• 한국세라믹학회지
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• 제28권1호
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• pp.60-66
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• 1991

The polymeric alumina sol was prepared by partial hydrolysis of aluminum sec-butoxide reacted with acetylacetone and its characteristics was investigated. The effects of alcohol solvent, acetylacetone, and acid concentration to the sol were investigated. FT-IR and Al27-MASNMR were used to study hydrolysis and polymerization reaction of aluminum complex. Synthesized sol showed the characteristics of polymeric alumina sol. To make a clear polymeric alumina sol, the optimum contents of acetylacetone, H2O and alcohol solvent were 0.4-0.6 mole, 0.25-1.25 mole, 3-5 mole per one mole alkoxide respectively. As a result of the Al27-MASNMR analysis, it was noted that hexa-penta-coordinated Al were main structure.

• 한국세라믹학회지
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• 제28권9호
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• pp.705-711
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• 1991

Alumina precursor sol was obtained by the reaction of Al(OC4H9)3 and acetylacetone in the solvent followed by the partial hydrolysis. This sol was measured by viscosity and the effect of pH. The powders obtained from this sol were calcined at the various temperatures. The transition of crystals and crystal state were investigated at the various temperatures. The powders dried at 90$^{\circ}C$ showed amorphous and ${\gamma}$-Al2O3 at 900$^{\circ}C$, ${\alpha}$-Al2O3 mono-phase at 1050$^{\circ}C$ respectively. As a result of Al27-MASNMR analysis, amorphous and ${\alpha}$-Al2O3 powders showed 6-coordinated Al, ${\gamma}$-Al2O3 4-coordinated Al respectively.

• 한국세라믹학회지
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• 제25권6호
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• pp.585-592
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• 1988

Aluminum sec-butoxide was synthesized from aluminum foil and alcohol. The characteristics of the alumina powder prepared from the synthesized alkoxide by the Yoldas method were studied. As a result of measuring the synthesized aluminum sec-butoxide by GC, the purity of the synthesized alkoxide was 98.7% on the basis of commercial alkoxide and the yield was 78.5%. A127-MASNMR analysis shows that powders dried at 9$0^{\circ}C$ and $\alpha$-Al2O3 have 6-cordinated structure and ${\gamma}$-Al2O3 has 4-coordinated structure. The characteristics of alumina powder prepared from the synthisized alkoxide showed the same characteristics with the alumina powder prepared from the commercial alkoxide.

• Bulletin of the Korean Chemical Society
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• 제34권1호
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• pp.143-148
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• 2013

Novel titanium containing solid core mesoporous shell silica has been synthesized by using octadecyltrichloro silane and triethylamine. The synthesized material was characterized by various physicochemical techniques. The mesoporous character of the material has been revealed from PXRD studies. The presence of octadecyltrichloro silane and triethylamine in the sample has been confirmed from EDAX studies. TG/DTA analysis reveals the thermal characteristics of the synthesized material. The presence of titanium in the frame work and its coordination state has been studies by UV-vis DR studies and XPS analysis. Chemical environment of Si in the framework of the material has been studied by $^{29}SiMASNMR$ studies. The surface area of the material is found to be around $550\;m^2g^{-1}$ and pore radius is of nano range from BET analysis. The spherical morphology and particle size of the core as well as shell has been found to be 300 nm and 50 nm respectively from TEM analysis. The catalytic application of this material towards the synthesis of caprolactam from cyclohexanone in presence of hydrogen peroxide through ammoxidation reaction has been investigated. The optimum conditions for the reaction have been established. The plausible mechanism for the formation of core silica and conversion of cyclohexanone has been proposed.

• The Korean Journal of Ceramics
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• 제4권4호
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• pp.323-330
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• 1998

Mixed oxide compounds of potential usefulness for fibre coatings (hexagonal celsian, $BaAl_2Si_2O_8$ and lanthanum hexaluminate, $LaAl_{11}O_{18}$) or for matrix materials (yttrium aluminium garnet, $Y_3Al_5O_{12}$) were prepared by hybrid sol-gel synthesis and their thermal crystallisation was monitored by thermal analysis, X-ray diffraction and multinuclear solid state MAS NMR. All the gels convert to the crystalline phase below about $12200^{\circ}C$, via amorphous intermediates in which the Al shows and NMR resonance at 36-38 ppm sometimes ascribed to Al in 5-fold coordination. Additional information about the structural changes during thermal treatment was provided by $^{29}Si$, $^{137}Ba$ and $^{89}Y$ MAS NMR spectroscopy, showing that the feldspar framework of celsian begins to be established by about $500^{\circ}C$ but the Ba is still moving into its polyhedral lattice sites about $400^{\circ}C$ after the sluggish onset of crystallization. Lanthanum hexaluminate and YAG crystallise sharply at 1230 and $930^{\circ}C$ respectively, the former via $\gamma-Al_2O_3$, the latter via $YAlO_3$. Yttrium moves into the garnet lattice sites less than $100^{\circ}C$ after crystallisation.