• Title/Summary/Keyword: Tube-furnace

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Separation of chlorine in a uranium compound by pyrohydrolysis and steam distillation, and its determination by ion chromatography (열가수분해 및 수증기증류에 의한 우라늄 화합물 중 염소 분리 및 이온크로마토그래피 정량)

  • Kim, Jung-Suk;Lee, Chang-Hun;Park, Soon-Dal;Han, Sun-Ho;Song, Kyu-Seok
    • Analytical Science and Technology
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    • v.23 no.1
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    • pp.45-53
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    • 2010
  • For the determination of chlorine in uranium compound, analytical methods by using a steam distillation and a pyrohydrolysis have been developed. The steam distillation apparatus was composed of steam generator, distilling flask and condenser etc. The samples were prepared with an aliquot of LiCl standard solution and a simulated spent nuclear fuel. A sample aliquot was mixed with a solution containing 0.2 M ferrous ammonium sulfate-0.5 M sulfamic acid 3 mL, phosphoric acid 6 mL and sulfuric acid 15 mL. The chloride was then distilled by steam at the temperature of $140^{\circ}C$ until a volume of $90{\pm}5\;mL$ is collected. The pyrohydrolysis equipment was composed of air introduction system, water supply, quartz reaction tube, combustion tube furnace, combustion boat and absorption vessel. The chloride was separated from powdered sample which is added with $U_3O_8$ accelerator, by pyrohydrolysis at the temperature of $950^{\circ}C$ for 1 hour in a quartz tube with a stream of air of 1 mL/min supplied from the water reservoir at $80^{\circ}C$. The chlorides collected in each absorption solution by two methods was diluted to 100 mL and measured with ion chromatography to determine the recovery yield. For the ion chromatographic determination of chlorine in molten salt retained in a metal ingot, the chlorine was separated by means of pyrohydrolysis after air and dry oxidation, and grinding for the sample.

Experimental Study of Char Oxidation and Kinetic Rate in O2/CO2 and O2/N2 Environments (O2/CO2조건과 O2/N2조건에서의 촤 연소특성 및 산화 반응성에 관한 실험적 연구)

  • Kim, Song-Gon;Lee, Cheon-Seong;Lee, Byoung-Hwa;Song, Ju-Hun;Chang, Young-June;Jeon, Chung-Hwan
    • Transactions of the Korean Society of Mechanical Engineers B
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    • v.34 no.12
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    • pp.1101-1109
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    • 2010
  • We investigated the combustion rate and kinetic rate of char when burning in oxygen-enriched atmospheres with either an $N_2$ or $CO_2$ bath gas in a drop tube furnace. The experiments were performed with sub-bituminous coal (Adaro) and bituminous coal (Coal valley) under atmospheric pressure conditions. Two different coals were investigated over 12 to 30 vol% oxygen and furnace temperatures of 900, 1100, and $1300^{\circ}C$. For both coals, the particle temperature and overall reaction rate are lower in the $CO_2$ bath gas. However, analysis of single-particle data shows that the surface-specific burning rate of char oxidation is similar in both gases. In addition, the kinetic rate and activation energy for each coal were similar for both gases. Generally, the particle temperature and overall reaction rate of sub-bituminous coal are higher than those of bituminous coal.

A Comparative Analysis of Whole Blood Cadmium by Atomic Absorption Spectrophotometry with a Graphite Furnace (흑연로 원자흡수분광법에 의한 혈액중 카드뮴 정량분석)

  • Park, Jong An;Oh, Hye Jeong;Lee, Jong Hwa
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.6 no.2
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    • pp.301-312
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    • 1996
  • This study was performed to search a optimal analyzing method of cadmium in whole-blood. Cadmium was determined by graphite furnace atomic absorption spectrometry(GFAAS). We investigated the effect of ashing temperature on the absorbance of cadmium in a simple dilution(ten-fold) method with triton X-100 and matrix modifier methods treated with $NH_4H_2PO_4$(1 and 3%) and $Pd(NO_3)_2$(0.00l and 0.005%) as matrix modifier. We also compared the reported reference values of standard blood with values resulted from optimal analyzing conditions of this study. In case of a simple dilution method, when ashing temperature was set at $450^{\circ}C$, the absorbance of sample and background were $0.334{\pm}0.012$ and $1.382{\pm}0.245$, respectively. Background level was higher than the value(0.8) that can be corrected by $D_2$ background correction method. As ashing temperature was rised to $500^{\circ}C$, the absorbance of sample and background were $0.178{\pm}0.008$ and $0.711{\pm}0.223$ respectively. The higher ashing temperature($450^{\circ}C-650^{\circ}C$) was, the lower the absorbance of sample was. In case of a matrix modifier method with $NH_4H_2PO_4$(1 and 3%), when ashing temperature was rised from $500^{\circ}C$ to $650^{\circ}C$, the absorbance of sample slightly changed. The absorbances of sample at $600^{\circ}C$ were $0.230{\pm}0.017$ and $0.137{\pm}0.012$, respectively. These values were larger than that of simple dilution method. But the absorbance of background was higher than the level that can be corrected by $D_2$ method. In case of a matrix modifier method with $Pd(NO_3)_2$(0.001 and 0.005%), the absorbance of sample and background were higher than those of other methods and were stable and reproducible. When ashing temperature was over $550^{\circ}C$, the absorbance of sample was significantly decreased. In case of 0.005% $Pd(NO_3)_2$ carbon residue remained in graphite tube affected the absorbance of sample and background. From these results, We propose that in case of a simple dilution(ten-fold) method with triton X-100 ashing temperature must be maintained below $400^{\circ}C$. In order to diminish the absorbance of background, the alternative method is attenuation of injection volume or multiplication of dilution ratio. We recommend $Pd(NO_3)_2$ than $NH_4H_2PO_4$ as a matrix modifier. In case of a matrix modifier method with $Pd(NO_3)_2$ ashing temperature might be maintained below $550^{\circ}C$.

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화학적 구조 설계를 통한 수계 Cu-In-S 잉크와 액상셀렌화 법의 개발을 통한 고효율의 CISSe 태양전지 제작

  • O, Yun-Jeong;Yang, U-Seok;Kim, Ji-Min;Mun, Ju-Ho
    • Proceedings of the Korean Vacuum Society Conference
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    • 2016.02a
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    • pp.428-428
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    • 2016
  • Copper indium sulfide (selenide) (CuIn(S,Se)2,CISSe)는 1.0~1.5 eV의 Direct band gap과 105 cm-1이 넘는 큰 광 흡수 계수를 가지고 있어 박막 태양전지의 흡수층으로써 연구되어 왔다. 최근 대량생산 및 저가 공정에 용이하다는 측면에서 용액 공정 기반 CISSe 태양전지 연구가 크게 주목 받고 있다. 용액공정 기반 중 하이드라진을 사용 한 경우 매우 높은 효율을 기록하였으나, 하이드라진 자체의 유독성과 폭발성 때문에 분위기 제어가 필요하고 여전히 저가화 및 대면적 제작에 한계가 있다. 따라서 알코올 솔젤 기반 CISSe 태양전지 제작 연구가 많이 진행되었으나, 결정립 성장 및 칼코겐 원자를 공급하기 위해 불가피하게 황화/셀렌화 후속 열처리 공정을 요구한다. 후속 열처리 공정은 폭발성의 황화수소/황화셀레늄 기체 분위기 제어와 고가의 장비를 필요로 한다. 본 연구에서는 매우 안정적이며 저가 용매인 물과 아민계 첨가제를 이용하여 Cu, In 전구체와 S, Se 이 포함된 Cu-In-S 잉크와 Se잉크를 제작하였다. 잉크 내에 S, Se을 첨가 함으로써 추가적인 후속공정 없이 비활성 가스 분위기에서 고품질의 CISSe 박막 제작을 가능케 하였다. 또한 Se 잉크 증착 횟수에 따른 결정 구조, 광학적 성질의 차이에 주목하였다. 따라서 수계 잉크를 대기 중에서 스핀코팅으로 박막을 제작한 후, Hot plate에서 건조하여 균일한 박막을 제조하고, 제작된 박막을 tube furnace에서 환원 분위기 및 비활성 가스 분위기에서 열처리 진행하여 $1.3{\mu}m$ 두께의 고품질의 CISSe 흡수층을 제작하였다. 이러한 흡수층에 대해 XRD, SEM, EDS 분석을 진행하여, 결정성, 미세구조, 및 조성을 확인하였으며, 제작된 흡수층 위에 버퍼층/투명전극층을 차례로 증착하여 CISSe 태양전지를 제작하여 셀 성능 및 양자 효율 특성을 파악하였다. 또한 액상 Raman 분석을 통해 결정립 성장 과정 메커니즘을 제시하였다.

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Heavy Metal Adsorption Characteristics and Produced of Food Waste Activated Carbon (음식물류 폐기물 활성탄의 제조 및 중금속 흡착특성)

  • Lee, Jun-Hee;Lee, Seung-Chul;Ju, Min;Kim, Ji-Hye;Lee, Don-Gil
    • Journal of Environmental Science International
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    • v.24 no.12
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    • pp.1601-1608
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    • 2015
  • This study evaluates heavy metal(Cu and Cr) adsorption characteristics produced from food waste charcoal extracted in an optimal operation condition after analyzing activated charcoal of iodine adsorption and heavy metals that derived from an activation process of carbide by the developed by-products of food waste treatment facility using the methods from previous studies. As experiment apparatus, this study used a tube-shaped high temp furnace. The mixing ratio of by-products of food waste treatment facility, carbide, and activation component($ZnCl_2$) was 1:1. The experiment was proceeded as adjusting the activation temperature from 400 to $800^{\circ}C$ and activation time from 30 to 120 minutes. The optimal activation condition for iodine absorption was 90 minutes at $700^{\circ}C$ and by using the produced food waste charcoal, this study conducted an experiment on absorption of heavy metals (Cu and Cr) as changing pH of artificial wastewater and stirring time. As a result, pH 7 showed the highest heavy metal decontamination ratio and in terms of stirring time, it revealed balance adsorption after 10 minutes. This result can be particularly applied as basic data for recyclability of high concentration organic waste, by-products of food waste treatment facility, as an food waste charcoal.

Preparation of Anhydrous Magnesium Chloride for a Fused Salt Electrolysis of Magnesium (마그네슘 용융염전해(溶融鹽電解)를 위한 무수(無水)염화마그네슘 제조(製造))

  • Eom, Hyoung-Choon;Park, Hyung-Kyu;Yoon, Ho-Sung
    • Resources Recycling
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    • v.16 no.1 s.75
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    • pp.37-43
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    • 2007
  • It was studied to prepare anhydrous magnesium chloride which could used as the raw material of a fused salt electrolysis of magnesium by dehydration of magnesium chloride hydrate. The dehydration was carried out in a tube furnace at $350{\sim}580^{\circ}C$. It was confirmed that magnesium chloride hydrate was oxdized to magnesia through the dehydration in ambient atmosphere, but anhydrous magnesium chloride could be obtained in hydrogen chloride gas atmosphere. And the crystallity of the product increased with increasing temperature and time of dehydration. All of the un-reacted hydrogen chloride gases which were generated during the dehydration in hydrogen chloride gas atmosphere could be recovered as hydrochloric solution, and it could be reused for chlorination of magnesia to prepare magnesium chloride hydrate.

Characteristics of Background Nanoparticle Concentration in a TiO2 Manufacturing Laboratory (TiO2 제조 실험실에서 나노입자의 배경농도 특징)

  • Park, Seung-Ho;Jung, Jae Hee;Lee, Seung-Bok;Bae, Gwi-Nam;Jie, Hyun Seock;Cho, So-Hye
    • Particle and aerosol research
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    • v.7 no.4
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    • pp.113-121
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    • 2011
  • The aerosol nanoparticles are suspected to be exposed to workers in nanomaterial manufacturing facilities. However, the exposure assessment method has not been established. One of important issues is to characterize background level of nanoparticles in workplaces. In this study, intensive aerosol measurements were made at a $TiO_2$ manufacturing laboratory for five consecutive days in May of 2010. The $TiO_2$ nanoparticles were manufactured by the thermal-condensation process in a heated tube furnace. The particle number size distribution was measured using a scanning mobility particle sizer every 5 min, in order to detect particles ranging from 14.5 to 664 nm in diameter. Total particle number concentration shows a severe diurnal variation irrespective of manufacturing process, which was governed by nanoparticles smaller than 50 nm in diameter. During the background monitoring periods, significant peak concentrations were observed between 2 p.m. and 3 p.m. due to the infiltration of secondary aerosol particles formed by photochemical smog. Although significant increase in nanoparticle concentration was also observed during the manufacturing process twice among three times, these particle peak concentrations were lower than those observed during the background measurement. It is suggested that the investigation of background particle contamination is needed prior to conducting main exposure assessment in nanomaterial manufacturing workplaces or laboratories.

Boron Diffused Layer Formation Process and Characteristics for High Efficiency N-type Crystalline Silicon Solar Cell Applications (N-type 고효율 태양전지용 Boron Diffused Layer의 형성 방법 및 특성 분석)

  • Shim, Gyeongbae;Park, Cheolmin;Yi, Junsin
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.30 no.3
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    • pp.139-143
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    • 2017
  • N-type crystalline silicon solar cells have high metal impurity tolerance and higher minority carrier lifetime that increases conversion efficiency. However, junction quality between the boron diffused layer and the n-type substrate is more important for increased efficiency. In this paper, the current status and prospects for boron diffused layers in N-type crystalline silicon solar cell applications are described. Boron diffused layer formation methods (thermal diffusion and co-diffusion using $a-SiO_X:B$), boron rich layer (BRL) and boron silicate glass (BSG) reactions, and analysis of the effects to improve junction characteristics are discussed. In-situ oxidation is performed to remove the boron rich layer. The oxidation process after diffusion shows a lower B-O peak than before the Oxidation process was changed into $SiO_2$ phase by FTIR and BRL. The $a-SiO_X:B$ layer is deposited by PECVD using $SiH_4$, $B_2H_6$, $H_2$, $CO_2$ gases in N-type wafer and annealed by thermal tube furnace for performing the P+ layer. MCLT (minority carrier lifetime) is improved by increasing $SiH_4$ and $B_2H_6$. When $a-SiO_X:B$ is removed, the Si-O peak decreases and the B-H peak declines a little, but MCLT is improved by hydrogen passivated inactive boron atoms. In this paper, we focused on the boron emitter for N-type crystalline solar cells.

Investigation of Ni/Cu Contact for Crystalline Silicon Solar Cells (결정질 실리콘 태양전지에 적용하기 위한 도금법으로 형성환 Ni/Cu 전극에 관한 연구)

  • Kim, Bum-Ho;Choi, Jun-Young;Lee, Eun-Joo;Lee, Soo-Hong
    • 한국신재생에너지학회:학술대회논문집
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    • 2007.06a
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    • pp.250-253
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    • 2007
  • An evaporated Ti/Pd/Ag contact system is most widely used to make high-efficiency silicon solar cells, however, the system is not cost effective due to expensive materials and vacuum techniques. Commercial solar cells with screen-printed contacts formed by using Ag paste suffer from a low fill factor and a high shading loss because of high contact resistance and low aspect ratio. Low-cost Ni and Cu metal contacts have been formed by using electroless plating and electroplating techniques to replace the Ti/Pd/Ag and screen-printed Ag contacts. Ni/Cu alloy is plated on a silicon substrate by electro-deposition of the alloy from an acetate electrolyte solution, and nickel-silicide formation at the interface between the silicon and the nickel enhances stability and reduces the contact resistance. It was, therefore, found that nickel-silicide was suitable for high-efficiency solar cell applications. The Ni contact was formed on the front grid pattern by electroless plating followed by anneal ing at $380{\sim}400^{\circ}C$ for $15{\sim}30$ min at $N_{2}$ gas to allow formation of a nickel-silicide in a tube furnace or a rapid thermal processing(RTP) chamber because nickel is transformed to NiSi at $380{\sim}400^{\circ}C$. The Ni plating solution is composed of a mixture of $NiCl_{2}$ as a main nickel source. Cu was electroplated on the Ni layer by using a light induced plating method. The Cu electroplating solution was made up of a commercially available acid sulfate bath and additives to reduce the stress of the copper layer. The Ni/Cu contact was found to be well suited for high-efficiency solar cells and was successfully formed by using electroless plating and electroplating, which are more cost effective than vacuum evaporation. In this paper, we investigated low-cost Ni/Cu contact formation by electroless and electroplating for crystalline silicon solar cells.

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The Effect of Promoters Addition on NOx Removal by $NH_3$ over V$V_2O_5/TiO_2$

  • Lee, Keon-Joo
    • Journal of Korean Society for Atmospheric Environment
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    • v.18 no.E1
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    • pp.29-36
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    • 2002
  • The selective catalytic reduction (SCR) reaction of promoter catalysts was investigated in this study. A pure anatase type of TiO$_2$ was used as support. Activation measurement of prepared catalysts was practiced on a fixed reactor packing by the glass bead after filling up catalysts in 1/4 inch stainless tube. The reaction temperature was measured by K-type thermocouple and catalyst was heated by electric furnace. The standard compositions of the simulated flue gas mixture in this study were as follows: NO 1,780ppm, NH$_3$1,780ppm, $O_2$1% and $N_2$ as balance gas. In this study, gas analyzer was used to measure the outgassing gas. Catalyst bed was handled for 1hr at 45$0^{\circ}C$, and the reactivity of the various catalyst was determined in a wide temperature range. Conversion of NH$_3$/NO ratio and of $O_2$ concentration was practiced at 1,1.5 and 2, respectively. The respective space velocity were as follows . 10,000, 15,000 and 17,000 hr-1. It was found that the maximum conversion temperature range was in a 5$0^{\circ}C$. It was also found toi be very sensitive at space velocity, $O_2$ concentration, and NH$_3$/NO ratio. We also noticed that the maximum conversion temperature of (W, Mo, Sn) -V$_2$O$_{5}$/TiO$_2$ catalysts was broad. Specially WO$_3$-V$_2$O$_{5}$TiO$_2$2 catalyst appeared nearly 100% conversion at not only above 30$0^{\circ}C$ ut also below 25$0^{\circ}C$. At over 30$0^{\circ}C$, NH$_3$ oxidation decreased with decrease of surface excess oxygen. In addition, WO$_3$-V$_2$O$_{5}$TiO$_2$ catalyst did not appear to affect space velocity, $O_2$ concentration, and NH$_3$/NO ratio.ratio.