Somayeh Azizi , Mohammad Hossein Ehsani , Amir Zareidoost , Atena Malakpour-Permlid , Anja Boisen , Fatemeh Ajalloueian
{"title":"在可生物降解的Mg上化学转化(Zr-Nb)薄膜制备用于骨固定的新型锆酸钠层的制备和表征","authors":"Somayeh Azizi , Mohammad Hossein Ehsani , Amir Zareidoost , Atena Malakpour-Permlid , Anja Boisen , Fatemeh Ajalloueian","doi":"10.1016/j.ceramint.2025.01.534","DOIUrl":null,"url":null,"abstract":"<div><div>Biodegradable Mg alloys have considerable promise for use in bone-fixation devices. Nonetheless, their clinical application is limited due to the high degradation rate of Mg, leading to deterioration of the mechanical properties, and drastic change in pH of the surrounding cellular environment of the implant during the healing process. Recently, the use of Na-containing biocompatible coatings on the Mg surface has created an innovative approach to overcome the above problems. In this study, a newly developed sodium–containing zirconate hydrogel layer with an amorphous structure has been designed and prepared through modification of the Nb-containing (Zr-Nb) thin films sputtered directly on pure Mg using wet chemical conversion in aqueous NaOH solution. The results of the Grazing incidence angle X-ray diffraction (GI-XRD), X-ray photoelectron spectroscopy (XPS), and Energy dispersive Spectroscopy (EDS) analyses have certified the formation of the desired layer on top of the thin films, indicating that ion exchange and chemical conversion between the surface layers and solution has been limited to less than 200 nm from the (Zr-Nb) thin film thickness, but without the morphological changes in the thin film's surface layers. In terms of reducing Mg degradation, the NaOH-treated sample has been demonstrated to be superior, compared to the other samples tested, representing a decrease in the corrosion rate (CR) from 3.49 mm.y<sup>−1</sup> to 0.75 mm.y<sup>−1</sup>, increase in the corrosion resistance (Rp) from 181.32 Ω cm<sup>2</sup> to 1911 Ω cm<sup>2</sup>. This increase in corrosion resistance can be ascribed to the Na <sup>+</sup> ions released from the modified layers, resulting in a change in the pH and composition of the surrounding solution environment. Mechanically, the indentation and nano-scratch testing results have explained a slight increase in Young's modulus of the NaOH-treated thin film compared to the untreated one and maintained the thin film's scratch properties after and before the chemical surface treatment which can be attributed to the thickness (<200 nm) of the modified layer. Cell culture studies have demonstrated enhanced cell viability of MG-63 cells in the NaOH-modified surfaces compared to the un-modified ones. These results demonstrate that the zirconate sodium layers have created the protective effect, appropriate cellular response, and nano-mechanical properties illustrating their potential for use in biodegradable bone-fixation devices.</div></div>","PeriodicalId":267,"journal":{"name":"Ceramics International","volume":"51 13","pages":"Pages 17607-17622"},"PeriodicalIF":5.1000,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Fabrication and characterization of novel sodium zirconate layers produced via chemical conversion of (Zr-Nb) thin films on biodegradable Mg for bone-fixation applications\",\"authors\":\"Somayeh Azizi , Mohammad Hossein Ehsani , Amir Zareidoost , Atena Malakpour-Permlid , Anja Boisen , Fatemeh Ajalloueian\",\"doi\":\"10.1016/j.ceramint.2025.01.534\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><div>Biodegradable Mg alloys have considerable promise for use in bone-fixation devices. Nonetheless, their clinical application is limited due to the high degradation rate of Mg, leading to deterioration of the mechanical properties, and drastic change in pH of the surrounding cellular environment of the implant during the healing process. Recently, the use of Na-containing biocompatible coatings on the Mg surface has created an innovative approach to overcome the above problems. In this study, a newly developed sodium–containing zirconate hydrogel layer with an amorphous structure has been designed and prepared through modification of the Nb-containing (Zr-Nb) thin films sputtered directly on pure Mg using wet chemical conversion in aqueous NaOH solution. The results of the Grazing incidence angle X-ray diffraction (GI-XRD), X-ray photoelectron spectroscopy (XPS), and Energy dispersive Spectroscopy (EDS) analyses have certified the formation of the desired layer on top of the thin films, indicating that ion exchange and chemical conversion between the surface layers and solution has been limited to less than 200 nm from the (Zr-Nb) thin film thickness, but without the morphological changes in the thin film's surface layers. In terms of reducing Mg degradation, the NaOH-treated sample has been demonstrated to be superior, compared to the other samples tested, representing a decrease in the corrosion rate (CR) from 3.49 mm.y<sup>−1</sup> to 0.75 mm.y<sup>−1</sup>, increase in the corrosion resistance (Rp) from 181.32 Ω cm<sup>2</sup> to 1911 Ω cm<sup>2</sup>. This increase in corrosion resistance can be ascribed to the Na <sup>+</sup> ions released from the modified layers, resulting in a change in the pH and composition of the surrounding solution environment. Mechanically, the indentation and nano-scratch testing results have explained a slight increase in Young's modulus of the NaOH-treated thin film compared to the untreated one and maintained the thin film's scratch properties after and before the chemical surface treatment which can be attributed to the thickness (<200 nm) of the modified layer. Cell culture studies have demonstrated enhanced cell viability of MG-63 cells in the NaOH-modified surfaces compared to the un-modified ones. These results demonstrate that the zirconate sodium layers have created the protective effect, appropriate cellular response, and nano-mechanical properties illustrating their potential for use in biodegradable bone-fixation devices.</div></div>\",\"PeriodicalId\":267,\"journal\":{\"name\":\"Ceramics International\",\"volume\":\"51 13\",\"pages\":\"Pages 17607-17622\"},\"PeriodicalIF\":5.1000,\"publicationDate\":\"2025-05-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Ceramics International\",\"FirstCategoryId\":\"88\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S0272884225005917\",\"RegionNum\":2,\"RegionCategory\":\"材料科学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q1\",\"JCRName\":\"MATERIALS SCIENCE, CERAMICS\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Ceramics International","FirstCategoryId":"88","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0272884225005917","RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"MATERIALS SCIENCE, CERAMICS","Score":null,"Total":0}
Fabrication and characterization of novel sodium zirconate layers produced via chemical conversion of (Zr-Nb) thin films on biodegradable Mg for bone-fixation applications
Biodegradable Mg alloys have considerable promise for use in bone-fixation devices. Nonetheless, their clinical application is limited due to the high degradation rate of Mg, leading to deterioration of the mechanical properties, and drastic change in pH of the surrounding cellular environment of the implant during the healing process. Recently, the use of Na-containing biocompatible coatings on the Mg surface has created an innovative approach to overcome the above problems. In this study, a newly developed sodium–containing zirconate hydrogel layer with an amorphous structure has been designed and prepared through modification of the Nb-containing (Zr-Nb) thin films sputtered directly on pure Mg using wet chemical conversion in aqueous NaOH solution. The results of the Grazing incidence angle X-ray diffraction (GI-XRD), X-ray photoelectron spectroscopy (XPS), and Energy dispersive Spectroscopy (EDS) analyses have certified the formation of the desired layer on top of the thin films, indicating that ion exchange and chemical conversion between the surface layers and solution has been limited to less than 200 nm from the (Zr-Nb) thin film thickness, but without the morphological changes in the thin film's surface layers. In terms of reducing Mg degradation, the NaOH-treated sample has been demonstrated to be superior, compared to the other samples tested, representing a decrease in the corrosion rate (CR) from 3.49 mm.y−1 to 0.75 mm.y−1, increase in the corrosion resistance (Rp) from 181.32 Ω cm2 to 1911 Ω cm2. This increase in corrosion resistance can be ascribed to the Na + ions released from the modified layers, resulting in a change in the pH and composition of the surrounding solution environment. Mechanically, the indentation and nano-scratch testing results have explained a slight increase in Young's modulus of the NaOH-treated thin film compared to the untreated one and maintained the thin film's scratch properties after and before the chemical surface treatment which can be attributed to the thickness (<200 nm) of the modified layer. Cell culture studies have demonstrated enhanced cell viability of MG-63 cells in the NaOH-modified surfaces compared to the un-modified ones. These results demonstrate that the zirconate sodium layers have created the protective effect, appropriate cellular response, and nano-mechanical properties illustrating their potential for use in biodegradable bone-fixation devices.
期刊介绍:
Ceramics International covers the science of advanced ceramic materials. The journal encourages contributions that demonstrate how an understanding of the basic chemical and physical phenomena may direct materials design and stimulate ideas for new or improved processing techniques, in order to obtain materials with desired structural features and properties.
Ceramics International covers oxide and non-oxide ceramics, functional glasses, glass ceramics, amorphous inorganic non-metallic materials (and their combinations with metal and organic materials), in the form of particulates, dense or porous bodies, thin/thick films and laminated, graded and composite structures. Process related topics such as ceramic-ceramic joints or joining ceramics with dissimilar materials, as well as surface finishing and conditioning are also covered. Besides traditional processing techniques, manufacturing routes of interest include innovative procedures benefiting from externally applied stresses, electromagnetic fields and energetic beams, as well as top-down and self-assembly nanotechnology approaches. In addition, the journal welcomes submissions on bio-inspired and bio-enabled materials designs, experimentally validated multi scale modelling and simulation for materials design, and the use of the most advanced chemical and physical characterization techniques of structure, properties and behaviour.
Technologically relevant low-dimensional systems are a particular focus of Ceramics International. These include 0, 1 and 2-D nanomaterials (also covering CNTs, graphene and related materials, and diamond-like carbons), their nanocomposites, as well as nano-hybrids and hierarchical multifunctional nanostructures that might integrate molecular, biological and electronic components.