• Title/Summary/Keyword: Precursor Solution

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Electrochemical Properties of Lithium Secondary Battery and the Synthesis of Spherical Li4Ti5O12 Powder by Using TiCl4 As a Starting Material (TiCl4를 출발원료로한 구형 Li4Ti5O12 분말합성 및 리튬이차 전지특성)

  • Choi, Byung-Hyun;Ji, Mi-Jung;Kwon, Yong-Jin;Kim, Eun-Kyung;Nahm, Sahn
    • Korean Journal of Materials Research
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    • v.20 no.12
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    • pp.669-675
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    • 2010
  • One of the greatest challenges for our society is providing powerful electrochemical energy conversion and storage devices. Rechargeable lithium-ion batteries and fuel cells are among the most promising candidates in terms of energy and power density. As the starting material, $TiCl_4{\cdot}YCl_3$ solution and dispersing agent (HCP) were mixed and synthesized using ammonia as the precipitation agent, in order to prepare the nano size Y doped spherical $TiO_2$ precursor. Then, the $Li_4Ti_5O_{12}$ was synthesized using solid state reaction method through the stoichiometric mixture of Y doped spherical $TiO_2$ precursor and LiOH. The Ti mole increased the concentration of the spherical particle size due to the addition of HPC with a similar particle size distribution in a well in which $Li_4Ti_5O_{12}$ spherical particles could be obtained. The optimal synthesis conditions and the molar ratio of the Ti 0.05 mol reaction at $50^{\circ}C$ for 30 minutes and at $850^{\circ}C$ for 6 hours heat treatment time were optimized. $Li_4Ti_5O_{12}$ was prepared by the above conditions as a working electrode after generating the Coin cell; then, electrochemical properties were evaluated when the voltage range of 1.5V was flat, the initial capacity was 141 mAh/g, and cycle retention rate was 86%; also, redox reactions between 1.5 and 1.7V, which arose from the insertion and deintercalation of 0.005 mole of Y doping is not a case of doping because the C-rate characteristics were significantly better.

Synthesis of Hectorite by Hydrothemal Method (저온 수열법에 의한 헥토라이트 합성)

  • Jang, Young-Nam;Chae, Soo-Chun;Ryu, Gyoung-Won;Kim, You-Dong;Jang, Hee-Dong;Bae, In-Kook
    • Journal of the Mineralogical Society of Korea
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    • v.20 no.1 s.51
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    • pp.1-6
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    • 2007
  • Hectorite was synthesized by a two-step hydrothermal process from $Mg(OH)_{2}$, water glass (${\sim}30\;wt%\;SiO_{2}$) and Li-compound at $90{\pm}5^{\circ}C$. The product shows excellent dispersion and swelling properties. The mixture of the starting materials was heated in a glass vessel for the first reaction with continuous stirring and the pH of the solution was adjusted to $6{\sim}8$, resulting in the formation of a precursor of hectorite. The excess salt components were washed out from the resulting slurry and then was matured in the glass vessel for the 2nd reaction. Li compound was added during the reaction. After a 10 h retention, the gel of hectorite was formed. The XRD pattern of the synthesized one was coincided with that of natural hectorite and SEM study revealed uniform grains 50 m in diameter. The d001 basal spacing of the product moved from 12 to $17.4\;{\AA}$ after glycolation treatment. The measured value of CEC and the swelling capacity was 90 cmol/kg and $60{\sim}70\;mL/2\;g$, respectively.

Synthesis of Prussian Blue Analogue and Magnetic and Adsorption Characteristics of MnFe2O4 (프러시안 블루 유사체의 합성 및 MnFe2O4의 자성과 흡착 특성)

  • Lee, Hye-In;Kang, Kuk-Hyoun;Lee, Dong-Kyu
    • Journal of the Korean Applied Science and Technology
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    • v.33 no.1
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    • pp.67-74
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    • 2016
  • The Prussian Blue Analogue(PBA) has three dimensional structure and the metal - organic framework material, and it has a variety configurations depending on the type of organic ligands. PBA has been receving an attention in the fields of biosensors, optical, catalytic, and hydrogen storage device. Also, it is an environmental friendly substance with a chemical stability. In addition, PBA is widely used in the filed of adsorption art since we can adjust the size of the fine pores. In this study, we synthesized $Mn_3[Fe(CN)_6]_2$, an organometallic framework chains by using a hydrothermal synthesis method. We used $K_4[Fe(CN)_6]$ and $MnCl_2$ as precursors. We also produced a manganese iron oxide, by baking the synthesized material. The effect of the size and shape of the particles was examined by controling pH of the precursor solution, the molar concentration of the precursor, and reaction time as the experimental variables. Synthesized absorbent was analyzed by XRD, SEM, FT-IR, UV-Vis, and TG / DTA to evaluate the adsorption properties of several dyes.

A Study on the Synthesis Behavior of Lithium Hydroxide by Type of Precipitant for Lithium Sulfate Recovered from Waste LIB (폐리튬이차전지에서 회수된 황산리튬 전구체로부터 침전제 종류별 수산화리튬 제조 거동 연구)

  • Joo, Soyeong;Kim, Dae-Guen;Byun, Suk-Hyun;Kim, Yong Hwan;Shim, Hyun-Woo
    • Resources Recycling
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    • v.30 no.1
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    • pp.44-52
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    • 2021
  • This study investigated the effect of the type of alkaline precipitant used on the synthesis of lithium hydroxide by examining the behavior of lithium hydroxide produced using lithium sulfate recovered from a waste lithium secondary battery as a raw material. The double-replacement reaction (DRR) process was used to remove the impurities contained in the lithium salt precursor of lithium sulfate and to improve the efficiency of the synthesis of lithium hydroxide. The experiment was conducted by control the molar ratio of the precursor ([Li]/[OH]), the reaction temperature, and the composition of the alkaline precipitant (KOH, Ca(OH)2, Ba(OH)2) used for the production of highly-crystalline lithium hydroxide. A secondary solid-liquid separation was performed following the reaction to remove the impurities generated, and the purified aqueous solution of lithium hydroxide was evaporated to remove the moisture and obtain the product as a powder. The crystallinity and synthesis behavior of the product were examined.

Preliminary Study on the Phase Transition of White Precipitates Found in the Acid Mine Drainage (산성광산배수에서 발견되는 흰색침전물의 상전이에 대한 예비 연구)

  • Yeo, Jin Woo;Kim, Yeongkyoo
    • Journal of the Mineralogical Society of Korea
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    • v.32 no.2
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    • pp.79-86
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    • 2019
  • The white aluminum phases in acid mine drainage usually precipitates when mixed with stream waters with relatively high pH. The minerals in white precipitates play important roles in controlling the behavior of heavy metals by adsorbing and coprecipitation. By the phase transition of these minerals in white precipitates, dissolution and readsorption of heavy metals may occur. This study was conducted to obtain preliminary information on the phase transition of the mineral phases in white precipitates. In this study, the mineral phase changes in the white precipitates collected from the stream around Dogye Mining Site over time were investigated with different pH values and temperatures. White precipitates consist mainly of basaluminite, amorphous $Al(OH)_3$ and a small amount of $Al_{13}$-tridecamer. During aging, the incongruent dissolution of the basaluminite occurs first, increasing the content of the amorphous $Al(OH)_3$. After that, pseudoboehmite is finally precipitated following the precursor phase of pseudoboehmite. At $80^{\circ}C$, this series of processes was clearly observed, but at relatively low temperatures, no noticeable changes were observed from the initial condition with coexisting basaluminite and amorphous $Al(OH)_3$. At high pH, the desorption of $SO{_4}^{2-}$ group in basaluminite was initiated to promote phase transition to the pseudoboehmite precursor. Over time, the solution pH decreases due to the dissolution and phase transition of the minerals, and even after the precipitation of pseudoboehmite, only the particle size slightly increased but no clear cystal form was observed.

Preparation of calcium phosphates by hydrothermal synthesis route (수열합성법에 의한 calcium phosphates 분말합성)

  • Moon, Sung Wook;Lee, Byeong Woo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.29 no.5
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    • pp.203-207
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    • 2019
  • Calcium phosphates such as hydroxyapatite (HAp), tricalcium phosphate (${\beta}$-TCP), and biphasic calcium phosphate (BCP, HAp/${\beta}$-TCP) have been prepared via hydrothermal treatment. The synthesis was conducted by reacting ($Ca(OH)_2$) aqueous solution with phosphoric acid ($H_3PO_4$) under different hydrothermal synthesis conditions (temperatures up to $150^{\circ}C$ and pH lower than 12). The effects of initial precursor Ca/P ratio (1.30, 1.50 and 1.67) and post heat treatment on the phase evolution behavior of the powders and sintered ceramics were investigated. The phases of resulting powders and sintered ceramics were controllable by adjusting the initial Ca/P ratio. A single HAp phase without any noticeable second phase was obtained for the initial Ca/P ratio of 1.67 in the overall heat treatment range. Pure ${\beta}$-TCP and biphasic calcium phosphate (HAp/${\beta}$-TCP) were synthesized from precursor solutions having Ca/P molar ratios of 1.30 and 1.50, respectively, after having been heat treated at $900^{\circ}C$ or higher. Dense ceramics with translucency were obtained at considerably lower sintering temperatures.

Antibacterial Effect of Gelatin/Ag Nanoparticle Biocomposite Prepared Using Solution Plasma Generated by Unipolar DC Power (단극성 직류전원으로 유도된 용액 플라즈마를 이용하여 제조한 젤라틴/은 나노입자 생체복합재료의 항균 효과)

  • Kim, Seong-Cheol;Yoon, Gook-Jin;Nam, Sang-Woo;Lee, Sang-Yul;Kim, Jung-Wan
    • Microbiology and Biotechnology Letters
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    • v.40 no.4
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    • pp.403-408
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    • 2012
  • Gelatin/Ag nanoparticle (AgNP) biocomposite was synthesized using the solution plasma process (SPP) that has been recently introduced as an effective method for synthesis of nanoparticles. In this study, gelatin/AgNP biocomposite was synthesized using various concentrations of Ag precursor ($AgNO_3$) and gelatin in the range of 1-5 mM and 1-3% (w/w), respectively, without using any chemical reducing agent. Physical properties of the gelatin/AgNP biocomposites were analyzed using EDS, FE-SEM, and TEM. The results indicated that spherical AgNPs with approximately 12~20 nm in diameter were synthesized successfully in the gelatin matrix by SPP. As the concentration of gelatin was increased (3%, w/w), disperse stability of AgNP was improved and micro-pores of gelatin became smaller and denser in the 3D scaffold. Bactericidal activity of the AgNPs was examined against Staphylococcus aureus and Escherichia coli by measuring zone of growth inhibition and decrease in colony forming unit (CFU). CFUs of S. aureus and E. coli were decreased approximately to 56% and 0%, respectively, by the gelatin/AgNP biocomposite, Ag5G3.

Recoverty of Lithium Carbonate and Nickel from Cathode Active Material LNO(Li2NiO2) of Precursor Process Byproducts (전구체 공정부산물 LNO(Li2NiO2)계 양극활물질로부터 탄산리튬 및 니켈 회수연구)

  • Pyo, Je-Jung;Wang, Jei-Pil
    • Resources Recycling
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    • v.28 no.4
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    • pp.30-36
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    • 2019
  • In this study, Li powder was recovered from the by-product of LNO ($Li_2NiO_2$) process, which is the positive electrode active material of waste lithium ion battery, through the $CO_2$ thermal reaction process. In the process of recovering Li powder, the $CO_2$ injection amount is 300 cc/min. The $Li_2NiO_2$ award was phase-separated into the $Li_2CO_3$ phase and the NiO phase by holding at $600^{\circ}C$ for 1 min. After this, the collected sample:distilled water = 1:50 weight ratio, and after leaching, the solution was subjected to vacuum filtration to recover $Li_2CO_3$ from the solution, and the NiO powder was recovered. In order to increase the purity of Ni, it was maintained in $H_2$ atmosphere for 3 hours to reduce NiO to Ni. Through the above-mentioned steps, the purity of Li was 2290 ppm and the recovery was 92.74% from the solution, and Ni was finally produced 90.1% purity, 92.6% recovery.

Hydrophilic Modification of Porous Polyvinylidene Fluoride Membrane by Pre-irradiating Electron Beam (전자빔 전조사를 이용한 Polyvinylidene Fluoride 다공막의 친수화 개질)

  • Choi, Yong-Jin;Lee, Sung-Won;Seo, Bong-Kuk;Kim, Min
    • Membrane Journal
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    • v.21 no.2
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    • pp.118-126
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    • 2011
  • A method of light pre-irradiation, one of methods modifying hydrophobic surface to hydrophilic surface in a membrane, was proposed to overcome the drawback of previous methods such as blending, chemical treatment and post-irradiation, Process of membrane preparation in the study was comprised of 4 parts as follows: firstly process of precursor preparation to introduce hydrophilic nature under atmosphere and aqueous vapor by irradiating electron beam (EB), secondly process of dope solution preparation to cast on non-woven fabrics, thirdly process of casting to prepare membrane and finally process of coagulation in non-solvent to form porous structure. The merit of this method might show simple process as well as homogenous modification compared to previous methods. To carry it out, precursor was prepared by irradiating EB to powder PVDF at 75~125 K Gray dose. Precursor prepared was analyzed by FTIR, EDS and DSC to confirm the introduction of hydrophilic function and its mechanism. From their results, it was inferred I conformed that hydrophilic function was hydroxy1 and it was introduced by dehydrozenation. Hydrophilicity of membranes prepared was evaluated by contact angle (pristine PVDF : $62^{\circ}$, 125 K Gray-PVDF$13^{\circ}$). Porosity was evaluated by mercury intrusion method, simultaneously morpholoy and surface pore size were observed by SEM phothographs. The result showed the trend that more dose of EB led to smaller pore size and to lower porosity (pristine PVDF : 82%, 125 K Gray-PVDF : 63%). Trend of water permeability was similar to result above (pristine PVDF : 892 LMH, 125 K Gray-PVDF : 355 LMH).

Silica and Iron Oxide Recovery and Mineral Carbonation from Serpentine Minerals Using Acid Dissolution and pH Swing Processes (산 처리와 pH 조절을 이용한 사문석군 광물로부터 규소와 철산화물 회수 및 광물 탄산화 연구)

  • Baek, Jiyeon;Jo, Yeonu;Lee, Jeongheon;Kwon, Nayoon;Kim, Yeram;Choi, Suk;Kim, Sunghee;Roh, Yul
    • Economic and Environmental Geology
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    • v.49 no.1
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    • pp.13-22
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    • 2016
  • The objectives of this study were to recover silica and iron oxides and $CO_2$ sequestration using serpentine via various acid dissolution and pH swing processes. Serpentine collected from Guhang-myeon in S. Korea were mainly composed of antigorite and magnetite consisting of $SiO_2$ (45.3 wt.%), MgO (41.3 wt.%), $Fe_2O_3$ (12.2 wt.%). Serpentine pulverized ($${\leq_-}75{\mu}m$$) and then dissolved in 3 different acids, HCl, $H_2SO_4$, $HNO_3$. Residues treated with acidic solution were recovered from the solution (step 1). And then the residual solution containing dissolved serpentine was titrated using $NH_4OH$. And pH of the solution increased up to pH=8.6 to obtain reddish precipitates (step 2). After recovery of the precipitates, the residual solution reacted with $CO_2$ and then pH increased up to pH=9.5 to precipitate white materials (step 3). The mineralogical characteristics of the original sample and harvested precipitates were examined by XRD, and TEM-EDS analyses. ICP-AES analysis was also used to investigate solution chemistry. The dissolved ions were Mg, Si, and Fe. The antigorite became noncrystralline silica after acid treatment (step 1). The precipitate at pH=8.6 was mainly amorphous iron oxide, of which size ranged from 2 to 10 nm and mainly consisting of Fe, O, and Si (step 2). At pH=9.5, nesquehonite [$Mg(HCO_3)(OH){\cdot}2(H_2O)$] and lasfordite [$MgCO_3{\cdot}H_2O$] were formed after reaction with $CO_2$ (step 3). The size of carbonated minerals was ranged from 1 to $6{\mu}m$. These results indicated that the acid treatment of serpentine and pH swing processes for the serpentine can be used for synthesis of other materials such as silica, iron oxides and magnesium carbonate. Also, This process may be useful for the precursor synthesis and $CO_2$ sequestration via mineral carbonation.