• Title/Summary/Keyword: precursor method.

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Enhanced Electrochemical Properties of All-Solid-State Batteries Using a Surface-Modified LiNi0.6Co0.2Mn0.2O2 Cathode

  • Lim, Chung Bum;Park, Yong Joon
    • Journal of Electrochemical Science and Technology
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    • v.11 no.4
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    • pp.411-420
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    • 2020
  • Undesirable interfacial reactions between the cathode and sulfide electrolyte deteriorate the electrochemical performance of all-solid-state cells based on sulfides, presenting a major challenge. Surface modification of cathodes using stable materials has been used as a method for reducing interfacial reactions. In this work, a precursor-based surface modification method using Zr and Mo was applied to a LiNi0.6Co0.2Mn0.2O2 cathode to enhance the interfacial stability between the cathode and sulfide electrolyte. The source ions (Zr and Mo) coated on the precursor-surface diffused into the structure during the heating process, and influenced the structural parameters. This indicated that the coating ions acted as dopants. They also formed a homogenous coating layer, which are expected to be layers of Li-Zr-O or Li-Mo-O, on the surface of the cathode. The composite electrodes containing the surface-modified LiNi0.6Co0.2Mn0.2O2 powders exhibited enhanced electrochemical properties. The impedance value of the cells and the formation of undesirable reaction products on the electrodes were also decreased due to surface modification. These results indicate that the precursor-based surface modification using Zr and Mo is an effective method for suppressing side reactions at the cathode/sulfide electrolyte interface.

Influence analysis of heat treatment on crystalline structure of ZrO2-SiO2 glass precursor synthesized by sol-gel method (졸-겔법으로 합성된 ZrO2-SiO2 유리전구체의 결정화구조에 미치는 열처리의 영향분석)

  • Chun, Kyung-Soo
    • Analytical Science and Technology
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    • v.25 no.1
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    • pp.3-6
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    • 2012
  • $xZrO_2-(1-x)SiO_2$ glass precursor with relatively high concentration of zirconium propoxide in metal alkoxide solution was obtained by sol-gel method and then heated at various temperature from 500 to $1,100^{\circ}C$ to investigate the effect of the thermal treatment on the crystalline structure of the glass precursor. Based on X-ray diffraction analysis, the crystalline peak was started to develop at temperature higher than $600^{\circ}C$, and the crystalline phase was considerably increased at $850^{\circ}C$ or higher. With increasing the thermal treatment temperature, the characteristic peaks, such as baddelyite, tetragonal-$ZrO_2$ and zircon, was shown at $35^{\circ}$, $50^{\circ}$ and $60^{\circ}$ of $2{\theta}$.

Characteristics of ZnO Nanorod/ZnO/Si(100) Grown by Hydrothermal Method (수열법으로 성장한 ZnO Nanorod/ZnO/Si(100)의 특성)

  • Jeong, Min-Ho;Jin, Yong-Sik;Choi, Sung-Min;Han, Duk-Dong;Choi, Dae-Kue
    • Korean Journal of Materials Research
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    • v.22 no.4
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    • pp.180-184
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    • 2012
  • Nanostructures of ZnO, such as nanowires, nanorods, nanorings, and nanobelts have been actively studied and applied in electronic or optical devices owing to the increased surface to volume ratio and quantum confinement that they provide. ZnO seed layer (about 40 nm thick) was deposited on Si(100) substrate by RF magnetron sputtering with power of 60 W for 5 min. ZnO nanorods were grown on ZnO seed layer/Si(100) substrate at $95^{\circ}C$ for 5 hr by hydrothermal method with concentrations of $Zn(NO_3)_2{\cdot}6H_2O$ [ZNH] and $(CH_2)_6N_4$ [HMT] precursors ranging from 0.02M to 0.1M. We observed the microstructure, crystal structure, and photoluminescence of the nanorods. The ZnO nanorods grew with hexahedron shape to the c-axis at (002), and increased their diameter and length with the increase of precursor concentration. In 0.06 M and 0.08 M precursors, the mean aspect ratio values of ZnO nanorods were 6.8 and 6.5; also, ZnO nanorods had good crystal quality. Near band edge emission (NBE) and a deep level emission (DLE) were observed in all ZnO nanorod samples. The highest peak of NBE and the lower DLE appeared in 0.06 M precursor; however, the highest peak of DLE and the lower peak of NBE appeared in the 0.02 M precursor. It is possible to explain these phenomena as results of the better crystal quality and homogeneous shape of the nanorods in the precursor solution of 0.06 M, and as resulting from the bed crystal quality and the formation of Zn vacancies in the nanorods due to the lack of $Zn^{++}$ in the 0.02 M precursor.

A study on the preparation and analysis of cordierite by sol-gel method (졸-겔법에 의한 코디어라이트 제조와 분석에 관한 연구)

  • Chun, Kyung Soo;Lee, Young Hwan
    • Analytical Science and Technology
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    • v.21 no.2
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    • pp.123-128
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    • 2008
  • The golden turbid solution of cordierite precursor was obtained by using magnesium ethoxide in sol-gel method, while the clear solution of cordierite precursor was obtained when 5%-$Zr(OC_3H_7)_4$ solution was used in the sol-gel reaction. $SiO_2$ component was confirmed by infrared spectra showing $1045cm^{-1}$ and the stretching vibration of gelish $SiO_4$ showed $1140cm^{-1}$ and $940cm^{-1}$. The component of $Al_2O_3$ showed at $580cm^{-1}$ and network structure of $Al_2O_6$ showed at $680cm^{-1}$. The component of MgO was confirmed at $575cm^{-1}$ as the stretching vibration. X-ray diffraction analysis showed ${\mu}$-cordierite crystal was showed up at temperature above $1000^{\circ}C$ at the mole ratio of cordierite precursor and water (1:5). ${\mu}$-Cordierite and ${\alpha}$-cordierite were coexisted at $1050^{\circ}C$ for the mole ratio of cordierite precursor and ammonia (1:5) while ${\alpha}$-cordierite was only existed at $1100^{\circ}C$ for the same mole ratio as mentioned above.

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.

Preparation of Mullite Precursor Using Silicic Acid Extracted by Tetrahydrofuran from Sodium Silicate (규산나트륨으로부터 Tetrahydrofuran으로 추출된 규산을 이용한 Mullite 전구체 제조)

  • 노재성;홍성수;이범재;이병기;박은희;정홍호
    • Journal of the Korean Ceramic Society
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    • v.33 no.8
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    • pp.915-920
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    • 1996
  • Fine mullite precursor was prepared by colloidal sol-gel processes. Aluminum isopropoxide $[Al(i-OC_3H_7)_3]$ as a starting material of $Al_2O_3$ and silicic acid extracted by THF from sodium silicate as a starting material of $SiO_2$ were used. Sodium silicate was first acidified by dilute sulfuric acid to form silicic acid. ; followed by extraction using THF, Mullite precursor was synthesized by sol-gel processes from aluminum isopropoxide and sillicic acid considering the degree of extraction of Si and the removal efficiency of Na. The impurity content of silicic acid extracted by THF was below 0.04% Synthetic mullite precursor consisted of $3Al_2O_3{\cdot}2SiO_2$ and showd spherical particles of $0.05{\mu}m$ diameter and below 0.462% of impurites. The mullite precursor was characterized by EDS, XRD, TG/DSC SEM, FT-IR spectroscopy ICP and TEM.

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Synthesis of Well-Distributed SnO2-Sn-Ag3Sn Nanoparticles in Carbon Nanofibers Using Co-Electrospinning (이중 전기방사법을 이용하여 SnO2-Sn-Ag3Sn 나노 입자가 균일하게 내재된 탄소 나노섬유의 합성)

  • An, Geon-Hyoung;Ahn, Hyo-Jin
    • Korean Journal of Materials Research
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    • v.23 no.2
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    • pp.143-148
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    • 2013
  • Well-distributed $SnO_2$-Sn-$Ag_3Sn$ nanoparticles embedded in carbon nanofibers were fabricated using a co-electrospinning method, which is set up with two coaxial capillaries. Their formation mechanisms were successfully demonstrated. The structural, morphological, and chemical compositional properties were investigated by field-emission scanning electron spectroscopy (FESEM), bright-field transmission electron microscopy (TEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). In particular, to obtain well-distributed $SnO_2$ and Sn and $Ag_3Sn$ nanoparticles in carbon nanofibers, the relative molar ratios of the Ag precursor to the Sn precursor including 7 wt% polyacrylonitrile (PAN) were controlled at 0.1, 0.2, and 0.3. The FESEM, bright-field TEM, XRD, and XPS results show that the nanoparticles consisting of $SnO_2$-Sn-$Ag_3Sn$ phases were in the range of ~4 nm-6 nm for sample A, ~5 nm-15 nm for sample B, ~9 nm-22 nm for sample C. In particular, for sample A, the nanoparticles were uniformly grown in the carbon nanofibers. Furthermore, when the amount of the Ag precursor and the Sn precursor was increased, the inorganic nanofibers consisting of the $SnO_2$-Sn-$Ag_3Sn$ nanoparticles were formed due to the decreased amount of the carbon nanofibers. Thus, well-distributed nanoparticles embedded in the carbon nanofibers were successfully synthesized at the optimum molar ratio (0.1) of the Ag precursor to the Sn precursor after calcination of $800^{\circ}C$.

Preparation of Carbon Films from Polyacrylonitrile@Lignin Composites, and Their Electrical Properties and Adsorption Behavior (폴리아크릴로나이트릴/리그닌 복합소재로부터 생성된 탄소 필름의 전기적 성질 및 흡착 성능)

  • Joonwon Bae
    • Applied Chemistry for Engineering
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    • v.34 no.2
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    • pp.106-110
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    • 2023
  • Lignin is compatible with various polymeric materials and useful as a carbon precursor. In this work, carbon monolith films were produced from polyacrylonitrile (PAN)@lignin precursor films by a controlled carbonization cycle. In addition, their morphological features, electrical properties, and adsorption behavior were analyzed and compared with those of carbonized PAN films. The successful formation of PAN@lignin precursor was confirmed by Fourier-transform infrared (FT-IR) spectroscopy. SEM was used to examine the morphology of precursor and carbonized films, revealing that both precursor and carbonized films retained structural stability following carbonization. A trace of lignin in the carbonized films was also found. The pore structure of the carbonized PAN@lignin film was measured using the BET method, indicating the formation of fairly uniform pores. The electrical properties were also analyzed to obtain the Ohmic relation, which demonstrated that the electrical signal was influenced by incoming materials. Finally, the carbonized PAN@lignin films were useful as adsorbents to remove metal ions. This study provides important information for future initiatives in relevant research fields.

Synthesis of Nickel Oxide (NiO) nanoparticles using nickel(II) nitrate hexahydrate as a precursor (Nickel(II) nitrate hexahydrate를 전구체로 사용한 산화니켈(NiO) 나노입자의 합성)

  • Soo-Jong Kim
    • The Journal of the Convergence on Culture Technology
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    • v.9 no.3
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    • pp.593-599
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    • 2023
  • Nickel oxide (NiO) nanoparticles were successfully synthesized by a simple liquid phase process for producing ceramics powder using a precursor impregnated with a nickel(II) nitrate hexahydrate aqueous solution in an industrial pulp. The microfibrile structure of the precursor impregnated with nickel nitrate hexahydrate aqueous solution was confirmed by scanning electron microscope (SEM), and the crystal structure and particle size of nickel oxide (NiO) particles produced as the heat treatment temperature of the precursor were analyzed by X-ray diffraction (XRD) and SEM. As a result, it was confirmed through XRD and SEM analysis that the temperature at which the organic material of the precursor is completely thermally decomposed was 495-500℃, and the size and crystallinity of the nickel oxide particles produced increased as the heat treatment temperature increased. The size of the nickel oxide particles obtained by heat treatment at 500-800℃ for 1 hour was 50-200 nm. It was confirmed by XRD and SEM analysis that a NiO crystal phase was formed at a heat treatment temperature of 380℃, only a single NiO phase existed until 800℃.

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.