• Title/Summary/Keyword: Gas Phase Synthesis

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Direct Synthesis of Dimethyl Ether from Syngas in a Slurry Phase and Gas Phase Reactor (액상 및 가상 반응기 내에서 디메틸에테르의 직접 합성에 관한 연구)

  • 최정운;이상호;심규성;김종원;김성현
    • Journal of Energy Engineering
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    • v.10 no.1
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    • pp.49-54
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    • 2001
  • 최근 자동차용 청정 연료로서의 이용 가능성으로 주목받는 디메틸에테르를 액상 혼합 반응기에서 직접 합성 가스로부터 합성하였다. 메탄올 함성촉매와 감마알루미나의 혼성촉매를 사용한 결과, $H_2$/CO=1일 때, 메탄올 함성 촉매와 탈수촉매의 비가 8:2인 경우, 가장 높은 메탄옥 환산 생산량을 보였다. 또한 공간속도의 변화에 따른 디메틸에테르, 메탄올, 이산화탄소, 메탄 등 각 생성물에 대한 선택도의 변화는 거의 없이 일정하였다. 메탄옥 합성 반응 촉매만을 사용한 경우, 생성물 중 각 성분의 선택도는 반응가스의 공간속도에 따라 달라졌는데, 반응가스의 공간속도가 작아지면 생성물 중 디메틸에테르의 선택도는 변화가 없었으나, 이산화탄소의 발생량이 많고 메탄올의 생성이 적어졌다. 동일한 반응 조건에서 액상 반응과 시강 반응을 비교한 결과, DME 수율이 액상의 경우가 더 높았다.

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Characterization of SiC nanowire synthesize by Thermal CVD

  • Jeong, Min-Uk;Kim, Min-Guk;Song, U-Seok;Jeong, Dae-Seong;Choe, Won-Cheol;Park, Jong-Yun
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.74-74
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    • 2010
  • One-dimensional nanosturctures such as nanowires and nanotube have been mainly proposed as important components of nano-electronic devices and are expected to play an integral part in design and construction of these devices. Silicon carbide(SiC) is one of a promising wide bandgap semiconductor that exhibits extraordinary properties, such as higher thermal conductivity, mechanical and chemical stability than silicon. Therefore, the synthesis of SiC-based nanowires(NWs) open a possibility for developing a potential application in nano-electronic devices which have to work under harsh environment. In this study, one-dimensional nanowires(NWs) of cubic phase silicon carbide($\beta$-SiC) were efficiently produced by thermal chemical vapor deposition(T-CVD) synthesis of mixtures containing Si powders and hydrocarbon in a alumina boat about $T\;=\;1400^{\circ}C$ SEM images are shown that the temperature below $1300^{\circ}C$ is not enough to synthesis the SiC NWs due to insufficient thermal energy for melting of Si Powder and decomposition of methane gas. However, the SiC NWs are produced over $1300^{\circ}C$ and the most efficient temperature for growth of SiC NWs is about $1400^{\circ}C$ with an average diameter range between 50 ~ 150 nm. Raman spectra revealed the crystal form of the synthesized SiC NWs is a cubic phase. Two distinct peaks at 795 and $970\;cm^{-1}$ over $1400^{\circ}C$ represent the TO and LO mode of the bulk $\beta$-SiC, respectively. In XRD spectra, this result was also verified with the strongest (111) peaks at $2{\theta}=35.7^{\circ}$, which is very close to (111) plane peak position of 3C-SiC over $1400 ^{\circ}C$ TEM images are represented to two typical $\beta$-SiC NWs structures. One is shown the defect-free $\beta$-SiC nanowire with a (111) interplane distance with 0.25 nm, and the other is the stacking-faulted $\beta$-SiC nanowire. Two SiC nanowires are covered with $SiO_2$ layer with a thickness of less 2 nm. Moreover, by changing the flow rate of methane gas, the 300 sccm is the optimal condition for synthesis of a large amount of $\beta$-SiC NWs.

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Preparation and Gas Permeability of ZIF-7 Membranes Prepared via Two-step Crystallization Technique

  • Li, Fang;Li, Qiming;Bao, Xinxia;Gui, Jianzhou;Yu, Xiaofei
    • Korean Chemical Engineering Research
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    • v.52 no.3
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    • pp.340-346
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    • 2014
  • Continuous and dense ZIF-7 membranes were successfully synthesized on ${\alpha}-Al_2O_3$ porous substrate via two-step crystallization technique. ZIF-7 seeding layer was first deposited on porous ${\alpha}-Al_2O_3$ substrate by in-situ low temperature crystallization, and then ZIF-7 membrane layer can be grown through the secondary high-temperature crystallization. Two synthesis solutions with different concentration were used to prepare ZIF-7 seeding layer and membrane layer on porous ${\alpha}-Al_2O_3$ substrate, respectively. As a result, a continuous and defect-free ZIF-7 membrane layer can be prepared on porous ${\alpha}-Al_2O_3$ substrate, as confirmed by scanning electron microscope. XRD characterization shows that the resulting membrane layer is composed of pure ZIF-7 phase without any impurity. A single gas permeation test of $H_2$, $O_2$, $CH_4$ or $CO_2$ was conducted based on our prepared ZIF-7 membrane. The ZIF-7 membrane exhibited excellent H2 molecular sieving properties due to its suitable pore aperture and defect-free membrane layer.

Synthesis and Characterization of (AgSbTe2)15(GeTe)85 Thermoelectric Powder by Gas Atomization Process (가스분무공정을 이용한 (AgSbTe2)15(GeTe)85 열전분말의 제조 및 특성평가)

  • Kim, Hyo-Seob;Lee, Jin-Kyu;Koo, Jar-Myung;Chun, Byong-Sun;Hong, Soon-Jik
    • Journal of Powder Materials
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    • v.18 no.5
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    • pp.449-455
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    • 2011
  • In this study, p-type $(AgSbTe_2)_{15}(GeTe)_{85}$: TAGS-85 compound powders were prepared by gas atomization process, and then their microstructures and mechanical properties were investigated. The fabricated powders were of spherical shape, had clean surface, and illustrated fine microstructure and homogeneous $AgSbTe_2$ + GeTe solid solution. Powder X-ray diffraction results revealed that the crystal structure of the TAGS-85 sample was single rhombohedral GeTe phase, which with a space group $R_{3m}$. The grain size of the powder particles increased while the micro Vickers hardness decreased with increasing annealing temperature within the range of 573 K and 723 K due to grain growth and loss of Te. In addition, the crystal structure of the powder went through a phase transformation from rhombohedral ($R_{3m}$) at low-temperature to cubic ($F_{m-3m}$) at high-temperature with increasing annealing temperature. The micro Vickers hardness of the as-atomized powder was around 165 Hv, while it decreased gradually to 130 Hv after annealing at 673K, which is still higher than most other fabrication processes.

Thermal plasma arc discharge method for high-yield production of hexagonal AlN nanoparticles: synthesis and characterization

  • Lakshmanan Kumaresan;Gurusamy Shanmugavelayutham;Subramani Surendran;Uk Sim
    • Journal of the Korean Ceramic Society
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    • v.59
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    • pp.338-349
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    • 2020
  • Large scale with high-purity hexagonal aluminum nitride nanoparticles (AlN NPs) was synthesized using DC thermal plasma arc discharge method (TPAD). Argon gas was used as the plasma forming gas, while ammonia (NH3) gas was used as the reactive gas, which was fed into the reactor at a constant flow rate of 5 LPM. In order to optimize the process for high yield, the experiments were carried out at various plasma input powers, such as 1.5, 3.0, and 4.5 kW. Following the optimization, to examine the influence of using pure nitrogen gas, an experiment was also carried out in the nitrogen ambience. The phase identification and structural determination of the synthesized NPs were carried out using XRD and Raman spectroscopic analyses. While the morphology, particle size, and elemental compositions of the synthesized NPs were observed from SEM, HRTEM, XPS, and EDX analyses. The photoluminescence response was confirmed from the PL spectrum. The PL emission peaks observed around 440 nm (2.8 eV) and 601 nm (2.07 eV), respectively, which correspond to the UV blue and red band emissions of both AlN and Al/AlN NPs. The results show that the synthesized nano-AlN NPs exhibit excellent crystallinity with a high yield of approximately 210 g/h. The current plasma technology can be regarded as a perfect potential process for developing nano-AlN powders with improved efficiency.

Observational Studies on Evolved Stars Using KVN and KaVA/EAVN

  • Cho, Se-Hyung;Yun, Youngjoo;Imai, Hiroshi
    • The Bulletin of The Korean Astronomical Society
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    • v.44 no.2
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    • pp.51.1-51.1
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    • 2019
  • At the commissioning phase of KVN from 2009 to 2013, single-dish survey and monitoring observations were performed toward about 1000 evolved stars and about 60 relatively strong SiO and H2O maser sources respectively. Based on these single-dish results and VLBI feasibility test observations at K/Q/W/D bands in 2014, KVN Key Science Project (KSP) has started from 2015 and will be completed in 2019 as KSP phase I. Here we present the overview of observational studies on evolved stars using KVN. In KSP phase I, we have focused on nine KSP sources which show a successful astrometrically registered maps of SiO and H2O masers using the source frequency phase referencing method. We aim at investigating the spatial structure and dynamical effect from 43/42/86/129 GHz SiO to 22 GHz H2O maser regions associated with a stellar pulsation and development of asymmetry in circumstellar envelopes. Using the combined network KaVA (KVN+Japanese VLBI network VERA), KaVA Large Program titled on "Expanded Study on Stellar Masers: ESTEMA Phase I" was performed from 2015 to 2016. Based on ESTEMA Phase I, EAVN Large Program titled on "EAVN Synthesis of Stellar Maser Animations: ESTEMA Phase II" was also performed from 2018. The ESTEMA II project aims to publish composite animations of circumstellar H2O and SiO masers, which taken from up to 6 long-period variable stars with a variety of the pulsation periods (333-1000 days). The animations will exhibit the three-dimensional kinematics of the maser gas clumps with complexity caused by stellar pulsation-driven shock waves and anisotropy of clump ejections from the stellar surface. Adding three EAVN telescopes (Tianma 65m, Nanshan 26m and NRO 45m telescopes) with KaVA always secures the high quality of the maser image frames through the monitoring program.

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Characterization of the High Energy Milled Boron Precursor Powders in the Synthesis of $MgB_2$ Superconductor ($MgB_2$ 초전도체의 합성에 미치는 고에너지 밀링에 의한 초기 보론 분말의 특성)

  • Lee, J.H.;Shin, S.Y.;Kim, C.J.;Park, H.W.
    • Progress in Superconductivity
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    • v.9 no.1
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    • pp.74-79
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    • 2007
  • We characterized the highly refined boron precursor powders which were attrition milled for different milling times. $MgB_2$ powder precursor was formed from elemental crystalline Mg and amorphous B powder. The microstructure was investigated by SEM. SEM results indicate that the size of the milled powders was reduced with increasing milling time, which were varied from 0 to 8 hours. We also studied thermal behavior of the starting precursor by DSC as a function of milling time. The thermal behavior of the powder precursors was influenced by milling time. In order to determine the thermal events at DSC peaks, we annealed the milled powder mixture at $600^{\circ}C$ and $650^{\circ}C$ under protective gas and then analyzed the formation of $MgB_2$ by the XRD. We observed that superconducting $MgB_2$ phase was formed at lower temperature by the longer high energy milling. These results show that the high energy milling of the boron precursor powder can improve the reactivity for the formation of $MgB_2$.

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Electrochemical studies of nano-scale solid electrolyte powder prepared by chemical synthesis process (화학적합성법에 의한 나노 고체 전해질 분말 합성 및 전기화학적 평가)

  • Kim, Young-Mi;Shin, Yu-Cheol;Kim, Ho-Sung
    • 한국신재생에너지학회:학술대회논문집
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    • 2009.06a
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    • pp.295-298
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    • 2009
  • Oxygen ionic conductors of CeScSZ electrolyte in SOFC unit cell are applied to anode and cathode as well as electrolyte to have the triple-phase-boundaries of electrochemical reaction, and it is required to decrease the sintering temperature of anode-supported electrolyte by the nanoscale of CeScSZ electrolyte powder. In this report, nanoscale CeScSZ electrolyte powder was synthesized by chemical synthesis method. The particle size, surface area and morphology of the powder were observed by SEM and BET. Thin film electrolyte of under $10{\mu}m$ was fabricated by tape casting using the synthesized CeScSZ electrolyte powder, and ionic conductivity and gas permeability of electrolyte film were evaluated. Finally the SOFC unit cell was fabricated using the anode-supported electrolyte prepared by a tape casting method and co-sintering, in which the active layer, measuring $20{\mu}m$, was introduced in the anode layer to provide a more efficient reaction. Electrochemical evaluations of the SOFC unit cell, including measurements such as power density and impedance, were performed and analyzed.

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Synthesis and E-Beam-Mediated Gas Phase Fragmentation of Thiol-Containing Furoxans for Nanopatterned Alkyne Formation on Gold Surface

  • Koo, Hyun-Seo;Park, Kyung-Moon;Hwang, Kwang-Jin
    • Bulletin of the Korean Chemical Society
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    • v.31 no.12
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    • pp.3583-3587
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    • 2010
  • Furoxanthiols PFT and BPFT possessing thiomethyl or thiobenzyl groups in the furoxan ring were designed and synthesized as potential light-sensitive alkyne precursors on a gold surface. The synthesis of thiofuroxans PFT and BPFT was performed from the corresponding halofuroxans 1b and 2c, respectively, by the substitution with potassium thioacetate in ethyl acetate/ethanol or DMF, followed by basic hydrolysis as the key reactions. Electron-beammediated fragmentation of furoxans 1c and 2d in a mass spectrometer afforded the corresponding aryl alkyne fragments, with the evolution of NO in high preference. In the cases of thiofuroxans PFT and BPFT, carbon-sulfur bond cleavage was observed as a representative fragmentation, producing M-SH and M-SAc peaks, which competed with the release of NO. In the fragmentation of mono-aryl furoxan 1c, the release of molecule of NO was predominately observed to produce an M-NO fragment as a base peak by the formation of trimembered thiiranium or azirine intermediate.

Radiolysis Assessment of $^{18}F$-FDG According to Automatic Synthesis Module (자동합성장치에 따른 $^{18}F$-FDG의 방사선분해 평가)

  • Kim, Si-Hwal;Kim, Dong-Il;Chi, Yong-Gi;Choi, Sung-Wook;Choi, Choon-Ki;Seok, Jae-Dong
    • The Korean Journal of Nuclear Medicine Technology
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    • v.16 no.1
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    • pp.8-11
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    • 2012
  • Purpose : Among quality control items, the radiochemical impurity must be below 10% of total radioactivity. In this regard, as the recently commercialized automatic synthesis module produces a large amount of 18F-FDG, radiolysis of radiopharmaceuticals is very likely to occur. Thus, this study compared the changes in radiochemical purity regarding radiolysis of $^{18}F$-FDG according to automatic synthesis module. Materials and methods : Cyclotron (PETtrace, GE Healthcare) was used to produce $^{18}F$ and automatic synthesis module (FASTlab, Tracerlab MX, GE Healthcare) was used to achieve synthesis into FDG. For radiochemical purity, Radio-TLC Scanner (AR 2000, Bioscan), GC (Gas Chromatograph, Agilent 7890A) was used to measure the content of ethanol included in $^{18}F$-FDG. Glass board applied with silica gel ($1{\times}10cm$) was used for stationary phase while a mixed liquid formed of acetonitrile and water (ratio 19:1) was used for mobile phase. High-concentration and low-concentration $^{18}F$-FDG were produced in each synthesis module and the radiochemical purity was measured every 2 hours. Results : The purity in low-concentration (below 2.59 GBq/mL) was measured as 99.26%, 98.69%, 98.25%, 98.09% in Tracerlab MX and as 99.09%, 97.83%, 96.89%, 96.62% in FASTlab according to 0, 2, 4, 6 hours changes, respectively. The purity in high-concentration (above 3.7 GBq/mL) was measured as 99.54%, 96.08%, 93.77%, 92.54% in Tracerlab MX and as 99.53%, 95.65%, 92.39%, 89.82% in FASTlab according to 0, 2, 4, 6 hours changes, respectively. Also, ethanol was not detected in GC of $^{18}F$-FDG produced in FASTlab, while 100~300 ppm ethanol was detected in Tracerlab MX. Conclusion : Whereas the change of radiochemical purity was only 3% in low-concentration $^{18}F$-FDG, the change was rapidly increased to 10% in high-concentration. Also, higher radiolysis were observed in $^{18}F$-FDG produced in FASTlab than Tracerlab MX. This is because ethanol is included in the synthesis stage of Tracerlab MX but not in the synthesis stage of FASTlab. Thus, radiolysis is influenced by radioactivity concentration than the inclusion of ethanol, which is the radioprotector. Therefore, after producing high-concentration $^{18}F$-FDG, the content must be diluted through saline to lower concentration.

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