• Title/Summary/Keyword: Precursor analysis

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Synthesis of Perforated Polygonal Cobalt Oxides using a Carbon Nanofiber Template (탄소나노섬유 모형을 이용한 천공된 다각형 코발트 산화물 합성)

  • Sin, Dong-Yo;An, Geon-Hyoung;Ahn, Hyo-Jin
    • Journal of Powder Materials
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    • v.22 no.5
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    • pp.350-355
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    • 2015
  • Perforated polygonal cobalt oxide ($Co_3O_4$) is synthesized using electrospinning and a hydrothermal method followed by the removal of a carbon nanofiber (CNF) template. To investigate their formation mechanism, thermogravimetric analysis, field-emission scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy are examined. To obtain the optimum condition of perforated polygonal $Co_3O_4$, we prepare three different weight ratios of the Co precursor and the CNF template: sample A (Co precursor:CNF template- 10:1), sample B (Co precursor:CNF template-3.2:1), and sample C (Co precursor:CNF template-2:1). Among them, sample A exhibits the perforated polygonal $Co_3O_4$ with a thin carbon layer (5.7-6.2 nm) owing to the removal of CNF template. However, sample B and sample C synthesized perforated round $Co_3O_4$ and destroyed $Co_3O_4$ powders, respectively, due to a decreased amount of Co precursor. The increased amount of the CNF template prevents the formation of polygonal $Co_3O_4$. For sample A, the optimized weight ratio of the Co precursor and CNF template may be related to the successful formation of perforated polygonal $Co_3O_4$. Thus, perforated polygonal $Co_3O_4$ can be applied to electrode materials of energy storage devices such as lithium ion batteries, supercapacitors, and fuel cells.

Synthesis of CuO nanoparticles by liquid phase precursor process (액상프리커서법에 의한 산화구리(CuO) 나노 입자의 합성)

  • Seong-Whan Shinn
    • The Journal of the Convergence on Culture Technology
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    • v.9 no.6
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    • pp.855-859
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    • 2023
  • Copper oxide (CuO) nanoparticles were successfully synthesized using a precursor in which industrial starch was impregnated with an aqueous solution of copper (II) nitrate trihydrate. The microstructure of the precursor impregnated with an aqueous solution of copper nitrate trihydrate was confirmed with a scanning electron microscope (SEM), and the particle size and the crystal structure of the copper oxide particles produced as the temperature of the heat treatment of the precursor increased was analyzed by X-ray diffraction (XRD) and the scanning electron microscope (SEM). As a result of the analysis, it was confirmed that the temperature at which the organic matter of the precursor is completely thermally decomposed is 450-490℃, and that the size and crystallinity of the copper oxide particles increased as the heat treatment temperature increased. The size of the copper oxide particles obtained through heat treatment at 500-800℃ during 1 hour was 100nm~2㎛. It was confirmed that the copper oxide crystalline phase is formed at a heat treatment temperature of 400℃, and only the copper oxide single phase existed up to 800℃. And it was also confirmed that the size of particles produced increased as the calcination temperature increased.

Synthesis and Characterization of Si-C-N Precursor by Using Chemical Vapor Condensation Method (화학기상응축법을 이용한 Si-C-N Precursor 분말의 합성 및 특성평가)

  • Kim, Hyoung-In;Kim, Dae-Jung;Hong, Jin-Seok;So, Myoung-Gi
    • Journal of the Korean Ceramic Society
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    • v.39 no.8
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    • pp.783-788
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    • 2002
  • In this study, nano-sized Si-C-N precursor powders were synthesized by Chemical Vapor Condensation Method(CVC) using TMS(Tetramethylsilane: Si($CH_3)_4$), $NH_3$ and $H_2$ gases under the various reaction conditions of the reaction temperature, TMS/$NH_3$ ratio and TMS/$H_2$ ratio. XRD and FESEM were used to analysis the crystalline phase and the average particle size of the synthesized powders. It was found that the obtained powders under the considering conditions were all spherical amorphous powder with the particle size of 87∼130 nm. The particle size was decreased as the reaction temperature increased and TMS/$NH_3$ and TMS/$H_2$ ratio decreased. As the results of EA analysis, it was found that the synthesized powders had been formed the powders composed of Si, N, C and H. Through FT-IR results, it was found that the synthesized powders were Si-C-N precursor powders with Si-C, Si-N and C-N bonds.

Morphological optimization of process parameters of randomly oriented carbon/carbon composite

  • Raunija, Thakur Sudesh Kumar;Manwatkar, Sushant Krunal;Sharma, Sharad Chandra;Verma, Anil
    • Carbon letters
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    • v.15 no.1
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    • pp.25-31
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    • 2014
  • A microstructure analysis is carried out to optimize the process parameters of a randomly oriented discrete length hybrid carbon fiber reinforced carbon matrix composite. The composite is fabricated by moulding of a slurry into a preform, followed by hot-pressing and carbonization. Heating rates of 0.1, 0.2, 0.3, 0.5, 1, and $3.3^{\circ}C/min$ and pressures of 5, 10, 15, and 20 MPa are applied during hot-pressing. Matrix precursor to reinforcement weight ratios of 70:30, 50:50, and 30:70 are also considered. A microstructure analysis of the carbon/carbon compacts is performed for each variant. Higher heating rates give bloated compacts whereas low heating rates give bloating-free, fine microstructure compacts. The compacts fabricated at higher pressure have displayed side oozing of molten pitch and discrete length carbon fibers. The microstructure of the compacts fabricated at low pressure shows a lack of densification. The compacts with low matrix precursor to reinforcement weight ratios have insufficient bonding agent to bind the reinforcement whereas the higher matrix precursor to reinforcement weight ratio results in a plaster-like structure. Based on the microstructure analysis, a heating rate of $0.2^{\circ}C/min$, pressure of 15 MPa, and a matrix precursor to reinforcement ratio of 50:50 are found to be optimum w.r.t attaining bloating-free densification and processing time.

Characterization of $Cu_2ZnSnSe_4$ thin film produced by selenization of metallic precursor (금속 프리커서의 셀렌화에 의한 $Cu_2ZnSnSe_4$ 박막의 특성)

  • Amal, M. Ikhlasul;Alfaruqy, M. Hilmy;Jang, Yun-Jung;Kim, Kyoo Ho
    • 한국신재생에너지학회:학술대회논문집
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    • 2010.06a
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    • pp.85.2-85.2
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    • 2010
  • $Cu_2ZnSnSe_4$ (CZTSe) is one of candidate to alternate $Cu(In,Ga)Se_2$ as solar absorber material for solar cell. The expensive elements of In and Ga are replaced by Zn and Sn, respectively to lower the material cost. In this study we fabricated CZTSe thin film by selenization of single precursor layer consisted metallic constituent. Precursor compositions ratio were selected to have Cu-poor and Zn-rich content and prepared by RF magnetron sputtering. Thermal processing was applied to introduce selenium into as-deposited films at temperatures ranging from 350 to 500 for time up to 120 minutes. Single precursor films showed amorphous structure and consist of individual elements of Cu, Zn, and Sn. It was confirmed by XRD analysis that synthesis of CZTSe compound is occurred from lower temperature process, although concurrently additional phases such as binary cooper selenides are also existed. The quality of CZTSe crystal was improved as temperature increased. We also investigated the optical and electrical properties of as-selenized CZTSe as well.

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Chemical Vapor Deposition of β-LiGaO2 Films on Si(100) Using a Novel Single Precursor

  • Sung, Myung M.;Kim, Chang G.;Kim, Yun-Soo
    • Bulletin of the Korean Chemical Society
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    • v.25 no.4
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    • pp.480-484
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    • 2004
  • $LiGaO_2$ films have been grown on Si (100) substrates using a new single precursor $[Li(OCH_2CH_2OCH_3)_2-Ga(CH_3)_2]_2$ under high vacuum conditions $(5{\times}10^{-6}Torr)$. The $[Li(OCH_2CH_2OCH_3)_2Ga(CH_3)_2]_2$ was synthe-sized and characterized by using spectroscopic methods and single-crystal X-ray diffraction analysis. The chemical composition, crystalline structure, and morphology of the deposited films were investigated by X-ray photoelectron spectroscopy, X-ray diffraction, and scanning electron microscopy. The results show that polycrystalline $LiGaO_2$ films preferentially oriented in the [010] direction can be deposited on Si (100) at 500-550$^{\circ}C$ by metal organic chemical vapor deposition (MOCVD). The single precursor $[LiOCH_2CH_2OCH_3)_2-Ga(CH_3)_2]_2$ has been found suitable for chemical vapor deposition of $LiGaO_2$ thin films on Si substrates.

Preparation of SnS Thin Films by MOCVD Method Using Single Source Precursor, Bis(3-mercapto-1-propanethiolato) Sn(II)

  • Park, Jong-Pil;Song, Mi-Yeon;Jung, Won-Mok;Lee, Won-Young;Lee, Jin-Ho;Kim, Hang-Geun;Shim, Il-Wun
    • Bulletin of the Korean Chemical Society
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    • v.33 no.10
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    • pp.3383-3386
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    • 2012
  • SnS thin films were deposited on glasses through metal organic chemical vapor deposition (MOCVD) method at relatively mild conditions, using bis(3-mercapto-1-propanethiolato) tin(II) precursor without toxic $H_2S$ gas. The MOCVD process was carried out in the temperature range of $300-400^{\circ}C$ and the average grain size in fabricated SnS films was about 500 nm. The optical band gap of the SnS film was about 1.3 eV which is in optimal range for harvesting solar radiation energy. The precursor and SnS films were characterized through infrared spectroscopy, nuclear magnetic resonance spectroscopy, DIP-EI mass spectroscopy, elemental analyses, thermal analysis, X-ray diffraction, and field emission scanning electron microscopic analyses.

PhaseTransformation of PbO-Precursor Prepared from Lead Nitrate (질산납으로부터 제조된 PbO-전구체의 산변태)

  • Choe, Byeong-Cheol;Lee, Mun-Ho
    • Korean Journal of Materials Research
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    • v.4 no.4
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    • pp.472-476
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    • 1994
  • Phase transformation of PbO-precursor prepared from $Pb(NO_{3})_{2}$ by precipitation technique was observed by TG-DTA, XRD, FT-IR, and Raman spectral analysis. PbO-precursor was derived from an aqueous solution of $Pb(NO_{3})_{2}$ at $45^{\circ}C$ and pH of 9.0. The precipitate showed it to be the mixture of hydrous lead oxynitrate and lead hydroxynitrate. With increasing heat-treatment temperature ranging up to $560^{\circ}C$, the precursor changed to $3Pb(NO_{3})_{2}$ . 7Pb0, $Pb(NO_{3})_{2}$. 5Pb0 and PbO(litharge), in turn. Finally, it transformed to massicot form of PbO above $560^{\circ}C$.

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Preparation and Characterization of Mesophase Pitches as a Matrix Precursor of Carbon Fiber Reinforced Carbon Composite (탄소/탄소 복합재 매트릭스 전구체로서의 메조페이스 핏치의 제조 및 특성에 관한 연구)

  • 정현진;임연수
    • Journal of the Korean Ceramic Society
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    • v.33 no.12
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    • pp.1387-1393
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    • 1996
  • A study on mesophase pitch as a matrix precursor of carbon fiber reinforced carbon (C/C) composite has been recently presented. This study is concerned with the production of mesophase pitch as matrix precursors for C/C composite from coal tar pitch. A commercial coal tar pitch was heat-treated at 25$0^{\circ}C$ for 2 hours to remove low molecular weight fraction from the pitch then increasing the temperature of the pitch to between 350~45$0^{\circ}C$ to produce mesophase pitch. The pitch was continuously stirred during this time and nitrogen gas was continuously bubbled through the pitch. Spherical and bulk mesophases were formed in the pitch after heat-treatment,. Parent and mesophae pitches were characterized by elemental analysis coke yield solubi-lity in tetrahydrofuran and hexane and an optical microscopy to measure the mesiophase content. It was neces-sary to produce C/C composite that a mesophase pitch with about 30-40 vol% mesophase spherulites can be infiltrated into a fiber preform without a filter effect as a matrix precursor conditions. This condition was satisfied with mesophase pitch heat treated at 40$0^{\circ}C$ for 2 hours. The other heat treatment conditions showed the nuclei of mesophase or bulk mesophae which were not satisfied with the matix precursor condition.

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Pyrolytic Conversion of Blended Precursors into Ti-Al-N Ceramic Composites

  • Cheng, Fei;Sugahara, Yoshiyuki;Kuoda, Kazuyuki
    • The Korean Journal of Ceramics
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    • v.6 no.1
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    • pp.32-36
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    • 2000
  • Pyrolytic preparations of Ti-Al-N ceramics from three blended precursors were investigated. The precursors were prepared stirring ($HA1N^{i}Pr_m$ and an aminolysis product of $Ti(NMe_2)_4$ with $MeHNCH_2CH_2$NHMe in $C_6/H_6$ . IR and $^1H\;NMR $analyses suggested that essentially no Ti-N-Al bonds were present in the precursors. Pyrolysis of the precursors under $NH_3-N_2$led to the formation of brown solids with ceramic yields of about 30%, and the Ti-Al ratios in the pyrolyzed products were close to those of the precursors. XRD analysis of the pyrolyzed product from the precursor with Ti:Al=5:1 indicated the formation of a NaCl-type compound as the only crystalline phase. Pyrolysis of the precursor with Ti:Al=2:1 led to the formation of AlN besides the major NaCl-type compound. A ceramic composite containing AlN and the NaCl-type compound was formed by pyrolysis of the precursor with Ti:Al=1:2.

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