Fabrication and Characterization of Wet-Spun Ti3C2Tx MXene Fibers

Öz

MXene fibers have attracted considerable attention for flexible electronics and wearable devices owing to their high electrical conductivity and solution processability. The morphology and electrical conductivity of wet-spun MXene fibers are strongly influenced by fabrication conditions. Continuous Ti₃C₂Tₓ MXene fibers were fabricated by wet spinning using colloidal dispersions with concentrations ranging from 25 to 80 mg mL-1. Fiber morphology and electrical conductivity were evaluated as a function of dispersion concentration. The electrical conductivity showed an increasing trend with concentration, reaching 446.06 S cm-1 for fibers prepared from the 80 mg mL-1 dispersion, compared with 58.95 S cm-1 for fibers prepared from the 25 mg mL-1 dispersion. This improvement is attributed to enhanced interflake contact and improved connectivity between MXene nanosheets at higher concentrations. Overall, the results demonstrate the successful fabrication of continuous MXene fibers across a range of dispersion concentrations and clarify the relationship between processing conditions, fiber morphology, and electrical conductivity, providing guidance for the optimization of MXene fiber fabrication for flexible electronic applications.

Anahtar Kelimeler

• Colloidal concentration
• Electrical conductivity
• Fiber morphology
• MXene fibers
• Ti3C2Tx
• Wet spinning

Destekleyen Kurum

The Scientific and Technological Research Council of Türkiye (TÜBİTAK)

Proje Numarası

221M523

Etik Beyan

This study did not involve human participants or animals. Therefore, ethical committee approval was not required.

Teşekkür

The authors gratefully acknowledge the financial support provided by TÜBİTAK under Project No. 221M523.

Islak Eğirme Yöntemiyle Üretilen Ti3C2Tx MXene Fiberin Üretimi ve Karakterizasyonu

Öz

MXene fiberler, yüksek elektriksel iletkenlikleri ve çözelti bazlı işlenebilirlikleri sayesinde esnek elektronikler ve giyilebilir cihazlar için önemli bir ilgi görmektedir. Islak eğirme yöntemiyle üretilen MXene fiberlerin morfolojisi ve elektriksel iletkenliği, üretim koşullarından güçlü şekilde etkilenmektedir. Bu çalışmada, 25–80 mg mL⁻¹ konsantrasyon aralığındaki kolloidal Ti₃C₂Tₓ MXene dispersiyonları kullanılarak sürekli MXene fiberler ıslak eğirme yöntemiyle üretilmiştir. Fiber morfolojisi ve elektriksel iletkenliği, dispersiyon konsantrasyonuna bağlı olarak değerlendirilmiştir. Elektriksel iletkenlik, konsantrasyonun artmasıyla birlikte yükselmiş ve 25 mg mL⁻¹ dispersiyondan üretilen fiberlerde 58.95 S cm⁻¹ iken, 80 mg mL⁻¹ dispersiyondan üretilen fiberlerde 446.06 S cm⁻¹ değerine ulaşmıştır. Bu iyileşme, yüksek konsantrasyonlarda MXene nanotabakaları arasındaki temasın ve bağlantının artmasına bağlanmaktadır. Sonuç olarak, farklı dispersiyon konsantrasyonlarında sürekli MXene fiberlerin başarıyla üretildiği gösterilmiş ve işlem koşulları, fiber morfolojisi ile elektriksel iletkenlik arasındaki ilişki ortaya konularak esnek elektronik uygulamaları için MXene fiber üretiminin optimize edilmesine yönelik yol gösterici bilgiler sunulmuştur.

Anahtar Kelimeler

• Ti3C2Tx
• Elektriksel iletkenlik
• Mxene fiber
• Kolloidal konsantrasyon
• ıslak eğirme
• fiber morfolojisi

Destekleyen Kurum

Türkiye Bilimsel ve Teknolojik Araştırma Kurumu (TÜBİTAK)

Proje Numarası

221M523

Etik Beyan

Bu çalışma kapsamında insan ve/veya deney hayvanları kullanılmadığından etik kurul onayı gerekmemektedir.

Teşekkür

Yazarlar, bu çalışmaya sağladığı mali destekten dolayı Türkiye Bilimsel ve Teknolojik Araştırma Kurumu'na (TÜBİTAK, Proje No: 221M523) teşekkür eder.

Kaynakça

1. Akıllı, A., Taymaz, B. H., Eskizeybek, V., & Kamış, H. (2025). Enhanced performance of MXene-based supercapacitor via new activated carbon-nafion composite cathode. Journal of Physics and Chemistry of Solids, 199, 112523. https://doi.org/10.1016/j.jpcs.2024.112523
2. Alhabeb, M., Maleski, K., Anasori, B., Lelyukh, P., Clark, L., Sin, S., & Gogotsi, Y. (2017). Guidelines for Synthesis and Processing of Two-Dimensional Titanium Carbide (Ti3C2Tx MXene). Chemistry of Materials, 29(18), 7633–7644. https://doi.org/10.1021/acs.chemmater.7b02847
3. Bilal, M., Khan, U., & Ihsanullah, I. (2023). MXenes: The emerging adsorbents for the removal of dyes from water. Journal of Molecular Liquids, 385, 122377. https://doi.org/10.1016/j.molliq.2023.122377
4. Eom, W., Shin, H., Ambade, R. B., Lee, S. H., Lee, K. H., Kang, D. J., & Han, T. H. (2020). Large-scale wet-spinning of highly electroconductive MXene fibers. Nature Communications, 11(1), 2825. https://doi.org/10.1038/s41467-020-16671-1
5. Feng, W., Luo, H., Wang, Y., Zeng, S., Deng, L., Zhou, X., Zhang, H., & Peng, S. (2018). Ti3C2 MXene: a promising microwave absorbing material. RSC Advances, 8(5), 2398–2403. https://doi.org/10.1039/C7RA12616F
6. Ghidiu, M., Lukatskaya, M. R., Zhao, M.-Q., Gogotsi, Y., & Barsoum, M. W. (2014). Conductive two-dimensional titanium carbide ‘clay’ with high volumetric capacitance. Nature, 516(7529), 78–81. https://doi.org/10.1038/nature13970
7. Ghosh, A., Pal, H., Das, T., Chatterjee, S., & Das, A. (2022). Synthesis and Characterization of MXene from MAX phase. Materials Today: Proceedings, 58, 714–716. https://doi.org/10.1016/j.matpr.2022.02.253
8. Guo, F., Kim, F., Han, T. H., Shenoy, V. B., Huang, J., & Hurt, R. H. (2011). Hydration-Responsive Folding and Unfolding in Graphene Oxide Liquid Crystal Phases. ACS Nano, 5(10), 8019–8025. https://doi.org/10.1021/nn2025644

9. Hao, W., Ren, S., Wu, X., Shen, X., & Cui, S. (2023). Recent advance in the construction of 3D porous structure Ti3C2Tx MXene and their multi-functional applications. Journal of Alloys and Compounds, 968, 172219. https://doi.org/10.1016/j.jallcom.2023.172219
10. He, N., Patil, S., Qu, J., Liao, J., Zhao, F., & Gao, W. (2020). Effects of Electrolyte Mediation and MXene Size in Fiber-Shaped Supercapacitors. ACS Applied Energy Materials, 3(3), 2949–2958. https://doi.org/10.1021/acsaem.0c00024
11. Hu, C., Lu, Z., Fang, C., Gao, Y., & Hu, W. (2025). Two-Dimensional MXene Liquid Crystal Morphology Materials: Mechanisms, Modifications, Macro-Formation, and Applications. Journal of Electronic Materials, 54(5), 3370–3388. https://doi.org/10.1007/s11664-025-11876-w
12. Jun, B.-M., Kim, S., Rho, H., Park, C. M., & Yoon, Y. (2020). Ultrasound-assisted Ti3C2Tx MXene adsorption of dyes: Removal performance and mechanism analyses via dynamic light scattering. Chemosphere, 254, 126827. https://doi.org/10.1016/j.chemosphere.2020.126827
13. Khamhanglit, C., Li, T., Sethu Madhavan, V. S., McDonald, J., Switalska, E., Sun, A. R., Xu, Y., Prasadam, I., Gu, Y., Evans, D. R., Leong, W. L., & Sonar, P. (2026). PEDOT:Tosylate on Biocompatible Chitosan Film by Vapor Phase Polymerization: Promising Technology toward Biocompatible and Wearable Organic Electrochemical Transistor. Small Structures, 7(2). https://doi.org/10.1002/sstr.202400642
14. Khiar, A. S. A., Puteh, R., & Arof, A. K. (2006). Conductivity studies of a chitosan-based polymer electrolyte. Physica B: Condensed Matter, 373(1), 23–27. https://doi.org/10.1016/j.physb.2005.10.104
15. Li, J., Miao, C., Bian, J., Seyedin, S., & Li, K. (2023). MXene fibers for electronic textiles: Progress and perspectives. Chinese Chemical Letters, 34(8), 107996. https://doi.org/10.1016/j.cclet.2022.107996
16. Li, S., Chandra Biswas, M., & Ford, E. (2022). Dual roles of sodium polyacrylate in alginate fiber wet-spinning: Modify the solution rheology and strengthen the fiber. Carbohydrate Polymers, 297, 120001. https://doi.org/10.1016/j.carbpol.2022.120001
17. Li, S., Fan, Z., Wu, G., Shao, Y., Xia, Z., Wei, C., Shen, F., Tong, X., Yu, J., Chen, K., Wang, M., Zhao, Y., Luo, Z., Jian, M., Sun, J., Kaner, R. B., & Shao, Y. (2021). Assembly of Nanofluidic MXene Fibers with Enhanced Ionic Transport and Capacitive Charge Storage by Flake Orientation. ACS Nano, 15(4), 7821–7832. https://doi.org/10.1021/acsnano.1c02271
18. Mojtabavi, M., VahidMohammadi, A., Liang, W., Beidaghi, M., & Wanunu, M. (2019). Single-Molecule Sensing Using Nanopores in Two-Dimensional Transition Metal Carbide (MXene) Membranes. ACS Nano, 13(3), 3042–3053. https://doi.org/10.1021/acsnano.8b08017
19. Naficy, S., Jalili, R., Aboutalebi, S. H., Gorkin III, R. A., Konstantinov, K., Innis, P. C., Spinks, G. M., Poulin, P., & Wallace, G. G. (2014). Graphene oxide dispersions: tuning rheology to enable fabrication. Materials Horizons, 1(3), 326–331. https://doi.org/10.1039/C3MH00144J
20. Naguib, M. (2020). Multifunctional Pure MXene Fiber from Liquid Crystals of Only Water and MXene. ACS Central Science, 6(3), 344–346. https://doi.org/10.1021/acscentsci.0c00180
21. Onat, B., Haspulat Taymaz, B., Eskizeybek, V., & Kamış, H. (2025). Optimized size sorting of MXene particles via centrifugal sedimentation: a practical approach using an empirical model and image processing technique. Particulate Science and Technology, 43(5), 756–766. https://doi.org/10.1080/02726351.2025.2486605
22. Onsager, L. (1949). THE EFFECTS OF SHAPE ON THE INTERACTION OF COLLOIDAL PARTICLES. Annals of the New York Academy of Sciences, 51(4), 627–659. https://doi.org/10.1111/j.1749-6632.1949.tb27296.x
23. Peng, Q., Guo, J., Zhang, Q., Xiang, J., Liu, B., Zhou, A., Liu, R., & Tian, Y. (2014). Unique Lead Adsorption Behavior of Activated Hydroxyl Group in Two-Dimensional Titanium Carbide. Journal of the American Chemical Society, 136(11), 4113–4116. https://doi.org/10.1021/ja500506k
24. Quan, J., Jiang, X., Ding, T., Ma, W., Li, M., Lan, C., Xiang, H., Li, W., Zhu, M., & Zhang, Y. (2025). Recent progress in MXene fiber: Materials, fabrication techniques, and potential applications. Chemical Engineering Journal, 503, 158320. https://doi.org/10.1016/j.cej.2024.158320
25. Sarkar, P., Chatterjee, K., Pal, P., & Das, K. (2025). Exploring the molarity of Lithium Fluoride in minimally intensive layer delamination (MILD) method for efficient room temperature synthesis of high quality Ti3C2Tx free-standing film. Materials Science in Semiconductor Processing, 185, 108881. https://doi.org/10.1016/j.mssp.2024.108881
26. Seok, S.-H., Choo, S., Kwak, J., Ju, H., Han, J.-H., Kang, W.-S., Lee, J., Kim, S.-Y., Lee, D. H., Lee, J., Wang, J., Song, S., Jo, W., Jung, B. M., Chae, H. G., Son, J. S., & Kwon, S.-Y. (2021). Synthesis of high quality 2D carbide MXene flakes using a highly purified MAX precursor for ink applications. Nanoscale Advances, 3(2), 517–527. https://doi.org/10.1039/D0NA00398K
27. Shahzad, F., Alhabeb, M., Hatter, C. B., Anasori, B., Man Hong, S., Koo, C. M., & Gogotsi, Y. (2016). Electromagnetic interference shielding with 2D transition metal carbides (MXenes). Science, 353(6304), 1137–1140. https://doi.org/10.1126/science.aag2421
28. Shekhirev, M., Busa, J., Shuck, C. E., Torres, A., Bagheri, S., Sinitskii, A., & Gogotsi, Y. (2022). Ultralarge Flakes of Ti 3 C 2 T x MXene via Soft Delamination. ACS Nano, 16(9), 13695–13703. https://doi.org/10.1021/acsnano.2c04506
29. Shin, H., Eom, W., Lee, K. H., Jeong, W., Kang, D. J., & Han, T. H. (2021). Highly Electroconductive and Mechanically Strong Ti 3 C 2 T x MXene Fibers Using a Deformable MXene Gel. ACS Nano, 15(2), 3320–3329. https://doi.org/10.1021/acsnano.0c10255
30. Taymaz, B. H., Kamış, H., Dziendzikowski, M., Kowalczyk, K., Dragan, K., & Eskizeybek, V. (2025). Enhancing structural health monitoring of fiber-reinforced polymer composites using piezoresistive Ti3C2Tx MXene fibers. Scientific Reports, 15(1), 2456. https://doi.org/10.1038/s41598-024-78338-x
31. Thakur, A., Kim, J., Wyatt, B. C., Gogotsi, Y., & Anasori, B. (2026). Composition–structure–property relationships in MXenes. Nature Reviews Materials, 11(7), 516–531. https://doi.org/10.1038/s41578-026-00911-9
32. Usman, K. A. S., Qin, S., Henderson, L. C., Zhang, J., Hegh, D. Y., & Razal, J. M. (2021). Ti 3 C 2 T x MXene: from dispersions to multifunctional architectures for diverse applications. Materials Horizons, 8(11), 2886–2912. https://doi.org/10.1039/D1MH00968K
33. Wang, B., Lai, X., Li, H., Jiang, C., Gao, J., & Zeng, X. (2021). Multifunctional MXene/Chitosan-Coated Cotton Fabric for Intelligent Fire Protection. ACS Applied Materials & Interfaces, 13(19), 23020–23029. https://doi.org/10.1021/acsami.1c05222
34. Wei, M., Li, Y., Yao, G., Deng, Y., Wu, N., Liu, W., Liu, J., Li, S., Li, Z., Zeng, Z., & Liu, J. (2027). Recent advances in wet spinning MXene-based fiber/textiles for electromagnetic interference shielding. Journal of Materials Science & Technology, 276, 66–81. https://doi.org/10.1016/j.jmst.2026.03.075
35. Wyatt, B. C., Nemani, S. K., Desai, K., Kaur, H., Zhang, B., & Anasori, B. (2021). High-temperature stability and phase transformations of titanium carbide (Ti3C2Tx) MXene. Journal of Physics: Condensed Matter, 33(22), 224002. https://doi.org/10.1088/1361-648X/abe793
36. Xu, Z., & Gao, C. (2011). Graphene chiral liquid crystals and macroscopic assembled fibres. Nature Communications, 2(1), 571. https://doi.org/10.1038/ncomms1583
37. Yang, M., Lou, H., Kong, X., Pang, R., Zhang, D., Meng, W., Li, M., Huang, X., Zhang, S., Shang, Y., & Cao, A. (2023). Recent Advances in MXene‐Based Fibers: Fabrication, Performance, and Application. Small Methods, 7(10). https://doi.org/10.1002/smtd.202300518
38. Zhang, J., Kada, S., Tang, J., Tao, J., Lynch, P. A., Ma, R., & Razal, J. M. (2026). A Knittable Neural‐Inspired MXene‐Aramid Fiber for Wearable High‐Fidelity Signal Transmission. Small Structures, 7(3). https://doi.org/10.1002/sstr.202500884
39. Zhang, J., Uzun, S., Seyedin, S., Lynch, P. A., Akuzum, B., Wang, Z., Qin, S., Alhabeb, M., Shuck, C. E., Lei, W., Kumbur, E. C., Yang, W., Wang, X., Dion, G., Razal, J. M., & Gogotsi, Y. (2020). Additive-Free MXene Liquid Crystals and Fibers. ACS Central Science, 6(2), 254–265. https://doi.org/10.1021/acscentsci.9b01217
40. Zhou, T., Yu, Y., He, B., Wang, Z., Xiong, T., Wang, Z., Liu, Y., Xin, J., Qi, M., Zhang, H., Zhou, X., Gao, L., Cheng, Q., & Wei, L. (2022). Ultra-compact MXene fibers by continuous and controllable synergy of interfacial interactions and thermal drawing-induced stresses. Nature Communications, 13(1), 4564. https://doi.org/10.1038/s41467-022-32361-6
41. Zhou, Y., Zhang, Y., Ruan, K., Guo, H., He, M., Qiu, H., & Gu, J. (2024). MXene-based fibers: Preparation, applications, and prospects. Science Bulletin, 69(17), 2776–2792. https://doi.org/10.1016/j.scib.2024.07.009