• Journal of the Korean Ceramic Society
• /
• v.30 no.3
• /
• pp.222-228
• /
• 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$0^{\circ}C$.

• Journal of the Korean institute of surface engineering
• /
• v.24 no.4
• /
• pp.196-205
• /
• 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.

• Journal of Powder Materials
• /
• v.26 no.4
• /
• pp.282-289
• /
• 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 $1-3{\mu}m$.

• Resources Recycling
• /
• v.28 no.5
• /
• pp.68-73
• /
• 2019

Ilmenite is one of the principal ores for the production of titanium dioxide. To produce titanium dioxide with purity higher than 99.9% from ilmenite, Ti(IV) should be separated from the dissolved impurities such as Fe(III), Si(IV), and Mn(II) present in ilmenite. In this work, a hydrometallurgical process was investigated to recover pure titanium dioxide from ilmenite by HCl leaching followed by separation and hydrolysis of Ti(IV). An optimum leaching condition was obtained by investigating the effect of HCl concentration, pulp density, and leaching time on the leaching percentage of Ti(IV), Fe(III), Si(IV), and Mn(II). Ammonium hydroxide and sodium hydroxide solutions were employed as neutralizing agents to hydrolyze Ti(IV) from the stripping solution of Ti(IV). Titanium dioxide of the anatase phase was obtained by calcination of the hydrolyzed precipitates with $NH_4OH$ solution. A hydrometallurgical process can be developed to produce pure $TiO_2$ powders from ilmenite.

• Korean Journal of Metals and Materials
• /
• v.49 no.11
• /
• pp.845-852
• /
• 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 $8.63{\times}10^{-6}{\Omega}{\cdot}cm$.

• Journal of the Korean Society for Heat Treatment
• /
• v.8 no.2
• /
• pp.137-148
• /
• 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.

• Korean Journal of Materials Research
• /
• v.26 no.6
• /
• pp.306-310
• /
• 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.

• Korean Journal of Materials Research
• /
• v.8 no.11
• /
• pp.987-992
• /
• 1998

Titanium aluminide intermetallic compound was formed from high purity elemental Ti and A1 foils by selfpropagating, high-temperature synthesis(SHS1 in hot press. Formation of $TiAl_3$ intermetallics at the interface between Ti and Al foil was observed to be controlled by temperature, pressure and heating rate. Especially, the heating rate is the most important role to form intermetallic compound by SHS reaction. According to DTA experiment, the SHS reactions appeared at two different temperatures below and above the melting point of Al. It was also observed that both SHS reaction temperatures increased with increasing the heating rate. After the SHS reaction of alternatively layered 10 Ti and 9 A1 foils at the heating rate of $20^{\circ}C$/min, the $700\mu\textrm{m}$ thick titanium aluminide sheet was formed by heat treatment at $810^{\circ}C$ for 4hours.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
• /
• v.21 no.1
• /
• pp.9-22
• /
• 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.

• Economic and Environmental Geology
• /
• v.37 no.4
• /
• pp.375-381
• /
• 2004

Pyrochlore was known as one of the most promising materials for the immobilization of radioactive actinide. This study includes the synthesis, phase relation and characteristics of pyrochlores (CaCeH$f_xTi_{2-x}O_7$=0.2, 0.6, 1.0, 1.4, 1.8, 2.0) in the system of Ca-Ce-Hf-Ti-O. The samples were prepared from high purity of starting materials under the pressure of 400kg/cm$^2$ at room temperature, and were sintered at 1200∼1$600^{\circ}C$ The synthesized samples were analyzed and identified with XRD. The optimal formation conditions of pyrochlores were at 1300∼150$0^{\circ}C$ under $O_2$ atmosphere with batch compositions. During synthesis, pyrochlore, perovskite and $A_{2}BO_{5}$ oxide were formed. The characteristics of this system is that parameter of pyrochlore was increased with the content of hafnium. This phenomenon was due to the difference of ionic size between hafnium and titanium in six coordinated site.