Crystal Phase Tuning and Electrochemical Properties of WO3/Graphene Oxide Nanocomposites: Impact of pH and Organic Acids

Authors

  • P. M. Gonçalves Departamento de Química, Biotecnologia e Engenharia de Bioprocessos, Universidade Federal de São João del-Rei – Campus Alto Paraopeba, Rodovia MG 443, Km 07, CEP 36497-899, Ouro Branco, MG, Brazil Author
  • L. A. T. Costa Departamento de Química, Biotecnologia e Engenharia de Bioprocessos, Universidade Federal de São João del-Rei – Campus Alto Paraopeba, Rodovia MG 443, Km 07, CEP 36497-899, Ouro Branco, MG, Brazil Author
  • D. T. Cestarolli Departamento de Química, Biotecnologia e Engenharia de Bioprocessos, Universidade Federal de São João del-Rei – Campus Alto Paraopeba, Rodovia MG 443, Km 07, CEP 36497-899, Ouro Branco, MG, Brazil Author
  • E. M. Guerra Departamento de Química, Biotecnologia e Engenharia de Bioprocessos, Universidade Federal de São João del-Rei – Campus Alto Paraopeba, Rodovia MG 443, Km 07, CEP 36497-899, Ouro Branco, MG, Brazil Author

DOI:

https://doi.org/10.32628/IJSRST2613113

Keywords:

WO3/graphene oxide composites, hydrothermal synthesis, structure-directing agents, electrochemical stability, cyclic voltammetry

Abstract

WO3/graphene oxide (GO) composites were synthesized via a two-step hydrothermal method using citric acid (CA) or oxalic acid (OA) as structure-directing agents at precisely controlled pH values (1.0, 1.5, and 2.0). While WO3/GO composites have been previously reported, this work systematically investigates the synergistic effect of organic acid coordination chemistry (tridentate CA vs. bidentate OA) and pH on the crystalline phase, interfacial interaction, and electrochemical stability of the composites. XRD confirmed pH-dependent phase formation (hexagonal at pH ≥ 1.5, monoclinic at pH 1.0) and revealed strong WO3–GO interactions through peak broadening and crystallite size modulation. FTIR and Raman spectroscopy indicated acid-dependent interfacial bonding, with CA promoting stronger interaction with GO functionalities. Electrochemically, the WO3/OA/GO composite at pH 1.5 exhibited excellent charge retention (87% over 50 cycles), while WO3/CA/GO at the same pH showed a 260% increase in charge capacity, indicating electrochemical activation during cycling. These results demonstrate that fine-tuning synthesis conditions (acid type + pH) enables precise control over composite structure and performance, offering a rational strategy for designing advanced WO3-based materials for energy storage and electrochromic applications.

Downloads

Download data is not yet available.

References

K. S. Novoselov, V. I. Fal’Ko, L. Colombo, P. R. Gellert, M. G. Schwab, and K. Kim, “A roadmap for graphene,” Nature, vol. 490, no. 7419, pp. 192–200, Oct. 2012, doi: 10.1038/NATURE11458;SUBJMETA.

D. C. Marcano et al., “Improved Synthesis of Graphene Oxide,” ACS Nano, vol. 4, no. 8, pp. 4806–4814, Aug. 2010, doi: 10.1021/NN1006368.

A. Bagri, C. Mattevi, M. Acik, Y. J. Chabal, M. Chhowalla, and V. B. Shenoy, “Structural evolution during the reduction of chemically derived graphene oxide,” Nat. Chem., vol. 2, no. 7, pp. 581–587, Jul. 2010, doi: 10.1038/NCHEM.686;SUBJMETA.

S. Pitiphattharabun et al., “Reduced graphene oxide/zinc oxide composite as an electrochemical sensor for acetylcholine detection,” Sci. Reports 2024 141, vol. 14, no. 1, pp. 14224-, Jun. 2024, doi: 10.1038/s41598-024-64238-7.

N. Taghiyeva et al., “Synthesis and Characterization of Novel Adsorbents Based on Functionalization of Graphene Oxide with Schiff Base and Reduced Schiff Base for Pesticide Removal,” Mater. 2024, Vol. 17, Page 4096, vol. 17, no. 16, p. 4096, Aug. 2024, doi: 10.3390/MA17164096.

S. Li, X. Liu, C. Fang, N. Liu, and D. Liu, “Surface modification and thermal performance of a graphene oxide/novolac epoxy composite,” RSC Adv., vol. 8, no. 37, pp. 20505–20516, Jun. 2018, doi: 10.1039/C8RA02847H.

P. Bhojane and P. M. Shirage, “Facile preparation of hexagonal WO3 nanopillars and its reduced graphene oxide nanocomposites for high-performance supercapacitor,” J. Energy Storage, vol. 55, p. 105649, Nov. 2022, doi: 10.1016/J.EST.2022.105649.

Y. Shao et al., “Design and Mechanisms of Asymmetric Supercapacitors,” Chem. Rev., vol. 118, no. 18, pp. 9233–9280, Sep. 2018, doi: 10.1021/ACS.CHEMREV.8B00252.

P. A. Shinde and S. C. Jun, “Review on Recent Progress in the Development of Tungsten Oxide Based Electrodes for Electrochemical Energy Storage,” ChemSusChem, vol. 13, no. 1, pp. 11–38, Jan. 2020, doi: 10.1002/CSSC.201902071.

M. Kaur, S. Singh, S. K. Mehta, and S. K. Kansal, “rGO-WO3 Heterostructure: Synthesis, Characterization and Utilization as an Efficient Adsorbent for the Removal of Fluoroquinolone Antibiotic Levofloxacin in an Aqueous Phase,” Molecules, vol. 27, no. 20, p. 6956, Oct. 2022, doi: 10.3390/MOLECULES27206956/S1.

F. Farivar, P. L. Yap, R. U. Karunagaran, and D. Losic, “Thermogravimetric Analysis (TGA) of Graphene Materials: Effect of Particle Size of Graphene, Graphene Oxide and Graphite on Thermal Parameters,” C 2021, Vol. 7, Page 41, vol. 7, no. 2, p. 41, Apr. 2021, doi: 10.3390/C7020041.

M. Kaur, S. Singh, S. K. Mehta, and S. K. Kansal, “rGO-WO3 Heterostructure: Synthesis, Characterization and Utilization as an Efficient Adsorbent for the Removal of Fluoroquinolone Antibiotic Levofloxacin in an Aqueous Phase,” Molecules, vol. 27, no. 20, p. 6956, Oct. 2022, doi: 10.3390/MOLECULES27206956/S1.

W. Han, Q. Shi, and R. Hu, “Advances in electrochemical energy devices constructed with tungsten oxide‐based nanomaterials,” Nanomaterials, vol. 11, no. 3, pp. 1–42, Mar. 2021, doi: 10.3390/NANO11030692.

X. Zhang, G. Jin, D. Wang, Z. Chen, M. Zhao, and G. Xi, “Crystallographic phase and morphology dependent hydrothermal synthesis of tungsten oxide for robust hydrogen evolution reaction,” J. Alloys Compd., vol. 875, p. 160054, Sep. 2021, doi: 10.1016/J.JALLCOM.2021.160054.

Y. E. Firat, “Pseudocapacitive energy storage properties of rGO-WO3 electrode synthesized by electrodeposition,” Mater. Sci. Semicond. Process., vol. 133, Oct. 2021, doi: 10.1016/J.MSSP.2021.105938.

E. T. Attar, N. H. Abu-Hamdeh, A. H. Milyani, H. A. Z. AL-bonsrulah, and A. E. A. M. A. Elamin, “Investigation for improvement of discharging rate within a renewable energy storage system with adding nano-powders,” J. Energy Storage, vol. 71, p. 108114, Nov. 2023, doi: 10.1016/J.EST.2023.108114.

Ö. Budak, N. F. Öztürk, and A. Koca, “Electrodeposited molybdenum-tungsten oxide thin films decorated with cobalt phthalocyanine-reduced graphene oxide composites as functional capacitance materials for asymmetric supercapacitors,” Mater. Sci. Semicond. Process., vol. 188, p. 109254, Mar. 2025, doi: 10.1016/J.MSSP.2024.109254.

Downloads

Published

20-04-2026

Issue

Section

Research Articles

How to Cite

[1]
P. M. Gonçalves, L. A. T. Costa, D. T. Cestarolli, and E. M. Guerra, Trans., “Crystal Phase Tuning and Electrochemical Properties of WO3/Graphene Oxide Nanocomposites: Impact of pH and Organic Acids”, Int J Sci Res Sci & Technol, vol. 13, no. 2, pp. 861–875, Apr. 2026, doi: 10.32628/IJSRST2613113.