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G. Mountjoy M.A. Holland P. Gunawidjaja G.W. Wallidge D.M. Pickup R.J. Newport M.E. Smith 《Journal of Sol-Gel Science and Technology》2003,26(1-3):161-164
The incorporation of transition-metal oxides into silica can give materials with useful optical, electronic or catalytic properties. For example, ZrO2-SiO2 and HfO2-SiO2 materials are of interest due to their high dielectric constants. Here we present a comparison of extended X-ray absorption fine structure and small-angle X-ray scattering results for acid-catalysed binary (MO2)
x
(SiO2)1 – x
(M = Ti, Zr or Hf) xerogels, with x up to 0.4 and heat treatments up to 750°C. Detailed observations for TiO2-SiO2 and ZrO2-SiO2 xerogels provide a basis for interpretation of new results for HfO2-SiO2 xerogels. At low concentrations metal atoms are homogeneously incorporated into the silica network. Ti adopts coordinations of 4 or 6, and Zr and Hf both adopt higher coordination of 6 or 7 (the larger coordinations being due to ambient moisture). At higher concentrations, phase separation of metal oxide occurs. Such regions become clearly separated from the silica network for TiO2, but remain very finely mixed with silica network for ZrO2 and HfO2. 相似文献
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Carmalt CJ Newport AC O'Neill SA Parkin IP White AJ Williams DJ 《Inorganic chemistry》2005,44(3):615-619
The mono(guanidinato) complex [Ti(NMe2)2Cl{i-PrNC[N(SiMe3)2]N-i-Pr}] (1) was prepared by reaction of [Ti(NMe2)2Cl2] with 1 or 2 equiv of the lithium guanidinate salt [Li{i-PrNC[N(SiMe3)2]N-i-Pr}]. Compound 1 has been characterized by X-ray crystallography. Treatment of TiCl4 with 2 equiv of [Li{i-PrNC[N(SiMe3)2]N-i-Pr}] resulted in the formation of dark red crystals. X-ray crystallography showed that these crystals consist of a 70:30 mixture of two bis(guanidinato) complexes, namely, [TiCl2{i-PrNC[N(SiMe3)2]N-i-Pr}{i-PrNC(N=CMe2)N-i-Pr}] (2) and [TiCl2{i-PrNC[N(SiMe3)2]N-i-Pr}{i-PrNC[N(H)-i-Pr]N-i-Pr}] (3). Both compounds 2 and 3 possess a transformed guanidinate ligand. Low-pressure chemical vapor deposition of either compound 1 or [TiCl2{i-PrNC(NMe2)N-i-Pr}] (4) at 600 degrees C results in thin films of titanium carbonitride. 相似文献
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G. Mountjoy M.A. Holland P. Gunawidjaja D.M. Pickup G.W. Wallidge M.E. Smith R.J. Newport 《Journal of Sol-Gel Science and Technology》2003,26(1-3):137-141
There has been much work on the binary TiO2-SiO2 and ZrO2-SiO2 materials prepared by sol-gel because of the beneficial properties resulting from incorporation of Ti and Zr. In contrast the ternary TiO2-ZrO2-SiO2 xerogels have been relatively little studied. We report the results of a study of those xerogels having Zr:Ti:Si ratios of 5:15:80, 10:10:80 and 15:5:80 heated to 750°C and to 1000°C. The study includes X-ray diffraction, small angle X-ray scattering, X-ray absorption spectroscopy at Ti and Zr K-edges, and 17O MAS-NMR. The study has benefited from close comparison with similar previous studies of the binary systems. The metal atoms in the ternary systems are shown to be predominantly homogeneously mixed in the silica network, as observed for the respective binary systems. The clear exception is for the sample with a minority of Zr, which after heat treatment at 750°C shows the presence of phase separation attributed to the formation of an amorphous precursor of ZrTiO4; at 1000°C this phase crystallises. In samples with higher Zr content the crystallisation of a ZrO2 tetragonal phase was observed. The data obtained illustrate well the strength of a research methodology in which a common batch of samples is studied using a coherent suite of modern structural probes. 相似文献
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We study the nonlinear Schrödinger equation with sequences of initial data that converge to a Dirac mass, and study the asymptotic behaviour of solutions. In doing so we find a connection to previously known long time asymptotics. We demonstrate a type of universality in the behaviour of solutions for real initial data, and we also show how this universality breaks down for examples of initial data that are not purely real. 相似文献
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Isoperimetric inequalities are applied to a moving-boundaryproblem for doubly-connected domains. This problem occurs forexample in electrochemistry, in which case the domains in questionare the electrolyte of an electrolytic cell. The two electrodessurrounding the electrolyte are assumed to grow or dissolve,at different rates in general, by electrochemical reaction.We obtain optimal estimates showing, for example, that the leastchange in volume of each electrode always occurs in sphericalsymmetry. 相似文献
10.
O'Dell LA Gunawidjaja PN Holland MA Mountjoy G Pickup DM Newport RJ Smith ME 《Solid state nuclear magnetic resonance》2008,33(1-2):16-24
The HfO2-SiO2 system is attracting interest as a possible new dielectric material in semiconductor devices. Knowledge of the location of hafnium within the silica network and the effect hafnium has on the structure will be central to the successful use of this material system in this application. Here, sol-gel techniques have been used to manufacture (HfO2)x(SiO2)1-x samples (x=0.1, 0.2 and 0.4, each heat treated at 250, 500 and 750 degrees C) and these have been characterised by magic angle spinning (MAS) NMR (1H, 13C, 17 O, 29Si), Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis. 29Si MAS NMR showed that increasing the hafnia content decreases the connectivity of the silicate network, i.e. increases the range of differently connected SiO4 (Qn) units with more having increased numbers of non-bridging oxygens (i.e. lower n). FTIR and 17 O MAS NMR showed unequivocally that the x=0.4 sample phase-separated at higher temperatures, while in the x=0.1 sample the hafnium was homogeneously mixed into the SiO2 phase without any phase separation. 相似文献