Yüzey modifiye LDPE mikrofiber katkılı PMMA kompozit üretimi ve mekanik karakterizasyonu

Öz

Polimetil metakrilat (PMMA), estetik görünümü, biyouyumluluğu ve işlenebilirliği nedeniyle restoratif diş hekimliğinde kullanılmaktadır. Ancak kırılganlığı uzun vadeli performansını kısıtlamaktadır. Bu çalışmada, PMMA’nın mekanik ve arayüz özelliklerini iyileştirmek amacıyla, plazma modifiye edilmiş elektrostatik eğirme yöntemiyle üretilen düşük yoğunluklu polietilen (LDPE) mikrofiberler kullanılmış ve akrilik reçine içerisinde farklı fiber yerleşimlerinin etkileri incelenmiştir. LDPE fiberleri matris arasındaki arayüz etkileşimini artırmak amacıyla plazma polimerizasyonu yoluyla 2-hidroksietil metakrilat (HEMA) ile kaplanmıştır. Temas açısı ölçümleri, yüzey modifikasyonunun başarısını doğrulamış, işlem görmemiş LDPE için 121,4°'den plazma sonrasında 16,2°'ye düşüş göstermiştir. Mekanik testler, plazma modifiyeli fiberin farklı yönlendirmeler ile eklemenin PMMA'nın genel performansını kontrol grubuna kıyasla iyileştirdiğini ortaya koymuştur (eğilme dayanımı: 2,544 ± 0,891 MPa; elastik modül: 0,377 ± 0,08 GPa; tokluk: 88010 ± 4410 kJ/m²). Elektrostatik eğirme yöntemiyle üretilmiş LDPE fiberli kompozitlerde, paralel hizalama eğilme dayanımını 5,145 ± 0,176 MPa'ya, elastik modülünü 1,223 ± 0,086 GPa'ya ve tokluğu 115807 ± 1724 kJ/m²'ye çıkarmıştır. Dik hizalamada sırasıyla 5,141 ± 1,54 MPa, 1,039 ± 0,058 GPa ve 199304 ± 3062 kJ/m² basınç üretmiştir. MTT sonuçları, hücre canlılığında istatistiksel olarak anlamlı bir azalma olmadığını (Kontrol: 0,407; Kompozit: 0,3896) gösterirmiştir. Sonuç olarak, plazma modifiye HEMA-LDPE mikrofiberler, PMMA’nın ıslanabilirliğini, mekanik performansını ve arayüz yapışmasını artırarak diş uygulamaları için umut verici yaklaşım sunmaktadır.

Anahtar Kelimeler

• “PMMA”
• “Polietilen”
• “Elektrostatik eğirme”
• “Plazma modifikasyonu”
• “Diş hekimliği”

Teşekkür

Tez çalışmasına katkılarından ötürü Prof. Dr. Emir Baki Denkbaş’a şükranlarımızı sunarız.

Production of surface-modified LDPE microfiber-reinforced PMMA composites and mechanical characterization

Öz

Polymethyl methacrylate (PMMA) is widely used in restorative dentistry due to its aesthetic appearance, biocompatibility, and ease of processing. However, its brittleness and limited fracture toughness limit its long-term performance. In this study, low-density polyethylene (LDPE) microfibers produced by electrospinning and treated with plasma modification were reinforced to improve the mechanical and interfacial properties of PMMA. The LDPE fibers were then coated with 2-hydroxyethyl methacrylate (HEMA) via plasma polymerization to increase adhesion between the fiber and the matrix. Contact angle measurements confirmed the success of the surface modification and showed a significant decrease from 121.4° for untreated LDPE to 16.2° after plasma treatment, indicating a significant increase in wettability. Mechanical tests revealed that adding plasma-modified fiber improved the overall performance of PMMA compared to the control group (flexural strength: 2.544 ± 0.891 MPa; elastic modulus: 0.377 ± 0.08 GPa; toughness: 88.010 ± 4.410 kJ/m²). In the composites with electrospun LDPE fibers, parallel alignment increased the flexural strength to 5.145 ± 0.176 MPa, the elastic modulus to 1.223 ± 0.086 GPa, and the toughness to 115.807 ± 1,724 kJ/m². Perpendicular alignment produced pressures of 5.141 ± 1.54 MPa, 1.039 ± 0.058 GPa, and 199.304 ± 3,062 kJ/m², respectively. MTT experiment results confirmed biocompatibility by showing no statistically significant decrease in cell viability (Control: 0.407; Composite: 0.3896). Overall, plasma-modified HEMA-coated LDPE microfibers showed strong potential for restorative dental applications by effectively enhancing the hydrophilicity, mechanical strength, and interfacial adhesion of PMMA without compromising biocompatibility.

Anahtar Kelimeler

• “PMMA”
• “Polyetyhlene”
• “Electro-spinning”
• “Plasma-modification”
• “Dentistry”

Teşekkür

We would like to express our gratitude to Prof. Dr. Emir Baki Denkbaş for his contributions to thesis.

Kaynakça

1. 1. Deb S., Polymers in dentistry, Proceedings of the Institution of Mechanical Engineers, Part H: Journal of Engineering in Medicine, 212 (6), 453-464, 1998.
2. 2. Kostić M., Igić M., Gligorijević N., Nikolić V., Stošić N., Nikolić L., The Use of Acrylate Polymers in Dentistry, Polymers, 14 (21), 4511, 2022.
3. 3. Uzunoğlu T., Altınten A., Synthesis and characterization of PMMA/PLA/clay biodegradable nanocomposites, Journal of the Faculty of Engineering and Architecture of Gazi University, 39 (4), 2163-2176, 2024.
4. 4. Gad M.M., Fouda S.M., Al-Harbi F.A., Näpänkangas R., Raustia A., PMMA denture base material enhancement: A review of fiber, filler, and nanofiller addition, International Journal of Nanomedicine, 12, 3801-3812, 2017.
5. 5. Raszewski Z., Nowakowska-Toporowska A., Nowakowska D., Więckiewicz W., Update on Acrylic Resins Used in Dentistry, Mini-Reviews in Medicinal Chemistry, 21 (15), 2130-2137, 2021.
6. 6. Al-Harbi F.A., Abdel-Halim M.S., Gad M.M., Fouda S.M., Baba N.Z., AlRumaih H.S., Akhtar S., Effect of Nanodiamond Addition on Flexural Strength, Impact Strength, and Surface Roughness of PMMA Denture Base, Journal of Prosthodontics, 28 (1), e417-e425, 2019.
7. 7. Alhareb A.O., Ahmad Z.A., Effect of Al2O3/ZrO2 reinforcement on the mechanical properties of PMMA denture base, Journal of Reinforced Plastics and Composites, 30 (1), 86-93, 2011.
8. 8. Tacir I.H., Kama J.D., Zortuk M., Eskimez S., Flexural properties of glass fibre reinforced acrylic resin polymers, Australian Dental Journal, 51 (1), 52-56, 2006.

9. 9. Chow W.S., Loo Y.K., Ariffin A., Arifin Z., Ishak M., Flexural Properties of Hydroxyapatite Reinforced Poly(Methyl Methacrylate) Composites, Journal of Reinforced Plastics and Composites, 27 (9), 945-952, 2008.
10. 10. Kilfoil B.M., Hesby R.A., Pelleu G.B., The tensile strength of a composite resin reinforced with carbon fibers, The Journal of Prosthetic Dentistry, 50 (1), 40-43, 1983.
11. 11. Saha S., Pal S., Mechanical characterization of commercially made carbon-fiber-reinforced polymethylmethacrylate, Journal of Biomedical Materials Research, 20 (6), 817-826, 1986.
12. 12. Apimanchindakul C., Na Nan P., Aimjirakul N., Effect of Reinforced Self-Cured Acrylic Resin on Flexural Strength, International Journal of Dentistry, 2022 (1), 2698995, 2022.
13. 13. Karaman A.I., Kir N., Belli S., Four applications of reinforced polyethylene fiber material in orthodontic practice, American Journal of Orthodontics and Dentofacial Orthopedics, 121 (6), 650-654, 2002.
14. 14. Mangoush E., Säilynoja E., Prinssi R., Lassila L., Vallittu P.K., Garoushi S., Comparative evaluation between glass and polyethylene fiber reinforced composites: A review of the current literature, Journal of Clinical and Experimental Dentistry, 9 (12), e1408, 2017.
15. 15. Ferrando C.Á., Murillo A.A., Cascales R.F., Agustin-Panadero R., Sauro S., Carreras-Presas C.M., Hirata R., Lijnev A., Revolutionizing Restorative Dentistry: The Role of Polyethylene Fiber in Biomimetic Dentin Reinforcement—Insights from In Vitro Research, Journal of Functional Biomaterials, 16 (2), 38, 2025.
16. 16. Ronca S., Polyethylene, Brydson’s Plastics Materials, Cilt 8, Editör: Marianne Gilbert, Oxford, İngiltere, 247-278, 2017.
17. 17. Demirors M., The history of polyethylene, ACS Symposium Series, 1080, 115-145, 2011.
18. 18. Shen S., Henry A., Tong J., Zheng R., Chen G., Polyethylene nanofibres with very high thermal conductivities, Nature Nanotechnology, 5 (4), 251-255, 2010.
19. 19. Liu X., Wang C., Cai Z., Hu Z., Zhu P., Fabrication and characterization of polyacrylonitrile and polyethylene glycol composite nanofibers by electrospinning, Journal of Energy Storage, 53, 105171, 2022.
20. 20. Vidotti H.A., Manso A.P., Leung V., Do Valle A.L., Ko F., Carvalho R.M., Flexural properties of experimental nanofiber reinforced composite are affected by resin composition and nanofiber/resin ratio, Dental Materials, 31 (9), 1132-1141, 2015.
21. 21. Uyar T., Çökeliler D., Doğan M., Koçum I.C., Karatay O., Denkbaş E.B., Electrospun nanofiber reinforcement of dental composites with electromagnetic alignment approach, Materials Science and Engineering: C, 62, 762-770, 2016.
22. 22. Kanbir Ö., Çavdar K., The effect of atmospheric pressure plasma treatment on the wettability and aging behavior of metal material surfaces, Journal of the Faculty of Engineering and Architecture of Gazi University, 39 (3), 1825-1836, 2024.
23. 23. Zebarjad S.M., Sajjadi S.A., Sdrabadi T.E., Sajjadi S.A., Yaghmaei A., Naderi B., A Study on Mechanical Properties of PMMA/Hydroxyapatite Nanocomposite, Engineering, 3 (8), 795-801, 2011.
24. 24. Karbhari V.M., Strassler H., Effect of fiber architecture on flexural characteristics and fracture of fiber-reinforced dental composites, Dental Materials, 23 (8), 960-968, 2007.
25. 25. Karbhari V.M., Wang Q., Influence of triaxial braid denier on ribbon-based fiber reinforced dental composites, Dental Materials, 23 (8), 969-976, 2007.
26. 26. Ratner B.D., Hoffman A.S., Schoen F.J., Lemons J.E., Biomaterials Science: An Introduction to Materials in Medicine, Academic Press, Oxford, İngiltere, 1996.
27. 27. Özdilek E., Samatya Yılmaz S., Aytac A., Production of liquid absorbent hollow nanofibers from hydrophobic poly(lactic acid) with optimum poly(butylene succinate) additive ratio, Journal of the Faculty of Engineering and Architecture of Gazi University, 40 (3), 1903-1920, 2025.
28. 28. Bayram C., Demirbilek M., Çalışkan N., Demirbilek M.E., Denkbaş E.B., Osteoblast Activity on Anodized Titania Nanotubes: Effect of Simulated Body Fluid Soaking Time, Journal of Biomedical Nanotechnology, 8 (3), 482-490, 2012.
29. 29. Majumdar P., Singh S.B., Dhara S., Chakraborty M., Influence of boron addition to Ti–13Zr–13Nb alloy on MG63 osteoblast cell viability and protein adsorption, Materials Science and Engineering: C, 46, 62-68, 2015.
30. 30. Catauro M., Bollino F., Papale F., Gallicchio M., Pacifico S., Influence of the polymer amount on bioactivity and biocompatibility of SiO2/PEG hybrid materials synthesized by sol–gel technique, Materials Science and Engineering: C, 48, 548-555, 2015.
31. 31. Anirudhan T.S., Divya P.L., Nima J., Synthesis and characterization of silane coated magnetic nanoparticles/glycidylmethacrylate-grafted-maleated cyclodextrin composite hydrogel as a drug carrier for the controlled delivery of 5-fluorouracil, Materials Science and Engineering: C, 55, 471-481, 2015.
32. 32. Solouk A., Cousins B.G., Mirzadeh H., Seifalian A.M., Application of plasma surface modification techniques to improve hemocompatibility of vascular grafts: A review, Biotechnology and Applied Biochemistry, 58 (5), 311-327, 2011.