• Journal of the Korean Electrochemical Society
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• v.25 no.3
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• pp.95-104
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• 2022

The development of non-flammable all-solid-state batteries (ASSLBs) has become a hot topic due to the known drawbacks of commercial lithium-ion batteries. As the possibility of applying sulfide solid electrolytes (SSEs) for electric vehicle batteries increases, efforts for the low-cost mass-production are actively underway. Until now, most studies have used high-energy mechanical milling, which is easy to control composition and impurities and can reduce the process time. Through this, various SSEs that exceed the Li⁺ conductivity of liquid electrolytes have been reported, and expectations for the realization of ASSLBs are growing. However, the high-energy mechanical milling method has disadvantages in obtaining the same physical properties when mass-produced, and in controlling the particle size or shape, so that physical properties deteriorate during the full process. On the other hand, wet chemical synthesis technology, which has advantages in mass production and low price, is still in the initial exploration stage. In this technology, SSEs are mainly manufactured through producing a particle-type, solution-type, or mixed-type precursor, but a clear understanding of the reaction mechanism hasn't been made yet. In this review, wet chemical synthesis technologies for SSEs are summarized regarding the reaction mechanism between the raw materials in the solvent.

• Carbon letters
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• v.28
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• pp.31-37
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• 2018

This paper examines a simple one-step and catalyst-free method for synthesizing carbon nanoparticles from aliphatic alcohols and n-hexane with linear molecule formations by using a stable solution plasma process with a bipolar pulse and an external resistor. When the external resistor is adopted, it is observed that the current spikes are dramatically decreased, which induced production of a more stable discharge. Six aliphatic linear alcohols (methanol-hexanol) containing carbon with oxygen sources are studied as possible precursors for the massive production of carbon nanoparticles. Additional study is also carried out with the use of n-hexane containing many carbons without an oxygen source in order to enhance the formation of carbon nanoparticles and to eliminate unwanted oxygen effects. The obtained carbon nanoparticles are characterized with field emission-scanning electron microscopy, energy dispersive X-ray spectroscopy, and Raman spectroscopy. The results show that with increasing carbon ratios in alcohol content, the synthesis rate of carbon nanoparticles is increased, whereas the size of the carbon nanoparticles is decreased. Moreover, the degree of graphitization of the carbon nanoparticles synthesized from 1-hexanol and n-hexane with a high carbon (C)/oxygen (O) ratio and low or no oxygen is observed to be greater than that of the carbon nanoparticles synthesized from the corresponding materials with a low C/O ratio.

• Journal of the Korean Electrochemical Society
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• v.10 no.1
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• pp.48-51
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• 2007

In order to investigate the effects of particle size and specific surface area(BET area) of spinel powder, $LiMn_2O_4$ were synthesized using metal oxide precursor by co-precipitation method(CoP) and solid state reaction (SSR) .X-ray diffraction(XRD) patterns revealed that the both prepared powder has a well developed spinel structure with Fd3m space group. The $LiMn_2O_4$ prepared by co-precipitation showed spherical morphology with narrow size distribution. However, the $LiMn_2O_4$ prepared by solid state reaction showed relatively smaller particles with irregular shape. The measured BET areas of the powers are $0.8m^2g^{-1}$ (CoP) and $3.6m^2g^{-1}$(SSR). The electrochemical performance of the Prepared $LiMn_2O_4$ powders was evaluated using coin type cells(CR2032) at elevated temperature ($55^{\circ}C$). The $LiMn_2O_4$ prepared by co-precipitation showed the better cycling performance(82.3%capacity retention at $50^{th}$ cycle) than that of the $LiMn_2O_4$(68.3%) prepared by solid state reaction at elevated temperature.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.17 no.6
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• pp.255-261
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• 2016

$CaCO_3$ was applied in various industries including rubber, plastics, paint, paper, food additives, and acid neutralizer, etc., owing to its excellent physical and chemical characteristics as well as various appearances of crystals and many reserves. In particular, research on controlling the structure and shape of $CaCO_3$ has attracted considerable attention recently, because the whiteness and physical characteristics of $CaCO_3$ depend on the size and shapes of the particles. In this study, $CaCO_3$ was synthesized using $CaCl_2$ and $(NH4)_2CO_3$, which has multi-shapes and structures, using a self-assembly method with a hydrothermal method. The structure and morphology of the $CaCO_3$ could be controlled by adjusting the pH and precursor concentration. In particular, the pH adjustment appeared to be a critical factor for the morphology and crystal form. In addition, the calcite and cubic shape were obtained at pH 7, while the mixed calcite, aragonite structure, and rod shapes appeared at pH 7 and over. Through an analysis of the particle formation process, the formation of the calcium carbonate particles was confirmed. The physicochemical properties of the synthesized $CaCO_3$ were analyzed by SEM, XRD, EDS, FTIR, and TG/DTA.

• Applied Chemistry for Engineering
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• v.10 no.5
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• pp.644-651
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• 1999

In this experiment the Iron phthalocyanine (FePc) films on Si-wafer and alumina pallet were prepared using vacuum sublimation with conditions of changing reaction time, temperature, and deposition rate. Then, some samples were annealed following annealing. Techniques such as XRD, SEM, and resistance measurement method, were dedicated to characterize the changes of surface structure, phase transformation and electric resistance sensitivity in accordance with change of film thickness. In proportion to the decrease of deposition temperature from $370^{\circ}C$ to $350^{\circ}C$, intensities of (200), (011), (211) and (114) planes of $\alpha$-phase were decreased and (100) plane of $\beta$-phase were appeared. The film thickness were controlled by regulating the volume of precursor material during rapid deposition. As a result, it was observed that crystalline particle size had been increased according to the increase of film thickness and $\alpha$-phase transformed to $\beta$-phase. In consequence of measuring the crystallinity of films annealed between $150^{\circ}C$ and $350^{\circ}C$, $\alpha$- to $\beta$-phase transformation was appeared to begin at $150^{\circ}C$ and completely transformed to $\beta$-phase at $350^{\circ}C$. Electric resistance sensitivity of FePc film to $NO_x$ gas along temperature change of FePc films was observed to be more stable with the decrease of the film thickness.

• Journal of the Korean Applied Science and Technology
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• v.24 no.2
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• pp.174-181
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• 2007

In this study, $SiO_2/poly(ethylene-co-vinyl$ alcohol)(EVOH) hybrid coating materials with gas barrier property could be produced using sol-gel method. The biaxially oriented polypropylene (BOPP) substrate with surface pretreatment was coated with the prepared hybrid sols containing various inorganic silicate component by a spin coating method. Crystallization behavior of the hybrids was investigated in terms of analysis of X-ray diffraction and cooling thermogram from DSC experiment. From the morphological observation of the $SiO_2/EVOH$ hybrid gel, it was confirmed that there existed an optimum content of inorganic silicate precursor, Tetraethylorthosilicate (TEOS), to produce hybrid materials with dense microstructure, exhibiting uniformly dispersed silica particles with average size below 100 nm. When TEOS was added at below or above the optimum content, particle clusters with large domain were observed, resulting in phase separation. This morphological result was found to be in good agreement with that of oxygen permeability of the hybrid coated films. In the case of film coated with hybrid prepared from addition of 0.01 - 0.02mol of TEOS, a remarkable improvement in barrier property could be obtained, however, with the addition of TEOS more than 0.04 mol, the barrier property was dramatically reduced because of phase separation and micro-crack formation on the film surface.

• Korean Chemical Engineering Research
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• v.54 no.6
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• pp.854-862
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• 2016

As the demand for a clean energy to replace fossil fuel being depleted increases, hydrogen energy is considered as a promising candidate for future energy source. Water electrolysis which produces hydrogen has high energy efficiency and stability but still has a large overpotential for oxygen evolution reaction (OER). In this study, $Co_3O_4$ catalysts with different morphology were prepared by spray pyrolysis from solutions which contain Co precursor and various organic additives (urea, sucrose, and citric acid), followed by post heat treatment. For the catalysts synthesized, X-ray diffraction (XRD) measurements were performed to identify their crystal structure. Morphology and surface shape of the catalysts were observed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Surface area and pore volume were examined by nitrogen adsortpion & desorption tests and X-ray photoelectron spectroscopy (XPS) was conducted to confirm nitrogen doping. Linear sweep voltammetry (LSV) was carried out to investigate OER activity of $Co_3O_4$ catalysts. As a result, bare-$Co_3O_4$ which has high surface area and small particle size determined by spray pyrolysis showed high activity toward OER.

• Korean Chemical Engineering Research
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• v.54 no.6
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• pp.746-752
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• 2016

In this study, soft carbon was prepared by carbonization of carbon precursor (pitch) obtained from PFO (pyrolysis fuel oil) heat treatment. Three carbon precursors prepared by the thermal reaction were 3903 (at $390^{\circ}C$ for 3 h), 4001 (at $400^{\circ}C$ for 1 h) and 4002 (at $400^{\circ}C$ for 2 h). After the prepared soft carbon was ground to a particle size of $25{\sim}35^{\circ}C$, the soft carbon was synthesised by the chemical treatment with boric acid ($H_3BO_3$). The prepared soft carbon were analysed by XRD, FE-SEM and XPS. Also, the electrochemical performances of soft carbon were investigated by constant current charge/discharge test, cyclic voltammetry and impedance tests in the electrolyte of $LiPF_6$ dissolved inorganic solvents (EC:DMC=1:1 vol%+VC 3 wt%). The coin cell using soft carbon of $25{\sim}35^{\circ}C$ with 3903 soft carbon ($H_3BO_3$/Pitch=3:100 in weight) has better initial capacity and efficiency (330 mAh/g, 82%) than those of other coin cells. Also, it was found that the retention rate capability of 2C/0.1C was 90% after 30 cycles.

• Applied Chemistry for Engineering
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• v.21 no.5
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• pp.590-592
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• 2010

Li-Mn spinel ($LiMn_2O_4$) is prepared by a hydrothermal process with K-Birnessite ($KMnO_4{\cdot}yH_2O$) as a precursor. The K-Birnessite obtained via a hydrothermal process with potassium permanganate [$KMnO_4$] and urea [$CO(NH_2)_2$] as starting materials are converted to Li-Mn spinel nanoparticles reacting with LiOH. The molar ratio of LiOH/K-Birnessite is adjusted in order to find the effect of the ratio on the structural, morphological and electrochemical performances of the Li-Mn spinel. X-ray diffraction (XRD) and field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDS), and thermogravimetry (TG) are used to investigate the crystal structure and morphology of the samples. Galvanostatic charge and discharge are carried out to measure the capacity and rate capability of the Li-Mn spinel. The capacity shows a maximum value of $117\;mAhg^{-1}$ when the molar ratio of LiOH/K-Birnessite is 0.8 and decreases with the increase of the ratio. However the rate capability is improved with the increase of the ratio due to the reduction of the particle size.

• Journal of the Microelectronics and Packaging Society
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• v.23 no.3
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• pp.51-56
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• 2016

To fabricate a copper (Cu)-based fine conductive filler having antioxidation property, submicron silver (Ag)-coated Cu particles were fabricated and their antioxidation property was evaluated. After synthesizing the Cu particles of $0.705{\mu}m$ in average diameter by a wet-reduction process, Ag-coated Cu particles were fabricated by successive Ag plating using ethylene grycol solvent. Main process parameters in the Ag plating were the concentration of reductant (ascorbic acid), the injection rate of Ag precursor solution, and the stirring rate in mixed solution. Thus, Ag plating characteristics and the formation of separate fine pure Ag phase were observed with different combinations of process parameters. As a result, formation of the separate pure Ag phase and aggregation between Ag-coated Cu particles could be suppressed by optimization of the process parameters. The Ag-coated Cu particles which were fabricated using optimal conditions showed slight aggregation, but excellent antioxidation property. For example, the particles indicated the weight gain not exceeding 0.1% until $225^{\circ}C$ when they were heated in air at the rate of $10^{\circ}C/min$ and no weight gain until 75 min when they were heated in air at $150^{\circ}C$.