• Proceedings of the Materials Research Society of Korea Conference
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• 2011.05a
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• pp.5-5
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• 2011

The research and development of hybrid electric vehicle (HEV), plug-in hybrid electric vehicle (PHEV) and electric vehicle (EV) are intensified due to the energy crisis and environmental concerns. In order to meet the challenging requirements of powering HEV, PHEV and EV, the current lithium battery technology needs to be significantly improved in terms of the cost, safety, power and energy density, as well as the calendar and cycle life. One new technology being developed is the utilization of composite cathode by mixing two different types of insertion compounds [e.g., spinel $LiMn_2O_4$ and layered $LiMO_2$ (M=Ni, Co, and Mn)]. Recently, some studies on mixing two different types of cathode materials to make a composite cathode have been reported, which were aimed at reducing cost and improving self-discharge. Numata et al. reported that when stored in a sealed can together with electrolyte at $80^{\circ}C$ for 10 days, the concentrations of both HF and $Mn^{2+}$ were lower in the can containing $LiMn_2O_4$ blended with $LiNi_{0.8}Co_{0.2}O_2$ than that containing $LiMn_2O_4$ only. That reports clearly showed that this blending technique can prevent the decline in capacity caused by cycling or storage at elevated temperatures. However, not much work has been reported on the charge-discharge characteristics and related structural phase transitions for these composite cathodes. In this presentation, we will report our in situ x-ray diffraction studies on this mixed composite cathode material during charge-discharge cycling. The mixed cathodes were incorporated into in situ XRD cells with a Li foil anode, a Celgard separator, and a 1M $LiPF_6$ electrolyte in a 1 : 1 EC : DMC solvent (LP 30 from EM Industries, Inc.). For in situ XRD cell, Mylar windows were used as has been described in detail elsewhere. All of these in situ XRD spectra were collected on beam line X18A at National Synchrotron Light Source (NSLS) at Brookhaven National Laboratory using two different detectors. One is a conventional scintillation detector with data collection at 0.02 degree in two theta angle for each step. The other is a wide angle position sensitive detector (PSD). The wavelengths used were 1.1950 ${\AA}$ for the scintillation detector and 0.9999 A for the PSD. The newly installed PSD at beam line X18A of NSLS can collect XRD patterns as short as a few minutes covering $90^{\circ}$ of two theta angles simultaneously with good signal to noise ratio. It significantly reduced the data collection time for each scan, giving us a great advantage in studying the phase transition in real time. The two theta angles of all the XRD spectra presented in this paper have been recalculated and converted to corresponding angles for ${\lambda}=1.54\;{\AA}$, which is the wavelength of conventional x-ray tube source with Cu-$k{\alpha}$ radiation, for easy comparison with data in other literatures. The structural changes of the composite cathode made by mixing spinel $LiMn_2O_4$ and layered $Li-Ni_{1/3}Co_{1/3}Mn_{1/3}O_2$ in 1 : 1 wt% in both Li-half and Li-ion cells during charge/discharge are studied by in situ XRD. During the first charge up to ~5.2 V vs. $Li/Li^+$, the in situ XRD spectra for the composite cathode in the Li-half cell track the structural changes of each component. At the early stage of charge, the lithium extraction takes place in the $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ component only. When the cell voltage reaches at ~4.0 V vs. $Li/Li^+$, lithium extraction from the spinel $LiMn_2O_4$ component starts and becomes the major contributor for the cell capacity due to the higher rate capability of $LiMn_2O_4$. When the voltage passed 4.3 V, the major structural changes are from the $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ component, while the $LiMn_2O_4$ component is almost unchanged. In the Li-ion cell using a MCMB anode and a composite cathode cycled between 2.5 V and 4.2 V, the structural changes are dominated by the spinel $LiMn_2O_4$ component, with much less changes in the layered $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ component, comparing with the Li-half cell results. These results give us valuable information about the structural changes relating to the contributions of each individual component to the cell capacity at certain charge/discharge state, which are helpful in designing and optimizing the composite cathode using spinel- and layered-type materials for Li-ion battery research. More detailed discussion will be presented at the meeting.

• Journal of Sensor Science and Technology
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• v.19 no.4
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• pp.291-296
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• 2010

Recently, recycling method of waste wafer has been an area of solar cell to cut costs. Micro_blasting is one of the promising candidates for recycling of waste wafer due to their extremely simple and cost-effective process. In this paper, we attempt to explore the effect of micro_blasting and DRE(damage removal etching) process for solar cell. The optimal process conditions of micro_blasting are as follows: $10{\mu}m$ sized $Al_2O_3$ powder, jetting pressure of 400 kPa, and scan_speed of 30 cm/s. And the particles formed on micro_blasted wafer were removed by DRE precess which was performed by using HNA(HF/$HNO_3$/$CH_3COOH$) and TMAH(tetramethyl ammonium hydroxide). Structural analysis was done using a-step and the XRD patterns.

• Korean Journal of Materials Research
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• v.27 no.9
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• pp.501-506
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• 2017

Surface morphology and optical properties such as transmittance and haze effect of glass etched by physical and chemical etching processes were investigated. The physical etching process was carried out by pen type sandblasting process with $15{\sim}20{\mu}m$ dia. of $Al_2O_3$ media; the chemical etching process was conducted using HF-based mixed etchant. Sandblasting was performed in terms of variables such as the distance of 8 cm between the gun nozzle and the glass substrate, the fixed air pressure of 0.5bar, and the constant speed control of the specimen stage. The chemical etching process was conducted with mixed etching solution prepared by combination of BHF (Buffered Hydrofluoric Acid), HCl, and distilled water. The morphology of the glass surface after sandblasting process displayed sharp collision vestiges with nonuniform shapes that could initiate fractures. The haze values of the sandblasted glass were quantitatively acceptable. However, based on visual observation, the desirable Anti-Glare effect was not achieved. On the other hand, irregularly shaped and sharp vestiges transformed into enlarged and smooth micro-spherical craters with the subsequent chemical etching process. The curvature of the spherical crater increased distinctly by 60 minutes and decreased gradually with increasing etching time. Further, the spherical craters with reduced curvature were uniformly distributed over the etched glass surface. The haze value increased sharply up to 55 % and the transmittance decreased by 90 % at 60 minutes of etching time. The ideal haze value range of 3~7 % and transmittance value range of above 90 % were achieved in the period of 240 to 720 minutes of etching time for the selected concentration of the chemical etchant.