• Title/Summary/Keyword: Reaction ball milling

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Effect of Edge-Chemistry on Graphene-Based Hybrid Electrode Materials for Energy Storage Device

  • Hyo-Young Kim;Ji-Woo Park;Seo Jeong Yoon;In-Yup Jeon;Young-Wan Ju
    • Journal of Electrochemical Science and Technology
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    • v.14 no.1
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    • pp.31-37
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    • 2023
  • Owing to the rapid climate change, a high-performance energy storage system (ESS) for efficient energy consumption has been receiving considerable attention. ESS, such as capacitors, usually has issues with the ion diffusion of electrode materials, resulting in a decrease in their capacitance. Notably, appropriate pore diameter and large specific surface area (SSA) may result in an effective ion diffusion. Therefore, graphene and multi-walled carbon nanotube (graphene@MWCNT) hybrid nanomaterials, with covalent bonds between the graphene and MWCNT, were prepared via an edge-chemistry reaction. The properties of these materials, such as high porosity, large SSA, and high electroconductivity, make them suitable to be used as electrode materials for capacitors. The optimal ratio of graphene to MWCNT can affect the electrochemical performance of the electrode material based on its physical and electrochemical properties. The supercapacitor using optimal graphene-based hybrid electrode material exhibited highest specific capacitance value as 158 F/g and excellent cycle stability.

Effect of $Al^{3+}$ Dopant on the Electrochemical Characteristics Of Spinel-type $Li_{4}Ti_{5}O_{12}$ (스피넬형 $Li_{4}Ti_{5}O_{12}$ 음극물질의 $Al^{3+}$ 첨가에 의한 전기화학적 성능 변화)

  • Jeong, Choong-Hoon;Lee, Eui-Kyung;Bang, Jong-Min;Lee, Bong-Hee;Cho, Byung-Won;Na, Byung-Ki
    • Clean Technology
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    • v.14 no.3
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    • pp.171-175
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    • 2008
  • The effect of the addition of $Al^{3+}$ dopant on the electrochemical characteristics of $Li_{4}Ti_{5}O_{12}$ was investigated. $Li_{4}Ti_{5}O_{12}$ is known as a 2ero-strain material, and $Li_{3.95}Al_{0.15}Ti_{4.9}O_{12}$ has been manufactured by solid-state reaction with high energy ball milling (HEBM). The samples were heated at 800, 900 and $1000^{\circ}C$ in electric furnace. The structural and surface structures were measured by XRD (X-ray diffraction) and SEM (scanning electron microscopy). Cut-off voltage of charge/discharge cycles was $1.0{\sim}3.0 V$ to investigate reversible capacity, cycle stability and plateau voltage. The reversible capacity of $Li_{3.95}Al_{0.15}Ti_{4.9}O_{12}$ was 138 mAh/g.

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Electrochemical Characteristics of Nano-sized A2MnPO4F (A = Li, Na) as Cathode Materials for Lithium ion Batteries

  • Cho, Woosuk;Song, Jun Ho;Kim, Sang-Min;Kim, Dong-Jin;Kang, Min-Gu;Kim, Jeom-Soo;Kim, Young-Jun
    • Journal of Electrochemical Science and Technology
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    • v.4 no.3
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    • pp.113-118
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    • 2013
  • Fluorophosphate, $Na_2MnPO_4F$ as new cathode material was synthesized by carbothermal treatment method. Prepared $Na_2MnPO_4F$ has particle size under 100 nm and residual carbon exists in surface of $Na_2MnPO_4F$. Additional carbon coating was performed in order to increase the electrochemical properties. Even capacity and overpotential were improved by carbon coating using mechanical ball milling, the reduced crystallinity limited the drastic improvement of the electrochemical properties. To solve this problem, re-heat treatment was involved to recover crystallinity and then notable improvement of electrochemical properties was obtained. Specific amount of $Li^+$ that participates in electrochemical $Li^+$ insertion / extraction reaction, was x = 1 in $Li_xNa_{2-x}MnPO_4F$ within the voltage range of 2.0 to 4.8 V. The doubled capacity by 2 electron reaction can be obtained when NMPF is charged to higher voltage over 4.8 V.

Synthesis Behavior of Ti-50.0 ~ 66.7at%Si Powders by In situ Thermal Analysis during Mechanical Alloying (기계적 합금화과정에서의 in situ 열분석에 의한 Ti-50.0~66.7at%Si 분말의 합성거동)

  • Byun Chang Sop;Lee Sang Ho;Lee Wonhee;Hyun Chang Yong;Kim Dong Kwan
    • Korean Journal of Materials Research
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    • v.14 no.5
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    • pp.310-314
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    • 2004
  • Mechanical alloying (MA) of Ti-50.0~66.7at%Si powders was carried out in a high-energy ball mill, and in situ thermal analysis was also made during MA. In order to classify the synthesis behavior of the powders with respect to at%Si, the synthesis behavior during MA was investigated by in situ thermal analysis and X-ray diffraction (XRD). In situ thermal analysis curves and XRD patterns of Ti-50.0~59.6at%Si powders showed that there were exothermic peaks during MA, indicating TiSi, $TiS_2$, and $Ti_{5}$ $Si_4$ phase formation by a rapid exothermic reaction of self-propagating high-temperature synthesis (SHS). Those of Ti-59.8~66.7 at%Si powders, however, showed that there were no peaks during MA, indicating any Ti silicide was not synthesised until MA 240 min. For Ti-50.0~59.6at%Si powders, the critical milling times for SHS increased from 34.5 min to 89.5 min and the temperature rise, $\Delta$T (=peak temperature-onset temperature) decreased form $26.2^{\circ}C$ to $17.1^{\circ}C$ as at%Si increased. The critical composition of Si for SHS reaction was found to be 59.6at% and the critical value of the negative heat of formation of Ti-59.6at%Si to be -1.48 kJ/g.

Synthesis of akermanite bioceramics by solid-state reaction and evaluation of its bioactivity (고상반응법에 의한 아커마나이트 분말의 합성 및 생체활성도 평가)

  • Go, Jaeeun;Lee, Jong Kook
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.32 no.5
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    • pp.191-198
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    • 2022
  • Zirconia and titanium alloys, which are mainly used for dental implant materials, have poor osseointegration and osteogenesis abilities due to their bioinertness with low bioactivity on surface. In order to improve their surface bioinertness, surface modification with a bioactive material is an easy and simple method. In this study, akermanite (Ca2MgSi2O7), a silicate-based bioceramic material with excellent bone bonding ability, was synthesized by a solid-state reaction and investigated its bioactivity from the analysis of surface dissolution and precipitation of hydroxyapatite particles in SBF solution. Calcium carbonate (CaCO3), magnesium carbonate (MgCO3), and silicon dioxide (SiO2) were used as starting materials. After homogeneous mixing of starting materials by ball milling and the drying of at oven, uniaxial pressing was performed to form a compacted disk, and then heat-treated at high temperature to induce the solid-state reaction to akermanite. Bioactivity of synthesized akermanite disk was evaluated with the reaction temperature from the immersion test in SBF solution. The higher the reaction temperature, the more pronounced the akermanite phase and the less the surface dissolution at particle surface. It resulted that synthesized akermanite particles had high bioactivity on particle surface, but it depended on reacted temperature and phase composition. Moderate dissolution occurred at particle surfaces and observed the new precipitated hydroxyapatite particles in synthetic akermanite with solid-state reaction at 1100℃.

Mechanical Properties and Bio-Compatibility of Ti-Nb-Zr-HA Biomaterial Fabricated by Rapid Sintering Using HEMM Powders (고에너지 밀링분말과 급속소결을 이용한 Ti-Nb-Zr-HA 생체복합재의 기계적 성질 및 생체적합성)

  • Park, Sang-Hoon;Woo, Kee-Do;Kim, Sang-Hyuk;Lee, Seung-Min;Kim, Ji-Young;Ko, Hye-Rim;Kim, Sang-Mi
    • Korean Journal of Materials Research
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    • v.21 no.7
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    • pp.384-390
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    • 2011
  • Ti-6Al-4V ELI (Extra Low Interstitial) alloy has been widely used as an alternative to bone due to its excellent biocompatibility. However, it still has many problems, including a high elastic modulus and toxicity. Therefore, nontoxic biomaterials with a low elastic modulus should be developed. However, the fabrication of a uniform coating is challenging. Moreover, the coating layer on Ti and Ti alloy substrates can be peeled off after implantation. To overcome these problems, it is necessary to produce bulk Ti and Ti alloy with hydroxyapatite (HA) composites. In this study, Ti, Nb, and Zr powders, which are biocompatible elements, were milled in a mixing machine (24h) and by planetary mechanical ball milling (1h, 4h, and 6h), respectively. Ti-35%Nb-7%Zr and Ti-35%Nb-7%Zr-10%HA composites were fabricated by spark plasma sintering (SPS) at $1000^{\circ}C$ under 70MPa using mixed and milled powders. The effects of HA addition and milling time on the biocompatibility and physical and mechanical properties of the Ti-35%Nb-7%Zr-(10%HA) alloys have been investigated. $Ti_2O$, CaO, $CaTiO_3$, and $Ti_xP_y$ phases were formed by chemical reaction during sintering. Vickers hardness of the sintered composites increases with increased milling time and by the addition of HA. The biocompatibilty of the HA added Ti-Nb-Zr alloys was improved, but the sintering ability was decreased.

A Study on the Preparation of SiC Nano powder from the Si Waste of Solar Cell Industry (태양전지 산업(産業)에서 배출(排出)되는 Si waste로부터 SiC 분말 제조에 관한 연구(硏究))

  • Jang, Eun-Jin;Kim, Young-Hee;Lee, Yoon-Joo;Kim, Soo-Ryong;Kwon, Woo-Teck
    • Resources Recycling
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    • v.19 no.5
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    • pp.44-49
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    • 2010
  • SiC powders have been recovered from silicon-containing waste slurry by carbothermal reduction method with carbon black. Large amount of silicon-containing waste slurry is generated from Solar Cell industry. In an environmental and economic point of view, retrieve of the valuable natural resource from the silicon waste is important. In this study, SiC powder recovered by the reaction ball-milled silicon powder from waste and carbon black at $1350^{\circ}C$ for 3h under vacuum condition. Physical properties of samples have been characterized using SEM, XRD, Particle size analyzer and FT-IR spectroscopy.

FABRICATIO0N OF NASICON ELECTROLYTES

  • Choi, Soon-Don;Park, Jung-Woo
    • Journal of Sensor Science and Technology
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    • v.4 no.1
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    • pp.35-42
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    • 1995
  • Conventional ball-milling technique was used to synthesize NASICON powders. The NASICON powders were made from three kinds of component powders : coarse($ZrO_{2}$, $Na_{3}PO_{4}$, $SiO_{2}$), fine ($ZrO_{2}$, $Na_{3}PO_{4}$, $SiO_{2}$) and fine ($ZrSiO_{4}$, $Na_{3}PO_{4}$) powders. The fine component powders were easily reacted to form the desired product at $1100^{\circ}C$ or higher, whereas incomplete reaction due to the coarse component powders occurred even at $1170^{\circ}C$. The finer the grain size of the starting powders was, the higher the bulk density of NASICON electrolyte after sintering was observed. Almost single phase NASICON electrolytes with more than 95% of the theoretical density, $3.27g/cm^{3}$, could be fabricated by sintering for $40{\sim}60$ hours at temperatures between 1150 and $1170^{\circ}C$.

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Synthesis and Electrochemical Characteristics of Mesoporous Silicon/Carbon/CNF Composite Anode (메조기공 Silicon/Carbon/CNF 음극소재 제조 및 전기화학적 특성)

  • Park, Ji Yong;Jung, Min Zy;Lee, Jong Dae
    • Applied Chemistry for Engineering
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    • v.26 no.5
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    • pp.543-548
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    • 2015
  • Si/C/CNF composites as anode materials for lithium-ion batteries were examined to improve the capacity and cycle performance. Si/C/CNF composites were prepared by the fabrication process including the synthesis and magnesiothermic reduction of SBA-15 to obtain Si/MgO by ball milling and the carbonization of phenol resin with CNF and HCl etching. Prepared Si/C/CNF composites were then analysed by BET, XRD, FE-SEM and TGA. Among SBA-15 samples synthesized at reaction temperatures between 50 and $70^{\circ}C$, the SBA-15 at $60^{\circ}C$ showed the largest specific surface area. Also the electrochemical performances of Si/C/CNF composites as an anode electrode were investigated by constant current charge/discharge test, cyclic voltammetry and impedance tests in the electrolyte of LiPF6 dissolved in mixed organic solvents (EC : DMC : EMC = 1 : 1 : 1 vol%). The coin cell using Si/C/CNF composites (Si : CNF = 97 : 3 in weight) showed better capacity (1,947 mAh/g) than that of other composition coin cells. The capacity retention ratio decreased from 84% (Si : CNF = 97 : 3 in weight) to 77% (Si : CNF = 89 : 11 in weight). It was found that the Si/C/CNF composite electrode shows an improved cycling performance and electric conductivity.

Study on Oxidation and Coercivity of Nd2Fe14B Compound Crystal (Nd2Fe14B 화합물 결정의 산화 및 보자력에 관한 연구)

  • Kwon, H.W.;Yu, J.H.
    • Journal of the Korean Magnetics Society
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    • v.22 no.3
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    • pp.85-90
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    • 2012
  • Oxidation of the $Nd_2Fe_{14}B$ compound crystal and its effect on the coercivity of the fine $Nd_2Fe_{14}B$ crystal particles were investigated. Oxidation kinetics of the $Nd_2Fe_{14}B$ compound crystal was investigated using an excessively grown $Nd_2Fe_{14}B$ grains in the $Nd_{15}Fe_{77}B_8$ alloy ingot. Oxidation of the $Nd_2Fe_{14}B$ compound crystal occurred by dissociation of the phase into multi-phase mixture of ${\alpha}$-Fe, $Fe_3B$, and Nd oxides. Oxidation rate of the $Nd_2Fe_{14}B$ compound crystal showed no dependence on the crystallographic direction. The oxidation reaction was modeled according to simple linear relationship. Activation energy for the oxidation of $Nd_2Fe_{14}B$ compound crystal was calculated to be approximately 26.8 kJ/mol. Fine $Nd_2Fe_{14}B$ crystal particles in near single domain size was prepared by ball milling of the HDDR-treated $Nd_{15}Fe_{77}B_8$ alloy, and these particles were used for investigating the effect of oxidation on the coercvity. The near single domain size $Nd_2Fe_{14}B$ crystal particles (${\fallingdotseq}0.3\;{\mu}m$) had high coercivity over 9 kOe. However, the coercivity was radically reduced as the temperature increased in air (<2 kOe at $200^{\circ}C$). This radical coercivity reduction was attributed to the soft magnetic phases, ${\alpha}$-Fe and $Fe_3B$, which were formed on the surface of the fine particles due to the oxidation.