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  • 1
    Electronic Resource
    Electronic Resource
    s.l. : American Chemical Society
    Journal of the American Chemical Society 108 (1986), S. 30-33 
    ISSN: 1520-5126
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Oxford, UK : Blackwell Science Inc
    Journal of the American Ceramic Society 88 (2005), S. 0 
    ISSN: 1551-2916
    Source: Blackwell Publishing Journal Backfiles 1879-2005
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Investigation of a series of synthetic alkali silicate gels and gels produced by the alkali silica reaction (ASR) in field concrete using 29Si NMR spectroscopy, X-ray diffraction, and bulk chemical analysis shows that local structures of the synthetic and field gels are quite similar. The most abundant Si sites for the field and synthetic gels with similar compositions have Q3 polymerization, and the number of non-bridging oxygens per Si is similar for these samples. These samples also yield a basal X-ray diffraction peak near 8–12 Å, suggesting that the structure is dominated by sheet-like units, consistent with the dominant Q3 polymerization. Calculations based on the relative site abundances of the sites observed by 29Si NMR and the bulk chemical compositions indicate that there is insufficient alkali to charge-balance all the non-bridging oxygens and that there is a significant concentration of Si–OH linkages. The results provide strong support for the basic structural concepts of the so-called kanemite model for ASR gel proposed by Wieker and coworkers, although the overall gel structure is likely to be more complex.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Westerville, Ohio : American Ceramics Society
    Journal of the American Ceramic Society 82 (1999), S. 0 
    ISSN: 1551-2916
    Source: Blackwell Publishing Journal Backfiles 1879-2005
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: The mid-, near-, and far-infrared (IR) spectra of synthetic, single-phase calcium silicate hydrates (C-S-H) with Ca/Si ratios (C/S) of 0.41–1.85, 1.4 nm tobermorite, 1.1 nm tobermorite, and jennite confirm the similarity of the structure of these phases and provide important new insight into their H2O and OH environments. The main mid-IR bands occur at 950–1100, 810–830, 660–670, and 440–450 cm−1, consistent with single silicate chain structures. For the C-S-H samples, the mid-IR bands change systematically with increasing C/S ratio, consistent with decreasing silicate polymerization and with an increasing content of jennite-like structural environments of C/S ratios 〉1.2. The 950–1100 cm−1 group of bands due to Si-O stretching shifts first to lower wave number due to decreasing polymerization and then to higher wave numbers, possibly reflecting an increase in jennite-like structural environments. Because IR spectroscopy is a local structural probe, the spatial distribution of the jennite-like domains cannot be determined from these data. A shoulder at ∼1200 cm−1 due to Si-O stretching vibrations in Q3 sites occurs only at C/S lessthan equal to 0.7. The 660–670 cm−1 band due to Si-O-Si bending broadens and decreases in intensity for samples with C/S 〉 0.88, consistent with depolymerization and decreased structural order. In the near-IR region, the combination band at 4567 cm−1 due to Si-OH stretching plus O-H stretching decreases in intensity and is absent at C/S greater than ∼1.2, indicating the absence of Si-OH linkages at C/S ratios greater than this. The primary Si-OH band at 3740 cm-1 decreases in a similar way. In the far-IR region, C-S-H samples with C/S ratio greater than ∼1.3 have increased absorption intensity at ∼300 cm−1, indicating the presence of CaOH environments, even though portlandite cannot be detected by X-ray diffraction for C/S ratios 〈1.5. These results, in combination with our previous NMR and Raman spectroscopic studies of the same samples, provide the basis for a more complete structural model for this type of C-S-H, which is described.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Westerville, Ohio : American Ceramics Society
    Journal of the American Ceramic Society 80 (1997), S. 0 
    ISSN: 1551-2916
    Source: Blackwell Publishing Journal Backfiles 1879-2005
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Transmission electron microscopy of synthetic jennite reveals strong streaking in the electron diffraction patterns along the [100], along which dark-field imaging and lattice fringing confirm the presence of a layering with a striation-like morphology. The average periodicity between the layers is ∼35 Å; however, there is significant variation around this value in the range of 20-40 Å, which is in agreement with the range of periodicities that are associated with the streaking in the diffraction patterns. These results clearly demonstrate the presence of a layering along the [100] with a periodicity that varies spatially throughout the specimen, which results in the presence of a disordered modulated structure. We believe that the disorder is induced by frozen-in fluctuations in the local calcium:silicon ratio, which correspondingly results in fluctuations in the local structural order and periodicity of the modulated structure. Similar studies of 1.4-nm tobermorite have revealed streaking along the [100]; however, it was weak and diffuse.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    s.l. : American Chemical Society
    The @journal of physical chemistry 〈Washington, DC〉 91 (1987), S. 1054-1058 
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology , Physics
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    s.l. : American Chemical Society
    Journal of the American Chemical Society 109 (1987), S. 1632-1635 
    ISSN: 1520-5126
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 7
    Electronic Resource
    Electronic Resource
    s.l. : American Chemical Society
    Journal of the American Chemical Society 105 (1983), S. 2483-2485 
    ISSN: 1520-5126
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 8
    Electronic Resource
    Electronic Resource
    [s.l.] : Nature Publishing Group
    Nature 325 (1987), S. 236-238 
    ISSN: 1476-4687
    Source: Nature Archives 1869 - 2009
    Topics: Biology , Chemistry and Pharmacology , Medicine , Natural Sciences in General , Physics
    Notes: [Auszug] The spectra were obtained for homogeneous, ordered plagioclases which had been purified from natural metamorphic and slowly cooled igneous rocks and had almost all been characterized by transmission electron microscopy, electron microprobe analysis, X-ray powder diffraction and high-temperature ...
    Type of Medium: Electronic Resource
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  • 9
    ISSN: 1432-2021
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Notes: Abstract Nuclear magnetic resonance spectroscopic data are presented for the cristobalite polymorphs of AlPO4 and SiO2 from RT to 770 K, through their respective α-β transitions. The nuclear magnetic resonance (NMR) data include chemical shifts for 31P, 27Al, and 29Si, 27Al quadrupole coupling parameters, and 31P and 27Al spin-lattice relaxation rates. Also presented are electron diffraction patterns of β-cristobalite AlPO4 that show diffuse scattering similar to that reported previously for SiO2. For the α-phases of both AlPO4 and SiO2, the chemical shifts decrease approximately linearly with increasing temperature from RT to Tc and discontinuously by -2 to -3 ppm from α to β. This result is consistent with a small, continuous increase in the mean T-O-T angle (〈θ〉) of the α-phases with increasing T and an increase of 〈θ〉 by about 4° across the α-β transition for both cristobalite and its AlPO4 analogue. Based on the 29Si chemical shifts, the mean Si-O-Si angle for β-cristobalite is 152.7±1° near Tc. For AlPO4-cristobalite, the 27Al nuclear quadrupole coupling constant (CQ) decreases approximately linearly from 1.2 MHz at RT to 0.94 MHz near Tc (493±10 K). At the α-β transition the 27Al CQ approaches zero, in agreement with the cubic average structure observed by diffraction. The satellite transitions retain a small frequency distribution above the α-β transition from electric field gradients attributed to defects. The short-range cubic symmetry of the Al-site and non-linear Al-O-P angle support a dynamically disordered model of the β-cristobalite structure. Complete averaging of the 27Al quadrupole coupling in the β-phase indicates that the lifetime of any short-range ordered domains must be shorter than about 1 μs.
    Type of Medium: Electronic Resource
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  • 10
    ISSN: 1432-2021
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Notes: Abstract We present 29Si MAS NMR data for a well-ordered natural anorthite, obtained in situ at temperatures of from 25 to 500° C, which follow the changes in the aluminosilicate framework through the P $$\bar 1$$ -I $$\bar 1$$ structural phase transition. Pairs of peaks due to sites offset by approximately 1/2 [111] converge through the P $$\bar 1$$ phase and only four peaks are present above about 241° C. The variation of the peak positions with temperature and correlations based on structural data for the P $$\bar 1$$ and I $$\bar 1$$ phases allow assignment of all the MAS-NMR peaks to crystallographic sites. A Landau-type analysis gives an expression that relates the separation of pairs of con verging peaks to the local order parameter for the P $$\bar 1$$ -I $$\bar 1$$ transition, from which we determine its temperature dependence. Data for the best-constrained set of peak positions give for the order parameter critical exponent β = 0.27±0.04, consistent with previous results indicating that the P $$\bar 1$$ -I $$\bar 1$$ transition in pure anorthite is tricritical. No significant change in the 29Si spin-lattice relaxation rate occurs across the P $$\bar 1$$ -I $$\bar 1$$ transition.
    Type of Medium: Electronic Resource
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