• Proceedings of the Korean Society Of Semiconductor Equipment Technology
• /
• 2003.12a
• /
• pp.1-6
• /
• 2003

Flow modulation chemical vapor deposition process has been reported as an alternative way to obtain low resistivity, low residual chlorine content and good step-coverage titanium nitride film. Flow and concentration characteristics in a vertical FMCVD reactor are analyzed by using computational fluid dynamics method. The results show that 1.0 second as Cl reduction period is too short and there is still $TiCl_4$ gas above the holder at the end of the period. Time variation of $TiCl_4$ gas concentration on the holder shows that at least 3.0 second is necessary as Cl reduction time for the sake of film characteristics.

• Journal of the Korean Chemical Society
• /
• v.4 no.1
• /
• pp.15-17
• /
• 1957

1. Preparation of Titanium tetrachloride; The following precesses were strictly followed as the preliminary step to obtain pure $TiOCl_2$, titanyl chloride; First, pure Titanium Oxide mixed with carbon is rolled into pills. After drying up perfectly, these pills are heated at 900∼1000${\circ}C$. And then the pills are subjected to the flow of $Cl_2$ gas in a quartz tube heated to 900-1000${\circ}C$. Thus Titanium tetrachloride is obtained. 2. Preparation of $TiOCl_2$ ; Yellowish trobrown solution is made by pouring 80 g of conc. HCl (sp.gr. 1.19) to 45 gr of Titanium tetrachloride (approx. 2 times of theoretical amount). Then this solution is kept settled for 5-days in a desiccator filled with phosphorous pentoxide at room temperature. As the colorless amorphous solid thus obtained is washed with aceton, 36.5 g of the pure salt are obtained. 3. Determination of composition. The analysis of the sample taken from the deposit desiccated gives the following data; (A) Qualitative analysis; a) $Ti(OH)_4$ is precipitated by adding NaOH in water solution of the salt. b) Adding $AgNO_3$ solution, the water solution of the salt gives white precipitate of AgCl. c) When acid and $H_2O_2$ are added, the solution turns its color to redish brown (This proves that $TiO^{++}$ was converted into $TiO^{++}$ by oxidation of $H_2O_2$. (B) Quantitative analysis; a) $Ti(OH)_4$ precipitated by $10{\%}$ NaOH isalitatsubjected consecutively to the filtration and ignition in porcelain crucible at approx. 1000${\circ}C$. , then $TiO_2$ thus formed is weighed and calculated into Ti content. b) Chlorine involved in water solution of the salt is determined by Vorhardt method. Result: The values obtained from previous analysis, devied by their atomic weight gives the following composition: Ti : Cl = 1 : 2 Therefore $TiOCl_2$ should be given as its molecular formula. 4. Summary. When $TiCl_4$ is additated into conc. HCl, $TiO^{++}$ formed exists as a stable form, and forms $TiOCl_2$. However $TiOCl_2$ is unstable to heating. When the temperature is raised to $65{\circ}C$the decomposition of the solution is accelerated, and gives $TiO_2$ aq. $TiOCl_2$ in addition is highly hygroscopic.

• Journal of the Korean Ceramic Society
• /
• v.37 no.10
• /
• pp.933-937
• /
• 2000

고기능성 전자재료용 TiO$_2$분말 및 박막제조에 사용되는 중간생성물인 TiCl$_4$는 99% 이상의 고순도가 요구된다. 고순도.미립의 TiO$_2$분말 및 TiCl$_4$는 황산법으로 제조한 저순도 TiO$_2$원료를 사용하여 염소화법으로 Ti-염화물 및 염화불순물로 제조한 후, 대부분의 염화불순물들은 3단계 과정을 거쳐 고순화 하였다. 대부분의 염화불순물은 분리.응축 및 분별증류로, VOCl$_3$는 mineral oil을 첨가하여 비등점을 변화시켜, 그리고 미량의 염화불순물은 열가수분해하여 침전시킨 후 유기용제 처리하여 제거하였다. 유기용제 처리는 TiO$_2$분말의 고순도화에 도움이 되었으며, 입자간의 응집을 적게 하여 TiO$_2$입자크기도 작아졌다. 또한 anatase에서 rutile 결정구조로의 전이온도도 낮아지는 부수적인 효과를 보였다.

• Journal of the Korean Ceramic Society
• /
• v.21 no.2
• /
• pp.165-173
• /
• 1984

It is desirable to establish reliable synthetic methods for electro-ceramic materials. To synthesize $SrTiO_3$ in this study direct solid state reactions and wet chemical processes were used. Previous study of $SrTiO_3$ synthesis included oxalated-method($SrTiO(C_2O_4)_2$.$4H_2O$) co-precipitation$(SrCO_3+TiO(OH)_2)$ and direct solid state reaction$(SrCO_3+TiO(OH)_2)$ The methods in question lead to intermediate inclusion during the reactions and less controllable in particle sizes of $SrTiO_3$. To obtain highly pure $SrTiO_3$ so-called "direct wet process method" was added in this investigation. In the study the "direct wet process" was for the first time applied to synthesize chemically pure and fine particle $SrTiO_3$. $SrCl_2$ and $TiCl_4$<\ulcornerTEX> at KOH solution at room temperature to 10$0^{\circ}C$ precipitated $SrTiO_3$ The particle size increased as temperature increased.mperature increased.

• Journal of the Korean institute of surface engineering
• /
• v.31 no.6
• /
• pp.359-370
• /
• 1998

TiAl-based intermetallic compounds were electro-bornizel in the mixture of $Na_2B_4O_7$, KCL and LiCl in the termetature rage between 850 and $1000^{\circ}C$for various times (1-5 hours)under the fixed current density of 0.5 A/$cm^2$. The optimized composition of electrolyte in this work was decided to be 76.9 wt% $Na_2B_4O_7$-19.2 wt.%(0.7KCl-0.3LiCl) -3.9 wt.% al. The samples with boronized layer were investigated by SEM, XRD and EDS. The surface micro-hardness of boronized TiAl was also evaluated using Micro Vickers Hardness Tester. The sample, boronized at $900^{\circ}C$ for 4 hours in the above composition of electrolyte under the current density of 0.5 A/$\textrm{cm}^2$, has about 36$\mu\textrm{m}$ think layer on the surface, and its surface micro-hardness was measured to be 1263 Hv. From the results of SEM, XRD and EDS, the layer consisted of $TiB_2$ sublayer and Al-oxide sub layer. Al-depleted layer below the Al-oxide sudlayer was also detected. The activation energy for formation of boronized layer in this study was calculated as 178 Kcal/moleK.

• Transactions of the Korean hydrogen and new energy society
• /
• v.13 no.3
• /
• pp.224-232
• /
• 2002

CdS-$TiO_2$ nano-composite sol was prepared by the sol-gel method in organic solvents at room temperature and further hydrothermal treatment at various temperatures to control the physical properties of the primary particles. Again, CdS-$TiO_2$ composite particulate films were made by casting CdS-$TiO_2$ sols onto $F:SnO_2$ conducting glass and then heat-treatment at $400^{\circ}C$. Physical properties of these 61ms were further controlled by the surface treatment with $TiCl_4$, aqueous solution. The photo currents and hydrogen production rates measured under the experimental conditions varied according to the $CdS/[CdS+TiO_2]$ mole ratio and the mixed-sol preparation method. For $CdS-TiO_2$ composite sols prepared in IPA, CdS particles were homogeneously surrounded by $TiO_2$ particles. Also, the surface treatment with $TiCl_4$ aqueous solution caused a considerable improvement in the photocatalytic activity, probably as a result of close contacts between the primary particles by the etching effect of $TiCl_4$. It was found that the photoelectrochemical performance of these particulate films could be effectively enhanced by this approach.

• Proceedings of the Korean Vacuum Society Conference
• /
• 2012.02a
• /
• pp.218-218
• /
• 2012

Nanocrystalline $SnO_2$ colloids are synthesized by hydrolysis of $SnCl_4{\cdot}5H_2O$ in aqueous ammonia solution. The synthesized $SnO_2$ nanoparticles with ca. 15 nm in diameter are coated on a fluorinedoped thin oxide (FTO) conductive substrate and heated at $550^{\circ}C$. The annealed $SnO_2$ film is treated with aqueous $TiCl_4$ solution, which is sensitzied with MK-2 dye (2-cyano-3-[5'''-(9-ethyl- 9H-carbazol-3-yl)-3',3'',3''',4-tetra-n-hexyl-[2,2',5',2'',5'',2''']-quater thiophen-5-yl]). Compared to bare $SnO_2$ film, the conversion efficiency is significantly improved from 0.22% to 3.13% after surface treatment of $SnO_2$ with $TiCl_4$, which is mainly due to the large increases in both photocurrent density from 1.33 to $9.46mA/cm^2$ and voltage from 315 to 634 mV. It is noted that little change in the amount of the adsorbed dye is detected from 1.21 for the bare $SnO_2$ to $1.28{\mu}mol/cm^2$ for the $TiCl_{4-}$ treated $SnO_2$. This indicates that the photocurrent density increased by more than 6 times is not closely related to the dye loading concentration. From the photocurrent and voltage transient spectroscopic studies, electron life time increases by about 13 order of magnitude, whereas electron diffusion coefficient decreases by about 3.6 times after $TiCl_4$ treatment. Slow electron diffusion rate offers sufficient time for regeneration kinetics. As a result, charge collection efficiency of about 40% before $TiCl_4$ treatment is improved to 95% after $TiCl_4$ treatment. The large increase in voltage is due to the significant increase in electron life time, associated with upward shift of fermi energy.

• Journal of the Korean Chemical Society
• /
• v.57 no.4
• /
• pp.483-488
• /
• 2013

Copper oxide (CuO) was synthesized from $CuCl_2$ by solution method. Anatase $TiO_2$ particle was dispersed into the solution before preparing CuO, so that $TiO_2$/CuO heterojunction was created through the nucleation of CuO onto the $TiO_2$ surface. Some amount of CuO was reduced to $Cu_2O$ by treating glucose into the solution, thereby preparing $TiO_2/Cu_xO$ complex. The obtained $TiO_2/Cu_xO$ complex showed advanced phtocatalytic activity under the sun light compared with the P-25 sample. In addition, the the $TiO_2/Cu_xO$ complex showed excellent antipathogenic effect.

• Journal of Korean Society of Environmental Engineers
• /
• v.27 no.9
• /
• pp.932-938
• /
• 2005

[ $TiO_2$ ] nanoparticles were prepared from the precipitation in $TiCl_4$ and the sol-gel profess in $Ti(OC_3H_7)_4$ as starting materials with various synthetic conditions. The samples were characterized by XRD, SEM, and TEM testing techniques. The photocatalytic degradation of congo red has been investigated in $TiO_2/UV$ process to evaluate photocatalytic activities for the samples. $TiO_2$ nanoparticles calcined at $400^{\circ}C$ had the best photocatalytic activity with the rate constant of the degradation of congo red as $0.0319\;min^{-1}$. The rate constant of $TiO_2$ photocatalysts was increased with the calcination temperature under $400^{\circ}C$ and decreased with the calcination temperature upper $400^{\circ}C$. In the case of $TiO_2$ photocatalysts, the photocatalytic activity wasn't greatly affected by the frequencies of usage. In the similar synthesis condition, the degradation efficiency of the $TiO_2$ particle prepared by $TiCl_4$ was increased to 8.8%, when the rate was compared with the sample prepared by $Ti(OC_3H_7)_4$. The photocatalytic activities of $TiO_2$ photocatalysts synthesized by $Ti(OC_3H_7)_4$ with various conditions were also discussed.

• Transactions of the Korean hydrogen and new energy society
• /
• v.13 no.1
• /
• pp.34-41
• /
• 2002

CdS and $TiO_2$ nanoparticles were made by the precipitation method and sol-gel method, respectively, and they were mixed mechanically and then treated with the hydrothermal processing. CdS-$TiO_2$ composite particulate films were thus prepared by casting CdS-$TiO_2$ mixed sol onto $SnO_2$ conducting glass and a subsequent heat-treatment at $400^{\circ}C$. Again, the physico-chemical and photoelectrochemical properties of these films were controlled by the surface treatment with $TiCl_4$ aqueous solution. The photocurrents and the hydrogen production rates measured under the present experimental conditions varied in the range of $3.5{\sim}4.5mA/cm^2$ and $0.3{\sim}1.8cc/cm^2$-hr, respectively, and showed the maximum values at the $CdS/[CdS+TiO_2]$ mole ratio of 0.2. Also, the surface treatment with $TiCl_4$ aqueous solution caused a considerable improvement in the photocatalytic activity, Probably as a result of close contacts between the primary particles by the etching effect of $TiCl_4$ It was found that the photoelectrochemical performance of these particulate films could be effectively enhanced by this approach.