (1994), S. 2775-2783 
    ISSN: 1573-4803
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract A process has been developed for bonding chrysotile asbestos into a robust, dimensionally-stable lightweight ceramic material by fusing it with sodium silicate and/or ground waste glass. The chrysotile can retain its desirable properties of fibrous morphology and porosity, but the fibre bundles are stabilized by fusion into a glassy matrix, reducing the respirable fibre concentration. The glass-bonded materials have good resistance to mechanical abrasion, and any resulting dust is found by SEM to be particularly free of fibres. The thermal treatment also converts the chrysotile into crystalline forsterite, which should destroy its cell toxicity. Other methods of glass-bonding chrysotile compacts (hot pressing and impregnating with glaze) were also investigated, and the properties of the resulting materials are reported.
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  • 10
    ISSN: 1573-4803
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract 27Al and 29Si magic-angle spinning(MAS) nuclear magnetic resonance(NMR)and complementary X-ray diffraction (XRD) studies of carbothermal formation of sialons from kaolinite and halloysite confirm that the reaction involves the initial formation of mullite (3Al2O3·2SiO2) and amorphous silica. In the presence of carbon, Si-N bonds are formed at ≈1200 °C, giving a continuum of silicon oxynitride compositions which become progressively more N-rich. These do not become sufficiently ordered to be detected by XRD until later in the reaction, when crystalline silicon oxynitride, possibly containing a little Al (O′-sialon) and x-phase sialon are formed, followed by β′-sialon. The O′- and x-phase sialons are transitory, but the β′-sialon persists throughout the reaction. Si-O bonds survive the destruction of the mullite and persist throughout the reaction, especially with kaolinite starting material. The 29Si MAS NMR results indicate that Si-C bonds are formed later in the reaction than previously suggested, the SiC phase behaving more like a secondary product than a transitory intermediate. Al-N bonds are not detectable by 27Al MAS NMR until very late in the reaction (after 8 h firing at 1400 °C), and coincide with the appearance of the secondary product AlN. The implications for the carbothermal reaction sequence in kaolinite and halloysite are discussed.
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