Structural and morphological characterization of tea-waste-derived carbon/TiO2 (AT–TiO2) composites prepared by solvent-assisted solid-state dispersion
Main Article Content
Abstract
Tea waste is an abundant agro-industrial residue but its valorization into functional inorganic composites remains largely unexplored. In this study, the waste was torrefied at 230 °C and combined with commercial TiO2 by a solvent-assisted solid-state dispersion route followed by calcination at 500 °C, giving a Tea-Waste-Derived carbon/ TiO2 material denoted AT– TiO2. A total of 3 AT: TiO2 mass ratios (9:1, 8:2 and 7:3) were prepared with pure AT and pure TiO2 controls processed identically, and characterized by XRD and SEM–EDS. XRD results showed that single-phase rutile retained its structure in every composite, with no peak shift and secondary phase. The carbon content was obtained in EDS pattern, due to the effect of using ethanol as a composite solvent. Scherrer analysis of the (110) reflection gave apparent crystallite sizes of 61, 34, 61, and 49 nm for pure TiO2 as well as the 9:1, 8:2 and 7:3 composites. SEM image analysis of 60 objects per sample, fitted to a log-normal distribution, gave median agglomerate sizes of 11.99 ± 0.51, 2.96 ± 0.32, 9.91 ± 0.74, 5.97 ± 0.66 and 11.00 ± 0.81 µm respectively. The 8:2 composite showed both the smallest median and the narrowest distribution (geometric standard deviation 1.56), indicating the most uniform dispersion. This study can serve as the basis for the development of biomass–inorganic composite materials with the potential to be applied in the fields of environmentally friendly adsorption and photocatalysis.
Article Details

This work is licensed under a Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International License.
This work is licensed under a Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International License.
References
Çakmak TG, Saricaoglu B, Ozkan G, Tomas M, Capanoglu E. Valorization of tea waste: composition, bioactivity, extraction methods, and utilization. Food Sci Nutr. 2024;12(5):3112-24. DOI: https://doi.org/10.1002/fsn3.4011
Hussain S, Anjali KP, Hassan ST, Dwivedi PB. Waste tea as a novel adsorbent: a review. Appl Water Sci. 2018;8(6):165. DOI: https://doi.org/10.1007/s13201-018-0824-5
Keiluweit M, Nico PS, Johnson MG, Kleber M. Dynamic molecular structure of plant biomass-derived black carbon (bochar). Environ Sci Technol. 2010;44(4):1247-53. DOI: https://doi.org/10.1021/es9031419
Mohan D, Sarswat A, Ok YS, Pittman CU. Organic and inorganic contaminants removal from water with biochar, a renewable, low cost and sustainable adsorbent – a critical review. Bioresour Technol. 2014;160:191-202. DOI: https://doi.org/10.1016/j.biortech.2014.01.120
Guerra-Que Z, López-Margalli KS, Urrieta-Saltijeral JM, Silahua-Pavón AA, Martínez-García H, García-Alamilla P, et al. Activated carbon synthesised from lignocellulosic cocoa pod husk via alkaline and acid treatment for methylene blue adsorption: optimisation by response surface methodology, kinetics, and isotherm modelling. RSC Adv. 2025;15(55):47231-54. DOI: https://doi.org/10.1039/D5RA05557A
Allen NS, Mahdjoub N, Vishnyakov V, Kelly PJ, Kriek RJ. The effect of crystalline phase (anatase, brookite and rutile) and size on the photocatalytic activity of calcined polymorphic titanium dioxide (TiO2). Polym Degrad Stab. 2018;150:31-6. DOI: https://doi.org/10.1016/j.polymdegradstab.2018.02.008
Cui ZH, Wu F, Jiang H. First-principles study of relative stability of rutile and anatase TiO2 using the random phase approximation. Phys Chem Chem Phys. 2016;18(43):29914-22. DOI: https://doi.org/10.1039/C6CP04973G
Listanti A, Taufiq A, Hidayat A, Sunaryono S. Investigasi Struktur dan Energi Band Gap Partikel Nano Tio2 Hasil Sintesis Menggunakan Metode Sol-Gel. J Phys Sci Eng. 2018;3(1):8-15. (In Indonesian) DOI: https://doi.org/10.17977/um024v3i12018p008
Fonseca-Cervantes OR, Pérez-Larios A, Romero Arellano VH, Sulbaran-Rangel B, Guzmán González CA. Effects in band gap for photocatalysis in TiO2 support by adding gold and ruthenium. Processes. 2020;8(9):1032. DOI: https://doi.org/10.3390/pr8091032
Hoffmann MR, Martin ST, Choi W, Bahnemann DW. Environmental applications of semiconductor photocatalysis. Chem Rev. 1995;95(1):69-96. DOI: https://doi.org/10.1021/cr00033a004
Schneider J, Matsuoka M, Takeuchi M, Zhang J, Horiuchi Y, Anpo M, et al. Understanding TiO2 photocatalysis: mechanisms and materials. Chem Rev. 2014;114(19):9919-86. DOI: https://doi.org/10.1021/cr5001892
Diebold U. The surface science of titanium dioxide. Surf Sci Rep. 2003;48(5-8):53-229. DOI: https://doi.org/10.1016/S0167-5729(02)00100-0
Chong MN, Jin B, Chow CWK, Saint C. Recent developments in photocatalytic water treatment technology: a review. Water Res. 2010;44(10):2997-3027. DOI: https://doi.org/10.1016/j.watres.2010.02.039
Meirelles MR, Giroto AS, Furukawa K, Gonçalves M. Valorization of lignocellulosic biomass for photocatalytic applications: development of activated carbon-TiO2 composites. ACS Sustainable Resour Manage. 2025;2(3):524-35. DOI: https://doi.org/10.1021/acssusresmgt.4c00512
Cañon-Tafur LA, Mateus-Maldonado JF, Lozano-Puentes HS, Herrera-Acosta CD, Sánchez-Matiz JJ, Díaz-Ariza LA, et al. Guadua angustifolia biochar/TiO2 composite and biochar as bio-based materials with environmental and agricultural application. Sci Rep. 2025;15(1):246. DOI: https://doi.org/10.1038/s41598-024-81761-9
Kanakaraju D, Natashya PP, Lim YC, Tan IAW. Functionalized TiO2-waste-derived photocatalytic materials for emerging pollutant degradation: synthesis and optimization. Environ Monit Assess. 2025;197(9):983. DOI: https://doi.org/10.1007/s10661-025-14431-6
Munir R, Hamdani D, Darnah, Marliana E, Munir R, Intifadhah SH, et al. The solid state dispersion method for synthesizing eggshells ES/TiO2 composite to enhance photocatalytic degradation methylene blue. MethodsX. 2025;14:103150. DOI: https://doi.org/10.1016/j.mex.2024.103150
Ali HA, Hameed NJ. The study of the particle size effect on the physical properties of TiO2/cellulose acetate composite films. J Mech Behav Mater. 2022;31(1):150-9. DOI: https://doi.org/10.1515/jmbm-2022-0019
Peñas-Garzón M, Gómez-Avilés A, Bedia J, Rodriguez JJ, Belver C. Effect of activating agent on the properties of TiO2/activated carbon heterostructures for solar photocatalytic degradation of acetaminophen. Materials. 2019;12(3):378. DOI: https://doi.org/10.3390/ma12030378
Moslehifard E, Robati Anaraki M, Shirkavand S. Effect of adding TiO2 nanoparticles on the SEM morphology and mechanical properties of conventional heat-cured acrylic resin. J Dent Res Dent Clin Dent Prospects. 2019;13(3):234-40. DOI: https://doi.org/10.15171/joddd.2019.036
Kurniawidi DW, Rahayu S, Budianto A, Saputra K, Agista WP, Suprayogi T, et al. Synthesis and characterization of TiO2/CaTiO3 perovskite composite derived from pinctada maxima shell waste. Sci Technol Indonesia. 2025;10(3):924-42. DOI: https://doi.org/10.26554/sti.2025.10.3.924-942
Cruz D, Ortiz-Oliveros HB, Flores-Espinosa RM, Ávila Pérez P, Ruiz-López II, Quiroz-Estrada KF. Synthesis of Ag/TiO2 composites by combustion modified and subsequent use in the photocatalytic degradation of dyes. J King Saud Univ Sci. 2022;34(4):101966. DOI: https://doi.org/10.1016/j.jksus.2022.101966
Ramadhani JP, Wahyuningsih S, Ramelan AH. Improving method of TiO2-Fe2O3 composite materials for self-cleaning glass preparation. IOP Conf Ser: Mater Sci Eng. 2019;578(1):012029. DOI: https://doi.org/10.1088/1757-899X/578/1/012029
Hikmah U, Yanti DR, Axala DLG, Hastuti E, Prasetyo A. Synthesis of material composite rGO-TIO2 from coconut shells by sol-gel methods as photocatalyst. Indonesian J Appl Phys. 2024;14(1):70. DOI: https://doi.org/10.13057/ijap.v14i1.77714
Kustiningsih I, Nurrahman F, Rinaldi HA, Jumiati IE, Sari DK, Jayanudin. Synthesize Fe3O4-TiO2 composite for methyl orange photocatalytic degradation. Mater Sci Forum. 2022;1057:129-35. DOI: https://doi.org/10.4028/p-9q4ts9
Chen WH, Peng J, Bi XT. A state-of-the-art review of biomass torrefaction, densification and applications. Renew Sustain Energy Rev. 2015;44:847-66. DOI: https://doi.org/10.1016/j.rser.2014.12.039
Prins MJ, Ptasinski KJ, Janssen FJJG. Torrefaction of wood: Part 1. Weight loss kinetics. J Anal Appl Pyrolysis. 2006;77(1):28-34. DOI: https://doi.org/10.1016/j.jaap.2006.01.002
Tiwari AK, Singh AK, Jha S, Tripathi SK, Awasthi RR, Mishra SK, et al. Green synthesis of TiO2 nanoparticles using Kinnow peel extracts and their antioxidant properties. Sci Rep. 2025;15(1):38307. DOI: https://doi.org/10.1038/s41598-025-22078-z
Bonelli B, Tammaro O, Martinovic F, Nasi R, Dell’Agli G, Rivolo P, et al. Reverse Micelle Strategy for the Synthesis of MnOx–TiO2 Active Catalysts for NH3‑Selective Catalytic Reduction of NOx at Both Low Temperature and Low Mn Content. ACS Omega. 2021;6(38):24562-74. DOI: https://doi.org/10.1021/acsomega.1c03153
