• Korean Chemical Engineering Research
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• v.58 no.1
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• pp.142-149
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• 2020

In this study, the electrochemical performance of Graphite/Silicon/Pitch composites as anode material was investigated to improve the low theoretical capacity of artificial graphite. Spherical artificial graphite surface was coated with polyvinylpyrrolidone (PVP) amphiphiles material to synthesize Graphite/Silica material by silica islands growth. The Graphite/Silicon/Pitch composites were prepared by petroleum pitch coating and magnesiothermic reduction. The Graphite/Silicon/Pitch composite electrodes manufactured using poly(vinylidene fluoride) (PVDF), carboxymethyl cellulose (CMC) and polyacrylic acid (PAA) binders. The coin type half cell was assembled using various electrolytes and additives. The Graphite/Silicon/Pitch composites were analysed by X-ray diffraction (XRD), scanning electron microscope (SEM) and a thermogravimetric analyzer (TGA). The electrochemical characteristics of Graphite/Silicon/Pitch composite were investigated by constant current charge/discharge, rate performance, cyclic voltammetry and electrochemical impedance spectroscopy. The Graphite/Silicon/Pitch composites showed high cycle stability at a graphite/silica/pitch ratio (1:4:8 wt%). When the electrode is prepared using PAA binder, the high capacity and stability is obtained. The coin type half cell assembled using EC: DMC: EMC electrolyte showed high initial capacity (719 mAh/g) and excellent cycle stability. The rate performance has an capacity retention (77%) at 2 C/0.1 C and an capacity recovery (88%) at 0.1 C / 0.1 C when the vinylene carbonate (VC) was added.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2016.11a
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• pp.177-177
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• 2016

우수한 내식성을 가지는 Zn 박막은 자동차, 가전제품, 전자제품 등에 사용되는 철 생산품의 수명 연장을 위하여 널리 사용되어 왔다. 최근 개발된 Zn-Mg 합금 박막은 Zn나 Mg에 비해 우수한 내식성을 나타내는 Zn-Mg 합금상을 형성하기 때문에 순수한 Zn 박막이나 다른 Zn 계 합금 박막에 비해 우수한 내식성을 가진다고 보고된 바 있다. 본 연구에서는 다양한 합금상의 형성을 위해 Mg 중간층 두께를 제어하며 Zn/Mg/Zn 다층 박막들을 합성하였으며 열처리를 통한 합금상의 변화, 그에 따른 박막의 내식성에 관해 연구하였다. Zn/Mg/Zn 다층 박막은 총 $4{\mu}m$의 두께로 Mg 중간층의 두께를 변화하였으며 비대칭 마그네트론 스퍼터링 공정을 이용하여 냉연강판 위에 합성하였다. 합성된 다층 박막은 다양한 Zn-Mg 합금상을 형성하기 위하여 진공로를 이용하여 $200^{\circ}C$에서 1시간 동안 어닐링 열처리를 실시하였다. 열처리 전, 후 Zn/Mg/Zn 다층 박막의 미세조직과 조성은 X선 회절 분석기 (XRD)와 전계방출형 주사전자현미경 (FE-SEM)과 글로우 방전 분광분석기 (GDEOES)를 사용하여 분석하였다. 어닐링 열처리를 통한 Zn-Mg 합금상 형성이 Zn/Mg/Zn 다층 박막의 내식성에 미치는 영향을 평가하기 위하여 동전위 분극시험과 EIS(Electrochemical impedance spectroscopy) 분석 실시하였다. FE-SEM과 GDOES 분석 결과, Zn/Mg/Zn 다층 박막들 각각의 중간층 Mg 두께는 1.5, 2.0, $2.5{\mu}m$ 였으며, 어닐링 열처리 후 중간층의 Mg이 상, 하부의 Zn 층으로 확산되면서 박막을 치밀한 구조로 변화시키는 것으로 확인되었다. XRD 분석 결과, 열처리를 하지 않은 Zn/Mg/Zn 다층 박막들에서는 Mg 상의 피크의 강도 차이만 존재할 뿐 Zn-Mg 합금상은 형성되지 않았다. 그러나 열처리를 후 Zn/Mg/Zn 다층 박막들에서 $MgZn_2$ 합금상이 형성되었으며, 중간층 Mg 두께가 $1.5{\mu}m$ 이하인 박막에서는 Zn 상이, 초과하는 박막에서는 Mg 상이 잔존하는 것을 확인하였다. EIS 분석 결과, 열처리 후 박막의 전하이동저항 값은 증가하며 박막의 어드미턴스 값이 감소하였으며 Bode phase plot을 통해 열처리 후 시정수(time constant)가 높은 주파수 영역에서 형성 되는 것을 확인하였다. 이는 열처리 후 Zn/Mg/Zn 다층 박막이 치밀해지고 내식성이 향상되었음을 나타낸다. 동전위 분극시험 결과에서도 마찬가지로 열처리 한 Zn/Mg/Zn 다층 박막들은 열처리 전 대비 내식성이 향상되는 것을 확인하였다. 열처리를 통한 Zn/Mg/Zn 다층 박막의 내식성의 향상은 우수한 내식성의 합금상의 형성과 박막 미세구조의 치밀화에 기인한다고 판단하였다. 또한 열처리 한 Zn/Mg/Zn 다층 박막들에서는 Zn와 $MgZn_2$ 상들이 공존 할 경우 가장 우수한 내식성을 나타내었으며, 이는 $MgZn_2$와 Zn 사이의 적은 전위 차이로 인해 갈바닉 부식 효과가 감소되었기 때문으로 판단된다.

• Korean Chemical Engineering Research
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• v.54 no.2
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• pp.157-162
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• 2016

Porous $Co(OH)_2$ nano-flake thin films were prepared by a potential-controlled electro-deposition technique at various deposition voltage (-0.75, -1.0, -1.2, and -1.4 V) on Ti-mesh substrates for supercapacitor application. The potential of electrode was controlled to regulate the film thickness and the amount of $Co(OH)_2$ nano-flake on the titanium substrate. The film thickness was shown to reach the maximum value of $34{\mu}m$ at -1.4 V of electrode potential, where 17.2 g of $Co(OH)_2$ was deposited on the substrate. The specific discharge capacitances were measured to be 226, 370, 720, and $1008mF\;cm^{-2}$ in the 1st cycle corresponding to the films which were formed at -0.75, -1.0, -1.2, and -1.4 V of electrode potentials, respectively. Then the discharge capacities were decreased to be 206, 349, 586 and $866mF/cm^{-2}$, where the persistency rates were 91, 94, 81, and 86%, respectively.

• Polymer(Korea)
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• v.35 no.6
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• pp.593-598
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• 2011

The IPA-co-HDO-co-(TPA/MA) copolymers for all-vanadium redox flow battery were synthesized by melt condensation polymerization using isophthalic acid(IPA), 1,6-hexandiol (HDO), terephthalic acid(TPA) and maleic anhydride(MA). The amination of chloromethylated IPA-co- HDO-co-(TPA/MA)(CIHTM) copolymer was carried out using trimethylamine, and the anion exchange membrane was also prepared by UV crosslinking reaction. The structure and thermal stability of IHTM copolymers were confirmed by FTIR, $^1H$ NMR, and TGA analysis. The anion membrane properties such as water uptake, ion exchange capacity, electric resistance and electrical conductivity, were measured by gravimetry, titration and LCR meter. The efficiency of the all-vanadium redox flow battery was analyzed. The ion exchange capacity, electric resistance and electrical conductivity were 1.10 meq/g, $1.98{\Omega}{\cdot}cm^2$, and 0.009 S/cm, respectively. The efficiency of charge-discharge, voltage, and energy for the allvanadium redox flow battery were 96.5, 74.6, 70.0%, respectively.

• Applied Chemistry for Engineering
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• v.29 no.6
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• pp.759-764
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• 2018

3D porous carbon electrodes (cNPIM), prepared by solution casting of a polymer of intrinsic microporosity (PIM-1) followed by nonsolvent-induced phase separation (NIPS) and carbonization are presented. In order to effectively control the pore size of 3D porous carbon structures, cNPIM was prepared by varying the THF ratio of mixed solvents. The SEM analysis revealed that cNPIMs have a unique 3D macroporous structure having a gradient pore structure, which is expected to grant a smooth and easy ion transfer capability as an electrode material. In addition, the cNPIMs presented a very large specific surface area ($2,101.1m^2/g$) with a narrow micropore size distribution (0.75 nm). Consequently, the cNPIM exhibits a high specific capacitance (304.8 F/g) and superior rate capability of 77% in an aqueous electrolyte. We believe that our approach can provide a variety of new 3D porous carbon materials for the application to an electrochemical energy storage.

• Journal of the Korean Electrochemical Society
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• v.22 no.2
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• pp.69-78
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• 2019

Lithium metal anode with the highest theoretical capacity to replace graphite anodes are being reviewed. However, the dendrite growth during repeated oxidation/reduction reaction on lithium metal surface, which results in poor cycle performance and safety issue has hindered its successful implementation. In our previous work, we solved this problem by using surface modification technique whereby a surface pattern on lithium metal anode is introduced. Although the micro-patterned Lithium metal electrode is beneficial to control Li metal deposition efficiently, it is difficult to control the mossy-like Li granulation at high current density ($>2.0mA\;cm^{-2}$). In this study, we introduce vinylene carbonate (VC) electrolyte additive on micro patterned lithium metal anode to suppress the lithium dendrite growth. Owing to the synergetic effect of micro-patterned lithium metal anode and VC electrolyte additive, lithium dendrite at a high current density is dense. As a result, we confirmed that the cycle performance was further improved about 6 times as compared with the reference electrode.

• Applied Chemistry for Engineering
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• v.33 no.1
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• pp.58-63
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• 2022

Graphite has been used as an anode material for lithium-ion batteries for the past 30 years due to its low de-/lithiation voltage, high theoretical capacity of 372 mAh/g, low price, and long life properties. Recently, all-solid-state lithium-ion batteries (ASSLB), which are composed of inorganic solid materials with high stability, have received great attention as electric vehicles and next-generation energy storage devices, but research works on graphite that works well for ASSLB systems are insufficient. Therefore, we induced the performance improvement of ASSLB anode electrode graphite material by removing the amorphous carbon present in the carbon material surface, acting as a resistive layer from the graphite. As a result of X-ray diffraction (XRD) analysis using heat treated graphite in air at 400, 500, and 600 ℃, the full width at half maximum (FWHM) at (002) peak was reduced compared to that of bare graphite, indicating that the crystallinity of graphite was improved after heat treatment. In addition, the discharge capacity, initial coulombic efficiency (ICE) and cycle stability increased as the crystallinity of graphite increased after heat treatment. In the case of graphite annealed in air at 500 ℃, the high capacity retention rate of 331.1 mAh/g and ICE of 86.2% and capacity retention of 92.7% after 10-cycle measurement were shown.

• Journal of the Korean Electrochemical Society
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• v.16 no.2
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• pp.59-64
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• 2013

Using $Na_2CO_3$ and $MeSO_4$ (Me = Ni, Co and Mn) as starting materials, the precursor of $[Ni_{0.6}Co_{0.2}Mn_{0.2}]CO_3$ has been synthesized by carbonate co-precipitation. The precursor was mixed with $Li_2CO_3$, and calcined at 750, 850, and$950^{\circ}C$ in air. Effect of calcinations temperature on characteristics of $Li[Ni_{0.6}Co_{0.2}Mn_{0.2}]O_2$ cathode materials was investigated. The structure and characteristics of $Li[Ni_{0.6}Co_{0.2}Mn_{0.2}]O_2$ were determined by X-ray diffraction (XRD), Scanning electron microscopy (SEM) and electrochemical measurements. The X-ray diffraction (XRD) results show that the intensity ratio of $I_{(003)}/I_{(104)}$ increased and the R-factor ratio decreased with the increase of calcinations temperature. And Scanning electron microscopy (SEM) result show that the primary particle size increased. Especially, the $Li[Ni_{0.6}Co_{0.2}Mn_{0.2}]O_2$ calcined at $950^{\circ}C$ for 24 H shows excellent electrochemical performances with reversible specific capacity of $165.3mAhg^{-1}$ [cut-off voltage 2.5~4.3 V, 0.1 C($17mAhg^{-1}$)] and good capacity retention of 95.4% after 50th charge/discharge cycles[cut-off voltage 2.5~4.3 V, 1 C($170mAhg^{-1}$)].

• Journal of the Korean Vacuum Society
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• v.10 no.1
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• pp.44-50
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• 2001

Metal oxide semiconductor (MOS) structures containing nanocrystals are fabricated by using rapid thermal oxidations of amorphous silicon films. The amorphous films are deposited either by electron beam deposition method or by electron beam deposition assisted by Ar ion beam during deposition. Post oxidation of e-beam deposited film results in relatively small hysteresis of capacitance-voltage (C-V) and the flat band voltage shift, $\DeltaV_{FB}$ is less than 1V indicative of the formation of low density nanocrystals in $SiO_2$ near $SiO_2$/Si interface. By contrast, we observe very large hysteresis in C-V characteristics for oxidized ion-beam assisted e-beam deposited sample. The flat band voltage shift is larger than 22V and the hysteresis becomes even broader as increasing injection times of holes at accumulation condition and electrons at inversion condition. The result indicates the formation of slow traps in $SiO_2$ near $SiO_2$/Si interface which might be related to large density nanocrystals. Roughly estimated trap density is $1{\times}10^{13}cm^{-2}$. Such a large hysteresis may be explained in terms of the activation of adatom migration by Ar ion during deposition. The activated migration may increase nucleation rate of Si nuclei in amorphous Si matrix. During post oxidation process, nuclei grow into nanocrystals. Therefore, ion beam assistance during deposition may be very feasible for MOS structure containing nanocrystals with large density which is a basic building block for single electron memory device.