Formation of TiO(OH)$_2$ Ultrafine Particles by Reverse Micelle

역마이셀에 의한 TiO(OH)$_2$ 미세분말 제조

  • 장화익 (강원지방중소기업청) ;
  • 강석원 (강원대학교 공과대학 화학공학과) ;
  • 이광래 (강원대학교 공과대학 화학공학과)
  • Published : 1998.06.01

Abstract

Titanium hydroxide (TiO({{{{ {OH }_{2 } }})) fine particles were produced by the reverse micelle technique. For the formation of titanium hydroxide (TiO({{{{ {OH }_{2 } }})) particles with the technique reversed micellar solution was prepared by solubilizing water into organic solvent (isooctane) with a surfactant and titanium alkoxide (tetraisopropyl orthotitanate) diluted with isopropyl alcohol was added to the reversed micellar solution. The hdrolyzed species (TiO({{{{ {OH }_{2 } }})) was formed by the hydrolysis of titanium alkoxide and titanium dioxide is then formed by the condensation of the hydrolyzed species. There are several process variables such as surfactants concentration of surface cosurfactant hydrolysis temperature and pH. In this work the ef-fects of process variables on paticle shapes particle size distribution and paticle agglomeration were bi-nodal for an anionic surfactant(AOT) in the whole range of temperature pH and surfactant concentration of this experiment. The addition of ethanol as a cosurfactant resulted in narrow particle size distribution of the experiment. The additiono of ethanol as a cosurfactant resulted in narrow particle size distribution and 0.12${\mu}{\textrm}{m}$ of smaller average particle diameter. FT-IR spectrum of particles shows the absorption peak of Ti-OH bonding and Ti-O bonding. An exothermic peak around 41$0^{\circ}C$ in TGA-DTA curve shows that crys- tallized anatase phase appears and completely transits to anatase around 45$0^{\circ}C$.

유기용메인 이소옥탄(isooctane)에 계면활성제를 이용하여 물을 역마이셀 형태로 생성시킨 후, 이소프로필 알코올(isopropyle alcohol)에 묽힌 티타늄알코옥사이드(tetraisopropyl orthotitanate)를 가하여 가수분해 반응를 거쳐 TiO(OH)2 분말을 제조하였다. 역마이셀에 의한 TiO(OH)2 분말 제조에 미치는 공정변수들인 계면활성제의 종류, 농도, 보조계면활성제, 가수분해 반응온도, pH등이 생성된 입자의 크기, 모양, 입도분포에 미치는 영향을 규명하였다. 비이온계활성제인 Span 80을 사용하였을 경우에는 Span 80의 농도변화, 가수분해 반응온도 변화, pH변화에 무관하게 입도분포가 uninodal형태였으나, 음이온계면활성제인 Aerosol-OT(AOT)를 사용하였을 경우, binodal형태를 나타내었다. 에타올(ethanol)을 cosurfactant로 첨가한 계(AOT, 1.0CMC, isooctane+ethanol, pH2.5, 30$^{\circ}C$)로 부터 생성된 입자는 평균입경이 0.12${\mu}{\textrm}{m}$ 으로서 미세할 뿐아니라 입도분포도 매우 좁은 것을 알 수 있다. 따라서, cosurfactant의 유무가 생성 입자의 입도분포에 큰 영향을 미치는 것을 알 수 있다. FT-IR 분석으로 T1-O 결합과 Ti-OH 결합에 의한 흡수피크를 확인하였고, TGA-DTA 분석결과에 의하면 41$0^{\circ}C$ 부근의 발열피크로 부터 비정질 구조에서 anatase 구조로 결정화가 시작됨을 알 수 있었으며, 온도 상승과 더불어 결정이 성장하여 약 45$0^{\circ}C$ 정도에서 비정질상이 anatase상의 결정구조로 완전히 전이됨을 확인하였다.

Keywords

References

  1. Mat. Sci. Eng. v.44 Basic Reactor Needs on High Temperature Ceramics for Energy Application H.K. Bowen
  2. Ceram. Bull. v.60 no.2 Nonconventional Powder Preparation Techniques D.W. Johnson
  3. Ceram. Bull. v.68 Powder Synthesis Research at CAMP S.K. Ellis;E.P. McNamara, Jr.
  4. Surfaces Interfaces and Colloids; Principles and Applications Drew Myers
  5. Introduction to Colloid and Surface Chemistry(4th ed.) D. J. Shaw
  6. Ind. Eng. Chem. Res. v.32 Mechnism of Formation of Titanium Dioxide Ultrafine Particles in Reverse Micelles by Hydrolysis of Titanium Tetrabutoxide T. Hirai;H. Sato;I. Komasawa
  7. J. Colloid and Interface Sci. v.93 no.1 Preparation and Characterization of Monodisperse Magnetite Sols in W/O Microemulsion M. Gobe;K. Kon-No;K. Kandori;A. Kitahara
  8. J. Dispersion Sci. and Tech. v.8 no.5&6 Preparation of CaCO₃Particles in Water Pool in Non aqueous Nonionic Surfactant Solutions K.Kandori;N.Shizuka;K.Kon-no;A.Kitahara
  9. J. Colloid and Interface Sci. v.115 no.2 Dispersion Stability of Nonaqueous Calcium Carbonate Dispersion Prepared in Water Core of w/o Microemulsion K. Kandori;K. Konno;A. Kltahara
  10. J. Colloid and Interface Sci. v.122 no.1 Formation of ionic Water/oil Microemulsions and Their Application in the preparation of CaCO₃Particles K. Kandori;K. Kon-No;A. Kitahara
  11. Surfactant Science Series v.51 Surface and Colloid Chemistry in Advanced Ceramics Processing R.J. Pugh;Lennart Bergstr m
  12. Accounts of Chem. Res. v.21 no.7 Microemulsions D. Langevin
  13. Foundations of Colloid Science v.Ⅱ R.J. Hunter
  14. Surfactant Science Series v.30 Microemulsions and Related Systems; Formulation, Solvency and Physical Properties M. Bourrel;R.S. Schechter
  15. J. Korean Ceramic Soc. v.33 no.4 Hydrothermal Synthesis of PbTiO₃Powders B.K. Park;T K Lee;K. G. Lee
  16. Better Ceramics Through Chemistry II Microporous Layers from Sol-gel Techniques A. Larbot;J.A. Alary;J.P. Fabre;C. Guizard;L. Cot
  17. J. Phys. Chem. v.75 Infrared Study of the Surface Titanium Dioxide-hydroxyl Groups M. Primet;P. Pichat;M.V. Mathieu
  18. Inorganic Chemistry v.2 T Titani
  19. Better Ceramics Through Chemistry II The gel Route to TiO₂Photoanodes S. Doeuff;M Henry;C. Sanchez