• Korean Journal of Materials Research
• /
• v.26 no.9
• /
• pp.486-492
• /
• 2016

Tungsten (W) thin film was deposited at $400^{\circ}C$ using pulsed chemical vapor deposition (pulsed CVD); film was then evaluated as a nucleation layer for W-plug deposition at the contact, with an ultrahigh aspect ratio of about 14~15 (top opening diameter: 240~250 nm, bottom diameter: 98~100 nm) for dynamic random access memory. The deposition stage of pulsed CVD has four steps resulting in one deposition cycle: (1) Reaction of $WF_6$ with $SiH_4$. (2) Inert gas purge. (3) $SiH_4$ exposure without $WF_6$ supply. (4) Inert gas purge while conventional CVD consists of the continuous reaction of $WF_6$ and $SiH_4$. The pulsed CVD-W film showed better conformality at contacts compared to that of conventional CVD-W nucleation layer. It was found that resistivities of films deposited by pulsed CVD were closely related with the phases formed and with the microstructure, as characterized by the grain size. A lower contact resistance was obtained by using pulsed CVD-W film as a nucleation layer compared to that of the conventional CVD-W nucleation layer, even though the former has a higher resistivity (${\sim}100{\mu}{\Omega}-cm$) than that of the latter (${\sim}25{\mu}{\Omega}-cm$). The plan-view scanning electron microscopy images after focused ion beam milling showed that the lower contact resistance of the pulsed CVD-W based W-plug fill scheme was mainly due to its better plug filling capability.

• Journal of the Korean Vacuum Society
• /
• v.17 no.5
• /
• pp.473-480
• /
• 2008

We have investigated the optimal growth conditions of carbon nanotubes (CNTs) using the chemical vapor deposition and the Ni nanoparticle arrays. The diameter of the CNT is shown to be controlled down to below 20 nm by changing the size of Ni particle. The position and size of Ni particles are controlled continuously by using wafer-scale compatible methods such as lithography, ion-milling, and chemical etching. Using optimal growth conditions of temperature, carbon feedstock, and carrier gases, we have demonstrated that an individual CNT can be grown from each Ni nanoparticle with almost 100% probability over wide area of $SiO_2/Si$ wafer. The position, diameter, and wall thickness of the CNT are shown to be controlled by adjusting the growth conditions.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
• /
• v.30 no.4
• /
• pp.246-252
• /
• 2017

Pulverized $FeS_2$ (pyrite) gives different discharge test results with as-received $FeS_2$ electrodes. The as-received $FeS_2$ electrode shows three voltage plateaus during the discharge test. However, the ball-milled $FeS_2$ electrode shows two voltage plateaus. To interpret this result, the effect of $FeS_2$ particle size on electrochemical reactions is investigated by unit cell discharge tests, SEM and XRD. As a result, it is found that the transition reaction product ($Li_2+xFe+xS_2$) of $FeS_2$ explains the difference. The as-received $FeS_2$ reacts according to three reaction steps ($FeS_2{\rightarrow}Li_3Fe_2S_4{\rightarrow}Li_2+xFe_1+xS_2{\rightarrow}LiFe_2S_4$). However, ball-milled $FeS_2$ reacts without the $Li_2+xFe_1+xS_2$ stage. In this study, this result is explained by the difference in electrochemical reaction mechanism. The as-received $FeS_2$ has a larger radius than the ball-milled $FeS_2$. Therefore, the lithium ion has to diffuse into the $FeS_2$ unreacted core, and $Li_2+xFe_1+xS_2$, the transition reaction product of as-received $FeS_2$, is formed during this stage.

• Korean Journal of Metals and Materials
• /
• v.49 no.2
• /
• pp.174-179
• /
• 2011

We investigated the surface morphology changes of a lithium/sulfur battery using multi-walled canbon nanotube added sulfur electrode during charge-discharge cycling. The Li/S cell showed the first discharge capacity of 1286 mAh/g-S, which utilized is 71% of the theoretical value. It decreased to 328 mAh/g-S at the 100th cycle, which corresponds to about 19% utilization of the total sulfur in the cathode. The spherical lumps of the reaction product were observed on the surface of the sulfur electrode. This material was verified as lithium sulfide by X-ray diffraction measurement. The pores in the separator were filled with reaction product. Thus the diffusion of the $Li^+$ ion decreased, which resulted in the decreased capacity of the Li/S cell.

• Journal of Powder Materials
• /
• v.28 no.6
• /
• pp.497-501
• /
• 2021

Cobalt (Co) is mainly used to prepare cathode materials for lithium-ion batteries (LIBs) and binder metals for WC-Co hard metals. Developing an effective method for recovering Co from WC-Co waste sludge is of immense significance. In this study, Co is extracted from waste cemented carbide soft scrap via mechanochemical milling. The leaching ratio of Co reaches approximately 93%, and the leached solution, from which impurities except nickel are removed by pH titration, exhibits a purity of approximately 97%. The titrated aqueous Co salts are precipitated using oxalic acid and hydroxide precipitation, and the effects of the precipitating agent (oxalic acid and hydroxide) on the cobalt microstructure are investigated. It is confirmed that the type of Co compound and the crystal growth direction change according to the precipitation method, both of which affect the microstructure of the cobalt powders. This novel mechanochemical process is of significant importance for the recovery of Co from waste WC-Co hard metal. The recycled Co can be applied as a cemented carbide binder or a cathode material for lithium secondary batteries.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.20 no.3
• /
• pp.141-146
• /
• 2010

$LiFePO_4$ doped with Cr showed improved electrochemical properties as a cathode material of lithium-ion batteries compared to the undoped. The improvement was thought that the doping would raise the electronic conductivity of the compounds. The electrical conductivity of $LiFe_{0.965}Cr_{0.03}B_{0.005}PO_4$ and $LiFe_{0.965}Cr_{0.03}Al_{0.005}PO_4$ powder was measured in the temperature range from 30 to $80^{\circ}C$. The doped powders were synthesized via mechanochemical milling and subsequent heat treatment at 675~$750^{\circ}C$ for 5~10h. The doping enhanced grain growth and electrical conductivity. The electrical conductivity of the $LiFe_{0.965}Cr_{0.03}Al_{0.005}PO_4$ powder at $30^{\circ}C$ was $1{\times}10^{-8}S/cm$, which was higher two orders of magnitude than that of the undoped.

• Journal of the Korean Electrochemical Society
• /
• v.15 no.2
• /
• pp.67-73
• /
• 2012

Spherical lithium manganese oxide spinel, $LiMn_{2-x}M_xO_4$ (M = Al, Mg, B) prepared by wet-milling, spray-drying, and sintering process has been investigated as a cathode material for lithium ion batteries. As-prepared powders exhibit various surface morphologies and internal density in terms of boron (B) doping level. It is found that the dopant B drives the growth of the primary particle and minimizes the surface area of the powder. As a result, the dopant enhances the internal density of the particles. Electrochemical tests demonstrated that the capacity of the synthesized material at 5 C could be maintained up to 90% of that at 0.2 C. The cycle performance of the material showed that the initial capacity was retained up to 80% even after 500 cycles under the high temperature of $60^{\circ}C$.

• Applied Chemistry for Engineering
• /
• v.26 no.5
• /
• pp.543-548
• /
• 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.

• Journal of the Korean Electrochemical Society
• /
• v.11 no.1
• /
• pp.47-50
• /
• 2008

A new anode composition material comprising of SiO and Graphite has been prepared by adopting High energy ball milling (HEBM) technique. The anode material shows high initial charge and discharge capacity values of 1139 and 568 mAh/g, respectively. The electrode sustains reversible discharge capacity value of 719 mAh/g at 30th cycle with a high coulombic efficiency${\sim}99%$. Since the materials formed during initial charge process the nano silicon/$Li_4SiO_3$ and $Li_2O$ remains as interdependent, it may be expected that the composite exhibiting higher amount of irreversibility$(Li_2O)$ will deliver higher reversible capacity. In this study, constant current-constant voltage (CC-CV) charge method was employed in place of usual constant current (CC) method in order to convert efficiently all the SiO particles which resulted high initial discharge capacity at the first cycle. We improved considerably the initial discharge specific capacity of SiO/G composite by pretreatment(CC-CV).

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
• /
• v.7 no.3
• /
• pp.175-182
• /
• 2009

The spent cationic exchange resins and anionic exchange resins were separated from mixed spent exchange resins by a fluidized bed gravimetric separator. The separated resins were identified by an elemental analysis and thermogravimetric analysis. The each test sample was prepared by diluting the slurry made by wet ball milling the cationic exchange resins and the anionic exchange resins separated as a spherical granular form for 24 hours. The resulting test samples showed a slurry form of less than $75{\mu}m$ of particle size and 25,000ppm of $COD_{cr}$. The decomposition conditions of each test samples from a thermal power plant were obtained with a lab-scale(reactor volume : 220mL) supercritical water oxidation(SCWO) facility. Then pilot plant(reactor volume : 24 L) tests were performed with the test samples from a thermal power plant and a nuclear power plant successively. Based on the optimal decomposition conditions and the operation experiences by lab-scale facility and the pilot plant, a commercial plant(capacity : 150kg/h) can be installed in a nuclear power plant was designed.