• Title/Summary/Keyword: TiCl4

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Kinetic Studies on Homopolymerization of $\alpha$-Methylstyrene and Sequential Block Copolymerization of Isobutylene with $\alpha$-Methylstyrene by Living/Controlled Cationic Polymerization (리빙/조절 양이온중합에 의한 알파메틸스티렌 호모중합 및 이소부틸렌과의 블록공중합에 대한 반응속도론 연구)

  • Wu, Yibo;Guo, Wenli;Li, Shuxin;Gong, Huiqing
    • Polymer(Korea)
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    • v.32 no.4
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    • pp.366-371
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    • 2008
  • The controlled/living cationic polymerization of $\alpha$-methylstyrene (${\alpha}MeSt$) and sequential block copolymerization of isobutylene (IB) with ${\alpha}MeSt$ were achieved using 2-chloro-2,4,4-trimethylpentane (TMPCl)/titanium tetrachloride ($TiCl_4$)/titanium isopropoxide ($Ti(OiPr)_4$)/2,6-ditert-butylpyridine (DtBP) initiating system in $CH_3Cl$/hexane(50/50 v/v) solvent mixture at $-80^{\circ}C$. The polymerization rate decreased with increasing $[Ti(OiPr)_4]/[TiCl_4]$ ratio in the homopolymerization of ${\alpha}MeSt$. The effects of $[Ti(OiPr)_4]/[TiCl_4]$ ratios and $PIB^+$ molecular weight on the polymerization rate and blocking efficiency were also investigated. Well-defined poly(isobutylene-b-$\alpha$-methylstyrene)s were demonstrated by $^1H$-NMR and triple detection SEC; refractive index (RI), multiangle laser light scattering (MALLS) and ultraviolet (UV) detectors. Blocking efficiencies for the poly(isobutylene-b-$\alpha$-methylstyrene)s of almost 100% were obtained when ${\alpha}MeSt$ was induced by PIB's of $M_n\;{\geq}\;41000$ at $[Ti(OiPr)_4]/[TiCl_4]=1$. Differential scanning calorimetry (DSC) of the block copolymers showed two glass transition temperatures, thereby demonstrating microphase separation.

Electrolytic Reduction Characteristics of Titanium Oxides in a LiCl-Li2O Molten Salt (LiCl-Li2O 용융염에서 타이타늄 산화물의 전해환원 특성)

  • Lee, Jeong;Kim, Sung-Wook;Lee, Sang-Kwon;Hur, Jin-Mok;Choi, Eun-Young
    • Journal of the Korean Electrochemical Society
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    • v.18 no.4
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    • pp.156-160
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    • 2015
  • Experiments using a metal oxide of a non-nuclear material as a fuel are very useful to develop a new electrolytic reducer for pyroprocessing. In this study, the titanium oxides (TiO and $TiO_2$) were selected and investigated as the non-nuclear fuel for the electrolytic reduction. The immersion tests of TiO and $TiO_2$ in a molten 1.0 wt.% $Li_2O$-LiCl salt revealed that they have solubility of 156 and 2100 ppm, respectively. Then, the Ti metals were successfully produced after the separate electrolytic reduction of TiO and $TiO_2$ in a molten 1.0 wt.% $Li_2O$-LiCl salt. However, Ti was detected on the platinum anode used for the electrolytic reduction of $TiO_2$ unlike TiO due to the dissolution of $TiO_2$ into the salt.

Effect of Calcium Ion and Initial pH on Phosphorus Removal using TiCl4 Coagulant (칼슘이온과 초기 pH가 TiCl4 응집제의 인 제거에 미치는 영향)

  • Kang, Seong Hyeon;Kang, Jang Hyeon;Kim, Han Gyul;Jeong, Hee Hoon;Kim, Jong Ho;Ahn, Johng-Hwa
    • Journal of Korean Society of Environmental Engineers
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    • v.39 no.3
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    • pp.164-168
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    • 2017
  • This study experimentally determined the effect of calcium ion ($Ca^{2+}$) (0-0.55 mM) and intial pH (4.0-10.0) on phosphorus (P) removal in synthetic wastewater (2 mg P/L) using titanium tetrachloride ($TiCl_4$) (0.12-0.18 mM). At TiCl4 concentration ([$TiCl_4$]) = 0.12 mM, the P removal efficiency was the highest (95.1%) at pH 7 but the efficiency decreased to 51.4% at pH 8. The P removal efficiency was 55.6% at $Ca^{2+}$ concentration ([$Ca^{2+}$]) = 0 mM but the efficiency increased to 90.5% at [$Ca^{2+}$] = 0.045 mM at [$TiCl_4$] = 0.12 mM. On the other hand, the P removal efficiency difference was not large (96.5-99.5%) with [$Ca^{2+}$] at [$TiCl_4$] = 0.15-0.18 mM. Within the design boundaries of $0.00{\leq}[Ca^{2+}]{\leq}0.18mM$ and $7.0{\leq}initial$ $pH{\leq}9.0$ at [$TiCl_4$] = 0.12 mM, the 90% P removal efficiency could be achieved at $[Ca2+]{\geq}0.10mM$ with pH 8.0 and $[Ca2+]{\geq}0.12mM$ with pH 9.0.

Preparation of High Purity $SrTiO_3$ by Coprecipitation and Strontium Titanyl Oxalates (공심법과 (Sr-Ti)수산염에 의한 고순도의 $SrTiO_3$ 합성에 관한 연구)

  • 이종권;이병하
    • Journal of the Korean Ceramic Society
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    • v.20 no.2
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    • pp.107-114
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    • 1983
  • Formation of Strontium titanate from the products of coprecipitation takes place at 110$0^{\circ}C$ which is 200-30$0^{\circ}C$ lower than that from mechanical mixtures of $SrCO_3$ and $TiO_2$. This is apparently due to the nature of the compounds formed by the reaction of mixtures of aqueous solutions of $SrCl_2$ and $TiCl_4$ with an ammoniacal solution of ammoni-um carbonate and ammonium hydroxide. A procedure is described for preparing strontium titanyl oxalate tetrahydrate in the several mole ratio of $TiCl_4$ to $SrCl_2$. STrontium titanyl oxalates decompose to titanate at elevated temperature. The coprecipitates and the fired specimen were subjected to examined thermal and X-ray analyses and microstruc-ture by SEM.

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The Influence of the Internal Donors in the Heterogenous Olefin Polymerization Catalyst on the Molecular Structure of Linear Low Density Polyethylene (불균일계 올레핀 중합촉매내 내부전자공여체가 선형 저밀도폴리에틸렌 분자구조에 미치는 영향)

  • Ko, Young Soo
    • Korean Chemical Engineering Research
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    • v.45 no.4
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    • pp.410-413
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    • 2007
  • The effect of internal donor(ID) in the heterogeneous Ziegler-Natta catalyst on the ethylene-1-butene copolymerization and the molecular structure of the resulting copolymer was investigated. $SiO_2$-supported $TiCl_4$ catalysts having ID/Ti molar ratio of 0.5 were prepared with ethyaluminium dichloride, magnesium alkyl, 2-ethyl-1-hexanol and $TiCl_4$. Three different IDs were employed such as ethylbenzoate(EB), diisobuylphthalate(DIBP) and dioctylphthalate(DOP). ID-added catalyst showed a larger fraction of Ti(+3) compared to that of no ID-added catalyst. The EB-added catalyst showed the highest activity in copolymerization. Xylene soluble value decreased by more than 50 % with ID-added catalysts compared to that of no ID-added catalyst. Crystaf analysis showed the chemical compositional distribution of PE copolymer was improved in the case of DIBP-added catalyst significantly. It could be explained that the presence of ID could make more even active sites and block the non-stereospecific active sites.

Phase Transition of $TiO_2$ prepared by HPPLT (저온균일침전법에 의해 제조된 $TiO_2$의 상변화)

  • Hwang, Du-Seon;Lee, Nam-Hui;Lee, Gang;Kim, Seon-Jae
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2003.03a
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    • pp.208-208
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    • 2003
  • 저온균일침전법(HPPLT)으로 제조된 TiO$_2$나노분말은 10$0^{\circ}C$이하의 온도에서 rutile상을 얻을 수 있다. 또한, rutile에서 anatase로의 상변화는 합성시간, 가열속도, 반응온도 그리고 음이온 첨가에 의해 일어난다고 보고되어졌지만, 금속양이온들에 의한 상변화는 알려진 바가 없다. 따라서, 다양한 양이온을 첨가하여 저온균일침전법에서 TiO$_2$의 상변화가 어떻게 일어나는지를 조사하였다. 출발원료인 TIC1$_4$를 사용하여 가수분해하여 0.67M의 TiOCl$_2$을 얻었다. 얻어진 TiOCl$_2$ 수용액에 각각 0.01M의 금속염화물(ZrOCl$_2$, NiCl$_2$, CuCl$_2$, FeCl$_3$, AlCl$_3$ 그리고 NbCl$_{5}$)을 첨가한 후 반응기에 넣고 10$0^{\circ}C$에서 4시간동안 가열하였다 가열한 후 얻어진 침전물에 NaOH 수용액을 이용하여 PH 7-8로 중화한 후 증류수로 Cl$^{-}$이온이 제거될 때까지 충분히 세척하였다. 세척된 침전물을 105$^{\circ}C$에서 24h동안 건조하여 분말을 얻었고, rutile에서 anatase로의 상변화특성을 관찰하기 위하여 XRD, SEM, TEM, ICP 분석을 실시하였다.

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Effects of Multi-layer and TiCl4 Treatment for TiO2 Electrode in Dye-sensitized Solar Cell (염료감응 태양전지의 TiO2 전극의 다중층 및 TiCl4 처리에 따른 효과)

  • Kim, Gyeong-Ok;Kim, Ki-Won;Cho, Kwon-Koo;Ryu, Kwang-Sun
    • Applied Chemistry for Engineering
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    • v.22 no.2
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    • pp.190-195
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    • 2011
  • To investigate the photon-trapping effect and scattering layer effect of $TiO_2$ multi-layer in dye-sensitized solar cell (DSSC) and the degree of recombination of electrons at the electrode treated $TiCl_4$, we formed electrodes of different conditions and obtained the most optimal electrode conditions. To estimate characteristics of the cell, IV curve, UV-Vis spectrophotometer, electrochemical impedance spectroscopy (EIS) and incident photon-to-current conversion efficiency (IPCE) were measured. As a result, we confirmed that the multi-layer's efficiency was higher than that of monolayer in the IV curve and the performance of $TiCl_4$ treated electrode was increased according to decreasing the impedance of EIS. Among several conditions, the efficiency of the cell with scattering layer is higher than that of a layer with the base electrode about 19%. Because the light scattering layer enhances the efficiency of the transmission wavelength and has long electron transfer path. Therefore, the value of the short circuit current increases approximately 10% and IPCE in the maximum peak also increases about 12%.

Role of HCl in Atomic Layer Deposition of TiO2 Thin Films from Titanium Tetrachloride and Water

  • Leem, Jina;Park, Inhye;Li, Yinshi;Zhou, Wenhao;Jin, Zhenyu;Shin, Seokhee;Min, Yo-Sep
    • Bulletin of the Korean Chemical Society
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    • v.35 no.4
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    • pp.1195-1201
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    • 2014
  • Atomic layer deposition (ALD) of $TiO_2$ thin film from $TiCl_4$ and $H_2O$ has been intensively studied since the invention of ALD method to grow thin films via chemical adsorptions of two precursors. However the role of HCl which is a gaseous byproduct in ALD chemistry for $TiO_2$ growth is still intriguing in terms of the growth mechanism. In order to investigate the role of HCl in $TiO_2$ ALD, HCl pulse and its purging steps are inserted in a typical sequence of $TiCl_4$ pulse-purge-$H_2O$ pulse-purge. When they are inserted after the first-half reaction (chemisorption of $TiCl_4$), the grown thickness of $TiO_2$ becomes thinner or thicker at lower or higher growth temperatures than $300^{\circ}C$, respectively. However the insertion after the second-half reaction (chemisorption of $H_2O$) results in severely reduced thicknesses in all growth temperatures. By using the result, we explain the growth mechanism and the role of HCl in $TiO_2$ ALD.

VHF-PECVD OF Ti/TiN WITH SILANE REDUCTION PROCESS

  • Mizuno, Shigeru
    • Journal of the Korean institute of surface engineering
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    • v.29 no.5
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    • pp.350-356
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    • 1996
  • This paper presents VHF-Plasma Enhanced Chemical Vapor Deposition (VHF-PECVD) of Ti/TiN with silne reduction process, using $TiCl_4$ source. VHF plasma, which is denser than a conventional RF plasma, produces a large number of radicals. Silane reduction process, which supplies silane radicals, more promotes dissociation of Ti-Cl bond than a conventional hydrogen reduction process. therefore, the VHF-PECVD with silane reduction process forms high quality Ti/TiN films, which have low level of Cl content(<0.2 at.%). In result, the resistivity for Ti or TiN is less than 200$\mu$$\Omega$cm. The surface morphology of Ti film is very smooth. The structure of TiN film is amorphous. Furthermore, excellent step coverage for the films is obtained.

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