• Title/Summary/Keyword: Precursor Solution

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Synthesis and Magnetic Characterization of Fe-nitride for Magnetic Recording (기록매체용 Iron-nitride의 합성 및 자기특성)

  • O, Yeong-U;Kim, Mun-Seop
    • Journal of the Korean Magnetics Society
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    • v.2 no.3
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    • pp.244-250
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    • 1992
  • Iron nitride $Fe_4N$ by partial substitution of nitrogen by carbon was prepared by nitriding the iron oxalate whose thermal decomposition gives a carburating atmosphere. Iron oxalates, the precursors, were prepared by precipitation and co-precipitation. The size and shape of the carbonitride particles could be controlled by modifying the conditions of preparation of the oxalate precursor. From the results of electron micrographs, it is clear that the $Fe_4N$ pigment particle maintains the original shape(needle shape) of the starting materials and that it consists of fine unit particles which link together to form a stereo-network structure. An investigation of the $Fe^{II}_3\;Fe^I_{1-x}\;Sn_xN_{1-y}C_y$ solid solution has shown that Sn plays the role of a growth inhibitor of the elementary microcrystallites of the iron carbonitride. The coercive force and saturation magnetization of iron carbonitride obtained from co-precipitated iron oxalate were 500 Oe and 120 emu/g, respectively.

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Effects of Doping Elements and the Amounts of Oxygen/Nitrogen Contents in Final Nitrides on the Characteristics of Red Pigment of Tantalum Nitrides (Ta3N5) (적색 안료인 탄탈륨 질화물(Ta3N5)의 특성에 도핑 물질 및 최종질화물의 산소/질소 함량이 미치는 영향)

  • Park, Eun-Young;Pee, Jae-Hwan;Kim, Yoo-Jin;Cho, Woo-Seok;Kim, Kyeong-Ja
    • Journal of Powder Materials
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    • v.16 no.6
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    • pp.396-402
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    • 2009
  • Tantalum nitrides ($Ta_3N_5$) have been developed to substitute the Cd based pigments for non-toxic red pigment. Various doping elements were doped to reduce the amount of high price Tantalum element used and preserve the red color tonality. Doping elements were added in the synthesizing process of precursor of amorphous tantalum oxides and then Tantalum nitrides doped with various elements were obtained by ammonolysis process. The average particle size of final nitrides with secondary phases was larger than the nitride without the secondary phases. Also secondary phases reduced the red color tonality of final products. On the other hand, final nitrides without secondary phase had orthorhombic crystal system and presented good red color. In other words, in the case of nitrides without secondary phases, doping elements made a solid solution of tantalum nitride. In this context, doping process controlled the ionic state of nitrides and the amount of oxygen/nitrogen in final nitrides affected the color tonality.

Preparation of Nanocrystalline ZnO Ultrafine Powder Using Ultrasonic Spraying Combustion Method (초음파분무 연소법에 의한 나노결정 ZnO 초미분체 제조)

  • Kim, Kwang-Su;Hwang, Du-Sun;Ku, Suk-Kyeon;Lee, Kang;Jeon, Chi-Jung;Lee, Eun-Gu;Kim, Sun-Jae
    • Korean Journal of Materials Research
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    • v.12 no.10
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    • pp.784-790
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    • 2002
  • For mass product of nanocrystalline ZnO ultrafine powders, self-sustaining combustion process(SCP) and ultrasonic spray combustion method(USCM) were applied at the same time. Ultrasonic spray gun was attached on top of the vertical type furnace. The droplet was sprayed into reaction zone of the furnace to form SCP which produces spherical shape with soft agglomerate crystalline ZnO particles. To characterize formed particles, fuel and oxidizing agent for SCP were used glycine and zinc nitrate or zinc hydroxide. Respectively, with changing combustion temperature and mixture ratio of oxidizing agent and fuel, the best ultrasonic spray conditions were obtained. To observe ultrasonic spray effect, two types of powder synthesis processes were compared. One was directly sprayed into furnace from the precursor solution (Type A), the other directly was heated on the hot plate without using spray gun (Type B). Powder obtained by type A was porous sponge shape with heavy agglomeration, but powder obtained using type B was finer primary particle size, spherical shape with weak agglomeration and bigger value of specific surface area. 9/ This can be due to much lower reaction temperature of type B at ignition time than type A. Synthesized nanocrystalline ZnO powders at the best ultrasonic spray conditions have primary particle size in range 20~30nm and specific surface area is about 20m$^2$/g.

Nano-sized Gd2O3:Eu Phosphor Prepared by Spray Pyrolysis (분무열분해 공정에 의해 합성되어진 나노 크기 Gd2O3:Eu형광체)

  • Kim, Eun-Joung;Kang, Yun-Chan;Park, Hee-Dong;Ryu, Seung-Kon
    • Korean Journal of Materials Research
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    • v.12 no.10
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    • pp.771-775
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    • 2002
  • $Gd_2$$O_3$:Eu phosphor particles with nano-sized and non-aggregation characteristics were prepared by spray pyrolysis using the spray solution containing polymeric precursor and $Li_2$$CO_3$ flux material. Nano-sized $Gd_2$$O_3$:Eu phosphor particles had higher brightness than the commercial $Y_2$$O_3$:Eu phosphor particles. The $Gd_2$$O_3$:Eu phosphor particles had nano-size and non-aggregation characteristics after heat-treatment at $1000^{\circ}C$ when the addition amount of $Li_2$$CO_3$ flux was 1 wt.% and 3 wt.%. The mean size of particles were 200 nm and 400 nm when the amount of flux was 1 wt.% and 3 wt.%, respectively. The prepared phosphor particles had higher photoluminescence intensity than that of the commercial product regardless of the content of$ Li_2$$CO_3$ flux and had the maximum brightness when the content of flux was 5 wt %. The photoluminescence intensity of the nano-sized $Gd_2$$O_3$:Eu phosphor particles containing 3 wt.% $Li_2$$CO_3$ flux was 125% in comparison with that of the micron-sized $Y_2$$O_3$:Eu commercial product.

One-step synthesis of dual-transition metal substitution on ionic liquid based N-doped mesoporous carbon for oxygen reduction reaction

  • Byambasuren, Ulziidelger;Jeon, Yukwon;Altansukh, Dorjgotov;Ji, Yunseong;Shul, Yong-Gun
    • Carbon letters
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    • v.17 no.1
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    • pp.53-64
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    • 2016
  • Nitrogen (N)-doped ordered mesoporous carbons (OMCs) with a dual transition metal system were synthesized as non-Pt catalysts for the ORR. The highly nitrogen doped OMCs were prepared by the precursor of ionic liquid (3-methyl-1-butylpyridine dicyanamide) for N/C species and a mesoporous silica template for the physical structure. Mostly, N-doped carbons are promoted by a single transition metal to improve catalytic activity for ORR in PEMFCs. In this study, our N-doped mesoporous carbons were promoted by the dual transition metals of iron and cobalt (Fe, Co), which were incorporated into the N-doped carbons lattice by subsequently heat treatments. All the prepared carbons were characterized by via transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). To evaluate the activities of synthesized doped carbons, linear sweep was recorded in an acidic solution to compare the ORR catalytic activities values for the use in the PEMFC system. The dual transition metal promotion improved the ORR activity compared with the single transition metal promotion, due to the increase in the quaternary nitrogen species from the structural change by the dual metals. The effect of different ratio of the dual metals into the N doped carbon were examined to evaluate the activities of the oxygen reduction reaction.

Synthesis of Sulfonated Poly(phenylene sulfide) via Soluble Precursor and its Ammonia Gas Adsorption (용해성 전구체를 통한 Sulfonated Poly(phenylene sulfide)의 합성과 암모니아가스 흡착)

  • Son, Won Keun;Kim, Hyun Suk;Park, Soo Gil
    • Applied Chemistry for Engineering
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    • v.10 no.5
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    • pp.666-671
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    • 1999
  • In this work, sulfonated poly(phenylene sulfide) (SPPS) was prepared by demethylation with aqueous NaOH solution after poly[methyl[4-(phenylthio)phenyl]sulfonium trifluoromethanesulfonate](PPST) was sulfonated with fumic sulfonic acid(10% $SO_{3}-H_{2}SO_{4}$). PPST soluble in organic solvents was synthesiszed by self-condensation polymerization of methyl-(phenylthio)phenyl sulfoxide(MPPSO). SPPS showed IR bands of asymmetric O=S=O stretching at $1200cm^{-1}$ and S-O stretching at $621cm^{-1}$ from $-SO_{3}H$ group. From the result, it could be known that sulfonic acid groups were introduced to poly(phenylene sulfide). when PPST was sulfonated for 12hr at $150^{\circ}C$, 1.48 sulfonic acid groups were introduced per repeat unit. The weight average molecular weight(Mw) of PPST and SPPS determined by high temperature GPC were 118323 and 131204, respectively. The SPPS exhibited adsorption capacity of ammonia gas $9.67mmol\;NH_{3}/g$ and it was much higher than that of active carbon or silica gel.

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The Effect of Diamine and Solvent on The Synthesis of Polyimides and Their Film Properties (폴리이미드의 합성과 필름의 물성에 미치는 디아민과 용매의 효과)

  • Choi, Hyeong-Ki;Lee, Ho-Sik;Chung, Chang-Nam;Kim, Jum-Sik
    • Applied Chemistry for Engineering
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    • v.2 no.3
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    • pp.253-261
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    • 1991
  • Polyamic acids, precursor polymers of polyimides have been obtained by the solution polycondensation of benzophenone tetracarboxylic dianhydride (BTDA) with 4, 4'-diamino diphenyl methane (MDA) and/or 3, 3'-dimethyl benzidine (OTB). The reaction was carried in two solvent systems such as m-cresol and m-cresol/xylene mixture. The results of TGA analysis showed that the polyimide films had good thermal stability with the initial decomposition temperature ranging from $540^{\circ}$ to $590^{\circ}$. According to DSC analysis of polymers, the glass transition temperature was over $340^{\circ}$. Polyimide film samples, showed good mechanical and electrical properties, had over $16Kg/mm^2$ of tensile strength and about 200 KV/mm of dielectric breakdown voltage. The properties of the copolymer from MAD/OTB were better than those of the homopolymer from MDA. And the polymer synthesized in m-cresol had lower properties than that obtained in m-cresol/xylene.

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Polymerization and Thermal Characteristics of Acrylonitrile/Dicyclohexylammonium 2-Cyanoacrylate Copolymers for Carbon Fiber Precursors

  • Kim, Ki-Young;Park, Woo-Lee;Chung, Yong-Sik;Shin, Dong-Geun;Han, Jin-Wook
    • Carbon letters
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    • v.12 no.1
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    • pp.31-38
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    • 2011
  • This study experimentally investigated dicyclohexylammonium 2-cyanoacrylate (CA) as a potential comonomer for polyacrylonitrile (PAN) based carbon fiber precursors. The P(AN-CA) copolymers with different CA contents (0.19-0.78 mol% in the feed) were polymerized using solution polymerization with 2,2-azobis(isobutyronitrile) as an initiator. The chemical structure and composition of P(AN-CA) copolymers were determined by proton nuclear magnetic resonance and elemental analysis, and the copolymer composition was similar to the feeding ratio of the monomers. The effects of CA comonomer on the thermal properties of its copolymers were characterized differential scanning calorimetry (DSC) in nitrogen and air atmospheres. The DSC curves of P(AN-CA) under nitrogen atmosphere indicated that the initiation temperature for cyclization of nitrile groups was reduced to around $235^{\circ}C$. The heat release and the activation energy for cyclization reactions were decreased in comparison with those of PAN homopolymers. On the other hand, under air atmosphere, the P(AN-CA) with 0.78 mol% CA content showed that the initiation temperature of cyclization was significantly lowered to $160.1^{\circ}C$. The activation energy value showed 116 kJ/mol, that was smaller than that of the copolymers with 0.82 mol% of itaconic acids. The thermal stability of P(AN-CA), evidenced by thermogravimetric analyses in air atmosphere, was found higher than PAN homopolymer and similar to P(AN-IA) copolymers. Therefore, this study successfully demonstrated the great potential of P(AN-CA) copolymers as carbon fiber precursors, taking advantages of the temperature-lowering effects of CA comonomers and higher thermal stability of the CA copolymers for the stabilizing processes.

An Antifungal Antibiotic Purified from Bacillus megaterium KL39, a Biocontrol Agent of Red-Pepper Phytophthora-Blight Disease

  • JUNG HEE KYOUNG;KIM SANG-DAL
    • Journal of Microbiology and Biotechnology
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    • v.15 no.5
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    • pp.1001-1010
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    • 2005
  • Bacillus megaterium KL39, an antibiotic-producing plant growth promoting rhizobacterium (PGPR), was selected from soil. The antifungal antibiotic, denoted KL39, was purified from culture filtrate by column chromatography using Dion HP-20, Silica gel, Sephadex LH-20, and prep-HPLC. Thin layer chromatography, employing the solvent system of ethanol:ammonia:water=8:1:1, showed the $R_{f}$. value of 0.32. The antibiotic KL39 showed a negative reaction with ninhydrin solution, positive with iodine vapor, and also positive with Ehrlich reagent. It was soluble in methanol, ethanol, butanol, and acetonitrile, but insoluble in chloroform, toluene, hexane, ethyl ether, or acetone. Its UV spectrum had the maximum absorption at 208 nm. Amino acid composition, FAB-mass, $^{1}H-NMR,\;^{13}C-NMR$, and atomic analyses showed that the antibiotic KL39 (MW=1,071) has a structure very similar to iturin E. The antibiotic KL39 has a broad antifungal spectrum against a variety of plant pathogenic fungi including Rhizoctonia solani, Pyricularia oryzae, Monilinia froeticola, Botrytis cinenea, Altenaria kikuchiana, Fusarium oxysporum, and F. solani. An MIC value of $10\;{\mu}g/ml$ was determined for Phytophthora capsici. Macromolecular incorporation studies with P. capsici using radioactive [$^{3}H-adenine$] as the precursor, indicated that the antibiotic KL39 strongly inhibits the DNA biosynthesis of the fungal cell. Microscopic observation of the antifungal action showed abnormal hyphal swelling of P. capsici. The purified antibiotic KL39 was very effective for the biocontrol of in vivo Phytophthora-blight disease of pepper.

Synthesis of Pt@TiO2 Nano-composite via Photochemical Reduction Method (광화학 환원방법을 이용한 Pt@TiO2 나노 복합체 합성)

  • Kim, Ji Young;Byun, Jong Min;Kim, Jin Woo;Kim, Young Do
    • Journal of Powder Materials
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    • v.21 no.2
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    • pp.119-123
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    • 2014
  • Pt has been widely used as catalyst for fuel cell and exhausted gas clean systems due to its high catalytic activity. Recently, there have been researches on fabricating composite materials of Pt as a method of reducing the amount of Pt due to its high price. One of the approaches for saving Pt used as catalyst is a core shell structure consisting of Pt layer on the core of the non-noble metal. In this study, the synthesis of Pt shell was conducted on the surface of $TiO_2$ particle, a non-noble material, by applying ultraviolet (UV) irradiation. Anatase $TiO_2$ particles with the average size of 20~30 nm were immersed in the ethanol dissolved with Pt precursor of $H_2PtCl_6{\cdot}6H_2O$ and exposed to UV irradiation with the wavelength of 365 nm. It was confirmed that Pt nano-particles were formed on the surface of $TiO_2$ particles by photochemical reduction of Pt ion from the solution. The morphology of the synthesized Pt@$TiO_2$ nano-composite was examined by TEM (Transmission Electron Microscopy).