• Korean Journal of Materials Research
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• v.33 no.7
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• pp.265-272
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• 2023

In this study, the synthesis of nitrobenzene was carried out using sulfated silica catalyst. The study delved into H₂SO₄/SiO₂ as a solid acid catalyst and the effect of its weight variation, as well as the use of a microwave batch reactor in the synthesis of nitrobenzene. SiO₂ was prepared using the sol-gel method from TEOS precursor. The formed gel was then refluxed with methanol and calcined at a temperature of 600 ℃. SiO₂ with a 200-mesh size was impregnated with 98 % H₂SO₄ by mixing for 1 h. The resulting 33 % (w/w) H₂SO₄/SiO₂ catalyst was separated by centrifugation, dried, and calcined at 600 ℃. The catalyst was then used as a solid acid catalyst in the synthesis of nitrobenzene. The weights of catalyst used were 0.5; 1; and 1.5 grams. The synthesis of nitrobenzene was carried out with a 1:3 ratio of benzene to nitric acid in a microwave batch reactor at 60 ℃ for 5 h. The resulting nitrobenzene liquid was analyzed using GC-MS to determine the selectivity of the catalyst. Likewise, the use of a microwave batch reactor was found to be appropriate and successful for the synthesis of nitrobenzene. The thermal energy produced by the microwave batch reactor was efficient enough to be used for the nitration reaction. Reactivity and selectivity tests demonstrated that 1 g of H₂SO₄/SiO₂ could generate an average benzene conversion of 40.33 %.

• Journal of the Korean Ceramic Society
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• v.51 no.6
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• pp.605-611
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• 2014

$SrGd_{2-x}(MoO_4)_4:Er^{3+}/Yb^3$ phosphors with doping concentrations of $Er^{3+}$+ and $Yb^{3+}$ ($x=Er^{3+}+Yb^{3+}$, $Er^{3+}=0.05$, 0.1, 0.2, and $Yb^{3+}=0.2$, 0.45) were successfully synthesized by the cyclic microwave-modified sol-gel method, and their upconversion mechanism and spectroscopic properties have been investigated in detail. Well-crystallized particles showed a fine and homogeneous morphology with grain sizes of $2-5{\mu}m$. Under excitation at 980 nm, $SrGd_{1.7}(MoO_4)_4:Er_{0.1}Yb_{0.2}$ and $SrGd_{1.5}(MoO_4)_4:Er_{0.05}Yb_{0.45}$ particles exhibited a strong 525-nm emission band, a weak 550-nm emission band in the green region, and a very weak 655-nm emission band in the red region. The Raman spectra of the doped particles indicated the domination of strong peaks at higher frequencies of 1023, 1092, and $1325cm^{-1}$ and at lower frequencies of 223, 2932, 365, 428, 538, and $594cm^{-1}$ induced by the incorporation of the $Er^{3+}$+ and $Yb^{3+}$+ elements into the $Gd^{3+}$ site in the crystal lattice, which resulted in the unit cell shrinkage accompanying a new phase formation of the $[MoO_4]^{2-}$ groups.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2004.07b
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• pp.648-651
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• 2004

Pb0.5Sr0.5TiO3(PST) thin films were deposited on the LaNiO3 (LNO(100))/Si and Pt/Ti/SiO2/Si substrates by the alkoxide-based sol-gel method. Structural and dielectric properties of PST thin films for the tunable microwave device applications were investigated. The PST films, which were directly grown on the Pt/Ti/SiO2/Si substrates showed the random orientation. For the LNO/Si substrates, the PST thin films exhibited highly (100) orientation. Compared with randomly oriented films, the highly (100)-oriented PST thin films showed better dielectric constant, tunability, and figure of merit (FOM). The dielectric constant, tunability, and FOM of the highly (100)-oriented PST thin film increased with increasing annealing temperature due to the decrease in lattice distortion. The differences in dielectric properties may be attributed to the change in the film stress and the in-plane oriented Polar axis depending on the substrate was used. The dielectric constants, dielectric loss and tunability of the PST thin films deposited on the LNO/Si substrates measured at 1 MHz were 483, 0.002, and 60.1%, respectively.

• Journal of Ceramic Processing Research
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• v.20 no.3
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• pp.222-230
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• 2019

Microwave hydrothermal-assisted sol-gel method was employed to synthesize the Fe doped TiO2 photocatalyst. The morphological analysis suggests anatase phase nanoparticles of ~20 nm with an SBET area of 283.99 ㎡/g. The doping of Fe ions in TiO2 created oxygen vacancies and Ti3+ species as revealed through the XPS analysis. The reduction of the band gap (3.1 to 2.8 eV) is occurred by doping effect. The as-prepared photocatalyst was applied for removal of NOx under solar light irradiation. The doping of Fe in TiO2 facilitates 75 % of NOx oxidation efficiency which is more than two-fold enhancement than the TiO2 photocatalyst. The possible reason of enhancement is associated with high surface area, oxygen vacancy, and reduction of the band gap. Also, the low production of toxic intermediates, NO2 gas, is further confirmed by Combustion Ion Chromatography. The mechanism related NOx oxidation by the doped photocatalyst is explained in this study.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2002.07b
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• pp.749-751
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• 2002

$(Pb_{1-x}Sr_x)TiO_3$ $(0.6{\leq}x{\leq}0.8)$ thin films were prepared by the MOD method for tunable microwave device application and their characteristics were investigated as a function of Sr content(x) and applied field. Thin films showed a homogeneous microstructure and the tetragonality(c/a) was slightly decreased with increasing Sr content. With increasing Sr content, Curie temperature of the thin films showed a decreasing tendency. For the PST thin films, the dielectric constant at room temperature, Tc, and $tan{\delta}$ were 750~1900, $-70^{\circ}{\sim}-30^{\circ}C$ and 0.025~0.04, respectively.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2002.07b
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• pp.1113-1115
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• 2002

Mesoporous silica, MCM-41, was synthesized by sol-gel method. The organic structure-directing agent must be removed to make the desired proes. To achieve this, alternative calcination method using microwave oven was adapted to this removal stage. Microwave calcination was shown to provide a novel, rapid and inexpensive method of praparing nanoporous material. It was studied how the porous structure, surface area and pore size distribution were changes under microwave calcination.

• Korean Journal of Metals and Materials
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• v.47 no.8
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• pp.516-521
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• 2009

In this study we report a rapid synthesis of nanoporous organo-functional silica (OFS) with unimodal and bimodal pore structures encompassing pores ranging from meso-to macroscale. The problems of tediousness and high production cost in the conventional syntheses are overcome by co-condensation of an inexpensive inorganic precursor, sodium silicate with an organosilane containing trimethyl groups. The insitu covalent anchoring of the non-polar trimethyl groups to the inner pore walls prohibits irreversible shrinkage of the wet-gel during microwave drying at ambient pressure and thus larger size pores (from ca. 20 to ca. 100 nm) can be retained in the dried silica. The drying process of the silylated wet-gels at an ambient pressure can be greatly accelerated upon microwave exposure instead of drying in an oven or furnace. Using this approach, anoporous and superhydrophobic silicas showing a wide variation in texture and morphology can be readily synthesized in roughly two hours. The effects of various sol-gel parameters solely on the textural properties of the organo-functional silica (OFS) have been investigated and discussed.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2004.07b
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• pp.768-771
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• 2004

Pb0.5,Sr0.5TiO3(PST) thin films were deposited on Si with MgO (100) buffer layer by the alkoxide-based sol-gel method. Structural and dielectric properties of PST thin films for the tunable microwave device applications were investigated. For the MgO/Si buffer layer, the PST thin films exhibited highly (100) orientation. The MgO buffer layer affects the stress state of the (100)-oriented PST thin films. The dielectric constant, tunability, and FOM of the highly (100)-oriented PST thin film increased with increasing annealing temperature due to the decrease in lattice distortion. The differences in dielectric properties may be attributed to the change in the film stress. The dielectric constants, dielectric loss and tunability of the PST thin films deposited on the MgO/Si substrates measured at 10 kHz were 822, 0.025, and 80.1%, respectively.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2003.08a
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• pp.31-34
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• 2003

($Ba_{0.6-x}Sr_{0.4}Ca_x)TiO_3$ (BSCT) (x=0.10, 0.15, 0.20) powder, prepared by the sol-gel method, were mixed with organic vehicle and the BSCT thick films were fabricated by the screen-printing techniques on alumina substrates using the BSCT paste. The structural and the electrical properties were investigated for various composition ratio and sintering temperature. BSCT thick film thickness, obtained by four printings, was approximately 110 ~ 120 ${\mu}m$. The Curie temperature and dielectric constant at room temperature were decreased with increasing Ca content. The relative dielectric constant, dielectric loss and tunability of the BSCT(50/40/10) specimen, which was sintered at $1420^{\circ}C$ and measured at 1MHz, were about 910, 0.46% and 9.28% at 5kV/cm, respectively.

• Korean Journal of Materials Research
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• v.29 no.12
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• pp.741-746
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• 2019

New triple tungstate phosphors NaPbLa(WO₄)₃:Yb³⁺/Ho³⁺ (x = Yb³⁺/Ho³⁺ = 7, 8, 9, 10) are successfully fabricated by microwave assisted sol-gel synthesis and their structural and frequency upconversion (UC) characteristics are investigated. The compounds crystallized in the tetragonal space group I4₁/a and the NaPbLa(WO₄)₃ host have unit cell parameters a = 5.3927(1) and c = 11.7961(3) Å, V = 343.05(2) ų, Z = 4. Under excitation at 980 nm, the phosphors have yellowish green emissions, which are derived from the intense ⁵S₂/⁵F₄→⁵I₈ transitions of Ho³⁺ ions in the green spectral range and strong ⁵F₅→⁵I₈ transitions in the red spectral range. The optimal Yb³⁺:Ho³⁺ ratio is revealed to be x = 9, which is attributed to the quenching effect of Ho³⁺ ions, as indicated by the composition dependence. The UC characteristics are evaluated in detail under consideration of the pump power dependence and Commission Internationale de L'Eclairage chromaticity. The spectroscopic features of Raman spectra are discussed in terms of the superposition of Ho³⁺ luminescence and vibrational lines. The possibility of controlling the spectral distribution of UC luminescence by the chemical content of tungstate hosts is demonstrated.