• Title/Summary/Keyword: anatase

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Thickness Determination of Ultrathin Gate Oxide Grown by Wet Oxidation

  • 장효식;황현상;이확주;조현모;김현경;문대원
    • Proceedings of the Korean Vacuum Society Conference
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    • 2000.02a
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    • pp.107-107
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    • 2000
  • 최근 반도체 소자의 고집적화 및 대용량화의 경향에 다라 MOSFET 소자 제작에 이동되는 게이트 산화막의 두께가 수 nm 정도까지 점점 얇아지는 추세이고 Giga-DRAM급 차세대 UNSI소자를 제작하기 위해 5nm이하의 게이트 절연막이 요구된다. 이런 절연막의 두께감소는 게이트 정전용량을 증가시켜 트랜지스터의 속도를 빠르게 하며, 동시에 저전압동작을 가능하게 하기 때문에 게이트 산화막의 두께는 MOS공정세대가 진행되어감에 따라 계속 감소할 것이다. 따라서 절연막 두께는 소자의 동작 특성을 결정하는 중요한 요소이므로 이에 대한 정확한 평가 방법의 확보는 공정 control 측면에서 필수적이다. 그러나, 절연막의 두께가 작아지면서 게이트 산화막과 crystalline siliconrksm이 계면효과가 박막의 두께에 심각한 영향을 주기 때문에 정확한 두께 계측이 어렵고 계측방법에 따라서 두께 계측의 차이가 난다. 따라서 차세대 반도체 소자의 개발 및 양산 체계를 확립하기 위해서는 산화막의 두께가 10nm보다 작은 1nm-5nm 수준의 박막 시료에 대한 두께 계측 방법이 확립이 되어야 한다. 따라서, 본 연구에서는 습식 산화 공정으로 제작된 3nm-7nm 의 게이트 절연막을 현재까지 알려진 다양한 두께 평가방법을 비교 연구하였다. 절연막을 MEIS (Medim Energy Ion Scattering), 0.015nm의 고감도를 가지는 SE (Spectroscopic Ellipsometry), XPS, 고분해능 전자현미경 (TEM)을 이용하여 측정 비교하였다. 또한 polysilicon gate를 가지는 MOS capacitor를 제작하여 소자의 Capacitance-Voltage 및 Current-Voltage를 측정하여 절연막 두께를 계산하여 가장 좋은 두께 계측 방법을 찾고자 한다.다. 마이크로스트립 링 공진기는 링의 원주길이가 전자기파 파장길이의 정수배가 되면 공진이 일어나는 구조이다. Fused quartz를 기판으로 하여 증착압력을 변수로 하여 TiO2 박막을 증착하였다. 그리고 그 위에 은 (silver)을 사용하여 링 패턴을 형성하였다. 이와 같이 공진기를 제작하여 network analyzer (HP 8510C)로 마이크로파 대역에서의 공진특서을 측정하였다. 공진특성으로부터 전체 품질계수와 유효유전율, 그리고 TiO2 박막의 품질계수를 얻어내었다. 측정결과 rutile에서 anatase로 박막의 상이 변할수록 유전율은 감소하고 유전손실은 증가하는 결과를 나타내었다.의 성장률이 둔화됨을 볼 수 있다. 또한 Silane 가스량이 적어지는 영역에서는 가스량의 감소에 의해 성장속도가 둔화됨을 볼 수 있다. 또한 Silane 가스량이 적어지는 영역에서는 가스량의 감소에 의해 성장속도가 줄어들어 성장률이 Silane가스량에 의해 지배됨을 볼 수 있다. UV-VIS spectrophotometer에 의한 비정질 SiC 박막의 투과도와 파장과의 관계에 있어 유리를 기판으로 사용했으므로 유리의투과도를 감안했으며, 유리에 대한 상대적인 비율 관계로 투과도를 나타냈었다. 또한 비저질 SiC 박막의 흡수계수는 Ellipsometry에 의해 측정된 Δ과 Ψ값을 이용하여 시뮬레이션한 결과로 비정질 SiC 박막의 두께를 이용하여 구하였다. 또한 Tauc Plot을 통해 박막의 optical band gap을 2.6~3.7eV로 조절할 수 있었다. 20$0^{\circ}C$이상으로 증가시켜도 광투과율은 큰 변화를 나타내지 않았다.부터 전분-지질복합제의 형성 촉진이 시사되었다.이것으로 인하여 호화억제에 의한 노화 방지효과가 기대되었지만 실제로 빵의 노화는 현저히 진행되었다

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Fabrication of Photocatalyst Glass Beads Coated with TiO2 Thin Film by a Layer-by-Layer Process (LBL법에 의해 TiO2막이 코팅된 광촉매 글라스 비드 제조)

  • Lee, Ji-Sun;Chae, Yoo-Jin;Lee, Mi-Jai;Kim, Sei-Ki;Hwang, Jong-Hee;Lim, Tae-Young;Hyun, Soong-Keun;Kim, Jin-Ho
    • Korean Journal of Materials Research
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    • v.22 no.7
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    • pp.379-383
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    • 2012
  • $TiO_2$ thin films consisting of positively charged poly(diallyldimethylammonium chloride)(PDDA) and negatively charged titanium(IV) bis(ammonium lactato) dihydroxide(TALH) were successfully fabricated on glass beads by a layer-by-layer(LBL) self-assembly method. The glass beads used here showed a positive charge in an acid range and negative charge in an alkaline range. The glass beads coated with the coating sequence of(PDDA/TALH)n showed a change in the surface morphology as a function of the number of bilayers. When the number of bilayers(n) of the(PDDA/TALH) thin film was 20, Ti element was observed on the surface of the coated glass beads. The thin films coated onto the glass beads had a main peak of the (101) crystal face and were highly crystallized with XRD diffraction peaks of anatase-type $TiO_2$ according to an XRD analysis. In addition, the $TiO_2$ thin films showed photocatalytic properties such that they could decompose a methyl orange solution under illumination with UV light. As the number of bilayers of the(PDDA/TALH) thin film increased, the photocatalytic property of the $TiO_2$-coated glass beads increased with the increase in the thin film thickness. The surface morphologies and optical properties of glass beads coated with $TiO_2$ thin films with different coating numbers were measured by field emission scanning electron microscopy(FE-SEM), X-ray diffraction(XRD) and by UV-Vis spectrophotometry(UV-vis).

Investigation on the Preparation Method of TiO2-mayenite for NOx Removal (질소산화물 제거를 위한 TiO2-mayenite 제조 방법에 관한 연구)

  • Park, Ji Hye;Park, Jung Jun;Park, Hee Ju;Yi, Kwang Bok
    • Clean Technology
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    • v.26 no.4
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    • pp.304-310
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    • 2020
  • In order to apply a photocatalyst (TiO2) to various building materials, TiO2-mayenite was prepared in this study. The TiO2 was synthesized using the sol-gel method by fixing titanium isopropoxide (TTIP) and urea at a ratio of 1 : 1. Later, they were calcined in a temperature range of 400-700 ℃ to analyze the properties according to temperature. BET, TGA, and XRD were used to analyze the physical and chemical properties of TiO2. The nitrogen oxide removal test was confirmed by measuring the change in the concentration of NO for 1 h according to KS L ISO 22197-1. The prepared TiO2 samples exhibited an anatase crystal structure below 600 ℃, and TiO2 (urea)-400 showed the highest nitrogen oxide removal rate at 2.35 µmol h-1. TiO2-mayenite was prepared using two methods: spraying TiO2 dispersion solution (s/s) and sol-gel solution (g/s). Through BET and XRD analysis, it was found that 5-TiO2 (g/s) prepared by spraying a sol-gel solution has maintained its crystallinity even after heat treatment. Also, 5-TiO2 (g/s)-500 showed the highest removal rate of 0.55 µmol h-1 in the nitrogen oxide removal test. To prepare TiO2-mayenite, it was confirmed that mayenite should be blended with TiO2 in a sol-gel state to maintain the crystal structure and exhibit a high nitrogen oxide removal rate.

Core-shell TiO2/Ag Nanoparticle Synthesis and Characterization for Conductive Paste (전도성 페이스트용 코어-쉘 TiO2/Ag 나노입자의 합성 및 특성 연구)

  • Sang-Bo, Sim;Jong-Dae, Han
    • Applied Chemistry for Engineering
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    • v.34 no.1
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    • pp.36-44
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    • 2023
  • Core-shell TiO2/Ag nanoparticles were synthesized by a modified sol-gel process and the reverse micelle method using acetoxime as a reducing agent in water/dodecylbenzenesulfonic acid (DDBA)/cyclohexane. The structure, shape, and size of the TiO2/Ag nanoparticles were investigated using X-ray diffraction (XRD), UV-visible spectroscopy, scanning electron microscope (SEM), transmission electron microscope (TEM), and thermogravimetric analysis (TGA). The size of TiO2/Ag nanoparticles could be controlled by changing the [water]/[DDBA] molar ratio values. The size and the polydispersity of TiO2/Ag nanoparticles increased when the [water]/[DDBA] molar ratio rose. The resultant Ag nanoparticles over the anatase crystal TiO2 nanoparticles exhibited a strong surface plasmon resonance (SPR) peak at about 430 nm. The SPR peak shifted to the red side with the increase in nanoparticle size. Conductive pastes with 70 wt% TiO2/Ag nanoparticles were prepared, and the pastes were coated on the PET films using a screen-printing method. The printed paste films of the TiO2/Ag nanoparticles demonstrated greater surface resistance than conventional Ag paste in the range of 405~630 μΩ/sq.

Fabrication of Fe-ACF/TiO2 composites and their photonic activity for organic dye (ACF/TiO2 복합체의 제조 및 유기 염료에 의한 광활성)

  • Zhang, Kan;Meng, Ze-Da;Ko, Weon-Bae;Oh, Won-Chun
    • Analytical Science and Technology
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    • v.22 no.3
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    • pp.254-262
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    • 2009
  • Activated carbon fiber treated with iron compound (Fe-ACF) was employed for preparation of Feactivated carbon fiber/$TiO_2$ (Fe-ACF/$TiO_2$) composite catalysts. Then, the prepared Fe-ACF/$TiO_2$ composite catalysts were characterized by employing BET, SEM, XRD and EDX instruments. It showed that BET surface area was related to adsorption capacity for each composite. The SEM results showed that ferric compound and titanium dioxide were distributed on the surfaces of ACF. The XRD results showed that Fe-ACF/$TiO_2$ composite mostly contained an anatase structure with a Fe mediated compound. EDX results showed the presence of C, O, and Ti with Fe peaks in Fe-ACF/$TiO_2$ composites. From photocataytic degradation effect, it was observed in the organic dye (Methylene blue, MB) degradation by these composites. Different degradation effect can be attributed to the synergetic effects of photo-Fenton reaction of Fe. It was considered that the combined reactions of Fe-ACF/$TiO_2$ produce powerful photo-Fenton process in the MB degradation.

The analysis for the HCl modification effect and formation of TiO2 on activated carbon fiber surface (활성탄소섬유 표면의 염산처리효과와 TiO2 형성에 관한 분석)

  • Oh, Won-Chun;Han, Sang-Bum;Bae, Jang-Soon
    • Analytical Science and Technology
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    • v.20 no.4
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    • pp.279-288
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    • 2007
  • We have studied a method for the preparation of $ACF/TiO_2$ composites involving the penetrationof titanium n-butoxide (TNB) solution into activated carbon fiber. It was focused on the characterization of $TiO_2$ formed in prorous carbon was which increased with surface functional groups by hydrochloric acid treatment. The conversion of TNB to $TiO_2$ for the acid treatment effect must be important for the preparationof $ACF/TiO_2$ composites. From the characterization of surface properties, both the BET surface area and the total pore volume decreased as the distribution of $TiO_2$ on the activated carbon fiber surfaces after acid treatments.The changes in XRD pattern showed the typical anatase type on $ACF/TiO_2$ composite for the sample named FT, FT1 and FT2 treated with 0.05, 0.1 and 0.5 M, respectively. However, XRD patern of FT3 treated with 0.5M showed mixed amatase-rutile structure. According to the results of SEM micrographs, the titanium complexe particles were irregularly distributed around carbon. And some large clusters were found when an amount of acid treatment increased. The EDX results of $ACF/TiO_2$ composites showed the presence of C, O and P with strong Ti peaks. Finally, the excellent photocatalytic activity of the $ACF/TiO_2$ composites between relative concentration($c/c_o$) of MB (methylene blue) and UV irradiation time could be attributed to the both effects between photocatalysis of the formation of titania complexes and adsorptivity of the activated carbon fiber.

Control of Chlorinated Volatile Pollutants at Indoor Air Levels Using Polymer-based Photocatalyst, Composite

  • Kim, Byeong-Chan;Kim, Hye-Jin;Kim, Ji-Eun;Park, Eun-Ju;Noh, Ji-Sun;Kang, Hyun-Jung;Shin, Seung-Ho;Jo, Wan-Kuen
    • Clean Technology
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    • v.19 no.2
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    • pp.105-112
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    • 2013
  • In this study, polyaniline (PANI)-based $TiO_2$ (PANI-$TiO_2$) composites calcined at different temperatures were prepared and their applications for control of trichloroethylene (TCE) and tetrachloroethylene (TTCE) at indoor air levels were investigated. For these target compounds, the photocatalytic control efficiencies of PANI-$TiO_2$ composites did not exhibit any trend with varying calcination temperatures (CTs). Rather, the average control efficiencies of PANI-$TiO_2$ composites over 3-h photocatalytic process increased from 61 to 72% and from 21 to 39% for TCE and TTCE, respectively, as the CT increased from 350 to $450^{\circ}C$. However, for both the target compounds, the average control efficiencies of PANI-$TiO_2$ composites decreased gradually as the CT increased further to 550 and $650^{\circ}C$. These results were ascribed to contents of anatase crystal phase and specific surface area of different particle sizes in the PANI-$TiO_2$ composites, which were demonstrated by the X-ray diffraction and scanning electron microscopy images, respectively. At the lowest input concentration (IC, 0.1 ppm), average control efficiencies of TCE and TTCE were 72 and 39%, respectively, whereas at the highest IC (1.0 ppm) they were 52 and 18%, respectively. As stream flow rate increased from 0.1 to 1.0 L $min^{-1}$, the average control efficiencies of TCE and TTCE decreased from ca. 100 to 47% and ca. 100 to 18%, respectively. In addition, the average control efficiencies of TCE and TTCE decreased from ca. 100 to 23% and ca. 100 to 8%, respectively as the relative humidity increased from 20 to 95%. Overall, these findings indicated that as-prepared PANI-$TiO_2$ composites could be used efficiently for control of chlorinated compounds at indoor air levels;if operational conditions were optimized.

SURFACE CHARACTERISTICS AND BIOACTIVITY OF ANODICALLY OXIDIZED TITANIUM SURFACES (양극산화에 의한 티타늄 산화막의 표면 특성 및 생체 활성에 관한 연구)

  • Lee, Sang-Han;Cho, In-Ho
    • The Journal of Korean Academy of Prosthodontics
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    • v.45 no.1
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    • pp.85-97
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    • 2007
  • Statement of problem: Recently, anodic oxidation of cp-titanium is a popular method for treatment of titanium implant surfaces. It is a relatively easy process, and the thickness, structure, composition, and the microstructure of the oxide layer can be variably modified. Moreover the biological properties of the oxide layer can be controlled. Purpose: In this study, the roughness, microstructure, crystal structure of the variously treated groups (current, voltage, frequency, electrolyte, thermal treatment) were evaluated. And the specimens were soaked in simulated body fluid (SBF) to evaluate the effects of the surface characteristics and the oxide layers on the bioactivity of the specimens which were directly related to bone formation and integration. Materials and methods: Surface treatments consisted of either anodization or anodization followed thermal treatment. Specimens were divided into seven groups, depending on their anodizing treatment conditions: constant current mode (350V for group 2), constant voltage mode (155V for group 3), 60 Hz pulse series (230V for group 4, 300V for group 5), and 1000 Hz pulse series (400V for group 6, 460V for group 7). Non-treated native surfaces were used as controls (group 1). In addition, for the purpose of evaluating the effects of thermal treatment, each group was heat treated by elevating the temperature by $5^{\circ}C$ per minute until $600^{\circ}C$ for 1 hour, and then bench cured. Using scanning electron microscope (SEM), porous oxide layers were observed on treated surfaces. The crystal structures and phases of titania were identified by thin-film x-ray diffractmeter (TF-XRD). Atomic force microscope (AFM) was used for roughness measurement (Sa, Sq). To evaluate bioactivity of modified titanium surfaces, each group was soaked in SBF for 168 hours (1 week), and then changed surface characteristics were analyzed by SEM and TF-XRD. Results: On basis of our findings, we concluded the following results. 1. Most groups showed morphologically porous structures. Except group 2, all groups showed fine to coarse convex structures, and the groups with superior quantity of oxide products showed superior morphology. 2. As a result of combined anodization and thermal treatment, there were no effects on composition of crystalline structure. But, heat treatment influenced the quantity of formation of the oxide products (rutile / anatase). 3. Roughness decreased in the order of groups 7,5,2,3,6,4,1 and there was statistical difference between group 7 and the others (p<0.05), but group 7 did not show any bioactivity within a week. 4. In groups that implanted ions (Ca/P) on the oxide layer through current and voltage control, showed superior morphology, and oxide products, but did not express any bioactivity within a week. 5. In group 3, the oxide layer was uniformly organized with rutile, with almost no titanium peak. And there were abnormally more [101] orientations of rutile crystalline structure, and bonelike apatite formation could be seen around these crystalline structures. Conclusion: As a result of control of various factors in anodization (current, voltage, frequency, electrolytes, thermal treatment), the surface morphology, micro-porosity, the 2nd phase formation, crystalline structure, thickness of the oxide layer could be modified. And even more, the bioactivity of the specimens in vitro could be induced. Thus anodic oxidation can be considered as an excellent surface treatment method that will able to not only control the physical properties but enhance the biological characteristics of the oxide layer. Furthermore, it is recommended in near future animal research to prove these results.

Surface characteristics and stability of implants treated with alkali and heat (알칼리와 열처리에 의한 임플란트의 표면 특성 및 골유착 안정성에 관한 연구)

  • Song, Yun-Seok;Cho, In-Ho
    • The Journal of Korean Academy of Prosthodontics
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    • v.46 no.5
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    • pp.490-499
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    • 2008
  • Statement of problem: Bioactive materials must have the ability to spontaneously form a bone like apatite layer on their surface and induce direct biochemical bonding to bone. A simple chemical treatment via alkali and heat has been revealed to induce bioactivity in titanium. Purpose: The purpose of this study was to evaluate the surface characteristics and stability of alkali and heat treated implants. Material and methods: Specimens were divided into three groups; group 1 was the control group with machined surface implants, groups 2 and 3 were treated with alkali solutions and heat treated in the atmosphere and vacuum conditions respectively. The surface characteristics were observed with FESEM, XPS, TF-XRD and AFM. Stability was evaluated with the resonance frequency analysis, periotest and removal torque values. One-way ANOVA and Duncan test were used for statistical analysis. Results: 1. Groups treated with alkali and heat showed similar characteristics. Groups 2 and 3 showed high compositions of Na ions on the surface with sub-micron sized pores compared to group 1. Group 2 showed mixed compositions of anatase and rutile with superior contents of rutile. 2. Resonance frequency analysis : The ISQ of group 2 showed significantly higher values than that of groups 1 and 3 at 12 weeks. The ISQ of groups 1 and 2 showed significant increase after 4 weeks, and the ISQ of group 3 increased significantly after 2 and 4 weeks respectively (P < .05). 3. Periotest: The PTV of groups 1 and 2 showed significant decrease after 4 weeks, and the PTV of group 3 showed significant decrease after 2 and 4 weeks respectively (P < .05). 4. Removal torque analysis: The removal torque value of group 2 was significantly higher than those of groups 1 and 3 at 2, 4 and 8 weeks. The removal torque values of groups 1 and 3 showed increase at 4 and 12 weeks, but the removal torque value of group 2 showed increase after 4 weeks (P < .05). Conclusion: An oxide layer with appropriate crystal structure and amorphous sodium titanate layer can be obtained on titanium implants through alkali and heat treatment in the atmosphere, and even alkali and heat treatment in vacuum conditions, provided a bioactive surface containing sodium. These surface layers can be considered to be effective for enhancement of osseointegration and reduction of healing period for implant treatment.

Solvothermal Preparation of Nanocrystalline TiO2 Using Alcohol-water Mixed Solvent (알코올-물 혼합용액을 이용하는 Solvothermal 법에 의한 나노크기의 TiO2 제조)

  • Lee, Sang Geun;Park, Seong Soo;Hong, Seong Soo;Park, Jong Myung;Lee, Seung Ho;Kim, Dae Sung;Lee, Gun Dae
    • Applied Chemistry for Engineering
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    • v.22 no.6
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    • pp.685-690
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    • 2011
  • In this study, a solvothermal reaction to prepare nanocrystalline titania was carried out using $TiCl_4$ and mixed solvents of alcohol and water. The effects of the type and the composition of alcohol on the crystal structure and agglomeration of final $TiO_2$ products were investigated. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) as well as scanning electron microscopy (SEM). In the solvothermal reaction using the n-butanol solutions with different volume ratios of n-butanol/water (100/0, 75/25, 50/50, 25/75, 0/100), the extent of agglomeration of obtained rutile $TiO_2$ was found to change with the volume ratio of n-butanol/water, and the n-butanol/water ratio of 75/25 revealed the best result for the preparation of well-dispersed nanocrystalline $TiO_2$ powders. The crystal phase of $TiO_2$ prepared through the solvothermal reaction changed with the type of alcohol in solvent (alcohol/water = 75/25). $TiO_2$ products obtained with the aqueous solutions of methanol, ethanol and isopropanol have an anatase phase, while that with n-butanol has a rutile phase. The results showed that, in the solvothermal reaction using both $TiCl_4$ as a starting material and the alcohol-water mixed solvents without any other additive, the enhancement of dispersion and control of crystal structure of $TiO_2$ products can be feasible by simply varying the composition and type of alcohol in the mixed solvents.