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 Sun Ha Lee1, Yangkyu Ahn1*, In Jung2, Keunwoo Lee2

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Presentation on theme: " Sun Ha Lee1, Yangkyu Ahn1*, In Jung2, Keunwoo Lee2"— Presentation transcript:

1 Preparation of Spherical Silica-coated Ceria Nanoparticles by Sol-Gel Method
 Sun Ha Lee1, Yangkyu Ahn1*, In Jung2, Keunwoo Lee2  1Department of Nanochemistry & Biochemistry, Konyang University, Korea 2 Inochem, BI Center, Konyang University, Korea Tel

2 Abstract DEPARTMENT OF NANOCHEMISTRY & BIOCHEMISTRY KONYANG UNIVERSITY
Monodispersed spherical silica-coated ceria nanoparticles were prepared through a sol-gel process using tetraethylorthosilicate (TEOS) and ceria fine particles. In this process, ceria fine particles were also prepared from cerium nitrate. The mean size of ceria particles was 300nm. Silica nanoparticles with narrow particle size distribution were prepared by controlled hydrolysis of TEOS solution. The silica sols were obtained by peptization, the process of redispersing a coagulated colloid, and were coated on ceria particles by the control of the weight ratio of silica/ceria and the pH of the mixture in aqueous solution. The morphologies of particles were characterized with scaning electron microscopy(SEM), transmission electron microscopy(TEM) and atomic force microscopy(AFM). The coating thickness of silica particles obtained by using this method was controlled in the range of nm.      DEPARTMENT OF NANOCHEMISTRY & BIOCHEMISTRY KONYANG UNIVERSITY

3 Sol-Gel Method Sol-gel process : With thermal decomposition of the gelation due to the hydrolysis and condensation reaction of the alcoxide or organic compounds and the vaporization due to same thermal reaction the oxide thin film production. DEPARTMENT OF NANOCHEMISTRY & BIOCHEMISTRY KONYANG UNIVERSITY

4 Sol-Gel Application Powders, Grains and Spheres Fibers Thin films and coatings -Optical coating -Electronic films -Protective films -Porous films Monoliths -Fiber optic preform -Lenses -Graded refractive index glass -Transparent foam application Composites Porous gels and membranes DEPARTMENT OF NANOCHEMISTRY & BIOCHEMISTRY KONYANG UNIVERSITY

5 Sol-Gel Process for Colloidal Silica
Growing TEOS EtOH NH4OH H2O Generation of seed Fabrication process of silica sol Application(Coating or Powder) Mixing Hydrolysis Reaction DEPARTMENT OF NANOCHEMISTRY & BIOCHEMISTRY KONYANG UNIVERSITY

6 Synthesis Process of Nanosized Ceria Powder
Ce(CO3)9H2O+HCl, HNO3 (Dissolution) Filtering Cerium Hydroxide Washing Firing Milling Work for Sol Drying CeO2-Sol CeO2 Powder DEPARTMENT OF NANOCHEMISTRY & BIOCHEMISTRY KONYANG UNIVERSITY

7 NH OH 4 SiO 2 TEOS TEOS EtOH EtOH EtOH Synthesis of Nanosized Silica
Stop reaction 4 SiO 2 TEOS TEOS EtOH EtOH S H S H EtOH optimum conditions:  add TEOS, mmol  stirring time : 30 min  stirring temperature : room temperature optimum conditions:  add NH4OH, mmol  stirring time : 2hr  stirring temperature : 45℃ Washing by centrifuge SiO2 Drying at 80℃ DEPARTMENT OF NANOCHEMISTRY & BIOCHEMISTRY KONYANG UNIVERSITY

8 TEOS EtOH NH 4 OH CeO 2 EtOH TEOS
Preparation of Silica Coated Ceria Particles optimum conditions:  1hr stirring at 45℃  1hr stirring at room temperature SiO2 H S TEOS EtOH NH 4 OH CeO 2 30nm CeO2 EtOH H S TEOS 300nm Drying for 24hr at 80℃ DEPARTMENT OF NANOCHEMISTRY & BIOCHEMISTRY KONYANG UNIVERSITY

9 Size Control by Base/TEOS Ratio
(1) EtOH/TEOS molar rate NH3/TEOS molar rate Particles size (nm) (1) 35.14 0.14 25 (2) 30.04 64 (3) 26.62 97 (4) 24.08 115 (2) (3) (4) at 45℃ NH3/TEOS molar rate EtOH/TEOS molar rate Particles size (nm) (1) 0.11 30.04 32 (2) 0.13 57 (3) 0.14 82 (4) 0.17 117 (4) (3) (2) (1) at 45℃ DEPARTMENT OF NANOCHEMISTRY & BIOCHEMISTRY KONYANG UNIVERSITY

10 Size Control by Ethanol/TEOS Ratio
(1) EtOH/TEOS molar rate NH3/TEOS molar rate Particles size (nm) (1) 35.14 0.14 25 (2) 30.04 64 (3) 26.62 97 (4) 24.08 115 (2) (3) (4) at 45℃ NH3/TEOS molar rate EtOH/TEOS molar rate Particles size (nm) (1) 0.11 30.04 32 (2) 0.13 57 (3) 0.14 82 (4) 0.17 117 (4) (3) (2) (1) at 45℃ DEPARTMENT OF NANOCHEMISTRY & BIOCHEMISTRY KONYANG UNIVERSITY

11 Characterization of Silica Sol
AFM image (2) (1) Mean(nm) 45.6 45.1 42.2 temperature (℃) Particles size (nm) (1) 45 74 (2) 25 110 DEPARTMENT OF NANOCHEMISTRY & BIOCHEMISTRY KONYANG UNIVERSITY

12 SEM Images of Colloidal Silica
DEPARTMENT OF NANOCHEMISTRY & BIOCHEMISTRY KONYANG UNIVERSITY

13 X-ray diffraction pattern
XRD Analysis Results X-ray diffraction pattern Silica - amorphous Silica coated ceria Ceria - crystal DEPARTMENT OF NANOCHEMISTRY & BIOCHEMISTRY KONYANG UNIVERSITY

14 Microscopic Images of the Samples
Silica coated ceria powder Silica nanopowder ( 30 nm) ceria powder (250 ~ 350nm) DEPARTMENT OF NANOCHEMISTRY & BIOCHEMISTRY KONYANG UNIVERSITY

15 Conclusions (1) The nanosize of the colloidal silica can controlled by ethanol/TEOS molar ratio. (2) The size of the colloidal silica can controlled by base/TEOS molar ratio. (3) Monodispersed particles were prepared by hydrolysis of TEOS in semi-batch reactor, and allowed to coat by addition of ceria particles. DEPARTMENT OF NANOCHEMISTRY & BIOCHEMISTRY KONYANG UNIVERSITY

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