Skip to main content
SpringerLink
Log in

Preparation and characterization of a nitrogen-doped mesoporous carbon aerogel and its polymer precursor

  • Published:
Journal of Thermal Analysis and Calorimetry Aims and scope Submit manuscript

Abstract

Nitrogen-containing carbon aerogel was prepared from resorcinol–melamine–formaldehyde (R–M–F) polymer gel precursor. The polymer gel was supercritically dried with CO2, and the carbonization of the resulting polymer aerogel under nitrogen atmosphere at 900 °C yielded the carbon aerogel. The polymer and carbon aerogels were characterized with TG/DTA–MS, low-temperature nitrogen adsorption/desorption (− 196 °C), FTIR, Raman, powder XRD and SEM–EDX techniques. The thermal decomposition of the polymer aerogel had two major steps. The first step was at 150 °C, where the unreacted monomers and the residual solvent were released, and the second one at 300 °C, where the species belonging to the polymer network decomposition could be detected. The pyrolytic conversion of the polymer aerogel was successful, as 0.89 at.% nitrogen was retained in the carbon matrix. The nitrogen-doped carbon aerogel was amorphous and possessed a hierarchical porous structure. It had a significant specific surface area (890 m2 g−1) and pore volume (4.7 cm3 g−1). TG/DTA–MS measurement revealed that during storage in ambient conditions surface functional groups formed, which were released upon annealing.

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
Fig. 9

Similar content being viewed by others

References

  1. Hu P, Tan B, Long M. Advanced nanoarchitectures of carbon aerogels for multifunctional environmental applications. Nanotechnol. Rev. 2016;5:23–39.

    Article  Google Scholar 

  2. Moreno-Castilla C, Maldonado-Hódar FJ. Carbon aerogels for catalysis applications: an overview. Carbon. 2005;43:455–65.

    Article  CAS  Google Scholar 

  3. Veselá P, Slovák V. Organic xerogels based on condensation of different m-substituted phenols with formaldehyde: Preparation and TG-MS study. J Therm Anal Calorim. 2014;116:663–9.

    Article  Google Scholar 

  4. Jin M, Luo N, Li G, Luo Y. The thermal decomposition mechanism of nitrocellulose aerogel. J Therm Anal Calorim. 2015;121:901–8.

    Article  CAS  Google Scholar 

  5. Horvat G, Fajfar T, Perva Uzunalić A, Knez Ž, Novak Z. Thermal properties of polysaccharide aerogels. J Therm Anal Calorim. 2017;127:363–70.

    Article  CAS  Google Scholar 

  6. Schwan M, Ratke L. Flexible carbon aerogels. C. 2016;2:22.

    Google Scholar 

  7. Nagy B, Villar-Rodil S, Tascón JMD, Bakos I, László K. Nitrogen doped mesoporous carbon aerogels and implications for electrocatalytic oxygen reduction reactions. Microporous Mesoporous Mater. 2016;230:135–44.

    Article  CAS  Google Scholar 

  8. Tian HY, Buckley CE, Wang SB, Zhou MF. Enhanced hydrogen storage capacity in carbon aerogels treated with KOH. Carbon. 2009;47:2128–30.

    Article  CAS  Google Scholar 

  9. Wang X, Liu L, Wang X, Bai L, Wu H, Zhang X, et al. Preparation and performances of carbon aerogel microspheres for the application of supercapacitor. J Solid State Electrochem. 2011;15:643–8.

    Article  CAS  Google Scholar 

  10. Zhang S, Gross AF, Van Atta SL, Lopez M, Liu P, Ahn CC, et al. The synthesis and hydrogen storage properties of a MgH2 incorporated carbon aerogel scaffold. Nanotechnology, vol. 20. Bristol: IOP Publishing; 2009. p. 204027.

    Google Scholar 

  11. Pekala RW, Farmer JC, Alviso CT, Tran TD, Mayer ST, Miller JM, et al. Carbon aerogels for electrochemical applications. J Non Cryst Solids. 1998;225:74–80.

    Article  CAS  Google Scholar 

  12. Wang Y, Chang B, Guan D, Dong X. Mesoporous activated carbon spheres derived from resorcinol-formaldehyde resin with high performance for supercapacitors. J Solid State Electrochem. 2015;19:1783–91.

    Article  CAS  Google Scholar 

  13. Tsujimura S, Kamitaka Y, Kano K. Diffusion-controlled oxygen reduction on multi-copper oxidase-adsorbed carbon aerogel electrodes without mediator. Fuel Cells. 2007;7:463–9.

    Article  CAS  Google Scholar 

  14. Pekala RW. Organic aerogels from the polycondensation of resorcinol with formaldehyde. J Mater Sci. 1989;24:3221–7.

    Article  CAS  Google Scholar 

  15. Jin Y, Wu M, Zhao G, Li M. Photocatalysis-enhanced electrosorption process for degradation of high-concentration dye wastewater on TiO2/carbon aerogel. Chem Eng J. 2011;168:1248–55.

    Article  CAS  Google Scholar 

  16. Geng D, Chen YY, Chen YY, Li Y, Li R, Sun X, et al. High oxygen-reduction activity and durability of nitrogen-doped graphene. Energy Environ Sci. 2011;4:760.

    Article  CAS  Google Scholar 

  17. Long D, Zhang J, Yang J, Hu Z, Cheng G, Liu X, et al. Chemical state of nitrogen in carbon aerogels issued from phenol-melamine-formaldehyde gels. Carbon. 2008;46:1259–62.

    Article  CAS  Google Scholar 

  18. Rasines G, Lavela P, Macías C, Zafra MC, Tirado JL, Parra JB, et al. N-doped monolithic carbon aerogel electrodes with optimized features for the electrosorption of ions. Carbon. 2015;83:262–74.

    Article  CAS  Google Scholar 

  19. Veselá P, Slovák V. Pyrolysis of N-doped organic aerogels with relation to sorption properties. J Therm Anal Calorim. 2012;108:475–80.

    Article  Google Scholar 

  20. Liu X, Li S, Mei J, Lau W-M, Mi R, Li Y, et al. From melamine–resorcinol–formaldehyde to nitrogen-doped carbon xerogels with micro-and meso-pores for lithium batteries. J Mater Chem A. 2014;2:14429–38.

    Article  CAS  Google Scholar 

  21. Jin H, Zhang H, Zhong H, Zhang J, Mukundan R, Garland N, et al. Nitrogen-doped carbon xerogel: a novel carbon-based electrocatalyst for oxygen reduction reaction in proton exchange membrane (PEM) fuel cells. Energy Environ Sci R Soc Chem. 2011;4:3389.

    Article  CAS  Google Scholar 

  22. Nagy B, Villar-Rodil S, Tascón JMD, Bakos I, László K. Nitrogen doped mesoporous carbon aerogels and implications for electrocatalytic oxygen reduction reactions. Microporous Mesoporous Mater. 2016;230:135–44.

    Article  CAS  Google Scholar 

  23. Veselá P, Slovák V. Monitoring of N-doped organic xerogels pyrolysis by TG-MS. J Therm Anal Calorim. 2013;113:209–17.

    Article  Google Scholar 

  24. Brunauer S, Emmett PH, Teller E. Adsorption of gases in multimolecular layers. J Am Chem Soc. 1938;60:309–19.

    Article  CAS  Google Scholar 

  25. Dubinin MM, Radushkevich LV. The equation of the characteristic curve of activated charcoal. Dokl Akad Nauk SSSR. 1947;55:327–9.

    CAS  Google Scholar 

  26. Françoise Rouquerol GMJRKSWS. Adsorption by powders and porous solids, second edition: principles, methodology and applications [Internet]. Acad. Press. 1999 [cited 2017 May 22]. p. 647. Available from: https://books.google.hu/books?hl=en&lr=&id=UOE-ZscCYncC&oi=fnd&pg=PP1&dq=Adsorption+by+Powders+and+Porous+Solids&ots=0R1XIBpnix&sig=KX9hHmrIFZSewWz4wsxWBDusDsg&redir_esc=y#v=onepage&q=Adsorption by Powders and Porous Solids&f = false.

  27. Al-Muhtaseb SA, Ritter JA. Preparation and properties of resorcinol-formaldehyde organic and carbon gels. Adv Mater. 2003;15:101–14.

    Article  CAS  Google Scholar 

  28. Kim S, Kim HJ. Effect of addition of polyvinyl acetate to melamine-formaldehyde resin on the adhesion and formaldehyde emission in engineered flooring. Int J Adhes Adhes. 2005;25:456–61.

    Article  CAS  Google Scholar 

  29. Ullah S, Bustam MA, Nadeem M, Naz MY, Tan WL, Shariff AM. Synthesis and thermal degradation studies of melamine formaldehyde resins. Sci World J. 2014;19:225.

    Google Scholar 

  30. Macias C, Rasines G, García T, Zafra M, Lavela P, Tirado J, et al. Synthesis of porous and mechanically compliant carbon aerogels using conductive and structural additives. Gels. 2016;2:4.

    Article  Google Scholar 

  31. Zhou HH, Xu S, Su HP, Wang M, Qiao WM, Ling LC, et al. Facile preparation and ultra-microporous structure of melamine-resorcinol-formaldehyde polymeric microspheres. Chem Commun. 2013;49:3763–5.

    Article  CAS  Google Scholar 

Download references

Acknowledgements

I. M. Szilágyi thanks for a János Bolyai Research Fellowship of the Hungarian Academy of Sciences and an ÚNKP-17-4-IV-BME-188 grant supported by the ÚNKP-17-4-IV New National Excellence Program of the Ministry of Human Capacities, Hungary. The research within Project No. VEKOP-2.3.2-16-2017-00013 was supported by the European Union and the State of Hungary, co-financed by the European Regional Development Fund. An OTKA 109558 grant, an NRDI K 124212 grant and an NRDI TNN_16 123631 grant are acknowledged. The authors are grateful to Mr. György Bosznai for the technical assistance.

Author information

Authors and Affiliations

  1. Department of Inorganic and Analytical Chemistry, Budapest University of Technology and Economics, Szent Gellért tér 4, Budapest, 1111, Hungary

    László Péter Bakos, Joshua Mensah & Imre Miklós Szilágyi

  2. Department of Physical Chemistry and Materials Science, Budapest University of Technology and Economics, Budafoki út 8. F. I. building, Budapest, 1111, Hungary

    Krisztina László

  3. Department of Organic Chemistry and Technology, Budapest University of Technology and Economics, Budafoki út 8. F. II. building, Budapest, 1111, Hungary

    Tamás Igricz

Authors
  1. László Péter Bakos
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Joshua Mensah
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Krisztina László
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Tamás Igricz
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Imre Miklós Szilágyi
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to László Péter Bakos.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Bakos, L.P., Mensah, J., László, K. et al. Preparation and characterization of a nitrogen-doped mesoporous carbon aerogel and its polymer precursor. J Therm Anal Calorim 134, 933–939 (2018). https://doi.org/10.1007/s10973-018-7318-4

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10973-018-7318-4

Keywords

Search

Navigation