Small-Angle Neutron Scattering and 27Al Nmr Studies on the Microstructure and Composition of Alumina Sol-Gels

1990 ◽  
Vol 180 ◽  
Author(s):  
L. F. Nazar ◽  
D. G. Napier ◽  
D. Lapham ◽  
E. Epperson

ABSTRACTWe have used small angle neutron scattering, static light scattering and 27Al NMR to examine the structure and composition of alumina sol-gels formed by the hydrolysis of aluminum alkoxides. For LT sols at low acid concentrations, and HT gels over a wide range of acid concentration, 27Al solution NMR suggests, by the dearth of spectral resonances, that high molecular weight species are being formed. Analysis of the small angle neutron scattering data in the Porod regime indicates these sol-gels exhibit a power-law dependence consistent with mass fractal dimensions ranging from 1.45 to 1.8. These fractal dimensions are consistent with models based on diffusion limited cluster aggregation. The fractal dimensions do not differ significantly between LT and HT sols at the same acid concentration. However, for both temperature regimes, the fractal dimension increases with increasing acid concentration, suggesting a progression to a more compact network. Static light scattering measurements indicate the Guiner radii of the cluster aggregates vary from 600 to 2000Å.

2006 ◽  
Vol 39 (2) ◽  
pp. 202-208 ◽  
Author(s):  
Josef Innerlohinger ◽  
Mario Villa ◽  
Matthias Baron ◽  
Otto Glatter

Ultra-small-angle neutron scattering (USANS) probes the sameqregime as static light scattering (LS), making USANS an additional tool for the study of structures between 100 nm and 10 µm. Dense oil-in-water emulsions, which have already been characterized intensively by light scattering, are investigated in this study as a model system using USANS. The two basic problems of such scattering studies are the following: on the one hand, one has to use different scattering theories for USANS and LS, and on the other hand, in both cases one has to deal not only with particle interactions but also with multiple-scattering effects. For neutron scattering it is always possible to use the simpler Rayleigh–Debye–Gans (RDG) theory instead of the Lorenz–Mie theory, which generally describes light scattering from micrometre-sized globular objects. The samples have different contrasts in neutron and light scattering, such that only low-contrast (close to index match) LS data can be interpreted by the RDG theory. The data evaluation is performed by means of the generalized indirect Fourier transformation (GIFT) method, which enables the simultaneous calculation of the form and structure factors. The results are discussed and compared with those from light scattering experiments, taking into account the advantages of both methods. The effect of multiple scattering and its influence on data evaluation is also examined. Data evaluation by applying the GIFT method works well for both neutron and light scattering data, with results of comparable quality. The advantages of light scattering are the fast data acquisition and the large number of data points. USANS, on the other hand, covers a widerqrange and the problem of multiple scattering is not as severe as for light scattering, but still must not be neglected.


1996 ◽  
Vol 457 ◽  
Author(s):  
J. Weissmüller ◽  
R. D. McMichael ◽  
J. Barker ◽  
H. J. Brown ◽  
U. Erb ◽  
...  

ABSTRACTWe report on a combined theoretical and experimental study of the magnetic microstructure of a single component, single phase, Pore-free nanocrystalline ferromagnetic material. From the equations of micro-magnetics we conclude that the magnetic microstructure is the convolution product of an anisotropy field microstructure and of a response function with a correlation length lH that depends on the applied field Ha. We derive equations for small angle neutron scattering by such structures, and present experimental scattering data for electrodeposited nanocrystalline Ni, the first where for a wide range of Ha the dominant scattering contribution is from the purely magnetic microstructure, not from nuclear or magnetic contrast at pores or second phases. The variation of the scattering cross section with Ha is in excellent agreement with the theory, indicating that the underlying changes in the magnetic microstructure with Ha are not displacements of domain walls, but changes in lH and hence in the magnetic response to an entirely stationary anisotropy field microstructure. At 20K the anisotropy fields are dominated by magnetocrystalline anisotropy, but at 300K the perturbation is from a much stronger interaction which maintains some moments aligned antiparallel to the field direction at Ha as high as 1.4MA/m (18kOe).


2013 ◽  
Vol 46 (3) ◽  
pp. 788-790 ◽  
Author(s):  
Andreas Michels ◽  
Jens-Peter Bick

Real-space magnetic small-angle neutron scattering data from nanocrystalline cobalt and nickel have been analysed in terms of a recently developed micromagnetic theory for the autocorrelation function of the spin misalignment [Michels (2010).Phys. Rev. B,82, 024433]. The approach provides information on the exchange-stiffness constant and on the mean magnetic `anisotropy-field' radius.


1985 ◽  
Vol 18 (6) ◽  
pp. 467-472 ◽  
Author(s):  
N. F. Berk ◽  
K. A. Hardman-Rhyne

Microstructural parameters of high-purity alumina powder are determined quantitatively throughout the bulk of the material using small-angle neutron scattering techniques. A unified theoretical and experimental approach for analyzing multiple scattering data is developed to obtain values for particle size, volume fraction and surface area. It is shown how particle size and volume fraction can be measured in a practical way from SANS data totally dominated by incoherent multiple scattering (`beam broadening'). The general phase-shift dependence of single-particle scattering is incorporated into the multiple scattering formalism, and it is also shown that the diffractive limit (small phase shift) applies even for phase shifts as large as unity (particle radii of order 1 μm). The stability of the Porod law against multiple scattering and the phase-shift scale are described, a useful empirical formula for analysis of beam broadening data is exhibited, and the applicability of the formulations to polydispersed systems is discussed.


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