• Title/Summary/Keyword: Liquid Phase Precursor Method

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Hierarchically porous carbon aerogels with high specific surface area prepared from ionic liquids via salt templating method

  • Zhang, Zhen;Feng, Junzong;Jiang, Yonggang;Feng, Jian
    • Carbon letters
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    • v.28
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    • pp.47-54
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    • 2018
  • High surface carbon aerogels with hierarchical and tunable pore structure were prepared using ionic liquid as carbon precursor via a simple salt templating method. The as-prepared carbon aerogels were characterized by nitrogen sorption measurement and scanning electron microscopy. Through instant visual observation experiments, it was found that salt eutectics not only serve as solvents, porogens, and templates, but also play an important role of foaming agents in the preparation of carbon aerogels. When the pyrolyzing temperature rises from 800 to $1000^{\circ}C$, the higher temperature deepens the carbonization reaction further to form a nanoporous interconnected fractal structure and increase the contribution of super-micropores and small mesopores and improve the specific surface area and pore volume, while having few effects on the macropores. As the mass ratio of ionic liquid to salt eutectics drops from 55% to 15%, that is, the content of salt eutectics increases, the salt eutectics gradually aggregate from ion pairs, to clusters with minimal free energy, and finally to a continuous salt phase, leading to the formation of micropores, uniform mesopores, and macropores, respectively; these processes cause BET specific surface area initially to increase but subsequently to decrease. With the mass ratio of ionic liquids to salts at 35% and carbonization temperature at $900^{\circ}C$, the specific surface area of the resultant carbon aerogels reached $2309m^2g^{-1}$. By controlling the carbonization temperature and mass ratio of the raw materials, the hierarchically porous architecture of carbon aerogels can be tuned; this advantage will promote their use in the fields of electrodes and adsorption.

Influence of transient surface hydrogen on Aluminum catalyzed Silicon nanowire growth

  • Sin, Nae-Cheol
    • Proceedings of the Korean Vacuum Society Conference
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    • 2016.02a
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    • pp.125.2-125.2
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    • 2016
  • Semiconductor nanowires are essential building blocks for various nanotechnologies including energy conversion, optoelectronics, and thermoelectric devices. Bottom-up synthetic approach utilizing metal catalyst and vapor phase precursor molecules (i.e., vapor - liquid - solid (VLS) method) is widely employed to grow semiconductor nanowires. Al has received attention as growth catalyst since it is free from contamination issue of Si nanowire leading to the deterioration of electrical properties. Al-catalyzed Si nanowire growth, however, unlike Au-Si system, has relatively narrow window for stable growth, showing highly tapered sidewall structure at high temperature condition. Although surface chemistry is generally known for its role on the crystal growth, it is still unclear how surface adsorbates such as hydrogen atoms and the nanowire sidewall morphology interrelate in VLS growth. Here, we use real-time in situ infrared spectroscopy to confirm the presence of surface hydrogen atoms chemisorbed on Si nanowire sidewalls grown from Al catalyst and demonstrate they are necessary to prevent unwanted tapering of nanowire. We analyze the surface coverage of hydrogen atoms quantitatively via comparison of Si-H vibration modes measured during growth with those obtained from postgrowth measurement. Our findings suggest that the surface adsorbed hydrogen plays a critical role in preventing nanowire sidewall tapering and provide new insights for the role of surface chemistry in VLS growth.

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Fabrication and Characterization of Ag Particles by Polyol Process and Wet Chemical Process (폴리올 공정과 액상 환원 공정에 따른 은 입자 제조 및 특성 평가)

  • Yoo, Juyeon;Jang, Hyosung;Lee, Kun-Jae
    • Journal of Powder Materials
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    • v.23 no.4
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    • pp.297-302
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    • 2016
  • Ag nanoparticles are extensively studied and utilized due to their excellent catalysis, antibiosis and optical properties. They can be easily synthesized by chemical reduction methods and it is possible to prepare particles of uniform size and high purity. These methods are divided into vapor methods and liquid phase reduction methods. In the present study, Ag particles are prepared and analyzed through two chemical reduction methods using solvents containing a silver nitrate precursor. When Ag ions are reduced using a reductant in the aqueous solution, it is possible to control the Ag particle size by controlling the formic acid ratio. In addition, in the Polyol process, Ag nanoparticles prepared at various temperatures and reaction time conditions have multiple twinned and anisotropic structures, and the particle size variation can be confirmed using field emissions scanning electron microscopy and by analyzing the UV-vis spectrum.

Stability of PS Opals in Supercritical Carbon Dioxide and Synthesis of Silica Inverse Opals

  • Yu, Hye-Min;Kim, Ah-Ram;Moon, Jun-Hyuk;Lim, Jong-Sung;Choi, Kyu-Yong
    • Bulletin of the Korean Chemical Society
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    • v.32 no.7
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    • pp.2178-2182
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    • 2011
  • Recently, the synthesis of ordered macroporous materials has received much attention due to its potential use as photonic band gap materials.$^1$ In this study, we have used the three-dimensional (3D) latex array template impregnated with benzenesulfonic acid (BSA), which is capable of catalyzing the reaction using tetraethyl orthosilicate (TEOS) as a precursor and distilled water. The polystyrene (PS) templates were reacted with TEOS in $scCO_2$ at 40 $^{\circ}C$ and at 80 bar. In the reactor, TEOS was filtrated into the PS particle lattice. After the reaction, porous silica materials were obtained by calcinations of the template. The stability test of the PS template in pure $CO_2$ was conducted before the main experiment. Scanning electron microscopy (SEM) images showed that the reaction in $scCO_2$ takes place only on the particle surface. This new method using $scCO_2$ has advantages over conventional sol-gel processes in its capability to control the fluid properties such as viscosity and interfacial tension. It has been found that the reaction in $scCO_2$ occurs only on the particle surface, making the proposed technique as more rapid and sustainable method of synthesizing inverse opal materials than conventional coating processes in the liquid phase and in the vapor phase.

Microstructural Characterization of MOCVD RuOx Thin Films and Effects of Annealing Gas Ambient (MOCVD RuOx 박막의 미세구조 특성평가와 열처리 가스환경 영향)

  • Kim, Gyeong-Won;Kim, Nam-Su;Choe, Il-Sang;Kim, Ho-Jeong;Park, Ju-Cheol
    • The Transactions of the Korean Institute of Electrical Engineers C
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    • v.51 no.9
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    • pp.423-429
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    • 2002
  • RuOx thin films were fabricated by the method of liquid delivery MOCVD using Ru(C$_{8}$ $H_{13}$ $O_2$)$_3$ as the precursor and their thermal effects and conductivity were investigated. Ru films deposited at 25$0^{\circ}C$ were annealed at $650^{\circ}C$ for 1min with Ar, $N_2$ or N $H_3$ ambient. The changes of the micro-structure, the surface morphology and the electrical resistivity of the Ru films after annealing were studied. Ar gas was more effective than $N_2$ and N $H_3$ gases as an ambient gas for the post annealing of the Ru films, because of smaller resistivity and denser grains. The X-ray diffraction and X-ray photoelectron spectroscopy results indicate that the Ru $O_2$ phase and the silicidation are not observed regardless of the ambient gases. The minimum resistivity of the Ru film is found to have the value of 26.35 $\mu$Ω-cm in Ar ambient. Voids were formed at Ru/TiN interface of the Ru layer after annea1ing in $N_2$ ambient. The $N_2$ gas generated due to the oxidation of the TiN layer accumulated at the Ru/TiN interface, forming bubbles; consequently, the stacked film may peel off the Ru/TiN interface.e.

Sensitive determination of paroxetine in canine plasma by liquid chromatography-tandem mass spectrometry (LC-MS/MS) (LC-MS/MS를 이용한 비글견 혈장 중 파록세틴의 고감도 분석)

  • Chang, Kyu Young;Kang, Seung Woo;Han, Sang Beom;Youm, Jeong-Rok;Lee, Kyung Ryul;Lee, Hee Joo
    • Analytical Science and Technology
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    • v.20 no.2
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    • pp.138-146
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    • 2007
  • A simple and sensitive method for the determination of paroxetine in canine plasma was developed and validated by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry (LC-/MS/MS). Fluoxetine was used as an internal standard. Paroxetine and internal standard in plasma samples were extracted using TBME (tert-butyl methyl ether). A centrifuged upper layer was then evaporated and reconstituted with mobile phase of 50% acetonitrile adjusted to pH 3 by formic acid. The reconstituted samples were injected into a Capcell Pak UG120 ($2.0{\times}150mm$, $5{\mu}m$) column. Using MS/MS with SRM (selective reaction monitoring) mode, the transitions (precursor to product) monitored were m/z $330{\rightarrow}192$ for paroxetine, and m/z $310{\rightarrow}148$ for internal standard. Linear detection responses were obtained for paroxetine concentration range of 0.02~5 ng/mL. A correlation coefficient of linear regression ($R^2$) was 0.9993. Detection of paroxetine in canine plasma was accurate and precise, with limit of quantification at 0.02 ng/mL. The method has been successfully applied to pharmacokinetic study of paroxetine in healthy beagle dogs.

A Study on the Change of Condensable Particulate Matter by the SO2 Concentration among Combustion Gases (연소 배출가스 중 SO2 농도에 따른 응축성먼지 변화에 관한 연구)

  • Yu, JeongHun;Lim, SeulGi;Song, Jihan;Lee, DoYoung;Yu, MyeongSang;Kim, JongHo
    • Journal of Korean Society for Atmospheric Environment
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    • v.34 no.5
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    • pp.651-658
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    • 2018
  • Particulate matter (PM) emitted from fossil fuel-combustion facilities can be classified as either filterable or condensable PM. The U.S. Environmental Protection Agency (EPA) defined condensable PM as material that is in the phase of vapor at the stack temperature of the sampling location which condenses, reacts upon cooling and dilution in the ambient air to form solid or liquid in a few second after the discharge from the stack. Condensable PM passed through the filter media and it is typically ignored. But condensable PM was defined as a component of primary PM. This study investigates the change of condensable PM according to the variation in the sulfur dioxide of combustion gas. Domestic oil boilers were used as the source of emission ($SO_2$) and the level of $SO_2$ concentration (0, 50, 80, and 120 ppm) was adjusted by diluting general light oil and marine gas oil (MGO) that contains sulfur less than 0.5%. Condensable PM was measured as 2.72, 6.10, 8.38, and $13.34mg/m^3$ when $SO_2$ concentration in combustion gas were 0, 50, 80, and 120 ppm respectively. The condensable PM tended to increase as the concentration of $SO_2$ increased. Some of the gaseous air pollutants emitted from the stack should be considered precursors of condensable PM. The gas phase pollutants which converted into condensable PM should reduced for condensable PM control.

Microstructure Analysis of Cu/Bi2212 High Temperature Superconducting Tapes with Meat-Treatment Atmosphere (열처리 분위기에 따른 동/Bi2212 고온초전도 테입의 미세구조)

  • Han, Sang-Chul;Sung, Tae-Hyun;Han, Young-Hee;Lee, Jun-Seong;Lee, Won-Tak;Kim, Sang-Jun
    • 한국초전도학회:학술대회논문집
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    • v.9
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    • pp.388-391
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    • 1999
  • Well oriented Bi2212 superconductor thick films were formed successfully on a copper substrate by liquid reaction between a Cu-free precursor and Cu tape method in which Cu-free BSCO powder mixture was' printed on copper plate and heat-treated. And we examined the effect of heat-treatment atmosphere for the superconducting properties and microstructure of Bi2212. The composition of Cu-free BSCO powder mixture was Bi$_2O_3$ : SrCO$_3$ : CaCO$_3$ = 1.2~2 : 1 : 1 and the heat-treatment for the superconducting formation reaction was performed in air, oxygen, nitrogen and low oxygen pressure. At heat-treatment temperature, the printing layer partially melt by reacting with CuO of the oxidizing copper plate, and the nonsuperconducting phases present in the melt are typically Bi-free phases and Cu-free phases. Among the nonsuperconducting phases, it is known that the (Sr,Ca)CuO$_3$ phase restrain the formation of the Bi2212 superconducting phase. Because a kind of the nonsuperconducting phases is controled by the oxygen partial pressure, the optimum condition in which the remnants of the second phases don't leave in the fully processed conductor was determined by XRD and the critical tempera to re (Tc) analysis.

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Synthesis of Single-Crystalline InSb Nanowires Using CVD Method and Study of Growth Mechanism in Open and Close System (CVD 방법을 이용한 단결정 InSb 나노와이어의 성장과 Open/Close 시스템에서의 반응 메커니즘 연구)

  • Kang, Eun Ji;Park, Yi-Seul;Lee, Jin Seok
    • Journal of the Korean Vacuum Society
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    • v.22 no.6
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    • pp.306-312
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    • 2013
  • Single-crystalline InSb nanowire was synthesized on $SiO_2$ wafer via vapor-liquid-solid (VLS) mechanism using chemical vapor deposition method. According to the source container system (open or close) which contain InSb powder and $SiO_2$ wafer, the single-crystalline InSb nanowires have different growth mechanisms. Structural characterization of the InSb nanowires was examined by scanning electron microscope (SEM). Composition of the nanowires was investigated using x-ray diffraction (XRD) and energy dispersive x-ray spectroscopy (EDS). This study demonstrates that length and diameter of the InSb nanowires are long and thick using open-boat system by VLS and additional vapor-solid (VS) mechanisms, because open-boat system can carry a large amount of vapor-phase InSb precursor than close-boat system.

A Novel Approach for Controlling Process Uniformity with a Large Area VHF Source for Solar Applications

  • Tanaka, T.
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.08a
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    • pp.146-147
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    • 2011
  • Processing a large area substrate for liquid crystal display (LCD) or solar panel applications in a capacitively coupled plasma (CCP) reactor is becoming increasingly challenging because of the size of the substrate size is no longer negligible compared to the wavelength of the applied radio frequency (RF) power. The situation is even worse when the driving frequency is increased to the Very High Frequency (VHF) range. When the substrate size is still smaller than 1/8 of the wavelength, one can obtain reasonably uniform process results by utilizing with methods such as tailoring the precursor gas distribution by adjustingthrough shower head hole distribution or hole size modification, locally adjusting the distance between the substrate and the electrode, and shaping shower head holes to modulate the hollow cathode effect modifying theand plasma density distribution by shaping shower head holes to adjust the follow cathode effect. At higher frequencies, such as 40 MHz for Gen 8.5 (2.2 m${\times}$2.6 m substrate), these methods are not effective, because the substrate is large enough that first node of the standing wave appears within the substrate. In such a case, the plasma discharge cannot be sustained at the node and results in an extremely non-uniform process. At Applied Materials, we have studied several methods of modifying the standing wave pattern to adjusting improve process non-uniformity for a Gen 8.5 size CCP reactor operating in the VHF range. First, we used magnetic materials (ferrite) to modify wave propagation. We placed ferrite blocks along two opposing edges of the powered electrode. This changes the boundary condition for electro-magnetic waves, and as a result, the standing wave pattern is significantly stretched towards the ferrite lined edges. In conjunction with a phase modulation technique, we have seen improvement in process uniformity. Another method involves feeding 40 MHz from four feed points near the four corners of the electrode. The phase between each feed points are dynamically adjusted to modify the resulting interference pattern, which in turn modulate the plasma distribution in time and affect the process uniformity. We achieved process uniformity of <20% with this method. A third method involves using two frequencies. In this case 40 MHz is used in a supplementary manner to improve the performance of 13 MHz process. Even at 13 MHz, the RF electric field falls off around the corners and edges on a Gen 8.5 substrate. Although, the conventional methods mentioned above improve the uniformity, they have limitations, and they cannot compensate especially as the applied power is increased, which causes the wavelength becomes shorter. 40 MHz is used to overcome such limitations. 13 MHz is applied at the center, and 40 MHz at the four corners. By modulating the interference between the signals from the four feed points, we found that 40 MHz power is preferentially channeled towards the edges and corners. We will discuss an innovative method of controlling 40 MHz to achieve this effect.

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