Investigation of Antibacterial Properties of Ti6Al4V Implants Coated with Zinc-Added Materials by the Electrophoretic Method

Öz

Implant materials are biomaterials that are placed within the body to support, repair, or completely replace the function of damaged or missing tissues. These materials must possess properties such as biocompatibility, corrosion resistance, mechanical strength, and biological stability. This study focuses on the preparation of zinc (Zn)-doped hydroxyapatite (HA) coatings on Ti6Al4V alloy implant materials using the electrophoretic deposition (EPD) method, and investigates the microstructural, chemical, and antibacterial properties of the resulting coatings. Various EPD parameters (30–90V, 90s) were tested to assess their effects on coating thickness, surface morphology, and bioactivity. Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray (EDX) analyses revealed that Zn doping improved the coating's density and homogeneity, enhanced surface roughness, and promoted apatite formation. Simulated Body Fluid (SBF) tests confirmed increased bioactivity in the Zn-doped samples. Additionally, antibacterial tests indicated that Zn doping imparted antimicrobial resistance to the coating.

Anahtar Kelimeler

• Electrophoretic deposition (EPD)
• Bioactivity
• Antibacterial
• SBF
• Implant

Elektroforetik Yöntem İle Çinko Katkılı Malzemelerle Kaplanmış Ti6Al4V İmplantların Antibakteriyel Özelliklerinin İncelenmesi

Öz

İmplant malzemeler, vücut içine yerleştirilerek hasarlı veya eksik dokuların işlevini desteklemek, onarmak ya da tamamen yerine geçirmek amacıyla kullanılan biyomalzemelerdir. Bu malzemeler; biyouyumluluk, korozyon direnci, mekanik dayanım ve biyolojik stabilite gibi özelliklere sahip olmalıdır. Bu çalışmada, Ti6Al4V alaşımı implant malzemeler üzerine elektroforetik biriktirme (EPD) yöntemiyle Çinko (Zn) katkılı Hidroksiapatit (HA) kaplamaların hazırlanmasını ve elde edilen kaplamaların mikroyapısal, kimyasal ve antibakteriyel özelliklerinin incelenmesini kapsamaktadır. EPD parametreleri (30-90 V, 90 sn) değiştirilerek kaplama kalınlığı, yüzey morfolojisi ve biyoaktivite üzerindeki etkileri araştırılmıştır. SEM-EDX analizleri Zn katkısının kaplama yoğunluğunu ve homojenliğini artırdığını, yüzey pürüzlülüğünü ve apatit oluşumunu desteklediğini göstermiştir. Sentetik vücut sıvısı (SBF) testleri, Zn katkılı numunelerde biyoaktivitenin arttığını doğrulamıştır. Antibakteriyel sonuçlarda ise Zn katkısının levha üzerindeki kaplamanın antimikrobiyal olarak dayanım gösterdiğini kanıtlamıştır.

Anahtar Kelimeler

• Elektroforetik biriktirme (EPD)
• Biyoaktivite
• Antibakteriyel
• SBF
• İmplant

Kaynakça

1. Akram, W., Zahid, R., Usama, R. M., AlQahtani, S. A., Dahshan, M., Basit, M. A., & Yasir, M. (2023). Enhancement of antibacterial properties, surface morphology and in vitro bioactivity of hydroxyapatite-zinc oxide nanocomposite coating by electrophoretic deposition technique. Bioengineering, 10(6), 693. https://doi.org/10.3390/bioengineering10060693
2. Behera, R. R., Das, A., Pamu, D., Pandey, L. M., & Sankar, M. R. (2018). Mechano-tribological properties and in vitro bioactivity of biphasic calcium phosphate coating on Ti-6Al-4V. Journal of Mechanical Behavior of Biomedical Materials, 86, 143–157. https://doi.org/10.1016/j.jmbbm.2018.06.012
3. Besra, L., & Liu, M. (2007). A review on fundamentals and applications of electrophoretic deposition (EPD). Progress in Materials Science, 52(1), 1–61. https://doi.org/10.1016/j.pmatsci.2006.07.001
4. Bhattacharjee, A., Bandyopadhyay, A., & Bose, S. (2022). Plasma sprayed fluoride and zinc doped hydroxyapatite coated titanium for load-bearing implants. Surface and Coatings Technology, 440, 128464. https://doi.org/10.1016/j.surfcoat.2022.128464
5. Boccaccini, A.R., Keim, S., Ma, R., Li, Y., Zhitomirsky, I. (2010). Electrophoretic deposition of biomaterials. Journal of The Royal Society Interface, 7 (Suppl 5), S581–613. https://doi.org/10.1098/rsif.2010.0156.focus
6. Dornelas, J., Dornelas, G., Rossi, A., Piattelli, A., Di Pietro, N., Romasco, T., Mourão, C. F., & Alves, G. G. (2024). The incorporation of zinc into hydroxyapatite and its influence on the cellular response to biomaterials: A systematic review. Journal of Functional Biomaterials, 15(4), 178. https://doi.org/10.3390/jfb15040178
7. Fathyunes, L., Hosseini, M., & Khalil-Allafi, J. (2024). In-vitro biocompatibility, antibacterial activity, and corrosion resistance of HA-TiO2/ZnO coating fabricated by plasma electrolytic oxidation on Ti6Al4V. Materials Today Communications, 40, 109443. https://doi.org/10.1016/j.mtcomm.2024.109443
8. Hu, X., Mei, S., Wang, F., Tang, S., Xie, D., Ding, C., Du, W., Zhao, J., Yang, L., Wu, Z., Wei, J. (2021). A microporous surface containing Si3N4/Ta microparticles of PEKK exhibits both antibacterial and osteogenic activity for inducing cellular response and improving osseointegration, Bioactive Materials, 6(10), 3136-3149.https://doi.org/10.1016/j.bioactmat.2021.02.027

9. Jahani, B., & Wang, X. (2021). The effects of surface roughness on the functionality of Ti13Nb13Zr orthopedic implants. Biomedical Journal of Scientific & Technical Research, 38(1), 30058–30067. https://doi.org/10.26717/BJSTR.2021.38.006093
10. Jingxuan, L., Tianyu, Z., Ziming, L., Yan, W., Ruiqiang, H., & Di, H. (2023). Engineered functional doped hydroxyapatite coating on titanium implants for osseointegration. Journal of Materials Research and Technology, 27, 122–152. https://doi.org/10.1016/j.jmrt.2023.09.049
11. Krupa, D., Baszkiewicz, J., Rajchel, B., Barcz, A., Sobczak, J. W., Biliński, A., & Borowski, T. (2007). Effect of calcium-ion implantation on the corrosion resistance and bioactivity of the Ti6Al4V alloy. Vacuum, 81(10), 1310–1313. https://doi.org/10.1016/j.vacuum.2007.03.003
12. Lewallen, E. A., Trousdale, W. H., Thâler, R., Yao, J. J., Xu, W., Denbeigh, J. M., & Van Wijnen, A. J. (2021). Surface roughness of titanium orthopedic implants alters the biological phenotype of human mesenchymal stromal cells. Tissue Engineering Part A, 27(23–24), 1503–1516. https://doi.org/10.1089/ten.tea.2021.0029
13. Malheiros, S. S., Borges, M. H. R., Rangel, E. C., Fortulan, C. A., Cruz, N. C. da, Barao, V. A. R., & Nagay, B. E. (2025). Zinc-doped antibacterial coating as a single approach to unlock multifunctional and highly resistant titanium implant surfaces. ACS Applied Materials & Interfaces, 17(12), 18022–18041. https://doi.org/10.1021/acsami.5b00000
14. Pani, R., Behera, R. R., & Roy, S. (2022). Electrophoretic deposition of hydroxyapatite coating: A state of art. Materials Today: Proceedings, 62(6), 4086–4093. https://doi.org/10.1016/j.matpr.2022.03.497
15. Pantoja-Pertegal, J. L., Diaz-Parralejo, A., Macias-Garcia, A., Sánchez-González, J., & Cuerda-Correa, E. M. (2021). Design, preparation, and characterization of Yttria-Stabilized Zirconia (YSZ) coatings obtained by electrophoretic deposition (EPD). Ceramics International, 47(10), 13312–13321. https://doi.org/10.1016/j.ceramint.2021.01.196
16. Rachele, S., Bellucci, D., Candidato, R.T., Lusvarghi, L., Bolelli, G., Pawlowski, L., Candiani, G., Altomare, L., Nardo, L. N., Cannillo, V. (2018). Bioactive Zn-doped hydroxyapatite coatings and their antibacterial efficacy against Escherichia coli and Staphylococcus aureus. Surface and Coatings Technology, 35, 84-91. https://doi.org/10.1016/j.surfcoat.2018.08.017
17. Rezić, I., & Meštrović, E. (2023). Characterization of nanoparticles in antimicrobial coatings for medical applications—A review. Coatings, 13(11), 1830. https://doi.org/10.3390/coatings13111830
18. Safavi, M. S., Walsh, F. C., Surmeneva, M. A., Surmenev, R. A., & Khalil-Allafi, J. (2021). Electrodeposited Hydroxyapatite-Based Biocoatings: Recent progress and future challenges. Coatings, 11(1), 110. https://doi.org/10.3390/coatings11010110
19. Uysal, İ., Yılmaz, B., & Evis, Z. (2021). Zn-doped hydroxyapatite in biomedical applications. Journal of the Australian Ceramic Society, 57(4), 869–897. https://doi.org/10.1007/s41779-021-00624-9
20. Vranceanu, D. M., Ungureanu, E., Ionescu, I. C., Parau, A. C., Pruna, V., Titorencu, I., Badea, M., Gălbău, C. Ş., Idomir, M., Dinu, M., Dragomir, A. V., & Cotrut, C. M. (2024). In vitro characterization of hydroxyapatite-based coatings doped with Mg or Zn electrochemically deposited on nanostructured titanium. Biomimetics, 9(4), 244. https://doi.org/10.3390/biomimetics9040244
21. Wu, Y., Wan, K., Lu, J., Yuan, C., Cui, Y., Duan, R., & Yu, J. (2025). Research progress on surface modification of titanium implants. Coatings, 15(2), 229. https://doi.org/10.3390/coatings15020229
22. Zhang, H., Wu, Z., Wang, Z., Yan, X., Duan, X., & Sun, H. (2025). Advanced surface modification techniques for titanium implants: a review of osteogenic and antibacterial strategies. Frontiers in Bioengineering and Biotechnology, 13, 1549439. https://doi.org/10.3389/fbioe.2025.1549439