• 한국세라믹학회지
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• 제30권3호
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• pp.222-228
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• 1993

In order to obtian TiO2 fine powder of high purity, the new method which is different from the sulfate process and the chloride one was employed. TiO2 was syntehsized by the reaction between elemental titanium particles and H2O2 solutiosn at 30~7$0^{\circ}C$, and then TiO2 powder was characterized using XRD, SEM, TEM, DTA and FT-IR. It was found that the initial reaction rate was fast at a high temperature due to the high generation of activated oxygen associated with thedecomposition of H2O2. However, the reaction was slowly proceeded at a low temperature due to slow decomposition of H2O2. In this experimental range, the optimum temeprature was ocnsidered to be about 5$0^{\circ}C$. The primary particles of the hydrous titanium dioxide (TiO2 gel) before aging were spherical, and their mean sizes were about 50nm. The similar shapes and sizes were observed with calcinatin at 40$0^{\circ}C$. The FT-IR spectrum of Ti-OH in the TiO2 gel powder appeared at around 3380cm-1, 1630cm-1 and 530cm-1. This gel powder was crystallized into the anatase type TiO2 at 300~40$0^{\circ}C$.

• 한국표면공학회지
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• 제24권4호
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• pp.196-205
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• 1991

Multi-level thin films are very important in ULSI applications because of their high electromigration resistance. This study presents the effects of titanium, titanium nitride and titanium tungsten underlayers of the stability of multi-aluminum thin films during isothermal annealing. High purity Al(99.999%) films have been electron-beam evaporated on Ti, TiN, TiW films formed on SiO2/Si (P-type(100))-wafer substrates by RF-sputtering in Ar gas ambient. The hillock growth was increased with annealing temperatures. Growth of hillocks was observed during isothermal annealing of the thin films by scanning electron microscopy. The hillock growth was believed to appear due to the recrystallization process driven by stress relaxation during isothermal annealing. Thermomigration damage was also presented in thin films by grain boundary grooving processes. It is shown that underlayers of Al/TiN/SiO2, Al/TiW/SiO2 thin films are preferrable to Al/SiO2 thin film metallization.

• 한국분말재료학회지
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• 제26권4호
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• pp.282-289
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• 2019

Ti has received considerable attention for aerospace, vehicle, and semiconductor industry applications because of its acid-resistant nature, low density, and high mechanical strength. A common precursor used for preparing Ti materials is $TiCl_4$. To prepare high-purity $TiCl_4$, a process based on the removal of $VOCl_3$ has been widely applied. However, $VOCl_3$ removal by distillation and condensation is difficult because of the similar physical properties of $TiCl_4$ and $VOCl_3$. To circumvent this problem, in this study, we have developed a process for $VOCl_3$ removal using Cu powder and mineral oil as purifying agents. The effects of reaction time and temperature, and ratio of purifying agents on the $VOCl_3$ removal efficiency are investigated by chemical and structural measurements. Clear $TiCl_4$ is obtained after the removal of $VOCl_3$. Notably, complete removal of $VOCl_3$ is achieved with 2.0 wt% of mineral oil. Moreover, the refined $TiCl_4$ is used as a precursor for the synthesis of Ti powder. Ti powder is fabricated by a thermal reduction process at $1,100^{\circ}C$ using an $H_2-Ar$ gas mixture. The average size of the Ti powder particles is in the range of $1-3{\mu}m$.

• 자원리싸이클링
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• 제28권5호
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• pp.68-73
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• 2019

타이타늄 철석은 이산화 타이타늄 제조를 위해 사용되는 주요 광석 중 하나이다. 순도 99.9% 이상의 이산화 타이타늄 제조를 위해, 타이타늄 철석에 존재하는 철(III), 규소(IV) 그리고 망간(II)과 같은 불순물로부터 타이타늄(IV)을 분리해야 한다. 본 논문에서는 타이타늄 철석으로부터 염산 침출 및 고순도 타이타늄(IV) 용액으로부터 가수분해를 통해 고순도 이산화 타이타늄 습식 제련 공정을 조사했다. 타이타늄(IV), 철(III), 규소(IV) 그리고 망간(II)의 침출률에 대한 염산 농도, 광액농도 그리고 침출 시간에 따른 영향에 대해 조사했고 최적 침출 조건을 얻었다. 타이타늄(IV)을 가수분해하기 위한 중화제로 수산화암모늄 및 수산화나트륨 용액을 사용했다. 수산화 암모늄 용액으로 가수 분해된 침전물을 소성하여 아나타제상의 이산화 타이타늄을 얻었다. 타이타늄 철석으로부터 고순도 이산화 타이타늄 분말 제조를 위한 습식 제련 공정이 개발 가능하다.

• 대한금속재료학회지
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• 제49권11호
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• pp.845-852
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• 2011

The Spark Plasma Sintering(SPS) method offers a means of fabricating a sintered-body having high density without grain growth through short sintering time and a one-step process. A titanium compact having high density and purity was fabricated by the SPS process. It can be used to fabricate a Ti sputtering target with controlled parameters such as sintering temperature, heating rate, and pressure to establish the optimized processing conditions. The compact/target(?) has a diameter of ${\Phi}150{\times}6.35mm$. The density, purity, phase transformation, and microstructure of the Ti compact were analyzed by Archimedes, ICP, XRD and FE-SEM. A Ti thin-film fabricated on a $Si/SiO_2$ substrate by a sputtering device (SRN-100) was analyzed by XRD, TEM, and SIMS. Density and grain size were up to 99% and below $40{\mu}m$, respectively. The specific resistivity of the optimized Ti target was $8.63{\times}10^{-6}{\Omega}{\cdot}cm$.

• 열처리공학회지
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• 제8권2호
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• pp.137-148
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• 1995

The nitridation kinetics of titanium powder were studied by isothermal and non-isothermal (dynamic) methods in high purity nitrogen under I atm pressure. For the comparison with nitridation, the oxidation kinetics of titanium powder were also studied in dry oxygen at I atm pressure. An automatic recording electrobalance was used to measure the weight gain as a function of time and temperature. For the reaction with nitrogen, the nitride was formed at over $700^{\circ}C$. The reaction with nitrogen followed the parabolic rate law, and the activation energy was calculated to be 31 kcal/mol in the isothermal method (above $900^{\circ}C$). The non-stoichiometric TiNx has been synthesized by the nitridation at a proper temperature and time, followed by the homogenizing treatment above $1100^{\circ}C$. In comparison with the stoichiometric $TiN_{1.0}$ and the non-stoichiometric TiNx ($TiN_{0.5}$ and $TiN_{0.65}$), the hot oxidation characteristics of the former is superior to that of the latter. However, both non-stoichiometric nitrides make little difference in the hot oxidation characteristics.

• 한국재료학회지
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• 제26권6호
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• pp.306-310
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• 2016

To produce 4N grade high-purity silica powder from natural ore, the mineralogical characteristics of natural silica ore were investigated and their effects on the purification process were revealed. The Chinese silica mineral ore used was composed of iron and aluminum as main impurities and calcium, magnesium, potassium, sodium, and titanium as trace impurities; these trace impurities generally exist as either single oxides or complex oxides. It was confirmed that liberation and acidic washing of the impurities were highly dependent on the particle size of the ground silica ore and on its mineralogical characteristics such as the distribution and phases of existing impurities. It is suggested that appropriate size reduction of silica ore should be realized for optimized purification according to the origin of the natural silica ore. A single step purification process, the mechano-chemical washing (MCW) process, was proposed and verified in comparison with the conventional multi step washing process.

• 한국재료학회지
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• 제8권11호
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• pp.987-992
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• 1998

Ti 과 AI의 고순도 원소 박판을 이용하여 열간프레스장치에서 고온자전합성법으로 TiAI계 금속간화합물을 제조하였다. 원소 박판에서 $TiAl_3$ 금속간화합물을 제조하는 데 승온속도, 압력, 온도 등의 변수가 고온자전합성에 영향을 미치는 중요한 인자다. 특히 승온속도는 반응합성온도를 결정하는 인자로서 본 실험에서 DTA 분석을 이용하여 공정변수를 결정하였다. DTA 분석결과에 따르면, Ti와 AI의 계면에서 반응합성은 AI의 용융점 이하와 이상의 온도에서 두 번 발생함을 알 수 있다. 또한 승온속도가 증가할수록 두 반응합성온도는 증가하였다. 10층의 Ti 박판과 9층의 AI 박판을 $20^{\circ}C$/min의 승온속도로 고온자전합성시킨 후, $810^{\circ}C$와 240MPa의 압력에서 4시간 동안 열처리한 결과 $700\mu\textrm{m}$ 두께의 TiAI계 금속간화합물 판재를 제조하였으며, XRD 회절과 SEM으로 확인하였다.

• 방사성폐기물학회지
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• 제21권1호
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• pp.9-22
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• 2023

Spin-off pyroprocessing technology and inert anode materials to replace the conventional carbon-based smelting process for critical materials were introduced. Efforts to select inert anode materials through numerical analysis and selected experimental results were devised for the high-throughput reduction of oxide feedstocks. The electrochemical properties of the inert anode material were evaluated, and stable electrolysis behavior and CaCu generation were observed during molten salt recycling. Thereafter, CuTi was prepared by reacting rutile (TiO₂) with CaCu in a Ti crucible. The formation of CuTi was confirmed when the concentration of CaO in the molten salt was controlled at 7.5mol%. A laboratory-scale electrorefining study was conducted using CuTi(Zr, Hf) alloys as the anodes, with a Ti electrodeposit conforming to the ASTM B299 standard recovered using a pilot-scale electrorefining device.

• 자원환경지질
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• 제37권4호
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• pp.375-381
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• 2004

장주기 방사성 폐기물인 악티나이드 원소들을 고정화시킬 수 있는 파이로클로어 (pyrochlore; CaCeH$f_xTi_{2-x}O_7$=0.2, 0.6, 1.0, 1.4, 1.8, 2.0)를 합성하여 상평형 관계 및 특성을 연구하였다. 혼합된 시료는 상온에서 400kg/$cm^2$의 압력으로 성형한 후, 산소분위기에서 1200∼1$600^{\circ}C$ 범위로 소결온도를 변화시키면서 소성하였다. 합성된 시료는 XRD를 사용하여 상분석을 실시하였다. 실험결과, 파이로클로어의 최적 합성조건은 산소분위기 하에서, 각각의 조성에 따라, 1300∼150$0^{\circ}C$로 매우 다양하였다. 합성시 생성된 상으로는 페롭스카이트, 파이로클로어 및 $A_{2}BO_{5}$산화물 등이 있으며, 본 계의 특성은 Hf의 함량증가에 따라 페롭스카이트 및 파이로클로어의 격자상수가 증가한다는 점이다. 이같은 현상은 육배위 자리를 차지하고 있는 Hf와 Ti의 이온반경의 차이에서 비롯된 것이다.