Preparation of Ag Fine Particles from Aqueous Silver Solution by Reduction Reaction

Ag 水溶液으로부터 還元反應에 의한 Ag 微粒子의 製造 硏究

  • Lee, Hwa-Young (Metals Processing Research Center, Korea Institute of Science & Technology) ;
  • Jin, Seon-Ah (School of Advanced Materials & Engineering, Kookmin University) ;
  • Han, Young-Ju (School of Advanced Materials & Engineering, Kookmin University)
  • 이화영 (韓國科學技術硏究院 金屬工程硏究센터) ;
  • 진선아 (國民大學校 新素材工學部) ;
  • 한영주 (國民大學校 新素材工學部)
  • Published : 2005.02.01

Abstract

A study on the preparation of Ag fine particles was performed through a reduction reaction using ascorbic acids as a reductant, which is one of the indispensable processes for the recycling of silver-bearing wastes. Silver nitrate solution in the range of 10~120 mmole/l was used and Tamol NN8906 or PVP was also used as a dispersant in the preparation of Ag fine particles size analyze, SEM, and TEM to determine the particle size and morphology of them. As a result, the reduction reaction of silver ions with ascorbic acid reached equilibrium within 10 min. It was found that about 60% excess of ascorbic acid was required in order to reduce completely silver ions in the solution. The particle size distribution of Ag particles prepared through the reduction reaction showed typically biomodal or trimodal distribution. Especially, initial Ag concentration in the solution, the type and amount of dispersant added during the reduction reaction played an important role in determining the mean particle size of Ag particles.

국내 폐은 원료로부터 고부가가치 Ag powder를 제조하기 위한 연구의 일환으로써 ascorbic acid를 환원제로 사용한 Ag 미립자 제조실험을 수행하였다. Ag 수용액은 질산은을 10~120 mmole/l의 범위로 용해시켜 사용하였으며, Ag 미립자의 응집방지를 위한 분산제로는 Tamol NN8906 및 PVP를 각각 사용하였다. 환원반응을 통하여 제조한 Ag 미립자는 X-선 회절분석, 입도분석, SEM 및 TEM 분석을 실시하여 morphology 와 평균입도를 측정하였다. ascorbic acid에 의한 수용액중 Ag 이온의 환원반응은 10분 이내에 거의 평형상태에 도달하였으며, 완전한 Ag 이온의 환원을 위해서는 ascorbic acid 첨가량이 이론치의 1.6배가 소요되었다. 생성된 Ag 미립자의 입도분포는 bimodal 혹은 trimodal의 분포곡선을 보였으며, Ag 미립자의 평균입도는 분산제 종류 및 첨가량과 수용액 중 초기 Ag 농도에 따라 달라지는 것으로 나타났다.

Keywords

References

  1. Sutugin, A. G. and Fuchs, N. A., 1968: Formation of condensation aerosils at high vapor supersaturation, J. Colloid and Interface Science, 27(2), pp. 216-228 https://doi.org/10.1016/0021-9797(68)90029-5
  2. Kruis, F. E., Goossens, A. and Fissan, H., 1996: Synthesis of semiconducting nanoparticles, J. Aerosol Science, 27(1), pp. 5165-5166
  3. Li, R. et al., 2003: Study of fine silver powder from AgOH slurry by hydrothermal techniques, J. Materials Processing Technology, 137, pp. 55-59 https://doi.org/10.1016/S0924-0136(02)01062-2
  4. Zhu, Y., Qian, Y., Zhang, M. and Chen, Z., 1993: Preparation of nanocrystalline silver powders by gammaray radiation combined with hydrothermal treatment, Materials Letters, 17(5), pp. 314-318 https://doi.org/10.1016/0167-577X(93)90021-O
  5. Junqing, H. et al., 2001: Hydrothermal preparation and characterization of nanocrystalline silver gallium sulfides, Solid State Sciences, 3(3), pp. 275-278 https://doi.org/10.1016/S1293-2558(00)01139-0
  6. Day, D. A., Zook, A. L., Barshick, C. M., and Hess, K. R., 1997: Electrochemical Deposition of metals in the preparation of standard materials for GDMS, Microchemical J., 55(2), pp. 208-221 https://doi.org/10.1006/mchj.1996.1415
  7. Chou, K. S. and Ren, C. Y., 2000: Synthesis of nanosized silver particles by chemical reduction method, Materials Chemistry and Physics, 64, pp. 241-246 https://doi.org/10.1016/S0254-0584(00)00223-6
  8. Sondi, I., Goia, D. V. and Matijevic, E., 2003: Preparation of highly concentrated stable dispersions of uniform silver nanoparticles, J. Colloid and Interface Science, 260, pp. 75-81 https://doi.org/10.1016/S0021-9797(02)00205-9
  9. Khanna, P. K. and Subbarao, V. V. V. S., 2003: Nanosized silver powder via reduction of silver nitrate by sodium formaldehydesulfoxylate in acidic pH medium, Materials Letters, 57, pp. 2242-2245 https://doi.org/10.1016/S0167-577X(02)01203-X
  10. Liz-Marzan, L. M. and Lado-Tourino, I., 1996: Reduction and stabilization of silver nanoparticles in ethanol by nonionic surfactants, Langmuir, 12, pp. 3585-3589 https://doi.org/10.1021/la951501e
  11. Rane, S. B. et al., 2003: Influence of surfactants treatment on silver powder and its thick films, Materials Letters, 57, pp. 3096-3100 https://doi.org/10.1016/S0167-577X(03)00003-X
  12. Pastoriza-Santos, I. and Liz-Marzan, L. M., 2002: Formation of PVP-protected metal nanoparticles in DMF, Langmuir, 18, pp. 2888-2894 https://doi.org/10.1021/la015578g
  13. Pastoriza-Santos, I. and Liz-Marzan, L. M., 2002: Synthesis of silver nanoprisms in DMF, Nano Letters, 2(8), pp. 903-905 https://doi.org/10.1021/nl025638i