• Title/Summary/Keyword: EDS Process

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Investigating the Au-Cu thick layers Electrodeposition Rate with Pulsed Current by Optimization of the Operation Condition

  • Babaei, Hamid;Khosravi, Morteza;Sovizi, Mohamad Reza;Khorramie, Saeid Abedini
    • Journal of Electrochemical Science and Technology
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    • v.11 no.2
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    • pp.172-179
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    • 2020
  • The impact of effective parameters on the electrodeposition rate optimization of Au-Cu alloy at high thicknesses on the silver substrate was investigated in the present study. After ensuring the formation of gold alloy deposits with the desired and standard percentage of gold with the cartage of 18K and other standard karats that should be observed in the manufacturing of the gold and jewelry artifacts, comparing the rate of gold-copper deposition by direct and pulsed current was done. The rate of deposition with pulse current was significantly higher than direct current. In this process, the duty cycle parameter was effectively optimized by the "one factor at a time" method to achieve maximum deposition rate. Particular parameters in this work were direct and pulse current densities, bath temperature, concentration of gold and cyanide ions in electrolyte, pH, agitation and wetting agent additive. Scanning electron microscopy (SEM) and surface chemical analysis system (EDS) were used to study the effect of deposition on the cross-sections of the formed layers. The results revealed that the Au-Cu alloy layer formed with concentrations of 6gr·L-1 Au, 55gr·L-1 Cu, 24 gr·L-1 KCN and 1 ml·L-1 Lauryl dimethyl amine oxide (LDAO) in the 0.6 mA·cm-2 average current density and 30% duty cycle, had 0.841 ㎛·min-1 Which was the highest deposition rate. The use of electrodeposition of pure and alloy gold thick layers as a production method can reduce the use of gold metal in the production of hallow gold artifacts, create sophisticated and unique models, and diversify production by maintaining standard karats, hardness, thickness and mechanical strength. This will not only make the process economical, it will also provide significant added value to the gold artifacts. By pulsating of currents and increasing the duty cycle means reducing the pulse off-time, and if the pulse off-time becomes too short, the electric double layer would not have sufficient growth time, and its thickness decreases. These results show the effect of pulsed current on increasing the electrodeposition rate of Au-Cu alloy confirming the previous studies on the effect of pulsed current on increasing the deposition rate of Au-Cu alloy.

Studies on the Preservative Condition and the Ultrastructure of Hair of Newly Found Sixteenth Century Mummy in Paju (파주에서 발견된 16세기 미라 머리카락의 미세구조과 보존상태에 관한 연구)

  • Lee, Gwi-Yeong;Chang, Byung-Soo
    • Applied Microscopy
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    • v.35 no.4
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    • pp.24-31
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    • 2005
  • The preservative condition and ultrastructure on the mummified hair collected from newly found female mummy in Paju, were investigated by using scanning and transmission electron microscopes. The female mummy was found in september, 2002 during the traditional reburial process for the buried ones. The hair of 16th century mummy showed very intact appearances during observation with electron microscope. And the structures of the cortex, medulla and cuticle were well preserved. The cuticle layer was easily discernable, which are composed of six to seven cuticular cells. Each cuticular cells surrounded and thus seperated from its neighbors by intercellular membrane complex. In the cortex, many macrofibrils and some melanin granules between them were observed. We observed well preserved rod form macrofibrils running parallel along the direction of hair shaft. Especially, melanin granules were aggregated in the cortex which was adjacent to the cuticlu layer. As to the cause for the well-preservation of 440 year old hair sample, the presence of surface coat on the hair, which are composed of various materials. As calcium was included in the surface coat in Electron Dispersive X-ray Spectroscopy (EDS), the hardening process of the surface coat by calcium might inhibit the water or microorganism infiltration into the hair.

Microstructure of Co-base superalloy prepared by a investment casting (정밀주조법으로 제조된 Co계 초내열 합금의 미세구조)

  • Lee, Jung-Il;Lee, Ho Jun;Cho, Hyun Su;Paeng, Jong Min;Park, Jong Bum;Ryu, Jeong Ho
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.27 no.6
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    • pp.313-318
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    • 2017
  • The microstructure of a cobalt-base superalloy (ECY768) obtained by an investment casting process was studied. This work focuses on the resulting microstructures arising from different melt and mold temperatures in normal industrial environmental conditions. The characterization of the samples was carried out using optical microscopy, field emission scanning electron microscopy and energy-dispersive spectroscopy. In this study, the as-cast microstructure is an ${\alpha}-Co$ (face-centered cubic) dendritic matrix with the presence of a secondary phase, such as $M_{23}C_6-type$ carbides precipitated at grain boundaries. These precipitates are the main strengthening mechanism in this type of alloy. Other minority phases, such as the MC-type phase, was also detected and their presence could be linked to the manufacturing process and environment.

Morphology and Crystal Orientation of Mg Films formed on Hot Dip Galvanized Steel by PVD Method at Ar or N2 Gas Pressures and Their Corrosion Resistances (Ar 및 N2 가스압 중에서 PVD법에 의해 용융아연 도금 강재상 형성한 Mg 막의 모폴로지 및 결정배향성과 그 내식성)

  • Hwang, Seong-Hwa;Park, Jae-Hyeok;Park, Jun-Mu;Choe, In-Hye;Kim, Sun-Ho;Lee, Myeong-Hun
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2017.05a
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    • pp.166-166
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    • 2017
  • 금속 재료 중 철강은 기계적 특성이 우수하고 대량생산이 가능하여 선박, 건축, 자동차 등 다양한 분야에 기초재료로써 널리 사용되고 있다. 그러나 스테인리스강 등과 같은 일부 특수한 용도의 강을 제외하고는 부식환경에 취약한 특성을 가지기 때문에 내식성을 향상을 위한 표면처리에 관한 연구가 활발히 진행되고 있다. 가장 일반적으로 습식법(wet process)을 통해 표면상에 아연(Zn)을 도금해 사용하며, 아연이 자체적으로 포함한 희생양극(sacrificial anode) 및 차폐(barrier) 효과가 철강의 부식을 방지하게 된다. 하지만 산업의 고도화에 따라 더욱 가혹해진 노출환경으로 인해 고내식 강재에 대한 수요가 점차 증가하고 있으며, 아연코팅 층의 두께를 증가하여 내식성을 확보하는 방안은 미래 환경 및 자원적인 측면에서 근본적인 해결책으로 제시하기 어려움이 있다. 한편, 건식 프로세스(wet process)로 대별되는 PVD(physical vacuum deposition)에 의해 내식성을 향상시키고자 하는 연구들이 다양하게 진행되고 있다. 이것은 표면에 고순도 양질의 금속 막을 형성시킴으로써 외부환경과의 반응을 효과적으로 제어가 가능하며, 형성된 막은 그 물질의 고유 특성뿐만 아니라 제작 조건에 따른 표면의 기하학적 혹은 결정학적 구조에 의해 크게 영향을 받게 된다. 본 연구에서는 실용금속 중 이온화 경향이 가장 크고 산소와 반응하여 투과성이 작은 산화 피막 형성이 유리한 마그네슘(Mg)을 활용해 표면의 전기화학적 특성을 향상시켰다. 또한 금속 증착 중 진공도조절을 위해 도입되는 불활성 가스로 아르곤(Ar) 및 질소($N_2$)를 사용하여 표면에 형성한 막의 모폴로지 및 결정배향성이 내식성에 미치는 상관관계를 해석하고자 하였다. 실험방법으로 PVD법 중 비교적 간편하고 기초적인 지침을 제시하기 적합할 것으로 고려된 진공증착(vacuum evaporation)법을 이용해 아르곤 및 질소 분위기에서 진공도를 조절하며 용융아연도금상 Mg막을 형성하였다. 제작조건별 막의 기초 특성을 분석하기위해 SEM, EDS, XRD를 이용하였고, 결정배향성(crystal orientation) 분석을 위해 면간격(d-value)과 상대강도(relative intensity)를 확인하였다. 또한 내식성 평가로 염수분무(salt sprat test) 및 양극분극(anode polarization)을 각각 실시하였다. 실험결과에 따르면, Ar 및 $N_2$ 모두에서 가스압이 증가할수록 코팅층의 증착량은 적어지고 입상정(granular structure)의 모폴로지 형성 및 면간격과 상대강도가 증가하는 것이 확인되었다. 또한 쳄버 내 동일 진공도에서, $N_2$ 도입 시 Mg막은 더욱 치밀하고 미세한 입상정의 모폴로지로 형성되며 면간격과 상대강도는 더욱 증가한 것으로 나타났다. 내식성 평가에서 저진공 $N_2$ 조건에서 형성시킨 막이 가장 우수한 내식성이 나타났는데, 이는 상대적으로 불안정하고 반응하기 유리한 입계면적을 많이 포함한 입상정 모폴로지 및 표면에너지가 높은면의 면점유율 증가로 인해 외부환경과의 신속한 반응은 물론 안정적인 피막형성이 용이하였기 때문일 것으로 사료된다. 이상으로 Ar 및 $N_2$ 가스압 조건에 따른 고내식 Mg 막의 유효성을 확인하였고 향후 내식성을 향상시키는 방법으로 응용 가능할 것으로 생각된다.

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The Effect of NH3 Concentration during Co-precipitation of Precursors from Leachate of Lithium-ion Battery Positive Electrode Active Materials (리튬이차전지 양극활물질의 암모니아 침출액에서 공침법에 의한 활물질 전구체의 합성에 대한 암모니아 농도의 영향)

  • Park, Sanghyuk;Ku, Heesuk;Lee, Kyoung-Joon;Song, Jun Ho;Kim, Sookyung;Sohn, Jeongsoo;Kwon, Kyungjung
    • Resources Recycling
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    • v.24 no.6
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    • pp.9-16
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    • 2015
  • In a recycling scheme of spent lithium ion batteries, a co-precipitation process for the re-synthesis of precursor is essential after the leaching of lithium ion battery scraps. In this study, the effect of ammonia as impurity during the co-precipitation process was investigated in order to re-synthesize a precursor of Ni-rich cathode active material $LiNi_{0.6}Co_{0.2}Mn_{0.2}O_2$ (NCM 622). As ammonia concentration increases from 1 M (the optimum condition for synthesis of the precursors based on 2 M of metal salt solution) to 4 M, the composition of obtained precursors deviates from the designed composition, most notably for Ni. The Ni co-precipitation efficiency gradually decreases from 100% to 87% when the concentration of ammonia solution increases from 1 M to 4 M. Meanwhile, the morphological properties of the obtained precursors such as sphericity, homogeneity and size distribution of particles were also investigated.

Material Characteristic of Slags and Iron Bloom Produced by Smelting Process Using Sand Iron (사철 제련을 통해 생산된 슬래그와 괴련철의 재료과학적 특성 비교)

  • Cho, Sung Mo;Cho, Hyun Kyung;Kwon, In Cheol;Cho, Nam Chul
    • Journal of Conservation Science
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    • v.34 no.1
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    • pp.39-50
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    • 2018
  • This study replicated traditional smelting methods to produce iron blooms from sand iron. The metallurgical properties of the slag and the iron blooms were analyzed. The sand iron materials used in the smelting experiments, which were based on ancient documents, were collected from Gyeong-Ju and Pohang. Analysis by WD-XRF and XRD showed that Gyeong-Ju's sand iron contains a high-titanium, with magnetite, and Pohang's sand iron contains a low-titanium, which magnetite and ilmenite were mixed. Analysis of the slag with XRD, and the micro-structure with metal microscopes and SEM-EDS, confirmed that the major compounds in the slag of the Gyeong-Ju's sand iron were fayalite and $w\ddot{u}stite$, and those in the slag of the Pohang's sand iron were titanomagnetite and fayalite. The differences in the main constituents were confirmed according to the Ti quantity. Finally, we observed the microstructures of the iron blooms. In the case of the iron bloom produced from Gyeong-Ju's sand iron, the outside was found to be dominantly a pearlite of eutectoid steel, while the inside was a hypo-eutectoid steel where ferrite and pearlite were mixed together. While, the major component of the iron bloom produced from Pohang's sand iron was ferrite, which is almost like pure iron. However, there were many impurities inside the iron blooms. Therefore, this experiment confirmed that making ironware required a process that involved removing internal impurities, refining, and welding. It will be an important data to identify the characteristics of iron by-products and the site through traditional iron-making experiments under various conditions.

The Methane Reforming by $CO_2$ Using Pelletized Co-Ru-Zr-Si Catalyst (성형 Co-Ru-Zr-Si 촉매를 이용한 이산화탄소에 의한 메탄 리포밍)

  • Nam, Jeong-Kwang;Lee, Ji-Hye;Song, Sang-Hoon;Ahn, Hong-Chan;Chang, Tae-Sun;Suh, Jeong-Kwon;Kim, Seong-Bo
    • Applied Chemistry for Engineering
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    • v.23 no.2
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    • pp.176-182
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    • 2012
  • The methane dry reforming has received the considerable attention in recent years, mainly as an attractive route to produce synthesis gas (CO, $H_2$) from green-house gases ($CH_4$, $CO_2$) for resources. However, this process has not been commercialized due to the high temperature and catalyst deactivation. In this study, Co-Ru-Zr catalysts supported on $SiO_2$ were studied for the characterization of methane dry reforming reaction and the preliminary data for process development were achieved. The crystal structure of catalysts was measured by XRD, the surface area and pore size were analyzed by BET, and the element composition of catalyst were analyzed by EDS. Conversions of methane and carbon dioxide were analyzed by GC. In addition, reaction rate constants were obtained from the reaction kinetic study and the optimum catalyst size that does not affect mass transfer from reactants was also determined. The selected pellet-type catalyst maintained activation for 720 h at $850^{\circ}C$.

Stabilization Mechanisms of Powdered and Bead Type Stabilizer Made of Mg-Fe Layered Double Hydroxide (LDH) for the Arsenic Contaminated Soil (Mg-Fe 이중층수산화물로 제조한 분말상과 입상 안정화제의 비소 오염토양 안정화 기작)

  • Kim, Seonhee;Kim, Kyeongtae;Oh, Yuna;Han, Yikyeong;Lee, Minhee
    • Journal of Soil and Groundwater Environment
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    • v.27 no.4
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    • pp.49-62
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    • 2022
  • The magnesium and iron-based layered double hydroxide (Mg-Fe LDH) was synthesized by the co-precipitation process and the bead type LDH (BLDH, 5~6 mm in diameter) was manufactured by using the Mg-Fe LDH and the starch as a binder. To evaluate the feasibility of the BLDH as the As stabilizer in the soil, various experiments were performed and the As stabilization efficiency of the BLDH was compared to that of powdered type LDH (PLDH, <149 ㎛ in diameter). For the As sorption batch experiment, the As sorption efficiency of both of the PLDH and the BLDH showed higher than 99%. For the stabilization experiment with soil, the As extraction reducing efficiency of the PLDH was higher than 87%, and for the BLDH, it was higher than 80%, suggesting that the BLDH has similar the feasibility of As stabilization for the contaminated soil, compared to the PLDH. From the continuous column experiments, when more than 7% BLDH was added into the soil, the As stabilization efficiency of the column maintained at over 91% for 7 pore volume flushing (simulating about 21 months of rainfall) and slowly decreased down to 64% after that time (to 36 months) under the non-equilibrium conditions. Results suggested that more than 7% of BLDH added in As-contaminated soil could be enough to stabilize As in soil for a long time. The main As fixation mechanisms on the LDH were also identified through the X-ray fluorescence (XRF), the X-ray diffraction (XRD), and the Fourier transform infrared (FT-IR) analyses. Results showed that the LDH has enough of an external surface adsorption capacity and an anion exchange capability at the interlayer spaces. Results of SEM/EDS and BET analyses also supported that the Mg-Fe LDH used in this study has sufficient porous structures and outer surfaces to fix the As. The reduction of carbonate (CO32-) and sulfate (SO42-) anions in the LDH after the reaction between As and the LDH was observed through the FT-IR, the XRF, and the XRD analyses, suggesting that the exchange of some of these anions with the arsenate (H2AsO4- or HAsO42-) occurs at the LDH interlayers during the stabilization process in soil.

Study of the corrosion effect of CO2 stream with SO2 and NO2 on a phosphate coated steel tube (SO2 및 NO2 포함 고압 CO2 스트림이 인산염 코팅 CO2 수송관 부식에 미치는 영향)

  • Cho, Meang-Ik;Kang, Seong-Gil;Huh, Cheol;Baek, Jong-Hwa
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.15 no.12
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    • pp.6973-6979
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    • 2014
  • To mitigate global warming and climate change, many countries are investing massively on the development of CCS technology, which is assumed to be the key technology to reduce $CO_2$ emissions. CCS technology is comprised of the capture, transport, and storage processes. During the capture process, impurities other than $CO_2$ are inevitably flowed into the $CO_2$ stream. In the present study, corrosion characteristics of a phosphate coated tube for $CO_2$ transportation was investigated with a $CO_2$ stream composed of $CO_2$, $H_2O$, $SO_2$, and $NO_2$. The test specimen was a phosphate coated steel tube, which was filled with $CO_2$ stream with the impurities mentioned above. SEM-EDS analysis is conducted to investigate the corrosion behavior. The results showed that although the H2O concentration did not exceed the solubility limit, corrosion occurred in the specimen, which has an inflow of $SO_2$ or $NO_2$. This suggests that the $SO_2$, $NO_2$ and $H_2O$ concentration should be strictly controlled. These results suggest that the $SO_2$ and $NO_2$ concentration should be controlled below 175ppm and 65ppm, respectively.

Silica and Iron Oxide Recovery and Mineral Carbonation from Serpentine Minerals Using Acid Dissolution and pH Swing Processes (산 처리와 pH 조절을 이용한 사문석군 광물로부터 규소와 철산화물 회수 및 광물 탄산화 연구)

  • Baek, Jiyeon;Jo, Yeonu;Lee, Jeongheon;Kwon, Nayoon;Kim, Yeram;Choi, Suk;Kim, Sunghee;Roh, Yul
    • Economic and Environmental Geology
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    • v.49 no.1
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    • pp.13-22
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    • 2016
  • The objectives of this study were to recover silica and iron oxides and $CO_2$ sequestration using serpentine via various acid dissolution and pH swing processes. Serpentine collected from Guhang-myeon in S. Korea were mainly composed of antigorite and magnetite consisting of $SiO_2$ (45.3 wt.%), MgO (41.3 wt.%), $Fe_2O_3$ (12.2 wt.%). Serpentine pulverized ($${\leq_-}75{\mu}m$$) and then dissolved in 3 different acids, HCl, $H_2SO_4$, $HNO_3$. Residues treated with acidic solution were recovered from the solution (step 1). And then the residual solution containing dissolved serpentine was titrated using $NH_4OH$. And pH of the solution increased up to pH=8.6 to obtain reddish precipitates (step 2). After recovery of the precipitates, the residual solution reacted with $CO_2$ and then pH increased up to pH=9.5 to precipitate white materials (step 3). The mineralogical characteristics of the original sample and harvested precipitates were examined by XRD, and TEM-EDS analyses. ICP-AES analysis was also used to investigate solution chemistry. The dissolved ions were Mg, Si, and Fe. The antigorite became noncrystralline silica after acid treatment (step 1). The precipitate at pH=8.6 was mainly amorphous iron oxide, of which size ranged from 2 to 10 nm and mainly consisting of Fe, O, and Si (step 2). At pH=9.5, nesquehonite [$Mg(HCO_3)(OH){\cdot}2(H_2O)$] and lasfordite [$MgCO_3{\cdot}H_2O$] were formed after reaction with $CO_2$ (step 3). The size of carbonated minerals was ranged from 1 to $6{\mu}m$. These results indicated that the acid treatment of serpentine and pH swing processes for the serpentine can be used for synthesis of other materials such as silica, iron oxides and magnesium carbonate. Also, This process may be useful for the precursor synthesis and $CO_2$ sequestration via mineral carbonation.