• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2009.06a
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• pp.104-104
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• 2009

Critical dimensions has rapidly shrunk to increase the degree of integration and to reduce the power consumption. However, it is accompanied with several problems like direct tunneling through the gate insulator layer and the low conductivity characteristic of poly-silicon. To cover these faults, the study of new materials is urgently needed. Recently, high dielectric materials like $Al_2O_3$, $ZrO_2$ and $HfO_2$ are being studied for equivalent oxide thickness (EOT). However, poly-silicon gate is not compatible with high-k materials for gate-insulator. To integrate high-k gate dielectric materials in nano-scale devices, metal gate electrodes are expected to be used in the future. Currently, metal gate electrode materials like TiN, TaN, and WN are being widely studied for next-generation nano-scale devices. The TaN gate electrode for metal/high-k gate stack is compatible with high-k materials. According to this trend, the study about dry etching technology of the TaN film is needed. In this study, we investigated the etch mechanism of the TaN thin film in an inductively coupled plasma (ICP) system with $O_2/BCl_3/Ar$ gas chemistry. The etch rates and selectivities of TaN thin films were investigated in terms of the gas mixing ratio, the RF power, the DC-bias voltage, and the process pressure. The characteristics of the plasma were estimated using optical emission spectroscopy (OES). The surface reactions after etching were investigated using X-ray photoelectron spectroscopy (XPS) and auger electron spectroscopy (AES).

• 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.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2010.06a
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• pp.11-11
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• 2010

Thin-film-transistors (TFTs) that can be deposited at low temperature have recently attracted lots of applications such as sensors, solar cell and displays, because of the great flexible electronics and transparent. Transparent and flexible transistors are being required that high mobility and large-area uniformity at low temperature [1]. But, unfortunately most of TFT structures are used to be $SiO_2$ as gate dielectric layer. The $SiO_2$ has disadvantaged that it is required to high driving voltage to achieve the same operating efficiency compared with other high-k materials and its thickness is thicker than high-k materials [2]. To solve this problem, we find lots of high-k materials as $HfO_2$, $ZrO_2$, $SiN_x$, $TiO_2$, $Al_2O_3$. Among the High-k materials, $Al_2O_3$ is one of the outstanding materials due to its properties are high dielectric constant ( ~9 ), relatively low leakage current, wide bandgap ( 8.7 eV ) and good device stability. For the realization of flexible displays, all processes should be performed at very low temperatures, but low temperature $Al_2O_3$ grown by sputtering showed deteriorated electrical performance. Further decrease in growth temperature induces a high density of charge traps in the gate oxide/channel. This study investigated the effect of growth temperatures of ALD grown $Al_2O_3$ layers on the TFT device performance. The ALD deposition showed high conformal and defect-free dielectric layers at low temperature compared with other deposition equipments [2]. After ITO was wet-chemically etched with HCl : $HNO_3$ = 3:1, $Al_2O_3$ layer was deposited by ALD at various growth temperatures or lift-off process. Amorphous InGaZnO channel layers were deposited by rf magnetron sputtering at a working pressure of 3 mTorr and $O_2$/Ar (1/29 sccm). The electrodes were formed with electron-beam evaporated Ti (30 nm) and Au (70 nm) bilayer. The TFT devices were heat-treated in a furnace at $300^{\circ}C$ and nitrogen atmosphere for 1 hour by rapid thermal treatment. The electrical properties of the oxide TFTs were measured using semiconductor parameter analyzer (4145B), and LCR meter.

• Journal of the Korean Ceramic Society
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• v.48 no.1
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• pp.1-5
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• 2011

Silicon carbide (SiC) has recently drawn an enormous industrial interest because of its useful mechanical properties such as thermal resistance, abrasion resistance and thermal conductivity at high temperature. RF Thermal plasma (PL-35 Induction Plasma, Tekna CO., Canada) has been utilized for synthesis of high purity SiC powder from cheap inorganic solution (Tetraethyl Orthosilicate, TEOS). It is found that the powders by thermal plasma consist of SiC with free carbon and amorphous silica ($SiO_2$) and, by thermal treatment and HF treatment, the impurities are driven off resulting high purity SiC nano-powder. The synthesized SiC powder lies below 30 nm and its properties such microstructure, phase composition, specific surface area and free carbon content have been characterized by X-ay diffraction (XRD), field emission scanning electron microscopy (FE-SEM), thermogravimetric (TG) and Brunauer-Emmett-Teller (BET).

• Journal of the Korean Ceramic Society
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• v.49 no.6
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• pp.523-527
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• 2012

Silicon carbide (SiC) has recently drawn an enormous amount of industrial interest due to its useful mechanical properties, such as its thermal resistance, abrasion resistance and thermal conductivity at high temperatures. In this study, RF thermal plasma (PL-35 Induction Plasma, Tekna CO., Canada) was utilized for the synthesis of high-purity SiC powder from an organic precursor (hexamethyldisilazane, vinyltrimethoxysilane). It was found that the SiC powders obtained by the RF thermal plasma treatment included free carbon and amorphous silica ($SiO_2$). The SiC powders were further purified by a thermal treatment and a HF treatment, resulting in high-purity SiC nano-powder. The particle diameter of the synthesized SiC powder was less than 30 nm. Detailed properties of the microstructure, phase composition, and free carbon content were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), a thermogravimetric (TG) analysis, according to the and Brunauer-Emmett-Teller (BET) specific surface area from N2 isotherms at 77 K.

• Korean Journal of Materials Research
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• v.34 no.5
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• pp.247-253
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• 2024

The separation of zirconium and hafnium using tributyl phosphate (TBP)-Dodecane extractants in nitric acid medium was performed. Zirconium oxychloride, used as extraction feed, was obtained from the synthesis of Kalimantan zircon sand concentrate smelted using NaOH. The extraction process was carried out by dissolving chloride-based metals in nitric acid media in the presence of sodium nitrate using TBP-Dodecane as an extractant. Some of the extraction parameters carried out in this study include variations in organic phase and aqueous phase (O/A), variations in contact time, and variations in nitric acid concentration. Extraction was carried out using a mechanical shaker according to the parameter conditions. X-ray fluorescence (XRF) was used for elemental (Zr and Hf) composition analysis of the aqueous solution. The results showed that zirconium was separated from hafnium at optimum conditions with an organic/aqueous ratio of 1:5, contact time of 75 min, and an HNO₃ concentration of 7 M. The resulting separation factor of zirconium and hafnium using TBP-Dodecane was 14.4887.

• Journal of the Korea Concrete Institute
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• v.17 no.5 s.89
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• pp.769-774
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• 2005

Fluosilicic acid(H2SiF6) is recovered as an aqueous solution which absorbs $SiF_4$ produced from the manufacturing of industrial-graded H3PO4 or HF. Generally, fluosilicates are the salts produced by the reaction of H2SiF6 and metal salts. Addition of fluosilicates to cement endows odd properties through unique chemical reaction with the fresh and hardened cement. This study was performed to know mechanical properties and watertightness using fluosilicates based composite made from fluosilicates and other compounds. Mix proportions for experiments were modulated at 0.45 of water to cement ratio and $0.0-2.0\%$ of adding ratio of fluosilicates based composite. Evaluation for mechanical properties of concrete was conducted to know fresh state of concrete, hardening state of concrete, and watertightness. Evaluation for watertightness of concrete was carried out permeability, absorption test and porosity analysis. In addition. Scanning Electron Microscopy(SEM) and Energy Dispersive X-Ray(EDX) used for investigating micro-structure and atomic component distributed in hardened concrete. It is ascertained that characteristics of mechanical properties and watertightness was more improved than non-added because of packing role of fluosilicates based composite and pozzolanic reaction of soluble $SiO_2$. Also, concrete added fluosilicates based composite had a tendency to delay setting time and only $0.5\%$ addition of fluosilicates based composite delayed 150 minutes compared with non-added.

• Proceedings of the Korean Vacuum Society Conference
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• 1999.07a
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• pp.115-115
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• 1999

GaN는 직접천이형 wide band gap(3.4eV) 반도체로서 청색/자외선 발광소자 및 고출력 전자장비등에의 응용성 때문에 폭넓게 연구되고 있다. 이러한 넓은 분야의 응용을 위해서는 열 적으로 안정된 Ohmic contact을 반드시 실현되어야 한다. n-type GaN의 경우에는 GaN계면에서의 N vacancy가 n-type carrier로 작용하기 때문에 Ti, Al, 같은 금속을 접합하여 nitride를 형성함에 의해서 낮은 접촉저항을 갖는 Ohmic contact을 하기가 쉽다. 그러나 p-type의 경우에는 일 함수가 크고 n-type와 다르게 nitride가 형성되지 않는 금속이 Ohmic contact을 할 가능성이 많다. 시료는 HF(HF:H2O=1:1)에서 10분간 초음파 세척을 한 후 깨끗한 물에 충분히 헹구었다. 그런 후에 고순도 Ar 가스로 건조시켰다. Pd와 Ni은 열적 증착법(thermal evaporation)을 사용하여 p-GaN에 상온에서 증착하였다. 현 연구에서는 열처리에 의한 Pd의 clustering을 줄이기 위해서 wetting이 좋은 Ni을 Pd 증착 전과 후에 삽입하였으며, monchromatic XPS(x-ray photoelectron spectroscopy) 와 SAM(scanning Auger microscopy)을 사용하여 열처리 전과 40$0^{\circ}C$, 52$0^{\circ}C$ 그리고 695$0^{\circ}C$에서 3분간 열처리 후의 온도에 따른 morphology 변화, 계면반응(interfacial reaction) 및 벤드 휨(band bending)을 비교 연구하였다. Nls core level peak를 사용한 band bending에서 Schottky barrier height는 Pd/Ni bi-layer 접합시 2.1eV를, Ni/Pd bi-layer의 경우에 2.01eV를 얻었으며, 이는 Pd와 Ni의 이상적인 Schottky barrier height 값 2.38eV, 2.35eV와 비교해 볼 때 매우 유사한 값임을 알 수 있다. 시료를 후열처리함에 의해 52$0^{\circ}C$까지는 barrier height는 큰 변화가 없으나, $650^{\circ}C$에서 3분 열처리 후에 0.36eV, 0.28eV 만큼 band가 더 ？을 알 수 있었다. Pd/Ni 및 Ni/Pd 접합시 $650^{\circ}C$까지 후 열 처리 과정에서 계면에서 matallic Ga은 온도에 비례하여 많은 양이 형성되어 표면으로 편석(segregation)되어지나, In-situ SAM을 이용한 depth profile을 통해서 Ni/Pd, Pd/Ni는 증착시 uniform하게 성장함을 알 수 있었으며, 후열처리 함에 의해서 점차적으로 morphology 의 변화가 일어나기 시작함을 볼 수 있었다. 이는 $650^{\circ}C$에서 열처리 한후의 ex-situ AFM을 통해서 재확인 할 수 있었다. 이상의 결과로부터 GaN에 Pd를 접합 시 심한 clustering이 형성되어 Ohoic contact에 문제가 있으나 Pd/Ni 혹은 Ni/Pd bi-layer를 사용함에 의해서 clustering의 크기를 줄일 수 있었다. Clustering의 크기는 Ni/Pd bi-layer의 경우가 작았으며, $650^{\circ}C$ 열처리 후에 barrier height는 Pd/Ni bi-layer의 경우에도 Ni의 영향을 받음을 알 수 있었다.

• Journal of the korean academy of Pediatric Dentistry
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• v.23 no.3
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• pp.640-658
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• 1996

The purpose of this study was to examine the mechanism of improving acid resistance of Nd-YAG laser irradiated tooth enamel and determine the most effective energy density for improving acid resistance. The bovine tooth enamel were lased with a pulsed Nd-YAG laser. The energy densities of exposed laser beam were varied from 10 to $70\;J/cm^2$. To investigate the degree of improving acid resistance by irradiation, all the samples were submerged to demineralize in 0.5 N $HClO_4$ solution for 1 minute. After 1 minute, 0.05 % $LaCl_3$ was added to the solution for interrupting the demineralization reaction. The amounts of dissolved calcium and phosphate in the solution were measured by using an atomic absorption spectrophotometer and the UV/VIS spectrophotometer, respectively. To examine the mechanism of improving acid resistance, X-ray diffraction analysis, infrared spectroscopy, and scanning electron microscopy were taken. The X-ray diffraction pattern of the samples were obtained in the $10^{\circ}{\sim}80^{\circ}2{\theta}$ range with $Cu-K{\alpha}$ radiation using M18HF(Mac Science Co.) with X-ray diffractometer operating at 40 KV and 300 mA. The infra-red spectra of the ground samples in 300 mg KBr pellets 10 mm diameter were obtained in the $4000cm^{-1}\;to\;400cm^{-1}$ range using JASCO 300E spectrophotometer. The scanning electron microscopy was carried out using JSM6400(JEOL Co.) with $500{\sim}2000$ times magnification. The results were as follow 1. The concentration of calcium dissolved from laser irradiated enamel with $50J/cm^2$ was significantly lesser than that of unlased control group (p<0.05) 2. From the result of the X-ray diffraction analysis, $\beta$-TCP, which increases acid solubility, was identified in lased enamel but the diffraction peaks of (002) and (004) became sharp with increasing energy density of laser irradiation. This means that the crystals in lased samples were grown through the c-axis and subsequently, the acid solubility of enamel decreased. 3. The a-axis parameter was slightly increased by laser irradiation, whereas the c-axis parameter was almost constant except for a little decrease at $50J/cm^2$. 4. In the infra-red spectra of lased enamels, phosphate bands ($600{\sim}500cm^{-1}$), B-carbonate bands (870, $1415{\sim}1455cm^{-1}$), and A-carbonate band ($1545cm^{-1}$) were observed. The amounts of phosphate bands and the B-carbonate bands were reduced, on the other hand, the amount of the A-carbonate band was increased by increase the energy density. 5. The SEM experiments reveal that the surface melting and recrystallization were appeared at $30J/cm^2$ and the cracks were observed at $70J/cm^2$. From above results, It may be suggested that the most effective energy density for improving acid resistance of tooth enamel with the irradiation of Nd-YAG laser was $50J/cm^2$. The mechanism of improving acid resistance were reduction of permeability due to surface melting and recrystallization of lased enamel and reduction of acid solubility of enamel due to decrease of carbonate content and growth of crystal.

• Proceedings of the Korean Vacuum Society Conference
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• 2013.02a
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• pp.399-399
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• 2013

Metal silicides는 Si 기반의microelectronic devices의 interconnect와 contact 물질 등에 사용하기 위하여 그 형성 mechanism과 전기적 특성에 대한 연구가 많이 이루어지고 있다. 이 중 Rare-earth(RE) silicides는 저온에서 silicides를 형성하고, n-type Si과 낮은 Schottky Barrier contact (~0.3 eV)을 이룬다. 또한 낮은 resistivity와 Si과의 작은 lattice mismatch, 그리고 epitaxial growth의 가능성, 높은 thermal stability 등의 장점을 갖고 있다. RE silicides 중 ytterbium silicide는 가장 낮은 electric work function을 갖고 있어 n-channel schottky barrier MOSFETs의 source/drain으로 주목받고 있다. 또한 Silicon 기반의 CMOSFETs의 성능 향상 한계로 인하여 germanium 기반의 소자에 대한 연구가 이루어져 왔다. Ge 기반 FETs 제작을 위해서는 낮은 source/drain series/contact resistances의 contact을 형성해야 한다. 본 연구에서는 저접촉 저항 contact material로서 ytterbium germanide의 가능성에 대해 고찰하고자 하였다. HRTEM과 EDS를 이용하여 ytterbium germanide의 미세구조 분석과 면저항 및 Schottky Barrier Heights 등의 전기적 특성 분석을 진행하였다. Low doped n-type Ge (100) wafer를 1%의 hydrofluoric (HF) acid solution에 세정하여 native oxide layer를 제거하고, 고진공에서 RF sputtering 법을 이용하여 ytterbium 30 nm를 먼저 증착하고, 그 위에 ytterbium의 oxidation을 방지하기 위한 capping layer로 100 nm 두께의 TiN을 증착하였다. 증착 후, rapid thermal anneal (RTA)을 이용하여 N2 분위기에서 $300{\sim}700^{\circ}C$에서 각각 1분간 열처리하여 ytterbium germanides를 형성하였다. Ytterbium germanide의 미세구조 분석은 transmission electron microscopy (JEM-2100F)을 이용하였다. 면 저항 측정을 위해 sulfuric acid와 hydrogen peroxide solution (H2SO4:H2O2=6:1)에서 strip을 진행하여 TiN과 unreacted Yb을 제거하였고, 4-point probe를 통하여 측정하였다. Yb germanides의 면저항은 열처리 온도 증가에 따라 감소하다 증가하는 경향을 보이고, $400{\sim}500^{\circ}C$에서 가장 작은 면저항을 나타내었다. HRTEM 분석 결과, deposition 과정에서 Yb과 Si의 intermixing이 일어나 amorphous layer가 존재하였고, 열처리 온도가 증가하면서 diffusion이 더 활발히 일어나 amorphous layer의 두께가 증가하였다. $350^{\circ}C$ 열처리 샘플에서 germanide/Ge interface에서 epitaxial 구조의 crystalline Yb germanide가 형성되었고, EDS 측정 및 diffraction pattern을 통하여 안정상인 YbGe2-X phase임을 확인하였다. 이러한 epitaxial growth는 면저항의 감소를 가져왔으며, 열처리 온도가 증가하면서 epitaxial layer가 증가하다가 고온에서 polycrystalline 구조의 Yb germanide가 형성되어 면저항의 증가를 가져왔다. Schottky Barrier Heights 측정 결과 또한 면저항 경향과 동일하게 열처리 증가에 따라 감소하다가 고온에서 다시 증가하였다.