• Korean Chemical Engineering Research
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• v.58 no.4
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• pp.658-664
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• 2020

Zeolite HY is wet impregnated with Ni (0.1, 0.3, 0.4, 0.5 wt%), Pt (0.1 wt%) and reduced in presence of hydrogen to form nanosized particles of Ni and Pt. All the catalysts were characterized by XRD, TEM, ESCA, NH₃-TPD, Pyridine adsorbed FT-IR and BET. Characterization results confirm that the Ni and Pt fractions effectively rehabilitated the physio-chemical properties of the zeolite HY catalysts. Further, all the reduced catalyst were screened with hydroisomerization of m-xylene at LHSV = 2.0 h^-1 in the temperature range 250-400 ℃ in steps of 50 ℃ in hydrogen atmosphere (20 ml/g). The addition of Ni to Pt catalyst increases hydroisomerization conversion, as well as maximizes p-xylene selectivity by restricting the pore size. The increasing trend in activity continues up to 0.3 wt% of Ni and 0.1 wt% Pt addition over zeolite HY. The increasing addition of Ni increases the total number of active metallic sites to exposed, which increases the metallic sites/acid sites ratio towards the optimum value for these reactions by better balance of synergic effect for stable activity. The rate of deactivation is pronounced on monometallic catalysts. The results confirm the threshold Ni addition is highly suitable for hydroisomerization reaction for product selectivity over Ni-Pt bimetallic/support catalysts.

• Bulletin of the Korean Chemical Society
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• v.35 no.2
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• pp.431-435
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• 2014

Zinc peroxide nanoparticles ($ZnO_2$ NPs) were prepared by reacting zinc(II) isobutylcarbamate, as an organometallic precursor, with hydrogen peroxide ($H_2O_2$) at $60^{\circ}C$. Polyethylene glycol and polyvinylpyrrolidone were used as stabilizers, which suppressed aggregation of the $ZnO_2$ NPs. Conditions such as concentrations of $H_2O_2$ and the stabilizer were systemically controlled to determine their effect on the formation of nano-sized $ZnO_2$ NPs. The formation of stable $ZnO_2$ NPs was confirmed by UV-vis, Raman spectroscopy, X-ray photoelectron spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM), and X-ray diffraction. The TEM images revealed that polyvinylpyrrolidone-stabilized $ZnO_2$ NPs (diameter, 10-30 nm) were well dispersed in the organic solvent. Quite pure ZnO NPs were obtained from the peroxide powder by simple heat treatment of $ZnO_2$. The transition temperature of $170^{\circ}C$ was determined by differential scanning calorimetry.

• Journal of Electrochemical Science and Technology
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• v.7 no.4
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• pp.316-326
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• 2016

Development and discovery of efficient, cost-effective, and robust electrocatalysts are imperative for practical and widespread implementation of water electrolysis and fuel cell techniques in the anticipated hydrogen economy. The electrochemical reactions involved in water electrolysis, i.e., hydrogen and oxygen evolution reactions, are complex inner-sphere reactions with slow multi-electron transfer kinetics. To develop active electrocatalysts for water electrolysis, the physicochemical properties of the electrode surfaces in electrolyte solutions should be investigated and understood in detail. When electrocatalysis is conducted using nanoparticles with large surface areas and active surface states, analytical techniques with sub-nanometer resolution are required, along with material development. Scanning electrochemical microscopy (SECM) is an electrochemical technique for studying the surface reactions and properties of various types of electrodes using a very small tip electrode. Recently, the morphological and chemical characteristics of single nanoparticles and bio-enzymes for catalytic reactions were studied with nanometer resolution by combining SECM with atomic force microscopy (AFM). Herein, SECM techniques are briefly reviewed, including the AFM-SECM technique, to facilitate further development and discovery of highly active, cost-effective, and robust electrode materials for efficient electrolysis and photolysis.

• Transactions of the Korean hydrogen and new energy society
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• v.27 no.3
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• pp.270-275
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• 2016

A simple solid state incorporation method was employed in order to incorporate Pd nanocatalyst into a Nafion film for polymer electrolyte membrane fuel cell (PEMFC) via the reduction of palladium (II) bis (acetylacetonate), $Pd(acac)_2$. It was sublimed, penetrated into Nafion film and then reduced to Pd nanoparticles simultaneously in a glass reactor of N2 atmosphere at $180^{\circ}C$ for 1, 3 and 5 min. This reaction was took place without any reducing agent and any solvent. The morphology of the Pd nanoparticles was observed by transmission electron microscopy (TEM), and Pd distribution was analyzed by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). And 23% modification of tensile strength of Pd/Nafion composite film was measured by universal testing machine and I-V curve was estimated by using a unit cell with $5{\times}5cm^2$ active area.

• Applied Chemistry for Engineering
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• v.26 no.4
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• pp.515-519
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• 2015

Complexes composed of hydrogen tetrachloroaurate (III) trihydrate ($HAuCl_4{\cdot}3H_2O$) and DNA were first formed for the synthesis of gold nanoparticle using a DNA template, which were validated using UV-Vis spectroscopy. The morphology of complexes were also characterized by scanning electron microscopy (SEM). DNA-mediated gold nanoparticles were synthesized by the chemical reduction of DNA-Au(III) complexes using hydrazine ($N_2H_4$) and sodium borohydride ($NaBH_4$) as reducing agents. The effects of reducing agent types and their concentration on the formation of gold nanoparticles were investigated. The results showed that hydarazine was the most effective for the reduction of DNA-Au(III) complex. The DNA-mediated gold nanoparticles were characterized SEM, particle size analyzer (PSA), and transmission electron microscopy (TEM). Gold nanoparticles with 55~80 nm in diameter were formed by the aggregation of smaller gold nanoparticles (~nm), which was confirmed in the DNA matrix.

• Bulletin of the Korean Chemical Society
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• v.27 no.5
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• pp.672-678
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• 2006

A new approach to fabricate an enzyme electrode was described based on the immobilization of horseradish peroxidase (HRP) on dithiobis-N-succinimidyl propionate (DTSP) self-assembled monolayer (SAM) formed on gold-nanoparticles (Au-NPs) which were electrochemically deposited onto glassy carbon electrode (GCE) surface. The overall surface area and average size of Au-NPs could be controlled by varying deposition time and were examined by Field Emission-Scanning Electron Microscope (FE-SEM). The $O_2$ reduction capability of the surface demonstrated that Au-NPs were thermodynamically stable enough to stay on GCE surface. The immobilized HRP electrode based on Au-NPs/GCE presented faster, more stable and sensitive amperometric response in the reduction of hydrogen peroxide than a HRP immobilized on DTSP/gold plate electrode not containing Au-NPs. The effects of operating potential, mediator concentration, and pH of buffer electrolyte solution on the performance of the HRP biosensor were investigated. In the optimized experimental conditions, the HRP immobilized GCE incorporating smaller-sized Au-NPs showed higher electrocatalytic activity due to the high surface area to volume ratio of Au-NPs in the biosensor. The HRP electrode showed a linear response to $H_2O_2$ in the concentration range of 1.4 $\mu$M-3.1 mM. The apparent Michaelis-Menten constant ($K _M\; ^{app}$) determined for the immobilized HRP electrodes showed a trend to be decreased by decreasing size of Au-NPs electrodeposited onto GCE.

• Transactions of the Korean hydrogen and new energy society
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• v.29 no.5
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• pp.450-457
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• 2018

To design the practical core-shell electrocatalysts, combination of core and shell materials is important to meet catalytic activity and durability target. In general, Pd is considered as a good core material due to its best activity caused by strain/ligand effect. Preparing Pd nanoparticles can be a starting point in fabricating core-shell type electrocatalysts, much simplified Pd preparing process is suggested by using carbon monoxide (CO) as a reducing agent and/or capping agent. The solvent composition and reaction temperature can control to nanosheet, tetrahedron, and sphere without using additional stabilizer. Among them, Pd nanosheet which has mainly (111) plane showed about 3 times higher electrocatalytic activity for oxygen reduction reaction (ORR) to the spherical Pd nanoparticles. The enhanced ORR activity of Pd nanosheets can be attributed to the exposure of Pd (111) surface and the high electrochemical surface area. Therefore, we demonstrated that the shape of Pd nanomaterials is easily controlled via a facile reduction method using CO, and (111) plane-oriented Pd nanosheets can be a promising ORR catalysts and core material for polymer electrolyte fuel cells (PEFCs).

• Nuclear Engineering and Technology
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• v.47 no.6
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• pp.738-745
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• 2015

The catalytic exchange of hydrogen isotopes between hydrogen and water has been known to be a very useful process for the separation of tritium from tritiated water. For the process, a highly active hydrophobic catalyst is needed. This study provides an effective fabrication method of size-controlled platinum/poly[styrene-divinylbenzene-tri(propylene glycol) diacrylate] [Pt/poly(SDB-TPGDA)] hydrophobic catalyst beads with a narrow size distribution. Platinum nanoparticles were prepared by ${\gamma}$-ray-induced reduction in the aqueous phase first, and then uniformly dispersed in SDB-TPGDA comonomer after the hydrophobization of platinum nanoparticles with alkylamine stabilizers. The porous Pt/poly(SDB-TPGDA) hydrophobic catalyst beads were synthesized by the UV-initiated polymerization of the mixture droplets prepared in a capillary-based microfluidic system. The size of as-prepared catalyst beads can be controlled in the range of $200-1,000{\mu}m$ by adjusting the flow rate of dispersed and continuous phases, as well as the viscosity of the continuous phase. Sorbitan monooleate and cyclohexanol were used as coporogens to control the porosities of the catalyst beads.

• Bulletin of the Korean Chemical Society
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• v.35 no.5
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• pp.1312-1316
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• 2014

Metal-carbon nanoreactors (MCNRs) were prepared from a pristine carbon cage (CC) using a simple and efficient template method with nano silica ball (NSB), pyrolysis fuel oil (PFO) and transition metals, such as palladium and gold. Metal nanoparticles were embedded in approximately 25 and 170 nm sized, highly ordered carbon cages. The newly developed Pd, Au and Au-Pd doped carbon nanoreactors were characterized by microanalysis, $N_2$ adsorption-desorption isotherm, powder X-ray diffraction (XRD), thermo-gravimetric analysis (TGA), scanning electron microscopy coupled with energy dispersive spectroscopy (SEM-EDS), transmission electron microscopy and inductively coupled plasma (ICP) analysis. The ordered MCNRs have exhibited dynamic hydrogen adsorption capability compared to the carbon cage.

• Transactions of the Korean hydrogen and new energy society
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• v.27 no.3
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• pp.264-269
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• 2016

A simple dry chemical approach was developed in order to load palladium (Pd) as a promoter on Pt/gas diffusion electrode (GDE) for polymer electrolyte membrane fuel cell (PEMFC). Palladium(II) bis (acetylacetonate), $Pd(acac)_2$ was sublimed, penetrated into Pt/GDE and then reduced to Pd nanoparticles simultaneously without any reducing agent and any solvent in a glass reactor of $N_2$ atmosphere at $180^{\circ}C$ for 3, 5 and 15 min. Pd distribution was analyzed by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS), and I-V curve was estimated by using a unit cell with $5{\times}5cm^2$ active area.