BIOWASTE TEMPLATED TiO2 NANOPARTICLES DOPED WITH IRON IONS: STRUCTURAL, MORPHOLOGICAL, AND OPTICAL CHARACTERIZATION

Nazlı Türkten; Yunus Karataş; Zekiye Cinar

doi:10.17780/ksujes.1728400

EN TR

BIOWASTE TEMPLATED TiO2 NANOPARTICLES DOPED WITH IRON IONS: STRUCTURAL, MORPHOLOGICAL, AND OPTICAL CHARACTERIZATION

Abstract

This study highlighted a facile preparation of a low-cost and efficient iron dopant photocatalyst using rice husk (RH) for water treatment. RH was not only used as a template but also as a multi-dopant source to prepare biowaste-templated TiO2 nanoparticles with iron ions (RH-Fe-TiO2). RH, as an agricultural waste, was used to prepare RH-Fe-TiO2 nanoparticles through a sol-gel method, followed by iron doping via a wet impregnation method. XRD analysis results indicated that the RH-Fe-TiO2 specimen contained a mixed phase, primarily composed of anatase and a smaller amount of rutile TiO2. The removal of the sacrificial template and the iron doping were confirmed through SEM-EDAX and XPS analysis. FTIR analysis also proved the presence of silicon derived from RH and iron dopant ions resulting from the doping procedure. The morphology of the RH-Fe-TiO2 specimen exhibited a fibrous and lamellar structure with cracks formed due to the removal of the sacrificial template. The iron doping process resulted in a reduction of the band gap and an observed red shift in the spectrum. The BET surface area of the photocatalyst was found to be 47 m2/g. The RH-Fe-TiO2 catalyst degraded 41% of 4-nitrophenol (4-NP) in 120 min.

Keywords

DEMİR İYONLARI KATKILI BİYO-ATIK İÇERİKLİ TiO2 NANO TANECİKLERİ: YAPISAL, MORFOLOJİK VE OPTİKSEL KARAKTERİZASYONU

Öz

Bu çalışmada, pirinç kabuğu (RH) kullanılması ile düşük maliyetli ve etkili bir demir katkılı fotokatalizörün su arıtımında kullanılması için kolay bir yöntemle sentezi konusu vurgulanmıştır. RH sadece bir şablon olarak kullanılmamış, aynı zamanda çoklu bir katkılandırma kaynağı olarak da demir iyonları içeren biyo-atık içerikli TiO2 nano taneciklerinin (RH-Fe-TiO2) hazırlanmasında kullanılmıştır. RH-Fe-TiO2 örneğinin hazırlanmasında tarımsal atık olan RH ile sol-jel yöntemi ve ardından ıslak emdirme yöntemi kullanılarak demir katkılandırılması sağlanmıştır. XRD analiz sonuçları, RH-Fe-TiO2 nano taneciklerinin başlıca anataz fazı ve eser miktarda rutil TiO2 fazı içeren bir faz karışımından oluştuğunu göstermiştir. SEM-EDAX ve XPS analizleri ile şablonunun uzaklaştırılması ve demir katkısının varlığı doğrulandı. FTIR analizi ile RH’den gelen silikonun ve katkılandırma işleminden oluşan demir iyonlarının varlığı kanıtlanmıştır. RH-Fe-TiO2 numunesinin morfolojisi, şablonunun uzaklaşması sonucunda oluşan çatlaklar içeren lifli ve lamelli bir yapı göstermiştir. Demir ile katkılandırma işlemi sonucunda, band boşluğu azalmış ve spektrumda kırmızıya doğru bir kayma gözlenmiştir. Fotokatalizörün BET yüzey alanı 47 m2/g olarak bulunmuştur. RH-Fe-TiO2 katalizörü, 4-nitrofenolün (4-NP) %41'ini 120 dakikada giderebilmiştir.

Anahtar Kelimeler

Kaynakça

Banu Yener, H., & Helvacı, Ş. Ş. (2015). Effect of synthesis temperature on the structural properties and photocatalytic activity of TiO2/SiO2 composites synthesized using rice husk ash as a SiO2 source. Separation and Purification Technology, 140, 84-93. https://doi.org/https://doi.org/10.1016/j.seppur.2014.11.013
Bibi, A., Bibi, S., Abu-Dieyeh, M., & Al-Ghouti, M. A. (2023). Towards sustainable physiochemical and biological techniques for the remediation of phenol from wastewater: A review on current applications and removal mechanisms. Journal of Cleaner Production, 417, 137810. https://doi.org/https://doi.org/10.1016/j.jclepro.2023.137810
Birben, N. C., Uyguner-Demirel, C. S., Kavurmaci, S. S., Gürkan, Y. Y., Turkten, N., Cinar, Z., & Bekbolet, M. (2017). Application of Fe-doped TiO2 specimens for the solar photocatalytic degradation of humic acid. Catalysis Today, 281, 78-84. https://doi.org/10.1016/j.cattod.2016.06.020
de Cordoba, M. C. F., Matos, J., Montaña, R., Poon, P. S., Lanfredi, S., Praxedes, F. R., Hernández-Garrido, J. C., Calvino, J. J., Rodríguez-Aguado, E., Rodríguez-Castellón, E., & Ania, C. O. (2019). Sunlight photoactivity of rice husks-derived biogenic silica. Catalysis Today, 328, 125-135. https://doi.org/https://doi.org/10.1016/j.cattod.2018.12.008
De Gregori da Rocha, J., Santana Junior, M. B., Pier Macuvele, D. L., Riella, H. G., Ienczak, J. L., Padoin, N., & Soares, C. (2025). Uncovering engineering and mechanistic insights in green synthesis of carbon dots from rice husks. Chemical Engineering Journal, 505, 159364. https://doi.org/https://doi.org/10.1016/j.cej.2025.159364
Gurkan, Y., Kasapbasi, E., Turkten, N., & Cinar, Z. (2017). Influence of Se/N Codoping on the Structural, Optical, Electronic and Photocatalytic Properties of TiO2. Molecules, 22(3), 414. http://www.mdpi.com/1420-3049/22/3/414
Hong, J., Cho, K.-H., Presser, V., & Su, X. (2022). Recent advances in wastewater treatment using semiconductor photocatalysts. Current Opinion in Green and Sustainable Chemistry, 36, 100644. https://doi.org/https://doi.org/10.1016/j.cogsc.2022.100644
Hui, C., Lei, Z., Xitang, W., Shujing, L., & Zhongxing, L. (2015). Preparation of Nanoporous TiO2/SiO2 Composite with Rice Husk as Template and Its Photocatalytic Property. Rare Metal Materials and Engineering, 44(7), 1607-1611. https://doi.org/https://doi.org/10.1016/S1875-5372(15)30101-6

Hung, W.-C., Chen, Y.-C., Chu, H., & Tseng, T.-K. (2008). Synthesis and characterization of TiO2 and Fe/TiO2 nanoparticles and their performance for photocatalytic degradation of 1,2-dichloroethane. Applied Surface Science, 255(5, Part 1), 2205-2213. https://doi.org/https://doi.org/10.1016/j.apsusc.2008.07.079
Hussain, M., Aadil, M., Cochran, E. W., Zulfiqar, S., Hassan, W., Kousar, T., Somaily, H. H., & Mahmood, F. (2024). Facile synthesis of a porous sorbent derived from the rice husk biomass: A new and highly efficient material for water remediation. Inorganic Chemistry Communications, 160, 112010. https://doi.org/https://doi.org/10.1016/j.inoche.2023.112010
Jahantiq, A., Ghanbari, R., Panahi, A. H., Ashrafi, S. D., Khatibi, A. D., Noorabadi, E., Meshkinian, A., & Kamani, H. (2020). Photocatalytic degradation of 2,4,6-trichlorophenol in aqueous solutions using synthesized Fe-doped TiO2 nanoparticles via response surface methodology. Desalination and Water Treatment, 183, 366-373. https://doi.org/https://doi.org/10.5004/dwt.2020.25249
Jayasaranya, N., Pavai, R. E., Sagadevan, S., Balu, L., & Manoharan, C. (2024). Enhanced room temperature gas sensing performance of iron-doped titanium dioxide nanocomposite. Applied Physics A, 130(8), 539. https://doi.org/10.1007/s00339-024-07688-0
Joseph, C. G., Taufiq-Yap, Y. H., Musta, B., Sarjadi, M. S., & Elilarasi, L. (2021). Application of Plasmonic Metal Nanoparticles in TiO2-SiO2 Composite as an Efficient Solar-Activated Photocatalyst: A Review Paper [Review]. Frontiers in Chemistry, Volume 8 - 2020. https://doi.org/10.3389/fchem.2020.568063
Kapridaki, C., Xynidis, N., Vazgiouraki, E., Kallithrakas-Kontos, N., & Maravelaki-Kalaitzaki, P. (2019). Characterization of Photoactive Fe-TiO2 Lime Coatings for Building Protection: The Role of Iron Content. Materials, 12(11), 1847. https://www.mdpi.com/1996-1944/12/11/1847
Komaraiah, D., Radha, E., Kalarikkal, N., Sivakumar, J., Ramana Reddy, M. V., & Sayanna, R. (2019). Structural, optical and photoluminescence studies of sol-gel synthesized pure and iron doped TiO2 photocatalysts. Ceramics International, 45(18, Part B), 25060-25068. https://doi.org/https://doi.org/10.1016/j.ceramint.2019.03.170
Kubelka, P., & Munk, F. A. (1931). Contribution to the optics of pigments. Zeitschrift für technische Physik, 12, 593-599.
Li, Z., Zheng, Z., Li, H., Xu, D., Li, X., Xiang, L., & Tu, S. (2023). Review on Rice Husk Biochar as an Adsorbent for Soil and Water Remediation. Plants, 12(7), 1524. https://www.mdpi.com/2223-7747/12/7/1524
Liou, T.-H., & Wang, S.-Y. (2025). Utilizing rice husk for sustainable production of mesoporous titania nanocomposites with highly adsorption and photocatalysis. Biomass and Bioenergy, 199, 107950. https://doi.org/https://doi.org/10.1016/j.biombioe.2025.107950
Matias, M. L., Pimentel, A., Reis-Machado, A. S., Rodrigues, J., Deuermeier, J., Fortunato, E., Martins, R., & Nunes, D. (2022). Enhanced Fe-TiO2 Solar Photocatalysts on Porous Platforms for Water Purification. Nanomaterials, 12(6), 1005. https://www.mdpi.com/2079-4991/12/6/1005
Mohd Zaki, R. S. R., Jusoh, R., Chanakaewsomboon, I., & Setiabudi, H. D. (2024). Recent advances in metal oxide photocatalysts for photocatalytic degradation of organic pollutants: A review on photocatalysts modification strategies. Materials Today: Proceedings, 107, 59-67. https://doi.org/https://doi.org/10.1016/j.matpr.2023.07.102
Onu, C. E., Ohale, P. E., Obiora-Okafo, I. A., Asadu, C. O., Okoye, C. C., Ojukwu, E. V., & Ezennajiego, E. E. (2022). Application of Rice Husk-Based Biomaterial in Textile Wastewater Treatment. In S. S. Muthu & A. Khadir (Eds.), Textile Wastewater Treatment: Sustainable Bio-nano Materials and Macromolecules, Volume 2 (pp. 231-250). Springer Nature Singapore. https://doi.org/10.1007/978-981-19-2852-9_12
Prabha, S., Durgalakshmi, D., Rajendran, S., & Lichtfouse, E. (2021). Plant-derived silica nanoparticles and composites for biosensors, bioimaging, drug delivery and supercapacitors: a review. Environmental Chemistry Letters, 19(2), 1667-1691. https://doi.org/10.1007/s10311-020-01123-5
Rangarajan, G., Jayaseelan, A., & Farnood, R. (2022). Photocatalytic reactive oxygen species generation and their mechanisms of action in pollutant removal with biochar supported photocatalysts: A review. Journal of Cleaner Production, 346, 131155. https://doi.org/https://doi.org/10.1016/j.jclepro.2022.131155
San, N., Hatipoǧlu, A., Koçtürk, G., & Çınar, Z. (2001). Prediction of primary intermediates and the photodegradation kinetics of 3-aminophenol in aqueous TiO2 suspensions. Journal of Photochemistry and Photobiology A: Chemistry, 139(2–3), 225-232. https://doi.org/http://dx.doi.org/10.1016/S1010-6030(01)00368-9
San, N., Hatipoğlu, A., Koçtürk, G., & Çınar, Z. (2002). Photocatalytic degradation of 4-nitrophenol in aqueous TiO2 suspensions: Theoretical prediction of the intermediates. Journal of Photochemistry and Photobiology A: Chemistry, 146(3), 189-197. https://doi.org/http://dx.doi.org/10.1016/S1010-6030(01)00620-7
Scherrer, P. (1918). Estimation of the size and internal structure of colloidal particles by means of röntgen. Nachrichten von der Gesellschaft der Wissenschaften zu Göttingen, 2, 96–100.
Sing, K. S. W. (1985). Reporting physisorption data for gas/solid systems with special reference to the determination of surface area and porosity (Recommendations 1984). In Pure and Applied Chemistry (Vol. 57, pp. 603).
Suhot, M. A., Hassan, M. Z., Aziz, S. a. A., & Md Daud, M. Y. (2021). Recent Progress of Rice Husk Reinforced Polymer Composites: A Review. Polymers, 13(15), 2391. https://www.mdpi.com/2073-4360/13/15/2391
Sujanto, R. Y., Herrera, S. G. M., & Negash, Y. T. (2024). Enhancing environmental sustainability in a Circular Waste Bioeconomy: A hierarchical framework driven by operational efficiency and agro-energy management. Cleaner and Circular Bioeconomy, 9, 100115. https://doi.org/https://doi.org/10.1016/j.clcb.2024.100115
Sun, J., Mu, Q., Kimura, H., Murugadoss, V., He, M., Du, W., & Hou, C. (2022). Oxidative degradation of phenols and substituted phenols in the water and atmosphere: a review. Advanced Composites and Hybrid Materials, 5(2), 627-640. https://doi.org/10.1007/s42114-022-00435-0
Thuan, D. V., Chu, T. T. H., Thanh, H. D. T., Le, M. V., Ngo, H. L., Le, C. L., & Thi, H. P. (2023). Adsorption and photodegradation of micropollutant in wastewater by photocatalyst TiO2/rice husk biochar. Environmental Research, 236, 116789. https://doi.org/https://doi.org/10.1016/j.envres.2023.116789
Turkten, N., Karatas, B., Karatas, Y., Cinar, Z., & Bekbolet, M. (2023). A facile synthesis of bio-inspired hierarchical microstructure TiO2: Characterization and photocatalytic activity. Environmental Progress & Sustainable Energy, 42(3), e14054. https://doi.org/https://doi.org/10.1002/ep.14054
Türkten, N., & Uyguner Demirel, C. S. (2020). Photocatalytic Activity of in-situ Fe-Doped TiO2 for Natural Organic Matter Removal [Organİk madde gİderİmİ İÇİn eŞ anli (in-situ) fe-katkili tİo2’nİn fookatalİtİk aktİvİtesİ]. Mühendislik Bilimleri ve Tasarım Dergisi, 8(3), 664-670. https://doi.org/10.21923/jesd.672750
Wang, W., Chen, H., Fang, J., & Lai, M. (2019). Large-scale preparation of rice-husk-derived mesoporous SiO2@TiO2 as efficient and promising photocatalysts for organic contaminants degradation. Applied Surface Science, 467-468, 1187-1194. https://doi.org/https://doi.org/10.1016/j.apsusc.2018.10.275 Yadav, V., & Shrotriya, S. (2024). Waste-to-Wealth. https://doi.org/10.1201/9781003327646
Yalçın, Y., Kılıç, M., & Çınar, Z. (2010). Fe+3-doped TiO2: A combined experimental and computational approach to the evaluation of visible light activity. Applied Catalysis B: Environmental, 99(3-4), 469-477. https://doi.org/10.1016/j.apcatb.2010.05.013
Zhaohui, H., Hui, C., Lei, Z., Xuan, H., Weixin, L., Wei, F., & Guanghui, W. (2018). Biogenic Hierarchical MIL-125/TiO2@SiO2 Derived from Rice Husk and Enhanced Photocatalytic Properties for Dye Degradation. Photochemistry and Photobiology, 94(3), 512-520. https://doi.org/https://doi.org/10.1111/php.12873
Zia, J., & Riaz, U. (2021). Photocatalytic degradation of water pollutants using conducting polymer-based nanohybrids: A review on recent trends and future prospects. Journal of Molecular Liquids, 340, 117162. https://doi.org/https://doi.org/10.1016/j.molliq.2021.117162

Ayrıntılar

Birincil Dil

İngilizce

Konular

Çevre Kirliliği ve Önlenmesi , Küresel Çevre Mühendisliği , Atıksu Arıtma Süreçleri

Bölüm

Araştırma Makalesi

Yazarlar

Nazlı Türkten
0000-0001-9343-3697
Türkiye

Yunus Karataş ^*
0000-0002-3826-463X
Türkiye

Zekiye Cinar
0009-0008-0377-6126
Türkiye

Yayımlanma Tarihi

3 Mart 2026

Gönderilme Tarihi

27 Haziran 2025

Kabul Tarihi

26 Temmuz 2025

Yayımlandığı Sayı

Yıl 2026 Cilt: 29 Sayı: 1

DOI

https://doi.org/10.17780/ksujes.1728400

IZ

https://izlik.org/JA43FB53LA

Kaynak Göster

RIS / Bibtex

APA

Türkten, N., Karataş, Y., & Cinar, Z. (2026). BIOWASTE TEMPLATED TiO2 NANOPARTICLES DOPED WITH IRON IONS: STRUCTURAL, MORPHOLOGICAL, AND OPTICAL CHARACTERIZATION. Kahramanmaraş Sütçü İmam Üniversitesi Mühendislik Bilimleri Dergisi, 29(1), 420-429. https://doi.org/10.17780/ksujes.1728400