Skip to main content
SpringerLink
Log in

Correlation between morphology and electrical conductivity of dried and carbonized multi-walled carbon nanotube/resorcinol–formaldehyde xerogel composites

  • Original Paper
  • Published:
Journal of Materials Science Aims and scope Submit manuscript

Abstract

Monolithic multi-walled carbon nanotube (MWCNT)/resorcinol–formaldehyde (RF) composite xerogel was synthesized by sol–gel polymerization of RF monomers in a surfactant-stabilized MWCNT aqueous suspension. The resulting composite wet gel was dried under ambient conditions and pyrolyzed in a N2 atmosphere to obtain MWCNT/carbon (C) nanoporous xerogel. TEM images showed that the nanotubes had been completely exfoliated in the starting solution before addition of the reagents. Optical microscopy and SEM micrographs revealed that there were aggregates of MWCNTs with diameters of up to 50 µm in the final composites. Nitrogen adsorption analysis and mercury porosimetry of the pristine MWCNT-free and composite gels showed that the density and pore texture of the xerogel materials were not modified by the nanotubes, but were strongly influenced by the addition of surfactant (sodium dodecyl benzene sulfonate, NaDBS). Electrical conductivity was measured for the organic (MWCNT/RF) and carbonized (MWCNT/C) composites and evaluations determined that this parameter increased in different ways as a function of MWCNT concentration. A percolating scaling law of the form σ ∝ (ϕ−ϕ c)t was obtained with a volume percolation threshold of ϕ c = 2.5 × 10−4 and a critical exponent (t) of 1.0 for the organic nanocomposite. After pyrolysis, the carbonized xerogels exhibited an entirely different behavior with a continuous sharp increase in electrical conductivity with nanotube loading (4.5-fold increase at 1.64 v % MWCNT). Comparison of the data for experimental conductivity with the effective medium theory enabled estimation of an average length for the conductive strings formed by connected nanotube aggregations throughout the carbon matrix.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7
Fig. 8

Similar content being viewed by others

References

  1. Pekala RW (1989) Organic aerogels from the polycondensation of resorcinol with formaldehyde. J Mater Sci 24:3221–3227. doi:10.1007/BF01139044

    Article  Google Scholar 

  2. Maldonado-Hódar FJ (2013) Advances in the development of nanostructured catalysts based on carbon gels. Catal Today 218:43–50

    Article  Google Scholar 

  3. Kim SJ, Hwang SW, Hyun SH (2005) Preparation of carbon aerogel electrodes for supercapacitor and their electrochemical characteristics. J Mater Sci 40:725–731. doi:10.1007/s10853-005-6313-x

    Article  Google Scholar 

  4. Mirzaeian M, Hall PJ (2009) Preparation of controlled porosity carbon aerogels for energy storage in rechargeable lithium oxygen batteries. Electrochim Acta 54:7444–7451

    Article  Google Scholar 

  5. Wiener M, Reichenauer G, Braxmeier S et al (2009) Carbon aerogel-based high-temperature thermal insulation. Int J Thermophys 30:1372–1385

    Article  Google Scholar 

  6. Gao X, Omosebi A, Landon J, Liu K (2015) Surface charge enhanced carbon electrodes for stable and efficient capacitive deionization using inverted adsorption–desorption behavior. Energy Environ Sci 8:897–909

    Article  Google Scholar 

  7. Liu N, Shen J, Liu D (2013) A Fe 2 O 3 nanoparticle/carbon aerogel composite for use as an anode material for lithium ion batteries. Electrochim Acta 97:271–277

    Article  Google Scholar 

  8. Worsley MA, Pauzauskie PJ, Kucheyev SO et al (2009) Properties of single-walled carbon nanotube-based aerogels as a function of nanotube loading. Acta Mater 57:5131–5136

    Article  Google Scholar 

  9. Bordjiba T, Mohamedi M (2011) Molding versus dispersion: effect of the preparation procedure on the capacitive and cycle life of carbon nanotubes aerogel composites. J Solid State Electrochem 15:765–771

    Article  Google Scholar 

  10. Worsley MA, Satcher JH Jr, Baumann TF (2008) Synthesis and characterization of monolithic carbon aerogel nanocomposites containing double-walled carbon nanotubes. Langmuir 24:9763–9766

    Article  Google Scholar 

  11. Bouchard J, Cayla A, Devaux E, Campagne C (2013) Electrical and thermal conductivities of multiwalled carbon nanotubes-reinforced high performance polymer nanocomposites. Compos Sci Technol 86:177–184

    Article  Google Scholar 

  12. Périé T, Brosse A-C, Tencé-Girault S, Leibler L (2012) Mechanical and electrical properties of multi walled carbon nanotube/ABC block terpolymer composites. Carbon 50:2918–2928

    Article  Google Scholar 

  13. Jiang L, Gao L, Sun J (2003) Production of aqueous colloidal dispersions of carbon nanotubes. J Colloid Interface Sci 260:89–94

    Article  Google Scholar 

  14. Bryning M. B.: Carbon nanotube networks in epoxy composites and aerogels. PhD Dissertation, University of Pennsylvania (2007)

  15. Sahoo NG, Rana S, Cho JW et al (2010) Polymer nanocomposites based on functionalized carbon nanotubes. Prog Polym Sci 35:837–867

    Article  Google Scholar 

  16. Li J, Ma PC, Chow WS et al (2007) Correlations between percolation threshold, dispersion state, and aspect ratio of carbon nanotubes. Adv Funct Mater 17:3207–3215

    Article  Google Scholar 

  17. Bao H, Sun Y, Xiong Z et al (2013) Effects of the dispersion state and aspect ratio of carbon nanotubes on their electrical percolation threshold in a polymer. J Appl Polym Sci 128:735–740

    Article  Google Scholar 

  18. Park KS, Youn JR (2012) Dispersion and aspect ratio of carbon nanotubes in aqueous suspension and their relationship with electrical resistivity of carbon nanotube filled polymer composites. Carbon 50:2322–2330

    Article  Google Scholar 

  19. Haghgoo M, Plougonven E, Yousefi AA et al (2012) Use of X-ray microtomography to study the homogeneity of carbon nanotube aqueous suspensions and carbon nanotube/polymer composites. Carbon 50:1703–1706

    Article  Google Scholar 

  20. Haghgoo M, Yousefi AA, Mehr MJZ et al (2014) Characterization of multi-walled carbon nanotube dispersion in resorcinol–formaldehyde aerogels. Microporous Mesoporous Mater 184:97–104

    Article  Google Scholar 

  21. Job N, Sabatier F, Pirard J-P et al (2006) Towards the production of carbon xerogel monoliths by optimizing convective drying conditions. Carbon 44:2534–2542

    Article  Google Scholar 

  22. Washburn EW (1921) Note on a method of determining the distribution of pore sizes in a porous material. Proc Natl Acad Sci USA 7:115–116

    Article  Google Scholar 

  23. Job N, Pirard R, Pirard J, Alié C (2006) Non Intrusive Mercury Porosimetry: pyrolysis of Resorcinol-Formaldehyde Xerogels. Part Part Syst Charact 23:72–81

    Article  Google Scholar 

  24. Job N, Pirard R, Marien J, Pirard J-P (2004) Porous carbon xerogels with texture tailored by pH control during sol–gel process. Carbon 42:619–628

    Article  Google Scholar 

  25. White B, Banerjee S, O’Brien S et al (2007) Zeta-potential measurements of surfactant-wrapped individual single-walled carbon nanotubes. J Phys Chem C 111:13684–13690

    Article  Google Scholar 

  26. Zhao W, Song C, Pehrsson PE (2002) Water-soluble and optically pH-sensitive single-walled carbon nanotubes from surface modification. J Am Chem Soc 124:12418–12419

    Article  Google Scholar 

  27. Heister E, Lamprecht C, Neves V et al (2010) Higher dispersion efficacy of functionalized carbon nanotubes in chemical and biological environments. ACS Nano 4:2615–2626

    Article  Google Scholar 

  28. Feng J, Zhang C, Feng J et al (2011) Carbon aerogel composites prepared by ambient drying and using oxidized polyacrylonitrile fibers as reinforcements. ACS Appl Mater Interfaces 3:4796–4803

    Article  Google Scholar 

  29. Job N, Théry A, Pirard R et al (2005) Carbon aerogels, cryogels and xerogels: influence of the drying method on the textural properties of porous carbon materials. Carbon 43:2481–2494

    Article  Google Scholar 

  30. Haghgoo M, Yousefi AA, Mehr MJZ (2012) Nano porous structure of resorcinol–formaldehyde xerogels and aerogels: effect of sodium dodecylbenzene sulfonate. Iran Polym J 21:211–219

    Article  Google Scholar 

  31. Bordjiba T, Mohamedi M, Dao LH (2007) Synthesis and electrochemical capacitance of binderless nanocomposite electrodes formed by dispersion of carbon nanotubes and carbon aerogels. J Power Sources 172:991–998

    Article  Google Scholar 

  32. Kohlmeyer RR, Lor M, Deng J et al (2011) Preparation of stable carbon nanotube aerogels with high electrical conductivity and porosity. Carbon 49:2352–2361

    Article  Google Scholar 

  33. Sandler JKW, Kirk JE, Kinloch IA et al (2003) Ultra-low electrical percolation threshold in carbon-nanotube-epoxy composites. Polymer 44:5893–5899

    Article  Google Scholar 

  34. Celzard A, McRae E, Deleuze C et al (1996) Critical concentration in percolating systems containing a high-aspect-ratio filler. Phys Rev B 53:6209

    Article  Google Scholar 

  35. Celzard A, Marêché JF, Payot F, Furdin G (2002) Electrical conductivity of carbonaceous powders. Carbon 40:2801–2815

    Article  Google Scholar 

  36. Bryning MB, Islam MF, Kikkawa JM, Yodh AG (2005) Very low conductivity threshold in bulk isotropic single-walled carbon nanotube-epoxy composites. Adv Mater 17:1186–1191

    Article  Google Scholar 

  37. Kovacs JZ, Velagala BS, Schulte K, Bauhofer W (2007) Two percolation thresholds in carbon nanotube epoxy composites. Compos Sci Technol 67:922–928

    Article  Google Scholar 

  38. Bauhofer W, Kovacs JZ (2009) A review and analysis of electrical percolation in carbon nanotube polymer composites. Compos Sci Technol 69:1486–1498

    Article  Google Scholar 

  39. Schueler R, Petermann J, Schulte K, Wentzel H (1997) Agglomeration and electrical percolation behavior of carbon black dispersed in epoxy resin. J Appl Polym Sci 63:1741–1746

    Article  Google Scholar 

  40. Kilbride BE, Coleman JN, Fraysse J et al (2002) Experimental observation of scaling laws for alternating current and direct current conductivity in polymer-carbon nanotube composite thin films. J Appl Phys 92:4024–4030

    Article  Google Scholar 

  41. Nan C-W, Birringer R, Clarke DR, Gleiter H (1997) Effective thermal conductivity of particulate composites with interfacial thermal resistance. J Appl Phys 81:6692–6699

    Article  Google Scholar 

Download references

Acknowledgements

The first author is grateful to Ministry of Science, Research and Technology of Iran for the financial support of the present work. The authors acknowledge Prof. P. Vanderbemden (University of Liège) for allowing them to use the Measurement and Instrumentation laboratory facilities. N.J. thanks the Fonds de Recherche Fondamentale Collective (FRFC n°2.4.542.10.F) and the Fonds de Bay for their financial support.

Author information

Authors and Affiliations

  1. Plastic Processing & Engineering Department, Iran Polymer and Petrochemical Institute (IPPI), Tehran, Iran

    Majid Haghgoo, Ali Akbar Yousefi & Mohammad Jalal Zohouriaan Mehr

  2. Laboratory of Chemical Engineering – Nanomaterials, Catalysis, Electrochemistry, Institute of Chemistry (B6a), University of Liège, Sart-Tilman, 4000, Liège, Belgium

    Alexandre F. Léonard & Nathalie Job

  3. SUPRATECS and Department of Electrical Engineering and Computer Science B28, University of Liège, Sart-Tilman, 4000, Liège, Belgium

    Matthieu P. Philippe

  4. Department of Biology, Ecology and Evolution & Cell for Support of Research and Teaching in Microscopy (ULg-CAREµ), Institute of Chemistry (B6c), University of Liège, Sart-Tilman, 4000, Liège, Belgium

    Philippe Compère

  5. Laboratory of Chemical Engineering – Products, Environment and Processes, Institute of Chemistry (B6a), University of Liège, Sart-Tilman, 4000, Liège, Belgium

    Angélique Léonard

Authors
  1. Majid Haghgoo
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Ali Akbar Yousefi
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Mohammad Jalal Zohouriaan Mehr
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Alexandre F. Léonard
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Matthieu P. Philippe
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. Philippe Compère
    View author publications

    You can also search for this author in PubMed Google Scholar

  7. Angélique Léonard
    View author publications

    You can also search for this author in PubMed Google Scholar

  8. Nathalie Job
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Majid Haghgoo.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Haghgoo, M., Yousefi, A.A., Mehr, M.J.Z. et al. Correlation between morphology and electrical conductivity of dried and carbonized multi-walled carbon nanotube/resorcinol–formaldehyde xerogel composites. J Mater Sci 50, 6007–6020 (2015). https://doi.org/10.1007/s10853-015-9148-0

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10853-015-9148-0

Keywords

Search

Navigation