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N-induced antibacterial capability of ZrO2-SiO2 glass ceramics by ion implantation
Uppsala University, Disciplinary Domain of Science and Technology, Technology, Department of Materials Science and Engineering, Applied Material Science.ORCID iD: 0009-0005-3234-5649
Uppsala University, Disciplinary Domain of Science and Technology, Technology, Department of Materials Science and Engineering, Applied Material Science.ORCID iD: 0000-0001-9529-650X
Uppsala University, Disciplinary Domain of Science and Technology, Technology, Department of Materials Science and Engineering, Solar Cell Technology.ORCID iD: 0000-0002-2101-3746
Uppsala University, Disciplinary Domain of Science and Technology, Physics, Department of Physics and Astronomy, Applied Nuclear Physics.ORCID iD: 0000-0002-5815-3742
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2025 (English)In: Applied Surface Science, ISSN 0169-4332, E-ISSN 1873-5584, Vol. 683, p. 161836-Article in journal (Refereed) Published
Abstract [en]

Periodontal disease caused by bacterial accumulation is a critical issue affecting the longevity of related materials and implants. Enhancing the antibacterial properties of glass ceramics remains a significant challenge. Due to their excellent mechanical properties, ZrO2-SiO2 glass ceramics have shown great potential in dental restoration. Here, to endow ZrO2-SiO2 glass ceramics with antibacterial properties, nitrogen ion implantation was performed to modify their surfaces. The effects of nitrogen fluence on the microstructural, mechanical and antibacterial properties were investigated. The results showed that phase transformation from tetragonal to monoclinic phase occurred after ion implantation. Surface hardening was observed in the sample under the low fluence ion implantation. Partial amorphization and blistering were observed at the highest fluence of 6.0  1017 ions/cm2. XPS analysis revealed that the implanted nitrogen ions mainly form O-Zr-N, N-Si-O and Si-N bonds. Staphylococcus aureus testing showed that the antibacterial properties of ZrO2-SiO2 glass ceramics can be enhanced after implantation, which may be attributed to the formation of reactive nitrogen species. The results show that nitrogen implantation can enhance the antibacterial properties of ZrO2-SiO2 glass ceramics without compromising their mechanical properties.

Place, publisher, year, edition, pages
Elsevier, 2025. Vol. 683, p. 161836-
National Category
Ceramics and Powder Metallurgical Materials
Identifiers
URN: urn:nbn:se:uu:diva-537934DOI: 10.1016/j.apsusc.2024.161836ISI: 001361493000001OAI: oai:DiVA.org:uu-537934DiVA, id: diva2:1895753
Available from: 2024-09-06 Created: 2024-09-06 Last updated: 2025-02-09Bibliographically approved
In thesis
1. High-performance SiO2 matrix glass ceramics
Open this publication in new window or tab >>High-performance SiO2 matrix glass ceramics
2024 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Silica-based glass ceramics are widely used in biomedical applications due to their exceptional biocompatibility and tailorable properties. However, their application is often limited by low mechanical strength, which can be improved by optimizing the crystalline phase that determines their final properties. Silicon nitride (Si3N4) and Zirconia (ZrO2) are particularly appealing ceramics due to their favorable combination of mechanical strength and biological compatibility. In this thesis, the development of two types of glass ceramics, Si3N4-SiO2 and ZrO2-SiO2 glass ceramics is explored to address these challenges by controlling their microstructure and engineering the nanointerfaces between ceramic/ceramic grains and ceramic grain/glass matrix.

In Si3N4-SiO2 glass ceramics, raw powders containing three different Si3N4 contents were prepared. The results showed that the β-Si3N4 crystalline phase is well distributed within the SiO2 matrix. The mechanical properties of the glass ceramics improved with increasing Si3N4 content and increasing sintering temperature, reaching a maximum flexural strength of 452±33 MPa and fracture toughness of 6.4±0.5 MPa∙m1/2 at 70 wt% Si3N4 composition. The highest antibacterial rate against S. epidermidis was observed in the 50SiN samples, at 79%. 

In the ZrO2-SiO2 glass ceramics, the raw powders with varying types (K+, Mg2+, Al3+, Ce4+, and Ta5+) and amounts of dopants were prepared by a modified sol-gel method. TEM results showed the ZrO2 crystals were embedded within the amorphous SiO2 matrix, with Mg2+, Al3+, and Ce4+ ions primarily segregating at the grain boundaries of ZrO2 crystals while K+ and Ta5+ ions mainly dissolved within the grains. The Mg-doped samples showed the highest toughness at 12.39±1.34 MPa∙m1/2, attributed to the enhanced interfacial strength between the dopants and ZrO2 crystals. FEM simulation shows that enhanced interfacial bonding lead to more diffused cracking and dissipating energy compared to the conventional interfacial weakening theory. The antibacterial performance of the ZrO2-SiO2  was improved by nitrogen ion implantation of the surface. The antibacterial rate against S.aureus reached 49 ± 24% for samples implanted at fluences of 1×1017 ions/cm².

In conclusion, different SiO2 matrix glass ceramics were developed with enhancing mechanical strength and antibacterial properties. The results indicate that these materials hold significant potential for biomedical applications.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2024. p. 66
Series
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1651-6214 ; 2447
Keywords
glass ceramics; silicon nitride; zirconia; toughness; antibacterial properties; spark plasma sintering
National Category
Materials Engineering Bio Materials
Research subject
Engineering Science with specialization in Materials Science
Identifiers
urn:nbn:se:uu:diva-537936 (URN)978-91-513-2226-1 (ISBN)
Public defence
2024-10-25, 101195 Heinz-Otto Kreiss, Ångströmlaboratoriet, Lägerhyddsvägen 1, Uppsala, 09:15 (English)
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Available from: 2024-10-03 Created: 2024-09-07 Last updated: 2024-10-03

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Zhou, HuasiEngqvist, HåkanDonzel-Gargand, OlivierPrimetzhofer, DanielXia, Wei

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