Applied Nanoscience

, Volume 9, Issue 2, pp 209–224 | Cite as

Optimization of the controllable crystal size of iron/zeolite nanocomposites using a Box–Behnken design and their catalytic activity

  • Nurazni Amat Bahari
  • Wan Nor Roslam Wan IsahakEmail author
  • Mohd Shahbudin Masdar
  • Muneer M. Ba-Abbad
Original Article


Experimental conditions for the synthesis of an iron nanoparticle (NPs)–zeolite composite (hereinafter denoted as Fe/zeolite NPs) via sol–gel method were optimized using a Box–Behnken design to produce a high formic acid yield. The effects of various parameters, including weight ratio of starting materials (Fe and zeolite), volume of polyethylene glycol (PEG) as a surfactant, and calcination temperature, on controllable crystallite size, and the relationship between crystallite size and formic acid yield were studied. The crystal size, as the main parameter indicating formic acid yield, of Fe NPs was evaluated through polynomial regression. Results revealed that the optimum conditions for producing small Fe NPs based on the model were obtained at a weight ratio of Fe to zeolite of 62.5%, a PEG volume of 2 mL, and a calcination temperature of 500 °C. The experimental results (52.02 nm) versus the predicted results (58.30 nm) of the crystal size of Fe NPs under the optimum synthesis conditions were similar. Furthermore, 62.5% Fe/zeolite NPs with a crystal size of 52.02 nm produced the highest formic acid concentration from CO2 hydrogenation. Conversely, 100% Fe/zeolite NPs had a smaller crystal size but exhibited a remarkably lower reaction performance. This high ratio of Fe and zeolite contributed to the increased agglomeration of Fe particles. The zeolite surface became fully covered and subsequently reduced the reactant interaction on catalyst surfaces.


  • Fe–zeolite nanocomposite was optimized using a Box–Behnken design.

  • The polynomial regression model showed the optimum nanoparticle (NP) crystal size of 52.02 nm.

  • Synthesis parameters significantly affected catalyst morphology and crystal.

  • The effect of calcination plays an important role on crystal and particle size.

  • The influence of NP crystallite size was evaluated in terms of formic acid production.


Box–Behnken design Fe/zeolite nanoparticles Optimization Carbon dioxide Formic acid 



The authors wish to thank Universiti Kebangsaan Malaysia (UKM) and Ministry of Higher Education for funding this project under Research Grant, DIP-2016-010, and GUP-2016-057, respectively, and the Centre of Research and Innovation Management (CRIM) UKM for the use of the instruments.

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.


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Copyright information

© King Abdulaziz City for Science and Technology 2018

Authors and Affiliations

  1. 1.Research Centre for Sustainable Process Technology (CESPRO), Faculty of Engineering and Built EnvironmentUniversiti Kebangsaan MalaysiaBangiMalaysia
  2. 2.Chemical Engineering Programme, Faculty of Engineering and Built EnvironmentUniversiti Kebangsaan MalaysiaBangiMalaysia
  3. 3.Department of Chemical Engineering, Faculty of Engineering and PetroleumHadhramout UniversityMukallaYemen

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