• Korean Chemical Engineering Research
• /
• v.45 no.6
• /
• pp.611-618
• /
• 2007

We demonstrate the sol-gel coating technique of colloidal clusters for producing hollow micro-particles with complex morphologies. Cross-linked amidine polystyrene (PS) microspheres were synthesized by emulsifier-free emulsion copolymerization of styrene and divinylbenzene. The amidine PS particles were self-organized inside toluene-in-water emulsion droplets to produce large quantities of colloidally stable clusters. These clusters were coated with thin silica shell by sol-gel reaction of tetraethylorthosilicate (TEOS) and ammonia, and the organic polystyrene cores were removed by calcination at high temperature to generate nonspherical hollow micro-particles with complex morphologies. This process can be used to prepare hollow particles with shapes such as doublets, tetrahedra, icosahedra, and others.

• Journal of Electrochemical Science and Technology
• /
• v.12 no.1
• /
• pp.137-145
• /
• 2021

Among the non-precious metal catalysts, iron-nitrogen doped carbon (Fe-N/C) catalysts have been recognized as the most promising candidates for an alternative to Pt-based catalysts for the oxygen reduction reaction (ORR) under alkaline and acidic conditions. In this study, the nano replication method using mesoporous silica, which features tunable primary particle sizes and shape, is employed to prepare the mesoporous Fe-N/C catalysts with different shapes. Platelet SBA-15, irregular KIT-6, and spherical silica particle (SSP) were selected as a template to generate three different kinds of shapes of the mesoporous Fe-N/C catalyst. Physicochemical properties of mesoporous Fe-N/C catalysts are characterized by using small-angle X-ray diffraction, nitrogen adsorption-desorption isotherms, and scanning electron microscopy images. According to the electrochemical evaluation, there is no morphological preference of mesoporous Fe-N/C catalysts toward the ORR activity with half-cell configuration under alkaline electrolyte. By implementing X-ray photoelectron spectroscopy analysis of Fe and N atoms in the mesoporous Fe-N/C catalysts, it is possible to verify that the activity towards ORR highly depends on the portions of "Fe-N" species in the catalysts regardless of the shape of catalysts. It was suggested that active site distribution in the Fe-N/C is one important factor towards ORR activity.

• Journal of Electrochemical Science and Technology
• /
• v.12 no.4
• /
• pp.458-464
• /
• 2021

Lithium ion batteries (LIBs) is a kind of rechargeable secondary battery, developed from lithium battery, lithium ions move between the positive and negative electrodes to realize the charging and discharging of external circuits. Zeolitic imidazolate frameworks (ZIFs) are porous crystalline materials in which organic imidazole esters are cross-linked to transition metals to form a framework structure. In this article, ZIF-67 is used as a sacrificial template to prepare nano porous carbon (NPC) coated cobalt nanoparticles. The final product Co/NPC composites with complete structure, regular morphology and uniform size were obtained by this method. The conductive network of cobalt and nitrogen doped carbon can shorten the lithium ion transport path and present high conductivity. In addition, amorphous carbon has more pores that can be fully in contact with the electrolyte during charging and discharging. At the same time, it also reduces the volume expansion during the cycle and slows down the rate of capacity attenuation caused by structure collapse. Co/NPC composites first discharge specific capacity up to 3115 mA h/g, under the current density of 200 mA/g, circular 200 reversible capacity as high as 751.1 mA h/g, and the excellent rate and resistance performance. The experimental results show that the Co/NPC composite material improves the electrical conductivity and electrochemical properties of the electrode. The cobalt based ZIF-67 as the precursor has opened the way for the design of highly performance electrodes for energy storage and electrochemical catalysis.

• Advances in nano research
• /
• v.14 no.6
• /
• pp.507-519
• /
• 2023

Postsurgical infections are caused by implant-related pathogenic microorganisms that lead to graft rejection. Hence, an intrinsically antibacterial material is required to produce a biocompatible biomaterial with osteogenic properties that could address this major issue. Hence, this current research aims to make strontium-doped hydroxyapatite nanorods (SrHANRs) via an ethylene diamine tetraacetic acid (EDTA)-enable microwave mediated method using Anodontia alba seashells for biomedical applications. This investigation also perceives that EDTA acts as a soft template to accomplish Sr-doping and mesoporous structures in pure hydroxyapatite nanorods (HANRs). The X-ray diffraction (XRD) and transmission electron microscopy (TEM) analysis reveals the crystalline and mesoporous structures, and Brunauer-Emmett-Teller (BET) indicates the surface area of all the samples, including pure HANRs and doped HANRs. In addition, the biocidal ability was tested using various implant-related infectious bacteria pathogens, and it was discovered that Sr-doped HANRs have excellent biocidal properties. Furthermore, toxicity evaluation using zebrafish reports the non-toxic nature of the produced HANRs. Incorporating Sr²⁺ ions into the HAp lattice would enhance biocompatibility, biocidal activity, and osteoconductive properties. As a result, the biocompatible HANRs materials synthesized with Sr-dopants may be effective in bone regeneration and antibacterial in-built implant applications.

• Proceedings of the Korean Vacuum Society Conference
• /
• 2012.08a
• /
• pp.222-222
• /
• 2012

Metal oxide gas sensors based on semiconductor type have attracted a great deal of attention due to their low cost, flexible production and simple usability. However, most works have been focused on n-type oxides, while the characteristics of p-type oxide gas sensors have been barely studied. An investigation on p-type oxides is very important in that the use of them makes possible the novel sensors such as p-n diode and tandem devices. Monoclinic cupric oxide (CuO) is p-type semiconductor with narrow band gap (~1.2 eV). This is composed of abundant, nontoxic elements on earth, and thus low-cost, environment-friendly devices can be realized. However, gas sensing properties of neat CuO were rarely explored and the mechanism still remains unclear. In this work, the neat CuO layers with highly ordered mesoporous structures were prepared by a template-free, one-pot solution-based method using novel ink solutions, formulated with copper formate tetrahydrate, hexylamine and ethyl cellulose. The shear viscosity of the formulated solutions was 5.79 Pa s at a shear rate of 1 s-1. The solutions were coated on SiO2/Si substrates by spin-coating (ink) and calcined for 1 h at the temperature of $200{\sim}600^{\circ}C$ in air. The surface and cross-sectional morphologies of the formed CuO layers were observed by a focused ion beam scanning electron microscopy (FIB-SEM) and porosity was determined by image analysis using simple computer-programming. XRD analysis showed phase evolutions of the layers, depending on the calcination temperature, and thermal decompositions of the neat precursor and the formulated ink were investigated by TGA and DSC. As a result, the formation of the porous structures was attributed to the vaporization of ethyl cellulose contained in the solutions. Mesoporous CuO, formed with the ink solution, consisted of grains and pores with nano-meter size. All of them were strongly dependent on calcination temperature. Sensing properties toward H2 and C2H5OH gases were examined as a function of operating temperature. High and fast responses toward H2 and C2H5OH gases were discussed in terms of crystallinity, nonstoichiometry and morphological factors such as porosity, grain size and surface-to-volume ratio. To our knowledge, the responses toward H2 and C2H5OH gases of these CuO gas sensors are comparable to previously reported values.

• Journal of the Korean institute of surface engineering
• /
• v.38 no.2
• /
• pp.65-68
• /
• 2005

The effect of crystal orientation and microstructure on the mechanical properties of $TaN_x$ was investigated. $TaN_x$ films were grown on $SiO_2$ substrates by ultrahigh vacuum unbalanced magnetron sputter deposition in mixed $Ar/N_2$ discharges at 20 mTorr (2.67 Pa) and at $350^{\circ}C$. Unlike the Ti-N system, in which TiN is the terminal phase, a large number of N-rich phases in the Ta-N system could lead to layers which had nano-sized lamella structure of coherent cubic and hexagonal phases, with a correct choice of nitrogen fraction in the sputtering mixture and ion irradiation energy during growth. The preferred orientations and the micro-structure of $TaN_x$ layers were controlled by varing incident ion energy $E_i\;(=30eV\~50eV)$ and nitrogen fractions $f_{N2}\;(=0.1\~0.15)$. $TaN_x$ layers were grown on (0002)-Ti underlayer as a crystallographic template in order to relieve the stress on the films. The structure of the $TaN_x$ film transformed from Bl-NaCl $\delta-TaN_x$ to lamellar structured Bl-NaCl $\delta-TaN_x$ + hexagonal $\varepsilon-TaN_x$ or Bl-NaCl $\delta-TaN_x$ + hexagonal $\gamma-TaN_x$ with increasing the ion energy at the same nitrogen fraction $f_{N2}$. The hardness of the films also increased by the structural change. At the nitrogen fraction of $0.1\~0.125$, the structure of the $TaN_x$ films was changed from $\delta-TaN_x\;+\;\varepsilon-TaN_x\;to\;\delta-TaN_x\;+\;\gamma-TaN_x$ with increasing the ion energy. However, at the nitrogen fraction of 0.15 the film structure did not change from $\delta-TaN_x\;+\;\varepsilon-TaN_x$ over the whole range of the applied ion energy. The hardness increased significantly from 21.1 GPa to 45.5 GPa with increasing the ion energy.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.25 no.4
• /
• pp.127-134
• /
• 2015

Aluminum nitride (AlN) single crystals have attracted much attention for a next-generation semiconductor application because of wide bandgap (6.2 eV), high thermal conductivity ($285W/m{\cdot}K$), high electrical resistivity (${\geq}10^{14}{\Omega}{\cdot}cm$), and high mechanical strength. The bulk AlN single crystals or thin film templates have been mainly grown by PVT (sublimation) method, flux method, solution growth method, and hydride vapor phase epitaxy (HVPE) method. Since AlN suffers difficulty in commercialization due to the defects that occur during single crystal growth, crystalline quality improvement via defects analyses is necessary. Etch pit density (EPD) analysis showed that the growth misorientations and the defects in the AlN surface exist. Transmission electron microscopy (TEM) and electron back-scattered diffraction (EBSD) analyses were employed to investigate the overall crystalline quality and various kinds of defects. TEM studies show that the morphology of the AlN is clearly influenced by stacking fault, dislocation, second phase, etc. In addition EBSD analysis also showed that the zinc blende polymorph of AlN exists as a growth defects resulting in dislocation initiator.