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1.
Glass films of pure SiO 2 and TiO 2 have been prepared on sodalime silica flat slide glasses by the sol-gel process using the dip-coating technique from TEOS and Ti(OC 3H 7) 4 solutions. The various parameters such as chemicals concentrations, viscosity, type of catalyst, withdrawal speed and temperature of densification leading to the obtention of good and adherent coatings with definite film thicknesses are reported. The same technique has been used for the depositon of layers of colored films SiO 2---M xO y (M = Co, Mn, Nd and Cr). Brilliant yellow coatings have been obtained with TiO 2---CeO 2. 相似文献
2.
Different solutions containing alkoxides of silicon, titanium, and zirconium have been prepared. Some of their properties like the time dependent viscosity and the gelling time have been measured and are reported here for different H 2O, HCl, ethanol and/or formamide contents. Microscope slides have been dip coated in these solutions. After baking, film thickness and chemical durability have been determined. In order to get good SiO2---TiO2---ZrO2 glass coatings, the withdrawal speed should not exceed 5 cm/min unless the viscosities of the solutions are reduced by the addition of ethanol. By such a dilution, the film thickness could also be reduced, while the addition of formamide caused a delayed increase of the viscosity and increased gelling times. For this reason, solutions containing formamide can be used for longer periods. The chemical durability of the substrates against boiling NaOH solution is enhanced by the SiO2---TiO2---ZrO2 glass coatings. 相似文献
3.
Various oxide films on SiO 2 glass substrates were irradiated by a laser beam. A continuous CO 2 laser source (wavelength 10.6 μm) was used for this purpose; the composition change at the surface layer was determined by Rutherford backscattering spectrometry (RBS). All the alkaline-earth oxides as well as those of lanthanum and yttrium, entered the glass after treatment. ZrO 2 and CeO 2, however, did not enter the SiO 2 glass due to laser irradiation. It is interesting, however, that a film of ZrO 2 + Al 2O mixture easily entered into the SiO 2 glass by laser processing. The conditions and mechanism of laser-enhanced interaction of ZrO 2 or other oxide films with SiO 2 glass surfaces are discussed especially in view of their structural behaviour in glass. 相似文献
4.
The gel formation of the (100- x)TiO 2· xSiO 2 ( x = 0–10 mol%) system has been studied. The progressive elimination of residues was followed by DTA and TGA curves. DTA curves showed that the formation of anatase during heat treatment could be sensibly slowed down with the increase of SiO 2. The relationship between the gel composition and crystallization temperature of anatase has been systematically investigated. The X-ray diffraction spectra demonstrated that the crystallization temperature of anatase is 400°C for TiO 2 gel and 430°C for 90TiO 2 - 10SiO 2 gel. The infrared absorption spectra were used to follow the structural transformation of gels heat-treated at different temperatures. With the help of EPR it is evident that titanium ions exist only in tetravalence. 相似文献
5.
A series of titania-silica glasses with 0–9% TiO 2 were fabricated using a sol/gel process. The sol was prepared by dispersing colloidal silica fume in an aqueous solution of titania which was synthesized through the acid-catalyzed hydrolysis of titanium isopropoxide. The sols gelled in 2–4 days, and then were dried for 6–8 days. The dry gels were sintered at 1450–1500°C to produce clear, dense, microstructure-free glasses. The gels underwent a total shrinkage of 50% to yield glass rods about 50 mm long and 5 mm in diameter, or glass discs about 4 cm in diameter and 5 mm thick. The drying step was most critical in the production of crack-free specimens. In the gel, the transmission electron microscope (TEM) revealed the presence of 1–5 nm rutile microcrystallites uniformly distributed within a network of colloidal silica particles. After sintering to 1450–1500°C, though, a dense, transparent, microstructure-free glass was created. Fourier transform infrared spectroscopy (FTIR) verified the formation of an amorphous solid-solution of titania and silica after sintering. The thermal expansion of the glasses was measured using a differential dilatometer. The average linear coefficients of thermal expansion (CTE @ 25–675°C) varied between +5 × 10−7 and −0.2 × 10−7°C−1 in the range 0 to 9% TiO2. The glass with 7.2% TiO2 exhibited a zero thermal expansion coefficient at 150–210°C. The hysteresis in CTE on heating and cooling was of the order of 0.01–0.02 ppm. 相似文献
6.
The preparation of glass-lined coating mould from gels in the ternary system of SiO 2–ZrO 2–B 2O 3 has been investigated. The crystallization characterization and high temperature structure stability of this coating mould are demonstrated. We can find that the crystallization of t-ZrO 2 as well as the tetragonal to monoclinic phase transformation are, respectively, retarded and impeded owing to the encasement of SiO 2 matrix. While the inhibitive effect of B 2O 3 on crystallization of the SiO 2–ZrO 2–B 2O 3 coating mould is explained. Finally, DD3 single crystal superalloy melt can realize highly undercooled rapid solidification by adopting this coating mould, which further evinces that SiO 2–ZrO 2–B 2O 3 coating mould has an ideal nucleation inhibition for superalloy. 相似文献
7.
Small-angle X-ray scattering was used to examine in situ formation of ZrO 2---SiO 2 structures in alcoholic solution of tetraethoxysilan (TEOS) as a function of the ratio of ZrO 2 to SiO 2. For the moment of the first measurement (15 min after the preparation) primary particles with Rg ≈ 1.5 nm exist in all investigated mixed gels. These particles aggregated to secondary clusters. The resulting clusters can be described by means of fractal theory, where the determining mechanism of formation is cluster-cluster aggregation (diffusion or chemical limited). The time of gelation is a function of the ZrO 2 concentration. The higher the ZrO 2 concentration in the solution, the faster is the aggregation to secondary clusters. Gelation times were between 170 and 970 h. 相似文献
8.
The colorless and transparent glasses in the Al 2O 3---B 2O 3---SiO 3 system with high B 2O 3 and SiO 2 content were prepared from gels at low temperature. Their IR spectra not only revealed the evolution of the gel to glass conversion, but also showed that the formation of mixed bonds in the glasses obtained did not show any effect due to the B 2O 3 content. The accuracy of the glass composition is dependent upon the SiO 2/B 2O 3 molar ratio. The higher the ratio, the less the deviation of the analyzed compositions of the resulting glasses from their original calculated values. It is obvious that the higher the ratio, the lower the thermal expansion coefficient and the higher the transformation temperature of the glass, and the temperature at which the thermal contraction reaches an equilibrium is higher. 相似文献
9.
The surface of a TiO 2 film electrode, about 1 μm thick, prepared by the sol-gel method, was modified by being additionally coated with about 0.1 μm thick TiO 2---SiO 2, TiO 2---ZrO 2 or TiO 2---Al 2O 3 films. The effect of the additional coating on the photoelectrochemical properties of a TiO 2 film electrode was investigated in detail. On addition of the second additive to TiO 2, the flat band potential was shifted toward negative potential for SiO 2 and positive potential for ZrO 2 and Al 2O 3, which is attributed to the change in the point of zero zeta potential (pzzp), not in the electron affinity ( EA). However, enhancement in photocurrent was not observed for all the cases. 相似文献
10.
We investigated the dependence of the Y 2O 3 film growth on Si surface at initial growth stage. The reflection high-energy electron diffraction, X-ray scattering, and atomic force microscopy showed that the film crystallinity and morphology strongly depended on whether Si surface contained O or not. In particular, the films grown on oxidized surfaces revealed significant improvement in crystallinity and surface smoothness. A well-ordered atomic structure of Y 2O 3 film was formed on 1.5 nm thick SiO 2 layer with the surface and interfacial roughness markedly enhanced, compared with the film grown on the clean Si surfaces. The epitaxial film on the oxidized Si surface exhibited extremely small mosaic structures at interface, while the film on the clean Si surface displayed an island-like growth with large mosaic structures. The nucleation sites for Y 2O 3 were provided by the reaction between SiO 2 and Y at the initial growth stage. The SiO 2 layer known to hinder crystal growth is found to enhance the nucleation of Y 2O 3, and provides a stable buffer layer against the silicide formation. Thus, the formation of the initial SiO 2 layer is the key to the high-quality epitaxial growth of Y 2O 3 on Si. 相似文献
11.
Glasses of compositions 5ZrO 2·5SiO 2(ZS), 5ZrO 2·Al 2O 3·4SiO 2(ZAS) and 5 5ZrO 2·0.5Al 2O 3·0.5Na 2O·4SiO 2(ZANS) were prepared by the sol-gel process from metal alkoxides and sintered to make glass-ceramics. Tetragonal ZrO 2 was precipitated by heat treatment at 900 to 1300°C. The activation energy for tetragonal ZrO 2 crystal growth was extremely high in Al 2O 3 containing glasses. ZAS and ZS were sintered to the near theoretical densities above 1200°C, at which the predominant phase was tetragonal ZrO 2. On the other hand, for ZANS, high densification was not attained owing to the large pores enclosed by the glass phase. Strength and fracture toughness increased with the densification and the crystal growth of tetragonal ZrO 2, reaching 450 MPa and 9 MN/m 1.5, respectively. 相似文献
12.
Alkoxide derived gels were prepared in the system Na 2O---B 2O 3---SiO 2. The gel compositions were situated in the liquid-liquid immiscibility area of the phase equilibrium diagram. Hydrolytic resistance tests were performed on the gels heat-treated at temperatures ranging between 120 to 850 °C. The Na2O, B2O3 and SiO2 extracted from the attack gels were analyzed. The experimental results indicate that the amount of B2O3 has a significant influence on the chemical durability of the heat-treated gels. At temperatures of 850 °C the greater the B2O3 mol% the greater are the amounts of Na2O and B2O3 extracted. Different behaviour was observed for gels heat-treated at 600 °C where the amounts of B2O3 and Na2O extracted slightly increases as the B2O3 mol% increases. Small amounts of extracted SiO2 were always observed. These results are complemented with other measurements so that an explanation of the controlling mechanism is given. 相似文献
13.
Thin films of CdS-doped SiO 2 glass were prepared by using the conventional pulsed laser deposition (PLD) technique. The laser target consisted of a specially constructed rotary wheel which provided easy control of the exposure-area ratio to expose alternately the two materials to the laser beam. The physical target assembly avoided the potential complications inherent in chemically mixed targets such as in the sol–gel method. Time-of-flight (TOF) spectra confirmed the existence of the SiO 2 and CdS components in the thin-film samples so produced. X-ray diffraction (XRD) and atomic force microscopy(AFM) results showed the different sizes and structures of the as-deposited and annealed films. The wurtzite phase of CdS was found in the 600 oC-annealed sample, while the as-deposited film showed a cubic–hexagonal mixed structure. In the corresponding PL (photoluminescence) spectra, a red shift of the CdS band edge emission was found, which may be a result of the interaction between the CdS nanocrystallite and SiO 2 at their interface. 相似文献
14.
We report the infrared and Raman studies of titanium doped vitreous silica glasses for a number of titanium concentrations. The vibrational modes associated with the randomly oriented chains of SiO 4 tetrahedra show broadenings and shifts. The LO-TO splitting of some Raman active modes decreases with increasing titanium concentration. This is attributed to the decrease in long-range coulomb fields associated with the chains of SiO 4 tetrahedra which are broken by the titanium atoms. The results are discussed in the context of random network models. An increase in the average intertetrahedral angle of the SiO 4 network is calculated from the data. This explains the anomalous decrease in the density of TiO 2---SiO 2 glasses with increasing titanium content. We identify two new modes associated with the distorted titanium tetrahedra. A polarized Raman mode at 1115 cm −1 which is infrared inactive and an unpolarized Raman mode at 945 cm −1 which is infrared active are observed. 相似文献
15.
The type and the amount of silicate groupings existing in glassy and crystalline 2PbO·SiO 2 have been determined by direct chemical methods: paper chromatography, trimethylsilylation combined with gas-liquid partition chromatography and by the molybdate method. The results obtained by these three different methods are in good agreement and demonstrate, that glassy 2PbO·SiO 2 and each of the three main crystalline polymorphs are characterized by its own specific silicate anion distribution: the distribution in vitreous 2PbO·SiO 2 is of a polyanionic nature; in T---Pb 2SiO 4 dimetic groups [Si 2O 7] 6− prevail; M 1---Pb 2SiO 4 contains predominantly [Si 4O 12] 8− rings and H---Pb 2SiO 4 is a typical polysilicate with chain anions [SiO 32−] n. The results fit a structural model according to which glass is a random array of discrete polyatomic groupings; the gradual transition from the glassy state to the stablest crystalline structure is connected with degradation and polymerization of silicate anions. 相似文献
16.
11B Fourier transform spectra have been used to study the structure of Na 2O---B 2O 3---SiO 2 glasses of mid-alkali content. Based on the measurements of the fraction N4 of four-coordinated borons, it has been found that for K = mol.% SiO 2/mol.% B 2O 3 8 and R = mol.% Na 2O/mol.% B 2O 3 = 1, N4 is obviously smaller than 1 rather than equal to 1 as assumed in the relevant literature. Only when R reaches a value appropriately greater than 1, can the case where N4 = 1 occur. A structural model suggested in this paper can satisfactorily explain the fact. 相似文献
17.
The conditions under which selective epitaxial growth (SEG) is achieved in UHV-CVD with Si 2H 6 are determined by the amount of Si 2H 6 molecules being supplied, and there is a critical gas supply amount ( Fc) beyond which SEG will break down and lose its selectivity. The value of Fc is itself determined by two factors, growth temperature and the material used for masking, i.e. SiO 2, Si 3N 4. We found that this limiting factor of Fc was increased through the addition of a small amount of Cl 2, and that after such addition, the resulting decrease in growth rate is minimal. 相似文献
18.
Thermally stimulated luminescence (TSL) and infrared (IR) spectroscopy were measured in plasma grown Si 1−xGe xO 2 ( x=0, 0.08, 0.15, 0.25, 0.5) with different thicknesses (12–40 nm). A comparison with the TSL properties of thermally grown SiO 2 and GeO 2 was also performed. A main IR absorption structure was detected, due to the superposition of the peaks related to the asymmetric O stretching modes of (i) Si–O–Si (at ≈1060 cm −1) and (ii) Si–O–Ge (at 1001 cm −1). Another peak at ≈860 cm −1 was observed only for Ge concentrations, x>0.15, corresponding to the asymmetric O stretching mode in Ge–O–Ge bonds. A TSL peak was observed at 70°C, and a smaller structure at around 200°C. The 70°C peak was more intense in all Ge rich layers than in plasma grown SiO 2. Based on the thickness dependence of the signal intensity we propose that at Ge concentrations 0.25 x0.5 TSL active defects are localised at interfacial regions (oxide/semiconductor, Ge poor/Ge rich internal interface, oxide external surface/atmosphere). Based on similarities between TSL glow curves in plasma grown Si 1−xGe xO 2, thermally grown GeO 2 and SiO 2 we propose that oxygen vacancy related defects are trapping states in Si 1−xGe xO 2 and GeO 2. 相似文献
19.
The structure of Li 2O·SiO 2 glass has been determined by the pair-function analysis of the radial distribution function (RDF) obtained by X-ray and neutron diffraction measurements. The structure models were constructed by the molecular dynamics method (MD). The calculated RDFs, the summation of the pair-functions of the model, were compared with the observed RDFs while varying the MD parameters. Taking advantage of the negative scattering length of Li for neutron diffraction, the glass structure was investigated in detail, and it was found that the chains of SiO 4 tetrahedra bend at 20 °, which is a little less than for the crystal (23.48 °). It is known that the larger the size of the alkali ions (Na + → K + → Cs +), the smaller the bending angle of the chains. It was found that this rule also applies to Li +. 相似文献
20.
The La L 1 and L 3 XANES and L 3 EXAFS have been investigated for the series of glasses 10K 2O---50SiO 2--- x La 2O 3 ( x = 1, 5, 10) and (10 − x)K 2O---40SiO 2−( x/3)La 2O 3 ( x = 7.5, 5, 2.5) and model compounds La 2O 3, LaAlO 3, LaPO 4, La 2NiO 4, La 2CuO 4 and La(OH) 3. An edge resonance at 25 eV above the L 1 edge in the glass spectra is concentration-dependent, decreasing in intensity with increasing lanthanum concentration. The 2s → nd forbidden transition increases with La 2O 3 concentration, indicating a reduction in the ‘average’ site symmetry of the first coordination shell of La. Mapping X( k) space, which is a new and promising technique, was employed to extract bond distance, coordination number and thermal parameters from the EXAFS. By this method, one calculates the complete X( k) space a function of all physically reasonable values of the adjusted parameters in all possible combinations. The advantage in this method is the assurance of a global minimum. Bond lengths were comparable to those obtained by Fourier transforming the phase corrected EXAFS. The values are 2.42 Å (± 0.03 Å) for La---O. The coordination numbers ( N ≤ 7 ± 1.5) were derived by mapping and comparison to the published structures for other La compounds. X( k) mapping is compared with least-squares fitting the data, and the correlation between the Debye-Waller factor and coordination number is also discussed. 相似文献
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