Controlled Syntheses of Multi-walled Carbon Nanotubes from Bimetallic Fe–Co Catalyst Supported on Kaolin by Chemical Vapour Deposition Method

  • A. Oyewemi
  • A. S. Abdulkareem
  • J. O. TijaniEmail author
  • M. T. Bankole
  • O. K. Abubakre
  • A. S. Afolabi
  • W. D. Roos
Research Article - Chemical Engineering


Multi-walled carbon nanotubes (MWCNTs) were synthesized via acetylene gas deposition over bimetallic Fe–Co/kaolin catalyst by chemical vapour deposition method. The effects of synthesis parameters such as calcination temperatures, reaction time, argon and acetylene flow rates on the CNTs yield were examined using \(2^{4}\) full factorial experimental design. The as-prepared nanomaterials were characterized by HRSEM/EDS, HRTEM, TGA, DLS, XRD, XPS and BET. The HRSEM/TGA revealed well dispersion of the metallic particles on the kaolin support with high thermal stability. XRD analysis of the catalyst confirmed the formation of mixed oxides of different intensities which can favour the growth of MWCNTs. The optimum conditions to obtain high catalyst yield of 88.9% were: mixing ratio of 1.6, stirring speed 1000 rpm, calcination temperature \(500\,{^{\circ }}\hbox {C}\) and calcination time 14 h. The HRSEM, HRTEM and XRD analyses showed that optimal controlled conditions to obtain homogeneous growth of high-quality graphitic MWCNTs of different inner and outer diameters were: reaction temperature of \(700\,{^{\circ }}\hbox {C}\), growing time 55 min, argon flow rate 220 mL/min and acetylene flow rate 180 mL/min. The BET analysis showed that the surface area of unpurified MWCNTs was \(275.5~\hbox {m}^{2}/\hbox {g}\) while pure MWCNTs increased to \(330.6~\hbox {m}^{2}/\hbox {g}\) after acid treatment. The statistical analysis showed that deposition temperature and acetylene flow rate positively exerted significant influence on the CNTs yield than other synthesis parameters, an evidence of thermodynamic-controlled mechanism. This study demonstrated that kaolin can act as an excellent substrate for MWCNTs growth compared to other commercial supports such as \(\hbox {CaCO}_{3}\), MgO, \(\hbox {Al}_{2}\hbox {O}_{3}\), \(\hbox {SiO}_{2}\).


Bimetallic Fe–Co catalyst Kaolin Multi-walled carbon nanotubes Catalytic chemical vapour deposition Factorial design 


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The authors acknowledged the financial support received from Tertiary Education Trust Fund (TETFund), Nigeria, under a grant number TETFUND/FUTMINNA/2014/025 and Centre for Genetic Engineering and Biotechnology (CGEB), Federal University of Technology, Minna, Nigeria, for allowing the students to conduct the experiment and also use the FTIR, Nano zetasizer and BET facilities. The authors are grateful to the following people for their technical assistance: Dr Remy Bucher (XRD, ithemba Labs, South Africa), Dr. Franscious Cummings (HRTEM, Physics Department, University of the Western Cape (UWC), South Africa), Andrian Joseph (HRSEM, Physics department, UWC, South Africa).

Compliance with Ethical Standards

Conflict of interest

The authors declare that they have no conflict of interest.


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Copyright information

© King Fahd University of Petroleum & Minerals 2019

Authors and Affiliations

  • A. Oyewemi
    • 1
  • A. S. Abdulkareem
    • 1
    • 6
  • J. O. Tijani
    • 3
    • 6
    Email author
  • M. T. Bankole
    • 3
    • 6
  • O. K. Abubakre
    • 2
    • 6
  • A. S. Afolabi
    • 4
  • W. D. Roos
    • 5
  1. 1.Department of Chemical EngineeringFederal University of Technology MinnaMinnaNigeria
  2. 2.Department of Mechanical EngineeringFederal University of Technology MinnaMinnaNigeria
  3. 3.Department of ChemistryFederal University of Technology MinnaMinnaNigeria
  4. 4.Department of Chemical, Materials and Metallurgical EngineeringBotswana International University of Science and Technology (BIUST)PalapyeBotswana
  5. 5.Department of PhysicsUniversity of the Free StateBloemfonteinRepublic of South Africa
  6. 6.Nanotechnology Research Group, Centre for Genetic Engineering and BiotechnologyFederal University of Technology MinnaMinnaNigeria

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