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Segmented tubular synthesis of monodispersed microsized copper oxalate

  • Xun Liu
  • Xing Chen
  • Kai HuangEmail author
Article

Abstract

Monodispersed microsized copper oxalate particles were prepared in a segmented continuous flow tube reactor, and the effect of the main parameters such as organic additive agent, initial copper ions concentration, residence time, and segmented media on the final products were investigated experimentally. The obtained copper oxalate microsized particles were disc-like in the presence of citrate ligand, which was the shape inducer for the precipitated copper oxalate. Thermodynamic equilibrium diagrams of the Cu(II)-oxalate-H2O, Cu(II)-oxalate-citrate-H2O, and Cu(II)-oxalate-EDTA-H2O solution systems were drawn to estimate the possible copper species under the experimental conditions and to explain the formation mechanisms of copper oxalate particles in the segmented fluidic reactor. Both theoretical and experimental results indicated that the presence of chelating reagents such as citrate and EDTA had distinct effect on the evolution of particle shape. Air and kerosene were tested as media for the fluidic flow segmentation, and the latter was verified to better promote the growth of copper oxalate particles. The present study provides an easy method to prepare monodispersed copper oxalate microsized particles in a continuous scaling-up way, which can be utilized to prepare the precursor material for conductive inks.

Keywords

segmented flow tube reactor copper oxalate powder monodispersed scaling-up shape inducer 

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References

  1. [1]
    F. Roux, S. Amtablian, M. Anton, et al., Chalcopyrite thin-film solar cells by industry-compatible ink-based process, Sol. Energy Mater. Sol. Cells, 115(2013), p. 86.CrossRefGoogle Scholar
  2. [2]
    H. Min, B. Lee, S. Jeong, and M. Lee, Fabrication of 10 µm-scale conductive Cu patterns by selective laser sintering of Cu complex ink, Opt. Laser Technol., 88(2017), p. 128.CrossRefGoogle Scholar
  3. [3]
    C.W. Chang, T.Y. Cheng, and Y.C. Liao, Encapsulated silver nanoparticles in water/oil emulsion for conductive inks, J. Taiwan Inst. Chem. Eng., 92(2018), p. 8.CrossRefGoogle Scholar
  4. [4]
    S. Bose, S. Chakraborty, and D. Sanyal, Water-ethylene glycol mediated synthesis of silver nanoparticles for conductive ink, Mater. Today Proc., 5(2018), No. 3, p. 9941.CrossRefGoogle Scholar
  5. [5]
    J. Kastner, T. Faury, H.M. Außerhuber, et al., Silver-based reactive ink for inkjet-printing of conductive lines on textiles, Microelectron. Eng., 176(2017), p. 84.CrossRefGoogle Scholar
  6. [6]
    Z.H. Wang, W. Wang, Z.K. Jiang, and D. Yu, Low temperature sintering nano-silver conductive ink printed on cotton fabric as printed electronics, Prog. Org. Coat., 101(2016), p. 604.CrossRefGoogle Scholar
  7. [7]
    B.J. De Gans, P.C. Duineveld, and U.S. Schubert, Inkjet printing of polymers: State of the art and future developments, Adv. Mater., 16(2010), No. 3, p. 203.CrossRefGoogle Scholar
  8. [8]
    D. Kim, S. Jeong, and J. Moon, Synthesis of silver nanoparticles using the polyol process and the influence of precursor injection, Nanotechnology, 17(2006), No. 16, p. 4019.CrossRefGoogle Scholar
  9. [9]
    T. Öhlund, A.K. Schuppert, M. Hurnmelgård, J. Bäckström, H.E. Nilsson, and H. Olin, Inkjet fabrication of copper patterns for flexible electronics: Using paper with active precoatings, ACS Appl. Mater. Interfaces, 7(2015), No. 33, p. 18273.CrossRefGoogle Scholar
  10. [10]
    Y. Hokita, M. Kanzaki, T. Sugiyama, R. Arakawa, and H. Kawasaki, High-concentration synthesis of sub-10 nm copper nanoparticles for application to conductive nanoinks, ACS Appl. Mater. Interfaces, 7(2015), No. 34, p. 19382.CrossRefGoogle Scholar
  11. [11]
    T. Sugiyama, M. Kanzaki, R. Arakawa, and H. Kawasaki, Low-temperature sintering of metallacyclic stabilized copper nanoparticles and adhesion enhancement of conductive copper film to a polyimide substrate, J. Mater. Sci. Mater. Electron., 27(2016), No. 7, p. 7540.CrossRefGoogle Scholar
  12. [12]
    A. Yabuki, Y. Tachibana, and I.W. Fathona, Synthesis of copper conductive film by low-temperature thermal decomposition of copper-aminediol complexes under an air atmosphere, Mater. Chem. Phys., 148(2014), No. 1–2, p. 299.CrossRefGoogle Scholar
  13. [13]
    A. Yabuki, N. Arriffin, and M. Yanase, Low-temperature synthesis of copper conductive film by thermal decomposition of copper-amine complexes, Thin Solid Films, 519(2011), No. 19, p. 6530.CrossRefGoogle Scholar
  14. [14]
    A. Yabuki and S. Tanaka, Electrically conductive copper film prepared at low temperature by thermal decomposition of copper amine complexes with various amines, Mater. Res. Bull., 47(2012), No. 12, p. 4107.CrossRefGoogle Scholar
  15. [15]
    D. Adner, F.M. Wolf, S. Möckel, J. Perelaer, U.S. Schubert, and H. Lang, Copper(II) ethylene glycol carboxylates as precursors for inkjet printing of conductive copper patterns, Thin Solid Films, 565(2014), p. 143.CrossRefGoogle Scholar
  16. [16]
    Y. Dong, X.D. Li, S.H. Liu, Q. Zhu, M. Zhang, J.G. Li, and X.D. Sun, Optimizing formulations of silver organic decomposition ink for producing highly-conductive features on flexible substrates: The case study of amines, Thin Solid Films, 616(2016), p. 635.CrossRefGoogle Scholar
  17. [17]
    A.T. Royappa, A.D. Royappa, R.F. Moral, et al., Copper(I) oxalate complexes: Synthesis, structures and surprises, Polyhedron, 119(2016), p. 563.CrossRefGoogle Scholar
  18. [18]
    A. Manz, N. Graber, and H.M. Widmer, Miniaturized total chemical analysis systems: A novel concept for chemical sensing, Sens. Actuators B, 1(1990), No. 1–6, p. 244.CrossRefGoogle Scholar
  19. [19]
    J.H. Chun, S. Lu, Y.S. Lee, and V.W. Pike, Fast and high-yield micro-reactor syntheses of ortho-substituted [18F]fluoroarenes from reactions of [18F]fluoride ion with diaryliodonium salts, J. Org. Chem., 75(2010), No. 10, p. 3332.CrossRefGoogle Scholar
  20. [20]
    S.J. Haswell, R.J. Middleton, B. O’Sullivan, V. Skelton, P. Watts, and P. Styring, ChemInform abstract: The application of micro reactors to synthesis chemistry, Cheminform, 32(2010), No. 23, DOI:  https://doi.org/10.1002/chin.200123238.
  21. [21]
    K. Schubert, J. Brandner, M. Fichtner, G. Linder, U. Schygulla, and A. Wenka, Microstructure devices for applications in thermal and chemical process engineering, Microscale Thermophys. Eng., 5(2001), No. 1, p. 17.CrossRefGoogle Scholar
  22. [22]
    K. Jähnisch, V. Hessel, H. Löwe, and M. Baerns, Chemistry in microstructured reactors, Angew. Chem. Int. Ed., 43(2004), No. 4, p. 406.CrossRefGoogle Scholar
  23. [23]
    M.T. Tang, Theory and Technology of Complex Metallurgy, Central South University Press, Changsha, 2011.Google Scholar
  24. [24]
    X.W. Yang and D.F. Qiu, Hydrometallurgy, 2nd Ed., Metallurgical Industry Press, Beijing, 2011.Google Scholar
  25. [25]
    X.L. Zhou, Z.G. Yan, and X.D. Han, From ascorbic acid to oxalate: Hydrothermal synthesis of copper oxalate microspheres and conversion to oxide, Mater. Lett., 118(2014), p. 39.CrossRefGoogle Scholar

Copyright information

© University of Science and Technology Beijing and Springer-Verlag GmbH Germany, part of Springer Nature 2019

Authors and Affiliations

  1. 1.School of Metallurgical and Ecological EngineeringUniversity of Science and Technology BeijingBeijingChina
  2. 2.Beijing Key Lab of Green Recycling and Extraction of MetalsUniversity of Science and Technology BeijingBeijingChina

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