• 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 $1-3{\mu}m$.

• Journal of the Korean Chemical Society
• /
• v.16 no.2
• /
• pp.80-83
• /
• 1972

The activity change of lysozyme resulted from its exposure to $Ti-H_2O_2$system in aqueous liquid at room temperature and to ${\gamma}$-irradiation in ice at $195^{\circ}K$ has been measured at room temperature with a Cary-14 spectrophotometer. The enzymatic activity of lysozyme which had been added to a previously flow-mixed solution of $TiCl_3$ and $H_2O_2$ (System I) was compared with the activity of a lysozyme-$H_2O_2$ solution after flow-mixing with $TiCl_3$ (System II), considering the differences between these two activity changes as the extent of the enzymatic inactivation by the involvement of OH radical reaction. The fraction of lysozyme inactivated by OH radical in the system containing 0.0025 M $TiCl_3-0.1M$ $H_2O_2$ (ph 3.5) was 13%, When the $TiCl_3$ concentration is double (pH 3.0), the fraction of enzyme inactivated increases to 36%. The activity of the system containing 0.025 M $TiCl_3-0.1$ M $H_2O_2$ (pH 1.5) was essentially zero. The results seem to support the previos view that the production of OH radical should be proportional to $TiCl_3$ concentration when $H_2O_2$ is present in excess. Increase in the extent of inactivation found in system I with increasing $TiCl_3$ concentration may be due to a pH effect. $H_2O_2$ seems to be less effective than $TiCl_3$ in the inactivation. 1% lysozyme solution, when ${\gamma}$-irradiated with a total dose of 3M rads, loses about 20% of its activity. Lowering of temperature also was found to yield a reduction in enzymatic activity.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
• /
• v.21 no.12
• /
• pp.1051-1056
• /
• 2008

In this study, the investigations of the TiN etching characteristics were carried out with addition of $Cl_2$ gas in an inductively coupled $BCl_3$-base plasma system. Dry etching of the TiN was studied by varying the etching parameters including $Cl_2$ gas addition ratio, RF power, DC-bias voltage and pressure. The etch rate of TiN thin film was maximum when the $Cl_2$ gas addition flow was 2 sccm with fixed other conditions. As the RF power DC-bias voltage were increased, the etch rate of TiN thin film showed increasing tendency. $BCl_3/Cl_2$/Ar plasmas were characterized by optical emission spectroscopy (OES) analysis. The chemical reaction on the surface of the etched TiN films was investigated with X-ray photoelectron spectroscopy (XPS).

• Journal of the Korean Ceramic Society
• /
• v.23 no.6
• /
• pp.45-51
• /
• 1986

$SrTiO_3$ reaction mechanism formed from $TiCl_4$ and $SrCl_2$ solution by direct-wet-process was studied. Through this study it is identified that crystalline $SrTiO_3$ is formed above pH 13.8 amorphous $SrTiO_3$ above pH7 and crystallization temperature of amorphous $SrTiO_3$ is at 37$0^{\circ}C$. the final products are composed of 60% crystalline $SrTiO_3$ and 40% amorphous $SrTiO_3$ The amorphous $SrTiO_3$ is identified with the IR absorption spectrum of Sr-Ti-O by FT-IR spectrometer. Under pH 7 gelationus metatitanate (H2TiO3) is formed from TiCl4 but above pH7 the activity by the formation of metatitnic acid ion $[TiO_3]^{2-}$ is so high that $SrTiO_3$is formed more easily through the reaction with $Sr^{2+}$.

• Journal of the Korean Institute of Telematics and Electronics D
• /
• v.36D no.4
• /
• pp.56-62
• /
• 1999

In this study, (Ba, Sr)$TiO_3$ thin films were etched with $Cl_2$/Ar gas mixing ratio in an inductively coupled plasma (ICP) by varying the etching parameter such as rf power, dc bias voltage, and chamber pressure. The etch rate was 56 nm/min under $Cl_2$/($Cl_2$+Ar) gas mixing ratio of 0.2, rf power of 600 W, dc bias voltage of 250 V, and chamber pressure of 5 mTorr. At this time, the selectivity of BST to Pt, $SiO_2$ was respectively 0.52, 0.43. The surface reaction of the etched (Ba, Sr)$TiO_3$ thin films was investigated with X-ray photoelectron spectroscopy (XPS). Ba is removed by chemical reaction between Sr and Cl to remove Sr. Ti is removed by chemical reaction such as $TiCl_4$ with ease. The results of secondary ion mass spectrometer (SIMS) analysis compared with the results of XPS analysis and the results were the same.

• Tribology and Lubricants
• /
• v.4 no.2
• /
• pp.36-43
• /
• 1988

Titanium carbide(TiC) and titanium nitride(TiN) flims were deposited on $Si_3N_4$-TiC composite cutting tools by chemical vapor deposition(CVD) using $TiCl_4-CH_4-H_2$ and $TiCl_4-H_2-N_2$ gas mixtures, respectively. The nonmetal to metal ratio of deposit increases with increasing $m_{C/Ti}$(mole ratio of CH$_4$ to TiCl$_4$ in the input) for TiC coatings and $m_{N/Ti}$(mole ratio of N$_2$ to TiCl$_4$ in the input) for TiN coatings. The nearly stoiahiometric films could be obtained under the deposition condition of $m_{C/Ti}$ between 1.15 and 1.61 for TiC, and that of $m_{N/Ti}$ between 25 and 28 for TiN. Also maximum microhardness of the coatings can be obtained in these ranges. The interfacial region of TiC coatings on $Si_3N_4$-TiC ceramics is wider than that of TiN coatings according to Auger depth profile analysis, which indicates good interfacial bonding for TiC. Experimental results show that TiC coatings have an randomly equiaxed structure and Columnar structure with(220) preferred orientation can be obtained for TiN coatings. And, multilayer coatings have a dense and equiaxed structure.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
• /
• v.24 no.9
• /
• pp.718-722
• /
• 2011

In this work, we investigated to the etching characteristics of the TiN thin film in He/$BCl_3/Cl_2$ plasma. The etch rate was measured by the gas mixing ratio, the RF power, the DC bias voltage and the process pressure. The maximum etch rate in He/$BCl_3/Cl_2$ plasma was 59 nm/min. The etch rate increased as the RF power and the DC-bias voltage was increased. The chemical reaction on the surface of the etched the TiN thin films was investigated with X-ray photoelectron spectroscopy (XPS). The intensity of Ti 2p and N 1s peaks are varied during etching process. A new peak was appeared in He/$BCl_3/Cl_2$ plasma. The new peak was revealed Ti-$Cl_x$ by Cl 2p peak of XPS wild scan spectra analysis.

• Journal of the Semiconductor & Display Technology
• /
• v.10 no.1
• /
• pp.95-99
• /
• 2011

$(1-x)BaTiO_3+(x)Cd_5(PO_4)_3Cl$ ceramics were prepared by the conventional ceramic technique, i.e., solid state reaction at high temperature. The concentration of $Cd_5(PO_4)_3C$ was varied from 0.01 to 0.15 mole fraction. In order to study the phase transitions of our ceramics, the Raman scattering spectra were measured as functions of concentration x and temperature. It was found that the soluble limit of $Cd_5(PO_4)_3Cl$ in $BaTiO_3$ was the x=0.05 composition and $BaTiO_3$ phase disappeared above x=0.10. A new phase identified as $Ba_4Ti_3P_2O_{15}$ was detected in all samples of our compositions. The Curie temperature shifts up to $130^{\circ}C$ as the concentration x increases from zero to 0.05 and shift down to $95^{\circ}C$ as further increases to 0.08. For the increase of the Curie temperature, it is suggested that it can result from the inhibition of displacement of $Ti^{4+}$ in the distorted octahedron due to well dispersed $Ba_4Ti_3P_2O_{15}$ and $Cd_5(PO_4)_3Cl$ phase.

• Tribology and Lubricants
• /
• v.4 no.2
• /
• pp.44-51
• /
• 1988

Titanium carbide(TiC), Titanium nitride(TiN), and Titanium carbonnitride(Ti(C,N)) films were deposited on $Si_3N_4$-TiC composite cutting tools by chemical vapor deposition(CVD) using $TiCl_4-CH_4-H_2$, $TiCl_4-N_2-H_2$, and $TiCl_4-CH_4-N_2-H_2$ gas mixtures, respectively. The experimental results indicate that TiC coatings compared with TiN coatings on $Si_3N_4$ -TiC ceramic have an improved microstructural property, good thermal shock resistance, and good interfacial bonding. However TiN coatings compared with TiC coatings have a low friction coefficient with steel and good chemical stability. It is found by cutting test that coated insert compared with $Si_3N_4$-TiC ceramic have a superior flank and crater wear resistance. And multilayer coating compared with monolayer coating shows a improved wear resistance.

• Journal of the Korean Vacuum Society
• /
• v.11 no.3
• /
• pp.159-165
• /
• 2002

The physical properties of the TiN films deposited by ALD using $TiCl_4$and $NH_3$have been investigated. The TiN deposition rate is ~0.6 $\AA$ under an optimum deposition condition and the resistivity of the TiN films is 200~350 $\mu\Omega$cm . According to the XRD analysis results TiN films are crystallized in the ALD process window. AES analysis results show that the Cl impurity concentration in the TiN films is lower than 1 at% and that the atomic ratio of the TiN films is 1:1. Also it is found by SEM observation that the step coverage of the TiN films on which TiN films with trenches the aspect ratio of which is 10:1 is excellent.