• Title/Summary/Keyword: chemical reduction method

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Volumetric Determination of Tungsten Lead Amalgam Method (탕그스텐의 용량분석법에 관하여 -Pb 아말감법)

  • Q. Won Choi;Kyung Rok Min
    • Journal of the Korean Chemical Society
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    • v.7 no.2
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    • pp.186-188
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    • 1963
  • An attempt to improve the method of volumetric determination of tungsten developed by Luke has been made successfully. Using amalgam coated lead instead of pure metallic lead in the reduction procedure. W(VI)-W(III) reduction has been found to be quantitative in rather concentrated hydrochloric acid. Since there was no excessive dissolution of lead via reduction of hydrogen ion, lead surface was totally accessible for the reduction of tungsten and no trouble was caused by dereposition of $PbCl_2$ crystals at the nozzle of Jones reductor. Furthermore, it has been confirmed that almost 100 mg. of $WO_3$ can be handled easily if the chloride concentration of the HCl is increased by adding solid $NH_4Cl$.

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Preparation and Characterization of Palladium Nanoparticles Supported on Nickel Hexacyanoferrate for Fuel Cell Application

  • Choi, Kwang-Hyun;Shokouhimehr, Mohammadreza;Kang, Yun Sik;Chung, Dong Young;Chung, Young-Hoon;Ahn, Minjeh;Sung, Yung-Eun
    • Bulletin of the Korean Chemical Society
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    • v.34 no.4
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    • pp.1195-1198
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    • 2013
  • Nickel hexacyanoferrate supported palladium nanoparticles (Pd-NiHCF NPs) were synthesized and studied for oxygen reduction reactions in direct methanol fuel cell. The NiHCF support was readily synthesized by a comixing of $Ni(OCOCH_3)_2$ and equimolar $K_3[Fe(CN)_6]$ solution into DI water under rigorous stirring. After the preparation of NiHCF support, Pd NPs were loaded on NiHCF via L-ascorbic acid reduction method at $80^{\circ}C$. Pd-NiHCF NPs were electrochemically active for oxygen reduction reaction in 0.1 M $HClO_4$ solution. X-ray absorption near edge structure analysis was conducted to measure the white line intensity of Pd-NiHCF to verify the OH adsorption. As a comparison, carbon supported Pd NPs exhibited same white line intensity. This study provides a general synthetic approach to easily load Pd NPs on porous coordination polymers such as NiHCF and can provide further light to load Pd based alloy NPs on NiHCF framework.

Electrochemical Reduction of SiO2 Granules to One-Dimensional Si Rods Using Ag-Si Eutectic Alloy

  • Lee, Han Ju;Seo, Won-Chul;Lim, Taeho
    • Journal of Electrochemical Science and Technology
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    • v.11 no.4
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    • pp.392-398
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    • 2020
  • Producing solar grade silicon using an inexpensive method is a key factor in lowering silicon solar cell costs; the direct electrochemical reduction of SiO2 in molten salt is one of the more promising candidates for manufacturing this silicon. In this study, SiO2 granules were electrochemically reduced in molten CaCl2 (850℃) using Ag-Si eutectic droplets that catalyze electrochemical reduction and purify the Si product. When Ag is used as the working electrode, the Ag-Si eutectic mixture is formed naturally during SiO2 reduction. However, since the Ag-Si eutectic droplets are liquid at 850℃, they are easily lost during the reduction process. To minimize the loss of liquid Ag-Si eutectic droplets, a cylindrical graphite container working electrode was introduced and Ag was added separately to the working electrode along with the SiO2 granules. The graphite container working electrode successfully prevented the loss of the Ag-Si eutectic droplets during reduction. As a result, the Ag-Si eutectic droplets acted as stable catalysts for the electrochemical reduction of SiO2, thereby producing one-dimensional Si rods through a mechanism similar to that of vapor-liquid-solid growth.

Preparation of Copper Fine Particles from Waste Copper by Chemical Reduction Method (폐동분으로부터 화학환원법에 의한 Cu 미립자 제조)

  • Kim, Yoon-Do;Song, Ki Chang;Song, Jong-Hyeok
    • Korean Chemical Engineering Research
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    • v.45 no.6
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    • pp.560-565
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    • 2007
  • Copper fine particles, ranging from $0.11{\mu}m$ to $0.64{\mu}m$ in average size, were prepared by a chemical reduction method using hydrazine ($N_2H_4$) as a reduction agent in waste copper solutions. The effect of the amount of hydrazine addition was investigated on the properties of the obtained powders. Also, the effect of the addition of dispersing agents [Polyvinyl alcohol (PVA), polyvinyl pyrrolidone (PVP)] during particle synthesis was studied. The powders, obtained from 1 M waste copper solutions, showed the mixtures of Cu and $Cu_2O$ crystals at low hydrazine addition amounts of 0.8 mol and 1.0 mol, while those exhibited pure Cu crystals at adequate hydrazine addition amount of 0.12 mol. The average size of the Cu powders decreased with increasing the concentrations of hydrazine and dispersing agents. The addition of PVA to the solutions as a dispersing agent was more effective than that of PVP in preventing the aggregation of particles.

Effect of Surfactant on Synthesis of Colloidal Ag Nanoparticles (콜로이드 Ag 나노입자 합성시 계면활성제의 영향)

  • Lee Jong-Kook;Choi Nam-Kyu;Seo Dong-Seok
    • Korean Journal of Materials Research
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    • v.15 no.5
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    • pp.340-347
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    • 2005
  • Silver nanoparticles were synthesized by chemical reduction method from aqueous silver nitrate solution ana hydrazine as a reduction agent. The morphology, particle size and shape were dependent on the mixing method, reaction temperature and time, molar ratio of hydrazine and silver nitrate, the kind of surfactant, and the addition of surfactant. The stability of the colloidal silver was achieved by the adsorption of surfactant molecules onto the particle. Silver nanoparticles have a characteristic absorption maximum at 430 nm under UV irradiation. It was found that the colloid was nanometer m size and formed very stable dispersion of silver. The Ag nanoparticles obtained showed the spherical shape with the size range of 10-30 nm.

Efficiency of a Direct Absorption Solar Collector using Ag Nanofluids Synthesized by Chemical Reduction Method (화학적 환원법으로 제조된 은나노유체를 사용한 직접흡수식 태양열 집열기의 효율)

  • Lee, Seung-Hyun;Park, Yong-Jun;Choi, Tae Jong;Jang, Seok Pil
    • Journal of the Korean Solar Energy Society
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    • v.34 no.5
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    • pp.65-72
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    • 2014
  • In this paper, the water-based Ag nanofluids are synthesized by the chemical reduction method and their extinction coefficients are measured by an in-house developed measurement device. The Ag nanofluids are manufactured by the chemical reduction method with the mixing of silver nitrate ($AgNO_3$) and sodium borohydride ($NaBH_4$) in an aqueous solution of polyvinyl pyrrolidone (PVP). The extinction coefficients of Ag nanofluids are measured by means of the in-house developed apparatus at a wavelength of 632.8nm according to the particle volume fractions. The results show that the extinction coefficient of water-based Ag nanofluids increases with the increase of nanoparticle concentrations. Finally, the temperature field and efficiency of direct absorption solar collector (DASC) are analytically estimated based on the measured extinction coefficient of water-based Ag nanofluids. The results indicate that the direct absorption solar collectors using nanofluids have the feasibility to improve the efficiency of conventional flat-plate solar collectors without using an absorber plate.

Characterization of Graphite Oxide Reduced by Thermal and/or Chemical Treatments

  • Kim, Jungsoo;Nam, Dae-Geun;Yeum, Jeong Hyun;Suh, Sungbu;Oh, Weontae
    • Transactions on Electrical and Electronic Materials
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    • v.16 no.5
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    • pp.274-279
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    • 2015
  • Reduced graphite oxides (rGOs) were prepared by the common graphite oxidation method and the subsequent reductions. The reduction of graphite oxides (GOs) was conducted chemically and/or thermally. To further reduce the as-prepared rGOs, GOs were treated with chemical/thermal reductions or thermal/chemical reductions, in which the reduction sequence was also considered. The structural changes of as-prepared rGOs, depending on reduction methods, were investigated by X-ray diffraction analyses, Raman spectroscopy, X-ray photoelectron spectroscopy, and scanning electron microscopy. In addition, we discuss the structural change of the rGOs and their closely related physical and electrical properties, such as thermogravimetry, nitrogen adsorption isotherm, and sheet resistance.

Development of cobalt encased in nitrogen and sulfur co-doped carbon nanotube for non-precious metal catalyst toward oxygen reduction reaction

  • Kim, Tae-Hyun;Sang, Byoung-In;Yi, Sung-Chul
    • Journal of Ceramic Processing Research
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    • v.19 no.6
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    • pp.499-503
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    • 2018
  • In this paper, cobalt embedded in nitrogen and sulfur co-doped carbon nanotubes (CoNSTs) were synthesized for oxygen reduction reaction (ORR) catalysts. The CoNSTs were prepared through a facile heat treatment method without any templates. Different amounts of the metal salt were employed to examine the physicochemical and electrochemical properties of the CoNSTs. The CoNSTs showed the bamboo-like tube morphology with the encased Co nanoparticles in the tubes. Through the x-ray photoelectron spectroscopy analysis, the catalysts exhibited different chemical states of the nitrogen and sulfur species. As a result, the CoNST performed high activity toward the ORR in an acidic condition with the onset potential of 0.863 V (vs. reversible hydrogen electrode). It was clearly demonstrated from the electrochemical characterizations that the quality of the nitrogen and sulfur species significantly influences the ORR activity rather than the total amount of the dopants.

Effect of Cobalt Loading on the Performance and Stability of Oxygen Reduction and Evolution Reactions in Rechargeable Zinc-air Batteries

  • Sheraz Ahmed;Joongpyo Shim;Gyungse Park
    • Journal of the Korean Chemical Society
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    • v.68 no.2
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    • pp.87-92
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    • 2024
  • The commercialization of rechargeable metal-air batteries is extremely desirable but designing stable oxygen reduction reaction (ORR) catalysts with non-noble metal still has faced challenges to replace platinum-based catalysts. The nonnoble metal catalysts for ORR were prepared to improve the catalytic performance and stability by the thermal decomposition of ZIF-8 with optimum cobalt loading. The porous carbon was obtained by the calcination of ZIF-8 and different loading amounts of Co nanoparticles were anchored onto porous carbon forming a Co/PC catalyst. Co/PC composite shows a significant increase in the ORR value of current and stability (500 h) due to the good electronic conductive PCN support and optimum cobalt metal loading. The significantly improved catalytic performance is ascribed to the chemical structure, synergistic effects, porous carbon networks, and rich active sites. This method develops a new pathway for a highly active and advantageous catalyst for electrochemical devices.

Synthesis and Oxygen Reduction Reaction Evaluation of 20% Pt/C for Polymer Electrolyte Fuel Cell (고분자전해질 연료전지용 20% Pt/C 캐소드 촉매 제조 및 산소환원반응 평가)

  • Kim, Jinhwan;Kang, Suk-Min;Thube, Dilip. R.;Ryu, Hojin
    • Korean Journal of Metals and Materials
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    • v.47 no.7
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    • pp.454-459
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    • 2009
  • In order to commercialize Polymer Electrolyte Fuel Cell (PEFC), the cathode catalyst such as Platinum supported Carbon (Pt/C) need to have a high activity of Oxygen Reduction Reaction (ORR). In this study, the 20% Pt/C was synthesized using the chemical reduction method while the crystallinity of Platinum (Pt) particles were controlled under heat treatment conditions. The activity of synthesized Pt catalysts was evaluated using electrochemical measurement. Compared with the $i_{ORR}$ at 0.8 V of 20% Pt/C heat-treated at $500^{\circ}C$ and the 20% Pt/C that were not heated and commercial 20% Pt/C, the $i_{ORR}$ at 0.8 V of 20% Pt/C heattreated at $500^{\circ}C$ was 9.5 and 1.7 times higher than those of the 20% Pt/C and commercial 20% Pt/C that were not heated. It was considered that the crystallinity and particle size affect the ORR activity of the Pt/C catalysts.