Elsevier

Scripta Materialia

Volume 44, Issues 8–9, 18 May 2001, Pages 2213-2217
Scripta Materialia

In situ characterization of TiO2 nanoparticle in chemical vapor condensation reactor

https://doi.org/10.1016/S1359-6462(01)00747-3Get rights and content

Introduction

Chemical vapor condensation (CVC) has been reported to be appropriate for synthesizing high purity and non-agglomerated ultra fine particles with superior functional properties [1]. However, the formation process of nanoparticles during the CVC process is not fully understood. This is mainly due to some limitations in the characterization of nanoparticles as well as a lack of knowledge on the roles of thermodynamic and kinetic parameters. Recently, the authors have reported that the flow rate of O2 reaction gas can modify the characteristics of TiO2 nanoparticles by a coagulation process in the reactor 2, 3. Unfortunately, however, there are still no acceptable explanations about the exact role of the O2 flow rate. This problem has been recognized to be due to the difficulty in direct measurement of the particle characteristics during the coagulation process. In the present study, we have first attempted to investigate the effect of the O2 reaction gas on the CVC process of TiO2 nanoparticles by a real time characterization technique using a scanning mobility particle sizer (SMPS) 4, 5. Based on this investigation, we examined closely the formation mechanism of TiO2 nanoparticles in the CVC process with the aid of TEM observation.

Section snippets

Experiment

Titanium-tetra-isopropoxide (TTIP) used as a precursor was poured into the evaporator (held at 250°C) by a micro pump with a flow rate of 0.14 ml/min. The precursor vapor was delivered into the reactor furnace by He carrier gas with a flow rate of 1 lpm (refer to Fig. 1). In order to investigate the effect of the O2 flow rate on the coagulation process of TiO2 particles in the CVC reactor, the O2 flow rate was varied by 2, 3 and 4 lpm of which total flow rates of O2+He consequently

Effect of O2 flow rate

In Fig. 2, the highly resolved size distributions of TiO2 particles measured by SMPS in the CVC reactor were plotted as a function of O2 flow rates. The particle size distributions were expressed by the normalized concentration by dividing the total particle number in unit volume. With the increasing O2 flow rate, the size distribution of TiO2 particles became narrow and the mean particle size decreased from 104 to 81 nm. This suggests that the mono-sized fine particles could be obtained at a

Conclusion

The effects of O2 flow rate on the particle coagulation in the CVC reactor were investigated using SMPS. With a decrease of O2 flow rate, the TiO2 particle size increased and the size distribution broadened with a longer residence time and a higher particle concentration. These characteristics in size were dominantly controlled by the ratio of O2 flow rate in the CVC reactor.

Acknowledgements

The authors wish to acknowledge the financial support of Hanyang University, Korea, made in the program year of 2000 and greatly thank Dr. S. T. Oh for his helpful comments.

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