• Title/Summary/Keyword: Precursor Solution

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Effect of pH on the Synthesis of $LiCoO_2$ with Malonic Acid and Its Charge/Discharge Behavior for a Lithium Secondary Battery

  • Kim, Do Hun;Jeong, Yu Deok;Kim, Sang Pil;Sim, Un Bo
    • Bulletin of the Korean Chemical Society
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    • v.21 no.11
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    • pp.1125-1132
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    • 2000
  • The pH effect of the precursor solution on the preparation of $LiCoO_2$ by a solution phase reaction containing malonic acid was carried out. Layered $LiCoO_2$ powders were obtained with the precursors prepared at the different pHs (4, 7, and 9) and heat-treated at $700^{\circ}C(LiCoO_2-700)$ or $850^{\circ}C(LiCoO_2-850)$ in air. pHs of the media for precursor synthesis affects the charge/discharge and electrochemical properties of the $LiCoO_2electrodes.$ Upon irrespective of pH of the precursor media, X-ray diffraction spectra recorded for $LiCoO_2-850$ powder showed higher peak intensity ratio of I(003)/I(104) than that of $LiCoO_2-700$, since the better crystallization of the former crystallized better. However, $LiCoO_2$ synthesized at pH 4 displayed an abnormal higher intensity ratio of I(003)/I(104) than those synthesized at pH 7 and 9. The surface morphology of the $LiCoO_2-850$ powders was rougher and more irregular than that of $LiCoO_2-700$ made from the precursor synthesized at pH 7 and 9. The $LiCoO_2electrodes$ prepared with the precursors synthesized at pH 7 and 9 showed a better electrochemical and charge/discharge characteristics. From the AC impedance spectroscopic experiments for the electrode made from the precursor prepared in pH 7, the chemical diffusivity of Li ions (DLi+) in $Li0.58CoO_2determined$ was 2.7 ${\times}$10-8 $cm^2s-1$. A cell composed of the $LiCoO_2-700$ cathode prepared in pH 7 with Lithium metal anode reveals an initial discharge specific capacity of 119.8 mAhg-1 at a current density of 10.0 mAg-1 between 3.5 V and 4.3 V. The full-cell composed with $LiCoO_2-700$ cathode prepared in pH 7 and the Mesocarbon Pitch-based Carbon Fiber (MPCF) anode separated by a Cellgard 2400 membrane showed a good cycleability. In addition, it was operated over 100 charge/discharge cycles and displayed an average reversible capacity of nearly 130 mAhg-1.

Synthesis of an Aspartame Precursor Using Thermolysin in Organic Two-Phase System (유기용매 이상계에서 Thermolysin에 의한 아스파탐 전구체 생산)

  • 이인영;안경섭;이선복
    • Microbiology and Biotechnology Letters
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    • v.20 no.1
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    • pp.61-67
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    • 1992
  • The synthesis of N-benzyloxycarbonyl-L-aspartyl-L-phenylalanine methyl ester(ZAPM), a precursor of aspartame, from N-benzyloxycarbonyl-L-aspartic acid(Z-Asp) and L-phenylalanine methyl ester hydrochloride(L-PM-HCl) was investigated in ethylacetate-MES buffer two-phase system using thermolysin. In organic two-phase system, the degree of spontaneous hydrolysis of L-PM. HCl was significantly reduced with increasing the volume ratio of organic to aqueous phase. Stability of thermolysin in organic two-phase system was found to be higher than that in MES buffer solution. More than 90% of initial enzyme activity was maintained after 10 days of incubation in case that the volume of organic phase was equal to that of buffer phase, while the half life of thermolysin was about 2 days in aqueous buffer solution. The results of partitioning of substrates and product in organic two-phase system showed that the difference in partition coefficients between substrates and product was maximum at pH 5.5. The optimal pH for 2-APM synthesis in organic two-phase system was found to be 5.5-5.8, which is consistent with the value expected from the partition experiments. As the concentration of substrates was increased the conversion yield of Z-APM was increased with concomitant reduction of L-PMqHC1 hydrolysis. In case that the concentration of L-PM-HCl and Z-Asp were 160 mM and 80 mM respectively, the conversion yield of Z-APM reached 90% after 28 hrs of reaction. The yield obtained at different volume ratio of organic phase compares well with the predicted equilibrium constant in biphasic system.

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Preparation of GdBCO Thin Film by Ex-situ Process using Nitrate Precursors (질산염 전구체 원료로 Ex-situ 공정에 의한 GdBCO 박막 제조)

  • Kim, Byeong-Joo;Lee, Chul-Sun;Lee, Jong-Beom;Lee, Jae-Hun;Moon, Seung-Hyun;Lee, Hee-Gyoun;Hong, Gye-Won
    • Progress in Superconductivity
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    • v.13 no.2
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    • pp.127-132
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    • 2011
  • Many research groups have been manufacturing coated conductor by various processes such as PLD, MOD, and MOCVD, but the methods with production cost suitable for wide and massive application of coated conductor did not develop yet. Spray pyrolysis method adopting ultrasonic atomization was tried as one of the possible option. GdBCO precursor films have been deposited on IBAD substrate by spray pyrolysis method at low temperature and converted to GdBCO by post heat treatment. Ultrasonic atomization was used to generate fine droplets from precursor solution of Gd, Ba, and Cu nitrate dissolved in water. Primary GdBCO films were deposited at $500^{\circ}C$ and oxygen partial pressure of 1 torr. After that, the films were converted at various temperatures and low oxygen partial pressures. C-Axis oriented films were obtained IBAD substrates at conversion temperature of around $870^{\circ}C$ and oxygen partial pressures of 500 mtorr ~ 1 torr in a vacuum. Thick c-axis epitaxial film with the thickness of 0.4 ~ 0.5 ${\mu}m$ was obtained on IBAD substrate. C-axis epitaxial GdBCO films were successfully prepared by ex-situ methods using nitrate precursors on IBAD metal substrate. Converted GdBCO films have very dense microstructures with good grain connectivity. EDS composition analysis of the film showed a number of Cu-rich phase in surface. The precursor solution having high copper concent with the composition of Gd : Ba : Cu = 1 : 2 : 4 showed the better grain connectivity and electrical conductivity.

Deposition of YBCO Films on Moving Substrate by a Spray Pyrolysis method (분무 열분해 CVD법으로 이동 중인 LaAlO_3(100) 단결정 위에 증착시킨 YBCO 박막의 특성)

  • Kim, Jae-Gun;Hong, Suk-Kwan;Kim, Ho-Jin;Yu, Seok-Koo;Cho, Han-Woo;Ahn, Jin-Hyun;Joo, Jin-Hoo;Lee, Hee-Gyoun;Hong, Gye-Won
    • Progress in Superconductivity
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    • v.8 no.1
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    • pp.93-97
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    • 2006
  • YBCO films were deposited on a moving substrate by a spray pyrolysis method using nitrate aqueous solution as precursors. Deposition was made on $LaAlO_3$(100) single crystal substrate by spraying precursor droplets generated by a concentric nozzle. The cation ratio of precursor solution was Y:Ba:Cu=1:2.65:4.5. The distance between nozzle and substrate was 15 cm. Substrate was transported with a speed ranging from 0.23 cm/min to 0.5 cm/min. Films were deposited at the pressure ranging from 10 Torr to 20 Torr and the deposition temperature was ranged from $740^{\circ}C\;to\;790^{\circ}C$. Oxygen partial pressure was controlled between 1 Tow and S Torr. Superconducting YBCO films were obtained from $740^{\circ}C\;to\;790^{\circ}C$ with an oxygen partial pressure of 3 Torr. Scanning electron microscope(SEM) and X-ray diffraction(XRD) observation revealed that films are smooth and highly texture with(001) plans parallel to substrate plane. Highest Jc was 0.72 $MA/cm^2$ at 77K and self-field for the film with a thickness of 0.15 m prepared at a substrate temperature of $740^{\circ}C$ and $PO_2$=3 Torr.

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Synthesis of the Water Dispersible L-Valine Capped ZnS:Mn Nanocrystal and the Crystal Structure of the Precursor Complex: [Zn(Val)2(H2O)]

  • Hwang, Cheong-Soo;Lee, Na-Rae;Kim, Young-Ah;Park, Youn-Bong
    • Bulletin of the Korean Chemical Society
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    • v.27 no.11
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    • pp.1809-1814
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    • 2006
  • The L-Valinate anion coordinating zinc complex, [$Zn(val)_2(H-2O)$], was isolated and structurally characterized by single crystal X-ray crystallography. The crystal possess orthorhombic symmetry with a space group $P2_12_12_1$, Z = 4, and a = 7.4279(2)$\AA$, b = 9.4342(2)$\AA$, c =20.5862(7)$\AA$ respectively. The compound features a penta-coordinate zinc ion in which the two valine anion molecules are directly coordinating the central zinc metal ion via their N (amine) and O (carboxylate) atoms, and an additional coordination to zinc is made by water molecule (solvent) to form a distorted square pyramidal structure. In addition, further synthesis of the valine capped ZnS:Mn nanocrystal from the reaction of [$Zn(val)_2(H-2O)$] precursor with $Na_2S$ and 1.95 weight % of $Mn^{2+}$ dopant is described. Obtained valine capped nanocrystal was water dispersible and was optically characterized by UV-vis and solution PL spectroscopy. The solution PL spectrum for the valine capped ZnS:Mn nanocrystal showed an excitation peak at 280 nm and a very narrow emission peak at 558 nm respectively. The measured and calculated PL efficiency of the nanocrystal in water was 15.8%. The obtained powders were characterized by XRD, HR-TEM, and EDXS analyses. The particle size of the nanocrystal was also measured via a TEM image. The measured average particle size was 3.3 nm.

Fabrication of Thin Film Transistors based on Sol-Gel Derived Oxide Semiconductor Layers by Ink-Jet Printing Technology

  • Mun, Ju-Ho;Kim, Dong-Jo;Song, Geun-Gyu;Jeong, Yeong-Min;Gu, Chang-Yeong
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2009.05a
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    • pp.16.1-16.1
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    • 2009
  • We have fabricated solution processed oxide semiconductor active layer for thin film transistors (TFTs). The oxide semiconductor layers were prepared by ink-jet printing the sol-gel precursor solution based on doped-ZnO. Inorganic ZnO-based thin films have drawn significant attention as an active channel layer for TFTs applications alternative to conventional Si-based materials and organic semiconducting materials, due to their wide energy band gap, optical transparency, high mobility, and better stability. However, in spite of such excellent device performances, the fabrication methods of ZnO related oxide active layer involve high cost vacuum processes such as sputtering and pulsed laser deposition. Herein we introduced the ink-jet printing technology to prepare the active layers of oxide semiconductor. Stable sol-gel precursor solutions were obtained by controlling the composition of precursor as well as solvents and stabilizers, and their influences on electrical performance of the transistors were demonstrated by measuring electrical parameters such as off-current, on-current, mobility, and threshold voltage. Microstructure and thermal behavior of the doped ZnO films were investigated by SEM, XRD, and TG/DTA. Furthermore, we studied the influence of the ink-jet printing conditions such as substrate temperature and surface treatment on the microstructure of the ink-jet printed active layers and electrical performance. The mobility value of the device with optimized condition was about 0.1-1.0 $cm^2/Vs$ and the on/off current ratio was about $10^6$. Our investigations demonstrate the feasibility of the ink-jet printed oxide TFTs toward successful application to cost-effective and mass-producible displays.

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Bandgap Control of (AlxGa1-x)2O3 Epilayers by Controlling Aqueous Precursor Mixing Ratio in Mist Chemical Vapor Deposition System (미스트화학기상증착시스템의 전구체 수용액 혼합비 조절을 통한 (AlxGa1-x)2O3 에피박막의 밴드갭 특성 제어 연구)

  • Kim, Kyoung-Ho;Shin, Yun-Ji;Jeong, Seong-Min;Bae, Si-Young
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.32 no.6
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    • pp.528-533
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    • 2019
  • We investigated the growth of $(Al_xGa_{1-x})_2O_3$ thin films on c-plane sapphire substrates that were grown by mist chemical vapor deposition (mist CVD). The precursor solution was prepared by mixing and dissolving source materials such as gallium acetylacetonate and aluminum acetylacetonate in deionized water. The [Al]/[Ga] mixing ratio (MR) of the precursor solution was adjusted in the range of 0~4.0. The Al contents of $(Al_xGa_{1-x})_2O_3$ thin films were increased from 8 to 13% with the increase of the MR of Al. As a result, the optical bandgap of the grown thin films changed from 5.18 to 5.38 eV. Therefore, it was determined that the optical bandgap of grown $(Al_xGa_{1-x})_2O_3$ thin films could be effectively engineered by controlling Al content.

The effect of precursor solution pH on the energy storage performance of 𝛼-MnO2 cathode for zinc-ion batteries synthesized via hydrothermal method (Zn 이온 배터리용 양극 𝛼-MnO2의 수열 합성 시 전구체 용액의 pH가 에너지 저장 성능에 미치는 영향)

  • Sang-Eun Chun
    • Journal of the Korean institute of surface engineering
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    • v.57 no.4
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    • pp.338-347
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    • 2024
  • 𝛼-MnO2 as a cathode material for Zn-ion batteries allows insertion and extraction of Zn ions within its tunnel structure during charge and discharge. The morphology and crystal structure of 𝛼-MnO2 particles critically determine their electrochemical behavior and energy storage performance. In this study, 𝛼-MnO2 was synthesized from precursor solutions under varying pH conditions using a hydrothermal method. The effects of pH values on the morphology, crystal structure, and electrochemical performance were systematically analyzed. The analysis revealed that materials synthesized at higher pH levels exhibited elongated and narrow nanorods with a lower specific surface area. In contrast, those formed at lower pH levels showed shorter, thicker nanorods with a higher specific surface area. This increased surface area at a lower pH enhanced the specific capacitance by providing a greater electrode/electrolyte interfacial area. By contrast, the material synthesized at higher pH conditions demonstrated superior rate capability, attributed to its crystal structure with wider lattice spacings. Wide lattice parameters in the material synthesized at higher pH conditions facilitated easier ion transport than at lower pH levels. Consequently, the study confirms that adjusting the pH of the precursor solution can optimize the electrochemical properties of 𝛼-MnO2 for Zn-ion batteries.