• Korean Journal of Materials Research
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• v.9 no.1
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• pp.14-17
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• 1999

Tin oxide films as an anode layer for microbatteries were deposited by using rf magnetron sputtering. Characterization of the films was carried out in terms of working pressure in the range of 5~30 mtorr. Rf power and substrate temperature during deposition were fixed at 2.5W/$\textrm{cm}^2$ and A.T., respectively. The crystal orientation of $SnO_2$films was changed from (110) to (101) or (211) with the increasing working pressure. Refractive index and film density of the films also decreased with the increasing working pressure. The $SnO_2$ thin film formed under optimum conditions was found to have a reversible capacity of 446.9$\mu$Ah/$\textrm{cm}^2$-$\mu\textrm{m}$ and good reversibility when the working pressure was fixed at 10mtorr. As the working pressure decreased, film density increased. It was thought that the capacity of $SnO_2$films increased due to the increase in the amount of active materials which can react with Li electrochemically. Furthermore, cycle characteristics of the anode material was also influenced by film stress.

• Journal of the Korean Vacuum Society
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• v.21 no.1
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• pp.12-16
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• 2012

Although silver is used for T-OLED (Top emitting organic Light-Emitting Diode) as reflective anode, it is not an ideal material due to its low work function. Thus, we study the effect of annealing and atmospheric pressure plasma treatment on Ag film that increases its work function by forming the thin silver oxide layer on its surface. In this study, we deposited silver on glass substrate using RF sputtering. Then we treated the Ag samples annealing at $300^{\circ}C$ for 30 minutes in atmosphere or treating the atmospheric plasma treatment for 30, 60, 90, 120s, respectively. We measured the change of the mechanical properties and the potential value of surface with each one at a different treatment type and time. We used nano-indenter system and KPFM (Kelvin Probe Force Microscopy). KPFM method can be measured the change of surface potential. The nanoindenter results showed that the plasma treatment samples for 30s, 120s had very low elastic modulus, hardness and Weibull modulus. However, annealed sample and plasma treated samples for 60s and 90s had better mechanical properties. Therefore, plasma treatment increases the uniformity thin film and the surface potential that is very effective for the performace of T-OLED.

• Journal of the Korean Electrochemical Society
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• v.15 no.4
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• pp.207-215
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• 2012

Soft carbons are prepared by heat-treatment of cokes with different amounts of phosphoric acid (2, 4.5, and 10 wt% vs. cokes) at $900^{\circ}C$ to be used as anode materials for lithium ion batteries. From electrochemical measurements combined with structural analyses, we confirm that abundant nano-pores are existed in the microstructure of soft carbons prepared with the phosphoric acid, which are responsible for further lithium ion storage. Significant increase in reversible capacity of soft carbon is attained in proportion to added amount of the phosphoric acid. We also demonstrate the effect of structural modification with phosphoric acid on electrochemical performance of soft carbon to elucidate the origin of additional capacity.

• Korean Chemical Engineering Research
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• v.50 no.1
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• pp.25-29
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• 2012

$TiO_2$ nanotubes are prepared from rutile prticles via an alkaline hydrothermal synthesis and the consequent heat treatment at $300{\sim}500^{\circ}C$. The physical and electrochemical properties of the $TiO_2$ nanotubes are characterized for use as a anode material of rechargeable lithium battery. In particular, the microscale dusts as an impurity component occurred in the purification step after the hydrothermal reaction are completely removed to yield $TiO_2$ nanotube with a higher specific surface area and more obvious crystalline phases. As the annealing temperature increases, the specific surface area is slightly decreased due to some aggregation between the isotropically dispersed nanotubes. Highest initial discharge capacity of 250 mAh $g^{-1}$ is achieved for the $TiO_2$ nanotube annealed at $300^{\circ}C$, whereas the $400^{\circ}C$ $TiO_2$ nanotube shows the superior cycle performance and high-rate capability.

• Korean Chemical Engineering Research
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• v.51 no.4
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• pp.411-417
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• 2013

To use as an anode material of lithium secondary battery, graphite-silicon composite powders are prepared by ball-milling with silicon nanoparticles (average diameter 100 nm, 0~50 wt%) and graphite powder (average diameter $15{\mu}m$) and their electrochemical properties are examined. As the silicon content increases, the graphite becomes smaller by the ball-milling and amorphous phase appears whereas the silicon do not suffer the change of nanocrystalline phases and embeds within the amorphous phase of graphite. Cyclic voltammetry at low scan rate reveals that typical oxidation peaks of graphite and silicon appear at 0.2~0.35 and 0.55~0.6 V, respectively, with higher reversibility for repeated cycles. In contrast, the high-scan-rate redox behavior is very irreversible for repeated cycles. High irreversible capacity is exhibited in the initial charging-discharging cycles, but it diminishes as the cycle number increases. The saturated discharge capacity achieves about 485 mAh $g^{-1}$ at 50th cycle for the composite of Si 20 wt%. This is due to the formation of amorphous graphite morphology by the adequate composition (C:Si=8:2 w/w), which efficiently buffers the volume change during alloying/dealloying between silicon and lithium.

• Applied Chemistry for Engineering
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• v.33 no.5
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• pp.496-501
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• 2022

In this study, an anode material for lithium secondary batteries was manufactured using petroleum-based residual oil, which is a petroleum refining by-product. Among petroleum-based residual oils, pyrolysis fuel oil (PFO), fluidized catalyst cracking-decant oil (FCC-DO), and vacuum residue (VR) were used as carbon precursors. The physicochemical characteristics of petroleum-based residual oil were confirmed through Matrix-assisted laser desorption/ionization Time-of-Flight (MALDI-TOF) and elemental analysis (EA), and the structural characteristics of anode materials manufactured from residual oil were evaluated using X-ray crystallography (XRD) and Raman spectroscopic techniques. VR was found to contain a wide range of molecular weight distributions and large amounts of impurities compared to PFO and FCC-DO, and PFO and FCC-DO exhibited almost similar physicochemical characteristics. From the XRD analysis results, carbonized PFO and FCC-DO showed similar d₀₀₂ values. However, it was confirmed that FCC-DO had a more developed layered structure than PFO in Lc (Length of a and c axes in the crystal system) and La values. In addition, FCC-DO showed the best cycle characteristics in electrochemical characteristics evaluation. According to the physicochemical and electrochemical results of the petroleum-based residual oil, FCC-DO is a better carbon precursor for a lithium secondary battery than PFO and VR.

• Applied Chemistry for Engineering
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• v.20 no.3
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• pp.296-300
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• 2009

Generation of chlorine dioxide ($ClO_2$) was studied by the un-divided electrochemical cell system using $RuO_2$ anode material. Sodium chlorite ($NaClO_2$) was used as a precursor compound of chlorine dioxide. Effect of various operating parameters such as feed solution flow rate, initial solution pH, $NaClO_2$ and NaCl conc., and applied current density on the produced chlorine dioxide concentration and solution pH were investigated in un-divided electrochemical cell system. Produced chlorine dioxide concentration and solution pH were strongly depends on the initial solution pH and feed solution flow rate. Sodium chloride (NaCl) was not only good electrolyte, it was also used as a raw material of chlorine dioxide with $NaClO_2$. Observed optimum conditions were flow rate of feed solution (90 mL/min), initial pH (2.3), $NaClO_2$ concentration (4.7 mM), NaCl concentration (100 mM), and current density ($5A/dm^2$). Produced chlorine dioxide concentration was around 350 mg/L and solution pH was around 3.

• 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.31 no.5
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• pp.514-519
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• 2020

Graphite materials for lithium ion battery anode materials are the most commercially available due to their structural stability and low price. Recently, research efforts have been conducted on carbon coatings by improving side reactions at the edge site of carbon materials. The carbon coating process has classified into a CVD by chemical reaction, wet coating process with solvent and dry coating by mechanical impact. In this paper, the rapid crush/coating process was used to solve the problem of which only few parts of the carbon precursor (pitch) can be used and also environmental problems caused by solvent removal in the wet coating process. When the ratio of needle coke to pitch was 8 : 2 wt%, and the rapid crush/coating process was carried out, it was confirmed that the fracture surface was coated by pitch. The pitch-coated sample was treated at 2400 ℃ and 41.8% improvement in 10C/0.1C rate characteristic was observed. It is considered that the material simply manufactured through the simple crush/coating process can be used as an anode electrode material for a lithium ion battery.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2008.06a
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• pp.241-241
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• 2008

Macrofore formation in silicon and other semiconductors using electrochemical etching processes has been, in the last years, a subject of great attention of both theory and practice. Its first reason of concern is new areas of macropore silicone applications arising from microelectromechanical systems processing (MEMS), membrane techniques, solar cells, sensors, photonic crystals, and new technologies like a silicon-on-nothing (SON) technology. Its formation mechanism with a rich variety of controllable microstructures and their many potential applications have been studied extensively recently. Porous silicon is formed by anodic etching of crystalline silicon in hydrofluoric acid. During the etching process holes are required to enable the dissolution of the silicon anode. For p-type silicon, holes are the majority charge carriers, therefore porous silicon can be formed under the action of a positive bias on the silicon anode. For n-type silicon, holes to dissolve silicon is supplied by illuminating n-type silicon with above-band-gap light which allows sufficient generation of holes. To make a desired three-dimensional nano- or micro-structures, pre-structuring the masked surface in KOH solution to form a periodic array of etch pits before electrochemical etching. Due to enhanced electric field, the holes are efficiently collected at the pore tips for etching. The depletion of holes in the space charge region prevents silicon dissolution at the sidewalls, enabling anisotropic etching for the trenches. This is correct theoretical explanation for n-type Si etching. However, there are a few experimental repors in p-type silicon, while a number of theoretical models have been worked out to explain experimental dependence observed. To perform ordered macrofore formaion for p-type silicon, various kinds of mask patterns to make initial KOH etch pits were used. In order to understand the roles played by the kinds of etching solution in the formation of pillar arrays, we have undertaken a systematic study of the solvent effects in mixtures of HF, N-dimethylformamide (DMF), iso-propanol, and mixtures of HF with water on the macrofore structure formation on monocrystalline p-type silicon with a resistivity varying between 10 ~ 0.01 $\Omega$ cm. The etching solution including the iso-propanol produced a best three dimensional pillar structures. The experimental results are discussed on the base of Lehmann's comprehensive model based on SCR width.