• 한국분말재료학회지
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• 제17권3호
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• pp.209-215
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• 2010

Mesoporous alumina particles were prepared by spray pyrolysis using cetyltrimethyl-ammonium bromide (CTAB) as a structure directing agent and the effect of Al precursor types on the texture properties was studied using $N_2$ adsorption isotherms, small-angle X-ray scattering (SAXS), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The surface area and the microstructure of alumina particles were significantly influenced by the Al precursor type. The largest BET surface area was obtained when Al chloride was used, whereas alumina particles prepared from Al acetate had the largest pore volume. According to small-angle X-ray scattering (SAXS) analysis, the alumina powders prepared using nitrate and acetate precursors had a clear single SAXS peak around $2{\theta}=1.0{\sim}1.5^{\circ}$, indicating that regular mesopores with sponge-like structure were produced. On the basis of TEM, SAXS, and $N_2$ isotherm results, the chloride precursor was most profitable to obtain the largest surface area ($265\;m^2/g$), whereas, the nitrate precursor is useful for the preparation of non-hollow mesoporous alumina with regular pore size, maintaining high surface area (${\sim}233\;m^2/g$).

• Bulletin of the Korean Chemical Society
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• 제35권12호
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• pp.3465-3474
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• 2014

Porous silica particles are the most prevailing raw material for stationary phases of liquid chromatography. During a long period of time, various methodologies for production of porous silica particles have been proposed, such as crashing and sieving of xerogel, traditional dry or wet process preparation of conventional spherical particles, preparation of hierarchical mesoporous particles by template-mediated pore formation, repeated formation of a thin layer of porous silica upon nonporous silica core (core-shell particles), and formation of specific silica monolith followed by grinding and calcination. Recent developments and applications of useful porous silica particles will be covered in this review. Discussion on sub-$3{\mu}m$ silica particles including nonporous silica particles, carbon or metal oxide clad silica particles, and molecularly imprinted silica particles, will also be included. Next, the individual preparation methods and their feasibilities will be collectively and critically compared and evaluated, being followed by conclusive remarks and future perspectives.

• Bulletin of the Korean Chemical Society
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• 제34권7호
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• pp.2155-2161
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• 2013

Composite materials of mesoporous carbon and carbon nanotubes were synthesized using Ni, Co and Pd-loaded CMK3 via a catalytic reaction of methane and $CO_2$. The CNTs grew from the pores of the mesoporous carbon supports, and they were attached tightly to the CMK3 surface in a densely tangled shape. The CNT/CMK3 composite showed both non-graphitic mesoporous structures, and graphitic characteristics originating from the MWCNTS grown in the pores of CMK3. The electrochemical properties of the materials were characterized by their electrorheological effects and cyclic voltammetry. The CNTs/CMK3 composites showed high electrical conductivity and current density. The CNT/CMK3 or KOH-modified CNT/CMK3 particles were incorporated in a PMMA matrix to improve the thermal and electrical conductivity. Even higher thermal conductivity was achieved by the addition of KOH-modified CNT/CMK3 particles.

• Bulletin of the Korean Chemical Society
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• 제29권5호
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• pp.1007-1012
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• 2008

Spray pyrolysis has been found as an excellent method for the preparation of mesoporous barium sulfate at higher temperature. Ethylene glycol, a reducing agent, and solvents had good inhibition effect for the preparation of $BaSO_4$ nano particles. The $BaSO_4$ solution was sprayed at 500 & 800 ${^{\circ}C}$ using different solvents such as methanol, ethanol, propanol and n-butyl alcohol. $N_2$ adsorption-desorption isotherm revealed that $BaSO_4$ is micropore free, possessing narrow mesopores size distribution and high BET surface areas of 72.52 $m^2\;g^{-1}$ at 800 ${^{\circ}C}$ using propanol as an additive. Scanning electron microscopy (SEM) indicates that the morphology of $BaSO_4$ nano material shows uniform shell like particles. Transmission electron microscopy (TEM) proved that the resulting BaSO4 nano particles were uniform in size and the average particle size was 4-8 nm. The surface functionality and ethylene glycol peaks were assessed by Fourier transform infrared resonance (FTIR) spectroscopy. Low intensity ethylene glycol specific absorption peak was observed in propanol which proved that propanol had good inhibition effect on the structural morphology of nano particles.

• Bulletin of the Korean Chemical Society
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• 제31권1호
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• pp.100-103
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• 2010

In this study, NO reduction behaviors of copper-loaded mesoporous molecular sieves (Cu/MCM-41) have been investigated. The Cu loading on MCM-41 surfaces was accomplished by a chemical reduction method with different Cu contents (5, 10, 20, and 40%). $N_2/77$ K adsorption isotherm characteristics, including the specific surface area and pore volume, were studied by BET's equation. NO reduction behaviors were confirmed by a gas chromatography. From the experimental results, the Cu loading amount on MCM-41 led to the increase of NO reduction efficiency in spite of decreasing the specific surface area of catalysts. This result indicates that highly ordered porous structure in the MCM-41 and the presence of active metal particles lead the synergistical NO reduction reactions due to the increase in adsorption energy of MCM-41 surfaces by the Cu particles.

• Korean Journal of Chemical Engineering
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• 제35권12호
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• pp.2480-2486
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• 2018

Mesoporous $TiO_2$ microspheres were prepared by spray pyrolysis for photocatalysis. Post modification of $TiO_2$ by heat treatment was performed to optimize its photocatalytic performance. First, spherical $TiO_2$ particles with mesoporous structure were synthesized at pyrolysis temperatures of 500, 600, and $700^{\circ}C$. After characterization by XRD, SEM, and $N_2$ adsorption, a sample prepared at $500^{\circ}C$ was found to possess desirable properties for photocatalytic performance through post-modification. In methylene blue degradation, mesoporous $TiO_2$ microspheres synthesized at $500^{\circ}C$ outperformed other microspheres. Furthermore, samples obtained by spray pyrolysis at $500^{\circ}C$ were calcined at various temperatures as a post-modification process. The sample calcined at $350^{\circ}C$ showed improved photocatalytic activity due to optimal anatase crystallinity and surface area.

• 전기화학회지
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• 제14권3호
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• pp.184-190
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• 2011

다공성 중공형태의 $LiMn_2O_4$는 실리카 템플레이트과 침전법에 의해 합성되었다. 합성한 $LiMn_2O_4$는 나노사이즈의 1차입자를 가지며 다공성 중공형태를 가지고 있었다. 실리카 템플레이트의 제거는 NaOH를 이용하여 화학적 에칭법이 사용되었다. NaOH의 농도를 높여줌에 따라 망간산화물 입자 크기가 증가 하며 다공성의 중공구가 형성되었다. X-선 회절 분석을 통하여 합성된 $LiMn_2O_4$는 Fd3m의 공간 그룹을 가지는 스피넬 구조가 형성된 것을 확인 할 수 있었다. 실리카와 망간염의 비율을 높여주었을 경우 합성된 $LiMn_2O_4$는 1차입자의 크기는 감소한다. 실리카와 망간염의 비율이 1 : 9 이상인 경우에서 마이크론 단위의 정방정계의 $LiMn_2O_4$가 합성되었다. 다공성 중공형태의 $LiMn_2O_4$의 전기화학적 특성을 평가하기 위하여 2032형태의 코인셀을 제작하여 충/방전 테스트를 하였다. 나노사이즈의 1차입자를 가진 시료의 경우에는 마이크론 사이즈의 1차입자를 가진 시료보다 용량은 낮았지만 용량유지율은 향상되는 것 확인 할 수 있었다.

• 한국입자에어로졸학회지
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• 제8권2호
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• pp.89-95
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• 2012

Spherical mesoporous silica particles, of which main pore diameter was 3.8 nm, were successfully prepared by spray pyrolysis from aqueous silicic acid. The effect of precursor concentration, reaction temperature, and the addition of urea and PEG on the particle diameter and pore properties such as pore diameter, total pore volume, and specific surface area were investigated by using FE-SEM, particle size analyzer, and nitrogen absorption-desorption analysis. With an increase of the precursor concentration from 0.2 M to 0.7 M, the average particle diameter, total pore volume, and specific surface area of the porous silica particles increased from 0.56 to $0.96\;{\mu}m$, 0.434 to $0.486\;cm^3/g$, 467.8 to $610.4\;m^2/g$, respectively. Within the temperature range $(600\;^{\circ}C{\sim}800\;^{\circ}C)$, there was no significant difference in the pore diameter, total pore volume, and specific surface area. In addition, the addition of urea as an expansion aid led to slight increases in particle diameter, pore diameter, and specific surface area. However, when the polyethylene glycol (PEG) as an organic template was used, the total pore volume of porous particles increased dramatically.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2011년도 제41회 하계 정기 학술대회 초록집
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• pp.200-200
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• 2011

Hierarchical mesoporous ZSM-5 with enhanced mesoporosity was synthesized by microwave through the rapid assembly via ionic interaction between sulfonic acid functionalized ZSM-5 nano particles and cationic surfactant. The catalytic performance of enhanced accessibility due to mesoporosity and acidity were investigated in the alkylation of mesitylene with benzyl alcohol as alkylating agent. The effect of mole ratio of aromatic with benzyl alcohol, reaction time and alkylation agent were also studied. The enhanced mesoporosity and acidity of sulfonic acid functionalized mesoporous ZSM-5 induced activity enhancement compared with non-functionalized mesoporous ZSM-5, sulfonic functionalized mesoporous ZSM-5 synthesized by hydrothermal method and conventional microporous ZSM-5. The sulfonic acid functionalized mesoporous ZSM-5 showed much higher chemoselectivity of benzylated mesitylene than others, whereas the others mainly show dibenzyl ether as product. This significant difference in catalytic selectivity was resulted from the existence of mesopores, which definitely allowed the benzylation in mesopores.

• Bulletin of the Korean Chemical Society
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• 제29권3호
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• pp.609-614
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• 2008

A periodic mesoporous organosilica material was synthesized by microwave heating (PMO-M) using 1,2-bis(trimethoxysilyl)ethane as a precursor in a cationic surfactant solution, and textural properties were compared with those of the product produced by conventional convection heating (PMO-C). These synthesized materials were characterized using XRD, TEM/SEM, N2 adsorption isotherm, 29Si and 13C NMR, and TGA, which confirmed their good structural orders and clear arrangements of uniform 3D-channels. Synthesis time was reduced from 21 h in PMO-C to 2-4 h in PMO-M. PMO-M was made of spherical particles of 1.5-2.2 m m size, whereas PMO-C was made of decaoctahedron-shaped particles of ca. 8.0 m m size. Effect of synthesis temperature, time, and heating mode on the PMO particle morphology was examined. The particle size of PMO-M could be controlled by changing the heating rate by adjusting microwave power level. PMO-M demonstrated improved separation of selected organic compounds compared to PMO-C in a reversed phase HPLC experiment. Ti-grafted PMO-M also resulted in higher conversion in liquid phase cyclohexene epoxidation than by Ti-PMO-C.