• Journal of the Korean Magnetic Resonance Society
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• v.14 no.2
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• pp.55-75
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• 2010

An ion-exchanged reaction of $MnCl_2$ with Al-incorporated solid core/mesoporous shell silica (AlSCMS) followed by calcinations generated manganese species, where average oxidation state of manganese ion is 3+, in the mesoporous materials. Dehydration results in the formation of $Mn^{2+}$ ion species, which can be characterized by electron spin resonance (ESR). The chemical environments of the manganese centers in Mn-AlSCMS were investigated by diffuse reflectance, UV-VIS and ESR spectroscopic methods. Upon drying at 323 K, part of manganese is oxidized to higher oxidation state ($Mn^{3+}$ and $Mn^{4+}$) and further increase in (average) oxidation state takes place upon calcinations at 823 K. It was found that the manganese species on the wall of the Mn-AlSCMS were transformed to tetrahedral $Mn^{3+}$ or $Mn^{4+}$ and further changed to square pyramid by additional coordination to water molecules upon hydration. The oxidized $Mn^{3+}$ or $Mn^{4+}$ species on the surfaces were reversibly reduced to $Mn^{2+}$ or $Mn^{3+}$ species or lower valances by thermal process. Mn(II) species I with a well resolved sextet was observed in calcined, hydrated Mn-AlSCMS, while Mn (II) species II with g = 5.1 and 3.2 observed in dehydrated Mn-AlSCMS. Both species I and II are considered to be non-framework Mn(II).

• Proceedings of the Korean Vacuum Society Conference
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• 2013.02a
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• pp.166-166
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• 2013

Mesoporous $SiO_2$-supported Ni catalysts (Ni/$SiO_2$ and Ni/$TiO_2$/$SiO_2$) were fabricated by atomic layer deposition (ALD), and their catalytic activity and stability were investigated in carbon dioxide reforming of methane (CRM) reaction at $800^{\circ}C$ The Ni/$SiO_2$ catalysts showed high stability as a result of confinement of Ni particles with a mean size of ~10 nm within the pores of $SiO_2$ support. Besides, X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and transmission electron microscopy (TEM) results showed that the Ni nanoparticles were partially buried inside the $SiO_2$ support. The strong interaction between Ni and the $SiO_2$ support could also be advantageous for long-term stability of the catalyst. In case of the Ni/$TiO_2$/$SiO_2$ catalyst, it was found that the catalytic activity of 10 nm-sized Ni nanoparticles was not much influenced by $TiO_2$ addition.

• Bulletin of the Korean Chemical Society
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• v.35 no.2
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• pp.377-382
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• 2014

Micro-/macroporous carbons (MMCs) were prepared using a hollow mesoporous silica capsule (HMSC) as a sacrificial hard template. The carbonization process after the infiltration of furfuryl alcohol into the template-free HMSC material afforded MMC materials in high yield. The hard template HMSC could be removed by HF etching without deteriorating the structure of MMC. The MMC materials were fully characterized by SEM, TEM, PXRD, XPS, and Raman spectroscopy. The replication processes were so successful that MMCs exhibited a hollow capsular structure with multimodal microporosity. Detailed textural properties of MMC materials were investigated by volumetric $N_2$ adsorption-desorption analysis at 77 K. To explore the gas sorption abilities of MMCs for other gases, $H_2$ and $CO_2$ sorption analyses were also performed at various temperatures. The multimodal MMC materials were found to be good sorbents for both $H_2$ and $CO_2$ at low pressure.

• Proceedings of the Korean Vacuum Society Conference
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• 2011.02a
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• pp.1-1
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• 2011

We developed a new generalized synthetic procedure, called as "heat-up process," to produce uniform-sized nanocrystals of many transition metals and oxides without a size selection process. We were able to synthesize uniform magnetite nanocrystals as much as 1 kilogram-scale from the thermolysis of Fe-oleate complex. Clever combination of different nanoscale materials will lead to the development of multifunctional nano-biomedical platforms for simultaneous targeted delivery, fast diagnosis, and efficient therapy. In this presentation, I would like to present some of our group's recent results on the designed fabrication of multifunctional nanostructured materials based on uniform-sized magnetite nanoparticles and their medical applications. Uniform ultrasmall iron oxide nanoparticles of <3 nm were synthesized by thermal decomposition of iron-oleate complex in the presence of oleyl alcohol. These ultrasmall iron oxide nanoparticles exhibited good T1 contrast effect. In in vivo T1 weighted blood pool magnetic resonance imaging (MRI), iron oxide nanoparticles showed longer circulation time than commercial gadolinium complex, enabling high resolution imaging. We used 80 nm-sized ferrimagnetic iron oxide nanocrystals for T2 MRI contrast agent for tracking transplanted pancreatic islet cells and single-cell MR imaging. We reported on the fabrication of monodisperse magnetite nanoparticles immobilized with uniform pore-sized mesoporous silica spheres for simultaneous MRI, fluorescence imaging, and drug delivery. We synthesized hollow magnetite nanocapsules and used them for both the MRI contrast agent and magnetic guided drug delivery vehicle.

• Korean Journal of Materials Research
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• v.22 no.10
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• pp.526-530
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• 2012

Silica-based ceramic-matrix composites have shown promise as advanced materials for many applications such as chemical catalysts, ceramics, pharmaceuticals, and electronics. $SiO_2$-CuO-$CeO_2$ multi-component powders and their thin film, using an oxalic acid template as a chelating agent, have larger surface areas and more uniform pore size distribution than those of inorganic acid catalysts. $SiO_2$-CuO-$CeO_2$ composite powders were synthesized using tetraethylorthosilicate, copper (II) nitrate hemi (pentahydrate), and cerium (III) nitrate hexahydrate with oxalic acid as template or pore-forming agent. The process of thermal evolution, the phase composition, and the surface morphology of these powders were monitored by thermogravimetry-differential thermal analysis (TG-DTA), X-ray diffractometry (XRD), field-emission scanning electron microscopy (FE-SEM), and energy dispersive X-ray spectrometry (EDXS). The mesoporous property of the powders was observed by Brunner-Emmett-Teller surface (BET) analysis. The improved surface area of this powder template with oxalic acid was $371.4m^2/g$. This multi-component thin film on stainless-steel was prepared by sol-gel dip coating with no cracks.

• Proceedings of the Korean Vacuum Society Conference
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• 2011.08a
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• pp.217-217
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• 2011

Recently, demand for thermally stable metal nanoparticles suitable for chemical reactions at high temperatures has increased to the point to require a solution to nanoparticle coalescence. Thermal stability of metal nanoparticles can be achieved by adopting core-shell models and encapsulating supported metal nanoparticles with mesoporous oxides [1,2]. However, to understand the role of metal-support interactions on catalytic activity and for surface analysis of complex structures, we developed a novel catalyst design by coating an ultra-thin layer of titania on Pt supported silica ($SiO_2/Pt@TiO_2$). This structure provides higher metal dispersion (~52% Pt/silica), high thermal stability (~600$^{\circ}C$) and maximization of the interaction between Pt and titania. The high thermal stability of $SiO_2/Pt@TiO_2$ enabled the investigation of CO oxidation studies at high temperatures, including ignition behavior, which is otherwise not possible on bare Pt nanoparticles due to sintering [3]. It was found that this hybrid catalyst exhibited a lower activation energy for CO oxidation because of the metal-support interaction. The concept of an ultra-thin active metal oxide coating on supported nanoparticles opens-up new avenues for synthesis of various hybrid nanocatalysts with combinations of different metals and oxides to investigate important model reactions at high-temperatures and in industrial reactions.

• Korean Journal of Materials Research
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• v.22 no.7
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• pp.362-367
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• 2012

Magnetite nanoparticles(NPs) have been the subject of much interest by researchers owing to their potential use as magnetic carriers in drug targeting and as a tumor treatment in cases of hyperthermia. However, magnetite nanoparticles with 10 nm in diameter easily aggregate and thus create large secondary particles. To disperse magnetite nanoparticles, this study proposes the infiltration of magnetite nanoparticles into hybrid silica aerogels. The feasible dispersion of magnetite is necessary to target tumor cells and to treat hyperthermia. Magnetite NPs have been synthesized by coprecipitation, hydrothermal and thermal decomposition methods. In particular, monodisperse magnetite NPs are known to be produced by the thermal decomposition of iron oleate. In this study, we thermally decomposed iron acetylacetonate in the presence of oleic acid, oleylamine and 1,2 hexadecanediol. We also attempted to disperse magnetite NPs within a mesoporous aerogels. Methyltriethoxysilicate(MTEOS)-based hybrid silica aerogels were synthesized by a supercritical drying method. To incorporate the magnetite nanoparticles into the hybrid aerogels, we devised two methods: adding the synthesized aerogel into a magnetite precursor solution followed by nucleation and crystal growth within the pores of the aerogels, and the infiltration of magnetite nanoparticles synthesized beforehand into aerogel matrices by immersing the aerogels in a magnetite nanoparticle colloid solution. An analysis using a vibrating sample magnetometer showed that approximately 20% of the magnetite nanoparticles were well dispersed in the aerogels. The composite samples showed that heating under an inductive magnetic field to a temperature of $45^{\circ}C$ is possible.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.30 no.2
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• pp.181-187
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• 2004

Preparations of mesoporous materials using various templates and their applicability have been intensively investigated for many years. We studied on synthesizing mesoporous Ti02 with pores in which sensitive compounds having weak physico-chemical properties such as thermal or UV irradiation and low solubility in solvent are trapped. Prior to trapping OMC in the pores of mesoporous titania, OMC was nano-emulsified in O/W system using Lecithin. Thereafter the OMC was trapped in the pores of mesoporous titania using sol-gel method. Main focus of this work is to prepare OMC-trapped mesoporous titania and to trace the stability and solubility of nano-emulsified OMC in the pores of mesoporous titania, and compared with that of mesoporous silica. OMC-trapped mesoporous Inorganic-Organic hybrid titania showed higher factors in sun protecting and a skin penetration phenomenon was reduced.

• Korean Chemical Engineering Research
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• v.53 no.3
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• pp.357-363
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• 2015

The development of the environment-friendly tire that meets the standard requirements according to tire labeling system can be improved through using highly homogeneous silica immobilized zinc oxide nanoparticles. In this study, a considerable amount of nanoporous silica was essentially added into nano zinc oxide to improve the physiochemical properties of the formed composite. The introduction of nanoporous silica materials in the composite facilitates the improvement of the wear-resistance and increases the elasticity of the tread. Therefore, the introduction of nanoporous silica can replace carbon black as filler in the formation of composites with desirable properties for conventional green tire. Herein, mesoporous silica immobilized zinc oxide nanoparticle with desirable properties for rubber compounds was investigated. Composites with homogeneous dispersion were obtained in the absence of dispersants. The dispersion stability was controlled through varying the molar ratio, ageing time and mixing order of the reactants. A superior dispersion was achieved in the sample obtained using 0.03 mol of zinc precursor as it had the smallest grain size (50.5 nm) and then immobilized in silica aged for 10 days. Moreover, the specific surface area of this sample was the highest ($649m^2/g$).

• Applied Chemistry for Engineering
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• v.34 no.2
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• pp.199-205
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• 2023

Arsenic is a highly toxic element, and its contamination is widespread around the world. The natural materials with high selectivity and efficiency toward pollutants are important in wastewater treatment technology. In this study, the mesoporous synthetic hectorite was synthesized by facile hydrothermal crystallization of gels comprising silica, magnesium hydroxide, and lithium fluoride. Additionally, the naturally available clay was modified using zirconium at room temperature. Both synthetic and modified natural clays were employed in the removal of arsenate from aquatic environments. The materials were fully characterized by scanning electron microscope (SEM), X-ray diffraction (XRD), and Fourier transform-infrared (FT-IR) analyses. The synthesized materials were used to remove arsenic (V) under varied physicochemical conditions. Both materials, i.e., Zr-bentonite and Zr-hectorite, showed high percentage removal of arsenic (V) at lower pH, and the efficiency decreased in an alkaline medium. The equilibrium-state sorption data agrees well with the Langmuir and Freundlich adsorption isotherms, and the maximum sorption capacity is found to be 4.608 and 2.207 mg/g for Zr-bentonite and Zr-hectorite, respectively. The kinetic data fits well with the pseudo-second order kinetic model. Furthermore, the effect of the background electrolytes study indicated that arsenic (V) is specifically sorbed at the surface of these two nanocomposites. This study demonstrated that zirconium intercalated synthetic hectorite as well as zirconium modified natural clays are effective and efficient materials for the selective removal of arsenic (V) from aqueous medium.