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Polyamic acid: nanoprecipitation and electrophoretic deposition on porous supports

  • Libor Brabec
  • Petr Sysel
  • Jan Plsek
  • Milan Kocirik
  • James H. Dickerson
Article

Abstract

Polyamic acid (PAA, a precursor of polyimide) was synthesized from 4,4′-oxydiphthalic anhydride and 4,4′-oxydianiline. PAA, dissolved in dimethylsulfoxide (DMSO), was precipitated into colloidal particles after its injection into acetone. The resulting particle size distribution was found to depend on aging time of PAA solutions, their concentration, and the manner in which the solutions were mixed with acetone. PAA particles of any size down to 10 nm appeared to be achievable by decreasing the acetone/DMSO ratio. Particles in DMSO/acetone suspensions were found to have a significant negative zeta potential. Therefore, there was no need to add organic bases to form PAA anions, in contrast to all previously published studies on the PAA electrodeposition. EPD was performed onto porous stainless-steel or alumina disks, which are suitable supports (reinforcements) for membranes. The slow evaporation of DMSO residue yielded dried polymer layers, comprised of 50–100 nm PAA globules. The outer surface of layers was usually covered with a very thin, continuous PAA skin. Such supported PAA layers—after a simple imidization step via a heat treatment—could be applied as thermally resistant membranes for gas separation.

Keywords

Dimethylsulfoxide EPD Polyimide Precipitation Zeta potential 

Supplementary material

11998_2017_4_MOESM1_ESM.docx (8.4 mb)
Supplementary material 1 (DOCX 8599 kb)

References

  1. 1.
    Assa, J, Spassova, E, Karamancheva, I, Dimitrova, T, Rangelov, N, Danev, G, “Thin Polyimide Layers—Preparation and Properties.” Vacuum, 51 185–188 (1998)CrossRefGoogle Scholar
  2. 2.
    Ha, Y, Choi, M-C, Jo, N, Kim, I, Ha, C-S, Han, D, Han, S, Han, M, “Polyimide Multilayer Thin Films Prepared via Spin Coating from Poly(Amic Acid) and Poly(Amic Acid) Ammonium Salt.” Macromol. Res., 16 725–733 (2008)CrossRefGoogle Scholar
  3. 3.
    Duggal, AR, Rogers, JA, Nelson, KA, “Real-Time Optical Characterization of Surface Acoustic Modes of Polyimide Thin-Film Coatings.” J. Appl. Phys., 72 2823–2839 (1992)CrossRefGoogle Scholar
  4. 4.
    Niwa, M, Kawakami, H, Kanamori, T, Shinbo, T, Kaito, A, Nagaoka, S, “Gas Separation of Asymmetric 6FDA Polyimide Membrane with Oriented Surface Skin Layer.” Macromolecules, 34 9039–9044 (2001)CrossRefGoogle Scholar
  5. 5.
    Frycova, M, Sysel, P, Kocirik, M, Brabec, L, Hrabanek, P, Prokopova, O, Bernauer, B, Zikanova, A, “Mixed Matrix Membranes Based on 3-Aminopropyltriethoxysilane Endcapped Polyimides and Silicalite-1.” J. Appl. Polym. Sci., 124 E233–E240 (2012)CrossRefGoogle Scholar
  6. 6.
    Cai, D, Su, J, Huang, M, Liu, Y, Wang, J, Dai, L, “Synthesis, Characterization and Hydrolytic Stability of Poly (Amic Acid) Ammonium Salt.” Polym. Degrad. Stab., 96 2174–2180 (2011)Google Scholar
  7. 7.
    Phillips, DC, “Electrolytically Formed Polyimide Films and Coatings: I. Electrodeposition from Colloidal Dispersions.” J. Electrochem. Soc., 119 1645–1649 (1972)CrossRefGoogle Scholar
  8. 8.
    Alvino, WM, Scala, LC, “Electrodeposition of Polymers from Nonaqueous Systems. I. Polyimides: Some Deposition Parameters.” J. Appl. Polym. Sci., 27 341–351 (1982)CrossRefGoogle Scholar
  9. 9.
    Alvino, WM, Fuller, TJ, Scala, LC, “Electrophoretic Deposition of Polymers. II. Polyimides: A Coulombic Study.” J. Appl. Polym. Sci., 28 267–282 (1983)CrossRefGoogle Scholar
  10. 10.
    Uebner, M, Ng, KM, “Electrodeposition of Polyimides from Nonaqueous Emulsions.” J. Appl. Polym. Sci., 36 1525–1540 (1988)CrossRefGoogle Scholar
  11. 11.
    Yang, C-P, Chen, Y-H, “Studies on the Electrodeposition of Polyimides.” Die Angew. Makromol. Chemie., 160 91–106 (1988)CrossRefGoogle Scholar
  12. 12.
    Buchwalter, SL, “Electrophoretic Deposition of Polyimides: Electrocoating on the Cathode.” In: Lupinski, JH, Moore, RS (eds.) Polymeric Materials for Electronics Packaging and Interconnection, pp. 154–167. ACS Symposium Series, Washington (1989)CrossRefGoogle Scholar
  13. 13.
    Iroh, JO, Yuan, W, “Surface Properties of Carbon Fibres Modified by Electrodeposition of Polyamic Acid.” Polymer (Guildf)., 37 4197–4203 (1996)CrossRefGoogle Scholar
  14. 14.
    Chen, Y, Iroh, JO, “Electrodeposition of BTDA-ODA-PDA Polyamic Acid Coatings on Carbon Fibers from Nonaqueous Emulsions.” Polym. Eng. Sci., 39 699–707 (1999)CrossRefGoogle Scholar
  15. 15.
    He, S, Zhang, S, Lu, C, Wu, G, Yang, Y, An, F, Guo, J, Li, H, “Polyimide Nano-Coating on Carbon Fibers by Electrophoretic Deposition.” Colloids Surf. A Physicochem. Eng. Asp., 381 118–122 (2011)CrossRefGoogle Scholar
  16. 16.
    Wang, C-A, Long, B, Lin, W, Huang, Y, Sun, J, “Poly(Amic Acid)–Clay Nacrelike Composites Prepared by Electrophoretic Deposition.” J. Mater. Res., 23 1706–1712 (2008)CrossRefGoogle Scholar
  17. 17.
    Ding, F, Tong, Y, Luo, X, Guan, H, Hu, B, “Preparation, Characterization, and Properties of Polyamic Acid Nano-Emulsion.” Polym. Adv. Technol., 22 2633–2637 (2011)CrossRefGoogle Scholar
  18. 18.
    Xiong, JY, Liu, XY, Chen, SB, Chung, TS, “Surfactant Free Fabrication of Polyimide Nanoparticles.” Appl. Phys. Lett., 85 5733–5735 (2004)CrossRefGoogle Scholar
  19. 19.
    Lin, T, Stickney, KW, Rogers, M, Riffle, JS, McGrath, JE, Marand, H, Yu, TH, Davis, RM, “Preparation of Submicrometre Polyimide Particles by Precipitation from Solution.” Polymer (Guildf)., 34 772–777 (1993)CrossRefGoogle Scholar
  20. 20.
    Kim, JH, Min, BR, Won, J, Park, HC, Kang, YS, “Phase Behavior and Mechanism of Membrane Formation for Polyimide/DMSO/Water System.” J. Membr. Sci., 187 47–55 (2001)CrossRefGoogle Scholar
  21. 21.
    Syal, V, Chauhan, S, Kumari, U, “Ultrasonic Velocity of Binary Mixtures of Acetone and Dioxane with Dimethylsulphoxide as One Component.” Indian J. Pure Appl. Phys., 43 844–848 (2005)Google Scholar
  22. 22.
    Ke, F, Song, N, Liang, D, Xu, H, “A Method to Break Charge Transfer Complex of Polyimide: A Study on Solution Behavior.” J. Appl. Polym. Sci., 127 797–803 (2013)CrossRefGoogle Scholar
  23. 23.
    Magarik, SY, “Macromolecules of Polyamic Acids and Polyimides.” In: Bessonov, MI, Zubkov, VA (eds.) Polyamic Acids and Polyimides: Synthesis, Transformations, and Structure, pp. 281–362. CRC Press, Boca Raton (1993)Google Scholar
  24. 24.
    Anthamatten, M, Letts, SA, Cook, RC, “Controlling Surface Roughness in Vapor-Deposited Poly (Amic Acid) Films by Solvent-Vapor Exposure.” Langmuir., 20 6288–6296 (2004)CrossRefGoogle Scholar
  25. 25.
    Ogura, T, Saito, Y, Higashihara, T, Ueda, M, “Formation of Spherical Nanoparticles in Poly(Amic Acid) Films.” Polym. Chem., 3 2165–2169 (2012)CrossRefGoogle Scholar
  26. 26.
    Lee, H, Won, J, Park, H, Lee, H, Kang, Y, “Effect of Poly (Amic Acid) Imidization on Solution Characteristics and Membrane Morphology.” J. Membr. Sci., 178 35–41 (2000)CrossRefGoogle Scholar
  27. 27.
    Luo, Y, Li, B, Liang, L, Tan, B, “Synthesis of Cost-Effective Porous Polyimides and Their Gas Storage Properties.” Chem. Commun. (Camb), 47 7704–7706 (2011)CrossRefGoogle Scholar

Copyright information

© American Coatings Association 2017

Authors and Affiliations

  1. 1.J. Heyrovsky Institute of Physical Chemistry of the CASPrague 8Czech Republic
  2. 2.University of Chemistry and TechnologyPrague 6Czech Republic
  3. 3.Department of PhysicsBrown UniversityProvidenceUSA

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