• Bulletin of the Korean Chemical Society
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• v.27 no.10
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• pp.1572-1576
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• 2006

A dimeric precursor, $[Cu(dmae)(OCOCH_3)(H_2O)]_2$ for the CVD of copper metal films, (dmaeH = N,N-dimethylaminoethanol) was synthesized by the reaction of copper(II) acetate monohydrate ($Cu(OCOCH_3)_2{\cdot}H_2O$) and dmaeH in toluene. The product was characterized by m.p. determination, elemental analysis and X-ray crystallography. Molecular structure of $[Cu(dmae)(OCOCH_3)(H_2O)]_2$ shows that a dimeric unit $[Cu(dmae)(OCOCH_3)(H_2O)]_2$ is linked to another through hydrogen bond and it undergoes facile decomposition at 300 C to deposit granular copper metal film under nitrogen atmosphere. The decomposition temperature, thermal behaviour, kinetic parameters, evolved gas pattern of the complex, morphology, and the composition of the film were also investigated.

• Journal of Powder Materials
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• v.14 no.1 s.60
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• pp.19-25
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• 2007

This study was focused on the optimization of low-pressure ultrasonic spraying process for synthesis of pure ${\gamma}-Fe_2O_3$ nanoparticles. As process variables, pressure in the reactor, precursor concentration, and reaction temperature were changed in order to control the chemical and microstructural properties of iron oxide nanoparticles including crystal phase, mean particle size and particle size distribution. X-ray diffraction (XRD) and transmission electron microscopy (TEM) studies revealed that pure ${\gamma}-Fe_2O_3$ nanoparticles with narrow particle size distribution of 5-15 nm were successfully synthesized from iron pentacarbonyl ($Fe(CO)_{5}$) in hexane under 30 mbar with precursor concentrations of 0.1M and 0.2M, at temperatures over $800^{\circ}C$. Also magnetic properties, coercivity ($H_c$) and saturation magnetization ($M_s$) were reported in terms of the microstructure of particles based on the results from vibration sampling magnetometer (VSM).

• Korean Journal of Materials Research
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• v.21 no.1
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• pp.67-71
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• 2011

La doped CuO-ZnO-$Al_2O_3$ powders are prepared by sol-gel method with aluminum isopropoxide and primary distilled water as precursor and solvent. In this synthesized process, the obtained metal oxides caused the precursor such as copper (II) nitrate hydrate and zinc (II) nitrate hexahydrate were added. To improve the surface areas of La doped CuO-ZnO-$Al_2O_3$ powder, sorbitan (z)-mono-9-octadecenoate (Span 80) was added. The synthesized powder was calcined at various temperatures. The dopant was found to affect the surface area and particle size of the mixed oxide, in conjunction with the calcined temperature. The structural analysis and textual properties of the synthesized powder were measured with an X-ray Diffractometer (XRD), a Field-Emission Scanning Electron Microscope (FE-SEM), Bruner-Emmett-Teller surface analysis (BET), Thermogravimetry-Differential Thermal analysis (TG/DTA), $^{27}Al$ solid state Nuclear Magnetic Resonance (NMR) and transform infrared microspectroscopy (FT-IR). An increase of surface area with Span 80 was observed on La doped CuO-ZnO-$Al_2O_3$ powders from $25m^2$/g to $41m^2$/g.

• Proceedings of the IEEK Conference
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• 2001.10a
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• pp.240-244
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• 2001

Recycling process involving mechanical, thermal, hydrometallurgical, and sol-gel step has been applied to recover cobalt and lithium from spent lithium ion batteries and to synthesize LiCoO$_2$from leach liquor as cathodic active materials. Electrode materials containing lithium and cobalt could be concentrated with 2-step thermal and mechanical treatment. Leaching behaviors of the lithium and cobalt in nitric acid media was investigated in terms of reaction variables. Hydrogen peroxide in 1 M HNO$_3$solution turned out to be an effective reducing agent by enhancing the leaching efficiency. O f many possible processes to produce LiCoO$_2$, the amorphous citrate precursor process (ACP) has been applied to synthesize powders with a large specific surface area and an exact stoichiometry. After leaching used LiCoO$_2$with nitric acid, the molar ratio of Li/Co in the leach liquor was adjusted at 1.1 by adding a fresh LiNO$_3$solution. Then, 1 M citric acid solution at a 100% stoichiometry was also added to prepare a gelatinous precursor. When the precursor was calcined at 95$0^{\circ}C$ for 24 hr, purely crystalline LiCoO$_2$was successfully obtained. The particle size and specific surface area of the resulting crystalline powders were 20 пm and 30 $\textrm{cm}^2$/g, respectively The LiCoO$_2$powder was proved to have good characteristics as cathode active materials in charge/discharge capacity and cyclic performance.

• Bulletin of the Korean Chemical Society
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• v.31 no.1
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• pp.47-51
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• 2010

A powder, containing 80 percent of blue cobalt aluminate $(CoAl_2O_4)$ crystallites, was synthesized at $210 ^{\circ}C$ using a (metal nitrate-malonic acid-ammonium hydroxide-ammonium nitrate) system. The optimal amount of concentrated ammonia water and initial decomposition temperature were determined for the blue $CoAl_2O_4$ crystallites preparation. Three $CoAl_2O_4$ precursor pastes, corresponding to the various amounts of concentrated ammonia water, were prepared by evaporating the initial solutions in an electric furnace fixed at $80 ^{\circ}C$ under a vacuum of 25 torr. The initial solution was used to dissolve the starting materials. The powder with the maximum content (80%) of blue $CoAl_2O_4$ crystallites was prepared when the prepared precursor was decomposed at $210 ^{\circ}C$. The blue $CoAl_2O_4$ crystallite content in the prepared sample decreased with increasing initial decomposition temperature. For 0.2 mole of the $Al^{3+}$ ion, the chemical compositions of the precursor corresponded to molar ratios of 0.4, 1.40, 2.56 and 2.00 for the $Co^{2+}$ ion, malonic acid, ammonia and ammonium nitrate per mole of the $Al^{3+}$ ion, respectively. The blue $CoAl_2O_4$ crystallite content in the sample decreased with the amount of ammonia deviated from the optimal value. The characteristics of the powders were examined using X-ray diffraction, optical microscopy, Fourier transformation infrared spectroscopy and the Brunauer-Emmett-Teller technique.

• Korean Journal of Materials Research
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• v.20 no.3
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• pp.142-147
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• 2010

Nano-sized $BaNd_2Ti_5O_{14}$ powders were prepared by the spray pyrolysis process. Sucrose used as the organic additive enabled the formation of nano-sized $BaNd_2Ti_5O_{14}$ powders. The powders prepared from the spray solution without sucrose had a spherical shape, dense structure and micron size before and after calcination. However, the precursor powders prepared from the spray solution with sucrose had a large size, and hollow and porous morphology. The precursor powders had an amorphous crystal structure because of the short residence time of the powders inside the hot wall reactor. The complete decomposition of sucrose did not occur inside the hot wall reactor. Therefore, the precursor powders obtained from the spray solution with sucrose of 0.5M had a carbon content of 39.2wt.%. The powders obtained from the spray solution with sucrose of 0.5M had a slightly aggregated structure of nano-sized primary powders of $BaNd_2Ti_5O_{14}$ crystalline phase after calcination at $1000^{\circ}C$. The calcined powders turned into nano-sized $BaNd_2Ti_5O_{14}$ powders after milling. The mean size of the $BaNd_2Ti_5O_{14}$ powders was 125 nm.

• Korean Journal of Materials Research
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• v.21 no.10
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• pp.568-572
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• 2011

The preparation of $Y_2O_3$-doped $ZrO_2$ nanoparticles in Igepal CO-520/cyclohexane reverse micelle solutions is studied here. In this work, we synthesized nanosized $Y_2O_3$-doped $ZrO_2$ powders in a reverse micelle process using aqueous ammonia as the precipitant. In this way, a hydroxide precursor was obtained from nitrate solutions dispersed in the nanosized aqueous domains of a microemulsion consisting of cyclohexane as the oil phase, with poly (oxyethylene) nonylphenylether (Igepal CO-520) as the non-ionic surfactant. The synthesized and calcined powders were characterized by thermogravimetrydifferential thermal analysis (TGA-DTA), X-ray diffraction analysis (XRD) and transmission electron microscopy (TEM). The crystallite size was found to nearly identical with an increase in the water-to-surfactant (R) molar ratio. A FTIR analysis was carried to monitor the elimination of residual oil and surfactant phases from the microemulsion-derived precursor and the calcined powder. The average particle size and distribution of the synthesized $Y_2O_3$-doped $ZrO_2$ were below 5 nm and narrow, respectively. The TG-DTA analysis showed that the phase of the $Y_2O_3$-doped $ZrO_2$ nanoparticles changes from the monoclinic phase to the tetragonal phase at temperatures close to $530^{\circ}C$. The phase of the synthesized $Y_2O_3$-doped $ZrO_2$ when heated to $600^{\circ}C$ was tetragonal $ZrO_2$.

• Journal of the Korean Electrochemical Society
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• v.18 no.1
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• pp.17-23
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• 2015

$Li_4Ti_5O_{12}$ (LTO) have attracted much attention of researchers in the field of energy storage, because of their excellent stability for electric vehicle application. A main drawback of LTO is however their insulating nature due to the wide bandgap, which should be addressed to enhance the battery performance. In this study, we investigated the effect of water solubility of dopant precursor on the electrochemical characteristics of conducting LTO prepared by doping with $Cr^{3+}$ ions with the well-known wet-mixing method. The solubility of dopant precursor directly affected the morphology and the phase of doped LTO, and therefore their battery performance. In the case of employing the most soluble dopant precursor, $Cr(NO_3)_2$, the doped LTO demonstrated a markedly enhanced discharge capacity at high C-rate (130mAh/g @ 10C), which is about 2 times higher value than that of bare LTO.

• Korean Journal of Materials Research
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• v.26 no.8
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• pp.430-437
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• 2016

Aluminum oxide ($Al_2O_3$) thin films were grown by atomic layer deposition (ALD) using a new Al metalorganic precursor, dimethyl aluminum sec-butoxide ($C_{12}H_{30}Al_2O_2$), and water vapor ($H_2O$) as the reactant at deposition temperatures ranging from 150 to $300^{\circ}C$. The ALD process showed typical self-limited film growth with precursor and reactant pulsing time at $250^{\circ}C$; the growth rate was 0.095 nm/cycle, with no incubation cycle. This is relatively lower and more controllable than the growth rate in the typical $ALD-Al_2O_3$ process, which uses trimethyl aluminum (TMA) and shows a growth rate of 0.11 nm/cycle. The as-deposited $ALD-Al_2O_3$ film was amorphous; X-ray diffraction and transmission electron microscopy confirmed that its amorphous state was maintained even after annealing at $1000^{\circ}C$. The refractive index of the $ALD-Al_2O_3$ films ranged from 1.45 to 1.67; these values were dependent on the deposition temperature. X-ray photoelectron spectroscopy showed that the $ALD-Al_2O_3$ films deposited at $250^{\circ}C$ were stoichiometric, with no carbon impurity. The step coverage of the $ALD-Al_2O_3$ film was perfect, at approximately 100%, at the dual trench structure, with an aspect ratio of approximately 6.3 (top opening size of 40 nm). With capacitance-voltage measurements of the $Al/ALD-Al_2O_3/p-Si$ structure, the dielectric constant of the $ALD-Al_2O_3$ films deposited at $250^{\circ}C$ was determined to be ~8.1, with a leakage current density on the order of $10^{-8}A/cm^2$ at 1 V.

• Carbon letters
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• v.10 no.3
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• pp.217-220
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• 2009

In this study, porous electrospun carbon fibers were prepared by electrospinning with PAN and $MgCl_2$, as a MgO precursor. MgO was selected as a substrate because of its chemical and thermal stability, no reaction with carbon, and ease of removal after carbonization by dissolving out in acidic solutions. $MgCl_2$ was mixed with polyacrylonitrile (PAN) solution as a precursor of MgO with various weight ratios of $MgCl_2$/PAN. The average diameter of porous electrospun carbon fibers increased from 1.3 to 3 ${\mu}m$, as the $MgCl_2$ to PAN weight ratio increased. During the stabilization step, $MgCl_2$ was hydrolyzed to MgOHCl by heat treatment. At elevated temperature of 823 K for carbonization step, MgOHCl was decomposed to MgO. Specific surface area and pore structure of prepared electrospun carbon fibers were decided by weight ratio of $MgCl_2$/PAN. The amount of hydrogen storage increased with increase of specific surface area and micropore volume of prepared electrospun carbon fibers.