SYNTHESIS OF ZINC OXIDE/CHITOSAN/CHITRONELLA ESSENTIAL OIL HYBRID NANOPARTICLES USING SOL-GEL METHOD: STRUCTURAL AND OPTICAL PROPERTIES
Authors
Budi Astuti , Nur 'Ainiyyah Hasni , Ari Sulistiyo Rini , Dimas Mohamad Ayubi , Agus Yulianto , Masturi Masturi , Teguh Darsono , Putut Marwoto , Sugianto Sugianto , Suriani Abu Bakar , Fatiatun FatiatunDOI:
10.29303/ipr.v8i2.419Published:
2025-05-08Issue:
Vol. 8 No. 2 (2025)Keywords:
ZnO nanoparticle, Sol gel method, structure, morphologyArticles
Downloads
How to Cite
Abstract
Due to their properties, ZnO nanoparticles have recently been used as an additive material in active food packaging. ZnO has a wide band gap of about 3.37 eV, making it effectively used under UV light. However, ZnO nanoparticles are not effectively used under visible light. This study successfully synthesized ZnO-Chitosan-Citronella Essential Oil hybrid nanoparticles using sol-gel methods. Adding chitosan and citronella essential oil will affect nanoparticles' structural and optical properties. The structural, morphological, and optical properties of characterized hybrid nanoparticles were studied using X-ray diffraction (XRD) and FTIR, scanning electron microscope (SEM), energy dispersive X-ray (EDX), and UV-Vis spectroscopy. From XRD, it was obtained that the ZnO nanoparticles produced have a hexagonal wurtzite crystal structure with angles of 2q = 31.76°, 34.48°, 36.30° which are crystal planes with orientations (100), (002), and (101), as well as several other peaks for planes (102), (110), (103), (200) and (112) with a crystallinity index value of 86.5390%, and crystallite size of 8.87nm and 7.5335 nm. From FTIR Characterization, Zn=O functional groups were also obtained at wave numbers 657 and 475 cm-1. The morphology of ZnO nanoparticles from SEM spectroscopy shows a spherical shape with agglomeration, and the composition of the components Zn, O, and N elements is found, which come from chitosan materials. Furthermore, from the UV-Vis spectroscopy characterization, it was obtained that the absorption occurred in the 380-600 nm region with a band gap energy of 3.25 eV (using the tauc plot method), which was slightly different from the empirical results of 3.30 eV. The results show potential future studies of hybrid nanoparticles, such as additive materials in active food packaging.References
D.M. Tajashwini, H.V. Harini, H.P. Nagaswarupa, R. Naik, V.V. Deshmukh, and N. Basavaraju, “An in-depth exploration of eco-friendly synthesis method for metal oxide nanoparticle and their role in photocatalysis for industrial dye degradation, chemical physics impact, vol. 7, pp. 100355, 2023.
C. Abed, S. Fernandes, S. Aouida, H. Elhouichet, F. Priego, Y. Castro, M.M. Gomes-Mancebo, and G. Munuera, “Processing and study of optical and electrical properties of (Mg, Al) co doped ZnO thin films prepared by RF magnetron sputtering for photovoltaic application”. Materials. Vol. 13, no. 9, pp. 1-12, 2020.
B. Astuti, P. Marwoto, A. Zhafirah, N. Hamid, D. Aryanto, S. Sugianto, S. Sulhadi, N. M. D. Putra, and F. Fianti, “Structure, morphology, and optical properties of ZnO:Mg thin film prepared by sol-gel spin coating method”, Jurnal Ilmiah Pendidikan Fisika Al-BiRuNi, Vol. 10. No. 2. Pp. 75-84, 2021.
M. Bakry, W. Ismail, M. Abdelfatah, and A. El-Shaer, “Low-cost fabrication methods of ZnO nanorods and their physical and photoelectrochemical properties for optoelectronic applications”, Scientific Reports Nature Portfolio, Vol. 14, pp. 23788, 2024.
B. Astuti, A. Zhafirah, V. A. Carieta, N Hamid, P Marwoto, S. Sugianto, U. Nurbaiti, F. D. Ratnasari, N. M. D. Putra, and D. Aryanto, “X-ray diffraction studies of ZnO:Cu thin films prepared using sol-gel method”, Journal of Physics: Conference Series, Vol. 1567, pp. 022004, 2020.
P. Laokul, N. Kanjana, R. Ratchatanee, S. Ruangjan, N. Kotsarn, A. Chingsungnoen, and P. Poolcharuansin, “Preparation of AgBr decorated ZnO/ZnS nanocomposite for photocatalytic and antibacterial applications”, Materials Chemistry and Physics, Vol. 295. Pp. 127112, 2023.
J. Gaur, S. Kumar, M. Pal, H. Kaur, K.M. Batoo, J.O. Momoh, and Supreet,” Current trends: Zinc oxide nanoparticles preparation via chemical and green method for the photocatalytic degradation of various organic dyes”, Hybrid Advances, Vol. 5, pp.100128, 2024.
S. Lee, K.H. Jin, H. Jung, K. Fukutani, J. Lee, C. Kwon, J. S. Kim, J. Kim, and H. W. Yeom, “Surface Doping and Dual Nature of the Band Gap in Excitonic Insulator Ta2NiSe5”, : ACS Nano, Vol. 18, pp. 24784−24791, 2024.
W. Wang, C. Xue, and X. Mao, “Chitosan: Structural modification, biological activity and application, Vol. 164, pp. 4532-4546, 2020.
I. Aranaz, A.R. Alcántara, M.C. Civera, C. Arias, B. Elorza, H.A. Caballero, and N. Acosta, “Chitosan: An Overview of Its Properties and Applications”, Polymers, Vol. 13, No. 19, pp. 3256, 2021.
E. Zabihi, A. Babaei, D. Shahrampour, Z. Arab-Bafrani, K.S. Mirshahidi, and H.J. Majidi, “Facile and Rapid in-situ Synthesis of Chitosan- ZnO Nano-Hybrids Applicable in Medical Purposes; a Novel Combination of Biomineralization, Ultrasound and Bio-Safe Morphology-Conducting Agent”, International Journal of Biological Macromolecules, Vol. 131, pp. 107-116, 2019.
L. Motelica, D. Ficai, O. Oprea, A. Ficai, R.D. Trusca, E. Andronescu, and A.M. Holban, “Biodegradable Alginate Films with ZnO Nanoparticles and Citronella Essential Oil—A Novel Antimicrobial Structure. " Vol. 13 No. 7, pp. 1020, 2021.
T.A.J. De Souza, L.R.R. Souza, and L.P. Franchi, “Silver Nanoparticles: An Integrated View of Green Synthesis Methods, Transformation in The Environment, and Toxicity”. Ecotoxicology and environmental safety, Vol. 171, pp. 691-700, 2019.
M.M. Baig, M.A. Yousuf, P.O. Agboola, M.A. Khan, I. Shakir, and M.F. Warsi, “Optimization of Different Wet Chemical Routes and Phase Evolution Studies of MnFe2O4 Nanoparticles Vol. 45, No. 10, pp. 12682-12690, 2019.
Basnet, P., & Chatterjee, S. (2020). Structure-Directing Property and Growth Mechanism Induced by Capping Agents in Nanostructured ZnO During Hydrothermal Synthesis—A Systematic Review. Nano-Structures & Nano-Objects, 22, 100426.
R.L. Manjunatha, D. Naik, and K.V. Usharani, “Nanotechnology Application in Agriculture: A review”, Journal of Pharmacognosy and Phytochemistry, Vol. 8, No. 3, pp. 1073-1083, 2019.
M. Parashar, V.K. Shukla, and R. Singh, “Metal Oxides Nanoparticles Via Sol–Gel Method: a Review on Synthesis, Characterization and Applications. Journal of Materials Science: Materials in Electronics, Vol. 31, pp. 3729-3749, 2020.
J. Singh, T. Dutta, K.H. Kim, M. Rawat, P. Samddar, and P. Kumar, “Green ’synthesis of metals and their oxide nanoparticles: applications for environmental remediation”, Journal of nanobiotechnology, Vol. 16 No. 1, pp. 1-24, 2018.
S. Ying, Z. Guan, P.C. Ofoegbu, P. Clubb, C. Rico, F. He, and J. Hong, “Green Synthesis of Nanoparticles: Current Developments and Limitations”, Environmental Technology & Innovation, Vol. 26, pp. 102336, 2022.
Y.X. Gan, A.H. Jayatissa, Z. Yu, X. Chen, and M. Li, “Hydrothermal Synthesis of Nanomaterials”, Journal of Nanomaterials, Vol. 2020, pp. 1-3, 2020.
M. D'Arienzo, R. Scotti, B. Di Credico, and M. Redaelli, “Synthesis and Characterization of Morphology-Controlled TiO2 Nanocrystals: Opportunities and Challenges for Their Application in Photocatalytic Materials”, Studies in Surface Science and Catalysis, Vol. 177, pp. 477-540, 2017.
D. Navas, S. Fuentes, A. Castro- Alvarez, and E. Chavez-Angel, “Review on sol-gel synthesis of perovskite and oxide nanomaterials. Gels. Vol. 7, No. 4, pp. 275, 2021.
R. Paul, “Sol-Gel Method: Overcoming the Limitation in Nanoparticle Synthesis, Vol. 11, pp. 008, 2023.
T. Gasti, S. Dixit, V.D. Hiremani, R.B. Chougale, S.P. Masti, S.K. Vootla, and B.S. Mudigoudra, “Chitosan/Pullulan Based Films Incorporated with Clove Essential Oil Loaded Chitosan-ZnO Hybrid Nanoparticles for Active Food Packaging”, Carbohydrate Polymers, Vol. 277, pp. 118866, 2022.
S.C. Chabattula, P.K. Gupta, S.K. Tripathi, R. Gahtori, P.Padhi, S. Mahapatra, B.K. Biswal, S.K. Singh, K. Dua, J. Ruokolainen, Y.K. Mishra, N.K. Jha, D.K. Bishi, and K.K. Kesari , “Anticancer therapeutic efficacy of biogenic Am-ZnO nanoparticles on 2D and 3D tumor models”, Materials Today Chemistry, Vol. 22, pp. 100618, 2021.
G. Sathishkumar, C. Rajkuberan, K. Manikandan, S. Prabukumar, J. DanielJohn, S. Sivaramakrishnan, “Facile biosynthesis of antimicrobial zinc oxide (ZnO) nanoflakes using leaf extract of Couroupita guianensis Aubl.”, Materials Letters, Vol. 188, pp. 383-386, 2017.
A.M Ismail, A.A. Menazea, H.A. Kabary, A.E. El-Sherbiny, and A. Samy, “The Influence of Calcination Temperature on Structural and Antimicrobial Characteristics of Zinc Oxide Nanoparticles Synthesized by Sol–Gel Method”, Journal of Molecular Structure, Vol. 1196, pp. 332-337, 2019.
K. A Abdullah, S. Awada, J. Zaraket and C. Salame, “Synthesis of ZnO Nanopowders By Using Sol-Gel and Studying Their Structural and Electrical Properties at Different Temperature”, Energy Procedia, Vol. 119, pp. 565–570, 2017.
P. Jamdagni, P. Khatri, and J.S. Rana, “Green synthesis of zinc oxide nanoparticles using flower extract of Nyctanthes arbor-tristis and their antifungal activity”, J. King Saud Univ. Sci. Vol. 30, pp. 168e175, 2018.
B. Bulcha, J. L. Tesfaye, D. Anatol, R. Shanmugam, L.P. Dwarampudi, N. Nagaprasad, V. L. Nirmal Bhargavi, and R. Krishnaraj, “Synthesis of Zinc Oxide Nanoparticles by Hydrothermal Methods and Spectroscopic Investigation of Ultraviolet Radiation Protective Properties”, Hindawi Journal of Nanomaterials, Vol. 2021, pp. 8617290, 2021.
B. Astuti, N. Abidah, E.A. Fatiha, and K.A. Nugraha, “Structure and morphology analysis of annealing post-treatment thin film titanium and copper-doped zinc oxide”, Indonesian Physical Review, Vol. 6, No. 3, pp. 334-345, 2023.
I. Khan, K. Saeed, and I. Khan, “Nanoparticles: Properties, Applications and Toxicities”, Arabian Journal of Chemistry, Vol. 12, No. 7, 908-931, 2019.
I. Uzun, “Methods of determining the degree of crystallinity of polymers with X‑ray diffraction: a review”, Journal of Polymer Research, Vol.30, pp. 394, 2023.
S. Mansy, H. Musleh, S. Shaat, J. Asad, and N. Al Dahoudi,” Computational and experimental study of wurtzite phase ZnO nanoparticles”, MaterialsTodayCommunications, Vol. 35, pp. 105688, 2023.
M. Kahouli, A. Barhoumi, Anis Bouzid, A. Al-Hajry, and S. Guermazi, “Structural and optical properties of ZnO nanoparticles prepared by direct precipitation method”, Superlattices and Microstructures, Vol. 85, pp. 7-23, 2015.
W. L. de Almeida, N. S. Ferreira, F. S. Rodembusch, and V. C. de Sausa, “Study of structural and optical properties of ZnO nanoparticles synthesized by an eco-friendly tapioca-assisted route”, Materials Chemistry and Physics, Vol. 258, pp. 123926, 2021.
W. L. de Almeida, L. C. Freisleben, B. C. Brambilla, V. G. Isoppo, F. S. Rodembusch, V. C. de Sousa, “Influence of starch used in the sol‑gel synthesis of ZnO nanopowders”, J Nanopart Res, Vol. 25, pp. 75, 2023.
M. S. Choi, H. G. Na, G. S. Shim et al., “Simple and scalable synthesis of urchin-like ZnO nanoparticles via a microwave-assisted drying process,” Ceramics International, vol. 47, no. 10, pp. 14621–14629, 2021.
K. F. Hasan, H. Wang, S. Mahmud, and C. Genyang, “Coloration of aramid fabric via in-situ biosynthesis of silver nanoparticles with enhanced antibacterial effect,” Inorganic Chemistry Communications, vol. 119, p. 108115, 2020.
A. K. Dikshit, P. Banerjee, N. Mukherjee, and P. Chakrabarti, “Theoretical optimization of double dielectric back reflector layer for thin c-Si based advanced solar cells with notable enhancement in MAPD,” Superlattices and Microstructures, vol. 149, p. 106747, 2021.
J. A. Delezuk, D. E. Ramírez-Herrera, B. Esteban-Fernández de Ávila, and J. Wang, “Chitosan-based water-propelled micro motors with strong antibacterial activity,” Nanoscale, vol. 9, no. 6, pp. 2195–2200, 2017.
N. A. Ibrahim, A. A. Nada, B. M. Eid, M. Al-Moghazy, A. G. Hassabo, and N. Y. Abou-Zeid, “Nano-structured metal oxides: synthesis, characterization and application for multifunctional cotton fabric,” Advances in Natural Sciences: Nanoscience and Nanotechnology, vol. 9, no. 3, p. 035014, 2018.
S. M. Costa, D. P. Ferreira, A. Ferreira, F. Vaz, and R. Fangueiro, “Multifunctional flax fibres based on the combined effect of silver and zinc oxide (Ag/ZnO) nanostructures,” Nanomaterials, vol. 8, no. 12, p. 1069, 2018.
R. Pandimurugan and S. Thambidurai, “UV protection and antibacterial properties of seaweed capped ZnO nanoparticles coated cotton fabrics,” International Journal of Biological Macromolecules, vol. 105, Partt 1, pp. 788–795, 2017.
S. Mohan, M. Vellakkat, A. Aravind, and U. Reka, “Hydrothermal synthesis and characterization of Zinc Oxide nanoparticles of various shapes under different reaction conditions”, NanoExpress, vol. 1, pp. 030028, 2020.
H. H.A. Alshamsi, and B.S. Hussein, “Hydrothermal preparation of silver-doped zinc oxide nanoparticles: studies, characterization and photocatalytic activities”, Orient. J. Chem, vol. 34, pp. 1898, 2018.
P. Ramesh, K. Saravanan, P. Manogar, J. Johnson, E. Vinoth, and M. Mayakannan, “Green synthesis and characterization of biocompatible zinc oxide nanoparticles and evaluation of its antibacterial potential”, Sensing and Bio-Sensing Research, vol. 31, pp. 100399, 2021.
X. Xiao, B. Peng, L. Cai, and X. Zhang, “The highly efficient catalytic properties for thermal decomposition of ammonium perchlorate using mesoporous ZnCo2O4 rods synthesized by the oxalate co-precipitation method”, Sci. Rep.. vol. 8, pp. 7571, 2018.
M. Patel, S. Mishra, R. Verma, and D. Shikha,”Synthesis of ZnO and CuO nanoparticles via Sol gel method and its characterization by using various technique”, Discover Materials, vol. 2, no. 1, pp. 1, 2022.
Y. Zare, “Study of Nanoparticles Aggregation/Agglomeration in Polymer Particulate Nanocomposites by Mechanical Properties”, Composites Part A: Applied Science and Manufacturing, vol. 84, pp. 158-164, 2016.
I. Khan, K. Saeed, and I. Khan, “Nanoparticles: Properties, Applications and Toxicities”, Arabian Journal of Chemistry, vol. 12, no. 7, pp. 908-931, 2019.
A.R. Zanatta, “Revisiting the optical bandgap of semiconductors and the proposal of a unifed methodology to its determination, Scientific Report-nature report, vol. 9, pp. 11225, 2019.
A. Tadji, A. Abderrahmane, M. Zerdali, and S. Hamzaoui, “Facile preparation of nanostructured ZnO via low-temperature hydrothermal method upon changing the precursor anion: The study of structural, morphological, and optical properties”, Materials Today Communications, vol. 31, pp. 103789, 2022.
K.P. Misra, S. Jain, A. Agarwala, N. Halder, and S. Chattopadhyay, “Effective Mass Model Supported Band Gap Variation in Cobalt-Doped ZnO Nanoparticles Obtained by Co-precipitation”, Semiconductors, vol. 54, pp. 3, 2020.
P. Laokul, N. Kanjana, R. Ratchatanee, S. Ruangjan, N. Kotsarn, A. Chingsungnoen, and P. Poolcharuansin, “Preparation of AgBr decorated ZnO/ZnS nanocomposite for photocatalytic and antibacterial applications”, Materials Chemistry and Physics, vol. 295, pp. 127112, 2023.
Mohammada, A., Al-Jafa, H. A., Ahmeda, H. S., Mohammedb, M., and Khodairc, Z, Structural and morphological studies of ZnO nanostructures. Journal of Ovonic Research, Vol.18, No.3, pp. 443-452, 2022.
Alwadai, N., Investigation on Structural, Optical, Thermal, and Dielectric Properties of Nanocomposite Films Based on Chitosan Containing Vanadium Pentoxide/Zinc Oxide and Their Potential for Optoelectronics Devices. Journal of Molecular Structure, 1312, 138491, 2024.
Hisham, F., Akmal, M. M., Ahmad, F. B., & Ahmad, K., Facile Extraction of Chitin and Chitosan from Shrimp Shell. Materials Today: Proceedings, Vol. 42, pp. 2369-2373, 2021.
Prasetyaningrum, A., Wicaksono, B. S., Hakiim, A., Ashianti, A. D., Manalu, S. F. C., Rokhati, N., Utomo, D.P., dan Djaeni, M., Ultrasound-Assisted Encapsulation of Citronella Oil in Alginate/Carrageenan Beads: Characterization and Kinetic Models. ChemEngineering, 7(1), 10, 2023.
Arya, S., Mahajan, P., Mahajan, S., Khosla, A., Datt, R., Gupta, V., Young S.J., & Oruganti, S. K., Influence of processing parameters to control morphology and optical properties of Sol-Gel synthesized ZnO nanoparticles. ECS Journal of Solid State Science and Technology, 10(2), 023002, 2021.
Singh, A., Wan, F., Yadav, K., Salvi, A., Thakur, P., & Thakur, A., Synergistic effect of ZnO nanoparticles with Cu2+ doping on antibacterial and photocatalytic activity. Inorganic Chemistry Communications, 157, 111425, 2023.
License

This work is licensed under a Creative Commons Attribution-NonCommercial-ShareAlike 4.0 International License.
Authors who publish with Indonesian Physical Review Journal, agree to the following terms:
- Authors retain copyright and grant the journal right of first publication with the work simultaneously licensed under a Creative Commons Attribution-ShareAlike 4.0 International Licence (CC BY SA-4.0). This license allows authors to use all articles, data sets, graphics, and appendices in data mining applications, search engines, web sites, blogs, and other platforms by providing an appropriate reference. The journal allows the author(s) to hold the copyright without restrictions and will retain publishing rights without restrictions.
- Authors are able to enter into separate, additional contractual arrangements for the non-exclusive distribution of the journal's published version of the work (e.g., post it to an institutional repository or publish it in a book), with an acknowledgment of its initial publication in Indonesian Physical Review Journal.
- Authors are permitted and encouraged to post their work online (e.g., in institutional repositories or on their website) prior to and during the submission process, as it can lead to productive exchanges, as well as earlier and greater citation of published work (See The Effect of Open Access).