Preparation of Ag Nano-Powder from Aqueous Silver Nitrate Solution through Reduction with Hydrazine Hydrate

Hydrazine Hydrate 환원(還元)에 의한 질산은(窒酸銀) 수용액(水溶液)으로부터 은(銀) 나노분말(粉末)의 제조(製造) 연구(硏究)

  • Lee, Hwa-Young (Battery Research Center, Korea Institute of Science & Technology)
  • 이화영 (한국과학기술연구원 이차전지연구센터)
  • Published : 2006.08.01

Abstract

The preparation of Ag nano-powder from aqueous silver nitrate solution, which would be available for the recycling of silver bearing wastes, was investigated by a reductive precipitation reaction using hydrazine hydrate as a reducing agent. Silver solution was prepared by dissolving silver nitrate with distilled water, and then the dispersant, Tamol NN8906 or Tween 20, was also mixed to avoid the agglomeration of particles during the reductive reaction followed by the addition of hydrazine hydrate to prepare Ag nano-particles. Ag particles obtained from the reduction reaction from silver solution were characterized using the particle size analyzer and TEM to determine the particle size distribution and morphology. It was found that about 100% excess of hydrazine hydrate was required to reduce completely silver ions in the solution. Ag powders with very narrow distribution could be obtained when Tamol NN8906 was used as the dispersant. In case of Tween 20, the particle size distribution showed typically the bimodal or multimodal distribution and the morphology of Ag particles was found to be irregular shape in both cases.

함은 폐재의 리싸이클링을 위한 연구의 일환으로써 Hydrazine Hydrate을 환원제로 사용하여 질산은 수용액으로부터 Ag 나노분말을 제조하기 위한 실험을 수행하였다. 이를 위해 질산은을 소정 농도로 증류수에 용해시킨 수용액에 Ag 미립자의 응집방지를 위한 분산제로써 Tamol NN8906 혹은 Tween 20을 미리 혼합한 다음 환원제인 Hydrazine Hydrate 용액을 첨가하는 방법으로 환원반응을 실시하였다. 환원반응을 통하여 제조한 Ag 미립자는 입도분석기 및 TEM 측정을 통하여 형상과 평균입도를 측정하였다. Hydrazine Hydrate에 의한 은의 환원을 위해서는 이론치의 약 2배를 첨가해 주어야 하는 것으로 나타났으며, Tamol NN8906을 분산제로 사용하여 제조한 Ag 나노분발은 매우 좁은 입도범위의 분포특성을 보여 주었다. Tween 20을 분산제로 사용한 경우의 입도 분포는 bimodal 혹은 multimodal distribution을 보였으며, 입자 모양에 있어서는 Tamol NN8906과 Tween 20이 모두 비슷하게 표면이 매끄러운 불규칙한 모양의 입자들로 구성되어 있었다.

Keywords

References

  1. Ko, T and Hwang, D. K., 2003: Preparation of'nanocrystalline lead zirconate powder by homogeneous precipitation, Materials Letters, 57, pp. 2472-2479 https://doi.org/10.1016/S0167-577X(02)01296-X
  2. Tan, Q. et al., 2003: Influence of polyelectrolyte dispersant on slip preparation of nano-sized tetragonal zirconia, Materials Chemistry and Physics, 80(3), pp. 615-619 https://doi.org/10.1016/S0254-0584(03)00103-2
  3. Li, Q. et al., 2003: Preparation of ultra fine $ MnO_2 $ powders by the solid state method reaction of $ KMnO_4 $, J. of Materials Processing Technology, 137, pp. 25-29 https://doi.org/10.1016/S0924-0136(02)01059-2
  4. 한국무역합회, 2004: '무역통계연감', 한국
  5. 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
  6. Kruis, F. E., Goossens, A. and Fissan, H., 1996: Synthesis of semiconducting nanoparticles, J. Aerosol Science, 27(1), pp. S 165-S 166 https://doi.org/10.1016/0021-8502(96)00155-3
  7. Chou, K. S. and Ren, C. Y., 2000: Synthesis ofnanosized 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. 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
  11. Zhu, Y., Qian, Y., Zhang, M. and Chen, Z., 1993: Preparation of nanocrystalline silver powders by gamma-ray radiation combined with hydrothermal treatment, Materials Letters, 17(5), pp. 314-318 https://doi.org/10.1016/0167-577X(93)90021-O
  12. 이화영, 진선아, 한영주, 2005: Ag 수용액으로부터 환원반응에 의한 Ag 미립자의 제조연구, 자원리싸이클링학회지, 14(1), pp. 26-32