Synthesis of multi-walled carbon nanotubes from natural precursors via modified pyrolytic nebulization

Authors

  • Isis Alejandra Hernandez Rivera Tecnológico Nacional de México/Instituto Tecnológico de Tijuana, Posgrado en Ciencias de la Ingeniería, Blvd. Industrial s/n col. Mesa de Otay, 22500, Tijuana, Baja California, México. https://orcid.org/0009-0006-8733-619X
    Competing Interests

    No conflict of interest declared.

  • Rocío Alejandra Cera García Tecnológico Nacional de México/Instituto Tecnológico de Tijuana, Departamento de Química y Bioquímica, Calz. del Tecnológico 12950. Tomas Aquino, 22414, Tijuana Baja California, México https://orcid.org/0009-0003-5653-2743
    Competing Interests

    No conflict of interest declared.

  • Victor Raúl López López Tecnológico Nacional de México/Instituto Tecnológico de Tijuana, Departamento de Ingeniería Aeronáutica, Calz. del Tecnológico 12950. Tomas Aquino, 22414, Tijuana, Baja California,, México. https://orcid.org/0000-0001-9145-7871
    Competing Interests

    No conflict of interest declared.

  • Luis Ernesto Solís Delgado Tecnológico Nacional de México/Instituto Tecnológico de Tijuana, Departamento de Química y Bioquímica, Calz. del Tecnológico 12950. Tomas Aquino, 22414, Tijuana, Baja California, México https://orcid.org/0000-0002-1489-7379
    Competing Interests

    No conflict of interest declared.

  • Balter Trujillo Navarrete Tecnológico Nacional de México/Instituto Tecnológico de Tijuana, Posgrado en Ciencias de la Ingeniería, Blvd. Industrial s/n col. Mesa de Otay, 22500, Tijuana, Baja California, México https://orcid.org/0000-0002-0196-1001
    Competing Interests

    No conflict of interest declared.

  • Francisco Paraguay Delgado Centro de Investigación en Materiales Avanzados, S. C. Av. Miguel de Cervantes Saavedra 120. Complejo industrial Chihuahua, 31136, Chihuahua, Chihuahua, México. https://orcid.org/0000-0002-3764-1595
    Competing Interests

    No conflict of interest declared.

  • Yadira Gochi Ponce Tecnológico Nacional de México/Instituto Tecnológico de Tijuana, Posgrado en Ciencias de la Ingeniería, Blvd. Industrial s/n col. Mesa de Otay, 22500, Tijuana, Baja California, México. https://orcid.org/0000-0002-1590-2432
    Competing Interests

    No conflict of interest declared.

DOI:

https://doi.org/10.37636/recit.v9n3e488

Keywords:

Green synthesis, Multi-walled carbon nanotubes, Natural precursors, Modified pyrolytic nebulization

Abstract

This study investigates the implementation of a green synthesis approach based on a modified spray pyrolysis method, aimed at developing a more environmentally sustainable process through the replacement of conventional hydrocarbon-derived precursors with naturally occurring compounds extracted from plant essential oils. Three different renewable precursor sources were selected, obtained by steam distillation and subsequently purified through rotary evaporation using dichloromethane as the extraction solvent. Four samples of multi-walled carbon nanotubes (MWCNTs), designated as RON, CLN, CNN, and CNT, were synthesized. The CNT sample was produced using a conventional commercial organic precursor and served as the reference material. All samples were synthesized under identical experimental conditions, including reaction temperature, carrier gas, gas flow rate, pressure, solution feed rate, reaction time, and substrate type. A comparative study was conducted to evaluate the properties of the synthesized MWCNTs. The nanomaterials were characterized using thermogravimetric analysis (TGA), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Raman spectroscopy. These characterization techniques were employed to assess their morphological, thermal, structural, and chemical stability properties. The results confirmed the successful formation of MWCNTs from all natural precursors (RON, CLN, and CNN). The synthesized materials exhibited distinct morphologies and varying production yields. In general, the MWCNTs derived from essential oils displayed a lower degree of crystallinity compared to the CNT sample synthesized from toluene. Nevertheless, their structural and thermal characteristics demonstrate that essential oils constitute viable and sustainable alternative carbon sources for the production of carbon nanotubes through modified spray pyrolysis. This work presents an experimental and comparative investigation focused on the synthesis of MWCNTs from three different natural precursors and the evaluation of their morphological, thermal, and structural properties relative to nanotubes produced from a conventional hydrocarbon precursor. Biocompatibility assessments were beyond the scope of the present study and were therefore not considered.

Downloads

Download data is not yet available.

References

[1] S. Iijima, “Helical microtubules of graphitic carbon,” Nature, vol. 354, pp. 56–58, 1991, doi: 10.1038/354056a0. DOI: https://doi.org/10.1038/354056a0

[2] P. Kesharwani, V. Mishra, and N. K. Jain, “Validating the anticancer potential of carbon nanotube-based therapeutics through cell line testing,” Drug Discovery Today, vol. 20, pp. 1049–1060, 2015, doi: 10.1016/j.drudis.2015.05.004. DOI: https://doi.org/10.1016/j.drudis.2015.05.004

[3] M. A. Saleemi, M. H. Fouladi, P. V. C. Yong, K. Chinna, N. K. Palanisamy, and E. H. Wong, “Toxicity of carbon nanotubes: Molecular mechanisms, signaling cascades, and remedies in biomedical applications,” Chem. Res. Toxicol., vol. 34, pp. 24–46, 2021, doi: 10.1021/acs.chemrestox.0c00172. DOI: https://doi.org/10.1021/acs.chemrestox.0c00172

[4] G. T. T. Le, P. Mala, S. Ratchahat, and T. Charinpanitkul, “Bio-based production of carbon nanotubes via co-pyrolysis of eucalyptus oil and ferrocene,” J. Anal. Appl. Pyrolysis, vol. 158, Art. no. 105257, 2021, doi: 10.1016/j.jaap.2021.105257. DOI: https://doi.org/10.1016/j.jaap.2021.105257

[5] E. T. Thostenson, Z. Ren, and T.-W. Chou, “Advances in the science and technology of carbon nanotubes and their composites: A review,” Compos. Sci. Technol., vol. 61, pp. 1899–1912, 2001, doi: 10.1016/S0266-3538(01)00094-X. DOI: https://doi.org/10.1016/S0266-3538(01)00094-X

[6] R. Kumar, R. S. Tiwari, and O. N. Srivastava, “Scalable synthesis of aligned carbon nanotube bundles using neem oil,” Nanoscale Res. Lett., vol. 6, pp. 2–7, 2011, doi: 10.1186/1556-276X-6-92. DOI: https://doi.org/10.1186/1556-276X-6-92

[7] R. Kumar, R. K. Singh, and D. P. Singh, “Natural and waste hydrocarbon precursors for the synthesis of carbon-based nanomaterials,” Renew. Sustain. Energy Rev., vol. 58, pp. 976–1006, 2016, doi: 10.1016/j.rser.2015.12.120. DOI: https://doi.org/10.1016/j.rser.2015.12.120

[8] M. E. Guerrero-Llamas, L. E. Solís-Delgado, L. J. Villarreal-Gómez, E. Méndez-Valenzuela, and Y. Gochi-Ponce, “Evaluación in vitro de nanomateriales de carbono para aplicaciones biotecnológicas,” Pädi, vol. 14, pp. 318–323, 2026, doi: 10.29057/icbi.v14iEspecial.15389. DOI: https://doi.org/10.29057/icbi.v14iEspecial.15389

[9] Z. H. Abdel, A. Abdul, F. Abdel, and S. S. Abdel Rehim, “Challenges on synthesis of carbon nanotubes from green oil using pyrolysis technique,” J. Anal. Appl. Pyrolysis, vol. 126, pp. 218–229, 2017, doi: 10.1016/j.jaap.2017.06.005. DOI: https://doi.org/10.1016/j.jaap.2017.06.005

[10] R. Sen, A. Govindaraj, and C. N. R. Rao, “Carbon nanotubes by the metallocene route,” Chem. Phys. Lett., vol. 267, pp. 276–280, 1998, doi: 10.1016/S0009-2614(97)00080-8. DOI: https://doi.org/10.1016/S0009-2614(97)00080-8

[11] M. J. Bronikowski, “CVD growth of carbon nanotube bundle arrays,” Carbon, vol. 44, pp. 2822–2832, 2006, doi: 10.1016/j.carbon.2006.03.022. DOI: https://doi.org/10.1016/j.carbon.2006.03.022

[12] K. Awasthi, R. Kumar, R. S. Tiwari, and O. N. Srivastava, “Large-scale synthesis of aligned carbon nanotubes using turpentine oil,” J. Exp. Nanosci., vol. 5, pp. 498–508, 2010, doi: 10.1080/17458081003664159. DOI: https://doi.org/10.1080/17458081003664159

[13] P. Ghosh, T. Soga, K. Ghosh, R. A. Afre, T. Jimbo, and Y. Ando, “Vertically aligned N-doped carbon nanotubes by spray pyrolysis,” J. Non-Cryst. Solids, vol. 354, pp. 4101–4106, 2008, doi: 10.1016/j.jnoncrysol.2008.05.053. DOI: https://doi.org/10.1016/j.jnoncrysol.2008.05.053

[14] P. Ghosh, R. A. Afre, T. Soga, and T. Jimbo, “Production of single-walled carbon nanotubes from eucalyptus oil,” Mater. Lett., vol. 61, pp. 3768–3770, 2007, doi: 10.1016/j.matlet.2006.12.030. DOI: https://doi.org/10.1016/j.matlet.2006.12.030

[15] R. Kumar, R. K. Singh, and R. S. Tiwari, “High-yield synthesis of nitrogen-doped carbon nanotubes using sesame oil,” Mater. Des., vol. 94, pp. 166–175, 2016, doi: 10.1016/j.matdes.2016.01.025. DOI: https://doi.org/10.1016/j.matdes.2016.01.025

[16] G. Late, B. Vishwanathan, S. Bhowmik, and M. Sharon, “Natural precursors for synthesis of carbon nanomaterials by CVD: A review,” Int. J. Sci. Res., vol. 7, pp. 2319–7064, 2016, doi: 10.21275/ART2018338.

[17] M. S. Azmina, A. B. Suriani, M. Salina et al., “Bio-hydrocarbon precursors for synthesis of carbon nanotubes,” Nano Hybrids, vol. 2, pp. 43–63, 2012, doi: 10.4028/www.scientific.net/NH.2.43. DOI: https://doi.org/10.4028/www.scientific.net/NH.2.43

[18] S. Paul and S. K. Samdarshi, “A green precursor for carbon nanotube synthesis,” New Carbon Mater., vol. 26, pp. 85–88, 2011, doi: 10.1016/S1872-5805(11)60068-1. DOI: https://doi.org/10.1016/S1872-5805(11)60068-1

[19] Y. Jiang, N. Wu, Y.-J. Fu et al., “Chemical composition and antimicrobial activity of rosemary essential oil,” Environ. Toxicol. Pharmacol., vol. 32, pp. 63–68, 2011, doi: 10.1016/j.etap.2011.03.011. DOI: https://doi.org/10.1016/j.etap.2011.03.011

[20] S. Nazirah, A. A. Azira, and M. Rusop, “Synthesis of carbon nanotubes from camphor oil,” Adv. Mater. Res., vol. 667, pp. 421–424, 2013, doi: 10.4028/www.scientific.net/AMR.667.421. DOI: https://doi.org/10.4028/www.scientific.net/AMR.667.421

[21] M. Kumar and Y. Ando, “Production of aligned carbon nanotubes from camphor,” Chem. Phys. Lett., vol. 374, pp. 521–526, 2003, doi: 10.1016/S0009-2614(03)00742-5. DOI: https://doi.org/10.1016/S0009-2614(03)00742-5

[22] J. Flores-Valdez, W. Villastrigo-López, A. Castañeda-Facio, C. López-Badillo, S. Esparza-González, P. Acuña-Vázquez y A. Sáenz-Galindo, “Funcionalización verde de nanotubos de carbono de pared múltiple con extracto de romero,” Revista Colombiana de Química, vol. 55,

pp. 3–8, 2026, doi: 10.15446/rev.colomb.quim.v55n1.119894. DOI: https://doi.org/10.15446/rev.colomb.quim.v55n1.119894

[23] G. P. Amaral et al., “Protective action of ethanolic extract of Rosmarinus officinalis L. in gastric ulcer prevention induced by ethanol in rats,” Food Chem. Toxicol., vol. 55, pp. 48–55, 2013, doi: 10.1016/j.fct.2012.12.038. DOI: https://doi.org/10.1016/j.fct.2012.12.038

[24] N. Mahato, M. Sinha, K. Sharma et al., “Extraction and purification of bioactive compounds from citrus wastes,” Foods, vol. 8, Art. no. 523, 2019, doi: 10.3390/foods8110523. DOI: https://doi.org/10.3390/foods8110523

[25] P. Agarwal, Z. Sebghatollahi, M. Kamal et al., “Citrus essential oils in aromatherapy,” Antioxidants, vol. 11, Art. no. 2374, 2022, doi: 10.3390/antiox11122374. DOI: https://doi.org/10.3390/antiox11122374

[26] M. Kačániová, N. Čmiková, N. L. Vukovic et al., “Citrus limon essential oil: Composition and biological properties,” Plants, vol. 13, Art. no. 524, 2024, doi: 10.3390/plants13040524. DOI: https://doi.org/10.3390/plants13040524

[27] J. A. Paz-González, Y. Gochi-Ponce, C. Velasco-Santos et al., “Enhancing PLA/carbon fiber composites with MWCNT fillers,” J. Compos. Sci., vol. 9, Art. no. 167, 2025, doi: 10.3390/jcs9040167. DOI: https://doi.org/10.3390/jcs9040167

(A) TEM micrographs of MWCNTs from batch RON, showing the number of layers and the visible outer and inner diameters, and (B) TEM micrograph of MWCNTs from batch CNT, showing the number of layers and the visible outer and inner diameters.

Published

2026-08-27

Data Availability Statement

I, Isis Alejandra Hernández, declare that I am making my data as a researcher available to the public.

How to Cite

Hernandez Rivera, I. A., Cera García, R. A., López López, V. R., Solís Delgado, L. E., Trujillo Navarrete, B., Paraguay Delgado, F., & Gochi Ponce, Y. (2026). Synthesis of multi-walled carbon nanotubes from natural precursors via modified pyrolytic nebulization. Revista De Ciencias Tecnológicas, 9(3), 1-18. https://doi.org/10.37636/recit.v9n3e488

Similar Articles

31-38 of 38

You may also start an advanced similarity search for this article.

Most read articles by the same author(s)