• Title/Summary/Keyword: controlled synthesis

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Pore-Controlled Synthesis of Mesoporous Silica Particles by Spray Pyrolysis from Aqueous Silicic Acid (규산 수용액으로부터 분무열분해법에 의한 기공 특성이 제어된 메조기공의 다공성 실리카 분말 합성)

  • Chang, Han Kwon;Lee, Jin Woo;Oh, Kyoung Joon;Jang, Hee Dong;Kil, Dae Sup;Choi, Jeong Woo
    • Particle and aerosol research
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    • v.8 no.2
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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.

Control of Both Foam and Dissolved Oxygen in the Presence of a Surfactant for Production of $\beta$-Carotene in Blakeslea trispora

  • Kim, Seon-Won;Lee, In-Young;Jeong, Jae-Cheol;Lee, Jung-Heon;Park, Young-Hoon
    • Journal of Microbiology and Biotechnology
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    • v.9 no.5
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    • pp.548-553
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    • 1999
  • A production of $\beta-Carotene$was attempted in a fed-batch culture of Blakeslea trispora by controlling both foam and dissolved oxygen in the presence of surfactant, Span 20. Results obtained from the shake flask cultures indicated that a high concentration of dissolved oxygen was needed for both cell growth and $\beta-Carotene$ synthesis, and the optimal concentration of glucose was found to be in the range of 50-100 g/l. In order to maintain the dissolved oxygen concentration level at higher than 50% of air saturation, pure oxygen was automatically sparged into the medium with air. Foam was controlled by bypassing air from the submerged aeration to the headspace in response to the foam that was caused by Span 20. High agitation speed was found to be detrimental to the cell growth due to shear damage, even though it provided sufficient dissolved oxygen. On the other hand, a low aeration speed caused stagnant regions in the fermentor because of improper mixing. Thus, for the fed-batch operation, agitation speed was increased gradually from 300 to 700 rpm to prevent cell damage at the initial stage of fermentation and to give efficient mixing for a viscous culture broth as the culture proceeded. By controlling dissolved oxygen and foam, a high concentration of $\beta-Carotene$otene (1,190 mg/l) was obtained in 6 days of the fed-batch culture of B. trispora with 2.5% of the dry cell weight, which was approximately 5 times higher than that of the batch cultures.

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Synthesis and Characterization of Large-Area and Highly Crystalline Molybdenum Disulphide Atomic Layer by Chemical Vapor Deposition

  • Park, Seung-Ho;Kim, Yooseok;Kim, Ji Sun;Lee, Su-Il;Cha, Myoung-Jun;Park, Chong-Yun
    • Proceedings of the Korean Vacuum Society Conference
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    • 2014.02a
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    • pp.356.1-356.1
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    • 2014
  • The Isolation of few-layered transition metal dichalcogenides has mainly been performed by mechanical and chemical exfoliation with very low yields. in particular, the two-dimensional layer of molybdenum disulfide (MoS2) has recently attracted much interest due to its direct-gap property and potential application in optoelectronics and energy harvesting. However, the synthetic approach to obtain high-quality and large-area MoS2 atomic thin layers is still rare. In this account, a controlled thermal reduction-sulfurization method is used to synthesize large-MoOx thin films are first deposited on Si/SiO2 substrates, which are then sulfurized (under vacuum) at high temperatures. Samples with different thicknesses have been analyzed by Raman spectroscopy and TEM, and their photoluminescence properties have been evaluated. We demonstrated the presence of mono-, bi-, and few-layered MoS2 on as-grown samples. It is well known that the electronic structure of these materials is very sensitive to the number of layer, ranging from indirect band gap semiconductor in the bulk phase to direct band gap semiconductor in monolayers. This synthetic approach is simple, scalable, and applicable to other transition metal dichalcogenides. Meanwhile, the obtained MoS2 films are transferable to arbitrary substrates, providing great opportunities to make layered composites by stacking various atomically thin layers.

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Synthesis of SiC Nanoparticles by a Sol-Gel Process (나노 실리카와 카본블랙이용 탄화열 반응으로 나노 SiC 합성 및 특성)

  • Jeong, Kwang-Jin;Bae, Dong-Sik
    • Korean Journal of Materials Research
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    • v.23 no.4
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    • pp.246-249
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    • 2013
  • Nano-sized ${\beta}$-SiC nanoparticles were synthesized combined with a sol-gel process and a carbothermal process. TEOS and carbon black were used as starting materials for the silicon source and carbon source, respectively. $SiO_2$ nanoparticles were synthesized using a sol-gel technique (Stober process) combined with hydrolysis and condensation. The size of the particles could be controlled by manipulating the relative rates of the hydrolysis and condensation reactions of tetraethyl orthosilicate (TEOS) within the micro-emulsion. The average particle size and morphology of synthesized silicon dioxide was about 100nm and spherical, respectively. The average particles size and morphology of the used carbon black powders was about 20nm and spherical, respectively. The molar ratio of silicon dioxide and carbon black was fixed to 1:3 in the preparation of each combination. $SiO_2$ and carbon black powders were mixed in ethanol and ball-milled for 12 h. After mixing, the slurries were dried at $80^{\circ}C$ in an oven. The dried powder mixtures were placed in alumina crucibles and synthesized in a tube furnace at $1400{\sim}1500^{\circ}C$ for 4 h with a heating rate of $10^{\circ}C$/min under flowing Ar gas (160 cc/min) and furnace cooling down to room temperature. SiC nanoparticles were characterized by XRD, TEM, and SAED. The XRD results showed that high purity beta silicon carbide with excellent crystallinity was synthesized. TEM revealed that the powders are spherical shape nanoparticles with diameters ranging from 15 to 30 nm with a narrow distribution.

Effect of Cosubstrate on tile Production of Poly(3-Hydroxybutyric-Co-3-Hydroxyvaleric) Acid from Glucose by Pseudomonas sp, HJ (Pseudomonas sp. HJ에 의한 포도당으로부터 Poly(3-Hydroxybutyric-Co-3-Hydroxyvaleric) Acid의 생합성에 대한 보조기질의 영향)

  • 손홍주;고명선이상준
    • KSBB Journal
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    • v.11 no.5
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    • pp.586-592
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    • 1996
  • Poly(3-hydroxybutyric-co-3-hydroxyvaleric) acid(PHB/HV) copolymer synthesis by Pseudomonas sp. HJ from glucose and cosubstrate was investigated. Taxonomic analysis suggested that Pseudomonas sp. HJ was best marched to Pseudomonas picketti having 78.8% similarity. Pseudomonas sp. HJ produced PHB/HV copolymer containing 60.8 mol% HV and 44.9 mol% HV when supplied with hexadecane and propionic acid as a cosubstrate, respectively. The HV composition in PHB/HV copolymer was controlled by varying the concentration of hexadecane and propionic acid. Propionic acid added after 24 hours of incubation was incorporated as the HV monomer in the PHB/HV copolymer up to 49.6 mol%.

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Si and Mg Coatings on the Hydroxyapatite Film Formed Ti-29Nb-xHf Alloys by Plasma Electrolyte Oxidation

  • Park, Seon-Yeong;Choe, Han-Cheol
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2017.05a
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    • pp.152-152
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    • 2017
  • Titanium and its alloys have been widely used for biomedical applications. However, the use of the Ti-6Al-4V alloy in biomaterial is then a subject of controversy because aluminum ions and vanadium oxide have potential detrimental influence on the human body due to vanadium and aluminum. Hence, recent works showed that the synthesis of new Ti-based alloys for implant application involves more biocompatible metallic alloying element,such as, Nb, Hf, Zr and Mo. In particular, Nb and Hf are one of the most effective Ti ${\beta}$-stabilizer and reducing the elastic modulus. Plasma electrolyte oxidation (PEO) is known as excellent method in the biocompatibility of biomaterial due to quickly coating time and controlled coating condition. The anodized oxide layer and diameter modulation of Ti alloys can be obtained function of improvement of cell adhesion. Silicon (Si) and magnesium (Mg) has a beneficial effect on bone. Si in particular has been found to be essential for normal bone and cartilage growth and development. In vitro studies have shown that Mg plays very important roles in essential for normal growth and metabolism of skeletal tissue in vertebrates and can be detected as minor constituents in teeth and bone. Therefore, in this study, Si and Mg coatings on the hydroxyapatite film formed Ti-29Nb-xHf alloys by plasma electrolyte oxidation has been investigated using several experimental techniques. Ti-29Nb-xHf (x= 0, 3, 7 and 15wt%, mass fraction) alloys were prepared Ti-29Nb-xHf alloys of containing Hf up from 0 wt% to 15 wt% were melted by using a vacuum furnace. Ti-29Nb-xHf alloys were homogenized for 2 hr at $1050^{\circ}C$. The electrolyte was Si and Mg ions containing calcium acetate monohydrate + calcium glycerophosphate at room temperature. The microstructure, phase and composition of Si and Mg coated oxide surface of Ti-29Nb-xHf alloys were examined by FE-SEM, EDS, and XRD.

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Effect of Heat Treatment Temperature and Atmosphere on the Microstructure of TiH2-WO3 Powder Mixtures (열처리 온도 및 분위기가 TiH2-WO3 혼합분말의 미세조직에 미치는 영향)

  • Lee, Han-Eol;Kim, Yeon Su;Oh, Sung-Tag
    • Journal of Powder Materials
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    • v.24 no.1
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    • pp.41-45
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    • 2017
  • The effects of the heat treatment temperature and of the atmosphere on the dehydrogenation and hydrogen reduction of ball-milled $TiH_2-WO_3$ powder mixtures are investigated for the synthesis of Ti-W powders with controlled microstructure. Homogeneously mixed powders with refined $TiH_2$ particles are successfully prepared by ball milling for 24h. X-ray diffraction (XRD) analyses show that the powder mixture heat-treated in Ar atmosphere is composed of Ti, $Ti_2O$, and W phases, regardless of the heat treatment temperature. However, XRD results for the powder mixture, heat-treated at $600^{\circ}C$ in a hydrogen atmosphere, show $TiH_2$ and TiH peaks as well as reaction phase peaks of Ti oxides and W, while the powder mixture heat-treated at $900^{\circ}C$ exhibits only XRD peaks attributed to Ti oxides and W. The formation behavior of the reaction phases that are dependent on the heat treatment temperature and on the atmosphere is explained by thermodynamic considerations for the dehydrogenation reaction of $TiH_2$, the hydrogen reduction of $WO_3$ and the partial oxidation of dehydrogenated Ti.

Development of Epoxy Composites with SWCNT for Highly Thermal Conductivity (고방열 재료 개발을 위한 에폭시/단일벽 탄소나노튜브 복합체 개발)

  • Kim, Hyeonil;Ko, Heung Cho;You, Nam-Ho
    • Composites Research
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    • v.33 no.1
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    • pp.7-12
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    • 2020
  • Over the past decade, liquid crystalline epoxy (LCER) has attracted much attention as a promising matrix for the development of efficient heat dissipation materials. This study presents a comprehensive study including synthesis, preparation and chacterization of polymer/inorganic composites using typical 4,4-diglycidyloxybiphenyl (DP) epoxy among LECR. To confirm the thermal conductivity of composite materials, we have prepared composite samples composed of epoxy resin and single-wall carbon nanotube (SWCNT) as a filler. In particular, DP composites exhibit higher thermal conductivity than commercial epoxy composites that use the same type of filler due to the highly ordered microstructure of the LCER. In addition, the thermal conductivity of the DP composite can be controlled by controlling the amount of filler. In particular, the DP composite containing a SWCNT content of 50 wt% has the highest thermal conductivity of 2.008 W/mK.

Synthesis of $TiO_2$ Powders by the Hydrolysis of Titanium n-Butoxide and Reaction Mechanism (Titanium n-Butoxide의 가수분해에 의한 $TiO_2$ 분말 합성과 반응 메커니즘)

  • Park, J.K.;Myung, J.J.;Chung, Y.S.;Kyong, J.B.;Kim, H.K.
    • Journal of the Korean Chemical Society
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    • v.43 no.5
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    • pp.505-510
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    • 1999
  • $TiO_2$ powders were prepared via hydrolysis of titanium n-butoxide in n-butanol and hydrolysis mechanism of titanium n-butoxide was studied using UV-Vis spectrometer. Hydrolysis reactions were controlled to proceed to pseudo-first order reaction in the presence of excess water. The phases of $TiO_2$ powders, prepared under the these conditions, were identified by XRD and reaction rates were calculated by Gugggenheim method. Prepared powders were noncrystalline states in their initial stage of formation but transformed to crystalline rutile structure by heating. Reaction mechanism of titanium n-butoxide was proposed as Interchange-Associative(Ia) mechanism, based on the data of n-value and termodynamic parameters which were determined from the rate constants.

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Invention of Ultralow - n SiO2 Thin Films

  • Dung, Mai Xuan;Lee, June-Key;Soun, Woo-Sik;Jeong, Hyun-Dam
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.08a
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    • pp.281-281
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    • 2010
  • Very low refractive index (<1.4) materials have been proved to be the key factor improving the performance of various optical components, such as reflectors, filters, photonic crystals, LEDs, and solar cell. Highly porous SiO2 are logically designed for ultralow refractive index materials because of the direct relation between porosity and index of refraction. Among them, ordered macroporous SiO2 is of potential material since their theoretically low refractive index ~1.10. However, in the conventional synthesis of ordered macroporous SiO2, the time required for the crystallization of organic nanoparticles, such as polystyrene (PS), from colloidal solution into well ordered template is typical long (several days for 1 cm substrate) due to the low interaction between particles and particle - substrate. In this study, polystyrene - polyacrylic acid (PS-AA) nanoparticles synthesized by miniemulsion polymerization method have hydrophilic polyacrylic acid tails on the surface of particles which increase the interaction between particle and with substrate giving rise to the formation of PS-AA film by simply spin - coating method. Less ordered with controlled thickness films of PS-AA on silicon wafer were successfully fabricated by changing the spinning speed or concentration of colloidal solution, as confirmed by FE-SEM. Based on these template films, a series of macroporous SiO2 films whose thicknesses varied from 300nm to ~1000nm were fabricated either by conventional sol - gel infiltration or gas phase deposition followed by thermal removal of organic template. Formations of SiO2 films consist of interconnected air balls with size ~100 nm were confirmed by FE-SEM and TEM. These highly porous SiO2 show very low refractive indices (<1.18) over a wide range of wavelength (from 200 to 1000nm) as shown by SE measurement. Refraction indices of SiO2 films at 633nm reported here are of ~1.10 which, to our best knowledge, are among the lowest values having been announced.

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