Skip to main content
SpringerLink
Log in

Process time variation and critical growth onset analysis for nanofoam formation in sucrose-based hydrothermal carbonization

  • Chemical routes to materials
  • Published:
Journal of Materials Science Aims and scope Submit manuscript

Abstract

The paper presents a systematic study of the formation of carbon nanofoam from sucrose by hydrothermal carbonization. It is shown that for the process temperature of 150 °C, carbonization is not a gradual process but rather occurs suddenly at a specific threshold time of 4.5 h. pH value and electrical conductivity (EC) of the sucrose solution were monitored during carbonization. In the first 4.5 h prior to carbonization, the sucrose solution shows a sharp drop from pH 7.8 to pH 2 and sharp increase of EC. From this point on the values of pH and EC remain approximately constant. After the 4.5 h threshold, we examined the evolution of mass yield, density and morphology of the resulting carbon nanofoam. The yield first shows a steep increase around 4.5 h and then a further gradual increase up to 38% at 54.6 h. The mass density just after the 4.5 h threshold is 0.28 g/cm3 and decreases with process time to reach a constant value of 0.14 g/cm3, between 20 and 54.6 h. This shows that desired conditions, such as low density and high yield, are obtained with sufficient process time below 5 h. Due to the release of intermediates of the conversion reaction into the sucrose solution, both pH and EC were found to be excellent indicators for the progression of hydrothermal carbonization.

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

Figure 1
Figure 2
Figure 3
Figure 4
Figure 5
Figure 6

Similar content being viewed by others

References

  1. Sattler KD (ed) (2020). 21st century nanoscience – a handbook: low-dimensional materials and morphologies (volume four), 1st edn. CRC Press, Boca Raton

    Google Scholar 

  2. Sattler KD (ed) (2016). Carbon nanomaterials sourcebook, two-volume set, 1st edn. CRC Press, Boca Raton

    Google Scholar 

  3. Wortmann M et al (2020). Chemical and morphological transition of poly(acrylonitrile)/poly(vinylidene fluoride) blend nanofibers during oxidative stabilization and incipient carbonization. Nanomaterials 10(6):1210

    CAS  Google Scholar 

  4. Liu C et al (2017). Facile synthesis of nickel nanofoam architectures for applications in li-ion batteries. Energ Technol 5(3):422–427

    CAS  Google Scholar 

  5. Iwu KO et al (2016). Facile synthesis of Ni nanofoam for flexible and low-cost non-enzymatic glucose sensing. Sens Actuators B-Chem 224:764–771

    CAS  Google Scholar 

  6. Lacerda JN et al (2020). Manganese oxide nanofoam prepared by pulsed laser deposition for high performance supercapacitor electrodes. Mater Chem Phys 242:122459

    CAS  Google Scholar 

  7. Iino T, Nakamura K (2009). Acoustic and acousto-optic characteristics of silicon nanofoam. Jpn J Appl Phys 48(7):07GE01

    Google Scholar 

  8. Jia H et al (2015). Deep eutectic solvent-assisted growth of gold nanofoams and their excellent catalytic properties. J Mol Liq 212:763–766

    CAS  Google Scholar 

  9. Dutta A et al (2018). Beyond copper in co2 electrolysis: effective hydrocarbon production on silver-nanofoam catalysts. ACS Catal 8(9):8357–8368

    CAS  Google Scholar 

  10. Lamaison S et al (2019). Zn-Cu alloy nanofoams as efficient catalysts for the reduction of co2 to syngas mixtures with a potential-independent h-2/co ratio. Chemsuschem 12(2):511–517

    CAS  Google Scholar 

  11. Jo H et al (2014). Novel method of powder-based processing of copper nanofoams for their potential use in energy applications. Mater Chem Phys 145(1–2):6–11

    CAS  Google Scholar 

  12. Vukovic I et al (2011). Supramolecular route to well-ordered metal nanofoams. ACS Nano 5(8):6339–6348

    CAS  Google Scholar 

  13. Bartunek V et al (2017). Facile synthesis of magnetic Co nanofoam by low-temperature thermal decomposition of Co glycerolate. Micro Nano Lett 12(5):278–280

    CAS  Google Scholar 

  14. Grant-Jacob JA, Mills B, Eason RW (2014). Parametric study of the rapid fabrication of glass nanofoam via femtosecond laser irradiation. J Phys D-Appl Phys 47(5):055105

    CAS  Google Scholar 

  15. Manzo DJ et al (2019). Structural and compositional analysis of GaSb nanofoams obtained by ion irradiation of sputtered films. Thin Solid Films 687:137447

    CAS  Google Scholar 

  16. Levesque A et al (2004). Monodisperse carbon nanopearls in a foam-like arrangement: a new carbon nano-compound for cold cathodes. Thin Solid Films 464:308–314

    Google Scholar 

  17. Sattler KD (ed) (2016). Carbon nanomaterials sourcebook: graphene, fullerenes, nanotubes, and nanodiamonds (volume one), 1st edn. CRC Press, Boca Raton

    Google Scholar 

  18. Sattler KD (ed) (2016). Carbon nanomaterials sourcebook: nanoparticles, nanocapsules, nanofibers, nanoporous structures, and nanocomposites (volume two), 1st edn. CRC Press, Boca Raton

    Google Scholar 

  19. Tekin K, Karagoz S, Bektas S (2014). A review of hydrothermal biomass processing. Renew Sustain Energy Rev 40:673–687

    CAS  Google Scholar 

  20. Funke A, Ziegler F (2010). Hydrothermal carbonization of biomass: A summary and discussion of chemical mechanisms for process engineering. Biofuels Bioprod Bioref-Biofpr 4(2):160–177

    CAS  Google Scholar 

  21. Hu B et al (2010). Engineering carbon materials from the hydrothermal carbonization process of biomass. Adv Mater 22(7):813–828

    CAS  Google Scholar 

  22. Titirici MM et al (2007). A direct synthesis of mesoporous carbons with bicontinuous pore morphology from crude plant material by hydrothermal carbonization. Chem Mater 19(17):4205–4212

    CAS  Google Scholar 

  23. Khan TA et al (2019). Synthesis and characterization of carbon microspheres from rubber wood by hydrothermal carbonization. J Chem Technol Biotechnol 94(5):1374–1383

    Google Scholar 

  24. Fuertes AB et al (2010). Chemical and structural properties of carbonaceous products obtained by pyrolysis and hydrothermal carbonisation of corn stover. Aust J Soil Res 48(6–7):618–626

    CAS  Google Scholar 

  25. Gupta A, Kour R, Brar LK (2019). Facile synthesis of carbon nanospheres from saccharides for photocatalytic applications. Sn Appl Sci 1(10):1–8

    CAS  Google Scholar 

  26. Sevilla M, Fuertes AB (2009). Chemical and structural properties of carbonaceous products obtained by hydrothermal carbonization of saccharides. Chemi-a Eur J 15(16):4195–4203

    CAS  Google Scholar 

  27. Frese N et al (2017). Diamond-like carbon nanofoam from low-temperature hydrothermal carbonization of a sucrose/naphtalene precurson solution. J Carbon Res 3:23

    Google Scholar 

  28. Mi YZ et al (2008). Synthesis of carbon micro-spheres by a glucose hydrothermal method. Mater Lett 62(8–9):1194–1196

    CAS  Google Scholar 

  29. Sevilla M, Fuertes AB (2009). The production of carbon materials by hydrothermal carbonization of cellulose. Carbon 47(9):2281–2289

    CAS  Google Scholar 

  30. Cheng YL et al (2017). Controllable morphologies of carbon microspheres via green hydrothermal method using fructose and xylose. Chem Lett 46(9):1400–1402

    CAS  Google Scholar 

  31. Lagazzo A et al (2016). Hydrothermal synthesis of pectin derived nanoporous carbon material. Mater Lett 171:212–215

    CAS  Google Scholar 

  32. Mitchell ST et al (2015). Ultralight carbon nanofoam from naphtalene-mediated hydrothermal sucrose carbonization. Carbon 95:434–441

    CAS  Google Scholar 

  33. Zhao HY et al (2017). Effects of additives on sucrose-derived activated carbon microspheres synthesized by hydrothermal carbonization. J Mater Sci 52(18):10787–10799. https://doi.org/10.1007/s10853-017-1258-4

    Article  CAS  Google Scholar 

  34. Chen JZ et al (2012). Calcium-assisted hydrothermal carbonization of an alginate for the production of carbon microspheres with unique surface nanopores. Mater Lett 67(1):365–368. https://doi.org/10.1016/j.matlet.2011.10.017

    Article  CAS  Google Scholar 

  35. Wortmann M et al (2020). On the reliability of highly magnified micrographs for structural analysis in materials science. Sci Rep 10(1):1–8

    Google Scholar 

  36. Smith M et al (2016). Improving the deconvolution and interpretation of XPS spectra from chars by ab initio calculations. Carbon 110:155–171

    CAS  Google Scholar 

  37. Baccile N et al (2009). Structural characterization of hydrothermal carbon spheres by advanced solid-state mas c-13 nmr investigations. J Phys Chem C 113(22):9644–9654

    CAS  Google Scholar 

  38. Lide DR (2005). CRC handbook of chemistry and physics, 86th edn. CRC (FL) Press, Baco Raton

    Google Scholar 

  39. Hao SW et al (2016). Activated carbon derived from hydrothermal treatment of sucrose and its air filtration application. RSC Adv 6(111):109950–109959

    CAS  Google Scholar 

  40. Qi YJ et al (2016). Mechanism for the formation and growth of carbonaceous spheres from sucrose by hydrothermal carbonization. RSC Adv 6(25):20814–20823

    CAS  Google Scholar 

  41. Wang Q et al (2001). Monodispersed hard carbon spherules with uniform nanopores. Carbon 39(14):2211–2214

    CAS  Google Scholar 

  42. Simsir H, Eltugral N, Karagoz S (2017). Hydrothermal carbonization for the preparation of hydrochars from glucose, cellulose, chitin, chitosan and wood chips via low-temperature and their characterization. Biores Technol 246:82–87

    CAS  Google Scholar 

  43. Frese N et al (2016). Fundamental properties of high-quality carbon nanofoam: from low to high density. Beilstein J Nanotechnol 7:2065–2073

    CAS  Google Scholar 

  44. Nizamuddin S et al (2017). An overview of effect of process parameters on hydrothermal carbonization of biomass. Renew Sustain Energy Rev 73:1289–1299

    CAS  Google Scholar 

Download references

Author information

Authors and Affiliations

  1. Department of Physics and Astronomy, University of Hawaii, Watanabe Hall, 2505 Correa Road, Honolulu, HI, 96822, USA

    Carrie Brooks, Julia Lee, Natalie Frese & Klaus Sattler

  2. Faculty of Physics, Bielefeld University, Universitätsstraße 25, 33615, Bielefeld, Germany

    Natalie Frese & Martin Wortmann

  3. Hawaii Institute of Geophysics and Planetology, School of Ocean and Earth Science and Technology (SOEST), University of Hawaii At Manoa, 1680 East-West Road, Honolulu, HI, 96822, USA

    Kenta Ohtaki

Authors
  1. Carrie Brooks
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Julia Lee
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Natalie Frese
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Kenta Ohtaki
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Martin Wortmann
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. Klaus Sattler
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Klaus Sattler.

Ethics declarations

Conflicts of interest

The authors did not receive support from any organization for the submitted work. No funding was received to assist with the preparation of this manuscript. No funding was received for conducting this study. No funds, grants, or other support was received.

Additional information

Handling Editor: Gregory Rutledge.

Publisher's Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Brooks, C., Lee, J., Frese, N. et al. Process time variation and critical growth onset analysis for nanofoam formation in sucrose-based hydrothermal carbonization. J Mater Sci 56, 15004–15011 (2021). https://doi.org/10.1007/s10853-021-06222-4

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10853-021-06222-4

Search

Navigation