• Journal of the Korean institute of surface engineering
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• v.32 no.3
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• pp.235-238
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• 1999

Silicon dioxide films were prepared by anodizing silicon wafers in an ethylene $glycol+HNO_3(0.04{\;}N)$ at 20 to $70^{\circ}C$. The voltage between silicon anode and platinum cathode was measured during this process. Under the constant current electrolysis, the voltage increased with oxide film growth. The transition time at which the voltage reached the predetermined value depended on the temperature of the electrolyte. After the time of electrolysis reached the transition time, the anodization was changed the constant voltage mode. The depth profile of oxide film/Si substrate was confirmed by XPS analysis to study the influence of the electrolyte temperature on the anodization. Usually, the oxide-silicon peaks disappear in the silicon substrate, however, this peak was not small at $45^{\circ}C$ in this region.

• Corrosion Science and Technology
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• v.21 no.6
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• pp.445-453
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• 2022

SiO_x was prepared from a mixture of Si and SiO₂ via high-energy ball milling as a negative electrode material for Li-ion batteries. The molar ratio of Si to SiO₂ as precursors and the milling time were varied to identify the synthetic condition that could exhibit desirable anode performances. With an appropriate milling time, the material showed a unique microstructure in which amorphous Si nanoparticles were intimately embedded within the SiO₂ matrix. The interface between the Si and SiO₂ was composed of silicon suboxides with Si oxidation states from 0 to +4 as proven by X-ray photoelectron spectroscopy and electrochemical analysis. With the addition of a conductive carbon (Super P carbon black) as a coating material, the SiO_x/C manifested superior specific capacity to a commercial SiO_x/C composite without compromising its cycle-life performance. The simple mechanochemical method described in this study will shed light on cost-effective synthesis of high-capacity silicon oxides as promising anode materials.

• Transactions on Electrical and Electronic Materials
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• v.15 no.4
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• pp.193-197
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• 2014

Si-carbon composites as anode materials for lithium rechargeable batteries were prepared simply by mixing Si nanoparticles with carbon black and/or graphite through a solution process. Si nanoparticles were well dispersed and deposited on the surface of the carbon in a tetrahydrofuran solution. Si-carbon composites showed more than 700 mAh/g of initial capacity under less than 20% loading of Si nanoparticle in the composites. While the electrode with only Si nanoparticles showed fast capacity fading during continuous cycling, Si-carbon composite electrodes showed higher capacities. The cycle performances of Si nanoparticles in composites containing graphite were improved due to the role of the graphite as a matrix.

• Journal of Electrochemical Science and Technology
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• v.4 no.3
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• pp.108-112
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• 2013

Lithium diffusivity of the silicon (Si)-based materials of Si-Cu and $SiO_x$ (x = 0.4, 0.85) with improved interfacial stability to electrolyte have been determined, using variable rate cyclic voltammetry with film model electrodes. Lithium diffusivity is found to depend on the intrinsic properties of anode material and electrolyte; the fraction of oxygen for $SiO_x$ (x = 0.4, 0.85), which is directly related to electrical conductivity, and the electrolyte type with different ionic conductivity and viscosity, carbonate-based liquid electrolyte or ionic liquid-based electrolyte, affect the lithium diffusivity.

• Journal of Korean Vacuum Science & Technology
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• v.3 no.1
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• pp.54-58
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• 1999

We deposited diamond-like carbon (DLC) films using ion beam sputtering of a graphite target on flat substrates for use as a thin film field emitter. An n-type silicon wafer, titanium-coated silicon, and indium tin oxide (ITO) coated glass were used as a substrate. All films exhibited a sudden increase in the emission after a breakdown occurred at high voltage. The morphology of the films after the breakdown depended on the substrate. On ITO and Ti substrates, the DLC film peeled off upon breakdown, but on the Si substrate the surface melting due to breakdown resulted in the formation of various structures such as a sharp point, mound, and crater. By scanning the deformed surface with a tip anode, we found that the emission was concentrated at the deformed sites, indicating that the field enhancement due to the morphology change was responsible for the increased emission.

• 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.

• Journal of Powder Materials
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• v.24 no.1
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• pp.24-28
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• 2017

Silicon alloys are considered promising anode active materials to replace Li-ion batteries by graphite powder, because they have a relatively high capacity of up to 4200 mAh/g, and are environmentally friendly and inexpensive ECO-materials. However, its poor charge/discharge properties, induced by cracking during cycles, constitute their most serious problem as anode electrode. In order to solve these problems, Si-Ge-Al alloys with porous structure are designed as anode alloy powders, to improve cycling stability. The alloys are melt-spun to obtain the rapidly solidified ribbons, and then ball-milled to make fine powders. The powders are etched using 1 M HCl solution, which gives the powders a porous structure by removing the element Al. Subsequently, in this study, the microstructures and the characteristics of the etched powders are evaluated for application as anode materials. As a result, the etched porous powder shows better electrochemical properties than as-milled Si-Ge-Al powder.

• Proceedings of the Korean Vacuum Society Conference
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• 2009.02a
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• pp.192.1-192.1
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• 2009

• Proceedings of the Materials Research Society of Korea Conference
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• 2005.05a
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• pp.207-207
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• 2005

• Korean Journal of Materials Research
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• v.34 no.7
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• pp.370-376
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• 2024

In this study, we report significant improvements in lithium-ion battery anodes cost and performance, by fabricating nano porous silicon (Si) particles from Si wafer sludge using the metal-assisted chemical etching (MACE) process. To solve the problem of volume expansion of Si during alloying/de-alloying with lithium ions, a layer was formed through nitric acid treatment, and Ag particles were removed at the same time. This layer acts as a core-shell structure that suppresses Si volume expansion. Additionally, the specific surface area of Si increased by controlling the etching time, which corresponds to the volume expansion of Si, showing a synergistic effect with the core-shell. This development not only contributes to the development of high-capacity anode materials, but also highlights the possibility of reducing manufacturing costs by utilizing waste Si wafer sludge. In addition, this method enhances the capacity retention rate of lithium-ion batteries by up to 38 %, marking a significant step forward in performance improvements.